ANKA Annual Report 2012 · with 65 of these being allocated beam-time. For Call 20 there were 105...

www.kit.edu

ANKA Annual Report 2012

www.anka.kit.edu

anka Synchrotron radiation facility

kit – University of the State Baden-Württemberg and national laboratory of the helmholtz association

AN

KA

An

nu

al R

epo

rt 2

012

www.kit.edu

Appendix

ANKA Publications 2012 92ANKA Seminars 98 Users´ Meeting 2012 102

Lab Report

Chemistry Lab 74Femtolab 76Laser Lab 78UHV Lab 80

Applications

Instrumentation 86Method development 86Applications 88

User Operation

FLUO 34INE 36IR1 38IR2 40SUL-X 42UV-CD 12 44WERA 46XAS 48MPI 52NANO 54PDIFF 58SCD 60IMAGE 62TOPO-TOMO 64LIGA I, II, II 68KNMF Laboratory for Synchrotron Radiation 70

BeamlinesAccelerator Report

ANKA Storage Ring Operation 14Accelerator Science and Technology 16Insertion Devices 26

Beamlines in Operation 6CALIPSO 8ANKA User Operation: Key Figures 10

Content

dfhkjsdf Dear Users, Friends and Partners of ANKA, 2012 was a year of high activity and of many good things happening at ANKA. The process of extending the ANKA hall is ongoing, with the design, installation, commissioning and upgrade of several beamlines. Construction has more or less been completed of the various ANKA hall extensions which will house the new beamlines and laboratories at the facility, and the unique laboratory infrastructure at ANKA has also expanded significantly - and all of this despite very tight resources!

On the accelerator front there has been significant progress in ANKA’s superconducting insertion device program, with the construction of the SCU15 & SCU20 undulators together with Babcock-Noell, and the collaboration with CERN and the Budker Institute to develop damping wigglers. In addition the ongoing program of replacement and refurbishment of power supplies and RF components and the introduction of new BPMs and a fast-feedback system signal improvements for the beam stability and operational reliability of the storage ring.

Installation and commissioning of the MOVPE Laboratory as part of the infrastructure for the NANO beamline has also progressed in 2012 which will pave the way for first in-situ studies of semiconductor growth at ANKA. An important part of the ANKA beamline program has been the installation of the new X-ray bio-microscope at NANO 2. This microscope will eventually be installed at the IMAGE beamline but will be commissioned and operated at NANO until the completion of the IMAGE beamline in 2015. At the IMAGE beamline hutch-building has been completed and temporary optics have been installed to perform initial experiments using white-beam tomographic methods. Specification and design of the optics and end-stations for the IMAGE/XMIC twin-beamlines is now in progress.

At the management and administrative level one important development was the re-structuring of the former Institute for Synchrotron Radiation (ISS) into two new organizational entities: the new Institute for Photon Science and Synchrotron Radiation (IPS) and the synchrotron radiation facility ANKA. The former is engaged in research activities centered around ANKA and other synchrotron sources while the organization ANKA is now responsible for operation of the storage ring itself. As such ANKA now has the status of an independent and full-fledged German National User Facility, with a particular research focus on THz/IR radiation and medium-energy X-rays.

Since June 2012 three new synchrotron technologies - X-Ray Absorption Spectroscopy, Polycrystalline Diffraction and Infrared/THz Spectroscopy & Ellipsometry - have been added to the KNMF portfolio, giving users access to three beamlines at ANKA which can now be applied for via the KNMF Web-portal.

In the coming years ANKA aims to further develop the unique integrated beamline and laboratory infrastructure at its disposal, with the mission to provide an outstanding research environment to an international user community. In addition, new in-house research & education programs are

currently being set up to ensure the continued excellent scientific output of KIT-internal research as well.

Of course 2013 will be a further busy year at ANKA, with preparations for POF 3 which is on the horizon. The high motivation of the ANKA staff and the strong support both from within KIT and from our external user community puts us in a good position to face these challenges.

In this spirit we want to thank all our users, staff and friends for the great support in 2012!

Tilo Baumbach, Anke-Susanne Müller and Clemens Heske

4

User Operation

Beamlines in Operation

CALIPSO

ANKA User Operation: Key Figures

User Operation

2012 ANKA ANNUAL REPORT | 76

Spectroscopy Beamlines

Beamline Technical Application Status

FLUO

XAS

INE

SUL-X

WERA

IR1

IR2

UV-CD12

X-ray fluorescence analysis (XRF), X-ray fluorescence microprobe (µ-XRF), total X-ray reflection fluorescence (TXRF)

Extended X-ray absorption fine structure (EXAFS), X-ray absorption near-edge structure (XANES), Q-EXAFS

Spectroscopy of actinide samples, multiple spectroscopy techniques, microscopy, diffraction methods

Soft X-ray spectroscopy, microscopy, and spectromicroscopy: PES, NEXAFS, SXMCD, imaging (PEEM), µ-PES, µ-NEXAFS, µ-SXMCD

Infrared/THz spectroscopy, ellipsometry

Infrared/THz spectroscopy, microspectroscopy, imaging, near-field nanospectroscopy

MicrofabricationBeamlines

X-ray diffraction (XRD), X-ray fluorescence spectroscopy (XRF), X-ray absorption spectroscopy in µ-focus

VUV / UV circular dichroism spectroscopy, oriented circular dichroism spectroscopy (OCD)


Scattering & ImagingBeamlines


PDIFF

SCD

NANO

MPI

TOPO-TOMO

IMAGE

Operational

Operational

In Commissioning

Operational

In Commissioning

In Commissioning

X-ray powder diffraction, ins-situ XRD, Röntgenography

Single crystal diffraction, SAD/MAD, ex-situ characterisation of (nanostructured) surfaces and interfaces with XRD, XRR, GID, GISAXS

X-ray diffraction (HR-XRD) with highest angular resolution, anomalous scattering, coherent scattering

Surface diffraction, XMCD

Topography, tomography, radiography

Radiography, tomography

LIGA I

LIGA II

LIGA III

X-ray lithography, Mask fabrication, patterning of thin microstructures

Deep X-ray lithography

Ultra-deep X-ray lithography

Operational

Operational

Operational

Operational

Operational

Operational

Operational

Operational

Operational

In Commissioning

Operational

Beamlines in Operation

Beamlines in Operation | CALIPSO | User Operation

User Operation Accelerator Report Beamline Report Lab Report Applications Appendix


The CALIPSO integrated infrastructure initiative (Coordinated Access to Lightsources to Promote Standards and Optimization) provides support for EU funded experiments to 14 European synchrotrons and free electron lasers, including ANKA. The Transnational Access Program, as for the previous ELISA initiative, will offer travel and subsistence for users from outside Germany. The program has started in June 2012 and will last until May 2015. The ANKA User Office welcomes applications for support through the CALIPSO initiative. In addition, a single entry point for applications for beamtime is currently under development as one of the major work packages to foster access to large scale facilities (see www.wayforlight.eu). CALIPSO also supports the European Synchrotron User Organisation (http://www.esuo.org).

CALIPSO Coordinated Access to Lightsources to Promote Standards and Optimization

Michael Hagelstein: [email protected]

COntACtBeamlines in Operation | CALIPSO | User Operation


COntACt


Modes of user operationANKA normally runs in one of two modes of user operation: • normal user operation (UO) at 2.5 GeV for hard and soft X-ray

applications, infrared spectroscopy and deep X-ray lithography, and• at 1.3 GeV for Terahertz and coherent IR research, and time-resolved

experiments which require use of the pulsed time-structure of the stored electron beam.

The storage ring was scheduled to provide a total of 108 days for normal user operation (2.5GeV) in 2012 with an additional 24 days for special user operation (SUO) at 1.3GeV. As a result of intermittent RF problems there were 10 days of regular UO lost, reducing the availability for users to around 90%. Further details can be found in the section on accelerator operation in this report.

Access to AnKAAccess to ANKA is via two proposal review rounds, held each year for the scheduling periods from October to March and April to September, respectively. Proposals are submitted via the user web portal system ANNA. Proposals are peer-reviewed based on scientific excellence by the ANKA Peer Review Committee (ANKA-PRC). Beamtime is free of charge provided that results are intended for publication in the scientific community. Since 2012 proposals for specific beamlines (X-ray absorption spectroscopy, powder diffraction, soft x-ray spectroscopy, and IR/THz spectroscopy) can also be submitted via the Karlsruhe Nano Micro Facility (KNMF) portal for scientific applications requiring access to both KNMF and ANKA facilities.

CallsDue to the fact that the award of beam-time for users is made half-yearly, with scheduling periods running from April to September and October to March, the number of proposals allocated beam-time in 2012 covers in fact

one full allocation period (Call 19, April 2012-September 2012) and two partial allocation periods (Call 18, October 2011-March 2012 and Call 20, October 2012-March 2013). For Calls 18 and 19 a total of 164 proposals were received for review by the ANKA Proposal Review Committee (PRC) with 65 of these being allocated beam-time. For Call 20 there were 105 proposals submitted, of which 42 were allocated beam-time. This is a factor of about 2.5 in the ratio of submitted to successful proposals, an increase of about 10% on the previous year.

Research fieldsThe distribution of scientific fields for proposals awarded beamtime in 2012 is shown in Figure 1. It can be seen that a large spectrum of research areas is represented at ANKA. The large fractions of beam-time for actinide, environmental and nano-micro research reflects the importance of these key areas in the scientific activities of KIT.

PublicationsIn 2012 the ANKA user community produced over 170 peer-reviewed publications . A selection of the most important scientific activities during the reporting period can be found in the ANKA Highlights Broschure 2012 while a complete list of refereed publications for 2012 can be found in the Appendix of this Annual Report (page 94).

AnKA User Operation: Key Figures

Research fields for proposals granted beam-time in 2012

Michael Hagelstein: [email protected] User Operation Accelerator Report Beamline Report Lab Report Applications Appendix

COntACt

Affiliation of AnKA users in 2012

Affiliation of German users in 2012

Beamlines in Operation | CALIPSO | User Operation

12

Accelerator Report

Storage Ring Operation

Accelerator Science and Technology

Accelerator Report


AnKA Storage Ring Operation in 2012


COntACt

ANKA is generally operated at an energy of 2.5 GeV with an injected beam current of 200 mA and a lifetime of around 20 hours. In addition beam is provided in dedicated shifts at 1.3 GeV for THz applications to operate at short bunch lengths. The storage ring has also become an integral part of the accelerator education and training program at KIT, offering a small fraction of the machine development time for hands-on tutorials for students.

In 2012 the storage ring was in operation for a total of 3794 hours. Of this time 58% was provided to user operation at 2.5 GeV and 11% for special user operation with short bunches. A further 21% of the time has been spent with injection and start-up after shutdowns or weekends. The accelerator development and consolidation program utilized a further 10% of the running time. The distribution of beam time is illustrated in figure 1. Of the 108 days scheduled for regular user operation 10 days were lost, mostly due to RF problems, resulting in a total availability (delivered to scheduled beam time in hrs) of 91%.

In order to improve the reliability of the RF system several parts have been either replaced or reconditioned. Most notable of these are the cables carrying heavy power-loads within the Klystrons. Furthermore, a large scale ANKA machine upgrade plan has been put into action. The following section gives an overview of this upgrade, which has already been completed during the time scale of this report.

To pave the way for a 100 fold increase in devices within the storage ring which communicate over TCP/IP a complete isolated private network has been commissioned. As the network is the communication backbone of the control system it must be very robust to ensure stable operation of the machine. The first devices to be used over this network were 40 new beam position monitoring (BPM) electronic systems. These BPMs not only substantially increase the reliability of the control system but also offer much

more in beam diagnostics such as first turn read out, turn by turn readout, and 10 kHz fast-feedback read out of the beam position. These new devices, along with the aging original ACS control system have motivated a decision to move completely to a new control system named EPICS.

One challenge was to move the control system high-level client for orbit correction to accept an EPICS connection instead of the old ACS, while at the same time still allowing control of the corrector magnets, which remained in the old control system. The intention is to replace these correctors with Ethernet based, fast response magnets and power supplies so as to take advantage of the BPM fast feedback correction system now available. Another new device installed in the ANKA storage ring is the NANO wiggler. Full control with EPICS together with the graphical user interface CSS was developed as a test case for new tools. This has set an ANKA standard which can be applied to any newly integrated device so as to keep the whole control and operation of the machine completely homogeneous.

Several new diagnostic techniques, such as locating of possible wake-fields using a standard satellite receiver unit have been implemented. Another is the use of Electrical Optical Sampling (EOS) for near-field electro-optical bunch length measurements, which has been installed within the UHV of the ANKA storage ring. Here a laser pulse is used to probe the field induced birefringence in an electro-optical crystal which after being spectrally decoded allows bunch lengths down to femtoseconds to be evaluated (see figure 2). Further details on the various developments in this field are given in the following section.

AcknowledgementI.Birkel, A.Böhm,T. Fischböck, E.Huttel, U. Krieg, R.Kubat, W.Möck, A.-S.Müller, S.Naknaimueung, A.Papash, S.Pfeifer, N.Smale, R.Stricker, A.Völker, U.Werdin, P.Wesolowski,.

Storage Ring Operation | Accelerator Science and Technology

Anke-Susanne Müller: [email protected]

COntACt

Figure 2: Schematic and installation of femtosecond laser pulse set-up for bunch-length measurements

Figure 1: Distribution delivered beam in 2012 (January-December)


The main components of the machine are the photo-injector gun using picosecond UV laser pulses to generate electron bunches from a cathode, a linac accelerating the bunches to 41 MeV, a magnetic D-shaped chicane to compress the bunches longitudinally, the THz radiation generation/extraction, and finally an electron dump (see Fig. 5). It is designed to cover a large charge range from a few pC to 3 nC and will be set up in the bunker building 351 northwest of the ANKA hall. It will be optimized to achieve ultra-short electron bunches with a root-mean-square (RMS) length down to a few femtoseconds. We will use coherent synchrotron, edge, and transition radiation (CSR, CER, and CTR) to generate very short and intense electro-magnetic pulses in the far-infrared/THz regime.

FLUTE is an accelerator physics test facility to develop and test new instrumentation and diagnostics needed for such short electron bunches. It will allow studying bunch compression schemes and comparing the experimental results to various simulation tools, as well as studying the complex non-linear dynamics due to coherent synchrotron bunch-radiation self-interactions, space charge effects and instabilities. This knowledge is the basis for future compact, broadband accelerator-based THz user-facilities. Furthermore, the generated intense electro-magnetic THz pulses can be used for various scientific experiments ranging from 2D spectroscopy, studying the influence of THz radiation on biomedical samples like stem cells to pump-probe setups of new materials.

To achieve these very short electron bunch lengths various simulation tools have been employed. We used the ASTRA programme [2] for the gun and the linac as space charge effects are dominant here. The strongest effects appear in the gun and the strongly diverging low-energy beam is focused by a solenoid after the gun. The acceleration in the linac increases the beam energy, thus reducing the space charge forces, and produces a chirp (energy variation along the longitudinal bunch direction). In the chicane/bunch compressor coherent synchrotron radiation (CSR) becomes more and more important. As the bunches become shorter they emit more and more CSR, which copropagates with the bunch and influences the bunch structure and therefore the CSR emission. This is especially true in the last magnet where the bunches are very short. This effect was simulated with the program CSRtrack [3]. The parameters optimized for the shortest RMS bunch length in the baseline model of FLUTE to be realized in the first of three construction phases are summarized in Table 1 and Figure 5 [4].

To provide computing time efficient methods to compute the final electric field in the optimization process, we developed analytical expressions valid for arbitrary bunch shapes. They allow us to calculate the expected electro-

magnetic THz pulse shape and corresponding spectrum from the electron distribution at the end of the compressor. In this way we can extend the simulation chain to optimize FLUTE not just for the ideal electron beam parameters but also directly for user-relevant parameters like THz peak field, single cycle pulse shape, and spectrum. The results, optimized for shortest bunch length, are shown in figures 6 and 7.

Furthermore, we have performed tolerance studies of the main components to find out which parameters (such as rotational or positional offsets) are critical for the manufacturing process as well as the later alignment.

First power tests and a bead-pull test of the FLUTE photo-injector electron gun have been performed successfully at the ELSA facility, University of Bonn, Germany, where we could temporarily use an radio frequency (RF) setup from MAX-lab, Lund, Sweden and software from RI Research Instruments GmbH, Bergisch Gladbach, Germany (see Fig. 8).

Accelerator Science and technology FLUtE: A Versatile Linac-based source of ultra-short THz pulses

Charge [Nc] Laser spot [mm] Laser pulse [ps] Magnetic field [T] Compressed bunch length [fs]

0.001 0.5 1 0.119 13

0.1 0.5 2 0.124 67

1 1.5 3 0.132 146

2 1.5 4 0.128 224

3 2.25 4 0.135 270

Table 1: Summary of the design parameters optimized for shortest obtainable RMS bunch length for various bunch charges in the baseline model of FLUTE [4].

............................................FLUtE

The ANKA-team at KIT, in collaboration with DESY and PSI, is currently designing and constructing a new accelerator test facility and an ultra-short far-infrared/THz pulse source [1]. This 15 m long source, named FLUtE (Ferninfrarot Linac- Und Test-Experiment---far infrared linac- and test-experiment), is based on a 41 MeV linear electron accelerator and will operate with a repetition rate of 10 Hz.

Storage Ring Operation | Accelerator Science and technology

[1] M. J. Nasse, M. Schuh, S. Naknaimueang, M. Schwarz, A. Plech, Y.-L. Mathis, R. Rossmanith, P. Wesolowski, E. Huttel, M. Schmelling, A.-S. Müller, Rev. Sci. Instrum. 84 (2013), 022705.

[2] K. Floettmann, „ASTRA, A Space Charge Tracking Algorithm“, http://www.desy.de/~mpyflo/

[3] M. Dohlus and T. Limberg, “CSRtrack”, www.desy.de/xfel-beam/csrtrack

[4] M. Schwarz (Ed.), FLUTE Conceptual Design Report, 2013

Authors: Somprasong Naknaimueang & Michael J. Nasse


Figure 5: Baseline layout for FLUTE [4]

Figure 6: Calculated THz spectrum of FLUTE for two representative bunch charges [1].

Figure 7: Calculated electro-magnetic THz pulse shape for two representative bunch charges. The pulse is assumed to be focused to a disc with 1 mm radius at a distance of 1 m from the source [1]. Figure 8. Preparation of the FLUTE gun at ELSA for bead-pull and RF tests


COntACt


A new dedicated ultra-fast data acquisition system for THz diagnostics was jointly developed in collaboration between the KIT institutes IPE, IMS and ANKA [1]. The main goal of the device is to allow for the acquisition of the THz signal emitted by every bunch for every turn up to 100,000 consecutive turns. Reducing the amount of data requires smart sampling for data reduction and the principle is shown in Figure 11. The processed data contain turn-by-turn information about the THz signal for every bucket. Figure 2 shows the THz signal of all 184 buckets recorded with an ultra-fast THz detector [2]. The filling patterns is clearly visible as well as the outbursts of THz radiation of individual bunches.

Using this new method a statistical analysis approach for investigation of bursting correlations can be applied. Figure 12 shows the matrix of correlation coefficients for all buckets at ANKA in multi bunch mode with high current. Averaging of correlation coefficient in dependance on the bucket distance leads to Figure 13. As the result a small but significant preference to positive values of correlation coefficient with a distance of up to 10 buckets observable. That means bursting is not statistically independent.

Using this measurement technique makes it possible for the first time to systematically study such a multi-bunch environment [2]. For example, Figure 3 shows that the bursting of bunches is correlated up to about ten bunches. Further studies are ongoing to better understand and, ultimately control, bursting of the multi-bunch system and make it accessible as a high intense THz source for users.Since a few years the ANKA synchrotron radiation facility offers for users

a low-alpha mode with reduced bunch length. This operation mode can be used for x-ray research with ultra-short pulses. The pulse length can be reduced down to sub-ps range. Additionally a very intense coherent synchrotron radiation is emitted for wavelength smaller than the bunch length. Thus strong amplification in THz range can be observed and used at the two operational infrared beamlines (IR1, IR2) at ANKA.

For bunches with high charge and reduced bunch length microbunch instabilities can be observed at the ANKA storage ring. The microbunching leads to high power THz bursts. The observation of this behavior can be used as diagnostics of longitudinal processes in the bunch. The THz-Group at ANKA uses very fast hot electron bolometer detector systems for investigations of longitudinal dynamics in these turbulent regimes. The frequency of THz bursts depends strongly on the bunch charge. Figure

9 shows the instability spectrogram of the THz signal for single bunch in low-alpha-mode. The synchrotron frequency can be observed at 13 kHz. Different bursting regimes can be observed. The onset of bursting is around 0.24 mA at approx. 40 kHz. The shown pattern is reproducible for chosen accelerator parameters. The slow intensity oscillation of the THz signal in bursting is shown in Figure 10. Here the signal was attenuated to cover the bursting peak intensity range. Investigations of bursting modes in histograms can help to identify changes in accelerator parameters and accelerator environments.

Observation with a modified geometrical impedance using a scraper show a clear dependence of typical bursting frequencies on impedance. The spectrogram is an accurate indicator for changes in vacuum chamber geometry.

Figure 9: Spectrogram of the THz signal shows different bursting regimes for different bunch currents. Bursting sets in above a threshold current and serves as a fingerprint for machine parameters.

Author: Vitali JudinANKA, Synchrotron Radiation Facility, Karlsruhe Institute of Technology, Germany

ANKA Operation | Accelerator Science and technology


Figure 11: Principle of the data acquisition system [2].

Figure 12: Measured THz signal of all 184 buckets at ANKA over 10,000 turns. The filling pattern of three bunch trains is visible [2].

Figure 13: Average correlation coefficient of the THz signal of buckets as a function of bucket distance, showing that the THz signals of individual bunches are correlated up to a distance of ten buckets. [2]

Author: Vitali JudinANKA, Synchrotron Radiation Facility, Karlsruhe Institute of Technology, Germany


COntACt

Accelerator Science and technology Accelerator Physics at AnKA

Figure 8: Measured THz signal at ANKA in the low-alpha mode in the bursting regime.

Diagnostics of longitudinal instabilities using THz radiation

THz Bursting Diagnostics based on ultra-fast data acquisition system

[1] M. Caselle et al., An ultra-fast data acquisition system for coherent synchrotron radiation with terahertz detectors, Journal of Instrumentation, vol. 9

[2] A.-S. Müller et al., Studies of Bunch-Bunch Interactions in the ANKA Storage Ring with Coherent Synchrotron Radiation using an Ultra-Fast Terahertz Detection System, IPAC 2013




An LNB (Low Noise Block) is a down converter operating at 11 GHz and is commonly used to receive satellite television. It is thus a cheap and compact but never the less a highly sensitive detector. The LNB is capable of conveniently detecting the GHz-signal emitted by electron bunches in the ANKA storage ring even though the low-GHz frequencies are shielded by the vacuum chamber. The LNB signal (figure 14) shows spikes that are related to structures in the vacuum chamber [1] and has been employed to measure relative changes in bunch length online. Recently, measuring the polarization of the LNB signal revealed that the first small part is polarized while the main part is not (figure 15). The polarized part is likely originating from edge-radiation emitted directly by the bunch, while the large unpolarized part is due to wake fields trailing the bunch up to about half the ANKA circumference. The long wake fields can then effect trailing bunches and influence their THz bursting. Studying them with the help of an easy to use LNB leads, therefore, for a better understanding of the multi-bunch THz bursting.

Figure 14: A typical LNB signal envelope emitted by the electron bunch, which consists of a polarised part (blue) and non-polarised part (red). The entire signal lasts for almost the entire 384ns it takes a bunch to complete one circle at ANKA.

When ANKA is operated in the low-alpha mode, the short bunches emit THz radiation coherently, which leads to highly intense THz radiation. Since the spectrum of coherent radiation encodes information on the longitudinal bunch shape, coherent THz radiation provides another diagnostics tool for the beamdynamics. Moreover, the THz beamline will enable user experiments in this new frequency regime.Therefore, a new dedicated beamline for THz radiation is planned at ANKA.

Figure 16: Simulated intensity Profile of the edge radiation at 1 THz at the end of the vacuum chamber.

It has to fit into the existing infrastructure and, thus, the available room is strongly confined. A large aperture is needed to avoid attenuation and diffraction effects. In designing the beamline, the RF-wave nature of the THz radiation has to be taken into account. The favored optic for the beamline is a combination of two Gaussian telescopes, which provide a wavelength independent focus point. The basic design of the beamline is completed and will be developed into a conceptual design report.

Figure 17: Place of the new THz beamline.

One of most important parameters of accelerators is their electron beam energy. So far, the method of resonant depolarization was used to accurately determine the energy at ~2.5GeV of the ANKA storage ring. However, for lower energies this method becomes cumbersome. One good alternative is by detection of Compton backscattered photons. When laser photons scatter off relativistic electrons, highly collimated gamma rays can be generated in the propagating direction of the electrons, which is normally called Compton backscattering. With the collision angle fixed and

the energy of the laser photons already known, the electron energy can be determined by the maximum energy of the gamma rays detected. Until now, the feasibility to perform the measurement either in the booster with an optical cavity or in the storage ring has been studied and simulated, with electron beam parameters given by AT and Compton backscattered photons by CAIN2.35. The simulation results for a promising location in the storage ring can be seen in figure 18.

Figure 18: Simulated photon energy spectrum for transverse collision between 2 W CO2 CW laser photons and 1.3 GeV electrons in the storage ring for 10 minutes

Author: Jan Christoph Heip, KIT - ANKA, Synchrotron Radiation Facility, Karlsruhe, Germany

Author: Cheng Chang, KIT - ANKA, Synchrotron Radiation Facility, Karlsruhe, Germany Germany


COntACt


Diagnostics using a microwave detector

Figure 15: Angular dependence of the LNB signal, obtained by rotating the LNB. On the left hand side the measurements show the expected dependence for detection of polarised radiation with a polarity sensitive detector. On the right hand side there is no significant dependence on the orientation if the detector.

[1] A.-S. Mueller et al., Beamdynamics Newsletter 57, p. 154, 2012.

Design study for a THz beamline at ANKA

Studies for a Compton backscattering based beam energy measurement




The streak camera is able to resolve the longitudinal shape and of the electron bunches over hundreds of consecutive turns. This is done by converting temporal information into a spacial distribution. To automatically evaluate this data a new software has been developed. Using parallel computing it can suppress noise and accurately track beam characteristics such as the bunch length and synchrotron oscillation on-line.

This new data processing is especially useful for the low-alpha operation, that offers reduced bunch length: It made it possible to resolve current dependent fluctuation of bunch length in the sub-mm-range. This fluctuation seems to be connected to the occurrence of radiation bursts in the THz regime.

Figure 19: Bunch length and fluctuation measured in one of the low-alpha configurations possible at ANKA [1].

In October 2012 the world’s first system for near-field electro-opticalbunch length measurements at a storage ring has been installed at AnKA.

The technique which is established at linear accelerators, allows single-shot measurements of the electric-field of an bypassing electron bunch with a sub-ps resolution. In addition to that, long-range wake-fields induced by the bunch can be studied with it. The basic working principle of electro-optical measurements based on the technique of spectral decoding (EOSD) can be seen in figure 20.A chirped laser pulse is modulated by the strong electric-field of a bypassing electron bunch (figure 21). Because of the chirp this temporal modulation is also a spectral modulation and can then be analyzed in a single shot spectrometer.For the measurements during the single bunch low-alpha operation, the electro-optical crystal has to be brought close (about 5 mm distance) to theelectron beam. The geometrical structure of the crystal holder can induce strong wake-fields which will trail a bypassing electron bunch. Those wake-fields can also be measured with the system. Figure 22 shows good agreement between the measured and simulated electric-field inside the electro-optical crystal. Here only the first peak is caused by the Coloumb field of the electron bunch and the trailing peaks are all caused by wake-fields. During ANKA`s low-alpha operation, the bunch length is reduced drastically down to a few picoseconds (RMS) in order to generate coherent synchrotron

Figure 20: Working principle of electro-optical spectraldecoding.

Figure 23: Three bunch profiles measured during low-alpha operation (short-bunch-operation) along with the fluctuations of the measurement background.

a key parameter that determines the spectral characteristics of the emitted CSR. Those dynamic changes of the longitudinal bunch profile - also called microbunching - have been predicted by theory, but have never been observed at a storage ring, because one needs single-shot measurements with a sub-ps accuracy for it, which is not trivial to achieve. Especially if the

Figure 22: Measured and simulated temporal electric field inside the electro-optical crystal. Published in [1].

References[1] B. Kehrer et al. “Numerical Wakefield Calculations for Electro-Optical Measurements” - Proceedings of the IPACʼ13, Shanghai, China, 2013, MOPME01

[2] N. Hiller et al. “Electro-Optical Bunch Length Measurements at the ANKA Storage Ring” - Proceedings of the IPAC’13, Shanghai, China, 2013, MOPME014

Author: Nicole Hiller, Laboratory for applications of synchrotron radiation, Karlsruhe Institute of Technology, Germany

Author: Patrik Schönfeldt KIT - ANKA, Synchrotron Radiation Facility, Karlsruhe, Germany


COntACt

Streak camera studies of longitudinal bunch behavior above the microbunching threshold


[1] P. Schönfeldt et al, Proceedings IPAC 2013, MOPEA020

First Electro-Optical System for Near-Field Bunch Length Measurements installed at ANKA*

Figure 21: fs laser pulse is stretched (gratings), polarized, passing through elec.opt.crystal, e- pulse is changing polarization, laser pulse is analyzed, gives bunch length

Polarizing beam splitter

Beam coming from laser (red)

Incident beam strikes grating (red), exit beam (orange)

Beam going in crystal (orange) and out of crystal (green)

used technique has to be non-invasive to the beam. First measurement results with the electro-optical setup at ANKA have now revealed a measurable substructre forming on the electron bunches and three bunchprofiles along with background fluctuations are shown in figure 23. More details about the measurements and more results can be found under [2].

radiation (CSR). When compressing electron-bunches in storage rings, a bursting behaviour of the emitted CSR can be observed for certain machine conditions (high bunch current and strong compression). Those bursts of radiation could be caused by dynamic changes to the temporal shape of the electron bunches as the longitudinal bunch profile is




Figure 25: Optics functions for a hybrid low-alpha optics at ANKA which provides short electron bunches at 2.5 GeV [1].

References: [1] Streichert et al., ICAP2012 Authors: Vitali Judin, ANKA, Karlsruhe Institute of Technology, Synchrotron Radiation Facility, Karlsruhe, GermanyMarcus Schwarz, LAS, Karlsruhe Institute of Technology, Laboratory for applications of synchrotron radiation.

Detecting and analyzing beam losses can be a useful tool in monitoring beam behavior, protecting sensitive machine components and optimizing various processes, for example injection efficiency and beam loss recovery. Therefore the underlying physics have been taken into considerations while performing simulations for different loss mechanisms and following interaction processes leading to multiplication of secondary particles as well as beam loss

measurements to cross-check simulations and investigate loss behavior at the ANKA storage ring. By discussing results of simulations and measurements as well as distinguishing between different loss characteristics the goal of these investigations is to provide a set of requirements for a new improved beam loss monitor system for ANKA. In cooperation with the Institute of Photonics and Quantum Electronics (IPQ) a new detector is in development.

Author: Edmund Hertle, KIT - ANKA, Synchrotron Radiation Facility, Karlsruhe, Germany


COntACt

Investigation of Beam Losses at the ANKA Storage Ring

For optimization of existing as well as for development of new beam optics at ANKA an approach with multiobjective genetic algorithms (MOGA) was applied. This method is an alternative to global scan of all stable settings (GLASS). In comparison to GLASS it delivers only the single optimized solution with desired parameters, but about 50 times faster using the same computational power. Once MOGA was set up for ANKA, it is possible to optimize for specific purposes.

Using MOGA a new beam optics solution that reduces the emittance from 50 nm rad down to 38.3 nm rad was obtained for ANKA [1], as shown in Fig. 24.

MOGA results show the pareto-optima, where one parameter cannot be improved without worsening the other. The paralized GLASS scan took about 28 hours, compared to 4 hours for MOGA on a single-core PC.Since the bunch length increases with energy the low-alpha mode for short electron bunches requires ANKA to run at 1.3 GeV, which in turn reduces the x-ray energy. To combine high energy and short x-ray pulses a new hybrid low-alpha-optics at 2.5 GeV was calculated [1]. The bunch length could be reduced down to 2 ps. That allows a combination of the intense coherent THz radiation and nominal user operation. The optical functions are shown in Fig. 25.

Figure 24: Using MOGA with 38.3 nm rad.

Optimization of the ANKA beam optics using multi-objective genetic algorithms



The main activities of the last year have been:

1. New working program within collaboration with BNGWe have defined a new working program within the collaboration with our industrial partner to develop a:• superconducting undulator with 20 mm period length (SCU20) for

the NANO beamline. The choice of the 20 mm period length for the superconducting undulator for the NANO beamline has been done to optimize the flux at energies in the range 15-20 keV.

• superconducting undulator with 15 mm period length (SCU15) for low emittance third generation light sources to be tested at ANKA. In low emittance sources with full energy injector the allowed vacuum gap, and consequently the magnetic gap, are smaller than by ANKA. In the following (see Fig. 1) we show the advantages of a 15 mm period length superconducting undulator with respect to a cryogenic

permanent magnet undulator with 17.7 mm period length for middle energy low emittance third generation light sources.

• superconducting undulator wiggler (SCUW) with a period length switchable from 18 mm to 54 mm for the IMAGE beamline. The choice of the 18 mm period length for the superconducting undulator for the IMAGE beamline has been done to optimize the flux at 5, 8 and 20 keV for a vacuum gap of 7 mm. The wiggler allows to reach up to 65 keV.

1.1. Superconducting undulator demonstrator The first step in the development is a superconducting undulator demonstrator (SCU15DEMO) to be tested with beam at ANKA. The main parameters of the device, already described in the previous report, are listed in Table 1.

Table 1: The main parameters of the SCU15DEMO.

The beam vacuum chamber is quite challenging since, together with the requirements for a UHV radiation hard environment and the necessity to keep the resistive losses as low as possible [1], it needs to open to 15 mm during electron beam injection and energy ramping in the ANKA storage ring. The chamber has been manufactured and successfully passed the vacuum test reaching < 3 x 10-10 mbar in cold conditions. The SCU15DEMO is under assembly. In the following the spectral performance of the SCU15DEMO and of a SCU15 with higher mechanical tolerances and lower phase error is compared with the competing cryogenic permanent magnet technology at ANKA and at low emittance sources. The´field calculated from the Radia [2] simulations, using the pole height (±25μm) and the half period length deviations (±10μm) measured for the two coils of the SCU15DEMO at room temperature [3], has an r.m.s phase error of 5.6° over 186 poles [4]. Local field measurements of the 1.5 m long coils were performed in a liquid helium bath cryostat at CERN. The 1.5 m long coils reached 855 A/mm2 [4] allowing to reach a peak field on axis at 8 mm magnetic gap of 0.69 T. The measured field shows, after mechanical shimming, an r.m.s. phase error of 7.4° on 106 poles, over a length of 0.795 m [4].The expected flux at ANKA, calculated with B2E [5] from the measured shimmed field is, in several energy ranges, higher than the one of an ideal cryogenic permanent magnet undulator (CPMU), e.g., as designed for the DLS [6, 7] (see figure 27).

Accelerator Science and technology Insertion Devices

The use of mechanical shims to reduce the bimetallic effect, applicable to fixed gap undulators, together with further adjustment to keep the gap uniform to within 40 μm, would make it possible to reach an r.m.s phase error of ~ 3.5° without additional correction coils. For the installation of the SCU15DEMO at ANKA, where the gap is movable, BNG has pre-bent the coils at room temperature to try to compensate the bending measured at 4 K.For low emittance third generation light sources the brilliance is often regarded as the relevant figure of merit. Since most of the beamlines work collecting the flux through a variable aperture at a defined distance from the source, we decided to consider as figure of merit the flux through a finite angular acceptance defined by a rectangular aperture to collect ±2σ of the first harmonic produced by the maximum peak field on axis.The flux of the SCU15 and of an ideal CPMU calculated for the DLS and for MAXIV using the parameters as in Ref. [7] is shown in Fig. 1. To compete with the CPMU technology the field quality of a SCU15 for those low emittance sources must be higher than for ANKA. Because of the lack of a shimming technique for SCUs easily applicable to long devices (> 1 m) it is of course important to evaluate the real requirements on the r.m.s. phase errors for present and future applications. The flux calculated with B2E by the field simulated with Radia taking into account the mechanical tolerances measured at room temperature and with an r.m.s phase error of 5.6° is reduced not more than 10% at the harmonics with respect to

the one produced by the ideal field. This is demonstrated up to the 15th harmonic in Fig. 2. No significant flux reduction is observed in the higher harmonics, even in case of MAXIV, the lowest emittance case considered. The reason is that, for this aperture and at least for r.m.s. phase errors of about 6°, the flux reduction at the higher harmonics is dominated by the energy spread of > 0.001, which is the same for all three synchrotrons. Cases for higher phase error need to be analysed. We can conclude that an r.m.s. phase error of about 6° is sufficient (flux reduction < 25%) for the existing and planned storage rings up to the 15th harmonic [7].

Period length (average) 15 ±0.01 mm

Maximum magnetic field > 0.69 T

K > 0.96

Vacuum gap closed > 7 mm

Vacuum gap open > 15 mm

Number of full periods 100

Beam heat load 4 W

Figure 27: Top left: Profiles of the measured field before (magenta line) and after (blue line) mechanical shimming, of the ideal field (black line) and of the field simulated withRadia [2] (red line) using the pole height (δ 50 μm) and the half period length (δ20 μm) deviations measured for the two coils at room temperature [3]. The inset shows a zoom of the positive and negative field peaks. Flux calculated with B2E [5] using the four fields shown on the top left figure and the ANKA (bottom left), DLS (top right) and MAXIV (bottom right) beam parameters [7] through a slit of 4 mm x 0.9 mm, 1.2 mm x 0.6 mm and 0.68 mm x 0.64 mm, respectively, at 10 m distance from the middle of the undulator. Compared are also the convolutions of the flux produced by an ideal SCU with λU=15 mm, by the measured shimmed field and by an ideal CPMU with λU=17.7 mm [6]. The two insets show the comparison at photon energies > 10 keV.

Authors: S. Casalbuoni, S. Gerstl, N. Glamann, A. Grau, T. Holubek, Ch. Meuter, D. Saez de, Jauregui, R. VouttaKIT - ANKA, Synchrotron Radiation Facility, Karlsruhe, Germany

Information

At AnKA we pursue a research and development program to develop superconducting (sc) insertion devices (IDs).

Of fundamental importance for the realization of this program are: i) a close collaboration with our industrial partner Babcock noell GmbH (BnG), and ii) the instrumentation developed and under development to perform R&D. This includes improvements and quality management of the magnetic field properties and understanding of the beam heat load mechanisms to a cold bore.

............................................

1Definition of a new working program within the collaboration with our industrial partner

2Final acceptance test of the cryostat of the facility for magnetic field measurements of 2 m long superconducting undulator coils and first tests performed with a conduction cooled mock-up coil

3Installation of a cold vacuum chamber for diagnostics in the Diamond Light Source (DLS) and preliminary measurements of the beam heat load

4 Design and manufacturing of a superconducting switch

5 Tests for possible applications of new materials to sc IDs


User Operation Accelerator Report Beamline Report Lab Report Applications Appendix Anke-Susanne Müller: [email protected]

Sara Casalbuoni: [email protected]

COntACt


In figure 27 it is shown that the SCU15 has a higher flux than the CPMU in several energy ranges. The energy range is wider for MAXIV, which emittance is two order of magnitude smaller than the one of ANKA and one order of magnitude smaller than the one of the DLS. The reason is that the undulators can work in low emittance sources with a smaller magnetic gap, which allows to increase the maximum magnetic peak field on axis. Before manufacturing the final 1.5 m long coils of the SCU20, SCU15 and SCUW are foreseen two mock-ups for each:

• Mock-up 1: one half undulator coil, 150 mm long, to measure the quench current, to qualify the wire and the winding scheme in a liquid helium bath in the facility CASPER I (ChAracterization SetuP for field Error Reduction) [8]

• Mock-up 2: two undulator coils, 300 mm long, to qualify the manufacturing and assembling procedures, and to test the magnetic field quality and the conduction cooilng concept in the horizontal in vacuum facility CASPER II [9]

With the SCU15DEMO we have learned that keeping the mechanical tolerances in the cold is much more challenging for longer coils. So, the lessons learned with the mock-ups will be first implemented in the SCU15 1.5 m long coils. The tests of these long coils first in CASPER II, then with beam in ANKA, will allow us to improve the design and manufacturing of the long coils for the SCU20 and SCUW.The know-how gained with the design, manufacturing and testing of all these deviceswill flow in a technical design report for a superconducting undulator for small emittance third generation light sources.The SCU20 and SCU15 Mock-up 1 have already been manufactured and successfully tested.

2. Instrumentation for magnetic field measurements of 2 m long superconducting undulator coils

CASPER II is a horizontal cryogen-free test stand that will be used to perform quality certification (max. length 1500 mm, max. diameter 500 mm) of new conduction cooled superconducting IDs. It will also serve to test small prototype coils in a cryogen free environment. CASPER II is under construction: a successful final acceptance test of the cryostat has been performed in Summer 2011. Quench tests performed with a 10 plate mock-up successfully confirmed its functionality [10]. The magnetic field along the beam axis will be measured by Hall probes fixed to a sledge moved by a linear stage. The precisions are ΔB < 1 mT and Δz < 1 μm. Field integral measurements will be performed using the stretched wire technique. In order to allow local and integral field measurements in the same thermal cycle, the wire will be stored in the guiding rails of the Hall probe sledge when the Hall probe is in use. When the Hall probe is fully retracted and clear of the gap, the stretched wire can be pulled out.


With the aim of measuring the beam heat load on a cold bore, needed to specify the cooling power for the cryogenic design of superconducting IDs, and in order to gain a deeper understanding in the beam heat load mechanisms, a cold vacuum chamber for diagnostics (COLDDIAG) was built [11]. With the equipped instrumentation, which includes temperature sensors, pressure gauges, mass spectrometers, as well as retarding field analyzers, it is possible to measure the beam heat load, total pressure, gas content, as well as the flux of electrons and/or ions hitting the chamber walls. We are offering its installation in different synchrotron light sources with different energies and beam

characteristics. After successful factory acceptance test [12] and calibration of the beam heat load measurement, COLDDIAG was installed in the storage ring at the Diamond Light Source (DLS) in November 2011 [13]. Due to a mechanical failure of the thermal transition of the cold beam tube, the cryostat had to be removed after one week of operation. After optimizing the design of the liner thermal transition, COLDDIAG was successfully installed a second time in the DLS in August 2012 (see figure 30) and is taking data since then.

Figure 28: Ratio of the flux produced by the field simulated with Radia taking into account the mechanical tolerances measured at room temperature and with an r.m.s phase error of 5.6°, to the one from an ideal field at the different harmonics for ANKA, the DLS, and MAXIV [7].

Figure 29: CASPER II and schematic side view of temperature test setup during the final acceptance test.

Figure 30: COLDDIAG installed in the Diamond Light Source (DLS)

Figure 31: Beam heat load in COLDDIAG measured for different filling patterns as a function of the average beam current. The black curve was measured in 2011 during the first installation. The crosses display the beam heat load measured for the 270 mm long upstream warm sections. The predictions from resistive wall heating calculations for the cold liner section and a RRR of 10 and 200 are indicated by circles [14].




COntACt

3. A cold vacuum chamber for diagnostics


4. Superconducting switchWe have designed and manufactured a conduction cooled superconducting switch (SCS) that can be applied to switch the period length as well as to switch different correction coils (see figure 32). The superconducting switch allows to reduce the number of power supplies and consequently the thermal load to the device. Applications to conduction cooled cryogen free insertion devices as the ones under development at ANKA in collaboration with Babcock Noell GmbH [16] make use of cryocoolers, which have typically a cooling power of 1–1.5 W at 4 K. For this reason, we need for our application a SCS which must not dissipate more than a fraction of a Watt. A first successful test in an ad hoc conduction cooled environment has been performed demonstrating a minimum power dissipation of 200 mW per heater [17].Even if this would already allow the application of the SCS to a cryogen free ID, we believe that the minimum power level needed for switching can be further reduced by lowering the pressure, and consequently convection cooling, in the in-vacuum housing used in the first test at CASPER I. For this reason the next test is foreseen in a cryogen free environment in the facility CASPER II at ANKA.

5. New materialsThe “work horse” wire material for superconducting magnets are multifilament NbTi wires, which today are also used for superconducting IDs. Even higher magnetic fields can be reached by using a conductor with enhanced critical current density, such as a NbTi wire with artificial pinning centers (APC), developed by SupraMagnetics, Inc. [18] and not yet commercially available. A racetrack coil has been built and measured to study the possible use of NbTi APC wire in SCUs [19]. The critical current characteristic of a short wire and the load line of a racetrack coil, designed to simulate the field configuration on the conductor as in a superconducting undulator, have been measured in a liquid helium bath. Based on the measured loadline, the simulations of the magnetic field on axis have been performed. The advantages of the performance of an undulator made with NbTi APC wire having similar properties of the measured one are shown in figure 33.

Promising for future applications in SCUs are HTS (High Temperature Superconductor) tapes. Their engineering current density is rapidly increasing and they can be operated at higher temperatures than NbTi, allowing to sustain higher beam heat loads. HTS tapes can be used for planar SCUs in geometries similar to the ones used for NbTi wire. A short mock-up has been designed and manufactured by BNG [20] and tested in the facility CASPER I at ANKA/KIT, at 4 K reaching similar results as obtained with the SCU15DEMO.Together with the group of W. Goldacker (Institute of Technical Physics, KIT) we follow at ANKA the proposal from S. Prestemon et al. [21] of an HTS tape stacked undulator for free electron lasers applications. The concept is particularly promising for narrow-gap, short period < 10 mm regimes. To define the current path allowing a sinusoidal magnetic field on axis the HTS tape is structured. While S. Prestemon et al. [21] etch the tape using

lithography techniques, we will use a Triumpf picosec YAG–IR laser from the group of W. Goldacker, meant to structure Roebel cables with the aim to reduce the AC losses. We have measured for the first time the magnetic field performance of such a HTS tape [22]. The measured magnetic field


profile is shown in figure 34.Still open issues in both the above described applications of HTS tape to SCUs are the quench detection and protection, radiation damage, engineering current density as a function of the magnetic field, stress and geometry, test field accuracy and the joint resistance of 50 – 100 nΩ cm2

[23]. This last point could be solved for a planar HTS SCU by using a winding scheme with no joints.

References: [1] D. Saez de Jauregui, T. Baumbach, S. Casalbuoni, S. Gerstl, A. Grau, M. Hagelstein, C. Heske, T. Holubek, B. Krause, A. Seiler, S. Stankov, L. Weinhardt , C.Z. Antoine, Y. Boudigou, C. Boffo, Proceedings of the International Particle Accelerator Physics Conference, New Orleans, LA, 2012. http://accelconf.web.cern.ch/accelconf/[2] O. Chubar, P. Elleaume, J. Chavanne, J. Synchrotron Rad. 5, 481 (1998).[3] C. Boffo, W. Walter, T. Baumbach, S. Casalbuoni, S. Gerstl, A. Grau, M. Hagelstein, D. Saez de Jauregui IEEE Trans. On Appl. Supercond. 21-3,1756-1759 (2011).[4] S. Casalbuoni, T. Baumbach, S. Gerstl, A. Grau, M. Hagelstein, D. Saez de Jauregui, C. Boffo, J. Steinmann, W. Walter, IEEE Trans. on Appl. Supercond. 21-3, 1760-1763 (2011).

[5] P. Elleaume, X. Marechal, Report ESRF-R/ID-9154 (1991).[6] C.W. Ostenfeld and M. Pedersen, Proceedings of the International Particle Accelerator Physics Conference Kyoto, Japan 2010.[7] S. Casalbuoni, T. Baumbach, S. Gerstl, A. Grau, M. Hagelstein, T. Holubek, D. Saez de Jauregui, C. Boffo, W. Walter, Proceedings of the International Particle Accelerator Physics Conference, New Orleans, LA, 2012. http://accelconf.web.cern.ch/accelconf/[8] E. Mashkina, A. Grau, C. Boffo, M. Borlein, T. Baumbach, S. Casalbuoni, M. Hagelstein, R. Rossmanith, E. Steffens, W. Walter, IEEE Trans. App. Supercond. 18-2, 1637–1640 (2008).[9] A. Grau, T. Baumbach, S. Casalbuoni, S. Gerstl, M. Hagelstein, D. Saez de Jauregui, IEEE Trans. on Appl. Supercond. 21-3, 2312-2315 (2011).[10] A. Grau, T. Baumbach, S. Casalbuoni, S. Gerstl, M. Hagelstein, T. Holubek, D. Saez de Jauregui, IEEE Trans. on Appl. Supercond. 22, 9001504 (2012).[11] S. Casalbuoni, T. Baumbach, S. Gerstl , A. Grau, M. Hagelstein, D. Saez de Jauregui, C. Boffo, G. Sikler, V. Baglin, R.Cimino, M. Commisso, B. Spataro, A. Mostacci, M. Cox, J. Schouten, E. Wall´en, R. Weigel, J. Clarke, D. Scott, T. Bradshaw, I. Shinton, R. Jones, IEEETrans. on Appl. Supercond. 21-3, 2300-2303 (2011).[12] S. Gerstl, T. Baumbach, S. Casalbuoni, A. Grau, M. Hagelstein, T. Holubek, D. Saez de Jauregui, V. Baglin, C. Boffo, G. Sikler, T. Bradshaw, R. Cimino, M. Commisso, A. Mostacci, B. Spataro, J. Clarke, R. Jones, D. Scott, M. Cox, J. Schouten, I. Shinton, E. Wallèn, R. Weigel, Proceedings of IPAC11, San Sebastian, Spain 2011.[13] S. Gerstl, T. Baumbach, S. Casalbuoni, A. Grau, M. Hagelstein, D. Saez de Jauregui, T. Holubek, R. Bartolini, M. Cox, J. Schouten, R. Walker, M. Migliorati, B. Spataro, I. Shinton, Proceedings of IPAC12, New Orleans, Louisiana, 2012.[14] S. Gerstl, S. Casalbuoni, A. Grau, D. Saez de Jauregui, T. Holubek, R. Voutta, R. Bartolini, M. P. Cox, E. C. Longhi, G. Rehm, J. C. Schouten, R. Walker, R. Walker, M. Migliorati, B. Spataro, Proceedings of IPAC13, Shanghai, China, 2013.[15] S. Casalbuoni , M. Migliorati, A. Mostacci, L. Palumbo, B. Spataro, JINST 7 P11008 (2012).[16] S. Casalbuoni, T. Baumbach, S. Gerstl, A. Grau, M. Hagelstein, T. Holubek, D. Saez de Jauregui,C. Boffo, W. Walter, SYNCHROTRON RADIATION NEWS, 14-19 Vol. 24, No. 3, 2011.[17] T. Holubek, T. Baumbach, S. Casalbuoni, S. Gerstl, A. Grau, M. Hagelstein, D. Saez de Jauregui, C. Boffo, and W. Walter, IEEE Trans. on Appl. Supercond. 23-3, 3800104 (2013).[18] http://www.supramagnetics.com/[19] T. Holubek, S. Casalbuoni, S. Gerstl, A. Grau, D. Saez de Jauregui, M. Kläser, Th. Schneider, L. Motowidlo, Physics Procedia Volume 36, 2012, 1098–1102.[20] C. Boffo, http://www.maxlab.lu.se/usermeeting/2010/sessions/IDmax2010/[21] S. Prestemon , D. Arbelaez , S. Davies, D. R. Dietderich, D. Lee, F. Minervini and R. D. Schlueter, IEEE Trans. on Appl. Supercond. 21-3, 1880-1883 (2011).[22] T. Holubek, S. Casalbuoni, S. Gerstl, A. Grau, D. Saez de Jauregui, W. Goldacker and R. Nast, IEEE Trans. on Appl. Supercond. 23-3, 4602204 (2013).[23] V. Selvamanickam, http://www.itep.kit.edu/hts4fusion2011/

Figure 32: Left: current of 1000 A flowing through circuit 1 (top) and the field produced by the test coil, measured with the Hall probe (bottom), versus time. Top right: Scheme of the measurement setup showing two electrically separated circuits. Bottom right: superconducting switch [17].

Figure 33: Brilliance for a middle energy low emittance light source as a function of photon energy for a SCU, a CPMU and an in vacuum undulator (IVU) with the same magnetic length and vacuum gap [17].

Figure 34: Magnetic field line profiles 2.05 mm above centre of structured tape for 300, 500 and 600 A.




COntACt

32

FLUOX-ray fluorescence spectroscopy beamline

Spectroscopy

INEBeamline for actinide research

IR1Infrared beamline for spectroscopy and ellipsometry

IR2Infrared beamline for microspectroscopy and nanospectroscopy

SUL-XX-ray beamline for environmental research

UV-CD12Vacuum-UV beamline for synchrotron circular dichroism spectroscopy

WERASoft x-ray analysis facility

XASX-ray absorption spectroscopy beamline

Beamline Report


IntroductionIn 2012 the main areas of user experiments were biology and medicine, environmental research and archeometry.The beamline is also routinely used for the characterization of X-ray optics for beam focussing and imaging including also set-ups for X-ray microscopy.

Current upgradesFaster scanning and more precise alignment of focussing optics are the main directives for ongoing improvements of the set-up. The conventional step by step scanning mode will be complemented and eventually replaced by continuous scanning thus reducing idle times of movement settling and detector read-out to essentially zero. When measurement times can be as small as 20 ms users can record large sample area maps, do pre-scans in order to identify interesting areas or three dimensional images. For these purposes a XIA-Mercury detector electronic is currently being installed and the sample holder is equipped with new motorized stages with position encoders. The new stages are also more rigid and stiff then the old ones.

FLUO X-ray fluorescence spectroscopy beamline

Spectroscopy

............................................Information

The FLUO beamline is situated at a bending magnet port. It is equipped with a double multilayer monochromator, providing high photon flux at moderate energy resolution, and is predominantly used for X-ray fluorescence measurements and mappings with spatial resolution in the micrometer range. With Confocal X-ray Fluorescence and X-ray Fluorescence Tomography, depth-resolved measurements are possible, allowing access to three-dimensional mappings of major, minor, and trace elements in a sample.

FLUO | INE | IR1 | IR2 | SUL-X | UV-CD12 | WERA | XAS | MPI | NANO | PDIFF | SCD | IMAGE | TOPO-TOMO | LIGA I, II, III

Rolf Simon: [email protected]

Beamline: +49 (0)721 608 26307

COntACt



characterize U-rich regions in thin section samples of corroded cement matrices retrieved from the Asse II salt mine in Northern Germany after long-term exposure to salt (NaCl, MgCl2) brines [2] or U contaminated sludge samples obtained from a decantation pond of a uranium treatment facility in France. Generally, in these samples regions of interest are pre-selected from SEM backscattering images, showing high contrast for U-rich aggregates (hot spots) embedded in the sample matrix. A polycapillary optic mounted on a hexapod positioning unit is used to focus monochromatic radiation to a beam spot-size of 25-30 µm for µ-XRF and µ-XAFS measurements. Samples are mounted on a three-axis positioning stage with the sample surface at a 45° angle to the incident beam for 2D scanning. The third axis defines the focal distance. A silicon drift detector is used for collecting X-ray fluorescence radiation. By mounting an identical polycapillary lens in front of the detector (confocal detection geometry, distribution maps reconstructed from scanning µ-XRF data can be selected for µ-XAFS and µ-XRD analysis. Diffraction patterns are collected in Laue transmission mode on erasable X-ray sensitive films, mounted perpendicular to the beam, downstream from the sample. In this case, a single bounce capillary is used to deliver a low divergent ~35 µm focused beam.

High resolution X-ray emission spectroscopy (HRXES)

In 2012 the design and manufacture of the multi-analyzer crystal (MAC) spectrometer for high energy resolution X-ray emission spectroscopy (HRXES) have been completed (Fig. 2). The spectrometer assembly comprises a mobile and a stationary positioning unit, both supplied by HUBER Diffraktionstechnik GmbH (Rimsting, Germany). The five analyzer crystal positioning stages possess four degrees of freedom each. The crystal stages are mounted on a common granite block, which is installed on a mobile rack, hosting power supplies and motion controllers for all 23 spectrometer axes. The stationary detector positioning unit comprises three degrees

of freedom (a long and a short linear stage and a rotation stage), which allow the detector to be moved along the Rowland circle. Initial mechanical spectrometer performance tests and adaption of the control software were started in the 2012/2013 ANKA winter shutdown. The MAC spectrometer

will be commissioned and exhaustively tested in various pilot experiments at the INE-Beamline in 2013. The capability of the HR-XANES and RIXS techniques to measure the relative energy and population differences between An/Ln f and d states in materials with small structural variations is extremely valuable for fine-tuning theoretical approaches for quantum chemical simulation of the corresponding spectra [3]. These techniques will, e.g., shed light onto the degree of stabilization of the An 5f valence orbitals across the actinide series or onto the amount of orbital mixing between An/Ln valence and ligand molecular orbitals in An/Ln complexes.

AcknowledgementMany thanks to H. Blank (Bonn University), A. Bauer, A. Neumann, V. Krepper, J. Thomas and C. Marquardt (all INE), T. Hoffmann and G. Christill (both KIT-KSM) for invaluable technical and logistic support. References[1] J. Rothe et al., Rev. Sci. Instrum. 83, 043105 (2012)[2] J. Rothe et al., Journal of Physics: Conference Series, 2013 (in print)[3] T. Vitova et al., Journal of Physics: Conference Series, 2013 (in print)

IntroductionContinuous development and adaption of in-situ speciation methods capable of providing molecular-scale information on key parameters determining radionuclide mobility in the barrier system surrounding a future repository for heat producing nuclear waste (HAW) is necessary, with emphasis on methods applicable for long-lived actinide (An) elements and fission products. The INE-Beamline for actinide science [1] at ANKA was designed, constructed, and is operated as a flexible experimental station for spectroscopic investigation of these elements. The INE-Beamline is the only facility of its kind in Europe offering access to radiochemistry laboratories with state-of-the-art analytical and microscopy equipment in direct proximity to a synchrotron light source with dedicated equipment for X-ray spectroscopic radionuclide characterization on the same research campus. Although its design is optimized for X-ray absorption spectroscopy (XAS) applications, because of this unique constellation the INE-Beamline makes continual efforts to increase the portfolio of available methods to meet users’ needs, in addition to user support in planning, performing and evaluating experiments, including addressing all relevant radiation safety and personal security clearance issues.

User operationIn 2012 more than 50% of all available beamtime shifts were given to external user groups. The time available for INE in-house research amounted to ~30% of all user operation shifts. Ten days were spent for maintenance, development and pilot experiments. INE in-house projects at the beamline cover a broad range of topics related to safe disposal of HAW, with emphasis on An complexation and surface sorption phenomena, and alternative disposal strategies, e.g., the reduction of HAW radiotoxicity. INE in-house projects in 2012 included studies of molybdate phases in simulated nuclear waste glasses, high temperature investigations of Am(III) complexation by sulphate and lactate, polarized XAFS measurements of lanthanide (Ln) and Th(IV) doped brucite and hectorite minerals, investigations of Np complexation by propionate, nitrate and fulvate ligands, studies of tetravalent An complexation by liquid/liquid extraction ligands, structural characterization of trivalent An and Ln complexes of transferrin, and measurements on sorption and redox speciation of Np(V) on Illite mineral phases. General user research projects received beamtime following PRC evaluation and as approved ACTINET-i3 ‘Joint Research Projects’ (both together comprising more than 30% of all available shifts) or through direct cooperation with KIT-INE. In 2012 external user groups from a total of 12 German and European research institutions visited ANKA to conduct experiments at the INE-Beamline. As in previous years, a significant percentage of in-house and PRC beamtime was used by PhD students to perform experiments in the framework of their theses (~20% of all available shifts).

Upgrades in 2012Since 2009 considerable efforts have been undertaken at the INE-Beamline to implement spatial resolution in the µm regime for the investigation of radioactive samples with heterogeneous elemental or phase distributions. In this context, µ-XAFS (µ-XANES/µ-EXAFS), µ-XRF and µ-XRD have been combined, e.g., to

InE Beamline for Actinide Research

Jörg Rothe: [email protected] Prüßmann: [email protected]

Beamline: +49 (0)721 608 28295

Figure 1. left: polycapillary setup for µ-XAFS/XRF measurements at the INE-Beamline – the silicon drift detector (SDD) is depicted with a secondary capillary mounted for confocal measurements (VLM: visible light microscope); right: 3D U distribution in contaminated sludge sample (scales in µm).

Figure 2: 3D CAD model (left) and photo of the MAC spectrometer during initial mechanical performance tests (right).

............................................Information

The INE-Beamline at ANKA is dedicated to actinide research with emphasis on X-ray spectroscopic techniques. The synchrotron based activities at the INE-Beamline are embedded in INE’s in-house research, thereby allowing a combination of analytical and instrumental methods, notably laser techniques and microscopic methods.

Spectroscopy

FLUO | InE | IR1 | IR2 | SUL-X | UV-CD12 | WERA | XAS | MPI | NANO | PDIFF | SCD | IMAGE | TOPO-TOMO | LIGA I, II, III


COntACt


David Moss: [email protected]

Yves-Laurent Mathis: [email protected]

Biliana Gasharova: [email protected]

Michael Süpfle: [email protected]

Beamline: +49 (0)721 608 26724

COntACt

Spectroscopy



v

IntroductionIR1 was one of the original complement of five analytical and three lithography beamlines that were available at ANKA when it opened for the general user community in March 2003. It was at IR1 that the first synchrotron light from the ANKA storage ring was observed in February 2000, and ANKA’s first user experiment was also carried out here in December 2001, leading to the first publication of scientific research at ANKA [1].

The beamline was a bold and controversial departure from the standard approach to infrared beamline design current at that time, since it utilized synchrotron edge radiation rather than classical bending magnet radiation in order to extract a high photon flux at very long wavelengths without needing an excessively large vertical acceptance angle. ANKA’s proof of the feasibility of this concept has proven highly influential, with new infrared

beamlines at SOLEIL (France), DIAMOND (UK), ESRF (France), ELETTRA (Italy, SSLS (Singapore), CLS (Canada), Australian Synchrotron, NSRRC (Taiwan)and NSLS-II (USA) all designed to use edge radiation.

There were originally two experimental stations at IR1. One was a station for vacuum IR ellipsometry (Fig. 1), constructed and operated by the group of Christian Bernhard, then at the Max Planck Institute for Solid State Research. The other was a station for IR microscopy, funded by ANKA’s Synchrotron Environmental Laboratory project: this was the first synchrotron infrared microspectroscopy station in Germany and only the third in Europe, following those at LURE in France and SRS Daresbury in the U.K. The two experimental stations at IR1 received approximately equal shares of the beamtime until 2009, when the IR microscopy station was removed for transfer to the new beamline IR2.

IR1 Beamline for IR/tHz Ellipsometry and Spectroscopy

............................................Information

The IR1 beamline at ANKA with its experimental station for IR/THz ellipsometry, operated jointly by the Max Planck Institute for Solid State Research in Stuttgart and the University of Fribourg in Switzerland, is primarily used for research work in the area of solid-state physics, for example in investigations of the mechanism of high temperature superconductivity. The FTIR vacuum spectrometer of this station can be used for IR/THz spectroscopy in any field of science.

User operationThe IR1 beamline continues to be used primarily by the groups of Christian Bernhard (University of Fribourg) and Alexander Boris (Max Planck Institute for Solid State Research) at the vacuum IR ellipsometry station, resulting in some excellent publications in 2012 [2, 3].

The IR1 beamline is also used regularly by the THz group (LAS, KIT), who exploit the beamline’s extraction optics and diagnostic port for ultrafast studies of the electron beam temporal structure in low a mode (Fig, 2), see also chapter Accelerator Science and Technology. Recently the studies were extended to the IR2 beamline. Our regular users at IR1 also include the group of Michael Siegel (IMS, KIT) who develops ultra fast THz detectors which are then characterized with the coherent IR/THz synchrotron beam [4] (Fig. 3).

Upgrades in 2012 There were no major upgrades or major commissioning work at IR1 on the ANKA/IPS side, largely due to the concentration of resources on problem-solving at IR2. However, the group of Christine Kuntscher (University of Augsburg) made considerable progress in the commissioning of their custom-built experimental station for studies of solids at extreme temperature and pressure (Figs. 4 and 5). These experiments showed that the concept works, however the need to transport and install the equipment for every period of beamtime is far from ideal. Since there is considerable interest from different users communities including solid state physics, geo sciences, materials sciences, etc. for research under extreme conditions at the IR beamlines at ANKA, Christine Kuntscher together with Natalia Dubrovinskaia (University Bayreuth) applied to the BMBF for a dedicated experimental station at IR1 for work under extremely high pressure, low and high temperatures. To our great satisfaction this proposal was successful. We are now beginning the detailed planning phase for this project, which may include an extension of the IR1 hutch in order to be able to provide more space for the equipment.

Figure 1: The ellipsometric assembly at IR1. Key: (IFS) = Bruker IFS 66v/S FTIR spectrophotometer, (P) = polarizer , (A) = analyzer, (D) = liquid He cooled bolometer detector

Figure 2: The THz group‘s experimental setup for electron beam time structure studies in operation at the IR1 diagnostic port.

Figure 3: The experimental setup of the IMS group is in the foreground, behind it is the IR1 diagnostic port.

Figure 4: Christine Kuntscher at the IR1 beamline with her experimental station for infrared spectroscopy at extreme pressures and temperatures.

Figure 5: The heart of Christine Kuntscher’s experimental setup is a long-focus IR microscope designed to accommodate a diamond anvil cell and a liquid He cryostat.

References1. Boris et al. (2002) Josephson Plasma Resonance and Phonon Anomalies in

Trilayer Bi2Sr2Ca2Cu3O10. Phys. Rev. Lett. 89:277001-1-4

2. Charnukha et al. (2012) Optical conductivity of superconducting Rb2Fe4Se5 single crystals. Phys. Rev. B 85:100504-1-5

3. Wang et al. (2012) Macroscopic phase segregation in superconducting K0.73Fe1.67Se2 as seen by muon spin rotation and infrared spectroscopy. Phys. Rev. B 85: 214503-1-8

4. Probst et al. (2012) Superconducting YBa2Cu3O7-delta thin film detectors for picosecond THz pulses. J. Low Temp. Phys. 167, 898-903


David Moss: [email protected]

Yves-Laurent Mathis: [email protected]

Biliana Gasharova: [email protected]

Michael Süpfle: [email protected]

Beamline: +49 (0)721 608 26724

COntACt

Spectroscopy


User Operation Accelerator Report Beamline Report Lab Report Applications Appendix User Operation Accelerator Report Beamline Report Lab Report Applications Appendix


In the design of the IR2 beamline there has been a special focus on reduction of ground vibrations. The infrared beam is transported by mirrors, and due to the long optical path length the mirror vibrations add up directly to the synchrotron beam fluctuations. Especially the water cooling of the primary extraction mirror introduces additional oscillations that can be seen as intensity fluctuations at the experimental stations. Therefore a fast feedback system similar to the one at the ALS infrared beamline has been installed. In a first step the characteristic fluctuation frequencies of the IR2 beamline have been measured. In the future they will be damped by a piezo driven mirror system that stabilizes the beam to ensure constant measurement conditions at the IR2 experimental stations.

Since Bruker Optics no longer supports their older IR spectromers such as the IFS66v/S currently at IR2, a new Vertex80v FTIR spectrometer was purchased. Its coupling to the beamline and IR microscope will require re-design of the station

and compatibility tests. In order not to further delay the opening of the IR2 microscopy station, its installation and commissioning will follow at a later date.

Progress has also been made with the second experimental station at IR 2, the infrared nanoscope (Fig. 5). The purpose of this unique instrument is to provide broadband infrared spectroscopy and imaging at a lateral resolution orders of magnitude better than the diffraction-limited resolution provided by conventional optics. This is achieved by exploiting the field enhancement effect at an AFM tip as it contacts the surface of the sample: the infrared light reflected at the tip position is extracted from the general reflected signal by locking onto the AFM tapping frequency, giving a lateral resolution determined effectively by the size of the AFM tip. The experimental station, based around a commercial AFM from WITec, was developed by our partners from the Martina Havenith group (University of Bochum) within the framework of a BMBF Verbundsforschung project. In 2012 the coupling through the FTIR Vertex80v has been realized (Fig. 6) and the coupling of the IR synchrotron beam into the nanoscope is currently under design.

User operationIn 2012 the IR microscopy station has been in regular use with its built-in thermal light source, in particular for the IR group’s continuing contributions to the award winning Celitement® project. An innovative reaction cell for hydrothermal synthesis was designed and commissioned in collaboration with the Building Materials group of ITC (KIT). It allows for complementary in-situ investigation of reaction kinetics at both the IR microscope as well as at the SUL-X beamline. The IR microscope has been further used in a number of KIT-internal collaborations within the framework of the BioInterfaces program and for projects of some external users.

After the successful commissioning of the IR microscope with synchrotron light in August 2013 the station has been opened for external users. The first external user groups and in-house projects for work with IR synchrotron light are scheduled for September 2013.

v

IntroductionWhen ANKA opened for the general user community in March 2003, the IR beamline with its IR microspectroscopy station immediately became ANKA’s most heavily oversubscribed beamline with over 400% overdemand. Within 5 years, the decision had been taken to move the IR miccroscope to a new infrared beamline in order to provide more beamtime by no longer having to share the beam with the vacuum ellipsometry station. This also provided the opportunity to make a number of improvements to the design of the beamline in order to enhance performance even further. This ambitious project required an extended period of time until satisfactory solutions could be found for all the technical issues. It is therefore with great pleasure that we report that IR2 is now open for users.

The lateral resolution achievable with conventional synchrotron IR microscopy is restricted by classical optical diffraction limit, which is an increasingly significant limitation into the long wavelength range. A novel near-field approach is being implemented at IR2’s second experimental station, in which lock-in detection of field-enhanced scattering from a tapping AFM tip will provide broad-band IR spectroscopy with a lateral resolution two orders of magnitude better than the optical diffraction limit.

Construction progressFurther issues that have delayed the opening of this new IR microspectroscopy beamline have been identified and solved. The unacceptable temperature increase upon irradiation with synchrotron light of the actively cooled surface of the extraction mirror was traced to an error in the contractor’s design for the water cooler. After several improvement attempts a new cooler has been designed, assembled (Fig. 1) and installed at IR2 (Fig. 2) in the January 2013 shutdown. Finally, bake out and conditioning with synchrotron beam (Fig. 3) confirmed that the beamline is now working as designed. Consequently a basic commissioning with synchrotron light could be conducted. Test experiments at the IR2 diagnostic port (Fig. 4) and with the IR microscope showed that the introduction of the window changer further downstream, just one of the improvements compared to the design of IR1, indeed leads to increased flux.

IR2 Beamline for IR/THz Micro and Nano Spectroscopy


WERA | U V-CD 12 | I R1 | I R2 | X AS | F LUO | SUL-X | INE | L IGA | S CD | I MAGE | T OPO-TOMO | S CD | P DIFF | N ANO | M PI-MF

Spectroscopy

David Moss: [email protected] Yves-Laurent Mathis: [email protected]

Biliana Gasharova: [email protected] Michael Süpfle: [email protected]

Beamline: +49 (0)721 608 26613

CONTACT

Figure 4: The experimental setup of the THz group with two bolometer detectors, behind it is the IR2 diagnostic port.

Figure 2: The holder containing the extraction mirror M1 is installed at IR2 after re-designing of the water cooling system.

............................................Information

The IR2 beamline is ANKA’s second infrared beamline, constructed primarily in order to provide more beamtime at the experimental station for IR/THz microspectrosopy due to the consistently high demand for this techique amongst ANKA’s users. In a subsequent development, BMBF funding obtained by the University of Bochum was used to establish an additional experimental station for near-field IR/THz nanospectroscopy which is currently under construction.

Figure 1: Assembling the new water cooler of the extraction mirror M1 of the IR2 beamline.

Figure 3: The IR2 synchrotron light in the visible range, projected on a sheet of paper 4 m from the diagnostic port.

Figure 6: The IR nanoscope under construction at IR2.

Figure 5: IR2 beamline experimental stations: on the right-hand side in the foreground is the IR microscopy station with a Bruker IFS66v/S spectrometer coupled to an IRScope II infrared microscope equipped with single element and imaging detectors, and on the left-hand side the new IR nanoscopy stati-on with the WITec AFM (in the acoustic isolation box) and Bruker Vertex 80v FTIR spectrometer. In the background are the fast feedback system, window changer and diagnostic port.


Status The SUL X-ray beamline enables to investigate samples – without remounting them – sequentially with X-ray fluorescence spectroscopy (XRF), X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD). It uses a wiggler as radiation source, focuses the beam with two mirrors to a slit that defines a new source with adjustable size. A Kirk Patrick Baez mirror system is subsequently used to de-magnify the new source to the sample position. The monochromatic beam is generated in a double crystal monochromator with presently two sets of crystals in use to cover an energy range from 2.14 (P K-edge) to 20 keV (Nb K-edge, U L3-edge) (Si(111)) and for higher energy resolution in the range of 5 to 20 keV (Si(311)). For XAS in transmission mode three ionization chambers are installed. For XRF and XAS in fluorescence mode a 7 element Si(Li) detector (210 mm2 detector area) and a single element SDD detector (50 mm2 detector area) are available, All detectors except the SDD detector can be operated under vacuum to reach K absorption edges of e.g., P, S, Cl. Also the CCD detector for XRD is vacuum compatible to avoid its dismounting during vacuum operation. Besides bulk analysis microfocus XRF, XAS and XRD, grazing incidence XAFS (GI-XAFS), total e-yield XAFS or fast continuous measuring XAFS (Q-XAFS) are offered to users. The beamsize can be varied from approximately 1 x 1 mm2 to 50 x 40 µm2. Q-scans allow XANES measurements in typically 1 min. Total e-yield measurements are restricted to conductive samples.Since 2007 the beamline is operating almost 100% in user operation, needing now some time for major upgrades.

UpgradesThe signal to noise ration of the ionization chambers has been improved by replacing them with new ones of less dead volume from ADC which almost doubles the count rates. To enable for example reflectivity measurements an avalanche photodiode providing the required large dynamic range has been installed on the detector arm of the goniometer. Readout times for complete fluorescence spectra could be reduced from 300 ms down to 30 ms by exchanging the old amplifier electronic for the fluorescence detectors (7 element SiLi and 1 element SDD) to the xmap electronic (XIA). A more failsafe operation of beamline devices like CCD detector or light microscope is expected from their controlling via tango servers. As an additional benefit the alignment microscope can be used now in different magnifications because the drift of the image center during zooming is automatically corrected. After 7 years of continuous operation some components of the beamline

required a major technical overhauling. Two motors and the Si(111) crystals of the DCM were replaced. Also the 7 element SiLi detector is currently at the factory site for a basic maintenance. On users demand a flow-through cell for liquids with Kapton windows and micro pumps are now available needing only small amounts of liquid. Without its flow through option this cell has been successfully applied during measurements for an industrial customer.The capacity for mounting samples as pellets has been increased from 6 to 18 by printing out a newly designed holder with a 3D printer.Within inhouse research activities a CCD detector (PCO edge) was purchased, implemented and tested to trigger the development of full field spectroscopy that will enable simultaneous recording of several thousands of transmission X-ray absorption spectra. Application fields are for example imaging of red-ox gradients in materials for catalysis.

SUL-X X-ray beamline for Environmental Studies

............................................Information

SUL-X is the X-ray beamline of the ANKA Synchrotron Radiation Laboratory for Environmental Studies. It offers bulk and microfocused X-ray analytical techniques for a wide energy range to contribute for example to a better understanding of heterogeneous systems as they occur in the environment of contaminated sites.

Ralph Steininger: [email protected]

Jörg Göttlicher: [email protected]

Beamline: +49 (0)721 608 26307

COntACt

Spectroscopy



Figure 1: Avalanche photodiode (APD) mounted on the 2theta arm next to the CCD detector. For reflectivity measurements a slit system can be mounted in front of the APD.

Figure 2: Flow-through cell (right) with connected micro pump (left at the rim of the beaker) and pump controller (background). (Yellow) Kapton foils are used as cell windows.

Future upgradesA compact theta-2theta goniometer in vertical geometry for small samples is under construction that will enable for example measurements of X-ray absorption spectra in different crystallographic orientations of single crystals. It can also be equipped optional with a photodiode or avalanche photodiode as detector. Because no conventional cryogenic sample holder fits to the SUL-X base plate a specific cryo stage is under construction for cooling samples down to -100°C. It could be used for samples being sensitive to beam damage or to investigate phase transformations. There are plans to replace the SiLi detector with a larger SDD, accepting higher count rates and therefore being more capable of detecting trace elements.

User OperationDuring the last calls the majority of beamtime at the SUL-X beamline is donated to users. The highest fraction of proposals during April 2012 until March 2013 came from the environmental research (56% of the granted proposal, 57% of all proposals), Material Science (31% of the granted proposals, 22% of all proposals), and to equal fractions from LSC, CM, NMT, CAT.Apart from the users time approximately 24% of the total beamtime is used for in-house research, about 4% for industrial use and 9% for improvements and 5% for maintenance, the latter is increasing due to the aging of the components. Main in-house research activities included the analyses of thin films (Eu, V for hard coatings) with EXAFS and XRD. A hydrothermal reaction chamber that can be operated up to 10 bar pressure has been constructed from the KIT Celitement group and is used to track mineral phase reaction in different T,p,t paths with respect to the development of a new cement type. The full field spectroscopy method was tested at reference samples. The investigation of sulfur speciation has been extended to additional silicates. The user publication of Lalinská-Voleková et. al (2012) about the weathering products of Fe-As-Sb mine wastes and soils at several Sb deposits in Slovakia received the Hawley Medal of the Canadian Mineralogical Society for the best publication in the Canadian Mineralogist 2012.

Publications of users1. R.M. Bolanz, J. Majzlan, LJurkovic J. Göttlicher, Mineralogy, geochemistry,

and arsenic speciation in coal combustion waste from Nováky, Slovakia, Fuel, (2012) 94,125–136

2. Bertrand, L., Cotte, M., Stampanoni, M., Thoury, M., Marone, F., & Schöder, S., "Development and trends in synchrotron studies of ancient and historical materials", Physics reports-Review section of physics letters 519 (2012/10) pp. 51-96

3. West, M., Ellis, A. T., Potts, P. J., Streli, C., Vanhoof, C., Wegrzynek, D., & Wobrauschek, P., "Atomic spectrometry update-X-ray fluorescence spectrometry", Journal of Analytical Atomic Spectrometry 27 (2012) pp. 1603-1644

4. O. Noked, A.Melchior , R.Shuker, T.Livneh, R.Steininger, B.J.Kennedy d, E.Sterer“Pressure-induced amorphization of La1/3TaO3”, Journal of Solid State Chemistry 202 (2013) 38–42

5. Farnsworth, C. E., Voegelin, A., & Hering, J. G., "Manganese Oxidation Induced by Water Table Fluctuations in a Sand Column", Environmental Science & Technology 46 (2012/1/3) pp. 277-284

6. Shen, L., Yang, S.-W., Xiang, S., Liu, T., Zhao, B., Ng, M. F., Goettlicher, J., Yi, J., Li, S., Wang, L., Ding, J., Chen, B., Wei, S.-H., & Feng, Y. P., "Origin of Long-Range Ferromagnetic Ordering in Metal-Organic Frameworks with Antiferromagnetic Dimeric-Cu(II) Building Units", Journal of the American Chemical Society 134 (2012/10/17) pp. 17286-17290

7. Och, L. M., Müller, B., Voegelin, A., Ulrich, A., Göttlicher, J., Steininger, R., Mangold, S., Vologina E.G., & Sturm, M., "New insights into the formation and burial of Fe/Mn accumulations in Lake Baikal sediments", Chemical Geology 330 (2012/9) pp. 244-259

8. Pekov, I. V., Chukanov, N. V., Britvin, S. N., Kabalov, Y., Göttlicher, J., Yapaskurt, V., Zadov, A. E., Krivovichev, S., Schüller, W., & Ternes, B., "The sulfite anion in ettringite-group minerals: a new mineral species hielscherite Ca3Si(OH)6(SO4)(SO3)·11H2O, and the thaumasite-hielscherite solid-solution series", Mineralogical Magazine 76 (2012/10/1) pp. 1133-1152

9. LALINSKÁ-VOLEKOVÁ, B., Majzlan, J., Klimko, T., Chovan, M., Kucerova, G., Michnova, J., Hovoric, R., Göttlicher, J., & Steininger, R., "Mineralogy of Weathering Products of Fe-As-Sb Mine Wastes and Soils at several Sb Deposits in Slovakia", Canadian Mineralogist 50 (2012/4/11) pp. 481-500

10. Chukanov, N. V., Varlamov, D. A., Nestola, F., Belakovskiy, D. I., Goettlicher, J., Britvin, S., Lanza, A., & Jancev, S., "Piemonite - (Pb), CaPbAl2Mn3+[Si2O7][SiO4]O(OH), a new mineral species of the epidote supergroup", Journal of Mineralogy and Geochemistry = Neues Jahrbuch für Mineralogie - Abhandlungen 189 (2012/7) pp. 275-286

11. Czapla, J., Kwiatek, W. M., Lekki, J., Steininger, R., & Göttlicher, J., "Determination of Changes in Sulphur Oxidation States in Prostate Cancer Cells", Acta Physica Polonica A 121 (2012/3/14) pp. 497-501

12. Paikaray, S., Göttlicher, J., & Peiffer, S., "As(III) retention kinetics, equilibrium and redox stability on biosynthesized schwertmannite and its fate and control on schwertmannite stability on acidic (pH 3.0) aqueous exposure", Chemosphere 86 (2012/3/14) pp. 557-564

13. Tampieri, A., D'Alessandro, T., Sandri, M., Sprio, S., Landi, E., Bertinetti, L., Panseri, S., Pepponi, G., Goettlicher, J., Banobre-Lopez, M., & O. Noked a,b,n, A.Melchior a, R.Shuker b, T.Livneh a, R.Steininger c, B.J.Kennedy d, E.Sterer a,e, “Pressure-induced amorphization of La1/3TaO3”, Journal of Solid State Chemistry 202 (2013) 38–42 Rivas, J., "Intrinsic magnetism and hyoerthermia in bioactive Fe-doped hydroxyapatite", Acta Biomaterialia 8 (2012) pp. 843-851

14. Ziegler S, Dolch K., Geiger K., Krause S, Asskamp M., Eusterhues K., Kriews M., Wilhelms-Dick D., Goettlicher J., Majzlan J., Gescher J. (2013) Oxygen-dependent niche formation of a pyrite-dependent acidophilic consortium built by archaea and bacteriaThe ISME Journal (2013), 1–13

Inhouse research1. Goettlicher J., Kotelnikov A., Suk N., Kovalski A., Vitova T., Steininger

R. (2013) Sulfur K X-ray absorption near edge structure spectroscopy on the photochrome sodalite variety hackmanites. Z. Kristallogr., 228, 157-171

2. Stefan Mangold, Ralph Steininger, Tomy dos Santos Rolo, Jörg Göttlicher “Full field spectroscopic imaging at the ANKA-XAS- and -SUL-X-Beamlines”, Journal of Physics: Conference Series 430 (2013) 012022, 15th International Conference on X-ray Absorption Fine Structure (XAFS15)

3. D Issenmann, S Ibrahimkutty, R Steininger, J Göttlicher, T Baumbach, N Hiller, A-S Müller, A Plech, „Ultrafast laser pump X-ray probe experiments by means of asynchronous sampling” Journal of Physics: Conference Series 425 (2013) 092007


For call 21 over 50% of available beamtime is awarded to external projects (including the 20% U.K. contingent). IBG-2´s in-house research was mostly focusing on secondary structure analysis and aggregation behavior of different antimicrobial and cell-penetrating membrane-active peptides (KIGAKI, Sb056, TP10, SAP) and their mutants in aqueous, micellar or lipidic environments and reconstitution studies of helical transmembrane segments of the oncoprotein E5 and its natural receptor PDGFR β in unsaturated lipids of varying hydrocarbon chain length.

Beamline improvements and upgrades in 2012

SRCD measurements at UV-CD12 in the first year of user operation still were compromised from a relatively low photon flux of 7x1010 photons s-1, requiring long data collection times and resulting in reduced sample throughput. In the April 2012 shutdown the old LiF exit window with deteriorated light transmission due to color center formation, which had been induced by the intense UV beam, was exchanged by a new CaF2 window. A major upgrade in the July 2012 ANKA shutdown was the replacement of the preexisting dipole chamber (14 mrad acceptance angle) by a new dipole chamber with a twofold horizontal acceptance angle of 30.8 mrad. Due to these actions taken, the VUV photon flux could be increased to 1x1012 photons s-1 and baseline noise has been reduced by a factor of 3, while typical CD spectral data acquisition times per sample decreased from ~40 min. to ~7-20 min. As a result of dipole chamber exchange a total of 11 user operation beamtime days in August/September 2012 had to be used for extensive re-calibrations and re-adjustments of optical components (grating, PEM, detector).

Figure 3: View of new dipole chamber with a twofold acceptance angle integrated into UV-CD12´s bending magnet. Due to this the photon flux could be increased to 1x1012 ph/s @ 200 nm, 1 nm SBW and 160 mA

Figure 4: Comparison of baseline noise level in the wavelength range 180 - 200 nm before and after dipole chamber replacement (100 µm cylindrical cell filled with water @150 mA beam current, 1 nm SBW, 1 scan, no smoothing). The RMSD baseline noise has been reduced from ±0.3 mdeg to ±0.1 mdeg.

Planned upgradeIn the July 2013 shutdown it is planned to integrate a newly developed sample chamber with a rotatable cell holder for automated oriented CD (OCD) measurements in the experimental setup. Synchrotron-radiation based OCD will be a valuable complementary method to oriented solid-state NMR for getting a global view on peptide secondary structure, alignment and aggregation behaviour in macroscopically oriented lipid membranes. SR-OCD is expected to provide improved spectral data quality at wavelengths < 200 nm compared with conventional OCD especially for unsaturated and long-chain lipid environments.

References

J. Bürck, S. Roth, D. A. Moss, A. S. Ulrich, “Synchrotron radiation circular dichroism (SRCD) at ANKA: new prospects for structural biology

StatusThe Synchrotron Radiation Source (SRS) at the Daresbury Laboratory, which was the world’s first particle accelerator built specifically for the production of synchrotron light, was closed in August 2008 after nearly 30 years of distinguished service. UV-CD12, a high flux vacuum ultraviolet beamline for steady-state and time-resolved synchrotron radiation circular dichroism (SRCD) was a relatively recent addition to the SRS facility having been opened for users in 2003. Conceived and financed by the BBSRC Centre for Protein and Membrane Structure and Dynamics, UV-CD12 was the highest flux SRCD beamline in the world and has been producing consistently excellent scientific output. SRCD is a rapidly growing biophysical technique for (secondary and tertiary) structure analysis of proteins, nucleic acids, carbohydrates and other biomaterials. Due to the fact that the CD group at the Institute of Biological Interfaces (IBG-2, KIT Campus North) had some ten years experience with conventional CD techniques, following the closure of SRS UV-CD12 was donated to IBG-2 and ANKA in order to continue its working life and become active again as a facility for internal use within Helmholtz Association´s program “BioInterfaces” as well as for the external user community. After the beamline components and experimental setup for liquid-state measurements of proteins had been assembled and installed by IBG-2 and IPS staff in 2010, commissioning work was finalized in early summer 2011 and regular user operation started in October 2011 (call 18).

User access to UV-CD12 at ANKAUV-CD12 is a CRG beamline at ANKA, operated by the neighboring IBG-2. 20% of the beamtime is used by this institute for in-house research and support of other KIT projects within the “BioInterfaces” program. Over a period of 5 years, which started in October 2011, another 20% of beamtime is granted to the existing British user community in exchange for the gift of the beamline. The remaining beamtime is available to ANKA’s user community via the standard peer-review application procedure.

User operationIn the last 1.5 years of regular user operation UV-CD12 has proven to be a valuable tool for structural biology research and confirmed the expected performance. This can be deduced from the fact that three experienced British user groups - among these SRCD experts Prof. B.A. Wallace and Prof. R. Janes from the University of London - in each call were using the 20% U.K. contingent to full capacity. Moreover, starting already in call 18 the

Figure 1: View of the exit slit section with the UHV exit window, the CD data acquisi-tion and control electronics, the optical table with the SRCD experimental setup and the work bench for mounting of the sample cuvette holder

beamline repeatedly has attracted external users from German universities (Hamburg, Kaiserslautern, Marburg), which performed, e.g., conformational or ligand binding studies on various bio-macromolecules such as myelin-related proteins, synthetic mini-collagens or the model membrane protein Mistic, which is investigated for understanding the forces that govern the folding and stability of membrane proteins. A group from Brasil had beamtime for studying the folding of the antimicrobial peptide Plantaricin in different bacterial model membranes to understand the mechanism of action of this natural food preservative.

UV-CD 12 Beamline for Circular Dichroism Spectroscopy in the Ultra-Violet Wavelength Range

............................................Information

UV-CD12 is a high flux vacuum-ultraviolet/ultraviolet beamline for steady-state synchrotron radiation circular dichroism (SRCD). It is owned and operated by KIT´s Institute of Biological Interfaces (IBG-2)

Jochen Bürck: [email protected]

Siegmar Roth: [email protected]

Bianca Posselt: [email protected]

Beamline: +49 (0)721 608 29222

COntACt

Spectroscopy



COntACt

Figure 2: Optical table with experimental setup for liquid-state SRCD measurements of proteins including a fast Peltier thermostat unit for protein thermal denaturation


With a bending magnet as the source, IFP’s soft x-ray analytics facility WERA covers photon energies from 100 to 1500 eV with a resolution E/ΔE up to 104. Linear and circular polarization can quickly be selected and switched. Experimental stations for photoemission electron microsopy (PEEM), for soft x-ray absorption (NEXAFS) and photoemission (PES, ARPES), and for soft x-ray magnetic dichroism (XMCD) are in operation. The latter is provided by the Max-Planck Institute for Intelligent Systems (MPI-IS), Stuttgart, in the framework of a long-term cooperation. The stations are connected in ultrahigh vacuum to preparation chambers such as for pulsed-laser deposition (PLD), for thin-film and surface preparation, and for carbon-based and other nanomaterials. Auxiliary in-situ analysis by methods like LEED and RHEED is available.

The spectroscopic techniques provide a multi-faceted and detailed picture of the electronic and magnetic structure, covering aspects like band or orbital character and occupancy, charge, orbital, or magnetic order, spin and orbital magnetic moments; they address diverse energy scales and various degrees of bulk and surface sensitivity; they can be made specific to elements, to lattice sites, or even to valences of a single element; and imaging of topographic, chemical, or magnetic contrast as well as spectromicroscopy (μ-NEXAFS, μ-PES, μ-ARPES, μ-XMCD) provides laterally resolved information. The setup is designed for combining all these spectroscopic and preparation techniques in order to obtain further insight.

Recently, MPI-IS has upgraded the XMCD station by a fast-ramp magnet providing high magnetic fields up to 7 T. Radiation from an undulator (presently on loan from NSRRC, Taiwan) will be available at WERA; all methods will benefit greatly from the increased photon flux and flux density at the sample.

Acknowledgements: We thank E. Goering, T. Tietze, and G. Schütz (MPI-IS Stuttgart), M. Merkel and N. Weber at Focus GmbH (Hünstetten), G. Schönhense (Universität Mainz), and C. S. Hwang and colleagues at the NSRRC (Hsinchu, Taiwan) for their continuing support.

WERA Soft x-ray analytics facility

Stefan Schuppler: [email protected] +49 (0)721 608 24631Peter Nagel: +49 (0)721 608 24631

Michael Merz: [email protected] +49 (0)721 608 24631 Beamline +49 (0)721 608 28153

COntACt

Spectroscopy/Imaging



COntACt


beamline at the high quality level. 4 days of beamtime per year were used to show the capabilities of the beamline for radiography. These complex experiments can be done only in cooperation with the beamline scientist.

Status

The XAS beamline spans the energy range from 2.4 to 27 keV. This covers the K-edges from S to Cd, and up to the L-edge of U. The double crystal monochromator design allows exchanging the two parallel mounted Si(111) and Si(311) crystal pairs within minutes. There are two principal modes of detection: transmission and fluorescence measurements. The fluorescence radiation emitted by the sample as a function of photon energy is recorded using different energy dispersive detector. Additional to standard EXAFS the XAS beamline offers grazing incident XAFS (GI-XAFS) and Q-XAFS. While the standard XAFS-mode is suited for measurement longer than 30 min, the Q-XAFS mode enables scan times of 30 sec. Even with this mode it is possible to read out the complete fluorescence spectrum for each incoming photon energy due to the XIA-XMap electronic (1 year stable user operation). This will enable a multi-peak fitting of the fluorescence spectra throughout the spectrum and, thus, a higher precision of the resulting data. Typical beam size is 8 mm (hor) x 1 mm (ver) (range 1 x 1 mm2 to 20 x 2 mm2).

The XAS beamline offers different types of sample stages: While the high throughput sample stage offers fast sample exchange at standard conditions, a closed cycle He-cryostat can be used for measurements down to 15 K. A goniometer can be used for the integration of large set-up’s (75 kg) and GI-XAS measurements. In future a sample stage based on cooling with liquid N2 will offer faster sample exchange with cryostat.

Developments In winter 2012/13 and spring 2013 we re-optimized the bragg-axis of the DCM and could improve the position times during step scan to below 0.7 seconds per point. Upgrades on the Q-XAFS scan macro now allows to use three different acquisition times during one continues scan. To allow changing the reference foil during multi-edge Q-XAFS scans (for example: Mn, Fe, Co) the movement of the reference sample is now possible within 3.5 seconds. One PI-Hexapod offers an additional option to position the sample very fast.

A new heavy load experimental table (6 degree of freedom) was installed in summer shutdown 2013 to be able to handle experiments with heavier und more complex sample cells. Even with the 6 degree of freedom, the

table surface is now 8 cm lower as before (beam height over table 53 cm). In addition to these two advantages, the re-alignment of the experimental set-up after changed positions of the electron beam can be done within 1h. The detector systems are now installed on a multi detector holder, which enables fast changes from 5 element Ge-detector to the vortex detector. In future a 6 element SDD with a 100 mm2 per element will be available. This detector offers even higher throughput with an energy resolution below 210 eV at 260 ns peaking time. The monolithic design has the advantage of nearly no dead space in between the detector pixel. A liquid sample cell was developed in cooperation with SUL. The advanced design of the cell provides very small changes of the volume due to very low vibration of the pump and very stiff windows.

Planned Upgrades To enable faster changes of the set-up a laser alignment systems and a special clamp system is in development. In the mid term future it is planned to develop a new cryostat system and to extend the low energy set-up to be able to handle small in-situ set-ups.

User operationThe XAS beamline is constantly overbooked and the maximum possible user operation is mainly limited by the availability of technical- and IT-support. Hot topics are battery science, catalysis, thin layers and environmental science. The quota of complex in-situ experiments is constantly increasing. A reasonable maintenance time of less than 10 % is used to keep the

XAS Multipurpose high throughput XAS beamline

............................................Information

The ANKA XAS beamline offers XAnES (X-ray Absorption Near-Edge Structure) and EXAFS (Extended X-ray Absorption Fine Structure) measurements in transmission and fluorescence mode, spanning the energy range from 2.4 (Sulphur K edge) to 27 keV (Cd K-edge). The typical beam size is 8 mm (hor) x 1 mm (ver), but beam sizes of 1 x 1 mm2 to 20 x 2 mm2 are easily available. Beside the standard XAFS measurements, Quick-XAFS and grazing incidence XAFS are possible.

Stefan Mangold: [email protected]

Beamline: +49 (0)721 608 26647

COntACt

Figure 1: The experimental hutch with 5 element germanium detector

Figure 2: Experimental table (under construction)

Spectroscopy



MPIStructural characterization of materials

Scattering and Imaging

NANOHigh resolution X-ray diffraction beamline, surface and interface scattering

PDIFFX-ray powder diffraction beamline

SCDSingle crystal X-ray diffraction beamline

IMAGEX-ray imaging beamline

TOPO-TOMOX-ray topography and tomography beamline

Beamline Report


MPI BeamlineStructural characterization of materials

Scattering

Peter Wochner: [email protected]: +49 (0)721 608 26728

COntACtFLUO | INE | IR1 | IR2 | SUL-X | UV-CD12 | WERA | XAS | MPI | NANO | PDIFF | SCD | IMAGE | TOPO-TOMO | LIGA I, II, III


COntACt

StatusThe MPI beamline is best suited for the in-situ investigation of structural and magnetic properties of nano-scaled systems, i.e., surfaces, interfaces, nanoparticles, thin films and multilayers under industrially and environmentally relevant conditions like high temperature/gas pressures, external mechanical forces, aggressive gas atmospheres or strong electric or magnetic fields. The available X-ray technologies are X-ray diffraction and reflectivity, crystal truncation rod scattering, grazing incidence diffraction, and (thin film) powder diffraction. It is owned and operated by a consortium of Max-Planck-Institutes.

The core areas of user’s experiments in 2012 included

• Structure of rare earth transition-metal oxide single crystals, thin films and multilayers

• Ex-situ studies of semiconductor nanostructures

• Oxidation of metallic alloys

• In-situ growth of metallic alloy films

• In-situ stress measurements and fault structures in metallic alloy thin films

• In-situ reactive changes of the surface structure and morphology of intermetallic phases

Developments On April 2012 the organizational structure of the beam line changed from being a general scientific facility of the Max-Planck-Institute for Intelligent Systems to a CRG consisting of several Max-Planck-Institutes as well as KIT.It is planned to upgrade the beamline significantly to ensure a reliable operation by changing all motor power supplies and controllers to ANKA’s standard Middex controllers. The detector arm will be modified to eliminate possible collisions and a 12 foil absorber changer will replace the 4 foil one. A new small closed cycle refrigerator for our small Huber Eulerian cradle should provide cooling down to 10K.

Figure2: 2+3 diffractometer in the experimental hutch. The experimental stage can take up heavy duty sample environments for in situ experiments.Figure 1: Schematic Layout of the MPI-MF beamline optics.

Beamline optics


3D reciprocal space mapping of diffuse scattering for the study of stacking faults in semi-polar 10-11 GaN layers grown from Sidewalls of (11-23) patterned sapphire substrate

Nonpolar and semipolar-oriented InGaN-based Light-emitting diodes (LEDs) have been fabricated using various oriented semipolar and nonpolar GaN layers with the main focus to achieve a reduced internal electric field and optical polarization anisotropy toward the surface. The achievements and the challenges in the developments of nonpolar/semipolar nitride LEDs, and prospecting future potentials and requirements were recently summarized by Masui et al [1]. It is fairly known that semipolar and nonpolar GaN layers grown on sapphire substrate have a very high density of threading dislocations (TDs) and stacking faults (SFs). It was found that the nucleation of GaN on the c-plane-like sapphire sidewall results in selective growth from the sapphire sidewall, and nonpolar or semipolar GaN can be obtained. Okada et al [2] and Scholz [2] have explained the growth concept as follow: Trenches that are a few micrometers in width and depth are prepared on a foreign substrate to ensure that one sidewall of the trenches acts as a nucleation plane for c-plane GaN growth. 3D reciprocal space mapping (3D-RSM) of semi-polar GaN oriented 10-11grown on (11-23) patterned sapphire substrate is found to be a powerful and crucial method for the analysis of diffuse scattering originating from the stacking faults which are diffracting in the non-coplanar geometry. 3D-RSM method enabling to distinguish clearly between the diffuse scattering signals coming from the prismatic stacking faults and from the basal plan stacking fault and from the partial dislocation in semi-polar GaN. Figure 1a shows the 3D RSM of the reflection 10-11 where the three characteristic streaks are visible, the

stacking fault streak, the crystal truncation rod CTR and monochromator streak M besides diffuse scattering around the main peak which originating from the partial dislocation PD. The 3D-RSM was recorded at the Nano beamline using the linear detector Mythen 1K having 1280 channels with 50 µm channel size. The distance sample-detector of 1421 mm offers the angular resolution of 0.002 degrees. Any diffraction plan could be easily derived from 3D-RSM to perform 2D-RSM which gives the plan containing simultaneously. By fitting the profile along the streak using the Monte-Carlo simulation approach of Barchuk and Holy et al [3], the stacking fault could be determined.

nAnO High resolution X-ray diffraction beamline

Scattering

Sondes Bauer: [email protected] Beamline: +49 (0)721 608 29126

COntACt

............................................Information

The beamline has two operational stations: NANO1 and NANO2 in implementation and testing phase. NANO1 is mostly devoted to the investigation of thin film structure and nanostructure using high resolution X-ray diffraction and X-ray diffuse scattering methods while NANO2 is dedicated to the application of Full field Transmission X-ray microscopy in the field of material science at room temperature and in the biological field in the cryo-environment.

Figure 1: (a) 3D-RSM of the 10-11 GaN oriented sample grown on 11-23 sapphire substrate. (b); 2D-RSM derived from the cutting plan containing the SF-streak. (c) ?

Sergey Lazarev1, Sondes Bauer1, Tobias Meisch2, Martin Bauer3, Ingo Tischer4, Ferdinand Scholz2 and Tilo Baumbach1

1: Karlsruhe Institute of Technology (KIT), Synchrotron Facility ANKA, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany.2: Institute of Optoelectronic, Albert-Einstein-Allee 4589081, Ulm University, Ulm, Germany.3: Precision Motors Deutsche Minebea GmbH, Villingen-Schwenningen, Germany

Figure 2: Schematic presentation of the semi-polar grown on n-patterned sapphire substrate with SiN interlayer.

FLUO | INE | IR1 | IR2 | SUL-X | UV-CD12 | WERA | XAS | MPI | nAnO | PDIFF | SCD | IMAGE | TOPO-TOMO | LIGA I, II, III


COntACt

Time-resolved measurements during the fabrication of semiconductor nanostructures require highly specialised equipment. The unique constellation of growth- and characterization laboratories and nearby heavy-duty synchrotron equipment at the NANO beamline provide an environment best suited for in-situ studies.

In-situ experiments aim at reveiling dynamical processes which are paramount for the thorough understanding and tailoring of the final properties of state-of-the art nanostructures, such as quantum dots, nanowires, etc.

At the NANO beamline, the operation of a specialised MBE growth-chamber was implemented in late 2012. During first test experiments X-ray methods like time-resolved fast reciprocal-space-mapping and GISAXS have been successfully applied using a 2D PILATUS 100K and a PILATUS 2M detector respectively.

For further information on the MBE system, please refer to the lab report on page 81.

Development of in-situ X-ray diffraction methods: Implementation of the portable MBE system

Figure 3: Portable MBE system mounted on the heavy-duty diffractometer of NANO at ANKA.


Scattering

Sondes Bauer: [email protected] Beamline: +49 (0)721 608 29126

COntACtFLUO | INE | IR1 | IR2 | SUL-X | UV-CD12 | WERA | XAS | MPI | nAnO | PDIFF | SCD | IMAGE | TOPO-TOMO | LIGA I, II, III


COntACt

nAnO

Nonpolar and semipolar-oriented InGaN-based light-emitting diodes (LEDs) following various approaches have been fabricated with the main focus to achieve a reduced internal electric field and optical polarization anisotropy toward the surface [1]. It is known that semipolar and nonpolar GaN layers grown on sapphire substrates have a very high density of threading dislocations (TDs) and stacking faults (SFs). Several groups have proposed epitaxial lateral overgrowth via selective area growth on patterned substrates by metal–organic vapor phase epitaxy (MOVPE) [1-6] as an advantageous method for obtaining large-area nonpolar and semipolar GaN layers. It was found that the nucleation of GaN on the c-plane-like sapphire sidewall results in selective growth from the sapphire sidewall, and therefore nonpolar or semipolar GaN can be obtained. Okada and Scholz [3,4] have explained the growth concept as follows: Trenches that are a few micrometers in width and depth are prepared on a foreign substrate to ensure that one sidewall of the trenches acts as a nucleation plane for c-plane GaN growth. Under optimized conditions, the epitaxial process starts on the sidewall and continues laterally over the ridges, resulting in the formation of a continuous semipolar GaN layer. Since the basal stacking faults (BFSs) are formed in periodically “-c” wings, their distribution will be consequently inhomogeneous and periodic. For a local resolved mapping of the basal stacking fault density, the focusing of the X-ray beam down to few micrometers is highly required. A micro-focus beam of 10 μm has been reached at the NANO beamline using

component refractive lenses fabricated by Vladimir Nazmov at the Institute of Microstructure Technology IMT. Semi-polar GaN materials grown with the orientation 10-11 on n-patterned sapphire substrate with and without SiN interlayer have been investigated using X-ray micro-diffraction with the goal to determine the stacking fault distribution with a local resolution. A schematic presentation of the semi-polar grown samples S1 and S2 on n-patterned sapphire substrate is shown in figure 5.Figure 6 shows the mapping of the broadening of the profile of sample S2 along the streak with a resolution of 10 μm. The visibility of the diffuse scattering streak on the 2D Pilatus 100 K detector is an indication of the presence of the stacking fault in semipolar GaN grown samples (figure 6). The broadening of the profile along the streak is proportional to the stacking fault density. The deposition of the SiN interlayer on the –c-wing has reduced the stacking fault density and therefore decreases the value of the broadening of the streak profile as shown in figure 4.Local distribution of the BSFs density performed by the microfocus experiment at the NANO beamline for the (10-11) GaN samples S1 and S2 enables determining the ρBSF maps from the FWHM of the BSFs profiles. The ρBSF maps demonstrate the inhomogeneity of the basal stacking fault density distribution (figure 7). Moreover, the correlation of the ρBSF

periodicity with the semipolar GaN stripes is demonstrated. It should be

emphasized that locally resolved investigation of BSFs using microfocus beam is highly recommended for semipolar GaN grown on pre-patterned sapphire substrate since the BSFs distribution is strongly infuenced by the GaN stripe formation.

References:

[1] T. Wunderer, F. Lipski, J. Hertkorn, P. Brückner, F. Scholz, M. Feneberg, M. Schirra, K. Thonke, A. Chuvilin and U. Kaiser (2008), Phys. Stat. Sol. C 5, No6, 2059[2] S. Schwaiger, L. Argut, Th. Wunderer, R. Rösch, F. Lipski, J. Biskupek, U. Kaiser and F. Scholz (2010), Appl. Phys. Lett. 96, 231905[3] N. Okada, A. Kurisu, K. Murakami, K. Tadatamo (2009), Appl.Phys. Exp. 2, 091001[4] F. Scholz (2012), Semicond. Sci. Technol. 27, 024002[5] S. Schwaiger, S. Metzner, T. Wunderer, I. Argut, J. Thalmair, F. Lipski, M. Wieneke, J. Blaesing, F. Bertram, J. Zweck, A. Krost, J. Christen, and F. Scholz (2011), Phys. Status Solidi B 248, 588[6] Y. Honda, Y. Kawaguchi, S. Ohtake, M. Tanaka, and N. Sawaki (2001) J. Cryst. Growth 230, 346 [7] V. K. Kabra, and D. Pandey (1995) Acta Cryst. A 51, 329

Samples Results: ScansSet-up

Local Resolved Determination of Stacking Fault in Semi-Polar GaN using Microfocus X-ray diffraction at the NANO Beamline

Figure 4: a) View of the microfocus experiment with b) compound refractive lens (CRL) manufactured by LIGA (IMT) and the c) CRL’s structures

Figure 7: Comparison of the BSFs density scans of a) sample S1 without SiN mask, and b) sample S2 with SiN mask.

Figure 6: The sketch of the experiment with 2D detector (a), the single frame of the 10-11 GaN reflection with BSFs streak in the plane of the detector and the fit of the I(Qstr) profile along the streak.

b)

a)

c)

a)

b)

Figure 5: Schematic presentation of the semi-polar grown samples S1 and S2 on n-patterned sapphire substrate without (a) and with (b) SiN interlayer respectively.

a)

b)

Sondes Bauer1, Sergey Lazarev1, Vladimir Nazmov2, Tobias Meisch3, Ferdinand Scholz3 and Tilo Baumbach1

1 Karlsruhe Institute of Technology (KIT), Synchrotron Facility ANKA, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany2 Karlsruhe Institute of Technology (KIT), Institute of Microstructure Technology, Hermann-von-Helmholtz-Platz 1, 76344 Eggestein-Leopoldshafen, Germany3Institute of Optoelectronic, Albert-Einstein-Allee 45, 89081 Ulm University, Ulm, Germany

Experiment


Scattering


StatusThe ANKA-PDIFF beamline is designed for diffraction experiments on bulk and thin film polycrystalline materials. The main application of the beamline is the investigation of bulk polycrystalline and nanocrystalline materials un-der varying in-situ conditions, and for high-resolution powder diffraction and residual-stress and texture measurements. In addition the beamline is well suited to performing high-resolution scattering studies on single-crystals and epitaxial thin films.

The beamline is situated on a bending magnet and delivers monochromat-ic X-rays in the energy range between approximately 6keV and 20keV. The beamline optics consist of a focusing cylindrical mirror and a Si-111 double crystal monochromator.

The experimental station houses two independent diffractometers, each opti-mised for specific types of experiments:

• Station 1: a heavy-duty 3-axis powder diffractometer capable of car-rying simultaneous multiple detector systems and sample loads up to approx. 60kg for in-situ characterisation of nanocrystalline and microcrystalline materials under non-ambient conditions. This dif-fractometer is equipped with 2 main detectors: a 165mm diameter 2D CCD camera and a 90° 1D detector for simultaneous registration of x-ray scattering over a large 2Theta range.

• Station 2: a 4-circle Kappa diffractometer carrying up to approx. 5kg loads and equipped with either analyzer-crystal or Soller collimator optics for high angular resolution studies. This instrument can also optionally carry the CCD camera or the 1D linear detector.

A number of sample environments allow for heating and cooling experiments in both reflection and transmission geometry between approximately -180°C and 1000°C. A tensile/compression stage (2kN) is also available for in-situ mechanical deformation studies.

DevelopmentsThe major effort in the past year has been to improve the facilities for in-si-tu experiments being done on the large (heavy-duty) powder diffractom-eter. One aspect of this has been the development and installation of a 3-axis translation stage for the mounting and positioning of various sample chambers. In the near future this will allow users to mount their own sample chambers based on a standard technical description of the available space and mounting details on the XYZ-translation stage. Additionally a motor-ized linear stage is now in construction which will replace the manual stage carrying the CCD detector. The motorized stage allows automatic adjust-ment of the position of the CCD camera from approx. 140mm to 1000mm from the sample.A motorized beam-stop for the CCD camera which implements a small area PIN-diode for measurement of the direct beam intensity has recently been installed.

On the 4-circle Kappa instrument a compact XYZ-stage has been realized for positioning of flat (thin-film etc.) samples. An additional high-resolution Soller-collimator has also been installed which provides a factor of 10 to 20 in-creased intensity compared to the high resolution analyzer setup but with a fac-tor of around 2 to 3 decreased angular resolution. For experiments which don’t require the highest angular resolution this collimator is ideal since it speeds up measurements by an order of magnitude with tolerable loss in resolution.

On the software side there have been significant improvements in the stability of the TANGO-driver for the Princeton CCD camera which mean that this detector is really now in a useable state, with many groups now utilizing this exclusively for their experiments. Coupled to this we have implemented additional SPEC macros to improve automated data-acqui-sition, temperature and positional control and visualization during in-situ experiments.

User OperationThe improvements on the heavy-duty diffractometer are reflected in the increased usage of the instrument in 2011-2012 - over 50% of the projects on the beamline were performed on the new diffractometer. Of particular mention are the studies performed by groups from the Institute for Applied Materials and the Institute (KIT-South Campus) and the Institute of Nanotechnology (KIT-North Campus) who have installed their own sample-conditioning setups at the beamline to perform state-of-the-art in-situ experiments.

PDIFF X-ray powder diffraction beamline

............................................Information

The ANKA-PDIFF beamline is a facility for diffraction experiments which require high resolution in both energy and scattering angle. It is optimized in the first instance, but not exclusively, for experiments on polycrystalline materials.

User Operation Accelerator Report Beamline Report Lab Report Applications Appendix Stephen Doyle: [email protected]

Beamline: +49 (0)721 608 26648

COntACt

Figure 1: CCD image.Figure 2: Integrated/calibrated 2theta-intensity data .

Figure 3: In-situ XRD setup for investigation of phase changes in Li-ion cells (Indris et al. INT, KIT-Campus Nord).

Figure 4: Cell for in-situ XRD.

Area Diffraction Machine


StatusAt the ANKA-SCD beamline the structure of complex, crystallized moleculescan be revealed by means of Single Crystal X-ray Diractometry. This technique yields the atomic coordinates within the unit cell of a single crystal. Due to the high incoming photon flux, ANKA-SCD is often used for the structure determination of small or weakly diffracting crystals. Two single-crystal diffractometers are available for this purpose that can be used alternatively, one equipped with a large (Ø 340mm2) but comparatively slow image plate detector and one with a small (60∙60mm2) but relatively fast CCD detector. In addition, diffraction studies on surfaces and interfaces, such as semiconductor interfaces, also nanostructured surfaces and interfaces, are feasible. A 6+2 - circle diffractometer that we received as a permanent loan from the LAS at KIT Campus South is available for this task. It features X-ray diffraction methods such as Reciprocal Space Mapping, X-Ray Reflectometry and Grazing Incidence Diffraction.

DevelopmentsAfter the installation of the 6-circle diffractometer in 2006 the instrument was gradually upgaded to perform tasks in the fields of surface and interface characterisation. These upgrades comprehended new detectors, a crystal analyser and a collimating beam path equipped with motorized slits for GID studies. The added devices enhanced the methodical capabilities of the instrument, but also inreased the load on the detector arm (the “del” arm) until the maximum allowed load was exceeded. At the same time the collimating beam path reduced the degrees if freedom of the instrument by introducing the possibility of mechanical collisions. Therefore the decision was made to design a new leightweight analyser and a leightweight collimating beam path with a compact slit drive. By this the entrance slits can be placed close to the sample with little obstuction of the diffractometer circle movements. The analyser possesses two motorized circles now, one for the analyser crystal and one for the detector. Previously only one circle was motorized because of weight considerations. Now we use a small stepper motor driven goniometer circle (MICOS) to dene the 2θ position of the detector, and a SMARACT rotary positioner SR-5714-S with piezo drive and encoder for defining the angular position of the analyser crystal. Not only does this reduce the load on the “del” arm considerably, but it also allows to define the θ setting of the analyser crystal with a resolution down to 0:05”. The SMARACT rotary positioner can be addressed in the same way as any ordinary stepper motor in the spec control interface by means of a TANGO driver. This renders collective scans, e.g. θ – 2 scans of the analyser, possible by invoking the usual spec macros like d2scan. Three basic experimental congurations of the station will be supported: Mythen 1K PSD with or without analyser, or point detector (YAP or NaI) with beam collimating path. Fast locking elements allow for a quick change of the configurations.For a quick and easy alignment of the goniometer center with respect to the incoming monochromatic beam the instrument has been made moveable in both vertical and horizontal directions perpendicular to the beam by remote control. For that purpose an assembly of motorized jacks and a motorized side translation for the tombstone that carries the diffractometer has been designed and built. The movement of the jacks is synchronized by a spec macro and can be enabled and disabled by electromagnetic brakes.

On the side of the beamline optics, all the old motor controllers from the first phase of beamline construction at ANKA have been replaced by state-of-the-art motor controllers and end phases. This has payed of in a significantly enhanced stability, repeatability and resolution of the positioning of the beamline optical components. The ongoing upgrade program aims at implementing Small Angle X-Ray Scattering and Grazing Incidence Small Angle X-Ray Scattering as methods available to the regular user. This will be achieved by installing a large (Ø 165mm) CCD camera that we received as a permanent loan from the NANO beamline on a rail behind the 6+2 - circle diffractometer and bridging the distance with flight tubes.

User operation

PRC reviewed beamtime at ANKA-SCD was dedicated to the determinationof structures from a variety of systems, such as large paramagnetig aggregates of Transition-metal and Lanthanide cations, novel binary tin halides, polynuclear and luminescent oligonuclear spin transition compounds, semiconduclor cluster molecules, novel catalysts, and to the structural investigation of isotopically enriched silicon multilayers. The organic semiconductor Rubrene has been studied with high-pressure single crystal diffractometry at a photon wavelength of 0.72 Å. The use of a shorter photon wavelength is always desirable for high-pressure diffraction studies, because it increases the transmission of the diamond anvil cell and at the same time the accessible part of reciprocal space. A numerical feasibility study has shown that by lowering the grazing angle of the X-ray mirror and taking the DCM crystal bender to its limits, the SCD beamline can be used at a photon wavelength down to 0.6 Å, of course at the expense of photon flux which will be outbalanced by the increased transmission of the cell. A significant amount of in-house beamtime went into studies of AlGaN epilayers grown on Sapphire with coplanar and non-coplanar diffraction. Densities of screw and edge threading dislocations in these films could been determined 1, an important information for the optimization of these materials for their application in ultraviolet light emitting diodes (UV-LEDs). Furthermore the structure of Eu films on Si substrates and the partial relaxation of LSO:Tb scintillating materials on YbSO substrates have been studied with X-ray diraction.

1S. Lazarev, M. Barchuk, S. Bauer, K. Forghani, V. Holý, F. Scholz and T. Baumbach, J. Appl. Cryst. (2013). 46, 120-127

Scattering

Gernoth Buth: [email protected] Beamline: +49 (0)721 608 26723



Figure 5: Experimental end station with image plateFigure 4: Experimental end station CCD Figure 3: Beamline optical components

SCD Single crystal X-ray diffraction beamline


Imaging


IMAGE/XMICin commissioning

User Operation Accelerator Report Beamline Report Lab Report Applications Appendix Sondes Bauer: [email protected]

COntACt

............................................Information

The twin beamlines IMAGE/XMIC are being constructed in the western straight-section of the ANKA storage ring (Figure 1)The photon source will be a combined superconducting undulator/wiggler, which is currently under development. With this new source, IMAGE/XMIC will cover two energy ranges (in the undulator mode from 4 keV to 20 keV and in the wiggler mode up to 100 keV) and offer X-ray imaging methods tailored to the performance parameters of the ANKA radiation source.

The IMAGE/XMIC beamline will give the possibility to perform experiments simultaneously in two different experimental stations. Three experimental stations will be established for two-dimensional and three-dimensional imaging methods in the hard X-ray range using absorption, phase, and Bragg/Laue diffraction contrast:

Station 1 is a full-field transmission X-ray microscope for hard X-rays, located in the first experimental hutch.

Station 2 for fast white-beam computed tomography/laminography, including coherent imaging by in-line holography, grating interferometry, and 3D micro-diffraction imaging methods, located in the second experimental hutch.

Station 3 will be a hard X-ray microscope dedicated for non-destructive testing based on different types of deep X-ray lithographical lenses with resolution down to 20 nm.

The concept of the twin beamline is shown in Figure 2 and it includes a crystal monochromator, which will be used to horizontally split the beam into two parts.

Half of the beam will be reflected by the crystal monochromator and laterally shifted by 800 mm, then forming the so-called side branch (XMIC), while the second half of the beam will propagate past the monochromator uninfluenced, being the main branch (IMAGE) of the beamline. In the main branch, the beamline optics are designed for a versatile operation with a double-multilayer monochromator (DMM) for projection imaging and microscopy applications, and a double-crystal monochromator (DCM) allowing full-field microdiffraction imaging and diffraction-enhanced imaging. Partially coherent X-rays will be available by reducing the source size in white-beam mode through slits in the Front-End. The side branch will operate in monochromatic mode exclusively, offering focusing capabilities.The hard X-ray microscopy setup dedicated for biological samples will be placed in the Experimental Station 1. Currently, it is installed and operational at the NANO beamline (Figure 3). The full-field transmission microscope is specified for an energy range from 2 keV to 12 keV, based on capillary condensers and high resolution zone plates with a spatial resolution of 30 nm. 2D radiography and 3D tomography are possible in absorption contrast as well as Zernike phase contrast. An X-ray fluorescence detector adds the possibility of mapping elemental compositions within the sample. The high penetration depth of hard X-rays allows for imaging of samples up to several tens of µm thickness. The microscope is equipped with a cryogenic sample environment for vitrified samples in order to enable imaging of biological samples as close to their natural state as possible. Furthermore, the cryogenic sample environment contributes to minimizing radiation damage. First experiments have been successfully conducted.As one of the two experimental stations which will be located in experimental hutch 2 of the IMAGE beamline, the UFO-CODE station is currently in the specification stage. It will cover a variety of scan geometries, contrast mechanisms, and a wide range of temporal resolutions in a single setup for highest flexibility, enabling the full potential of the beamline to be exploited. Besides radiography, both tomographic and laminographic scan geometries will be used for 3D imaging, each mode with the possibility to be operated

Figure 2: The IMAGE beamline layout, using the laterally reflecting crystal as beamsplitter. The optics in the main branch have been designed to deliver either white beam, high-intensity pink beam (with the double-multilayer monochromator) or highly monochromatic beam (with a double-crystal monochromator) for different applications.

Figure 1: Schematic drawing of the IMAGE beamline and the northwest hall extension. The first experimental hutch will host the full-field transmission X-ray microscopy station. The second experimental hutch will host a multi-purpose imaging station for fast tomography, laminography and diffraction imaging, and a hard X-ray microscope dedicated for non-destructive testing based on different types of deep X-ray lithographical lenses.

with various contrast modalities. Using white-beam combined with a flexible transmission detector system optimized for high frame rates, these methods will aim for high speed applications, e.g. enabling tomographic imaging in the sub-second regime. High sample throughput will be enabled by an automatic sample exchange system. Monochromatized X-rays delivered by either the DMM or the DCM will allow for high contrast and high resolution down to the sub-micron range. In addition to absorption contrast, propagation based phase contrast and grating interferometry will give access to complementary sample properties. In addition to transmission based methods, the UFO-CODE station will implement an operation mode dedicated for diffraction imaging experiments like rocking curve imaging or diffraction tomography. This will be supported by a dedicated detector system providing flexible detector positioning in

the whole hemisphere above the sample, allowing diffracted X-rays far off the primary beam direction to be caught.The other experimental station at the IMAGE/XMIC beamline will be dedicated to the hard X-ray Microscopy and Quality Assurance of the optical components, so-called MiQA station. The MiQA is designed to operate in the wide X-ray energy range of 10 keV to 60 keV, ,implementing complementary imaging contrasts in the resolution range of 500 µm up to 40 nm. Furthermore, the MiQA station will serve in characterization and thus in development of the optical components, for example lenses and mirrors with the focus on optical components produced by deep X-ray lithography. To be built as part of Karlsruhe Nano and Micro Facility (KNMF), MiQA station will be completed by an access to KNMF laboratory infrastructure for method-specific lenses fabrication and sample preparation.

The conceptual design of the beamline has been completed. The infrastructures, including the radiation security hutches, the control rooms and the laboratories will be built up (Figure 4) during the 2013 summer shutdown. The Front-End section will be installed with a wiggler insertion device from Daresboury Synchrotron. The first diagnostic elements are currently under construction.

Figure 5: White beam temporary station at the Image beamline. The radiation beam shutter is placed on the right side of the image. The experimental station is positioned on the left side, after a 12 m long vacuum tube.

Planned Implementation

Figure 3: Hard X-ray microscope, to be installed at the NANO beamline and TXM installed a the experimental station Nano2

The radiation security checks (TÜV) of the Image beamline will be accomplished at the end of August 2013, and the first experiments will be performed starting October 2013.The beamline will be operational in white beam mode, and the experiments will be performed in a white-beam temporary station placed in the optical hutch (Figure 5).

Figure 4: Overview of the IMAGE/XMIC beamline infrastructure.


Scattering

FLUO | INE | IR1 | IR2 | SUL-X | UV-CD12 | WERA | XAS | MPI | NANO | PDIFF | SCD | IMAGE | tOPO-tOMO | LIGA I, II, III

StatusSynchrotron X-ray topography delivers a detailed map of the distribution/structure of lattice defects and strains in crystalline samples (dislocations, micropipes, stacking faults), for example in new materials or microelectronic components. Laue X-ray topography provides cross-sectional slice images through the sample (in a manner analogous to TEM) with a fine lateral resolution (<1µm) over large areas.Microtomography and microradiography allows, in a non-destructive manner, to image the internal structure of an object. Microtomography using synchrotron light sources delivers 3D images of the object with high resolutions down to the submicrometer range, an excellent signal-to-noise ratio and additional contrast modes like phase contrast and holotomography. Typical applications for microtomography and microradiography are the detection of voids and pores in industrial components, imaging of tissue and other soft materials in biological and life science, and the characterization of fibre structures and diffusion processes by subsequent 3D image analysis.

DevelopmentDuring the last years the beamline has been equipped with highly specialized components, like optical tables, linear and rotary stages, slit systems, a double multilayer monochromator, detector systems and cameras. Instead of new major investments, in 2012 the main focus has been put on the reliability of the beamline. Existing bugs, mechanical or IT-related, have been fixed and tested. Spare parts of crucial components like a PCO 4000 camera or optical transmitters have been bought in order to guarantee an operational beamline in case of a technical defect.The detectors are an essential part for high resolution X-ray imaging. Therefore, the detector pool at TOPO-TOMO has been upgraded to provide a variety of detector systems suitable for different applications. Detector optics are available both for white and monochromatic beam, ranging from total magnification of 1x to 50x. Depending on the experimental requirements, the detector can be chosen for high sensitivity (0.7 FPS, 5000 gray levels, 9 µm pixel size) or high speed (5400 FPS, 700 gray levels, 20 µm pixel size).

User operationWhite beam X-ray topography: Detailed information on defect distributions in crystals can be provided by synchrotron X-ray topography in which an intense, highly collimated beam of X-rays is directed onto a crystalline sample in Laue or Bragg configuration. This non-destructive analysis technique is mainly used for the study of dislocations, planar defects, stacking faults, growth defects or large precipitates (figure 1). Also very small local defects like nm-scale voids in Si can be imaged as well as long range strain in electronic devices.

High resolution synchrotron radiography and microtomography: High-resolution and phase contrast radiography are used to investigate micro-structured, multi-component material systems, e.g. to detect delaminations between substrates and glob tops encapsulating wire-bonded devices. Radiographs taken from different projection angles allow to obtain three-dimensional information with a spatial resolution down to the sub-micrometer range by means of computed microtomography (compare figure 2 + 3).

The subsequent application of 3D image analysis methods can be used for the determination of size distributions, orientations or spatial correlations within the tomographic, multi-constituent volume images.Phase-contrast imaging with a grating interferometer: Phase-contrast imaging with a grating interferometer (figure 4) provides determination of the refractive index distribution within a sample even for materials with similar refractive indices.

tOPO-tOMO

............................................Information

The TOPO-TOMO beamline is devoted to conventional X-ray topography and micro-imaging both in 2D (radiography) and 3D (tomography). Digital white-beam topography in projection and section topography mode as well as digital white and pink (102 energy resolution) beam radiography and microtomography in absorption and phase contrast are available.

User Operation Accelerator Report Beamline Report Lab Report Applications Appendix Thorsten Müller: [email protected]

COntACt

Figure 2: Volume rendering of the head of a newt larva (Euproctus platycephalus).

Figure 1: X-ray diffraction imaging metrology of 200 mm Si wafer. Ex-situ at room temperature after 60 seconds plateau annealing at 1000 °C(a) t = 0 sec: Laser label and slip bands originating from the notch, (b) t = 168 sec: Crossing of <110> slip bands from the wafers edge, (c) t = 326 sec: <110> slip bands from the wafers edge and defects without dislocation loop formation, (d) t = 442 sec: Defect near the centre of a widely dislocation free area.

Figure 3: Volume rendering of the head of the stick insect Peruphasma schultei. Thick virtual slices allow examination of internal structural details without losing the 3D impression.

Figure 4: Example of the radiography results obtained with a grating interferometer (from left to right): Absorption contrast, differential phase contrast and dark-field (scattering) images of a human tooth with a dental filling.

The TOPO-TOMO white beam station enables high phase sensitivity and spatial resolution of about 5 μm together with a short exposure time below 1 s. By combining a grating interferometer with computed tomography the refractive index distribution can be acquired in a 3D volume.

LIGA I, II, III X-ray lithography beamlines

Micro-Fabrication

Beamline Report


StatusIn 2012 about 20 projects were carried out to develop and fabricate high aspect ratio microstructure components for applications in fluidics, optics and mechanics as well as mould inserts for replication. All projects were done under the frame of KNMF and the external ones underwent KNMF’s review process. Part of the projects are also embedded in the EUMINAfab project (FP7), the European Research Infrastructure offering open access to state of the art of multimaterial micro and nanotechnologies. Project partners come from several countries, like France, Italy and England. In addition the beamlines were also used by the company microworks to manufacture precise LIGA structures for industrial use. All in all 63 % of the beam time was given to external users. In the context of these activities more than 360 samples were processed at the lithography beamlines.

Developments / Planned UpgradesBesides the development and characterisation of new resist formulations within several BMBF projects (INNOLIGA, RöLinGi) a major upgrade will be the upscaling of LIGA III. This will include a double mirror system for multi pupose usage of the beamline.

User operation The majority of user projects concentrated on the fabrication of highly sophisticated micro structures with dimensions down to the 100 nanometers range and extreme aspect ratio (Fluidic Chips, RF MEMS structures, moulding tools, X-ray lenses and X-ray grating structures). In cooperation with the Swansea University (UK) we developed a moulding tool for the fabrication of fluidic chips. A new generation of X-ray LIGA mould inserts was created and investigated within a PhD thesis. RF MEMS structures like metal and polymer antennas were produced with several material properties. This was done together with the TRLabs and the University of Saskatchewan (Canada). X-ray-full-field-microscopy needs lenses e.g. for high photon energies up

to 30keV. As the refractive power of all lens material is very weak, a few hundret biconcave parabolic shaped lens elements are necessary for a focal length of a few centimeters. X-ray lithography is a very suitable process to create these structures. X-ray microscopy experiments with our lenses have been carried out at several synchrotrons like ANKA, Petra III and the ESRF. The quality of our X-ray gratings could be improved further. Actual computer tomography experiments show an improved efficiency due to thinner base material for the gratings and better quality of the lamellas.

The results of these projects have been reported in 16 referenced journals.

LIGA I, II, III X-ray lithography beamlines

Micro-Fabrication

............................................Information

The Institute for Microstructure Technology (IMT) operates the cleanroom facility which is equipped with three LIGA beamlines to perform X-ray lithography. Each beamline is dedicated to a specific task in the LIGA-process, which are high resolution X-ray mask making (LIGA I), deep X-ray lithography (LIGA II) and ultra deep X-ray lithography (LIGA III; currently under commissioning; see coming upgrades) depending on the available spectrum which is filtered by a dedicated mirror in case of LIGA I and LIGA II.

Martin Börner: [email protected] +49 (0)721 608 24437

Pascal Meyer:[email protected] +49 (0)721 608 23924

Franz Josef Pantenburg: [email protected] +49 (0)721 608 22600

Beamline +49 (0)721 608 26855



Figure 2: Look into the exposure station: X-ray lithography mask and a 4 “ - wafer with PMMA coating could be seen.

A more detailed description of the activities can be found in the KNMF Annual Report 2012!

Key parameters of the beamline

LIGA I LIGA II LIGA III

Energy range 2.2 keV - 3,3 keV 2.5 keV – 12.4 keV from 2.5 keV upwards

Source 1.5 T bending magnet,bending radius: 5.559 m

1.5 T bending magnet,bending radius: 5.559 m

1.5 T bending magnet,bending radius: 5.559 m

Optics Be-window thickness: 175 µm in total gracing incidence mirror: Si/200nm Cr @ 15.4 mradoptional low-z filters: C, Al

Be-window thickness: 225 µm in totalgracing incidence mirror: Si/200nm Ni @ 4.85 mradoptional low-z filters and band-pass filters: C, Al, Ti, V, Fe, Ni, Cu

Be-window thickness: 225 µm

Distance: source point-mask plane

14.84 m 14.73 m 15.324 m

Distance: source point -mirror

8.61 m 9.20 m -

Be-window aperture 20 mm (vertical) * 110 mm (horizontal)

20 mm (vertical) * 110 mm (horizontal)

20 mm (vertical) * 110 mm (horizontal)

Usable horizontal fan 108 mm 108 mm 108 mm

Sample / sample envi-ronment

100 mbar He 100 mbar He 100 mbar He

Experimental setup JenOptik Dex02 X-ray scan-ner with tilting option (+/- 60°) and rotation option (362°)

JenOptik DexKfK X-ray scanner with tilting option (+/- 60°),power reduced exposure by using a chopper (optional)

JenOptik DexKfK X-ray scanner with tilting option (+/- 60°),power reduced exposure by using a chopper (optional)

Alignment / instrum. overlay / accuracy

internal, 0.5 µm external, 2 µm external, 2 µm

Software Dex control software with in-terface to beamline control software

Dex control software with in-terface to beamline control software

Dex control software with in-terface to beamline control software

Figure 1: Opened experimental hutch of LIGA II with the exposure station inside. Outside (front): Control Rack of LIGA II.


Introduction The national German synchrotron radiation facility ANKA at KIT is engaged in the KNMF activities of its Laboratories for Microfabrication and Synchrotron Radiation. Within these labs, AnKA’s beamlines provide dedicated user service for the nanoscience and Microtechnology user communities. The beamtime is accessible via the portals for scientific proposal of both ANKA and the KNMF, and is based on a peer-review process. In 2012, 16 % of the available synchrotron beamtime distributed by the proposal review committee was assigned to the field of nanoscience and Microtechnology. A research example from the KNMF Laboratory for Synchrotron Radiation, studying complex hard coating materials, will be discussed below.

In the summer of 2012, three additional AnKA beamlines became accessible via the KnMF proposal portal. These beamlines focus on Infrared/THz spectroscopy and ellipsometry (IR1 beamline), polycrystalline/powder X-ray diffraction (PDIFF beamline), and X-ray absorption spectroscopy (XAS beamline).

The beamlines The IR1 beamline features classical synchrotron radiation and edge radiation from a bending magnet and offers infrared/THz spectroscopy and ellipsometry. The spectroscopy station is based on an FTIR spectrophotometer (Bruker IFS 66v/S), covering a spectral range from 4 to 10,000 cm-1 with a resolution down to 0.1 cm-1, and is equipped with high sensitivity detectors and appropriate beamsplitters. The ellipsometry set-up at IR1 is operated by MPI-FKF Stuttgart and the University of Fribourg, Switzerland, runs under vacuum, and features an optimized bolometer detector and a liquid He cryostat. Coherent THz emission can be exploited when the ANKA accelerator is operated in low-α mode, resulting in an extremely intense beam in the 5 – 50 cm-1 spectral range. In 2013, the IR2 beamline will see a completion of its front-end optimization and commissioning phase. It is envisioned to offer IR microscopy capabilities at IR2 as part of the KNMF Laboratory for Synchrotron Radiation in 2014. The XAS-beamline features X-ray absorption spectroscopy (XAS) on a dipole magnet source. Besides standard XAS measured in transmission (detection limit ~5%) and fluorescence (detection limit 1 mmol/L) modes, the beamline offers a “Quick-XAS” mode, allowing scans as fast as 30 seconds. Grazing incidence XAS provides surface sensitivity in the 50 nm range. The XAS

beamline spans the energy range from 2.4 to 27 keV, covering the K-edges from S to Cd, and up to the L-edge of U. Upgrades performed in 2012 focused on enhanced automation and faster data acquisition. Further ongoing upgrades will allow the use of heavier and larger experimental set-ups.

The PDIFF beamline allows hard X-ray diffraction investigations of bulk polycrystalline materials under varying in-situ conditions and for high-resolution powder diffraction, residual-stress, and texture measurements. It is also equipped to perform scattering studies on thin-films and epitaxial layers, and consists of two experimental stations, a heavy-duty 3-circle powder diffractometer and a 4-circle Kappa diffractometer carrying up to approx. 5 kg loads. The major upgrade efforts focus on the facilities for in-situ experiments on the heavy-duty powder diffractometer, including an implementation of an XYZ-stage for the positioning of various sample chambers and construction of a motorized linear stage for the large CCD detector, as well as the development of macros for automated measurements. As an example of research conducted within the framework of the KNMF Laboratory for Synchrotron Radiation (in combination with other KNMF facilities), we report on a study of a class of complex materials used as hard coating materials. This class is based on transition-metal carbides and nitrides and is used, e.g., as protective layers for cutting tools. For the design of new coatings, controlling the phase and texture formation is essential. In the case of multi-element materials, this is not trivial and influences strongly the mechanical properties of the coating. With measurements at the PDIFF and XAS beamlines, combined with XPS measurements, we were able to identify the composition-dependent phases of V-Al-C-N [Krause et al., J. Appl. Cryst. (2013), in print]. The structure formation of V-C was furthermore monitored in-situ by XRD [Fig. 1; Krause et al., J. Synchr. Rad. 19 (2012) 216]. In combination with AFM, TEM, and nano-indentation measurements, these results will help to understand the interplay between structure formation and coating properties of complex hard coating materials.

KnMF Laboratory for Synchrotron Radiation IR1, PDIFF, and XAS Beamlines

............................................

Figure 1: Experimental setup for in-situ sputter deposition. Figure 2: In-situ X-ray reflectivity measurements of VC as a function of deposition rate F. The power applied to the sputter target was varied periodically, resulting in a periodic change of the deposition rate.

Figure 3: TEM cross section Figure 4: C 1s XPS spectrum of a polycrystalline VC1-x film on a single-crystalline Si substrate with an amorphous SiOx interlayer.

............................................User Service

ANKA’s beamlines provide dedicated user service for the Nanoscience and Microtechnology user communities.

In 2012, three additional ANKA beamlines became accessible via the KNMF proposal portal: IR1 , PDIFF, XAS

Authors: T. Baumbach, S. Doyle, B. Gasharova, M. Hagelstein, J. Heinrich, C. Heske, B. Krause, S. Mangold, Y.-L. Mathis, D. Moss, and A.-S. Müller,

KIT - ANKA, Synchrotron Radiation Facility, Karlsruhe, Germany

Scattering


FLUO | INE | IR1 | IR2 | SUL-X | UV-CD12 | WERA | XAS | MPI | NANO | PDIFF | SCD | IMAGE | tOPO-tOMO | LIGA I, II, III

Jürgen Mohr: [email protected]

COntACt

............................................ Chemistry Lab

Femtolab

Laser Lab

UHV-Analysis Lab

Lab Report

Lab Report


The Laboratory is situated in the hall with direct access to the beamlines and has a diverse range of equipment from low and high temperature cupboards and other ancillary equipment, for example a coolable centrifuge (Figures 2 and 3). Experiments which involve complicated setups and/or preparations are possible but need to be clarified beforehand with the responsible people (Beamline Scientist, Contact Person of the Chemistry Laboratory) in order to check and facilitate usage. Safety is also another important aspect that has to be checked in advance with the responsible people.

In line with the changes concerning Safety at KIT and the updated register for chemical substances (ChemA) the registers section for the Institute has been split into different groups representing the various Laboratories and infrastructure of ANKA and IPS. The Chemistry Laboratory now has a separate computer specifically for access to ChemA and other additional Safety documentation available on the Internet such as the Material Safety Data Sheets from the company sites and other sources. To ease storage requirements and use, provide a temporary storage for some chemicals needed during experiments, two special (movable) safety cabinets (Figure 1) have been bought and located at strategic points in the ANKA Hall. The safety cupboards equipped with extraction filters are principally for extra storage of solvents although other chemicals may be stored (but only on request and following clarification) and will be available in late Sommer 2013.

Updated forms and regulations along with a pdf copy of the the Laboratory instruction which will be part of the new “safety instruction video” (available end of 2013) are available under the “User download” area on www.anka.kit.edu.

Chemistry Lab

David Batchelor: [email protected] Lab: +49 (0)721 608 26285

COntACt

............................................Support

The ANKA Chemistry Laboratory (2.1.3) is part of the user support infrastructure available to Scientists when they come to ANKA for their beamtime or experiments.

Questions as to its use should be sent beforehand to the beamline scientist and the Chemistry Laboratory (2.1.3) personnel to optimize and prepare for the planned and other connected experiments!

Chemistry Lab 2.1.3 | Femtolab | Laser Lab | UHV Lab


COntACt

Figure 1: Movable chemical storage (solvent) Safety cupboards

Figure 2: Preparation for an experiment in full swing

Figure 3: A relatively uncluttered Fume cupboard (lit).


The south-west extension of the ANKA hall hosts the Femtolab with the offline operation of the laser. The laser itself (500 MHz oscillator by Gigaoptics, pulse length 30 fs) is located on a mobile optical table, which also carries essential control electronics and can optionally be used under inert atmosphere (helium, nitrogen). Recently a nanosecond laser has been provided for high-power laser ablation on solid targets.

One central experiment is the application of pump-probe diffraction. The ultrashort femtosecond laser pulses excite a crystalline sample reversibly. The X-ray pulses are used to probe the lattice dynamics as well as thermal kinetics of the samples. The questions under investigation are phonon dynamics in thin-film systems and nanostructured materials, as well as rapid thermal kinetics of functional materials. When using this pump-probe method within the low-alpha mode of ANKA, taking advantage of the short X-ray pulses emitted during this mode of operation, one can improve the time resolution of this kind of investigations down to some few picoseconds [1].

A recent application in collaboration with groups from Münster, Klewe and Aarhus has been the study of dynamics and heat transfer kinetics in multilayer stacks made out of alternating isotopically pure semiconductor layers [2,3]. These can be isotopes of silicon or germanium. Such structures serve to tailor the thermoelectric properties of thin films by modifying thermal transport, but not the electrical one. We are addressing the questions of heat diffusion as well as coherent modifications of the phonon band structure in these materials.

Besides, nanostructured materials are studied, such as nanoparticle suspensions, nanoparticle [4] or nano-antenna layers (see figure 1) [5], which possess intriguing properties in the interaction with light. The near-field enhancement, which can create extremely high electrical field strength (1010 V/m) at tips of adequately-dimensioned triangles, is one challenging effect. It allows to structure surfaces down to a 20 nm length scale with visible-light radiation [6].

High-power laser ablation is a tool for producing defined nanoparticles of a wealth of different material classes. Despite its simplicity to use (just irradiate a solid target immersed in the selected liquid for suspension) the mechanisms behind nanoparticle creation and size definition are far from being understood. Together with a group from Essen-Duisburg we are running a research programme to resolve the main steps of this complex dynamic process by applying methods with high time resolution, such as visible-light imaging SAXS, or X-ray imaging. Pump-probe scattering with high-throughput ablation targets has already revealed several steps in the

Femtolab

Anton Plech: [email protected] Lab: +49 (0)721 608 28665

COntACt

Figure 1: Scanning electron micrograph of an array of gold nano-antennae (triangles) on a surface. Plasmonic near-field enhancement can be strong at the tips of the structures.

nanoparticle formation and agglomeration [7,8]. A view of the ablation chamber with target renewal and continuous water flushing is shown in figure 2.

References:[1] D. Issenmann, S. Ibrahimkutty, R. Steininger, J. Göttlicher, T. Baumbach, N. Hiller, A-S. Müller and A. Plech: Ultrafast laser pump x-ray probe experiments by means of asynchronous sampling, J. Phys.:Conf. Ser. 425 (2013) 092007

[2] H. Bracht, N. Wehmeier, S. Eon, A. Plech, D. Issenmann, J. Lundsgaard Hansen, A. Nylandsted Larsen, J.W. Ager III, E.E. Haller, Reduced thermal conductivity of isotopically modulated silicon multilayer structures, Appl. Phys. Lett. 101 (2012) 064103

[3] D. Issenmann, S. Eon, N. Wehmeier, H. Bracht, Gernot Buth, S. Ibrahimkutty, Anton Plech, Determination of nanoscale heat conductivity by time-resolved x-ray scattering, Thin Solid Films (2012) DOI: 10.1016/j.tsf.2012.10.132.

[4] V. Kotaidis, T. Dekorsy, S. Ibrahimkutty, D. Issenmann, D. Khakulin, A. Plech: Vibrational symmetry breaking of supported nanospheres, Phys. Rev. B Rapids 86 (2012) 100101

[5] A. Kolloch, T. Geldhauser, K. Ueno, H. Misawa, J. Boneberg, A. Plech, P. Leiderer: Femtosecond and Picosecond Near Field Ablation of Gold Nanotriangles: Nanostructuring and Nanomelting, Appl. Phys. A 104 (2011) 793-799

[6] A. Kolloch, P. Leiderer, S. Ibrahimkutty, D. Issenmann, A. Plech: Structural study of near-field ablation close to plasmon-resonant nanotriangles, J. Laser Appl., 24 (2012) 042015

[7] S. Ibrahimkutty, P. Wagener, A. Menzel, A. Plech, S. Barcikowski: Nanoparticle formation in a cavitation bubble after pulsed laser ablation in liquid studied with high time resolution SAXS, Appl Phys. Lett, 101 (2012) 103104

[8] P. Wagener, S. Ibrahimkutty, A. Menzel, A. Plech, and S. Barcikowski: Dynamics of silver nanoparticle formation and agglomeration inside the cavitation bubble after pulsed laser ablation in liquid, Phys. Chem. Chem. Phys., 15 (2013) 3068-74

Figure 2: View of the ablation chamber with the optical port for the focussing of the laser on the front left side and a continuous rotation of the target disk inside the seald chamber (black stepper motor coupled to the magnetic transducer). Water flow is used to replace the liquid between individual laser shots.



COntACt

Information

The activities of the Femtolab consist in the provision of laser-based methods to process materials, in particular on the nanoscale. As a major part a femtosecond laser system is operated to be used for pump-probe experiments with radiation from ANKA as probe radiation.

............................................


Introduction Lasers are one of the most influential inventions of the twentieth century because of their extraordinary characteristics of high brightness, high directionality, high coherence, high monochromaticity, and unique spatial and temporal distributions. Material processing by laser beams has been well established as an advanced manufacturing technology. A high-power laser beam can be focused to a power density up to 10-12 W/cm2. These unique features provide excellent manufacturing capabilities with high accuracy, high quality, high efficiency, non-contact processing, high controllability, and ease of automation. Laser material processing covers a large variety of processing technologies and research areas, including laser matter interaction, laser surface modification (laser transformation hardening, laser remelting, laser alloying, laser cladding, laser shock peening, laser cleaning, laser texturing, and laser glazing), laser welding, laser cutting and drilling, laser forming and manufacturing, and industrial applications. One of the process in which we are interested is the laser cladding which is a process whereby a new layer of material is deposited on a substrate by laser fusion of blown powders or pre-placed powder coatings. Multiple layers can be deposited to form shapes with complex geometry. The use of in-situ synchrotron X-ray diffraction during cladding process enables us to follow the evolution of the microstructure and phases as function of the cladding parameters like laser power density, beam spot size, traverse speed, power flow rate and laser beam absorption. Cladding materials are had facing allows powders (Co-based, Ni-based and Fe-based plus various carbides, those of the substrates are cast iron, mild steel, alloyed steel, non-ferrous metals and son) the working principle of the laser surface treatments which involves the absorption and then heat conduction is schematically presented in figure 1.

Experimental setup at ANKA

the laser system (for in-situ and ex-situ experiments): At the Nano beamline we have a Fiber-coupled Diode Laser LDF 600-6000 VG 4L, that consists of a diode laser head (water cooled), integrated in the laser power unit. The laser signal can travel through an optical fiber cable of 600 µm diameter and 5 m length. A second fiber cable of 600 µm diameter and 20 m lenght goes to the Nano1 experimental hutch for in-situ synchrotron radiation experiments at the diffractometer. The laser unit can work in the 900-1030 nm wavelenghts range. It has a power stability of <+-2% at a cooling water temperature of ΔT<1 °C, the beam has 66 mm mrad diversion and a maximun power of 6KW. Additionally, we have a visible 600-700 nm laser pilot to align and visualize the laser spot position.

Laser Lab Laser Laboratory Surface treatments

Sondes Bauer: [email protected] Lab: +49 (0)721 608 28012

COntACt

Laser processing chamber with temperature control

At the laboratory, we have a chamber to perform laser processing in vacuum or in controlled atmosphere (Ar, N2,He, etc.). This chamber is well suited for in situ experiments and it could be combined with the diffractometer at the experimental station NANO 1. The sample positioning and scanning could be carried out using motorised goniometer for stress analysis investigation and a X-Y-translation stage to scan the laser beam onto the sample during the cladding process. The laser process is controlled by two color pyrometer.

Figure 1: Laser Treatments process

Fig. 2: The Laser Laboratory Installation: The main components of the laser treatment experiments

Fig. 3,4: The chamber for the controlled atmosphere laser treatment experiments

Thermal elements connections and feedtrough from motor Turbo pump flange

Laser input windows Kapton windows for synchrotron Experiments

Laser Head optic

We can control all the laser process by a remote station

The main laser power unity

Optical fiber cable, It comes from the Laser power unity to the laser optic head

The laser optic head

Optic table


Pyrometer


COntACt


X-ray scattering of synchrotron radiation from nanoscale objects during their formation, i.e., in-situ, is a valuable tool for detailed studies of structure formation processes. However, the fundamental understanding of these processes often requires a combined approach using complementary characterization methods.The ANKA UHV (ultra-high vacuum) Analysis lab is a facility for in-situ growth studies combining a modular and extendable UHV cluster system for complementary surface analytics with several UHV growth chambers for in-situ X-ray experiments during thin film and nanostructure formation. Being situated in close proximity to the ANKA beamlines and to a dedicated chemistry lab for sample preparation, the UHV Analysis lab allows for studying various nanosystems, optimizing the use of the beamlines, and ensures a fast feedback between complementary measurements and X-ray experiments. The access to the lab is on a collaborative basis, flexible and independent of the scheduled synchrotron radiation experiments, thus providing sufficient time for optimization of growth parameters and detailed sample characterization before and after the in-situ X-ray studies

at ANKA beamlines.The UHV cluster (see Figure 1) is a large ultra-high vacuum transfer system offering several docking stations for portable and stationary growth chambers. Samples with a maximum size of 25 mm can be inserted directly via three loadlocks. The central analysis and surface preparation chambers are accessible from all growth chambers. Here, samples can be prepared by Argon sputtering (limited to a surface area of 10x10 mm2) and annealing. They can be analyzed by standard surface characterization methods such as reflection high energy electron diffraction (RHEED), low-energy electron diffraction (LEED), Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), UHV atomic force microscopy (AFM), and UHV scanning tunneling microscopy (STM). The UHV cluster is extendable and is develops according to the demands of future experiments. Presently, several deposition chambers for molecular beam epitaxy and sputter deposition are connected to the UHV cluster. They will be described in the following.

UHV-Analysis Lab

Figure 1: UHV cluster comprising several deposition and surface analysis chambers.

The Portable Synchrotron Molecular Beam Epitaxy (PMBE) system (Figure 2) of the research group “III-V Semiconductors” of the Institute for Photon Science and Synchrotron Radiation (IPS) is designed for real-time in-situ X-ray investigations of dynamic processes during epitaxial growth and annealing of III-V semiconductor nanostructures.The PMBE has a weight of 100 to 140 kg, depending on configuration, and is compatible to heavy-load diffractometers available, e.g., at the NANO and MPI beamlines at ANKA. Two symmetric CF100 Beryllium windows with opening angles of 22 degrees each allow for GID and GISAXS measurements during the deposition process.The growth chamber with a base pressure of 2 x 10-11 mbar is equipped with a RHEED gun for surface monitoring. Up to 6 standard thermal effusion cells with a volume of 2 cm3 can be used simultaneously for deposition. The sample manipulator with sample heating up to 900°C and nitrogen cooling shroud fulfills standard growth requirements. Up to 4 samples can be stored in a sample storage chamber attached to the growth chamber. Additionally, a UHV transport case with a base pressure of 8 x 10-11 mbar is available.The performance of the PMBE system was demonstrated during in-situ

Grazing Incidence Diffraction, Grazing Incidence Small Angle Scattering and High Resolution X-ray Diffraction experiments at the ESRF [1].The deposition process in the chamber was characterized and optimized for Gallium-assisted growth of Gallium-Arsenide nanowires on Silicon.The first in-situ X-ray experiments at the NANO beamline of ANKA were conducted in autumn 2012.

[1] T. Slobodskyy et al., Rev. Sci. Instrum. 83, 105112 (2012), DOI:10.1063/1.4759495

Portable synchrotron MBE chamber for III-V semiconductor nanostructuresContact PMBE: Philipp Schroth, Dongzhi Hu

Figure 3: The PMBE chamber docked to the UHV cluster.

Bärbel Krause: [email protected] Lab:+49 (0)721 608 28016 / 28017

COntACt

Overview



Figure 2: The PMBE chamber at the NANO beamline


The modular growth chamber for in-situ synchrotron radiation experiments during sputter deposition of thin films (see Figure 4) is operated by the Research Group “Sputtering” of the Institute for Photon Science and Synchrotron Radiation. The chamber is optimized for growth studies during RF and DC sputtering with target diameters between 1 and 3 inch, reactive sputtering, and codeposition. The portable chamber has a base pressure of 1 x 10-8 mbar. Samples can be heated up to 700°C, and a bias can be applied. Depending on the configuration, the sample stage can be rotated around the surface normal, or tilted relative to the deposition sources. Up to 5 samples can be stored within the chamber. Alternatively, samples can be introduced via a loadlock.Two beryllium windows with a horizontal opening angle of 100 degrees and a vertical opening angle of 50 degrees give access to the wide angular

range required for detailed texture studies. Various types of measurements including X-ray diffraction, X-ray reflectivity, and EXAFS measurements, can be performed during thin film deposition and annealing. A Langmuir probe for plasma diagnostics is available. A detailed description of the chamber can be found in Ref. [2]. Figure 5 shows schematically the experimental setup for in situ reflectivity measurements during sputter deposition of the hard coating material Vanadium Carbide. The experiments were performed at the MPI beamline. Both the reflected beam and the diffuse scattering were measured simultaneously, giving real-time information about the density, roughness and film thickness changes during deposition.

[2] Krause et al., J. Synchrotron Rad. 19 (2012) 216-222

UHV-Analysis lab

The Helmholtz-University Young Investigators Group “Nanodynamics” at IPS investigates the interplay between the structure, morphology, magnetism and lattice dynamics in rare earth based epitaxial nanostructures. The group operates the rare earth MBE growth chamber and the Magneto Optic Kerr Effect (MOKE) chamber, figure 6, that are permanently connected to the UHV cluster allowing for sample characterization by all available techniques in the UHV Analysis lab. The films and nanostructures are grown by evaporating the lanthanide metals from a four pocket e-beam evaporator and two high temperature effusion cells. A very high temperature (up to 2300°C) effusion cell is used for the evaporation of rare-earth oxides (high-k materials). The structure of the grown films is monitored in-situ by

RHEED. The magnetic properties of the rare-earth based nanostructures are investigated by a very low temperature (16 K - 290 K) MOKE set-up. A UHV chamber (figure 7) dedicated to temperature-dependent in-situ GISAX and XAS experiments at various beamlines of ANKA has been recently commissioned (June 2013). This chamber is equipped with Be windows and a manipulator that allows for sample heating up to 1100 K, cooling down to 100 K and sample rotation around the surface normal to ±180 degrees. The transportable UHV X-ray chamber can be docked to the UHV cluster for loading up to 5 samples and transferring them to the corresponding beamline for in-situ X-ray scattering or spectroscopy experiments.

Rare-earth growth chamber Contact REMBE: Svetoslav StankovSputtering chamber for in-situ X-ray studies

Contact sputtering chamber: Bärbel Krause

Figure 6: The UHV chamber for sample growth by molecular beam epitaxy and in- situ structure characterization by RHEED. Magnetic properties are studied by a low temperature MOKE setup.

Figure 7: The transportable UHV chamber for in-situ X-ray scattering and spec-troscopy experiments at ANKA beamlines. The base pressure of the chamber is 3x10-11 mbar. Up to 5 samples can be transported and investigated.

Figure 4: Portable sputter deposition chamber mounted on the heavy-load diffractometer at the MPI beamline.


User Operation Accelerator Report Beamline Report Lab Report Applications Appendix Bärbel Krause: [email protected]

Lab:+49 (0)721 608 28016 / 28017

COntACt

Figure 5: In situ X-ray reflectivity experiment during sputter deposition.

Applications

Instrumentation

Method development

Applications

Applications



IntroductionAnKA’s Imaging group is developing instrumentation and components, methods and techniques for X-ray imaging. In its main competence, the group is developing full-field methods for projection imaging, microscopy and 3D tomographic imaging based on absorption, phase and Bragg/Laue diffraction contrast.Synchrotron imaging methods with spatial resolution in the micrometer and nanometer range are increasingly relevant for material research and diagnostics in engineering sciences, micro system- and nanotechnologies, for structural imaging in nanobiology and life sciences, for non-destructive testing of components and devices, for paleontology, cultural heritage and other fields. These methods allow closing the gap between conventional 2D and 3D imaging performed with techniques based on X-ray table-top sources and electron microscopy methods, i.e. the gap in spatial resolution between about 10 micrometers and several ten nanometers. X-ray imaging techniques are largely non-destructive and allow using and combining various contrast mechanisms (absorption, X-ray fluorescence, Fresnel and Bragg diffraction, dichroism, etc.) to image geometrical, chemical and crystallographic structures of samples. In the following paragraphs, an overview over the progress in instrumentation and implementation, method development and application achieved during the past year will be given.

Instrumentation:

LaminographySynchrotron radiation computed laminography (SRCL) was developed for 3D imaging of regions of interest in flat, laterally extended objects. A set-up has been installed and tested at the TOPO-TOMO beamline and enables the use of multiple contrast modalities via absorption, propagation-based phase contrast and grating interferometry. The basic principle of synchrotron radiation computed laminography (SRCL) is shown in Figure 1. In order to realize the SRCL geometry, an accurate inclination of the sample rotary stage with respect to the X-ray beam has to be performed. To guarantee a large freedom of the laminographic angle θ, two designs have been proposed. Design I (Figure 1a) is a novel design which utilizes a horizontal rotation by using an additional rotary stage to enable a full circular tilting of the sample stage. The Design II (Figure 1b) realizes the tilting of the sample stage by simply using a goniometer stage in combination with a fixed-angle wedge [1]. Both designs have advantages and drawbacks. Comparing the degrees of freedom (DOF) for both designs, the novel Design I has a flexible inclination angle range from -180° to +180° , which allows to perform

1a) 1b) 3-D drawings of the different designs for the SRCL sample manipulator.

1c) 1d) Experimental setup corresponding to Designs I (a) and II (b), respectively. Both are available at the TOPO-TOMO beamline.

radiography (at θ = 0°) if there is an aperture through the sample rotary stage. The Design II only allows an accessible inclination angle range of 0° to +32° (i.e. limited by the travel range of the goniometer). Since both designs can complement each other and fit to different requirements or conditions, both have been implemented at the TOPO-TOMO beamline. Figures 1c and 1d show experimental implementations that correspond to Design I (a) and Design II (b), respectively. The comparison of their degrees of freedom is summarised in Table 5.1.

Similar to CT, SRCL can be combined with diverse contrast modes, including inline phase-contrast and Talbot interferometry in addition to the traditional absorption contrast. The combination of different scintillator crystals and microscope optics yields a large flexibility in spatial resolution values (pixel sizes from 0.36 to 6.1 µm). Especially, the combination of grating interferometer (GI) and SRCL (Figure 1(d)) has been implemented at TOMO-TOMO [2] in order to provide simultaneously absorption, differential phase and dark-field contrast modulus on naturally flat specimens [3], i.e. biological tissues, fossils or polymers. Multi-contrast SRCL has been installed at TOPO-TOMO and is available to cooperation projects. It opens opportunities for applications in the life and material sciences. In the near future, laminography combined with a tensile rig will allow us to conduct in-situ loading experiments on engineering materials, including aluminum sheets or industrial polymer plates.

Table 1: Comparision of the degree of freedoms (DOF) of both designs.

Design I Design IIsample size up to 30 × 30 mm2 (relatively

small samples)up to 150 × 150 mm2 (relatively large flat samples)

inclined angle -180°… +180° 0° … +32°

sample SX/SY manipulation manual/motorized goniometer headfor absorption contrast, closer sample-detector distance

Pusher system

load capacity up to 100 g up to 500 g

Visualization machines X-ray imaging techniques – and microtomography in particular – produce a huge amount of data that needs to be visualized for image analysis. An appropriate infrastructure of high performance computer systems equipped with high-end graphics software is therefore mandatory (see table 5.2 for a list of visualization machines). In addition to the already existing visualization machines anka-vis1

(Linux server) and anka-vis2 (Windows workstation), we recently installed two identical workstations (anka-vis3 & anka-vis4) especially designed for visualizing large multidimensional datasets. Both systems are equipped with various software packages, including Amira 5.3 for volume stack visualization and segmentation and CINEMA 4D R14 for post-processing of polygon meshes of segmented data.

machine system specifications

anka-vis1 CPU: 2x Intel Xeon [email protected] GHz

GPU: NVIDIA Quadro FX 5800 4GB

memory: 144 GB

operating system: Red Hat Enterprise Linux Server release 5.5 x64

software packages: Avizo 6, VG Studio Max 2.0, etc.

anka-vis2 CPU: Intel Core-i7 [email protected] GHz

GPU: NVIDIA GeForce GTX 580 4 GB

memory: 16 GB

operating system: Windows 7 x64

software packages: Amira 5.4.5, CINEMA 4D R14, Deep Exploration 6, Octopus, etc.

anka-vis3 CPU: Intel Core [email protected] GHz

and GPU: NVIDIA GeForce GTX 680 4 GB

anka-vis4 memory: 64 GB

operating system: Windows 7 x64

software packages: Amira 5.4.5, CINEMA 4D R14, Octopus, etc.

Table 2: List of visualization machines currently available at ANKA

Authors: Yin Chen, KIT - Institute for Photon Science and Synchrotron Radiation Technology, Karlsruhe, Germany Lukas Helfen, ESRF - European Synchrotron Radiation Facility, Grenoble, France / KIT - Institute for Synchrotron Radiation, Karlsruhe, Germany

Author: Thomas van de Kamp, KIT, Institute for Photon Science and Synchrotron Radiation, Karlsruhe, Germany

Instrumentation | Method development | Applications

Imaging Group Leader: Tilo Baumbach: [email protected] Group Coordinator: Ruth Heine: [email protected]

COntACt

Figure 1: Principle of CL at synchrotron beamlines with parallel-beam geometry.

1a) 1b)

1c) 1d)



IT control system ConcertThe ratio between the effective data acquisition time and hardware orchestration becomes smaller by high-speed experiments. As a consequence, control system inefficiencies in hardware handling become more pronounced. In order to deal with the inefficiencies, together with the Data Processing Group at the Institute for Data Processing and Electronics we developed a control system named Concert. The main goals are to provide standard device access, a parallel execution scheme and process abstraction.

Concert provides an application programming interface (API) for hardware used by high-speed experiments, which decouples its access details from functionality. This allows us to program hardware-dependent tasks without the knowledge of the device implementation details. So far, we implemented parameter scans, focusing and tomographic sample alignment.

All device access and tasks within Concert are performed in parallel, which can save a significant amount of time during the experiment. To be able to

guarantee an execution order for tasks and device accesses which need to collaborate, we provide a synchronization mechanism.

In order to save experiment startup time and hide the hardware details from the beamline user, we provide sessions. They are pre-programmed modules with hardware and task definitions, which are loaded on-demand. This way the user needs to know only the symbolic device and task names without the real hardware needed by the experiment and has everything at hand after loading one session module.

Concert is connected with a high-performance computing framework in order to evaluate the data in conducted tasks faster. It is possible to use with other control systems and extend for new device types, which makes it suitable not only for high-speed experiments, but for all synchrotron radiation experiments in general.

TheoryThe activites of the theory group have been focusing on research with respect to the conditions for successful in vivo 4D phase-contrast microtomography (PCµT) of early developmental stages of the African clawed frog Xenopus laevis, such as heat load, exposure per projection, propagation distance, X-ray energy, degree of coherence, applicable pixel sizes, and sample fixation. Experiments to demonstrate the feasibility of phase-contrast and dose studies were performed at ANKA and actual live-cell experiments were carried out at APS. In close discussions with biological experts at University of Heidelberg, Virginia Tech, Northwestern University, University of Toronto and KIT on Xenopus gastrulation, image analysis including segmentation of major cavities, cell tracking, and global as well as local flow-field analysis was performed for a sequence of 12 volumes capturing a good part of early gastrulation. The thus gained facts were put into hypotheses on the directionality of fluid exchange during archenteron inflation, the role of cells lining the archenteron, a transient ridge of ectoderm in the confrontation zone between head and ventral mesendoderm, and the loci of propulsion centers for collective and single cell motion [4,5]. Furthermore, life-cell PCµT was applied to neurulation with ongoing data processing. The results were presented at major international conferences and seminars (SRI2012, XTOP 2012, Gordon Conference on Cranial Placodes 2013, Biology and Synchrotron Radiation 2013, two APS seminars). We entertain vivid collaborations with mathematicians at CWI Amsterdam and with IPE-KIT to optimize algebraic reconstruction techniques, saving dose at the same resolution by using less projections in future in vivo applications of PCµT, and we investigate delay effects in dose expression both empirically and theoretically. This research is supported by BMBF, the US DOE under Contract No. DE-AC02-06CH11357, grants 05K12CK2 and 05K12VH1, and COST action MP1207 “Enhanced X-ray Tomographic Reconstruction: Experiment,

Modeling, and Algorithms”. Several third-party funding proposals are being worked out to research and set up a routine PCµT facility at ANKA’s new IMAGE beamline.

Presently, a duality extension of a previously published quasiparticle approach to high-resolution, single-distance phase retrieval [6,7] for strong phase objects to include absorption is being worked out, based on the discovery of a new approximate symmetry of Fresnel theory, with very promising intermediary results.

Figure 2: In vivo Xenopus laevis development around stage 12

Three-dimensional visualization of structural and elemental composition of bacterial biofilms Bacterial biofilms are well-known for their robustness against antimicrobial agents which manifests itself particularly in health care where contamination of medical implants and wounds poses a severe threat to human health. But also industrial equipments like ventilation and oil wells suffer from biofilm formation. Thus it is important to understand which mechanisms allow these complex structures to be robust to such an extent. We applied a correlative approach of hard X-ray phase contrast tomography (holotomography) as an outstanding method for visualizing 3D cellular architectures of thick and non-transparent biological samples combined with synchrotron-based scanning hard X-ray fluorescence microscopy (SXFM) as an excellent non-invasive way to investigate the elemental distribution within bulk samples to investigate the structural organization and elemental content of bacterial biofilms [8].

In cooperation with groups from the Institute of Functional Interfaces, the Institute for Biological Interfaces and scientists from the European Synchrotron Radiation Facility (ESRF), France, experiments were performed at the hard X-ray fluorescence (XRF) and holotomography nano-probe on the nano-imaging end station of beamline ID22 at ESRF. As can be seen in the volume rendering in Figure 3(e), two layers of bacteria that formed on each side of the sample support were reconstructed, and two different development states can be distinguished. It was possible to clearly resolve not only the bacteria on one side which are still in initial attachment (red arrow), but also bacteria in the state of irreversible attachment of on the other side of the membrane (blue arrow) with bacterial cells cemented to the substrate and forming nascent cell clusters. Furthermore, when combined with the fluorescence images, the elemental composition of bacterial cells and the clusters can be determined without ambiguity (compare Figure 3(d)). Phosphate is an indispensable component of many macromolecules, like proteins, nucleic acids, and lipids, so it is present within all cells as can be seen in Figure 3(c) and 3 (d). The map of the Fe content (Figure 3 (b) and 3 (d)) shows a different distribution with higher concentrations along the outlines of the cells indicating that Fe is richer along the cell membranes. One explanation for this distribution comes from the strong Fe binding agents called siderophores. They are suspected to be secreted by the bacteria to tightly bind Fe from the exterior of the cells and transport it into the cells as Fe is an essential trace nutrient for microbial life processes. This detailed analysis of the data, which is only possible due to the correlative approach, makes it obvious that three dimensional visualization of the bacterial biofilm is essential for the comprehensive understanding of the two dimensional fluorescence images.

Figure 3:(a): One cross section of the reconstructed tomogram showing single bacteria. (b)-(c): X-ray fluorescence images of the bacterial biofilm, with contrast adjusted independently (b: Fe, c: P). Scanned area 10 × 10 µm2. (Scanning pitch: 100 nm/pixel, dwell time: 0.2 s/pixel, FWHM of beam: 100 nm). (d): Overlapped image of elemental composition and reconstructed cross section (red: Fe, green: P, gray: cross section (a)). (e): Corresponding volume rendering of the same area. Scale bar is 5 µm (does not apply to the volume rendering).

References

[1] L. Helfen, A. Myagotin, P. Mikulik, P. Pernot, A. Voropaev, M. Elyyan,M. Di Michiel, J. Baruchel and T. Baumbach, On the implementation of computed laminography using synchrotron radiation, Rev. Sci. Instrum., 82 063702 (2011)[2] Y. Cheng, V. Altapova, L. Helfen, F. Xu, T. dos Santos Rolo, P. Vagovič, M. Fiederle and T. Baumbach, Multi-contrast computed laminography at ANKA light source, Journal of Physics (2012)[3] V. Altapova, L. Helfen, J. Butzer, J. Moosmann, D. Haenschke, S. Monninger, E. Frey, and T. Baumbach, Grating-based multiple contrast laminography of biological specimens, Physics in Medicine and Biology (2013)[4] J. Moosmann, A. Ershov, V. Altapova, T. Baumbach, M. S. Prasad, C. LaBonne, X. Xiao, J. Kashef, and R. Hofmann, X-ray phase-contrast in vivo mictotomography probes new aspects of Xenopus gastrulation, Nature 374–377 (2013)[5] Highlighted Research: Tal Nawy, Embryos under the X-ray, Nature Methods 10, 603 (2013)[6] J. Moosmann, R. Hofmann and T. Baumbach, Criticality in single-distance phase retrieval, Optics Express 19, 12066-12073 (2011)[7] R. Hofmann, J. Moosmann and T. Baumbach, Criticality in single-distance phase retrieval, Optics Express 19, 25881-25890 (2011)[8] Y. Yang, R. Heine, F. Xu, H. Suhonen, L. Helfen, A. Rosenhahn, T. Gorniak, S. Kirchen, T. Schwartz, T. Baumbach. “Three-dimensional visualization of structural and elemental composition of bacterial biofilms”, Journal of Physics (2012)

Authors: Ralf Hofmann and Julian Moosmann, KIT - Institute for Photon Science and Synchrotron Radiation, Karlsruhe, Germany

structure dynamics

Method development:

Instrumentation | Method development | Applications

Applications:

Imaging Group Leader: Tilo Baumbach: [email protected] Group Coordinator: Ruth Heine: [email protected]

COntACt

Author: Tomas Farago, KIT - Institute for Photon Science and Synchrotron Radiation, Karlsruhe, Germany

Authors: Ruth Heine and Yang Yang, KIT - Institute for Photon Science and Synchrotron Radiation, Karlsruhe, Germany

Appendix

ANKA Publications 2012

AnKA Seminars 2012

AnKA & KnMF Users‘ Meeting 2012

Appendix


1. A. M. Ako, M. S. Alam, M. Rahman, J. P. Hill, N. M. Sanchez-Ballester, K. Ariga, G. Buth, C. E. Anson, A. K. Powell, “Self-Assembly of a Mononuclear [FeIII(L)(EtOH)2] Complex Bearing an n-Dodecyl Chain on Solid Highly Oriented Pyrolytic Graphite Surfaces”, Chemistry - A European Journal 18 (2012) 16419-16425

2. V. Altapova, A. Ershov, T. dos Santos Rolo, E. Reznikova, J. Mohr, Y. L. Pivovarov, V.F. Pichugin, T. Baumbach, “Imaging Methods and Their Application at ANKA Light Source”, Journal of Surface Investigation. X-Ray, Synchrotron and Neutron Techniques 5 (2012) 394-397

3. V. Altapova, L. Helfen, A. Myagotin, D. Hänschke, J. Moosmann, J. Gunneweg, T. Baumbach, “Phase contrast laminography based on Talbot interferometry”, Optics Express 20 (2012) 6496-6508

4. U. Aygül, D. Batchelor, U. Dettinger, S. Yilmaz, S. Allard, U. Scherf, H. Peisert, T. Chassé, “Molecular Orientation in Polymer Films for Organic Solar Cells Studied by NEXAFS”, Journal of Physical Chemistry C 116 (2012) 4870-4874

5. M. Bär, S. Pookpanratana, L. Weinhardt, R.G. Wilks, B. Schubert, B. Marsen, T. Unold, M. Blum, S. Krause, Y. Zhang, A. Ranasinghe, K. Ramanathan, I. Repins, M.A. Conteras, S. Nishiwaki, X. Liu, N.R. Paudel, O. Fuchs, T.P. Niesen, W. Yang, F. Karg, A.D. Compaan, W.N. Shafarman, R. Noufi, H.-W. Schock, C. Heske, “Soft x-rays shedding light on thin-film solar cell surfaces and interfaces”, Journal of Electron Spectroscopy and Related Phenomena (2012) 064911-1-9

6. W. Bensch, J. Ophey, H. Hain, H. Gesswein, D. Chen, R. Mönig, P. A. Gruber, S. Indris, “Chemical and electrochemical insertion of Li into the spinel structure of CuCr2Se4: ex situ and in situ observations by X-ray diffraction and scanning electron microscopy”, Physical Chemistry Chemical Physics 14 (2012) 7509-7516

7. P. J. Bereciartua, F. J. Zuniga, J. M. Perez-Mato, V. Petricek, E. Vila, A. Castro, J. Rodriguez-Carvajal, S. Doyle, “Structure refinement and superspace description of the system Bi2(n+2)MonO6(n + 1) (n = 3, 4, 5 and 6) “, Acta Crystallographica Section B - Structural Science 68 (2012) 323-340

8. L. Bertrand, M. Cotte, M. Stampanoni, M. Thoury, F. Marone, S. Schöder, “Development and trends in synchrotron studies of ancient and historical materials”, Physics Reports - Review Section of Physics Letters 519 (2012) 51-96

9. L. Bertrand, L. Robinet, M. Thoury, K. Janssens, S. X. Cohen, S. Schöder, “Cultural heritage and archaeology materials studied by synchrotron spectroscopy and imaging”, Applied Physics A: Materials Science & Processing 106 (2012) 377-396

10. M. Blum, M. Odelius, L. Weinhardt, S. Pookpanratana, M. Bär, Y. Zhang, O. Fuchs, W. Yang, E. Umbach, C. Heske, “Ultra-fast proton dynamics in aqueous amino acid solutions studied by resonant inelastic soft x-ray scattering”, Journal of Physical Chemistry B 116 (2012) 13757-13764

11. A. A. C. Bode, V. Vonk, F. J. van den Bruele, D. J. Kok, A. M. Kerkenaar, M. F. Mantilla, S. Jiang, J. A. M. Meijer, W. J. P. van Enckevort, E. Vlieg, “Anticaking Activity of Ferrocyanide on Sodium Chloride Explained by Charge Mismatch”, Crystal Growth & Design 12 (2012) 1919-1924

12. R. M. Bolanz, J. Majzlan, L. Jurkovic, J. Göttlicher, “Mineralogy,

geochemistry and arsenic speciation in coal combustion waste from Novaky, Slovakia”, Fuel 94 (2012) 125-136

13. A. Boubnov, S. Dahl, E. Johnson, A. P. Molina, S. B. Simonsen, F. M. Cano, S. Helveg, L. J. Lemus-Yegres, J.-D. Grunwaldt, “Structure-activity relationships of Pt/Al2O3 catalysts for CO and NO oxidation at diesel exhaust conditions”, Applied Catalysis B 126 (2012) 315-325

14. H. Bracht, N. Wehmeier, S. Eon, A. Plech, D. Issenmann, J.L. Hansen, A. N. Larsen, J. W. Ager III, E.E. Haller, “Reduced thermal conductivity of isotopically modulated silicon multilayer structures”, Applied Physics Letters 101 (2012) 064103-1-4

15. A. Bremer, C. M. Ruff, D. Girnt, U. Müllich, J. Rothe, P. W. Roesky, P. J. Panak, A. Karpov, T. J. J. Müller, M. A. Denecke, A. Geist, “2,6-Bis(5-(2,2-dimethylpropyl)-1H-pyrazol-3-yl)pyridine as a Ligand for Efficient Actinide(III)/Lanthanide(III) Separation”, Inorganic Chemistry 51 (2012) 5199-5207

16. M. Bruns, C. Barth, P. Brüner, S. Engin, T. Grehl, C. Howell, P. Koelsch, P. Mack, P. Nagel, V. Trouillet, D. Wedlich, R. G. White, “Structure and chemical composition of mixed benzylguanine- and methoxy-terminated self-assembled monolayers for immobilization of biomolecules”, Surface and Interface Analysis 44 (2012) 909-913

17. U. Carvajal-Nunez, D. Prieur, T. Vitova, J. Somers, “Charge Distribution and Local Structure of Americium-Bearing Thorium Oxide Solid Solutions”, Inorganic Chemistry 51 (2012) 11762-11768

18. S. Casalbuoni, M. Migliorati, A.Mostacci, L.Palumbo, B. Spataro, “Beam heat load due to geometrical and resistive wall impedance in COLDDIAG”, Journal of Instrumentation 7 (2012) P11008-1-20

19. A. Charnukha, J. Deisenhofer, D. Pröpper, M. Schmidt, Z. Wang, Y. Goncharov, A. N. Yaresko, V. Tsurkan, B. Keimer, A. Loidl, and A. V. Boris, “Optical conductivity of superconducting Rb2Fe4Se5 single crystals”, Physical Review B 85 (2012) 100504-1-5

20. N. V. Chukanov, D.A. Varlamov, F. Nestola, D. I. Belakovsky, J. Göttlicher, S. Britvin, A. Lanza, S. Jancev, “Piemonite - (Pb), CaPbAl2Mn3+[Si2O7][SiO4]O(OH), a new mineral species of the epidote supergroup”, Journal of Mineralogy and Geochemistry 189 (2012) 275-286

21. O. Clemens, M. Bauer, R. Haberkorn, M. Springborg, H. P. Beck, “Synthesis and Characterization of Vanadium-Doped LiMnPO4-Compounds: LiMn(PO4)x(VO4)1-x (0.8 <= x <= 1.0)”, Chemistry of Materials 24 (2012) 4717-4724

22. F. Conrad, M. Bauer, D. Sheptyakov, S. Weyeneth, D. Jaeger, K. Hametner, P.-E. Car, J. Patscheider, D. Günther, G. R. Patzke, “New spinel oxide catalysts for visible-light-driven water oxidation”, RSC Advances 2 (2012) 3076-3082

23. J. Czapla, W. M. Kwiatek, J. Lekki, R. Steininger, J. Göttlicher, “Determination of changes in sulphur oxidation states in prostate cancer cells”, Acta Physica Polonica A 121 (2012) 497-501

24. M. K. Dalai, P. Pal, B. R. Sekhar, M. Merz, P. Nagel, S. Schuppler, C. Martin, “Electronic structure of the electron-doped Ca0.86Pr0.14MnO3”, Physical Review B 85 (2012) 155128-1-5

25. A. Diener, R. Köppe, “Synthesis of selenium doted pyrite single crystals prepared by chemical vapor transport”, Journal of Crystal Growth 349 (2012) 55-60

26. A. Diener, T. Neumann, U. Kramar, D. Schild, “Structure of selenium

AnKA Publications 2012 incorporated in pyrite and mackinawite as determined by XAFS analyses”, Journal of Contaminant Hydrology 133 (2012) 30-39

27. M. Ding, B. Wang, Z. Wang, J. Zhang, O. Fuhr, D. Fenske, S. Gao, “Constructing Single-Chain Magnets by Supramolecular π-π Stacking and Spin Canting: A Case Study on Manganese(III) Corroles”, Chemistry - A European Journal 18 (2012) 915-924

28. P. A. Douissard, A. Cecilia, X. Rochet, X. Chapel, T. Martin T. van de Kamp, L. Helfen, T. Baumbach, L. Luquot, X. Xiao, J. Meinhardt, A. Rack, “A versatile indirect detector design for hard X-ray microimaging”, Journal of Instrumentation 7 (2012) P09016-1-26

29. S. H. Eitel, M. Bauer, D. Schweinfurth, N. Deibel, B. Sarkar, H. Kelm, H.-J. Krüger, W. Frey, R. Peters, “Paramagnetic Palladacycles with Pd-III Centers Are Highly Active Catalysts for Asymmetric Aza-Claisen Rearrangements”, Journal of the American Chemical Society 134 (2012) 4683-4693

30. C. Falquez, R. Hofmann, T. Baumbach, “Charge-Density Waves in Deconfining SU(2) Yang-Mills Thermodynamics”, Quantum Matter 1 (2012) 153-158

31. C. E. Farnsworth, A. Voegelin, J. G. Hering, “Manganese Oxidation Induced by Water Table Fluctuations in a Sand Column”, Environmental Science & Technology 46 (2012) 277-284

32. N. Finck, K. Dardenne, D. Bosbach, H. Geckeis, “Selenide Retention by Mackinawite”, Environmental Science & Technology 46 (2012) 10004-10011

33. M. Fischer, D. N. Thomas, A. Krell, G. Nehrke, J. Göttlicher, L. Norman, K. M. Meiners, C. Riaux-Gobin, G. S. Dieckmann, “Quantification of ikaite in Antarctic sea ice”, The Cryosphere Discussions 6 (2012) 505-530

34. X. Gaona, J. Tits, K. Dardenne, X. Liu, J. Rothe, M. A. Denecke, E. Wieland, M. Altmaier, “Spectroscopic investigations of Np(V/VI) redox speciation in hyperalkaline TMA-(OH, Cl) solutions”, Radiochimica Acta 100 (2012) 759-770

35. A. Grau, T. Baumbach, S. Casalbuoni, S. Gerstl, M. Hagelstein, T. Holubek, D. Saez de Jauregui, “Cryogen—Free Setup for Local and Integral Magnetic Field Measurements of Superconducting Undulator Coils”, Proceedings of ASC 2012, IEEE-Transactions on Applied Superconductivity 22 (2012) 9001504-1-4

36. C. A. Gorski, L. Klüpfel, A. Voegelin, M. Sander, T. B. Hofstetter, “Redox Properties of Structural Fe in Clay Minerals. 2. Electrochemical and Spectroscopic Characterization of Electron Transfer Irreversibility in Ferruginous Smectite, SWa-1”, Environmental Science & Technology 46 (2012) 9369-9377

37. D. T. Haluzan, D. M. Klymyshyn, S. Achenbach, M. Börner, J. Mohr, “VM-TEST: Mechanical property measurement using electrostatically actuated vertical MEMS test structures fabricated in thick metal layers”, Microsystem Technologies 18 (2012) 443-452

38. D. Hänschke, L. Helfen, V. Altapova, A. Danilewsky, B. Tanner, T. Baumbach, “Three-dimensional imaging of dislocations by X-ray diffraction laminography”, Applied Physics Letters 101 (2012) 244103-1-4

39. M. Helfrich, P. Schroth, D. Grigoriev, S. Lazarev, R. Felici, T. Slobodskyy, T. Baumbach, D. Schaadt, “Growth and characterization of site-selective quantum dots”, Physica Status Solidi A 209 (2012) 2387-2401

40. T. Hofmann, T. H. Yu, M. L. Folse, L. Weinhardt, M. Bär, Y. Zhang, B.V. Merinov, D. Myers, W.A. Goddard, C. Heske, “Using Photoelectron Spectroscopy and Quantum Mechanics to Determine d-Band Energies of Metals for Catalytic Applications”, Journal of Physical Chemistry C 116 (2012) 24016-24026

41. G. M. Holder, A. Bowfield, M. Surman, M. Suepfle, D. Moss, C.

Tucker, T. R. Rudd, D. G. Fernig, E. A. Yatesf, P. Weightman, “Fundamental differences in model cell-surface polysaccharides revealed by complementary optical and spectroscopic techniques”, Soft Matter 8 (2012) 6521-6527

42. K. Holliday, S. Handley-Sidhu, K. Dardenne, J. Renshaw, L. Macaskie, C. Walther, T. Stumpf, “A New Incorporation Mechanism for Trivalent Actinides into Bioapatite: A TRLFS and EXAFS Study”, Langmuir 28 (2012) 3845-3851

43. T. Holubek, T. Baumbach, S. Casalbuoni, S. Gerstl, A. Grau, M. Hagelstein, D. Saez de Jauregui, C. Boffo, W. Walter, “A superconducting switch for insertion devices with variable period length”, Physics Procedia 36 (2012) 1093-1097

44. T. Holubek, S. Casalbuoni, S. Gerstl, A. Grau, D. Saez de Jauregui, M. Kläser, Th. Schneider, L. Motowidlo, “Possible application of NbTi artificial pinning centers wire for insertion devices” Physics Procedia 36 (2012) 1098-1102

45. C. Horntrich, P. Kregsamer, S. Smolek, A. Maderitsch, P. Wobrauschek, R. Simon, A. Nutsch, M. Knoerr, C. Streli, “Influence of the excitation energy on absorption effects in Total Reflection X-ray Fluorescence analysis”, Journal of Analytical Atomic Spectrometry 27 (2012) 340-345

46. J. Hu, A. Pohl, S. Wang, J. Rothe, M. Fichtner, “Additive Effects of LiBH4 and ZrCoH3 on the Hydrogen Sorption of the Li-Mg-N-H Hydrogen Storage System”, Journal of Physical Chemistry C 116 (2012) 20246-20253

47. F. Huber, D. Schild, T. Vitova, J. Rothe, R. Kirsch, T. Schäfer: “U(VI) removal kinetics in presence of synthetic magnetite nanoparticles”, Geochimica et Cosmochimica Acta 96 (2012) 154-173

48. S. Ibrahimkutty, P. Wagener, A. Menzel, A. Plech, S. Barcikowski, “Nanoparticle formation in a cavitation bubble after pulsed laser ablation in liquid studied with high time resolution small angle x-ray scattering”, Applied Physics Letters 101 (2012) 103104-1-4

49. D. Issenmann, N. Wehmeier, S. Eon, H. Bracht, G. Buth, S. Ibrahimkutty, A. Plech, “Determination of nanoscale heat conductivity by time-resolved X-ray scattering”, Thin Solid Films (2012) doi: 10.1016/j.tsf.2012.10.132

50. D. Issenmann, S. Schleef, S. Ibrahimkutty, G. Buth, T. Baumbach, A. Plech, M. Beyer, J. Demsar, “Lattice dynamics of laser excited ferroelectric BaTiO3”, Acta Physica Polonica A 121 (2012) 319-323

51. Yu. F. Ivanov, N. N. Koval, O. V. Krysina, T. Baumbach, S. Doyle, T. Slobodsky, N. A. Timchenko, R. M. Galimov, A. N. Shmakov, “Superhard nanocrystalline Ti-Cu-N coatings deposited by vacuum arc evaporation of a sintered cathode”, Surface & Coatings Technology 207 (2012) 430-434

52. R. Jennerjahn, R. Jackstell, I. Piras, R. Franke, H. Jiao, M. Bauer, M. Beller, “Benign Catalysis with Iron: Unique Selectivity in Catalytic Isomerization Reactions of Olefins”, ChemSusChem 5 (2012) 734-739

53. A. Jesorka, A. R. Holzwarth, A. Eichhöfer, C. M. Reddy, Y. Kinoshita, H. Tamiaki, M. Katterle, J.-V. Naubron, T. S. Balaban, “Water coordinated zinc dioxo-chlorin and porphyrin self-assemblies as chlorosomal mimics: variability of supramolecular interactions”, Photochemical & Photobiological Sciences 11 (2012) 1069-1080

54. T. Jochum, M.E. Ritz, C. Schuster, S.F. Funderburk, K. Jehle, K. Schmitz, F. Brinkmann, M. Hirtz, D. Moss, A. C. B. Cato, “Toxic and non-toxic aggregates from the SBMA and normal forms of androgen receptor have distinct oligomeric structures”, Biochemica et Biophysica Acta-Molecular Basis of Disease 1822 (2012) 1070-1078

55. H. Junge, N. Marquet, A. Kammer, S. Denurra, M. Bauer, S. Wohlrab,

AnKA Publications | ANKA Seminars | ANKA Users‘ Meeting

ISI- or SCOPUS-cited publications

Carina Braun: [email protected]



F. Gärtner, M. -M. Pohl, A. Spannenberg, S. Gladiali, M. Beller, “Water Oxidation with Molecularly Defined Iridium Complexes: Insights into Homogeneous versus Heterogeneous Catalysis”, Chemistry - A European Journal 18 (2012) 12749-12758

56. B. Kallinger, P. Berwian, J. Friedrich, G. Müller, A.-D. Weber, E. Volz, G. Trachta, E. Spiecker, B. Thomas, “Doping induced lattice misfit in 4H-SiC homoepitaxy”, Journal of Crystal Growth 349 (2012) 43-49

57. B. Kanngießer, W. Malzer, I. Mantouvalou, D. Sokaras, A. G. Karydas, “A deep view in cultural heritage—confocal micro X-ray spectroscopy for depth resolved elemental analysis”, Applied Physics A: Materials Science & Processing 106 (2012) 325-338

58. N. Kasper, P. Nolte, A. Stierle, “Stability of Surface and Bulk Oxides on Pd(111) Revisited by in Situ X-ray Diffraction”, Journal of Physical Chemistry C 116 (2012) 21459-21464

59. A. Klein, K. Butsch, S. Elmas, C. Biewer, D. Heift, S. Nitsche, I. Schlipf, H. Bertagnolli, “Oxido-pincer complexes of copper(II) - An EXAFS and EPR study of mono- and binuclear [(pydotH2)CuCl2]n (n = 1 or 2)”, Polyhedron 31 (2012) 649-656

60. M. Köhl. A. Minkevich, T. Baumbach, “Improved success rate and stability for phase retrieval by including randomized overrelaxation in the hybrid input output algorithm”, Optics Express 20 (2012) 17093-17106

61. A. Kolloch, P. Leiderer, S. Ibrahimkutty, D. Issenmann, A. Plech, “Structural study of near-field ablation close to plasmon-resonant nanotriangles”, Journal of Laser Applications 24 (2012) 042015-1-6

62. T. König, J. Schulze, M. Zuber, J. Butzer, E. Hamann, A. Cecilia, A. Zwerger, A. Fauler, M. Fiederle, U. Oelfke, “Imaging properties of small-pixel spectroscopic x-ray detectors based on cadmium telluride sensors”, Physics in Medicine and Biology 57 (2012) 6743-6759

63. B. Kosog, H. S. La Pierre, M. A. Denecke, F. W. Heinemann, K. Meyer: “Oxidation State Delineation via U LIII-Edge XANES in a Series of Isostructural Uranium Coordination Complexes”, Inorganic Chemistry 51 (2012) 7940-7944

64. V. Kotaidis, T. Dekorsy, S. D. Ibrahimkutty, D. Issenmann, D. Khakulin, A. Plech, “Vibrational symmetry breaking of supported nanospheres”, Physical Review B 86 (2012) 100101-1-5

65. B. Krause, S. Darma, M. Kaufholz, H. Gräfe, S. Ulrich, M. Mantilla, R,Weigel, S. Rembold, T. Baumbach, “Modular deposition chamber for in situ X-ray experiments during RF and DC magnetron sputtering”, Journal of Synchrotron Radiation 19 (2012) 216-222

66. R. Kretzschmar, T. Mansfeldt, P. N. Mandaliev, K. Barmettler, M. A. Marcus, A. Voegelin, “Speciation of Zn in Blast Furnace Sludge from Former Sedimentation Ponds Using Synchrotron X-ray Diffraction, Fluorescence, and Absorption Spectroscopy”, Environmental Science & Technology 46 (2012) 12381-12390

67. M. Krispin, A. Ullrich, S. Horn, “Crystal structure of iron-oxide nanoparticles synthesized from ferritin”, Journal of Nanoparticle Research 14 (2012) 669-1-11

68. O. V. Krysina, N. N. Koval, Yu. F. Ivanov, N. A. Timchenko, T. Baumbach, S. Doyle, T. Slobodskyy, “Nanocrystalline nitride coatings deposited by vacuum arc plasma-assisted method”, Journal of Physics: Conference Series 370 (2012) doi:10.1088/1742-6596/370/1/012021

69. P. Kurinskiy, A. Möslang, V. Chakin, T. Slobodskyy, A.A. Minkevich,

T. Baumbach, Ch. Dorn, A. A. Goraieb, “X-ray study of surface layers of air-annealed Be12Ti and Be12V samples using synchrotron radiation”, Fusion Engineering and Design 87 (2012) 872-875

70. B. Lalinska, J. Majzlan, T. Klimko, M. Chovan, G. Kucerova, J. Michnova, R. Hovoric, J. Göttlicher, R. Steininger, “Mineralogy of Weathering Products of Fe-As-Sb Mine Wastes and Soils at several Sb Deposits in Slovakia”, Canadian Mineralogist 50 (2012) 481-500

71. S. Lazarev, M. Barchuk, S. Bauer, V. Forghani, V. Holý, F. Scholz, T. Baumbach, “Study of threading dislocation density reduction in AIGaN epilayers by Monte-Carlo simulation of high resolution reciprocal space maps of two layer system”, Journal of Applied Crystallography 46 (2012) 120-127

72. S. Lazarev, S. Bauer, K. Forghani, M. Barchuk, F. Scholz, T. Baumbach, “High resolution synchrotron X-ray studies of phase separation phenomena and the scaling law for the threading dislocation densities reduction in high quality AIGaN”, Journal of Crystal Growth 370 (2012) 51-56

73. A. Léon, J. Rothe, H. Hahn, H. Gleiter, “Short range order around Sc atoms in Fe90Sc10 nanoglasses using fluorescence X-ray absorption spectroscopy”, Revue de Métallurgie 109 (2012) 35-39

74. T. Liu, R. Simon, D. Batchelor, V. Nazmov, M. Hagelstein, “A desktop x-ray monochromator for synchrotron radiation based on refraction in mosaic prism lenses”, Journal of Synchrotron Radiation 19 (2012) 191-197

75. E. Maire, T. Morgeneyer, C. Landron, J. Adrien, L. Helfen, “Bulk evaluation of ductile damage development using high resolution tomography and laminography”, Comptes Rendus Physique 13 (2012) 328-336

76. K. Matheis, A. Eichhoefer, F. Weigend, O. T. Ehrler, O. Hampe, M. M. Kappes, “Probing the Influence of Size and Composition on the Photoelectron Spectra of Cadmium Chalcogenide Cluster Dianions”, Journal of Physical Chemistry C 116 (2012) 13800-13809

77. V. Maurel, L. Helfen, F. N’Guyen, A. Koster, M. Di Michiel, T. Baumbach, T.F. Morgeneyer, “Three-dimensional investigation of thermal barrier coatings by synchrotron-radiation computed laminography”, Scripta Materialia 66 (2012) 471-474

78. K. Medjanik, D. Chercka, P. Nagel, M. Merz, S. Schuppler, M. Baumgarten, K. Müllen, S. A. Nepijko, H.-J. Elmers, G. Schönhense, H. O. Jeschke, R. Valenti, “Orbital-Resolved Partial Charge Transfer from the Methoxy Groups of Substituted Pyrenes in Complexes with Tetracyanoquinodimethane - A NEXAFS Study”, Journal of the American Chemical Society 134 (2012) 4694-4699

79. M. Merz, F. Eilers, Th. Wolf, P. Nagel, H. v. Löhneysen, S. Schuppler, “Electronic structure of single-crystalline Sr(Fe1-xCox)2As2 probed by x-ray absorption spectroscopy: Evidence for effectively isovalent substitution of Fe2+ by Co2+”, Physical Review B 86 (2012) 104503-1-7

80. P. Meyer, “Fast and accurate X-ray lithography simulation enabled by using Monte Carlo method. New version of DoseSim: a software dedicated to deep X-ray lithography (LIGA)”, Microsystem Technologies 18 (2012) 1971-1980

81. M. Miglierini, V. Prochazka, S. Stankov, P. Svec, M. Zajac, J. Kohout, A. Lancok, D. Janickovic, S. Svec, “Crystallization kinetics of nanocrystalline alloys revealed by in situ nuclear forward scattering of synchrotron radiation”, Physical Review B 87 (2012) 020202-1-4

AnKA Publications 2012 82. A. Myagotin, A. Ershov, L. Helfen, R. Verdejo, A. Belyaev T. Baumbach, “Coalescence analysis for evolving foams via optical flow computation on projection image sequences”, Journal of Synchrotron Radiation 19 (2012) 483-491

83. K. Myung-Whun, S. Y. Jang, T. Katsufuji, A. V. Boris, “Infrared phonon anomalies and orbital ordering in single-crystalline MnV2O4 spinel”, Physical Review B 85 (2012) 224423-1-5

84. U. Noseck, E.-L. Tullborg, J. Suksi, M. Laaksoharju, V. Havlová, M. A. Denecke, G. Buckau, “Real system analyses/natural analogues”, Applied Geochemistry 27 (2012) 490-500

85. L. M. Och, B. Müller, A. Voegelin, A. Ulrich, J. Göttlicher, R. Steininger, S. Mangold, E.G. Vologina, M. Sturm, “New insights into the formation and burial of Fe/Mn accumulations in Lake Baikal sediments”, Chemical Geology 330 (2012) 244-259

86. S. Paikaray, J. Göttlicher, S. Peiffer, “As(III) retention kinetics, equilibrium and redox stability on biosynthesized schwertmannite and its fate and control on schwertmannite stability on acidic (pH 3.0) aqueous exposure”, Chemosphere 86 (2012) 557-564

87. I. V. Pekov, N. V. Chukanov, S. N. Britvin, Y. Kabalov, J. Göttlicher, V. Yapaskurt, A. E. Zadov, S. Krivovichev, W. Schüller, B. Ternes, “The sulfite anion in ettringite-group minerals: a new mineral species hielscherite, Ca3Si(OH)6(SO4)(SO3)·11H2O, and the thaumasite-hielscherite solid-solution series”, Mineralogical Magazine 76 (2012) 1133-1152

88. S. Pookpanratana, R. France, R. Felix, R.G. Wilks, L. Weinhardt, T. Hofmann, L.T. Bismaths, S. Mulcahy, F. Kronast, T.D. Moustakas, M. Bär, C. Heske, “Microstructure of vanadium-based contacts on n-type GaN”, Journal of Physics D: Applied Physics 45 (2012) 105401-1-6

89. P. Probst, A. Scheuring, M. Hofherr, S. Wünsch, K. Il’in, A. Semenov, H.-W. Hübers, V. Judin, A.-S. Müller, J. Hänisch, B. Holzapfel, M. Siegel, “Superconducting YBa2Cu3O7-δ, Thin Film Detectors for Picosecond THz Pulses”, Journal of Low Temperature Physics 167 (2012) 898-903

90. P. Probst, A. Semenov, M. Ries, A. Hoehl, P. Rieger, A. Scheuring, V. Judin, S. Wünsch, K. Il‘in, N. Smale, Y.-L. Mathis, R. Müller, G. Ulm, G. Wüstefeld, H.-W. Hübers, J. Hänisch, B. Holzapfel, M. Siegel, A.-S. Müller, “Nonthermal response of YBa2Cu3O7-δ thin films to picosecond THz pulses”, Physical Review B 85 (2012) 174511-1-8

91. A. Rack, L. Assoufid, R. Dietsch, T. Weitkamp, S. B. Trabelsi, T. Rack, F. Siewert, M. Krämer, T. Holz, I. Zanette, W.-K. Lee, P. Cloetens, E. Ziegler, “Study of multilayer-reflected beam profiles and their coherence properties using beamlines ID19 (ESRF) and 32-ID (APS)”, AIP Conference Proceedings 1437 (2012) 15-17

92. S. Richter, A. Plech, M. Steinert, M. Heinrich, S. Döring, F. Zimmermann, U. Peschel, E.B. Kley, A. Tünnermann, S. Nolte, “On the fundamental structure of femtosecond laser-induced nanogratings”, Laser & Photonics Reviews 6 (2012) 787-792

93. A. Riedel, T. dos Santos Rolo, A. Cecilia, T. van de Kamp, “Sayrevilleinae Legalov, a newly recognised subfamily of fossil weevils (Coleoptera, Curculionoidea, Attelabidae) and the use of synchrotron microtomography to examine inclusions in amber”, Zoological Journal of the Linnean Society 165 (2012) 773-794

94. L. Roiban, L. Hartmann, A. Fiore, D. Djurado, F. Chandezon, P. Reiss, J.-F. Legrand, S. Doyle, M. Brinkmann, O. Ersen, “Mapping the 3D distribution of CdSe nanocrystals in highly oriented and nanostructured hybrid P3HT-CdSe films grown by directional epitaxial crystallization”, Nanoscale 4 (2012) 7212-7220

95. J. Rothe, S. Butorin, K. Dardenne, M. A. Denecke, B. Kienzler, M. Löble, V. Metz, A. Seibert, M. Steppert, T. Vitova, C. Walther, H. Geckeis, “The INE-beamline for actinide science at ANKA”, Review

of Scientific Instruments 83 (2012) 043105-1-1396. D. K. Satapathy, M. A. Uribe-Laverde, I. Marozau, V. K. Malik, S. Das,

Th. Wagner, C. Marcelot, J. Stahn, S. Brück, A. Rühm, S. Macke, T. Tietze, E. Goering, A. Frano, J.-H. Kim, M. Wu, E. Benckiser, B. Keimer, A. Devishvili, B. P. Toperverg, M. Merz, P. Nagel, S. Schuppler, C. Bernhard, “Magnetic Proximity Effect in YBa2Cu3O7/La2/3Ca1/3MnO3 and YBa2Cu3O7/LaMnO3+δ Superlattices”, Physical Review Letters 108 (2012) 197201-1-5

97. N. Schleicher, U. Kramar, V. Dietze, U. Kaminski, S. Norra, “Geochemical characterization of single atmospheric particles from the Eyjafjallajökull volcano eruption event collected at ground-based sampling sites in Germany”, Atmospheric Environment 48 (2012) 113-121

98. D. A. Schmidt, E. Bründermann, M. Havenith, “Combined far- and near-field chemical nanoscope at ANKA-IR2: applications and detection schemes”, 6th Workshop on Infrared Spectroscopy and Microscopy with Accelerator-Based Sources, Journal of Physics: Conference Series 359 (2012) DOI: 10.1088/1742-6596/359/1/012015

99. B. Schmidt-Hansberg, M. Sanyal, N. Grossiord, Y. Galagan, M. Baunach, M. F. G. Klein, A. Colsmann, P. Scharfer, U. Lemmer, H. Dosch, J. Michels, E. Barrena, W. Schabel, “Investigation of non-halogenated solvent mixtures for high throughput fabrication of polymer-fullerene solar cells”, Solar Energy Materials & Solar Cells 96 (2012) 195-201

100. D. Schörling, F. Antoniou, A. Bernhard, A. Bragin, M. Karppinen, R. Maccaferri, N. Mezentsev, Y. Papaphilippou, P. Peiffer, R. Rossmanith, G. Rumolo, S. Russenschuck, P. Vobly, K. Zolotarev, „Design and System Integration of the Superconducting Wiggler Magnets for the CLIC Damping Rings”, Physical Review Special Topics Accelerators and Beams 15 (2012) 042401-1-14

101. P. Schroth, T. Slobodskyy, D. Grigoriev, A. Minkevich, M. Riotte, S. Lazarev, E. Fohtung, D.Z. Hu, D.M. Schaadt, T. Baumbach, „Investigation of buried quantum dots using grazing incidence X-ray diffraction”, Materials Science and Engineering B 177 (2012) 721-724

102. L. Shen, S.-W. Yang, S. Xiang, T. Liu, B. Zhao, M.-F. Ng, J. Goettlicher, J. Yi, S. Li, L. Wang, J. Ding, B. Chen, S.-H. Wei, Y. P. Feng, “Origin of Long-Range Ferromagnetic Ordering in Metal−Organic Frameworks with Antiferromagnetic Dimeric-Cu(II) Building Units”, Journal of the American Chemical Society 134 (2012) 17286-17290

103. T. Slobodskyy, P. Schroth, D. Grigoriev, A. A. Minkevich, D. Z. Hu, D. Schaadt, T. Baumbach, “A portable molecular beam epitaxy system for in situ x-ray investigations at synchrotron beamlines”, Review of Scientific Instruments 83 (2012) 105112-105117

104. H. Sommer, K. Regenauer-Lieb, B. Gasharova, H.Jung, “The formation of volcanic centers at the Colorado Plateau as a result of the passage of aqueous fluid through the oceanic lithosphere and the subcontinental mantle: New implications for the planetary water cycle in the western United States”, Journal of Geodynamics 61 (2012) 154-171

105. M. J. Spallek, S. Stockinger, R. Goddard, O. Trapp, “Modular Palladium Bipyrazoles for the Isomerization of Allylbenzenes - Mechanistic Considerations and Insights into Catalyst Design and Activity, Role of Solvent, and Additive Effects”, Advanced Synthesis & Catalysis 354 (2012) 1466-1480

106. D. Tampieri, T. Allesandro, M. Sandri, S. Sprio, E. Landi, L. Bertinetti, S. Panseri, G. Pepponi, J. Göttlicher, M. Banobre-Lopez, J. Rivas, “Intrinsic magnetism and hyperthermia in bioactive Fe-doped hydroxyapatite”, Acta Biomaterialia 8 (2012) 843-851


User Operation Accelerator Report Beamline Report Lab Report Applications Appendix Carina Braun: [email protected]


107. V. Tauson, J. Göttlicher, A. N. Sapozhnikov, S. Mangold, E. E. Lustenberg, “Sulphur speciation in lazurite-type minerals (Na,Ca)8[Al6Si6O24](SO4,S)2 and their annealing products: a comparative XPS and XAS study”, European Journal of Mineralogy 24 (2012) 133-152

108. P. Thoma, A. Scheuring, M. Hofherr, S. Wünsch, K. Il’in, N. Smale, V. Judin, N. Hiller, A.-S. Müller, A. Semenov, H.-W. Hübers, M. Siegel, “Real-time measurement of picosecond THz pulses by an ultra-fast YBa2Cu3O7-d detection system”, Applied Physics Letters 101 (2012) 142601-1-4

109. P. Thoma, J. Raasch, A. Scheuring, M. Hofherr, K. Il’in, S. Wunsch, A. Semenov, H.-W. Hübers, V. Judin, A.-S. Müller, N. Smale, J. Hanisch, B. Holzapfel, M. Siegel, “Highly responsive Y-Ba-Cu-O thin film THz detectors with picosecond time resolution”, IEEE Transactions on Applied Superconductivity 23 (2012) doi: 10.1109/TASC.2012.2233851

110. M. Vespa, M. Rini, J. Spino, T. Vitova, J. Somers, “Fabrication and characterization of (U, Am)O2-x transmutation targets”, Journal of Nuclear Materials 421 (2012) 80-88

111. A. Vlad, A. Stierle, R. Westerström, S. Blomberg, A. Mikkelsen, E. Lundgren, “Oxygen interaction with the Pd(112) surface: From chemisorption to bulk oxide formation”, Physical Review B 86 (2012) 035407-1-9

112. M. Vogelgesang, S. Chilingaryan, T. dos Santos Rolo, A. Kopmann, “UFO: A Scalable GPU-based Image Processing Framework for On-line Monitoring”, 2012 IEEE 14th International Conference on High Performance Computing and Communications & 2012 IEEE 9th International Conference on Embedded Software and Systems (2012) 824-829

113. V. Vonk, J. Huijben, D. Kukuruznyak, A. Stierle, H. Hilgenkamp, A. Brinkman, S. Harkema, “Polar-discontinuity-retaining A-site intermixing and vacancies at SrTiO3/LaAlO3 interfaces”, Physical Review B 85 (2012) 045401-1-5

114. C. Walther, J. Rothe, B. Schimmelpfennig, M. Fuss, “Thorium nanochemistry: the solution structure of the Th(IV)-hydroxo pentamer”, Dalton Transactions 41 (2012) 10941-10947

115. C. N. Wang, P. Marsik, R. Schuster, A. Dubroka, M. Rössle, Ch. Niedermayer, G. D. Varma, A. F. Wang, X. H. Chen, T. Wolf, C. Bernhard, “Macroscopic phase segregation in superconducting K0.73Fe1.67Se2 as seen by muon spin rotation and infrared spectroscopy”, Physical Review B 85 (2012) 214503-1-8

116. L. Weinhardt, A. Benkert, F. Meyer, M. Blum, R.G. Wilks, W. Yang, M. Bär, F. Reinert, C. Heske, “Nuclear dynamics and spectator effects in resonant inelastic soft x-ray scattering of gas-phase water molecules”, Journal of Chemical Physics 136 (2012) 144311-1-6

117. M. West, A. T. Ellis, P. J. Potts, C. Streli, C. Vanhoof, D. Wegrzynek, P. Wobrauschek, “Atomic spectrometry update - X-ray fluorescence spectrometry”, Journal of Analytical Atomic Spectrometry 27 (2012) 1603-1644

118. F. Xu, L. Helfen, H. Suhonen, D. Elgrabli, S. Bayat, P. Reischig, T. Baumbach, T. Cloetens, “Correlative nanoscale 3d imaging of electron density and elemental composition in extended objects”, PloS ONE 7 (2012) e50124-1-6

119. F. Xu, L. Helfen, T. Baumbach, H. Suhonen, “Comparison of image quality in computed laminography and tomography”, Optics Express

20 (2012) 794-806120. S. R. Yeduru, A. Backen, C. Kübel, D. Wang, T. Scherer, S. Fähler,

L. Schultz, M. Kohl, “Microstructure of free-standing epitaxial Ni-Mn-Ga films before and after variant reorientation”, Scripta Materialia 66 (2012) 566-569

121. M. Zuber, T. König, E. Hamann, J. Butzer, A. Cecilia, M. Fiederle, U. Oelfke, “Synchrotron Measurements of the Energy Response Functions of CdTe Medipix2 MXR Detectors with Pixel Pitches of 110 and 165 µm”, Journal of Instrumentation 7 (2012) C12018

AnKA Publications 2012


1. S. Casalbuoni, S. Gerstl, A. Grau, T. Holubek, D. Saez de Jauregui, “Beam Heat Load And Pressure In The Superconducting Undulator Installed at ANKA”, Proceedings of the International Particle Accelerator Conference IPAC’12 (2012) 717-719

2. S. Casalbuoni, T. Baumbach, S. Gerstl, A. Grau, M. Hagelstein, T. Holubek, D. Saez de Jauregui, C. Boffo, W. Walter, “Calculated spectra from magnetic field measurements of 1,5 m superconducting undulator coils”, Proceedings of the International Particle Accelerator Conference IPAC’12 (2012) 711-713

3. A. Grau, T. Baumbach, S. Casalbuoni, S. Gerstl, M. Hagelstein, T. Holubek, D. Saez de Jauregui, “Cryogen-Free Field Measurement System for Superconducting Undulator Coils”, Proceedings of the International Particle Accelerator Conference IPAC’12 (2012) 714-716

4. E. Huttel, N. Hiller, V. Judin, B. Kehrer, S. Marsching, A.-S. Müller, N. J. Smale, “Characterization and Stabilization of Multi-Bunch Instabilities at the ANKA Storage Ring”, Proceedings of the International Particle Accelerator Conference IPAC’12 (2012) 2849-2851

5. V. Judin, N. Hiller, A. Hofmann, E. Huttel, B. Kehrer, M. Klein, S. Marsching, C. Meuter, A.-S. Müller, M. J. Nasse, M. Schuh, N. Smale, M. Streicher, “Spectral and temporal observations of CSR at ANKA”, Proceedings of the International Particle Accelerator Conference IPAC’12 (2012) 1623-1625

6. S. Marsching, N. Hiller, E. Huttel, V. Judin, B. Kehrer, M. Klein, C. Meuter, A.-S. Müller, M.J. Nasse, M. Schuh, N. J. Smale, M. Streichert, G. Rehm, “Commissioning of a New Beam-position Monitoring System at ANKA”, Proceedings of the International Particle Accelerator Conference IPAC’12 (2012) 825-827

7. J. Moosmann, V. Altapova, D. Hänschke, R. Hofmann, T. Baumbach, “Nonlinear, noniterative, single-distance phase retrieval and developmental Biology”, AIP Conference Proceedings 1437 (2012) 57-62

8. A.-S. Müller, N. Hiller, A. Hofmann, E. Huttel, K. Ilin, V. Judin, B. Kehrer, M. Klein, S. Marsching, C. Meuter S. Naknaimueang, M.J. Nasse, A. Plech, P. Probst, A. Scheuring, M. Schuh, M. Schwarz, M. Siegel, N. Smale, M. Streichert, F. Caspers, A. Semenov, H.W. Hubers, E. Brundermann, “Experimental Aspects of CSR in the ANKA storage Ring”, Beam Dynamics Newsletter 57 (2012) 154-165

9. S. Naknaimueang, E. Huttel, A.-S. Müller, M. J. Nasse, R. Rossmanith, M. Schuh, M. Schwarz, P. Wesolowski, M. Schmelling, “Optimization of beam optics parameters of the linear-based terahertz source FLUTE”, Proceedings of the International Particle Accelerator Conference IPAC’12 (2012) 1629-1631

10. D. Saez de Jauregui, T. Baumbach, S. Casalbuoni, A. Grau, S. Gerstl, M. Hagelstein, C. Heske, T. Holubek, B. Krause, A. Seiler, S. Stankov, L. Weinhardt, C. Boffo, C. Antoine, Y. Boudigou, “Characterization of vacuum chamber samples for superconducting insertion devices”, Proceedings of the International Particle Accelerator Conference IPAC’12 (2012) 723-725

11. D. Schoerling, P. Ferracin, P. Fessia, M. Karppinen, J. Mazet, S. Russenschuck, P. Peiffer, A. Grau, “First magnetic test of a superconducting Nb3Sn wiggler magnet for CLIC”, Proceedings of the International Particle Accelerator Conference IPAC’12 (2012) 1957-1959

12. M. Schwarz, E. Huttel, A.-S. Müller, S. Naknaimueang, M.J. Nasse, R. Rossmanith, M. Schuh, P. Wesolowski, M. Schmelling, “Comparison of Various Sources of Coherent THz radiation at FLUTE”, Proceedings of the International Particle Accelerator Conference IPAC’12 (2012) 568-570

13. R. Simon, V. Altapova, T. Baumbach, M. Kluge, A. Last, “Refractive optical elements and optical system for high energy x-ray Microscopy”, AIP Conference Proceedings 1437 (2012) 116-120

14. M. Streichert, N. Hiller, E. Huttel, V. Judin, B. Kehrer, M. Klein, S. Marsching, C. Meuter, M.J. Nasse, A.-S. Müller, M. Schuh, N. Smale, “Global Scan of All Stable Settings (GLASS) for the ANKA Storage Ring”, Proceedings ICAP 2012 Rostock - Warnemünde (2012) 239-241

15. M. Streichert, N. Hiller, E. Huttel, V. Judin, B. Kehrer, M. Klein, S. Marsching, C. Meuter, M.J. Nasse, A.-S. Müller, M. Schuh, N. Smale, “Global Optimization of the ANKA Lattice Using Multiobjective Genetic Algorithms (MOGA)”, Proceedings ICAP 2012 Rostock - Warnemünde (2012) 72-74

16. M. Streichert, V. A. Rodriguez, A. Bernhard, N. Hiller, E. Huttel, V. Judin, B. Kehrer, M. Klein, S. Marsching, C. Meuter, M.J. Nasse, A.-S. Müller, M Schuh, M. Schwarz, N.J. Smale, “Simulations of Fringe Fields and Multipoles for the ANKA Storage Ring Bending Magnets”, Proceedings of the International Particle Accelerator Conference IPAC’12 (2012) 1626-1628

Other refereed publications

User Operation Accelerator Report Beamline Report Lab Report Applications Appendix Carina Braun: [email protected]


04.12.2012 Yuan-Wei ChangMaterials Science and Engineering, National Chiao Tung University, Hsin-Chu, Taiwan (R.O.C.) In-Situ Failure Analysis during Electromigration Test Using Kelvin Bump Structure and Finite...

27.11.2012Dirk ZimochUsing the EPICS StreamDevice Driver

26.11.2012Elke ZimochGraphical User Interfaces for Large Research Facilities

19.11.2012Kevin E. SmithDepartment of Physics, Boston University, USAProbing the Origin of the Metal-to-Insulator Transition in Thin Film Vanadium Oxides

22.10.2012Jutta SchwarzkopfLeibniz Institute for Crystal Growth, Berlin, GermanyDeposition of strained ferroelectric NaNbO3 and KNbO3 thin films

19.10.2012Johanna NelsonStanford Linear Accelerator Center, Stanford, USAIn situ Imaging Studies of High Capacity Battery Materials Using Transmission X-ray Microscopy

05.10.2012Natalia Dubrovinskaia & Leonid DubrovinskyMaterial Physics und Technology at Extreme Conditions, Laboratory of Crystallography, Universität...Beyond Diamond or Novel Materials at High Pressure

05.10.2012Christine KuntscherExperimentalphysikII,Universit•atAugsburg,GermanyInfrared Microspectroscopy: A versatile tool to study the optical properties of small samples...

01.10.2012Timo AschenbrennerUniversity of Bremen, Institute of Solid State Physics, Semiconductor Epitaxy, Bremen, GermanyGrowth and characterisation of GaN-based nanostructures for light emitting devices

01.10.2012Stephan Gärtner & Thomas KrönerKIT, Karlsruhe, GermanyDie Bedeutung von IP in FuE-Einrichtungen

27.09.2012Karl BaneStanford Linear Accelerator Center, Stanford University, Stanford, USACorrugated pipe for terahertz radiation and dechirping

26.09.2012Karl BaneStanford Linear Accelerator Center, Stanford University, Stanford, USAWakefields of sub-picosecond electron bunches

20.09.2012Maria FeofilovaDepartment of Molecular Biophysics, Faculty of Physics, Saint-Petersburg State University, RussiaBiophysical investigation of interactions of cis- and transdiamminedichlorplatinum(II) with...

20.09.2012Melanie BauerHochschule MannheimEXPRESSION, PURIFICATION AND STRUCTURAL STUDIES OF THE VIRAL ‘PROTEIN X’

12.09.2012Laura Rubio LorenteCytotoxicity and Genotoxicity of Nanosilver

12.09.2012Deirdre O\’DonnellGalwayCharacterisation Of The Hot Plate Model Of Nociception In The Rat And Investigation Of The...

11.09.2012Matteo PellegriniDepartment of Neuroscience and Brain Technologies, Istituto Italiano di Tecnologia, Genova, ItalyNeuroprotective effect of mesenchimal stem cells in an animal model of amyotrophic lateral sclerosis

11.09.2012Julia SchweizerDresden, GermanyMössbauer Spectroscopy of Iron-Sulfur Protein LytB from Escherichia Coli

10.09.2012Cristian MocutaSynchrotron SOLEIL, Gif-sur-Yvette, FranceX-ray Diffraction Study of Semiconductor Hererostructures Using Micro- and Nano-focused X-ray Beams

03.09.2012Thilo F. MorgeneyerMines ParisTech, Centre des matériaux, CNRS UMR, Evry Cedex, FranceUse of 3D imaging techniques for assessment of damage in engineering materials

AnKA Seminars

ANKA Publications | ANKA Seminars | ANKA Users‘ Meeting

30.07.2012Carsten P. WelschUniversity of Liverpool / Cockcroft Institute, UKAccelerator and Beam Diagnostics R&D for Antimatter Studies

30.07.2012Stephan V. RothDESY, Hamburg, GermanyTailoring nanocomposite materials

19.07.2012Joachim WittbrodtDept. of Molecular Developmental Biology & Physiology, Centre for Organismal Studies, University...Seeing is believing- imaging and quantitative genetics

18.07.2012Xianghui XiaoAdvanced Photon Source, Argonne National Laboratory, USAPhase contrast imaging and its optimal condition

06.07.2012Efim GluskinAdvanced Photon Source, Argonne National Laboratory, USANew electromagnetic IDs at the APS

21.06.2012Eike JanochaHelmholtz-Zentrum Berlin für Materialien und Energie, GermanyEffects of deposition parameters on the structural and electronic properties of semiconductor...

18.06.2012George TsiakatourasMolecular beam epitaxy of the GaN semiconductor on diamond and r-plane sapphire substrates

15.06.2012Alexander NovokhatskiSLAC National Accelerator Laboratory, CA, USACoherent synchrotron radiation: theory and simulations.

14.06.2012Quanbao MaSurface Science Division & Center of Smart Interfaces, Technische Universität Darmstadt, GermanyZnO, Ge, InGaN and SiC Films: Growth and Properties

01.06.2012Emil-Alexandru BrujanDepartment of Hydraulics, University Politehnica Bucharest, RomaniaShock wave emission from a cloud of bubbles

22.05.2012Tim SaldittInst. für Röntgenphysik, Universität Göttingen, GermanyX-ray imaging and tomography of cells and tissues: from scanning beam diffraction to full field...

21.05.2012Dirk-Peter HertenCluster of Excellence and Institute for Physical Chemistry Heidelberg University, GermanyLearn counting, get better sight, and understand chemistry and biology better

Pawel Wesolowski: [email protected]


Figure 1: Prof. Momose (Institute of Multidisciplinary Research for Advanced Materials - IMRAM), giving a talk about developments with grating interferometry at ANKA


14.05.2012Stéphane SanfilippoSwissFEL, PSI, Villigen, SwitzerlandMagnetic measurements of the series SwissFEL Magnets and Undulators: Status and Plan

09.05.2012Przemysław PiekarzInstitute of Nuclear Physics, Polish Academy of Sciences, PolandAb initio studies of lattice dynamics in rare earths

07.05.2012Angela Intermite / Massimiliano PutignanoUniversity of Liverpool, United KingdomFrom photonics to accelerators: optical fibre beam loss monitoring system / Supersonic gas-jet...

03.05.2012Felix SchmittBen Ltaief LtaiefFB Physik, Freie Universität Duisburg-Essen, Duisburg, GermanyTwo and one photon photoemission spectroscopy techniques: Introduction and application to thin...

23.04.2012Enrica ChiadroniLaboratori Nazionali di Frascati – INFN, ItalyThe THz Beamlines at SPARC_LAB

20.04.2012Dagmar Kreikemeyer-LorenzoFritz-Haber-Institut der Max-Planck-Gesellschaft, Berlin, GermanyStructure determination of the reaction intermediates of methanol oxidation on copper surfaces...

19.04.2012Giuseppe MercurioPeter Grünberg Institut (PGI-3), Forschungszentrum Jülich, Germany and Jülich Aachen Research...Study of Molecule-Metal Interfaces by Means of the Normal Incidence X-ray Standing Wave Technique

19.04.2012Peter PeierSwissFEL, PSI, Villigen, SwitzerlandLongitudinal electron bunch and x-ray diagnostics for SwissFEL

16.04.2012Jörn GroosGeophysical Institute (GPI), KIT, Karlsruhe, GermanySeismic Noise: Basics and Implications for Experimental Physics

04.04.2012Thomas Koenig

German Cancer Research Center, GermanyFrom Greyscale to Colour: Modern Spectroscopic X-Ray Imaging

02.04.2012Niklas OttossonFOM Institute AMOLF, Amsterdam, The NetherlandsHow photoelectrons can aid our understanding of aqueous solutions

20.03.2012Philipp SchneiderInstitute for Biomechanics, ETH Zurich, Zurich, SwitzerlandRecent advances in quantitative and functional X-ray imaging of bone tissue for osteoporosis...

14.03.2012Hamed TarawnehSESAME, Allan, JordanStatus of SESAME Synchrotron Light Source

12.03.2012Alexander KostenkoQuantitative Imaging Group, Department of Imaging Science & Technology, Faculty of Applied Scienc...Compressive sensing for X-ray phase-contrast imaging

09.03.2012Jochen HillerTechnical University of Denmark (DTU), Department of Mechanical Engineering, Kgs. Lyngby, DenmarkDimensional X-ray Computed Tomography for Industrial Applications

07.03.2012Sebastian KalbfleischInstitut für Röntgenphysik, Georg-August-Universität Göttingen, GermanyWaveguide-based Holographic X-Ray Imaging at the Coherence Beamline P10 of PETRA III/DESY

05.03.2012Shara KalthoffMedizinische Fakultät der Universität Heidelberg, GermanyAlgebraic reconstruction technique

02.03.2012Christian KnöchelDepartment of Anatomy, University of California San Francisco, San Francisco and National Center...Cryogenic Soft X-ray Tomography of Biological Specimen

15.02.2012Gudrun LotzeSchool of Chemistry, University of Reading, Whiteknights and Diamond Light Source, Harwell Scienc...A versatile high-throughput system for solution SAXS

AnKA Seminars

ANKA Publications | ANKA Seminars | ANKA Users‘ Meeting

14.02.2012Klaus HaßNational Synchrotron Research Institute, Nakhon Ratchasima, ThailandFrequency Map Analysis of the Siam Photon Source Storage Ring with a wavelength shifter

13.02.2012Manuel Fernández MartínezEuropean Synchrotron Radiation Facility, Grenoble, FranceScattering and Imaging of Collagenous Tissues for Diagnostics

13.02.2012Riccardo BartoliniDiamond Light Source, United KingdomLight Sources R&D activity at Diamond

30.01.2012Pep CampmanyCELLS, SpainInstallation and commissioning of superconducting wiggler SCW30 at ALBA light source

User Operation Accelerator Report Beamline Report Lab Report Applications Appendix Pawel Wesolowski: [email protected]


On October 10-11, 2012, the ANKA synchrotron radiation facility and the Karlsruhe NanoMicro Facility (KNMF), both user research facilities at the Karlsruhe Institute of Technology (KIT) in Germany, hosted their fourth joint annual user meeting at the Ettlingen Castle. In the extraordinary ambiance of the baroque palace, the ANKA and KNMF directorates (represented by Clemens Heske and Jürgen Mohr, respectively) welcomed almost 200 participants representing universities, research facilities, and companies from 10 different countries. The meeting was kicked off by KIT Chief Science Officer Volker Saile, who emphasized the positive developments and increase in user numbers at both facilities.

Facility ReportIn his welcome talk, ANKA Director Clemens Heske explained the most important recent developments at ANKA in detail. The conversion of the former Institute for Synchrotron Radiation (ISS) into the new Institute for Photon Science and Synchrotron Radiation (IPS) also implicated a new status for the synchrotron radiation facility ANKA: formerly being part of the ISS, the facility now has the status of an independent and full-fledged German National User Facility, with a particular research focus on medium-energy X-rays and THz/IR radiation. ANKA strives to create a unique integrated beamline and laboratory infrastructure, with a mission to provide an outstanding research environment to an international user community,Clemens Heske displayed the ongoing process of extending the ANKA hall to create space for new beamlines and laboratories that will be established at the facility within the next three years, for example the IMAGE/XMIC twin-beamlines. These will feature three different operation modes, which promises exciting opportunities in areas such as Transmission Microscopy at high photon energies, Phase Contrast Tomography, and Laminography.

Jürgen Mohr presented the development of the KNMF on the way to an independent user facility. In the last year the number of users were strongly increased, so that the facility is already 40% used by external users, which is ahead of schedule. Scientific highlights have been achieved on the field of Nanopatterning, on TEM Tomography in Atomic Scale, on functionalization by Dip Pen Nanolithography, and on micro fabrication of X-ray optical components for Phase Contrast Imaging. The new available technologies for users within KNMF 3D Photon Laser Lithography, X-Ray Photonelectron Spectroscopy, Infrared Ellipsometry, X-Ray Absorption Spectroscopy and Powder X-Ray Diffraction were described by Jürgen Mohr. Together with the coming technologies in 2013, Nanoimprint technique, Helium ion microscopy and IR microscopy, KNMF is offering 26 highly advanced technologies for multimaterial micro and nano fabrication and characterization with the unique possibility to combine technologies and characterization methods to serve the users at the best.

Academic TalksDuring a wide range of academic talks, scientists from both facilities had the opportunity to discuss the year‘s research results in detail. On the first day, the multifaceted applications of synchrotron radiation were illustrated by the talks of four invited scientists. First, Tobias Reich (University of Mainz, Germany) presented detailed insights into the contribution of X-ray absorption spectroscopy to environmental actinide chemistry, presenting possible future solutions in the long-term remediation of high-level nuclear waste sites. The afternoon session was opened by Alexander Boris (Max-Planck-Institute for Solid State Research, Stuttgart, Germany) with a talk on the control of correlated electrons in transition-metal-oxide superlattices, followed by Electra Gizeli (University of Crete, Greece), explaining the

4th AnKA & KnMF Users‘ Meeting 2012

ANKA Publications | ANKA Seminars | AnKA Users‘ Meeting

functionalization of SAW biosensors by using L-DPN. Together with Tobias Weidner (Max-Planck-Institute for Polymer Research, Mainz, Germany) the assembled users watched mineral proteins at work, as seen by photoelectron spectroscopy. On the second day of the meeting, two parallel facility-specific workshops presented highlights of the previous year’s research activities. In the synchrotron-based workshop, a round of talks covering materials research at the micro- and nano-scale using diffraction techniques started with a presentation by Alexander Wanner (KIT). He illustrated the combination of high-speed detectors and high flux to probe the surface modification of steels during in-situ high-power laser treatment. Francesca Paola Anna Fabbiani (University of Göttingen, Germany) continued the session with recent examples of high-pressure synchrotron single-crystal XRD on molecular crystals, showing how high-pressure research can investigate pathways to novel polymorphic forms of pharmaceutical materials. It was also demonstrated how conformational and solvent-channel aspects of vitamin structures can be studied via high-pressure XRD, and how ordering of both the organic structure and the included water molecules can be followed by XRD. Simon Geier (University of Stuttgart, Germany) then presented the results of in-situ investigations of the crystallization of polyamide 6 in the presence of nano-structured impact modifiers. In his presentation, Simon Geier showed that in-situ XRD studies of the crystallization process as a function of additive concentration could be correlated with independent measurements of mechanical stiffness of the blend. Holger Gesswein (KIT) gave an introduction to the chemistry and crystallography of lithium-ion batteries and went on to present the results of recent in-situ synchrotron XRD and XAS investigations of the charging and discharging of lithium-ion electrode materials. It was also demonstrated how quasi-automatic Rietveld structure refinement of successive XRD data-sets with minimal user-intervention can follow the structural variations in these intercalation compounds as a function of charge state. Benham Khanbabaee (University of Siegen, Germany) then described how depth profiling of iron-implanted silicon has been studied by means of extremely asymmetric X-ray diffraction (EAD), showing how the influence of ion-bombardment on both strain and surface roughening can be characterized via the rocking curves of asymmetric reflections. Enrico Mugnaioli (University of Mainz, Germany) continued the scientific presentations with an overview of the concept and applications of Automated Diffraction Tomography, showing how by means of tomographic instead of crystallographic sampling of reciprocal space, increased diffraction information, reduced dynamical effects, and decreased radiation doses can

be achieved in the same experiment. This leads to improved solvability of structures from electron diffraction data. The synchrontron-based workshop concluded with a contribution by Vedran Vonk (University Nijmegen, The Netherlands), who demonstrated how the crystallographic structure and chemical composition of interfaces in ambient environments can be studied by surface x-ray diffraction and anomalous scattering.

User Committee Sessions and Poster Award

During the discussion sessions conducted by the International User Committees of both facilities, both user groups strongly appreciated the fast implementation of optimization measures suggested during last year‘s joint user meeting. Then, a poster session, in which 84 posters displayed the newest scientific findings at ANKA and KNMF, completed the program.

Three „Best Poster Awards“ were bestowed:

• First prize: „Chemical Micro- and Nanomicroscopy Applications for ANKA-IR2 Nanoscope“ by E. Edengeiser (University of Bochum, Germany), M. Mischo, E. Bründermann, D. A. Schmidt, J. Steinmann, B. Gasharova, Y.-L. Mathis, D. Moss and M. Havenith

• Second prize: “Discovering the Vanished Polychromy and Gilding of Phoenician Ivories Using the Colour X-ray Camera” by Marie Albéric (Université Pierre et Marie Curie Paris VI, France), Oliver Scharf, Katharina Müller, Andrea Wähning, Anjouar Bjeoumikhov, Ivan Ordavo, Rolf Simon, and Ina Reiche

• Honorable mention: „Utilizing XAS to Uncover the Structure and Oxidation State of Pt-based Diesel Oxidation Catalysts“ by Andreas Gänzler (KIT), Alexey Boubnov, Sabrina Conrad, Maria Casapu, and Jan-Dierk Grunwaldt.


Figure 1: Participants ot the Fourth ANKA and KNMF Users Meeting 2012

Figure 2: During the poster session, 84 posters displayed the newest scientific findings at ANKA and KNMF

ANKA Annual Report 2012 · with 65 of these being allocated beam-time. For Call 20 there were 105...

Documents

Transcript of ANKA Annual Report 2012 · with 65 of these being allocated beam-time. For Call 20 there were 105...