ANKA Instrumentation Book 2012 - KITThe vacuum system of the ANKA storage ring is made from...

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www.kit.edu

ANKA Synchrotron Radiation Facility at KIT

Directors: Prof. Dr. Tilo Baumbach,Prof. Dr. Clemens Heske, Prof. Dr. Anke-Susanne Müller

Contact address:Karlsruhe Institute of Technology (KIT)Campus NorthHermann-von-Helmholtz-Platz 176344 Eggenstein-Leopoldshafen

ANKA User Office:Phone: +49 (0)721 608 26186Fax: +49 (0)721 608 26789E-Mail: [email protected]

Publisher:Karlsruhe Institute of Technology (KIT)Kaiserstraße 12 · 76131 Karlsruhe

Status: September 2013

www.kit.edu

ANKA is the Synchrotron Radiation Facility of the Karlsruhe Institute of Technology (KIT). The facility is operated by the Institute for Photon Science and Synchrotron Radiation (IPS) and started user operation in 2003.As large-scale facility of the Hermann-von-Helmholtz Asso-ciation of German Research Centers, ANKA is part of the national and European infrastructure offered to scientific and commercial users for performing excellent science and relevant technological development.

The Karlsruhe Institute of Technology (KIT) represents the merger of Universität Karlsruhe (TH) with the Forschungszentrum Karlsruhe. Both partners are joining their forces in KIT in order to achieve an unprecedented quality of cooperation. With approx. 9.300 employees and an annual budget of three-quarter billon €, KIT strives to become a leading institution in selected science disciplines world-wide.

With its 18 research centres and an annual budget of approx 3,8 billion €, the Hermann-von-Helmholtz Association of German Research Centers is Germany´s largest research institution. The 36.000 employees produce top-rate scientific results in six research fields. The Helmholtz Association identifies and takes on the grand challenges of society, science and the economy, in particular through the investigation of highly complex systems.

www.anka.kit.edu

KIT – University of the State Baden-Württemberg and National Laboratory of the Helmholtz Association www.kit.edu

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ANKA Instrumentation Book 2012

ANKA SyNCHRoTRoN RADIATIoN FACILITy

www.anka.kit.edu

Accelerator / Insertion Devices

ANKA Control System 16

Beamlines at ANKA 20FLUO 26INE 30IRI 36IR2 38SUL-X 40UV-CD12 44WERA 48XAS 50MPI 56NANO 60PDIFF 66SCD 70IMAGE 74TOPO-TOMO 78LIGA I, II, III 84

ANKA Commercial Services 90

ANKA User Service 88

Design 4Injector 5Storage ring optics 6RF system 7Magnets 8Vacuum System 9Parameters 11Insertion Devices 12

ANKA Control System

Beamlines User Service

CoSCommercial Services

2012 ANKA INSTRUMENTATION BOOK | 3


Design

Injector

Storage Ring Optics

RF System

Magnets

Vacuum System

Parameters

Insertion Devices

4

User Service

Thema

Beamlines

Design of the accelerators

ANKA Control System Commercial Services

Design Injector Storage Ring Optics RF System Magnets Vacuum System Parameters Insertion Devices

The accelerator complex consists of a 53 MeV microtron as a preaccelerator, a 500 MeV booster synchrotron and a 2.5 GeV storage ring. The injector has a repetition rate of 1 Hz and the booster current is about 5 mA. Injection into the storage ring is two times a day; a nominal current of up to 200 mA is accumulated in the storage ring at 500 MeV and then ramped to 2.5 GeV. The lifetime of the stored beam at 2.5 GeV is 16 hours for 150 mA. Figure 1 gives an overview of the facility with the injector inside the radiation shield wall and figure 2 shows a photo of the ANKA hall.

Figure 2: View of the ANKA hall with the accelerator complex. The enclosure in the center houses the microtron and booster synchrotron; the 2.5 GeV storage ring with 110 m circumference is located close to the inner side of the concrete radiation protection wall.


Figure 1: Layout of the ANKA storage ring, the radiation shield wall and the injector


ContaCt

Commercial Services

Erhard Huttel: [email protected] +49 (0)721 608 26181Anke-Susanne Müller: [email protected] +49 (0)721 608 26260

Ingrid Birkel: [email protected] +49 (0)721 608 26183Pawel Wesolowski: [email protected] +49 (0)721 608 26063

Accelerator control room +49 (0)721 608 26281

Injector

Electrons are generated from a triode gun at 90 keV and are injected into a racetrack microtron. This gun was installed in 2009 and allows both multibunch and single bunch operation. The acceleration unit of the microtron is a 5.3 MV linac, through which the electrons pass 10 times to pick up the final energy of 53 MeV. The linac has a radiofrequency of 3 GHz and is powered by a 6 MW klystron. The main dipoles of the microtron have a field of 1.2 T. The microtron is shown in Figure 3.The electrons from the microtron are injected off-axis into the booster synchrotron in a multi-turn process with one kicker positioned opposite to the injection septum. The optics of the booster synchrotron consists of four pairs of 45° bends and horizontally focusing quadrupoles before and after each bend doublet; vertical focusing is achieved only by the edge fields of the bends. The dipole field is 1 T at 0.5 GeV, the dipole radius is 1.67 m. The quadrupoles have a length of 0.12 m, a bore radius of 38 mm, and a maximum field gradient of 6 T/m. Figure 4 shows a photo of the injector and the layout. The booster synchrotron has a circumference of 26.4 m.

The acceleration in the booster synchrotron is achieved by a single-cell, 500 MHz, 200 W cavity. The electrons are extracted from the booster synchrotron by a slow bump and a fast kick. For injection into the storage ring the beam in the storage ring is deflected towards the storage ring septum by means of three kickers.

Figure 3: Layout and photo of the 53 MeV racetrack microtron

Figure 4: Layout and photo of the 500 MeV booster synchrotron.

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Storage ring optics


Design Injector Storage Ring Optics RF system Magnets Vacuum system Parameters Insertion Devices

The circumference of the storage ring is 110.4 m. The optics of the storage ring is an eight-fold DBA (Double Bend Achromat) with two types of long straight sections. The DBA optics consists of one focusing quadrupole between the two bending magnets of the achromat, and one quadrupole doublet upstream and downstream of the bends. The sextupoles are installed between the bends. Figure

Figure 5: The 2010-standard low-β optics of the ANKA storage ring (left) and the low-α optics (right).


Figure 6: Section of the storage ring at ANKA.

5 shows the 50 nm·rad optics for user operation at 2.5 GeV and the low-α optics for short bunches at 1.3 GeV.Figure 6 shows a photo of a sevtin of the storage ring.Figure 6 shows a photo of a sevtin of the storage ring.


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RF system

The electrons in the storage ring are accelerated by four 500 MHz ELETTRA-type cavities. The cavities have a shunt impedance of R = UC / 2PC = 3.4 MΩ. The cavities are powered by two 250 kW klystrons, with each klystron feeding two cavities.

The cavities are located in two of the short straight sections. A photo of one of the SR cavity stations and the booster cavity is shown in Figure 7 (the cavities in the storage ring have the same form but a more elaborate cooling and tuning system).

The storage ring cavities are tuned both by squeezing the cavity body and by changing the cavity temperature. This allows to select a setting at 2.5 GeV for which no higher order modes are excited. At injection energy (0.5 GeV), damping due to radiation emission is small, and thus higher modes are always present. The higher order modes cause instabilities and limit the maximum achievable current.A photo of the RF Sation is shown in Figure 8.

Figure 7: The ELETTRA-type cavity in the booster.

Figure 8: Storage ring RF station.

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Thema


Design Injector Storage Ring Optics RF system Magnets Vacuum system Parameters Insertion Devices

Sixteen identical dipole magnets are installed in the storage ring. The iron length is 2.13 m, the gap is 42 mm, the bending radius is 5.559 m and the nominal field is 1.5 T. Five families of quadrupoles are installed with 8 magnets each; all have the same pole profile with a bore radius of 35 mm. The central quadrupole in the achromat has a length of 0.355 m, all the others 0.285 m, the magnet field gradient is around dB/dr = 18 T/m. Two families of sextupoles are installed with 16 vertical and 8 horizontal focusing sextupoles. The sextupoles have an iron length of 120 mm and a magnetic strength of d2B/dr2 = 500 T/m2. Photographs of the storage ring dipole, quadrupole and sextupole are shown in Figure 9-11.

DIPOLE MAGNET

Number 16

Deflection angle degrees 22.5

Field strength T 1.5

Deflection radius m 5.559

Figure 9: The magnets of the storage ring : dipole magnet.

Magnets



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Figure 11: The magnets of the storage ring: sextupole magnet.

Figure 10: The magnets of the storage ring: quadrupole magnet.

qUADRUPOLE MAGNET

Number 32/8

Gradient 18 T/m2

Length 285/ 355 mm

SExTUPOL MAGNET

Number 24

2nd gradient 500 T/m2

Length 120 mm

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Thema

Vacuum System


Design Injector Storage Ring Optics Magnets RF System Vacuum System Parameters Insertion Devices

The vacuum system of the ANKA storage ring is made from nonmagnetic 316LN stainless steel. The electron beam chamber has an internal width of 70 mm and a height of 32 mm. At a current of 200 mA, a radiation power of 125 kW has to be absorbed. The corresponding gas load of 2·10-6 mbar l/s has to be pumped to maintain a pressure of 10-9 mbar or better.

The chambers in the dipoles and the adjacent multipoles downstream, which receive most of the power and gas load, have ante chambers

equipped with lumped absorbers. All other vacuum chambers have distributed absorbers along the outer side of the chamber.

Pumping is performed by diode ion pumps (500 l/s close to the lumped absorbers, 150 l/s elsewhere). In total pumps with a nominal pumping speed of 20 000 l/s are installed. Pictures of the dipole vacuum chamber and the lumped absorber are shown in figures 12 and 13.

Figure 12: Dipole vacuum chamber.


Figure 13: Two different absorbers.


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ParametersMain parameters of the accelerator at 2.5 GeV

Parameter

Circumference 110.4 m

Number of sections with Insertions 5

Photon critical energy 6.0 keV

Injection energy 0.5 GeV

End energy 2.5 GeV

Operating electron beam current 180 mA

RF-frequency 500 MHz

Relative energy spread 1 x 10-3

Momentum compaction factor 0.01

Horizontal emittance 50 nmrad

Horizontal working point 6.73

Vertical working point 2.69

Horizontal beta-function, min-max 0.8 – 15 m

Vertical beta-function, min-max 1.7 – 30 m

Port 5°, hor. beam size, divergence 0.3, 0.19 mm/mrad (rms)

Port 5°, vert. beam size, divergence 0.1, 0.01 mm/mrad (rms)

Port 11.25°, hor. beam size, divergence 0.2, 0.24 mm/mrad (rms)

Port 11.25°, vert. beam size, divergence 0.1, 0.01 mm/mrad (rms)

Straight section, hor. beam size, divergence 0.9, 0.06 mm/mrad (rms)

Straight section, vert. beam size, divergence 0.1, 0.01 mm/mrad (rms)

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Thema

Insertion Devices



Design Injector Storage Ring Optics Magnets RF System Vacuum System Parameters Insertion Devices

ANKA has 8 straight sections: 4 are about 4.5 m long and the other 4 about 1.5 m long. Two of the short straight sections are used for the RF cavities and one for beam injection from the booster to the storage ring. The remaining short and the 4 long straight sections can be used for insertion devices.The calculated photon flux of the dipole magnet and the installed insertion devices are given in Figure 14.Four insertion devices are installed at ANKA, the high field wiggler W74 for the SUL-X beamline (Figure 15), a 100 mm period length undulator U 100 for the WERa beamline (Figure 16) and two wigglers with 200 mm period length for the NaNO and IMaGE beamlines.

Figure 14: On axis flux density of the installed insertion devices in comparison with the one of the dipole magnet.

Figure 15: The planar permanent-magnet SUL-X wiggler W74 is used both as a source for the X-ray beamline of the SUL and as a damping wiggler for the ANKA storage ring. The SUL-X wiggler can increase the beam life time of ANKA by several hours at 2.5 GeV.

Figure 16: The planar, permanent magnet undulator U100, a loan of the National Synchrotron Radiation Research Center, Taiwan.

W200


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Parameters of the installed insertion devicesW200 (Loan from Daresbury Lab)

W74 (Accel)

U100 (Loan from NSRRC)

period length (mm) 200 74 100

B (T) 1.07 1.23 0.47

min. magn. gap (mm) 45 16 45

max. magn. gap (mm) 200 250 > 100

vacuum gap (mm) 32 11 32

magn. length (mm) 1078 2109 2074

number of full periods 4.5 27 20

K 19.98 8.50 4.39

tot. power (kW) 0.89 2.44 0.34

beamline NANO, IMAGE SUL WERA

Sara Casalbuoni: [email protected] +49 (0)721 82 28369Stefan Gerstl: [email protected] +49 (0)721 82 26955

Nicole Glamann: [email protected] +49-(0)721 82 26180Andreas Grau: [email protected] +49 (0)721 82 26170

Tomas Holubek: [email protected] +49 (0)721 82 26004David Saez de Jauregui: [email protected] +49 (0)721 82 28193

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ANKA Control System


ANKA Control System

PVSS at aNKa

16

Beamlines User Service Commercial Services

can easily write their own macros or modify the provided standard macros to meet their particular needs. To control the various beamline components, VME-bus as well as GPIB-bus and TCP/IP are used. Since ANKA is migrating for beamline control to TANGO (see tango-controls.org), the communication between the different control systems as spec and WinCC OA is fully TANGO-based and also all new implemented devices are controlled via TANGO device servers (Fig. 2). The beamline control of the optics section is done via WinCC OA. All access to valves, absorbers and cooling is controlled and supervised by the S7 programmable logic controller (PLC), protecting the beamline components and the vacuum of the ANKA storage ring. The distributed structure of WinCC OA allows to control the beamline via LAN wherever required.

The personnel safety at the beamlines (BPSS) is guaranteed by an independent, fail-safe, three-processor PSS3100 PLC, which controls the status of all radiation shutters and the doors of the lead hutches. The safety system is also connected to the machine safety relay and triggers the RF-shutdown in the case of an emergency beam dump request from a beamline. The system safety hard- and software is certified. The BPSS control cabinet is located at each beamline and controls the status and error state of all safety components of a beamline. All beamline PSS3100 PLCs are connected via a safety bus to the central PSS3100 cabinet in the ANKA control room. The BPSS status is given to the user in a WinCC OA window on the beamline PC.

aNKa Control systemPVSS at aNKa

ANKA Control SystemAccelerator /

Insertion Devices

As Supervisory Control and Data Acquisition System (SCADA) for ANKA, WinCC Open Architecture (preliminary PVSS-II) is used, integrating most of the individual sub-control systems (Figure 1). WinCC OA runs under Windows and Linux. It is completely event driven with a central event manager and it allows connection of a variety of industrial devices with interfaces like OPC, SNMP and also field busses. All managers and drivers talk via TCP/IP with the central event manager, so the system can be distributed over as many systems as needed. The open C++ application interface (API) allows of own managers and drivers. WinCC OA allows virtually unlimited number of variables, the entire internal database can be stored into an ASCII file, easily be modified and re-imported. All control structures and data points can be updated on-line without stopping the system. A powerful ANSI-C like scripting language is used to adapt WinCC OA.

Accelerator ControlTo pave the way for a 100-fold increase in devices that communicate over TCP/IP a completely 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 increased the reliability of the control system substantially, but also offered much more in beam diagnostics, such as first turn read-out, turn-by-turn readout and a 10kHz fast feedback read out of the beam position. These new devices, along with the ageing old ACS control system, motivated a decision to move to a completely new control system (EPICS).

One challenge of the new BPM electronics was to move the control system high-level client for orbit correction to accept an EPIC connection instead of the old ACS while still allowing at the same time to control the corrector magnets that remained in the old control system. This was achieved by developing a software gateway that would allow EPICS clients to transparently access process variables in the ACS 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 was developed with EPICS and the graphical user interface CSS 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.

Beamline ControlThe command-line-based control environment ‘spec’ is the heart of the beamline experiment control. The measurement logic of spec is coded in macros using a C-like language. Thus, individual users

Storage Ring Control (EPIC)

Radiation Monito- ring System

Storage Ring Interlock (PLC)

Beamline Personnel Safety System (Pilz)

Cooling, Air Conditioning

Insertion Devices

Infrastructure Facilities

TCP / IP

RF Control

Beamline Control

Experiment Control(spec)

Figure 1: Status of Integration of the different control systems into WinCC OA.

WinCC OA


Commercial ServicesWolfgang Mexner: [email protected] +49 (0)721 608 26189

Hotline +49 (0)721 608 26614

Figure 2: Beamline control.

CONtaCt

WinCC OA

WinCC OAVME- Crate

Counter

Stepper

Fieldbus TANGO Server

RS232

Experiment I/O

Stepper

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Beamlines


Beamlines at ANKA

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ANKA Control System User Service Commercial Services

Beamlines at aNKaIntroduction and overview

Beamlines at anka

Beamlines

A description of present and planned ANKA beamlines is given in this chapter. It contains information about their primary applications, methods, instrumentation and planned upgrades. The beamlines are subdivided into spectroscopy beamlines, scattering and imaging beamlines, and microfabrication beamlines.

A summary of the beamlines with some key parameters and their experimental stations is listed in the following tables. Technical details of present and planned beamlines are described. Additional data, such as flux and characteristics of the beamline optics, will be presented separately in the beamline chapters.


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BEAMLINE TECHNICAL APPLICATION

ExPERIMENTAL STATION RANGE AND RESOLUTION SOURCE STATUS

FLUO x-ray fluorescence(xRF), x-rayfluorescence micropro-be (μ-xRF), total x-rayreflection fluorescence(TxRF)

Vacuum chamber, SiLi-detector

Energy range: 1-30 keVResolution: ∆E/E= 2x10-2

Dipole magnet

Operational

XaS Extended x-rayabsorption fine struc-ture (ExAFS), x-ray absorption near-edge fine structure (xANES), q-ExAFS

Ionization chambers, 5 element Ge detector, closed cycle He cryostat, 4 axis goniometer for GI-xAFS

Energy range: 2.4-27 keV

Dipole magnet

Operational

INE Spectroscopy of actin-ide samples; multiple spectroscopy micros-copy and diffraction methods(ExAFS, xES, xRD, μ-spectroscopy)

Ionization chambers, 5 element Ge detector, 4 axis goniometer for GI-xAFS, liquid N2 cryostat Vortex silicon drift detector

Energy range: 2.1-25 keVResolution: ∆E/E= 2x10-4

Dipole magnet

Operational

SUL-X x-ray diffraction (xRD),x-ray-Fluorescence (xRF) and x-ray absorp-tion in μ-focus

Vacuum chamber, ioniza-tion chambers, 7 element SiLi-detector, 4 axis diffrac-tometer + CCD detector

Energy range: 2.14-20 keVResolution: E∆/E= 2x10-4

(for Si(111) crystals)

Wiggler Operational

WERa Soft x-ray spectroscopy,microscopy, andspectromicroscopy:PES, NExAFS, xMCD,imaging (PEEM);μ-PES, μ-NExAFS,μ-xMCD

3 experimental chambers w/ associated preparation cham-bers, all UHV. PEEM, electron energy analyzer, fluorescence detector, LHe cryostats, UHV sample transfer

Energy range: 100-1500 eVResolution: E/∆E: 2x104

Dipole magnet

Operational

IR1 Infrared/THz spec-troscopy and ellipso-metry

FTIR spectrometer, ellipso-meter, liquid He cryostat

Spectral range: 4-10000 cm-1

Best spectral resolution: 0.1 cm-1

Dipole magnet edge

Operational

IR2 Infrared/THz, spec-troscopy, microspec-troscopy, imaging and near-field nanospec-troscopy

FTIR spectrometer, IR microscope, IR nanoscope, liquid He cryostat

Spectral range: 4-10000 cm-1

Best spectral resolution: 0.1 cm-1

Lateral resolution: diffraction limited (microscopy), 100-1000x beyond the diffraction limit

Dipole magnet edge

Operational

UV-CD12 VUV / UV circulardichroism spectroscopy,oriented circular dichroism (OCD)

Modular CD spectropola-rimeter, N2-purged sample chambers for liquid and solid-state samples

Spectral range: 120-350 nmWavelength resolution: 0.5-2.0 nm

Dipole magnet

Operational

Spectroscopy Beamlines

22



Beamlines



PDIFF x-ray powder diffrac-tion (xRPD), Rönt-genography, sing-le-crystal diffraction

4+2 circle diffractometer Energy range: 6-20 keVResolution: ∆E/E= 2x10-4

Dipole magnet

Operational

SCD Single crystal diffraction, single/multiple anoma-lous dispersion (SAD/MAD)

3 axis diffractometer w/ CCD detector and 2 axis diffractometer w/ ima-ge plate detector, 6 axis diffractometer w/ Nal point detector

Energy range: 4-20 keVResolution: ∆E/E= 3.5x10-4

Dipole magnet

Operational

NaNO x-ray diffraction (HR-xRD) with highest angular resolution, anomalous scattering, coherent scattering

Multi-purpose heavy-duty diffractometer; different growth chambers; cryostat; furnace

Energy range: 3-25 keVResolution: ∆E/E=10-4 to 10-2

Wiggler In Commissioning

MPI-MF (MPG)

Surface diffraction, xMCD

2+3 circle horizontal and vertical diffractometer for high load (300 kg)

Energy range: 5-20 keVResolution: ∆E/E= 2x10-4

Dipole magnet

Operational

IMaGE Radiography, tomo-graphy

Ultra-precise samplemanipulator; automatic sample changer system.2D detector system; energy-dispersive detector

Energy range: 7 - 65 keVResolution: ∆E/E= 10-2 to 10-4

Wiggler In Construction

tOPO- tOMO

Topography, Tomogra-phy, Radiography

4 axis goniometer, tomogra-phy stages, stages for 300 mm wafer

White beam,optional ∆E/E= 10-2

Dipole magnet

Operational



LIGa I Mask fabrication,patterning of thinmicrostructures,thin film x-ray litho-graphy

Scanner Energy range:2.2 – 3.3 keV

Dipole magnet

Operational

LIGa II Deep x-ray lithography Scanner Energy range:2.5 – 12.4 keV

Dipole magnet

Operational

LIGa III Ultra-deep x-raylithography

Scanner Energy range: 2.5 – 15.0 keV

Dipole magnet

In Commissioning

Scattering and Imaging Beamlines

Micro-Fabrication Beamlines

Beamlines at anka


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89

Legend for the schematic beamline layouts presented in the beamline description

Legend for the schematic beamline layouts presented in the beamline description

Bending magnet

Superconducting insertion device

Mirror

Double crystal monochromator

Multilayer - monochromator

Slits | aperture

Be window

Attenuator

X - ray Lens

Ionization Chamber

CCD Detector | Image Plate

Point Detector

Pin Diode

Fluorescence Detector (Si (Li), Ge)

Light Microscope

Vacuum Chamber

Sample Environment

In the following, the beamlines at ANKA will be presented with their main parameters, experimental capabilities and selected examples of research. The simplified beamline layouts use the following symbols for individual optical and experimental elements:


ContaCt

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 fpr synchrotron circular dichroism spectroscopy

WERaSoft x-ray analysis facility

XaSX-ray absorption spectroscopy beamline

26



Scientific applications x-ray Fluorescence Analysis is a well-established multi-element technique, capable of yielding accurate quantitative information on the elemental composition of materials. Synchrotron radiation x-ray fluorescence analysis (SR-xRF) is one of the few methods which offer sub-femtogram and sub-ppm levels of detectability, combined with a completely non-destructive manner of probing and a high level of accuracy. The high degree of linear polarization, combined with the high intensity of synchrotron radiation, can be effectively used to perform trace-level microanalysis.In general, the xRF technique does not require elaborate sample preparation: the sample can be used in its original state, without destruction by the measurement process. This is an important advantage of the method for analysis of precious works of art, as well as for many environmental and biological samples. Besides detailed information about chemical composition and trace element concentrations, (microprobe) xRF can also yield valuable information

about spatial elemental distribution.An important application of µ-xRF is the study of small particles, where the arrangement of phases and subclusters can be correlated to the processes of creation, alteration and ageing. For example, the analysis of radioactive environmental particles is yielding forensic information on nuclear accidents or nuclear weapon testing. A further example of small particles with tell-tale phase composition are geological tectites, such as meteor impact ejecta.

Spatial information is very important for accessing the bioavailability and thus the hazard potential of toxic or volatile elements in environmental sediments and soils. Using spatially resolved µxRF, toxic element bearing mineral phases can be identified and potential structure-related mobilization processes can be studied. Examples are arsenic bearing silicates in aquifer sediments (Bengal) and uranium in tertiary sediments as model systems for waste disposal.

Materials science applications such as the specification and localization of contaminants in high purity materials, or the homogeneity of alloys or thin films on µm length scales, benefit primarily from the high sensitivity and accuracy of SR-xRF.


Spectroscopy

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

FLUO is a beamline dedicated to X-ray fluorescence analysis. It is situated at a dipole magnet source.

BeamlinesFLUO | INE | IR1 | IR2 | SUL-x | UV-CD12 | WERA | xAS | MPI-MF | NANO | PDIFF | SCD | IMAGE | TOPO-TOMO | LIGA I, II, III

Figure 1: Schematic layout of the FLUO beamline.


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Figure 2: Experimental station for XRF: Ionisation chamber, lens stage, beam monitor, microscope, x-ray detector, sample stage and transmission monitor (from right to left).

CONtaCt

Rolf Simon: [email protected] +49 (0)721 608 26174David Batchelor: [email protected] +49 (0)721 608 28675

Ralf Lang: [email protected] +49 (0)721 608 23431Beamline +49 (0)721 608 26307

Available methodsx-Ray fluorescence microprobe (µ-xRF): This technique confines the analytical region of the sample being analyzed to a microscopically small area on the surface or even to a small volume element in the bulk. Resolution in the µm range can be attained.

Confocal x-ray fluorescence Microprobe: A method for obtaining three dimensional elemental distribution on a micrometer scale. In confocal µ-xRF, a (polycapillary) lens is placed in front of the detector, confining its field of view. This very flexible method allows the recording of elemental maps at different depth levels below the surface with a depth resolution of about 10-20 µm.

Total reflection x-ray fluorescence (TxRF): TxRF is the surface-sensitive variant of x-ray fluorescence analysis that is used either to detect trace impurities on the surface of flat samples (e.g. silicon wafers) or to analyze very small sample masses deposited on a polished substrate. Detection limits as low as 108 atoms/cm2 can be achieved.

Tomographic µ-xRF:A method for obtaining three-dimensional elemental distribution with resolution of a few micrometer. By using a CCD area detector and/or monitoring the transmitted beam, x-ray powder diffraction tomography and transmission tomography can be performed simultaneously, yielding complementary data.

Figure 3a: Compound refractive lens manufactured by LIGA (IMT).

Figure 3b: Micro-XRF setup (confocal).

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Spectroscopy


Key parameters of the beamlineEnergy range

1.5 keV - 33 keV

Energy resolution [∆E/E] 1.2x10-2 or white light

Source 1.5 T Bending magnet (EC = 6 keV)

Optics Double multilayer monochromator with W-Si multilayers in 2.7 nm period focusing optics: Compound refractive lenses, Poly-capillaries, Fresnel zone plate

Flux at samle postion Poly-capillary: 1x1011 ph/s @17 keV (12 µm x 12 µm)CRL: 2x109 ph/s @ 17 keV (5 µm x 2 µm)

Beam size at sample 5 mm (Hor) x 2 mm (Ver) down to 2 µm x 1 µm

Experimental setup/ sample environment

Air

Experimental setup/ detectors

1 Ionisation chamber, 2 PIN-diodes for monitoring

Software/ Data treatment/ Evaluation

SPEC, AxIL, Spectran, MC-simulation (MSIM), newplot, PyMca, xRDUA


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CONtaCt

Rolf Simon: [email protected] +49 (0)721 608 26174David Batchelor: [email protected] +49 (0)721 608 28675


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INEBeamline for actinide research

Spectroscopy

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

The INE-Beamline at ANKA is dedicated to actinide research with emphasis on X-ray spectroscopic techniques. It has been constructed and is operated by the Institute for Nuclear Waste Disposal (INE) at the KIT Campus North. Investigations on non-fissile radioisotopes up to 106 times the limit of exemption and fissile radioisotopes (Pu-239, U-235) up to 200 mg, contained within two layers of protection, are possible. 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.

Scientific applicationsResearch and development at INE is largely aimed at long-term safety assessment of proposed deep geological repositories for high-level, heat-producing nuclear waste disposal. To ensure sound safety assessment, a molecular understanding of processes determinant in the fate of radionuclides, notably the actinides, and their thermodynamic quantification is essential. Of central importance in such investigations is actinide speciation, or the actinide’s molecular, chemical and physical form. Actinide speciation determines transport properties (mobilization / immobilization), reactivity, bio-availability and, hence, their potential human and environmental risk. x-ray spectroscopic methods have proved to be valuable tools for actinide speciation research at INE, providing information on the coordination and redox chemistry of actinide cations, e.g., sorbed onto surfaces (e.g., at the mineral - water interface), occluded or included into the structure of precipitates, colloids, and secondary phases, as well as into glass and spent fuel and their corrosion products.

The INE-Beamline is used by many European groups for similar and various other applied and basic science investigations. The INE-Beamline is a pooled facility of the EU FP-7 project TALISMAN, follow-up of the ACTINET-I3 initiative.

Available methods, information contentStandard methods with monochromatic beamxAFS: characterization of bulk speciesxAFS / xRD: characterization of phase - pair distribution relationshipsTEY / FluoxAFS: for non transmission / low concentration experiments

Surface sensitive with grazing incidence (GI) techniquesGI-xAFS: characterization of surface sorbed speciesGI-xRD: identification of secondary phases on surfacesx-ray reflectivity: determination of surface layer thickness and roughnessStanding wave: characterization of atomic positions at surfaces

Spatial resolution with focused beam for “micro” techniquesµ-xAFS: chemical state imagingµ-xRF: elemental mappingµ-xRD: identification and distribution mapping of phases

Energy resolution with secondary monochromator (Johann spectrometer)HRxES: high resolution x-ray emission spectroscopyRIxS: resonant inelastic x-ray scattering

Combination of x-ray methods, e.g., xAFS / xRD, or x-ray methods with other techniques, e.g., laser spectroscopy, Raman spectroscopy, UV-Vis is possible.



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Figure 1: INE-Beamline – layout of optics and experimental stage.

Figure 2: Lemonnier-type DCM, built in cooperation with Bonn University (Physikalisches Institut).

Figure 3: Digitized beam intensity 3D view, profiles and camera output obtained with the single bounce capillary (IFG Berlin, Germany). Beam dimensions at 18.5 keV: FWHM 33 µm horizontal and 37 µm vertical.

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Kathy Dardenne: [email protected] +49 (0)721 608 26669 Nicolas Finck: [email protected] +49 (0)721 608 24321

Jörg Rothe: [email protected] +49 (0)721 608 24390Tonya Vitova: [email protected] +49 (0)721 608 24024

INE-Beamline +49 (0)721 608 28295

32



Spectroscopy

Instrumental characteristics The necessary infrastructure and safety equipment is available at the INE-Beamline for radioactive experiments. The available energy range at the INE-Beamline covers the K-edges from P (2.1 keV) to Pd (25 keV), including the L-edges of lanthanide elements and the lighter actinide elements (up to the Cf L3-edge).

The double crystal monochromator (DCM) design has a mechanically coupled movement of the second crystal while scanning the Bragg angle (Θ), enabling a fast fixed exit mode for quick-xAFS studies. Four pairs of DCM crystals are presently available, InSb(111), Si(111), Si(311), and Ge(422). The beamline optics include collimating and focusing Rh coated silicon mirrors for a ~500 µm × 500 µm beam spot at the sample position.

The instrumentation at the INE-Beamline is continuously improved and additions made to meet the demands of the user community. In the recent past, for example, specialized sample environments including

an electrochemical cell for in-situ redox-studies and a cell enabling high-T / pressure measurements were developed and commissioned. Microfocus options are now available for spatially resolved xRF, xAFS and xRD investigations using a focused x-ray beam with micrometer dimensions. Poly-capillary half-lenses, delivering a focused beam of ~25 µm in diameter and a single-bounce capillary (SBC) for ~35 µm in diameter (both IfG, Germany), are available. The SBC is specifically designed to adapt to the high horizontal divergence of the beam. Therewith, combined µ-xRD and µ-xAFS investigations are possible.

Figure 4: Photos of the multi-analyzer crystal spectrometer (MAC-Spectrometer) installed at the INE-Beamline.


INE


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Figure 5: The U L3 edge high-energy resolution X-ray absorption near edge (HR-XANES) spectrum of metastudtite measured 30 (black)/180 minutes (red) , and the conventional transmission mode XANES spectrum for measured simultaneously (green).

Figure 6 (left): Electrochemical cell in use at the INE-Beamline (left) during the measurement of an in-situ redox reaction of 237-Np. (right): Np L3 XANES spectra recorded at different stabilized oxidation states of Np.

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INE-Beamline +49 (0)721 608 28295

34



Spectroscopy

Beamlines

Key parameters of the INE beamline

Energy range2.1 keV - 25 keV (P to Pd K-edges, actinides up to the Cf L3-edge)

Flux ~ 2x1010 photons / sec at Zr K- / Pu L3-edges using Ge(422)

Source 1.5 T bending magnet (EC = 6 keV)

Optics Double crystal monochromator, water-cooled first crystal, mechanically coupled movement of the Second crystal to ensure fixed exit, D-MOSTAB, exchangeable crystal pairs InSb(111), Si(111), Si(311), Ge(422) Rh coated silicon mirrors (focusing, collimating) for a ~500 µm × 500 µm beam spot at sample position, SES X-ray beam position monitor, Optical microscope Microfocus options available:Poly-capillary half lenses, focused beam of ~ 25 µm in diameter (IfG, Germany)Single-bounce capillary, focused beam of ~35 µm in diameter (IfG, Germany)

Experimental setup / sample positioning

Standard sample holders for radioactive samples, other dimensions can be accommodated High precision HUBER sample positioning system, goniometer cradles, and auxiliary slits for both standard XAFS and surface sensitive grazing incidence techniquesHexapod (PI) for positioning of secondary focusing optics Heavy load hexapod (PI) for positioning of Johann spectrometer or other heavy equipmentLN2 cryostat (OI OptistatDN) for low temperature measurements1.2 x 3 m2 breadboard optical table Sealed media feed-through chicanes and separate ventilation / filter system for experimental hutchAccess through lock-room with hand / foot-contamination monitor

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


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Upgrades at the INE-beamline

The setup for confocal µ-xAFS and µ-xRF measurements based on polycapillary half-lenses was completed by integrating a new x/y/z-stage, which allows precise positioning of the silicon drift fluorescence detector (SDD) relative to the primary focus. All components (primary capillary hexapod positioning system, sample stage, detector stage, visible light microscope) were integrated and tested in the confocal geometry (Fig. 7a). The first 3D reconstitution of the uranium distribution in a uranium rich sediment based on confocal measurement at different depths is shown in (Fig. 7b). The microfocus setup is available for general user operation since ANKA Call 16 (Oct. 2010 – Mar. 2011) and the confocal setup is available for general user operation since call 21 (Apr. 2013 - Sep. 2013).

A major upgrade presently underway is the testing of a HRxF spectrometer using the multi analyser crystal spectrometer shown Fig. 4. This spectrometer provides wavelength dispersion of the emitted photon energies from a sample excited by incident x-rays and focuses them onto a position sensitive detector, e.g., a CCD camera. It can be used to remove lifetime broadening by registering the partial fluorescence yield emitted by the sample (i.e., recording a windowed signal from the energy-dispersed fluorescence emission while varying incident photon energy), thereby yielding highly resolved xAFS spectra, which often display resonant features not observed in conventional xAFS. The spectrometer can also be used for a wide range of other experiments, for example, resonant inelastic x-ray scattering (RIxS), which can be used to obtain bulk electron configuration information, valence-selective xAFS studies, where differences in local structure of an element present in mixed valence states can be studied, as well as site-selective xAFS studies, where the coordination structure of a metal bound to selected elements can be differentiated from that of all the other metal atoms.

Figure 7a: 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)

Figure 7b: 3D U distribution in contaminated sludge sample (scales in µm)

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INE-Beamline +49 (0)721 608 28295

36



IR1Infrared beamline for spectroscopy and ellipsometry

Spectroscopy

Scientific applications Infrared spectroscopy in general covers a huge range of scientific fields: chemistry, physics, biology, astronomy, geology, environment, nanoscience, materials research, forensic science, etc. IR 1 focuses especially on the strategic fields of the Institute for Photon Science and Synchrotron Radiation (e.g, condensed matter and materials research, nano technology, earth and environmental research, synchrotron technology). At the same time IR1 remains open for excellent user science from all fields of research.

As an infrared source, synchrotron radiation has five major advantages compared to conventional (black-body) laboratory sources:

• broader spectral range: continuous from far-IR to the visible • higher photon flux in the far-IR• higher brilliance: as it is almost a point source the light can be

focused down to a diffraction-limited size with a gain of up to 3 orders of magnitude in signal-to-noise

• pulsed source: the light is emitted from electron bunches, which allows fast time-resolved measurements (2 ns repetition rate, 150 ps pulse duration)

• intense coherent emission in the lower energy part of the far-IR / THz, with gain up to 105 compared to conventional synchrotron emission and with sub-ps pulse duration

Nowadays extraction of infrared radiation is part of almost all development programs in existing or planned synchrotron facilities. In parallel to the experimental applications of synchrotron infrared spectroscopy, a constant effort is in progress to investigate the fundamental properties of the radiation emitted in the IR/THz range. IR1 exploits the so-called edge radiation as the source (rather than classical synchrotron emission). Since this concept is now being adopted by other synchrotrons, ANKA’s efforts to derive an experimentally verified theoretical description are being followed with great interest by the relevant research community.

Current projects include accelerator-based IR-source development, studies of high-Tc superconducting materials, structural organization at the electrode-liquid interface and behavior of matter at extreme

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

IR 1 is an infrared beamline, it exploits the so-called edge radiation as the source rather than classical synchrotron emission.

Figure 3: The ellipsometric assembly at IR1.

Figure 2: Schematic principle of an ellipsometry experiment.

Figure 1: Layout of the IR1 beamline.



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pressure.

Available methods, obtainable parameters• IR spectroscopy in transmission, reflection, attenuated total

reflectance • IR ellipsometry

The ellipsometer (supplied by MPI-FKF, Stuttgart) is coupled to an FTIR spectrometer (Bruker IFS 66v/S) covering a spectral range from 4 to 10,000 cm-1 (0.5 meV to 1.24 eV, 2.5 mm to 1 μm) with a resolution down to 0.1 cm-1. It is equipped with high-sensitivity detectors [liquid-He cooled bolometers, liquid-N2 cooled MCT (HgCdTe) and InSb detectors, and Si or Ge diodes] and appropriate beamsplitters (Mylar films, multilayer, KBr and quartz). The instruments are evacuated or N2 purged to avoid water and CO2 absorption bands. The ellipsometer operates under vacuum and is provided with an optimized bolometer detector and a liquid He cryostat.

Ellipsometry is a technique which allows one to measure the complex dielectric function ε = ε1 + i ε2 of a given material very accurately and with high reproducibility. It measures the change in polarization of light upon non-normal reflection on the surface of a sample. The ellipsometry experiment set-up is shown in Figure 3. Unlike conventional reflection techniques, ellipsometry requires no reference measurement and no extrapolation of the reflectivity towards zero and infinite energy. This makes ellipsometry measurements more accurate and more reproducible than conventional reflection measurements.

Instrumental characteristics

Source, beam extraction and tranSport

Source Entrance edge of a bending magnet

Photon beam di-vergence

45 mrad (hor) x 15 mrad (vert)

Optics (extraction and trans-

port)

Mirror M1 plane made of beryllium, M2 toroid, CVD diamond window, M3 toroid, M4 planar, M5/M’5 planar

Photon flux (calcula-ted )

> 1013 photons/s/0.1% bw

ir ellipSometry Station

IR spectrometer Bruker IFS 66v/S

Typical beam diameter ≤ 1 mm

Wavelength range 2.5 mm - 1 μm

Energy range 4 – 10,000 cm-1 (0.5 meV – 1.24 eV)

Energy resolution > 0.1 cm-1

Beamsplitters Mylar 125 µm, 50 µm, 25 µm, Si/Mylar, KBr, quartz

Detectors Bolometer 1.8 K, bolometer 4.2 K, DTGS PE, MCT, DT-LaGS, InSb, Si diode

Software / data evaluation

OPUS, Origin, Igor Pro, CytoSpec

IR ellipsometer MPI-FKF custom made

Wavelength range 1 mm – 1 μm


Compensator without or with Si, ZnSe

Incidence angle 45 – 90°

Cryostat temperature range

8 – 500 K

Yves-Laurent Mathis: [email protected] +49 (0)721 608 26756David Moss: [email protected] +49 (0)721 608 22689

Biliana Gasharova: [email protected] +49 (0)721 608 26178Michael Süpfle:[email protected] +49 (0)721 608 28371

Beamline +49 (0)721 608 26724

38

Accelerator / Insertion Devices User Service Commercial Services

ANKA control system

IR2Infrared beamline for microspectroscopy and nanospectroscopy

Spectroscopy

FLUO | xAS | INE | SUL-x | WERA | IR1 | IR2 | UVCD-CD12 | PDIFF | SCD | NANO | MPI-MF | TOPO-TOMO | IMAGE | LIGA I, II, III

Scientific applications Techniques:IR spectroscopy, microspectroscopy and nanospectroscopy from far-IR to near-IR in transmission, normal or grazing incidence reflection, and attenuated total reflectance geometries.

Available methods, obtainable parameters IR2 is an edge radiation beamline based on design of IR1. Based on the experience with the operation of IR1, improvements in the design of IR2 have been made. Instead of a single diamond window, a window changer has been introduced with four windows optimized for the different spectral regions. Photon beam position instabilities will be corrected by a fast feedback system.

IR microscopy in combination with synchrotron infrared light allows diffraction-limited lateral resolution (ca. 3-10 micrometers in the mid IR), which is superior to the one achieved with conventional broadband sources. The FTIR spectrometer (Bruker IFS 66v/S) covering a spectral range from 4 to 10,000 cm-1 (0.5 meV to 1.24 eV, 2.5 mm to 1 μm) with a resolution down to 0.1 cm-1, is connected to an infrared microscope restricted to the domain 100-10,000 cm-1 (due to diffraction at lower

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

IR2 is a multipurpose IR/THz beamline dedicated to studies at micrometric and nanometric lateral resolution in condensed matter and materials research, nano science, geo and planetary sciences, environment, bio sciences and synchrotron technology.

Figure 2: Layout of the IR2 beamline.

Figure 1: IR microscope.

Beamlines

wavenumbers). It is equipped with a single-element liquid-N2 cooled MCT or a InSb 64x64 focal plane array imaging detector and a 4.2K bolometer. To avoid interference due to water and CO2 absorption bands, it is dry-N2 purged. Different objectives are available for transmission and reflection measurements. For sample positioning and mapping, a motorized stage with 1 μm resolution is used. Sample location and observation using fluorescence in the visible is possible. Samples can be studied in different environments (high temperature, low temperature, high pressure and fluids).

IR nanoscopy in combination with the brilliant synchrotron broadband infrared light of ANKA will allow spectroscopic imaging in the complete IR/THz spectral range of objects much smaller than the wavelength of the radiation used. The technique overcomes the diffraction limit by using the near field of a metal antenna in close proximity to the scanned sample surface. In 2007 Prof. Martina Havenith from the Ruhr University of Bochum was awarded a major BMBF research grant for the development of a near-field infrared nanoscope for imaging at sub-wavelength spatial resolution using synchrotron light at ANKA. Vertex 80v Bruker FTIR spectrometer and an Alpha300R WiTec AFM will constitute the heart of the new device.



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Source, beam extraction and tranSport

Source Entrance edge of a bending magnet

Photon beam di-vergence

45 mrad (hor) x 15 mrad (vert)

Optics (extraction and trans-

port)

Mirror M1 planar made of beryllium, M2 toroid, M3 to-roid, M4 planar, M5abcd planar, CVD diamond/z-cut quartz/CsI/BaF2 window changer, M6abcd planar, M7 toroid, M8 toroid, M9 planar piezo driven, M10 planar dichroic, M11 planar piezo driven, M12 planar dichroic

Photon flux (calculated ) > 1013 photons/s/0.1% bw

ir microScopy Station

IR spectrometer Bruker IFS 66v/S


Wavelength range 2.5 mm - 1 μm



Beamsplitters Mylar 50 µm, 6 µm, Si/Mylar 6 µm, KBr, CaF2

Detectors Bolometer 1.8 K, bolometer 4.2 K, DTGS PE, MCT, DT-LaGS, InSb, Si diode

Software / data evalua-tion

OPUS, Igor Pro, CytoSpec

IR microscope Bruker IRscope II

Typical beam diameter ~ 5 μm

Spatial resolution Diffraction limited (~ ½ wavelength)

Wavelength range 100 μm -1 μm


Objectives For IR: 15x and 36x Schwarz-schild, grazing incidence, ATR (Ge and Si)For VIS: 4x, 20x, 40x, 100x

Detectors Bolometer 4.2 K, MCT, FPA 64 x 64 pixels, InSb

ir nanoScopy experimental Station

IR spectrometer Bruker Vertex 80v


Wavelength range 2.5 mm – 1 μm



Beamsplitters Mylar 50 µm, 23 µm, Si/Mylar 6 µm, KBr

Detectors Bolometer 1.8 K, bolometer 4.2 K, DTGS PE, MCT, DTLaGS

Software / Data treat-ment /

Evaluation

OPUS, Igor Pro, CytoSpec, WITec project

IR nanoscope WITec AFM

Figure 1: IR microscope.

Yves-Laurent Mathis: [email protected] +49 (0)721 608 26756David Moss: [email protected] +49 (0)721 608 22689

Biliana Gasharova: [email protected] +49 (0)721 608 26178Michael Süpfle:[email protected] +49 (0)721 608 28371

Beamline +49 (0)721 608 26724

40



SUL-XX-ray beamline for environmental research

Spectroscopy

Scientific applicationsEnvironmental samples are generally complex (e.g., contaminated soils, mining dump sediments), consisting of mixtures of mineral phases (amorphous, crystalline, with micrometer or nano-scale particle sizes), microbes, and in some cases organic material. Spatial distribution, speciation, and phase association of trace levels of contaminants are the basis for risk assessment and development of remediation strategies (e.g., arsenic speciation and distribution in groundwater-related sediments). The SUL-x beamline addresses these issues by providing spatial resolution in the micrometer range with a combination of micro-focused techniques (x-ray fluorescence spectroscopy: xRF; x-ray absorption spectroscopy: xAS; x-ray diffraction: xRD).

The design of SUL-x was developed on the needs of national and international user groups from the environmental science community. Together with a facility for IR microspectroscopy, it forms the major part of the federal- and state-funded ‘Synchrotron Radiation Laboratory for Environmental Studies’ (SUL) at ANKA. With the advantages of its concept of combined experimental methods, the SUL laboratory will also benefit proposals from other research fields (e.g., material science, biology, health research).

The research is assigned mainly to molecular environmental science (MES), an emerging field that involves studies of chemical and biological processes affecting speciation, properties, behavior of contaminants, pollutants, and nutrients in the ecosphere. Synchrotron based techniques are fundamental for MES. A major driving force is the need to characterize, treat, and/or dispose of vast quantities of contaminated materials, including groundwater, sediments, and soils, and to process wastes. Besides high-level nuclear waste significant contributions come from mining and industrial wastes, atmospheric pollutants, etc., all of which have major impacts on human health and welfare. Addressing these problems requires the development of new characterization and processing technologies – efforts that require information on the chemical speciation of heavy metals, radionuclides, and xenobiotic organic compounds and their reactions with environmental materials.

Available methods, obtainable parametersThe SUL-x beamline closes the spectral gap between soft and hard x-ray spectroscopy, and allows to investigate samples – without remounting them – sequentially with the following methods and modes:

xRF: x-ray fluorescence spectroscopy xAS: x-ray absorption spectroscopy (2.14 keV up to 20 keV for P K-edge

to U L-edge)xRD: x-ray diffraction with adjustable beam size

Fluorescence spectroscopy with a microfocused beam enables elemental mapping of an extended sample (e.g., thin or polished sections of a contaminated soil sample).The wide energy range allows absorption spectroscopy for elements between P and U. xAS provides essential information about the local atomic geometry (ExAFS) and of the chemical state of the absorbing atom (xANES). It can be applied equally to investigate both ordered (crystalline) and disordered (amorphous, liquid) materials. Dilute species and light elements can be measured in fluorescence mode.x-ray diffraction measurements (e.g., of powder, aggregates of crystals, or laterally resolved on sample sections in transmission) enable the identification of mineral phases and correlations with pollutants to be found.

Adjustable beam dimensions in combination with automated sample-positioning and a diffractometer allow the investigation of distribution and chemical states of elements and their associations to mineral phases down to the µm scale, essential key parameters for environmental and health risk assessment.

Beamlines

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

SUL-X is an X-ray beamline for combined absorption, fluorescence, and diffraction measurements on environmentally relevant materials using a wiggler as source.

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


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Figure 1: Schematic layout of the SUL-X beamline.

CONtaCt

Ralph Steininger: [email protected] +49 (0)721 608 26173Jörg Göttlicher: [email protected] +49 (0)721 608 26070

Harald Zöller: [email protected] +49 (0)721 608 23329Wolfgang Möck: [email protected] +49 (0)721 608 28370

Beamline +49 (0)721 608 28293

42



Spectroscopy

Instrumental Characteristics On the basis of the performance specifications provided by the SUL user community, the SUL-x beamline has been set up to cover a wide energy range combining x-ray absorption spectroscopy, x-ray fluorescence analysis and x-ray diffraction, preferably using a microfocused beam. The main optical elements and calculated key parameters of the beamline are:

Beamlines

Key parameters of the BeamlineEnergy rang 2.14 keV – 20 keV (P K-edge up to U L-edge)

Energy resolution [∆E/E] Si(111) 2x10-4; Si(311) 1x10-4 (given resolutions are theoretical values)

Source Wiggler (27 pole, 74 mm)

Optics (from source towards experiment)

Toroidal mirror, horizontally focusing, vertically collimating; DCM with Si(111), Si(311) and mirror (white light); Cylindrical mirror with three co-atings, low energy band path, vertically focusing. Precise slit in focus, de-fining a virtual source with adjustable size; Elliptical Kirkpatrick Baez mir-ror system, focusing the virtual source; Monochromatic or “white light” beam path, selectable

Flux at samle postion 1,25x1011 (4 x 1010) ph / (sx0.1%BWx100mA) in spot size 0.35 mm(hor) x 0.2 mm (vert) (65x40 µm2) at 8 keV

Beam size at sample 0.5 mm (hor) x 0.3 mm (vert) down to 50 µm x 40 µm

Sample mounting Various holders to fix pellets, sections (up to about 70 mm (hor) x 30 mm (vert). Other sizes and mountings of irregular shaped samples can be realized on request.

Sample environment Flow-through cell is available, chambers for other environments (gases, T-controlled) are planned.

Experimental station Sample diffractometer with theta, phi circle and chi cradle (10°), xyz linear stages, CCD detector on horizontal 2theta circle for diffraction, 3 retrac-table ionization chambers for absorption, 7 element Si(Li) fluorescence detector for fluorescence, optical microscope; diffractometer and detec-tors all vacuum-compatible, additional detectors working in air: 1 element SDD for fluorescence, Avalanche photodiode for diffraction, Photodiode for diffraction.

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

SUL-X


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Figure 2a: SUL-X experimental station, view towards the incoming beam. Vacuum chamber with control electronics and fluorescence detector (right).

Figure 2b: View onto the SUL-X experimental station with (1) diffractometer, (2) sample holder, (3) ionization chambers, (4) fluorescence detector, (5) CCD detector, aside temporary SDD or avalanche diode or (8) photo diode, (6) light microscope, (7) reference sample holder. Dashed line represents primary beam direction.

CONtaCt

Ralph Steininger: [email protected] +49 (0)721 608 26173Jörg Göttlicher: [email protected] +49 (0)721 608 26070

Harald Zöller: [email protected] +49 (0)721 608 23329Wolfgang Möck: [email protected] +49 (0)721 608 28370

Beamline +49 (0)721 608 28293

44



UV-CD12Vacuum-UV beamline for synchrotron circular dichroism spectroscopy

Spectroscopy


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

UV-CD12 is a high flux vacuum-ultraviolet/ultraviolet beamline for steady-state synchrotron radiation circular dichroism (SRCD) spectroscopy. It is operated by KIT´s Institute of Biological Interfaces (IBG-2). The UV-CD12 beamline was conceived and designed by the Centre for Protein and Membrane Structure and Dynamics (CPMSD), a consortium of U.K. structural biologists. It was constructed at the SRS facility of the Daresbury Laboratory and opened for users in 2003. Following the closure of SRS in August 2008, UV-CD12 was donated to IBG-2 and ANKA in order to continue its working life. The synchrotron-based studies at UV-CD12 are integrated in IBG-2´s in-house research within the framework of the “BioInterfaces” program, thus complementing solid-state NMR and other biophysical techniques, which are well-established at IBG-2 for structural characterization of cell membrane-active peptides and proteins.

Scientific applications Circular dichroism (CD) spectroscopy in structural biology is used for investigations of the secondary structure of proteins and other chiral (bio)macromolecules. Typical applications include

• Determination of secondary structure of proteins that cannot be crystallized

• Investigation of the effects of the binding of ligands (e.g., drugs) on protein secondary structure

• Study of dynamic processes such as protein folding • Study of the effects of environment (e.g., pH, solvent, denaturing

agent, temperature) on protein structure • Determination of the secondary structure content of membrane

proteins • Study of enzyme active site changes• Investigation of protein-protein and protein-nucleic acid

interaction• Investigation of DNA and carbohydrate structure.

Synchrotron radiation as a VUV light source for CD spectroscopy allows for extension of the spectral range below the 190 nm limit of benchtop instruments, gives access to additional electronic transitions of the amide bond, and dramatically increases the power of the technique to distinguish protein structural motifs. The high photon flux yields excellent signal-to-noise ratio with minimal sample volumes and measuring times. Moreover, the natural linear polarization of the synchrotron beam is exploited.

Available methods, obtainable parameters CD spectroscopy: Protein structural motifs with different secondary structure have characteristic CD base spectra; deconvolution of experimental protein spectra with mixed structural features yields the fractional amounts of pure structural components (e.g., α-helix, β-strand). Precise temperature control accessories allow for flexible thermal ramping experiments (protein denaturation), and these data can be analyzed for functions such as Tm, ∆H and ∆S.

Oriented circular dichroism (OCD) spectroscopy: Fast and sensitive spectroscopic method for analyzing the secondary structure, orientation and aggregation behaviour of membrane-embedded peptides and proteins in solid samples, i.e., in model membranes (lipid bilayers) that are macroscopically aligned with respect to the light beam. SR-based OCD will allow study of the conditions where structurally relevant changes in peptide structure and orientation occur, especially for β-pleated and polyproline folds. It will contribute to our understanding of structure/function relationships of, e.g., antimicrobial peptides that lyse bacterial cell membranes (potential new antibiotics), cell-penetrating peptides that may translocate cargo through cell membranes without destroying them or hydrophobic membrane proteins that are involved in cell-signaling.

UpgradesRapid-mixing microfluidic system for time resolved spectroscopy: It is planned to equip the experimental station with a capability for simultaneous VUV-CD and FTIR measurements of protein folding and structural change kinetics using a microfluidic rapid-mixing system, thus exploiting the strong complementarity of these two techniques.



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Figure 1: Schematic layout of UV-CD12 beamline and experimental setup.

Figure 2: 3D view of UV-CD12 beamline at ANKA’s B2.2.5 bending magnet.

Jochen Bürck: [email protected] +49 (0)721 608 22690Siegmar Roth: [email protected] +49 (0)721 608 22672

Bianca Posselt: [email protected] +49 (0)721 608 23615Beamline +49 (0)721 608 29222

46



Spectroscopy


KEY PARAMETERS OF THE BEAMLINE

Source Bending magnet (1.5 T)

Photon beam divergence 30.8 mrad (hor) x 3.7 mrad (vert)

Optics Planar water-cooled mirror, Al-coated silicon toroidal holographic grating (300 grooves mm-1), Al-coated silicon

Beam size at sample point typ. 2.5 mm (hor) x 4.8 mm (vert) (@ 200 nm, 1 nm spectral bandwidth)

Photon flux ~ 1x1012 ph/s (@ 200 nm, 1 nm spectral bandwidth, 160 mA)

Wavelength range 130 – 350 nm

Energy range 3.5 – 9.5 eV

Wavelength resolution 0.5 to 2.0 nm

Sample cells Cylindrical: 0.1-1 mm path length,Demountable (quartz glass or CaF2): 3-15 µm path length, Rectangular: 1-10 mm path length

Experimental stationMgF2 Rochon polarizerPhotoelastic modulator: CaF2, 50 kHz (Hinds Instruments PEM-90), Detectors: Solar blind PM (Electron Tubes 9402B)

UV / Vis PM (Electron Tubes 9406B)Peltier element temperature control accessories for thermal scans (4-90°C temperature range)

Software/data treatment/evaluation

In-house built CD data aquisition software / CDTool / DichroWeb server (Birkbeck College, University of London)



UV-CD12


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CONtaCt

Jochen Bürck: [email protected] +49 (0)721 608 22690Siegmar Roth: [email protected] +49 (0)721 608 22672

Bianca Posselt: [email protected] +49 (0)721 608 23615Beamline +49 (0)721 608 29222

Figure 5: Cross-sectional view of OCD sample cell that allows for secondary structure and alignment analysis of helical peptides and proteins in model cell membranes under controlled humidity and temperature conditions. Inset: OCD spectra of two fragments of the pore-forming unit TatA from the membrane protein-export machinery reveal helical structure and parallel alignment with respect to the membrane plane for the amphiphilic segment and perpendicular orientation for the hydrophobic transmembrane part (as can be deduced from the intensity of the negative CD band around 208 nm).

Figure 3: Experimental setup for liquid-state SRCD measurements of proteins (including thermal scans).

Figure 4: View into the experimental cabin with the UV-CD12 post-monochromator section, the beamline electronics and the optical table with the SRCD experimental setup.

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WERaSoft x-ray analytics facility

Spectroscopy/ Imaging

Scientific applications WERA (“Weichröntgen-Analytik-Anlage”) is a beamline for soft x-ray spectroscopy, microscopy, and spectromicroscopy. It is owned and operated by the Institute for Solid-State Physics (IFP), Karlsruhe Institute of Technology (KIT).WERA provides important electron spectroscopies in the photon energy range 100 – 1500 eV and combines them in situ with photoemission microscopy. It facilitates combinatory studies of electronic and magnetic structure which have particular promise for strongly correlated, thin-film, and nanoscale materials.

Available methods, obtainable parametersPhotoemission, angle-resolved photoemission, resonant photoemission (PES, ARPES, ResPES): occupied electronic structure, band character, Fermi surface, element-specific band structure

Near-edge x-ray absorption (NExAFS): bulk-sensitive fluorescence yield; total and partial electron yield – unoccupied electronic structure; orbital character, occupation, crystal field and spin state; element- and site-specific information

Soft x-ray magnetic circular dichroism (xMCD): element-specific information on magnetism: spin and orbital magnetic moments, interactions, spin states, anisotropies

Photoemission electron microscopy (PEEM): imaging of topography and of chemical and magnetic contrast; laterally resolved spectromicroscopy: µ-PES, µ-ARPES, µ-NExAFS, µ-xMCD.

Upgrades Radiation from an undulator as an alternative light source to the bending magnet is planned to be available at WERA. All methods will benefit greatly from the increased photon flux and flux density at the sample. First, the U10 undulator presently on loan from the NSRRC, Taiwan, will be utilized.

Beamlines

Figure 1: Two of the three experimental stations at WERA.

Figure 2: Cooled gratings in the monochromator.

Figure 3: Schematic layout of the WERA beamline.

FLUO | INE | IR1 | IR2 | SUL-x | UV-CD12 | WERa | xAS | MPI-MF | NANO | PDIFF | SCD | IMAGE | TOPO-TOMO | LIGA I, II, III


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Figure 4: PEEM ’n‘ beam at WERA.

CONtaCt

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

Key parameters of the beamline

Energy range100 eV - 1500 eV

Energy resolution [∆E/E]

Typically 2x10-4; <1x10-4 demonstrated at N K absorption edge

Source For each experiment, choice between:• ANKA dipole. Quick selection of circular and linear polarization by aperture.• Undulator. In planning: For increased photon flux / flux density [planar undulator (period 10 cm; “U10”), on

loan from NSRRC, Taiwan. Later upgrade envisioned]

Optics Spherical grating monochromator. Bendable refocusing mirrors for optimum focus at sample position in all experimental stations

Beam size at sample Dipole source, PEEM chamber: typ. 0.4 mm (hor.) x 0.1 mm (vert.) FWHM

Sample / Sample environment

Ultrahigh vacuum (base pressure in 10-11 mbar range) PES/NEXAFS and XMCD chambers: sample temperatures down to 15 and 20 K, resp.

Experimental setup/ sample position

Three UHV chambers for in-situ sample preparation and characterization including RHEED. All sample transfers in UHV.


• PEEM chamber: photoemission electron microscope; resolution 30 nm (topography), 100 nm (spectromicroscopy); imaging energy filter• PES / NExAFS chamber: electron energy analyzer (2D detection; angular resolution); fluorescence detector; total and partial electron-yield detection; LEED• xMCD chamber (provided by Max-Planck Institute for Intelligent Systems Stuttgart, MPI-IS): fast ramp; magnetic field up to 7 T; detection modes: total electron yield, fluorescence yield

Software User beamline control software spec™ running on Linux system; Windows PCs for experiment control and data evaluation.

transmission

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ANKA Control System Commercial ServicesUser Service

XaSX-ray absorption spectroscopy beamline

Spectroscopy

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

Scientific applicationsxAS provides essential information about the local atomic geometry and the chemical state of the absorbing atom. The method is element specific and is not restricted to the crystalline phase, but may be used with highly disordered amorphous and liquid samples. At the xAS beamline, a cooperative multidisciplinary scientific program is established to solve scientific questions in the fields of:

Nanomaterials and catalytic systems: There is intense interest in the development of materials with nano-sized dimensions with novel catalytic, energy storage, or macroscopic properties. The KIT research group focuses on H-storage materials based on Ti-clusters, external groups on catalytic systems as nanostructured traps for SOx, and on Ni-doped carbon nano tube systems for tunable magnetic properties. An objective of characterization is to determine the structure and interatomic distances, and the mean oxidation state of atoms in the nanoparticle. The efficiency of new catalytic systems is studied in-situ by tracking the changes of the chemical state of educts or products using xAS in combination with mass spectrometry.

Environmental sciences: Contamination of the environment is a consequence of industrial and domestic processes and presents a health hazard and a limitation to the productive use of land. Current research is focused on Zn release to soils, a problem even from such seemingly harmless objects as electricity pylons, and on sulfuric acidification of surface waters, which leads to mobilization of toxic metals in mining areas. xAS is an extremely important tool in identifying the nature of toxic metals causing the contamination, thus allowing remedial strategies to be devised.

XAS is an X-ray absorption spectroscopy (XAS) beamline on a dipole magnet source. Due to the high flux the beamline is suited for highly diluted systems in bulk samples.

Available methods, obtainable parametersx-ray absorption near edge structure (xANES): valence and coordination geometry.

Extended x-ray absorption fine structure (ExAFS): interatomic distances to 0.02 Å resolution (up to 5-6 Å); coordination numbers, type of nearest neighbors.

There are two principal modes of detection: transmission and fluorescence measurements. The transmission technique uses ionization chambers (Figures 1a,b) and the detection limit is determined by the element of interest and the other elements comprising the sample. Typical values are ~5 % by weight. The fluorescence mode is applicable for the study of elements at lower concentrations (detection limit: ~1 mmol/L) and for “thick” samples where transmission. The fluorescence radiation emitted by the sample as a function of photon energy is recorded using an energy dispersive detector (Figures 3 and 4). Additional to standard ExAFS, the xAS beamline offers grazing incident xAFS (GI-xAFS) and q-xAFS. At the ANKA xAS beamline, a q-xAFS mode on a double crystal fixed exit monochromator (DCM-fe) has been implemented. Due to the combined movement of the Bragg axis and the two linear drives, the stability of the beam height on the sample position is maintained within much less than 10 µm. Combined with the xIA-xMAP electronics and the Struck counter card, a hardware triggered q-xAFS mode is implemented, which offers q-xAFS down to 45 s in fluorescence detection mode. Even in this very fast mode, it is be possible to read out the complete fluorescence spectrum for each incoming photon energy. This enables a multi-peak fitting of the fluorescence spectra throughout the spectrum and, thus, a higher precision of the resulting data, at a data rate of up to 8 Gb/day. The accuracy of the DCM and the high precision of the angular encoder allow both energy directions to be used, thereby reducing the delay between the scans.

BeamlinesFLUO | INE | IR1 | IR2 | SUL-x | UV-CD12 | WERA | XaS | MPI-MF | NANO | PDIFF | SCD | IMAGE | TOPO-TOMO | LIGA I, II, III


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Instrumental Characteristics 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.

Sample Environment A multi sample holder with 12 positions (transmission and fluorescence measurements possible) offers advanced automation options. The sample wheel can be adjusted in both directions perpendicular to the beam. For grazing-incidence measurements, a Huber goniometer with two additional slits can be used.

Figure 1a: Ionization chambers for experiments > 3.5 keV. Figure 1b: Combined ionization- / sample chamber for low E XAS in transmission mode.

Upgrades of the BeamlineA new experimental table will be installed in 2013. This will enable better alignment option and much higher stability. A new 6 element

CONtaCt

Stefan Mangold : [email protected] +49 (0)721 608 26073David Batchelor: [email protected] +49 (0)721 608 28675


Figure 2: Schematic layout of the XAS beamline.


Commercial Services

CONtaCt

Stefan Mangold : [email protected] +49 (0)721 608 26073David Batchelor: [email protected] +49 (0)721 608 28675


Key parameters of the beamlineEnergy range 2.4 keV - 27 keV (S K-edge up to U L-edge, Cd K-edge)

Energy resolution [∆E/E] Si (111): 2x10-4; Si (311): 1x10-4


Optics Double crystal monochromator with two sets of Si crystals, MOSTAB, Planar Zerodur mirror to suppress higher harmonics at low energies

Flux at samle postion Si (111): 7x109 ph/s/mm2/100mA @ 9 keV

Beam size at sample 20mm (hor) x 2mm (ver) down to 1mm x 1mm, typical 8mm x 1mm

Sample environment Closed cycle He-cryostat (15 K - 320 K, 0.1 K accuracy), liquid N2-cryostat (-130 - +140 °C, in commissioning)


3 ionization chambers (transmission mode)2 combined ionization chambers optimized for xAFS at the low energy range5 element high purity germanium solid state fluorescencedetector (Canberra Ultra-LEGe), 1 element silicon drift detector (Vortex-90Ex,Hitachi High-Tech Science), 6 element 100 mm2 silicon drift detector (SGx Sensortech, in commissio-ning), detector read-out with xMap-electronic in mapping mode

Software/ Data treatment/ Evaluation

xAFSmass, GiFeffit, iFeffit, Sixpack


MPI-MFBeamline

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

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Beamlines

MPIBeamline for structural characterization of materials

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

A beamline for the structural characterization of materials owned and operated by a consortium of Max-Planck Institutes.

Scientific applicationsThe beamline is best suited for the structural in-situ characterizationof materials in reduced dimensions, like surfaces, interfaces, thin films, multilayers and nano-crystalline compound materials. In the future there will be an increased need to study such systems under industrially and environmentally relevant conditions, such as high temperature/pressure, external mechanical forces, aggressive gas atmospheres or high electric or magnetic fields and low temperatures [1].

the main research activities carried out at the beamline are:

1) Structure of rare earth transition-metal oxide single crystals, thin films and multilayers. 2) In-situ stress measurements and fault structures in metallic alloy thin films. 3) In-situ reactive changes of the surface structure and morphology of intermetallic phases. 4) In-situ growth of metallic alloy films. 5) Oxidation of metallic alloys. 6) In-situ studies of semiconductor nanostructures.

Available methods, obtainable parameters,physical properties

types of experiments that can be performed:

Crystal truncation rod measurements to study the atomic structure of surfaces and buried interfaces

Experiments under grazing incidence to obtain nm scale depth resolved structural and chemical information

Specular and off-specular reflectivity measurements providing the sample electron density profile normal to the surface and the surface and interface roughness profiles

Resonant scattering measurements to characterize collective electronic phenomena

In-situ diffraction experiments at high temperatures and under gas atmospheres using heavy sample environments

Time resolved experiments to study growth kinetics and interface evolution under controlled conditions.

Figure 1: Schematic Layout of the MPI beamline optics.

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


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CONtaCt

Instrumental characteristics The beamline can either be operated in monochromatic, pink or white beam mode. The key parameters of the beamline are summarized in the table at the end of this section. Figure 1 shows a drawing of the beamline optics. The main optical elements are a Rh coated Si mirror and the double crystal monochromator (DCM). The DCM consists of a flat Si(111) single crystal and a sagittal Si(111) crystal bender for horizontal focusing. The mirror allows to cut the energy spectrum of the incident photons at its higher end to suppress the harmonic content in the monochromatic beam. In addition it is used to focus the beam in the vertical direction.

Two pairs of horizontal and vertical slits allow to pre-select the beam size on the sample. The heart of the experimental end station is a 2+3 diffractometer that can be operated either in horizontal or vertical sample normal mode (Figure 2). The sample stage has 4 degrees of freedom in the vertical configuration and 5 degrees of freedom in the horizontal configuration. The vertical axis sample rotation stage can support a weight up to 300 kg. The detector arm has in addition two degrees of freedom combined with the possibility of slit rotation on top of the detector arm. All rotations provide an angular resolution of 0.00025°. The detector arm itself is designed to support two detectors simultaneously. The whole instrument is aligned in the incident x-ray beam using a jackable table (colored blue in Figure 2). Two motorized horizontal and vertical slits are mounted on the detector arm. In front of the instrument another pair of slits define [2] the incident beam size. Behind the incident slits an ionization chamber is installed to monitor the photon flux. Figure 3 shows an in-situ oxidation chamber, as mounted on the diffractometer; the growth of oxide islands can be monitored in situ by a 2D and a point detector simultaneously. In the experimental hutch a crane is installed that is used to handle heavier sample environments. A small Eulerian cradle can be mounted to run the instrument as a vertical four circle diffractometer.

Figure2: 2+3 diffractometer in the experimental hutch. The experimental stage can take up heavy duty sample environments for in situ experiments.

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

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Beamlines

Key parameters of the beamline

Energy range 6 keV - 20 keV

Energy resolution [∆E/E] 3 10-4 @ 9 keV

Source 1.5 T bending magnet (EC = 6 keV), 0.3 mrad horizontal, 0.03 mrad vertical

Flux at sample position 10+12 ph/s/0.1%bw @ 9 keV

Optics double crystal monochromator with a pair set of Si(111) crystals, second crystal allows horizontal focusing of the beam Rh coated mirror, vertical focusing possible

Beam size at sample could be focused to 0,5mm (hor) x 0,3 mm (ver)

Sample / sample environment UHV/HP chamber, HT oven, cryostat, tensile tester, fast capillary spinner

Experimental setup / sample positioning

1st station: multiple circle diffractometer, horizontal / vertical sample normal geometry, horizontal / vertical four circle geometry, COR 5 m from DCM2nd station: horizontal six circle diffractometer, COR 10 m from DCM

Experimental setup / detectors . NaI scintillation counter. LaCl_3 scintillation counter. 10 ·10 mm2 avalanche photodiode. 2D gas filled wired detector. MAR 165 CCD camera. Si/Ge energy dispersive detector. Mythen 1 k 1D detector. Pilatus 100 k 2D detector

Software: Control system / Data treatment / evaluation

SPEC, software for reflectivity and crystal truncation rod analysis, software for reciprocal space mapping

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

MPI


Commercial Services

Upgrades of the beamline Several upgrades for the beamline have been performed, concerning its performance and the flux available at the sample position. 1) Software upgrade: the old RST system was removed and all beamline components can be controlled via SPEC. The more reliable alignment resulted in an increase of the photon flux at the sample by a factor of two, without any change on the hardware. 2) A 2nd fluorescent screen was installed on the beamline: in order to do a faster alignment of the beamline, it is necessary to be able to monitor the beam position after the mirror. 3) A beam polarization monitor was installed in the white beam after the first pair of slits and commissioned. It is needed to guarantee fully linear polarization of the incident beam, which is essential for the xMCD experiments and diffraction experiments. 4) A fast shutter/pin diode system for detector protection and direct beam alignment was installed. 5) The lengths of the experimental hutch was extended by 3 m. This allows the future installation of a fast 4-circle diffractometer. Its center of rotation (COR) is set about 10 m from the DCM, thus allowing for a focused beam at energies up to 16 keV.

Figure 3. In-situ oxidation chamber mounted on the diffractometer; a simultaneous detection using a 2D and a point detector is possible.

Planned upgrades• Installation of a fast 4-circle diffractometer allowing a focused beam

up to 16 keV.• Upgrade of the vacuum and shutter control system to PVSS• Replacement of all motor power supplies and controllers to ANKA’s standard Middex controllers.• The detector arm will be modified to eliminate possible collisions• Installation of a small closed cycle refrigerator for the small Huber Eulerian cradle• Installation of an in-vacuum 16 fold absorber system• Installation of a motorized vacuum beamtube and collimator

system for the incident beam to reduce background from air scattering

• Installation of a dedicated lever-type slit system with flight tube for area detectors.

References:

[1] A. Stierle et al., Rev. Sci. Inst. 75, 5302 (2004).[2] J. Böhm et al., Rev. Sci. Inst. 75, 1110 (2004).

CONtaCt

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

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Scientific applications x-ray diffraction probes the spatial arrangement of atoms in a crystal lattice. It is sensitive not only to chemical composition and lattice parameters, but also to the strain and the strain distribution, lattice defects and dislocations as well as to the shape and size distribution of nanostructures. Since the advent of synchrotron radiation, the range of applications has been extended from bulk crystals to thin films and multilayers, epitaxial superlattices, nanostructures, nano-crystalline materials and even to magnetic structures and multilayers.The NANO instrumentation was specified to allow in-situ characterization using synchrotron radiation. One of our focus

NaNO High Resolution X-ray Diffraction and Surface & Interface Scattering Beamline


is to investigate the changes in structural parameters such as lattice parameters, chemical composition, layer thickness, surface and interface roughness, inter-diffusion, crystal lattice quality/homogeneity, strain distribution, nanostructure geometry (size/shape/correlations) during the growth process of individual monolayers as function of temperature, deposition time, pressure and flow-rate of material. The achievement of the beamline is to realize time resolved x-ray diffraction and surface scattering measurements during growth and deposition processes, which offers novel opportunities for internal and external users.

Current status of the instrumental development at the beamline During 2012, a continuous methodical implementation was carried out at the beamline. This included testing of the different functionalities of the beamline to make them reliably used for the dedicated applications. For that purpose, selected experiments such as in-situ MBE investigations and local resolved investigations of defects using microfocus beam have been performed at the experimental station NANO1 to evaluate the reliability of the set-up. The methods dedicated at the beamline like symmetric, asymmetric and grazing incidence diffraction with high resolution in reciprocal space have been implemented by measuring AlGaN samples grown on sapphire substrate, provided by the Institute of Optoelectronics in Ulm.The optics of the beamline offer the possibilities to work in three modes-monochromatic, pink and white beam, corresponding to an energy resolution varying between 10-4 and 10-2.The pink mode (energy resolution of 10-3) was brought to operation at the beamline for the commissioning of the x-ray transmission microscopy at the experimentation station NANO2, which is functional. For that purpose, a double multilayer based on NiB4C has been commissioned taking advantage of the wide band width for higher flux in the 1012 ph/s/100 mA range. The concept of the beamline to operate the two experimental stations NANO1 and NANO2 alternatively is illustrated in Scenario 1 and 2.

Current status of the opticsThe beamline was operational using the super-conducting undulator SCU14 source until June 2012. The 1 T Wiggler replaced the undulator source in September 2012. The layout of the Nano beamline is composed of 4 mirrors and two monochromators.The performance of the beamline has been evaluated. The beam profile has been measured at profile monitor PM2 and compared to the simulated profile. In addition, the flux spectrum was measured with a calibrated photodiode at the sample position in the case of the focused beam. The simulation of the photon flux at the sample with the undulator source was performed with the xtrace program [1]. The good agreement between the measured and the simulated spectra indicates the beamline optics is well aligned and is

Figure 1: The Nano Team at the NANO station: David Haas, Sondes Bauer, Sergey Lazarev, Andrei Scheibe, Andreas Breitenstein, Denis Jakel, Erhan Cilbir and Stefan Uhlemann, as well as Thorsten Schwarz and Ingo Müllner.

Beamlines

Information

NANO is operational since September 2012, using a permanent 1T wiggler on loan from Daresbury. 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 full-field Transmission X-ray microscopy in a material science at room temperature and in the biological field in the cryo-environment.

............................................and its auxiliary In-Situ Infrastructure Characterization Labs

FLUO | INE | IR1 | IR2 | SUL-x | UV-CD12 | WERA | xAS | MPI | NaNO | PDIFF | SCD | IMAGE | TOPO-TOMO | LIGA I, II, III


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Figure 2: Scenario 1: Operation of NANO1 dedicated for high resolution X-ray diffraction of thin films and Nanostructured materials. The multipurpose diffractometer is placed at the measurement position

Figure 3: Scenario 2: mounting of the shielded tube in NANO1 and the operation of the hard X-ray transmission microscope TXM in the second station NANO2. The first station NANO1 is accessible during the experiment at NANO2. This concept is very useful for using the beam time efficiently and carry on with the instrumental installation parallel to the commissioning with the beam.

Sondes Bauer. [email protected] +49 (0)72160 82-6489Beamline +49 (0)72160 82-9126

operational as it is specified.The parameters of the optics are summarized in the table. Due to the Rh and Pt double coating of the reflecting mirrors at the beamline, the energy cut-off was extended to 30 keV. x-ray diffraction at high

energy has opened a field of detecting several diffraction peaks using a two dimensional detector (Pilatus 2M) with a detection area of 254 x 289 mm2.

Figure 4: Set-up of the beamline

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Beamlines

Key parameters of the beamlineEnergy range 3 keV – 30 keV

Source Permanent Wiggler of 5 periods and with 2mm period length. The B field is 1T

Optics ▪ Two horizontally collimating/focusing ▪ mirrors with variable benders ▪ Two vertically collimating/focusing ▪ mirrors with variable benders ▪ Double crystal monochromator with ▪ two pairs of crystals (Si111 & Si311) ▪ Double multilayer monochromator with two

pairs of multilayers (Ni/B4C and Mo/B4C). ▪ Four slits used partially to protect the ▪ mirrors from overfilling. ▪ Diagnostics: 2 profile monitors, 4 fluorescent

screens, 2 intensity monitors, ionisation chamber and polarisation monitor

Energy resolution

(∆E/E)

∆E/E=10-2: Multilayer Ni/B4C and Pd/B4C,∆E/E=10-3: Multilayer Mo/B4C and Pd/B4C,∆E/E=10-4: Crystal monochromator Si111, Si311

Beam parameter in the focused

and collimated modes

size (HxV)(FWHM) = 171μm x 39 μm, divergence (HxV)(FWHM) = 0.315 x 0.2 mrad

Size HxV [FWHM]=2 x 0.74 mmDivergence HxV [FWHM]=0.02 x0.0037 mrad

relative horizontal position [mm]

In-situ structure characterization at experimental station NANO1

Cryo-Vacuum chamber with Be-dome for temperature treatment from -200 up to 400 °CA Be-dome is available at the beamline to carry out a temperature treatment from -200 up to 400 °C. It offers for example the possibility to investigate the crystalline phase transformation and domain formation in ferroelectrics materials. The dome gives the advantages to realize the coplanar and non-coplanar diffraction geometries experiments.The cooling of the sample up to -200 °C could be performed either with the liquid Nitrogen N2 or with Helium. The layout out of the Cryo-vacuum chamber combined into the diffractometer is illustrated in the figure where the Be-dome is shown. On the right side, the fixation of the sample with the maximum dimensions of 10x10 mm is shown.

In-situ MOVPE growth characterisation of GaN In-situ Metal Organic Vapor Epitaxy MOVPE laboratory is established at ANKA to investigate the evolution of the structure of GaN based materials during the growth process. The MOVPE reactor could be used off-line to optimise the growth parameter as well as on-line in the experimental hutch. In order to realize the x-ray in-situ characterization of GaN in NANO1 using the MOVPE reactor, 12 gas lines are installed at the beamline in addition to the manifold. The schematic presentation of the in-situ MOVPE laboratory of nitride based materials is displayed by the organograms where the different parts composing the In-Situ MOVPE laboratory such gas panel, gas lines, reaction and scrubber are described. This laboratory in implementation phase and attended to be operational in February 2014.

Status12 lines are installed:6 Lines for Metal-Organic MoMo1: Trimethylaluminium, TMAlMo2: Trimethylgallium TMGaMo3: Trimethylindium TMInMo4: IS(Cyclopentadienyl)- MAGN Cp2MG for Mg dopingMo5: TriethylgalliumMo6: Variable3 lines for N2, 1 line for NH31 line for H2, 1 line for SiH4

Building of gasStorageNH3. H2. SiH4

MOVPE Lab L1for Ex-Situ growth

In-Situ MOVPE Labat NANO

Gas line between L1and L2

Gas Panel

Reactor

In-Situ MOVPE laboratory for III-Nitride-based materials at aNKa

x-ray “T” shape window

GID: in-plan strain, defect

FLUO | INE | IR1 | IR2 | SUL-x | UV-CD12 | WERA | xAS | MPI | NaNO | PDIFF | SCD | IMAGE | TOPO-TOMO | LIGA I, II, III


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CONtaCt

Sondes Bauer: [email protected] +49 (0)72160 82-6489Beamline +49 (0)72160 82-9126

Detector systems at NANOThe beamline offers a versatile choice of detectors varying from point, linear to 2D detectors. The in-situ investigation of growth process requires detector having a fast read-out, high dynamic range and efficiency like the single counting detector. A listing of the available detector available to the user are given in the table.

X-ray-Eye Photonic Science x-Ray FDI-2 Camera System Active input area of 8.98 (h) x 6.71 (v) mm with 1392 x1040 pixels for beam imaging

Point Detector

1-FMB Oxford Cyberstar NaI Point Detector (48 mm opening) sensitive point detector Rise time 10%-90% <2 ns 2- FMB Oxford Avalanche Photodiode (10 x 10 mm²) very fast point detector for in-situ-characterization

Linear Detector

1-Hecus PSD-50M – classic gas filled wire detector (resolution μ 13 µm)2-Mythen Detector, fast pixel detec-tor,50 µm resolution, read out 0.3 ms.

CCD Detector

Princeton Instruments quad-RO: 4320 2048 x 2048 pixels w/a pixel size of 24 x 24 µm², read out: 1.4 s

Energy Dispersive

Detector

Vortex-60Ex w/xIA Saturn-ALL Electronic

PILatUS 100K-S

Detection area: 83.8 x 33.5 mm2, pixel size: 172µm2, Dynamic 20Bits, readout 2.3 ms, point spread function 1 pixel

PILatUS 2M Detection area: 254 x 289 mm2, pixel size: 172µm2, Dynamic 20 Bits,readout 1.15 ms. Framing rate 60 Hz

Diffractometer in configuration “C”, corresponding to the vertical geometry, combined with the cryo-vacuum chamber.

Cryo-vacuum chamber, showing the sample holder

Cryo-vacuum chamber, covered with Be-dome

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BeamlinesFLUO | INE | IR1 | IR2 | SUL-x | UV-CD12 | WERA | xAS | MPI | NaNO | PDIFF | SCD | IMAGE | TOPO-TOMO | LIGA I, II, III

Multipurpose diffractometer dedicated for in-situ X-ray scattering characterization

The multipurpose diffractometer represents the heart of the beamline; it offers three main configurations A, B and C, depending on the size and the load of the environmental chamber used for the in-situ processing investigation. An overview of the different set-ups designed in combination with diffractometer as well as real experiments which took place at the beamline is presented below.

Euler Cradle for stress analysis combined with the MOVPE reactor

Cryo-Vacuum chamber with Bedome for temperature treatment from -200 up to 400 °C. The highest angular limit toward the aoutgoing beam is -135 degrees

Cryo-Vacuum chamber with Be-dome for temperature treatment from -200 up to 400 °C. The lower angular limit toward the incoming beam is 70 degrees

Horizontal geometry for heavy weight of 500 kg

Mounting of the MBE on the diffractometer

First in-situ MBE X-ray diffraction of GaAS nonowires

Position corresponding to theta=0


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The commissioning of the full-field hard x-ray transmission microscope at the experimental station NANO2 started in September 2012. The microscope has been specified as full-field transmission hard x-ray transmission with 30 nm 2D resolution, with the possibility to perform Near Edge Spectroscopy (xANES) for chemical imaging. Scanning x-ray fluorescence mapping with 2 µm spatial resolution is aimed to be achieved. The TxM has special features due to the possibility of cryogenic handling in addition to the automatic loading and unloading of sample. The TxM is well-suited for material science applications as well as for biomedical and biological applications.

TXM installed a the experimental station NANO2 in commisiong phase

Layout of the TXM, showing the main components of the set-up

aBSORPtION CONtRaSt

5 to 11 keV, Large field of view (40 µm FOV, 20 nm pixel size at sample). High resolution (20 µm FOV, 10 nm pixel size at sample, 25 µm DOF

First result obtained in November 2012: 30 nm star pattern (30 nm lines and spaces), imaged at 5 keV in High Resolution Absorption Contrast Mode

CONtaCt

Sondes Bauer: [email protected] +49 (0)72160 82-6489Beamline +49 (0)72160 82-9126

Hard X-ray transmission microcopy at experimental station NANO2

ZERNIKE PHaSE CONtRaSt

5 and 8 keV, high resolution (20 µm FOV, 10 nm pixel size at sample, 25 µm DOF)

First result obtained in November 2012: 30 nm star pattern imaged at 5 keV in HRES Zernike phase contrast mode

[1] Sondes Trabelsi Bauer, Martin Bauer, Ralph Steininger and Tilo Baumbach, Simulation of x-ray beamlines with the new ray tracing tool xTrace, published in Nuclear Inst. and Methods in Physics Research, A 2007.[2] Sergey Lazarev, Mike Barchuk, Sondes Bauer, Kamran. Forghani, Vaclav. Holy´, Ferdinand. Scholz and T Baumbach, J. Appl. Cryst. (2013). 46, 120–127[3] Lazarev, S., Bauer, S., Forghani, K., Barchuk, M., Scholz, F. & Baumbach, T. (2013). J. Cryst. Growth. In press.

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Available methods, obtainable parameters• Symmetric and asymmetric powder diffraction in either

reflection (Bragg-Brentano) or transmission (capillary) geometry,

• 4-circle scattering experiments with or without an analyzer: texture, sin2ϕ-method, grazing incidence scattering, reciprocal space mapping,

• Microstructure analysis: characterization of residual stresses, particle size determination, texture, film thickness

• quantitative phase identification of polycrystalline mixtures.

Scientific applications The main use of the beamline is for the investigation of polycrystalline materials under varying in-situ conditions and for high-resolution powder diffraction, residual-stress and texture measurements. It is also well suited to performing high-resolution scattering studies on single crystals, epitaxial layers and bulk single-crystalline materials.

• Real-time In-situ characterization of nanostructural and microstructural properties of metals and alloys,

• In-situ powder studies of crystallographic phase changes in bulk polycrystalline materials,

• High-resolution powder diffraction for the structural characterization of mineralogical phases,

• Microstructure investigations of inorganic refractory and electro-optical materials

• Residual-stress and texture analysis in functional poly-crystalline thin films.

PDIFFX-ray powder diffraction beamline


Figure 1: Schematic layout of the PDIFF beamline

Beamlines

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

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



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Figure 2: Schematic diagram of degrees of freedom of the new heavy duty diffractometer

Figure 4: The Kappa diffractometer consists of 3 sample orientation circles (Ω, Χ, Φ) and 3 detector circles (2θ, 2 x analyzer stage).

Figure 3: The heavy-duty diffractometer with capillary furnace and 1D and 2D detectors

Figure 2: The new heavy duty diffractometer

21 3

1st 2carranddetecollisetu

Theta-circle ying 2D-CCD camera either analyser / ctor or Soller mator / detector p

2nd 2Theta-circle carrying1D 90° PSD

lateral and vertical translation axes for centering of diffractometer on the beam axis

sample rotation stage

With the installation of the focusing mirror it is now possible to focus the x-ray beam both horizontally and vertically between energies of 6 and 21keV. The mirror consists of a sagitally fixed cylinder which can be bent meridionally to allow variation of the effective vertical beam size at the sample position. Since the bending radius can be varied it is possible to optimize the vertical focus for either the forward of rear experimental station. The horizontal focus is optimized for the front experimental station, which results in a horizontal beam size of approx. 500μm fwhm at this point, and around 2mm horizontal size at the rear station. Figure 3: View of the VH-focusing mirror during installation, Nov. 2009

Stephen Doyle: [email protected] +49 (0)721 608 28194 Udo Krieg: [email protected] +49 (0)721 608 28372

Beamline +49 (0)721 608 26648

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Beamlines

Instrumental parameters and equipment, infrastructure The PDIFF beamline provides vertically and horizontally focused radiation between approx. 6 and 20 keV for scattering (diffraction) experiments requiring high energy resolution and high angular resolution. The principle optical setup of the beamline consists of a vertically and horizontally focusing mirror and a fixed-exit double crystal monochromator [Si(III)].

the experimental facilities consist of two independent diffractometers each optimized for specific types of experiments:

Station 1: A heavy-duty 3-circle powder diffractometer capable of carrying multiple detector systems and sample loads up to approx.80 kg, designed for in-situ characterization of nanocrystalline andmicrocrystalline materials under non-ambient conditions. This diffractometer is equipped with 2 main detectors: a 165 mm 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. 5 kg loads and equipped with either analyzer or Soller collimator optics for high angular resolution studies. This instrument can also optionally carry the CCD or 1D linear detectors.

A number of sample environments are available for heating and cooling of samples in both reflection and transmission geometry (up to around 1000°C in oxygen atmospheres). A tensile/compression stage (2kN) is also available for in-situ mechanical deformation studies.

Figure 5: heating chamber (MRI) for XRD (Bragg-Brentano) under vacuum or in gas atmospheres.

Figure 6: heating chamber for XRD (glass capillary, transmission).Figure 7: tensile testing stage and CCD camera setup for extension of thin films, transmission XRD.


PDIFF


ContaCtCONtaCt

Stephen Doyle: [email protected] +49 (0)721 608 28194 Udo Krieg: [email protected] +49 (0)721 608 28372

Beamline +49 (0)721 608 26648

KEY PARAMETERS OF THE BEAMLINE

Energy / Wavelength range 6 - 20 keV / 2.1 - 0.62 Å

Energy resolution [∆E/E] ≈ 2x10-4 (at 10 keV)


Optics Upward reflecting Rh-coated cylindrical mirror (fixed horiz. focus, variable vert. focus), Si(111) double-crystal monochromator

Flux at 1st sample position ≈ 1010 photons/(s x 0.1%bw) in 1 mm2 @ 10 keV

Typical beam cross section (fwhm) 0.6 mm (H) x 0.3 mm (V) (focused) at the 3-circle diffractometer2 mm (H) x 0.3 mm (V) (focused) at the 4-circle instrument

Experimental setup / sample environment

1) 3-circle powder diffractometer (2θ1, 2θ2, θ(Ω)) with 2D and 1D detectors2) Kappa-diffractometer with 3 sample orientation circles (Ω, Κ, Φ) anddetector circle (2θ) equipped with Ge(111)-anaylzer

Experimental setup / detectors 1) Princeton Instruments 2084x2084 pixel CCD-camera, INEL 90° linear detector, 2xMythen 1K fast silicon strip detectors, scintillation detectors with optionally analyser, slits or Soller collimators

Software / Data treatment / Databases / Evaluation

Spec instrument control, ICSD, PDF-2-search-match, TOPAS, SimRef, SHELX, FullProf, Crystallographica, Matlab, Origin etc.

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Single crystal diffraction (SCD): Yields electron density maps and atomic coordinates within the asymmetric unit of the unit cell of a single crystal.

Single / multiple anomalous dispersion (SAD/MAD) to determine the scattering phases from the anomalous signals of heavy atoms in vicinity of absorption edges.

Wide angle x-Ray scattering (WAxS) to derive pair distribution functions of soft condensed matter. WAxS, particularly suited for the investigation of structural properties of polymers, provides information about the order within the crystalline regions of a sample and about the fraction of crystalline material.

Reciprocal space mapping, x-Ray reflectometry, grazing incidence diffraction, grazing incidence small angle scattering and similar methods for the study of surface and interface structure are currently under commissioning using the 6-circle diffractometer.

Scientific applications The SCD beamline allows structure determination of large crystallized molecules with lattice parameters up to approximately 20 nm. The high incoming photon flux and low beam divergence allows for taking data from small or weakly diffracting crystals or with higher resolution. Sample sizes typically range between (0.1 mm)³ and (0.5 mm)³, but structures have been derived from crystals as small as 20 µm x 20 µm x 250 µm. The versatile scattering geometry of a six-circle diffractometer facilitates ex-situ diffraction studies of surfaces and interfaces. Crystal structure determination: Knowledge of the structure is a key to understanding the properties of nanoscaled materials, such as artificial self-assembling porphyrins, semiconductor cluster crystals, or high-nuclearity transition-metal aggregates. The synthesis and structure investigation of self-assembling porphyrins mimicking chlorosomal bacteriochlorophylls (see Figure 1 for just one example) is a potential major design step towards artificial antennae capable of harvesting sunlight.

For semiconductor cluster crystals, the detailed knowledge of the cluster structure allows in connection with other physical measurements for the establishment of correlations of structure and properties. High-nuclearity transition-metal aggregates may have magnetic properties intermediate between those of small finite aggregates and extended solids. Magnetic interactions can depend critically on metal-ligand bond lengths and angles within the bridges between the metal centers. By determining such geometries to a good level of precision the structure and magnetic behaviour can be correlated.Making use of the instrument capability to measure Bragg reflections with high redundancy, it has been demonstrated at ANKA-SCD that the anomalous signal of sulfur in cubic Insulin is sufficient to determine scattering phases and derive the electron density map with SAD at an incoming wavelength as short as 0.1 nm.

Semiconductor surfaces and interfaces: Surface and interface properties of structured semiconductors play a crucial role in applications such as blue laser diodes. Lattice relaxation at interfaces can be studied by Reciprocal Space Mapping. Grazing Incidence Diffraction and Grazing Incidence Small Angle Scattering have been used to investigate nanostructured surfaces and quantum dots on semiconductor surfaces and nanostructured surfaces.

Available methods, obtainable parameters

SCDSingle crystal X- ray diffraction beamline


Figure 1: Crystal Structure of 5-hydroxyethyl-15-acetyl-Zn-Por.Balaban, T. S. et al., Chemistry - A European Journal 11, 2267-2275 (2005).

Beamlines

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

SCD is a beamline on a dipole magnet source, dedicated to structure determination of single crystals.



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Figure 2: Schematic layout of the SCD beamline.

Gernot Buth: [email protected] +49 (0)721 608 26185 Volker Heger: [email protected] +49 (0)721 608 23313

Beamline +49 (0)721 608 26723

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Beamlines

Instrumental parameters and equipment, infrastructure The SCD beamline optics comprise an x-ray mirror with bending mechanism and a sagittally bent 2nd crystal, together allowing to focus the beam on the sample crystal in both directions. The beamline offers an energy range from 4 keV to 20 keV. This covers the K-edges from Ti to Mo, and L-edges from I to U, enabling Multiple Anomalous Dispersion (MAD) phasing with the most common heavy atom derivates, e.g., Se, Br, Hg, Au, Ag, Pt, W, Zn, Fe.

three end stations are available: One six-circle diffractometer with a linear or a (YAP or NaI) point detector, one CDD-Detector and one image plate for large area exposure.

Figure 4: Experimental end station with image plate

Figure 5: Experimental end station CCD. Figure 3: Beamline optical components.


SCD


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*Intensity drops considerably on both ends of the spectrum, below about 6 keV due to air and window absorption and above about 17 keV due to limitations of the DCM crystal bending radius and the bending magnet spectrum

KEy PaRaMEtERS OF tHE BEaMLINESource 1.5 T Bending magnet (EC = 6 keV)

Energy range 4 keV - 20 keV → Ti to Mo K-edge, I to U L-edge*

Energy resolution [∆E/E] Si (111): 3.5 x 10-4 @ 9 keV

Optics Flat Rh coated Si mirror with bending mechanism, double crystal monochromator with bender on the 2nd crystal

Beam size at sample Approx. 2 mm (hor) x 1 mm (ver), depending on focusing conditions

Flux at sample position Si(111): 3x10+10 ph/s/0.1%bw in 1 mm2 @ 9 keV

Experimental setup / sample stage

One 6-circle diffractometer with additional 2 circle analyzertwo diffractometers with ω, fixed χ, φ - circles

Experimental setup / sample environment

N2 cryo cooler (80 K - 400 K, 0.1 K accuracy, Oxford Cryosystems)

Experimental setup /detectors Mythen 1K PSD, NaI and YAP point detectors (6-circle diffractometer)Ø 340 mm Image Plate (STOE IPDS 2)62 mm x 62 mm CCD ( < 2 sec.total read time, (60 µm)2 resolution, Bruker AxS SMART APEx)Energy resolving SDD for fluorescence scans, 140 eV resolution @ 5.9 keV (Ketek AxAS)

Software / Data treatment / Evaluation

spec, PyMca, x-AREA, x-RED, x-SHAPE, APEx2

Gernot Buth: [email protected] +49 (0)721 608 26185 Volker Heger: [email protected] +49 (0)721 608 23313

Beamline +49 (0)721 608 26723

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Beamlines

IMaGE/XMICin commissioning

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

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.

FLUO | INE | IR1 | IR2 | SUL-x | UV-CD12 | WERA | xAS | MPI | NANO | PDIFF | SCD | IMaGE | TOPO-TOMO | LIGA I, II, III


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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 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-

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

End section will be installed with a wiggler insertion device from Daresboury Synchrotron. The first diagnostic elements are currently under construction.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.

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

CONtaCt

Tilo Baumbach: [email protected] +49 (0) 721 608 26820Sondes Bauer: [email protected] +49 (0)72160 82-6489

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).

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KEy PaRaMEtERS OF tHE BEaMLINEEnergy range 3 keV - 65 keV

Energy resolution [∆E/E] Beamline operational in white beam, pink beam (10-2- 10-3) and monochromatic beam (10-4) mode.

Proposed source Superconducting wiggler (Bmax=3.2 T, K=13.5, Ec=13.1 keV) / undulator (Bmax=0.86/K=1.2, Ec=2.36 keV) W200

Source size (HxV) [sigma] σH= 0.825 mm, σV= 0.024 mm, can be reduced to 5 µm x 5 µm by slits at intermediate focus position

Optics The fan of the wiggler will be split using a crystal monochromator which will reflect the beam laterally. This will give two branches using the same source. The optics of the monochromatic side branch will consist of vertically and horizontally focusing mirrors and diagnostic elements while the main branch will be operational in white, pink and monochromatic beam and. It will be composed of two pairs of slits, DCM, DMM and dia-gnostic modules.

Simulation of the beam profile at sample positi-

on at the main branch in white beam

beam size of 120 mm (hor) x 30 mm (vart)

Simulation of the beam profile at sample positi-

on at the main branch in DCM beam

Experimental setup Three experimental stations are planned:• One experimental station will be constructed at the side branch and will be dedicated to

hard x-ray microscopy including different imaging modes like absorption, phase contrast and scanning combined with fluorescence,

• The second experimental station dedicated to white beam fast tomography will be built on the main branch,

• The third experimental station dedicated to diffraction enhanced imaging will be installed at the main branch.

Beamlines

IMaGE/XMICin commissioning

FLUO | INE | IR1 | IR2 | SUL-x | UV-CD12 | WERA | xAS | MPI | NANO | PDIFF | SCD | IMaGE | TOPO-TOMO | LIGA I, II, III


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Instrumental characteristicsThree main experimental stations will be implemented for microscopy, diffraction imaging and tomography/laminography.

As 2D detectors, CCD-based detector systems with different, interchangeable optics systems (to provide different spatial resolutions / pixel sizes) will be used. CMOS and frame-transfer CCDs suited for fast real-time imaging at the new beamline are already under extensive commissioning at ANKA today. The FReLoN 2K14 CCD detector, already in use at ANKA, offers a unique combination of fast readout and high dynamic range which ideally matches the requirements of both real-time and slower, high-sensitivity studies.

Moreover, new detector concepts could be applied to improve measurement speed: hybrid pixel arrays, for example based on GaAs or CdTe sensor layers, have high quantum efficiency and allow energy discrimination in white-beam mode.A double-multilayer monochromator will provide selectable energy in a range between 3 and 40 keV. An additional double-crystal monochromator will be used to obtain a reduced energy window and to access higher x-ray energies up to 65 keV (compatible with the superconducting undulator/wiggler).

To attain spatial resolutions on the sub-μm scale, an ultra-precise sample manipulator with precise sample positioning during a scan is required. Laminography needs an adjustable tomographic rotation axis for imaging of flat, laterally extended objects. An automatic sample changer system allows one to prepare a series of samples which can be scanned unattendedly, maximising sample through put.

Since phase-contrast imaging is a major point of interest, the beamline optical devices and windows are subjected to stringent requirements concerning surface properties (e.g. flatness) and bulk properties (e.g., lack of inclusions and residual porosity). A polished CVD diamond window close to the experiment is the only interfering element in the beamline (differentially pumped vacuum tube). The coherence conditions can be improved by aperture slits in the front end.

CONtaCt

Tilo Baumbach: [email protected] +49 (0) 721 608 26820Sondes Bauer: [email protected] +49 (0)72160 82-6489

Experimental setup / detectors

Indirect and direct converting area detectors, resolution 1 µm to 50 µm

Software / Data treat-ment / evaluation

SPEC, MAVI (Modular Algorithms for Image Analysis), Volume Graphics VGStudioMax, PyHST, ITK/VTK, IDL, MatLab

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Microtomography and microradiography allows, in a non-destructive manner, to image the internal structure of an object. Microtomography using synchrotron light sources delivers three-dimensional (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:

• detection of voids and pores in industrial components;• imaging tissue and other soft materials in biological and life

science;• pore formation in metal foams, evolution of particle coarsening

in materials science;• crack propagation;• characterization of fibre structures, porous media, particle

agglomerations by microtomography and a subsequent 3D• image analysis;• diffusion processes in woven materials.


tOPO-tOMO X-ray topography and tomography beamline

Scientific applications The TOPO-TOMO beamline, designed and constructed with the support of the Crystallographic Institute of the University of Freiburg, provides optimal conditions for white-beam Laue topography. A large distance of 30 m between the x-ray source and the sample position as well as the possibility to reduce the effective source size by a pair of slits near the source ensure good transverse coherence, i.e., high angular resolution.

Synchrotron 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:

• large area sample mapping giving a full image of strain/defect topography of the sample;

• cross-sectional slice images through the sample (in a manner analogous to TEM);

• 3D directionality of crystal defects;• fine lateral resolution (<1 µm) over large areas.

Figure 1: Schematic layout of the TOPO-TOMO beamline.

Beamlines

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

The TOPO-TOMO beamline currently hosts the topography experimental station and the microradiography and microtomography setup for white beam and monochromatic X-ray imaging.

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


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Figure 2: X-ray diffraction imaging metrology of a 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 wafer edge, (c) t = 326 sec: <110> slip bands from the wafer edge and defects without dislocation loop formation, (d) t = 442 sec: Defect near the centre of a widely dislocation free area.

Figure 5: 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: Volume rendering of the head of a newt larva (Euproctus platycephalus).

CONtaCt

Thorsten Müller: [email protected] +49 (0)721 608 29217Beamline +49 (0)721 608 26649

Figure 3: TOPO-TOMO-grating-interferometer: 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.

White 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 (compare Figure 2). Also very small local defects like nm-scale voids in Si can be imaged as well as long range strain in electronic devices.

Phase contrast imaging with a grating interferometer (Figure 3) provides determination of the refractive index distribution within a sample even for materials with similar refractive indices. 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.

Available methods, obtainable parameters, physical propertiesHigh-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 3D information with a spatial resolution down to the sub-micrometer range by means of computed microtomography (compare Figure 4 and 5). 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.

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Instrumental Characteristics Good coherence conditions and low background are realized by aperture slits in the front end, 25 m away from the sample. A polished Be-window close to the experiment is the only x-ray optical element in the beamline. A set of in-vacuum filters on two independent sliders can be used to change the spectral distribution of the white beam. A Double-Multilayer Monochromator (DMM) with two independent stripes - Si/W and Si/P4B on Si substrate - is installed. With monochromatic radiation, quantitative absorption and phase contrast imaging can be exploited, being sensitive to material and atomic numbers and to the local electron density.

Two motorized tables are installed in the beamline, each one dedicated to a specific class of experiments, so that switching between experimental geometries can be done by simple exchange of the optical tables, which minimizes the required time for set up.

The TOPO table is dedicated for experiments with white-beam topography and grating interferometry. Equipped with a positioning tower from miCos, it allows mapping of large Si wafers with a diameter of 450 mm by white-beam topography. Furthermore, due to high resolution x-ray slits, a large beam up to a horizontal dimension of 80 mm is available, which is especiall suitable for section topography.

The TOMO table (Figure 6), a fast white-beam tomographic imaging station, allows tomographic scans based on radiographic projection images with spatial resolution up to 2.5 µm (“microscope”) or large field of view (5 mm x 15 mm, limited by the beam size) and moderate spatial resolution in the order of 10 µm (“macroscope”). The setup is equipped with a robot for fast sample exchange eliminating the necessity of entering the experimental hutch for switching between samples (compare Figure 6).

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).

Figure 6: TOMO table for tomographic experiments equipped with a robotic system for automated sample exchange.

BeamlinesFLUO | INE | IR1 | IR2 | SUL-x | UV-CD12 | WERA | xAS | MPI | NANO | PDIFF | SCD | IMAGE | tOPO-tOMO | LIGA I, II, III

tOPO-tOMO


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KEy PaRaMEtERS OF tHE BEaMLINE

Energy range 6 keV - 40 keV

Energy resolution [∆E/E] White light and optional 2% bandwidth

Source 1.5 T Bending magnet (EC = 6 keV), 2 mrad horizontal, 0.5 mrad vertical

Source size 800 µm x 200 µm (FWHM, horizontal x vertical), can be reduced to 5 µm x 5 µm with slits

Distance source - sample 30 m

Optics Primary slits (in the front end, 5 m from the source)Secondary slits (26.5 m from the source)Be window, 0.25 mm thick, polished (27.5 m from source)

Monochromator Double-Multilayer Monochromator (DMM) providing a monochromatic beam with a bandwidth of approx. 2% over an energy range from 6 keV to 40 keV (peak flux 1011 ph/s/mm2 @ 200 mA ring current, between 10 and 20 keV). Adjustable beam offset.

attenuators Filter stage 1: Al 1mm; Al 0.2 mm; Be 0.6 mmFilter stage 2: Cu 0.05 mm; Al 0.5 mm; Be 0.2 mm

Flux at sample position ~1x1016 ph/s (10 mm x 10 mm), white beam

Beam size at sample up to 80 mm (horizontal) x 6 mm (vertical)

Sample environment Inert gas, air

Detectors Photographic films (sub-µm resolution, field of view: approx. 15 x 20 cm2),Scintillator, coupled via microscope optics to a CCD (high dynamic range, PCO4000, 9 µm pixel size, or FReLoN 2k14bit, 14 µm pixel size) or CMOS (fast imaging, Photron SA-1, 20 µm pixel size), two optics available: macroscope (1.4x, 3.6x) and microscope (3x, 5x, 10x, 25x, 50x).Typical working parameters are:25 x 17 mm2 field of view at a pixel size of 6.4 µm (PCO + macroscope M = 1.5x);10 x 7 mm2 field of view at a pixel size of 2.5 µm (PCO + microscope M = 3x);1.4 x 0.9 mm2 field of view at a pixel size of 0.35 µm (PCO + microscope M = 25x).

Software Instrument control: SPEC / PCO CamWare / TANGO camera server Topography data analysis: Orient-Express Tomography data visualization: VG Studio Max, Amira, AVS Express, Avizo, CINEMA 4D & Deep Exploration Image processing: IDL, MatLab, Octave Image analysis: MAVI, ImageJTomographic reconstruction: PyHST, Octopus

CONtaCt

Thorsten Müller: [email protected] +49 (0)721 608 29217Beamline +49 (0)721 608 26649


ContaCt

LIGa I, II, III X-ray lithography beamlines

Micro-Fabrication

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Micro-Fabrication

Scientific applications In x-ray lithography an x-ray mask is copied into an x-ray sensitive resist by synchrotron radiation via shadow printing. The resist thicknesses range from 5 µm up to several millimeters thick layers. x-rays from a synchrotron radiation source are used primarily to penetrate those thick layers, while keeping the top to bottom dose-ratio in a specific range, and due to their high parallelism, allowing the fabrication of very high vertical microstructures with a side wall roughness in the optical range ( ≤ 20 nm).

The x-ray mask consists of an x-ray transparent membrane, such as a 2.5 µm thick titanium membrane or a 500 µm thick beryllium sheet, and gold absorber structures to stop incoming x-rays. The contrast of the mask and therefore the thickness of the gold absorbers has to be sufficient to reduce the top dose in the resist below the minimal deve-loping dose underneath the gold absorber structures and to reduce the dose from secondary electrons produced at the boundary layer in the substrate, by x-rays penetrating the gold absorber structures and absorbed in the metallic substrate. Otherwise sidewall attacks by the chemical developer and insufficient adhesion of freestanding resist structures occur.

The combination of e-beam writing and x-ray mask making with synchrotron radiation allows the fabrication of structure details as small as 200 nm in 200 µm resist layers. Those structure details are not achievable by any other x-ray mask making method (e.g., laser writing and UV-lithography).

LIGa I, II, III X-ray lithography beamlines

Available methods, obtainable parameters, physical propertiesAligned exposures for pre-structured substrates are available and used on a routine basis. Moveable micro structures are fabricated using the sacrificial layer technique, where a pre-structured titanium interface on the substrate is selectively etched against the metallic microstructure. Structures with different level heights are processed by using micro milled and drilled substrates. At LIGA II an external alignment system is available, while an internal alignment system is installed at LIGA I. In both cases, the pre-structured substrates are aligned relative to the x-ray mask via a microscope and pattern recognition hard- and software for fast and accurate alignment. An instrumental accuracy of 0.5 µm has been measured.

Beamlines

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

The microstructure laboratory at ANKA consists of three beamlines for X-ray lithography, each dedicated to a specific task in the LIGA-process, which are high resolution X-ray mask manufacturing (LIGA I), deep X-ray lithography (LIGA II) and ultra deep X-ray lithography (LIGA III). The whole laboratory is placed inside a clean room for accurate environment conditions. The experimental equipment, together with the microstructure fabrication capabilities at IMT/KIT, is a unique installation for high precision and high aspect ratio microstructure fabrication.

Figure 1(a): High resolution X-ray mask fabricated at LIGA I, smallest structure detail 200 nm.

Figure 1(b): Crossed X-ray lens structures fabricated at LIGA II, height 500 µm.

Figure 1(c): 200 µm thick nickel gear beneath a 1600 µm UDXRL resist structure, fabricated at LIGA III.

Examples of deep x-ray lithography structures fabricated at ANKA:

FLUO | INE | IR1 | IR2 | SUL-x | UV-CD12 | WERA | xAS | MPI | NANO | PDIFF | SCD | IMAGE | TOPO-TOMO | LIGa I, II, III


Commercial Services

Martin Börner: [email protected] +49 (0)721 608 24437Pascal Meyer: [email protected] +49 (0)721 608 23924

Franz Josef Pantenburg: [email protected] +49 (0)721 608 22600Beamline +49 (0)721 608 26855

CONtaCt

Figure 2: Beamlines LIGA I and II use grazing incidence mirrors; a chromium-coated silicon mirror for sub-µm lithography and mask making (LIGA I) and a nickel-coated silicon mirror for standard deep X-ray lithography (LIGA II).

Figure 3: Schematic layout of the LIGA III beamline. LIGA III uses the white synchrotron radiation from a dipole magnet.

Figure 4: Opened experimental hutch of LIGA II with the exposure station inside. Outside (front): Control Rack of LIGA II.

Figure 5: Look into the exposure station: X-ray litho-graphy mask and a 4 “ - wafer with PMMA coating could be seen.

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Accelerator / Insertion devices Commercial ServicesUser Service

Beamlines

ANKA control system

Micro-Fabrication

Key parameters of the beamlines

LIGa I LIGa II LIGa III

Energy range 2.2 keV - 3.3 keV 2.5 keV – 12.4 keV > 2.5 keV

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

Distance: source point -mirror

8.61 m 9.20 m -

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

20 mm (vertical) x 110 mm (horizontal)

20 mm (vertical) x 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

FLUO | INE | IR1 | IR2 | SUL-x | UV-CD12 | WERA | xAS | MPI | NANO | PDIFF | SCD | IMAGE | TOPO-TOMO | LIGa I, II, III


Commercial Services

Martin Börner: [email protected] +49 (0)721 608 24437Pascal Meyer: [email protected] +49 (0)721 608 23924

Franz Josef Pantenburg: [email protected] +49 (0)721 608 22600Beamline +49 (0)721 608 26855

CONtaCt

Instrumental characteristics Three beamlines are installed and equipped with state-of-the-art x-ray scanners, fabricated by JenOptik in collaboration with IMT/KIT.

Each beamline is dedicated to a specific task:

• High resolution X-ray, • Mask fabrication, • Deep X-ray lithography and ultra deep X-ray lithography.

The white spectrum from ANKA dipole magnets is tailored to the energy range of interest (LIGA I, LIGA II) using grazing incidence mirrors as low energy pass-filters and low-Z filter foils, mounted in a filter chamber, as high energy pass-filters (Figure 6). LIGA III uses the white beam tailored only by the needed windows and filters.

A homogeneous synchrotron radiation fan of 108 mm width is

available at all scanner locations. Exposures are performed under a 100 mbar He atmosphere. The high precision x-ray scanners move the mask/resist-package with a speed of up to 50 mm/sec vertically through the synchrotron radiation beam to achieve a homogenous exposure field across the microstructure design window on the x-ray mask. An additional tilting device mounted on top of the vertical stage allows the fabrication of inclined microstructures. A tilting of up to 60° with accuracy of 0.05° is available. The combinations of inclined and vertical microstructures are realized by multiple irradiation inserting mechanically fabricated apertures in front of the x-ray mask. These apertures are adapted to the design of the microstructures and allow the irradiation of special areas of the x-ray mask. A repeatable overlay accuracy of apertures and x-ray masks of 30 µm have been measured.

Figure 6: Available spectral distributions at different X-ray lithography beamlines at the mask plane. While LIGA III uses the white synchrotron radiation spectrum of a dipole magnet, LIGA I and LIGA II use grazing incidence mirrors as low energy pass filter. Due to the high energy cut-off, X-ray masks with thinner gold absorbers and therefore higher accuracy can be used, leading to very precise microstructure products.

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aNKa USER SERVICE

The Karlsruhe Institute of Technology (KIT) runs ANKA as an attractive, highly efficient user facility and employs the broad, multi-disciplinary expertise of different KIT institutes to support the needs and demands of external users.

Calls for proposals are published every 6 months in scientific journals and distributed widely to universities, research centers and scientific associations. Beamtime is granted to external users free of charge via an independent peer review procedure, on the condition that the results will be published in scientific journals. The proposals are graded by a peer-review committee compromised of external experts according to their scientific excellence and technological relevance. In addition to regular proposals, applicants can apply for long-term projects and rapid access.

Cooperative research groups (CRGs) are institutions that operate their own beamlines or experimental stations and allow a certain beamtime fraction to be allocated via peer review or commercial services.

European networks, in which ANKA or its participating institutes are involved provide access to ANKA beamtime for other consortium members. Networks include the Integrating Action on European Light Sources Activities (CALIPSO) and European Infrastructure for Micro and Nano Fabrication and Characterization (EUMINAfab).

ANKA offers optimal conditions for industrial use of synchrotron radiation by rapid-access schemes and professional, industry-oriented project management. Methods development, projects with inherent scientific risk and long-term research projects for systematic studies can be conducted. The various modes of access for users and customers to ANKA are illustrated and described in Figure 2.

Commercial access is provided to customers by ANKA Commercial Service (ANKA-CoS).

Accelerator / Insertion Devices Commercial ServicesUser Service

Beamlines

ANKA Control System

Figure 1: Poster session at ANKA & KNMF Users’ Meeting


Jacqueline Heinrich: [email protected] +49 (0)721 608 26188 Margit Costarelli: [email protected] +49 (0)721 608 26288Commercial Services

CONtaCt

COLLaBORatIVE RESEaRCH GROUPS

Figure 2: Graphical representation of the five access routes to beamtime at ANKA, via Calls for Proposals, Karlsruhe Institute of Technology in-house research in the HGF programs, collaborative research groups (CRGs), European networks and ANKA Commercial Services.

EXtERNaL PaRtNERS OF tHE KIt’S INStItUtES

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Proprietary industrial use of synchrotron radiation is one of the major tasks of ANKA. Therefore, special attention is given to industrial users by our dedicated business team.

ANKA Commercial Services (ANKA-CoS) provides users from industry an exclusive and fast access to synchrotron radiation and ensures a professional execution of projects.

ANKA-CoS

aNKa Commercial Services


Beamlines


CoS

User Service

• Wide range of services available, ranging from data collection to full data analysis and interpretation.

• Experienced, support team at ANKA will support you no matter what problems you have

• Combined use of different methods to solve research and development issues

• Fast access to beam time (usually < one month)

• Attractive prices for one hour of radiation, long-time use with quantity discount, or individual full service offerings

• Confidentiality

• Access to the wide range of expertise at the Karlsruhe Institute of Technology

Figure 1: ANKA CoS exhibition booth


Services and business fields

• Synchrotron analytics and diagnostics: Chemical analysis Material diagnostics Non-destructive testing

• Synchrotron technology: Superconducting undulators X-ray compound refractive lenses

• LIGA micro-fabrication: Direct LIGA prototyping Replication, e.g., from polymer Development for serial production

The professional, customer oriented approach of ANKA-CoS has been certifitied by DIN EN ISO 9001:2000.

Commercial Services

CONtaCt

Dr. Manuella Werp: [email protected] +49 (0)721 608 28664Michael Drees: [email protected] +49 (0)721 608 26866

CONtaCt

Publisher: ANKA Synchrotron Radiation Facility, Karlsruhe Institute of Technology, a member of the Helmholtz Association. IPS, Institute for Photon Science and Synchrotron Radiation Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany

Publication date: September 2013

Reproductions: Allowed for individuals and non-profit organizations for non-commercial use only. Quoting from the report in the standard manner with proper referencing is permitted.

ANKA Instrumentation Book 2012 - KITThe vacuum system of the ANKA storage ring is made from...

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