New and Exciting at Bruker - MIT - Massachusetts Institute...
Transcript of New and Exciting at Bruker - MIT - Massachusetts Institute...
Liquid Metal – are you out of your mind?
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Imagine A high-performance X-ray source
• With a target that can not melt from power overload
• No need to spin a couple of pounds of copper at close to 10,000 rpm under high vacuum
• No water cooling – no water seals to change
• No “long-life” ceramic ball bearings to change
• No ferro-magnetic fluid seals to change
• No piercing noise
METALJET – Liquid Metal Jet X-ray source
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• X-ray source developed in collaboration with Excillum
• Multilayer optic HELIOS MX developed by Incoatec
• Integrated with the D8 VENTURE enclosure, KAPPA goniometer and PHOTON 100 detector
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D8 VENTURE with METALJET
• METALJET X-Ray Source• High-intensity Ga-Kα X-ray beam• 70 micrometer 7.5 mrad• Completely Air-cooled• Anode is always fresh with closed
loop of liquid Ga-rich Alloy • No Moving Parts
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D8 VENTURE with METALJET
• METALJET @ 200 W, 7.5 mrad
• µ-RAG @ 2.5 kW, 7.6 mrad
• Up to 3 times more flux compared to the high end TXS microfocus rotating anode
The METALJET – how does it work
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• The impact of electrons on the gallium target generate X-rays
• The solid anode of traditional sources is replaced by a high-speed jet of liquid gallium
• The liquid-metal surface is constantly regenerated to provide a fresh and smooth target
• The liquid metal can accept a much higher power load compared to a solid target
• The resulting X-ray beam is much brighter than any current home X-ray source
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METALJET- components
High-pressure Ga loop
Shutter electronics
Electron gun
Turbo pump
HELIOS MX
Focusing coil
HELIOS MX for Ga - A New Level of Precision and Quality
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• Advancements in X-ray source and optic have to go hand in hand
• Preserving the extreme source brightness requires an optic of highest quality
• More than a decade of experience in the field of synchrotron mirrors enabled Incoatec to develop a synchrotron-class optic for a home-lab instrument
• State-of-the-art graded multilayer deposition techniques make the HELIOS MX for METALJET our best X-ray mirror ever.
Gallium -The Better Copper
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• The METALJET target is a gallium-rich alloy with the Kα emission line of 1.34 Å
• Gallium provides the necessary diffraction spot spacing for accurate and reliable data reduction
• Less radiation damage with shorter-wavelength allow high-multiplicity data sets
• The very small beam and gallium’s shorter wavelength greatly improve the signal-to-noise ratio
• Increased detector sensitivity • Reduced X-ray absorption by the
sample, scattering by air and mother liquor
Extreme Brightness
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• The power-loading capability of microfocus X-ray targets scales with the diameter of the electron beam’s focus
• The brightness is inversely proportional to the source diameter
• By combining extreme power-loading capability with a small electron focus, a liquid-jet source can achieve unprecedented brightness at micron spot sizes
Best source stability for the smallest spot
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• Very high spatial stability of the source
• Spot position centroid standard deviation of smaller than 0.1 µmover 24 hours
• Monitored with a pinhole camera mechanically coupled to the source.
Smaller Samples Require More Stable Systems
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• The D8 VENTURE perfectly matches the demands of the small beam generated by the METALJET
• The smaller the beam, the more stable and accurate the entire experimental setup needs to be
• All goniometer axes intersect within a sphere of just seven micrometers
• The crystal remains perfectly centered in the X-ray beam during the entire data collection process
• Downstream alignment, allows easy alignment of the entire system.
• The anomalous signal for Ga-Kα is weaker than that from Cu-Kαbut significantly higher than that from Mo-Kα
Absolute configuration from GaKα
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F”(CuKα) F”(GaKα) F”(MoKα)
Cl 0.70 0.53 0.16
S 0.56 0.44 0.12
O 0.032 0.023 0.006
• Selected F” - values
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• Highest X-ray intensity - exclusive patented liquid-metal-jet technology. The liquid target is able to accept a power loading greater than conventional rotating X-ray sources
• Unprecedented brightness - extremely high power loading and smallest electron focus
• Perfect spot quality - the high-brightness LaB6 cathode and smooth, self-regenerating, liquid-metal target which provides exceptional spatial and emission stability
• Lower noise - the shorter-wavelength gallium Kα X-rays result in reduced background scatter
• Lower running costs - low power consumption, minimal cooling requirements, and the self-regenerating target
• Lower maintenance - advanced design for serviceability and the use of best components with highest reliability
THE METALJET Wrap-Up
PHOTON 100Shutterless data acquisition and continuous scans
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Michael RufProduct Manager [email protected]
PHOTON 100 Detector
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• Large 100 cm2 sensor for fast and efficient data collection
• Low-power consumption sensor for high reliability
• Air-cooled for low maintenance• High sensitivity• No glass fiber taper for superior
spatial accuracy• Optimized pixel size and point
spread function for superior signal• Large pixel volumes for best light
conversion• Shutter-less operation and
continuous scan mode for best data acquisition efficiency
• 3-year warranty
Shutterless data collection for unprecedented acquisition speed and data quality
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• On-camera data processing for best efficiency
• All the necessary image corrections are applied in a special real-time processor in the camera electronics
• The output data are fully corrected
• Facilitates operation of the detector in a true dead-time-free shutterless mode with continuous sample rotation
FPGA - Field-programmable gate array
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• Configured after manufacturing—hence "field-programmable".
• Large resources of logic gates and RAM blocks to implement complex digital computations
• fine-grained parallelism• Doing 4 operations at once
doesn't count; 1024 does• Ideal for pipelining
• A pipeline is a set of data processing elements connected in series, so that the output of one element is the input of the next one.
• Create a pipeline by dividing a complex operation into simpler operations.
Shutterless data collection for unprecedented acquisition speed and data quality
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• Shutterless data acquisition for overhead-free data collection
• data is read out while the camera is exposed to X-rays
• Eliminates the need to open and close the X-ray shutter
• Eliminates to stop, reposition and start the goniometer
• Eliminates mechanical jitter• In shutterless mode the sample
is constantly exposed to X-rays and continuously rotated which maximizes data acquisition efficiency
• Superior data quality in less time is possible today
PHOTON 100 Detector readout
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• Two sensors are read out in parallel
• Readout is pixel per pixel and row per row
• Readout of an 1024 ×1024 array takes 0.8 s
• Readout and on-camera processing are performed in less than one second
PHOTON 100 frame acquisitionone cycle
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expose
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• On-camera frame processing pipeline for overhead-free data acquisition
• Frame exposure and read-process-write are performed in parallel for overhead-free data acquisition
PHOTON 100 shutterless frame acquisitiontwo cycles
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expose
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• Frame exposure and read-process-write are performed in parallel for overhead-free data acquisition
PHOTON 100 shutterless frame acquisitiontwo cycles
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• 12 images collected and written in 13s
PHOTON 100 shutterless frame acquisitioncontinuous
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• 2 images collected and written in 12s
CCD correlated frame acquisition
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• 24 images collected with the PHOTON 100• 4 images collected with a CCD detector
PHOTON 100 - fast and efficient
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3s/3°Shuttered and shutterless diffraction images
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• -2 11 5 phi: 12°to 15°• -1 1 8 phi: 12°to 15°
-2 11 5
-1 1 8
-2 11 5
-1 1 8
Shuttered Shutterless
• -2 11 5 phi: 12.115° to 15.115°-1 1 8 phi: 12.182° to 15.182°
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• The skew for a reflection is negligible and orders of magnitudes smaller than the crystal mosaicity
• For the extreme case to the right of 3s/3°the skew of a reflection is only 0.002°
• For a typical 10s/0.5°image the skew for a reflection is only about 0.0001°
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What about skew? – Not an issue!
-2 11 5
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• Data acquisition and processing of shutterless data is completely transparent to the user
• Indexing routines have been modified to accommodate shutterless diffraction images
• Data integration has been adjusted to accommodate shutterless diffraction images
Data processing
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• The PHOTON 100 shutterless data acquisition mode allows data collection in a fraction of the time compared to “shuttered” mode.
• Data quality is always matched or even exceeded and always can be improved further by collecting data with higher multiplicity
• Compared to large-format CCD detectors the factor for time saving can increase to a factor of up to eight
• The shutterless data acquisition mode of the PHOTON 100 will start a paradigm shift from “improving data quality through increased exposure time” to “increasing data quality through increased multiplicity”
Shutterless data collection
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For Internal Use Only
• ECOlogical, ECOnomical
• Air cooled PHOTON 50 detector
• Sealed tubes operated at 1 kW – no external chillers needed
• Extension of the D8 QUEST crystallography solutions family
• Full experimental flexibility
The New D8 QUEST ECO
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D8 QUEST ECO Configuration
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• Sealed tube X-ray tube• Flat graphite monochromator• TRIUMPH (optional)• FIXED-CHI goniometer
• <7 micron Sphere of Confusion
• Manual track• PHOTON 50• Shutterless operation• All-air-cooled configuration• APEX2 software including ShelxTL
2012• XPRESSO –automation module• Windows7 PC• Linux (optional)• Low-temperature device (optional)
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The New D8 QUEST ECOPHOTON 50 CMOS Detector
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• Two times larger than a typical CCD chip
• 1:1 detection for up to 6 times higher sensitivity
• Zero-maintenance • No blooming, no streaking• better handling of strong reflections• Improved low-resolution data quality
compared to CCD• Shutterless operation
X-ray Source
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• For Mo & Cu• Automatic burn-in of X-ray
tubes to facilitate maximum tube lifetime
• Ramp-up and ramp-down to stand-by of the X-ray generator by software
• Top Hat profile, ideal for service crystallography
• State-of-the-art safety features
• Fully compliant with Machinery Directive 2006/42/EC
• TRIUMPH delivers 3.5 more intensity)
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• ECOnomical• Affordable • Low maintenance• 3-year warranty for KFF X-ray tubes (tube failure, ECO only)• 3-year warranty on PHOTON detector• 10-year warranty for the goniometer (ECO only)
The New D8 QUEST ECO
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