Data Collection with. VÅNTEC-2000 Detector

Transcription

1 Data Collection with IµS Source and VÅNTEC-2000 Detector

2 D8 System Configuration for Reflection Microfocus Source IµS Optics with Housing 2D Detector (VÅNTEC-2000) DHS 900 Heating Stage Sample Stage Bruker D8 GADDS with IµS

3 Comparison: IµS & VÅNTEC-2000 vs. Classical Setup Sample: Corundum standard Detection time: 100s, detector to sample distance: 158 / 154 mm Sealed Tube System IµS XRD 2 hybrid Cu X-ray: 40kV, 40mA with 40mm Göbel mirror collimator: 0.3mm Cu X-ray: 45kV, 0.65mA, collimator: 0.3mm snout total counts: 1,235K total counts: 78K

4 Comparison of Intensities Optics Incoatec BAXS ST BAXS ST Collimator 0.3mm 0.8mm 0.3mm Frame Intensity (CPS) 12.3K 10.2K 0.78K Peak intensity (CPS) Corundum (104) FWHM

5 IµS & VÅNTEC-2000 symmetrical reflection 600 sec collection time sample to detector 15 cm The five fingers of quartz 300 Sample: quartz powder Lin (Counts)

6 Resolution on Lab6 Sample 60 seconds sample-detector distance 29.2 cm FW HM of LaB6 sample fitted with PV function 105, ,000 95,000 90,000 85,000 80,000 75,000 70,000 65,000 60,000 55,000 50,000 45,000 40,000 35,000 30,000 25,000 20,000 15,000 10,000 5, ,

7 Citric Acid, Measured in Transmission with IµS and VÅNTEC IµS focused on the Vantec 2000 detector - 15 sec collection time

8 Citric Acid, Measured in Transmission with Sealed Tube and 0.3mm Collimator - Sample-detector distance 29 cm mm collimator - VÅNTEC-2000 detector sec collection time

9 Citric Acid, Measured in Transmission Lin (Counts) Sample-detector distance 29 cm mm collimator sec collection time Theta - Scale File: citric acid trans 300 col_00 [001].raw - Step: Step time: 120. s (*) - Citric acid - C6H8O7

10 Comparison IµS and Sealed Tube System: Citric Acid, Measured in Transmission Lin (Cps) Theta - Scale File: citric acid trans 300 col_00 [001].raw - Step: Step time: 120. s File: citric_acid3.raw - Step: Step time: 15. s (*) - Citric acid - C6H8O7 - Sample-detector distance 29 cm mm collimator - VÅNTEC-2000 detector - The scan was multiplied by a factor o 56 for comparison - IµS with focusing optics focused on detector. The intensity gain depends on the available sample amount and was at least 100 times higher for this example. - The lower signalbackground is caused by the improvised beam stop.

11 VANTEC-2000 Detector, Sealed Tube: Citric Acid, Measured in Transmission Comparison 0.3 mm and 0.1 mm Collimator Lin (Counts) Sample-detector distance 29 cm - VÅNTEC-2000 detector mm collimator mm collimator Step: Step time: 120. s Step: Step time: 600. s (*) - Citric acid - C6H8O7 2-Theta - Scale

12 VANTEC-2000 Detector: Citric Acid, Measured in Transmission Peak Fit with PVII Function - Sample-detector distance 29 cm - VÅNTEC-2000 detector mm collimator - The FWHM values (blue labels on the peaks) are slightly lower compared to LaB6 because of the transparency effect (the sample was not thin enough).

13 Comparison: Ibuprofen IµS & VÅNTEC-2000 vs. Classical Setup Sealed Tube 0.3 mm collimator Sample-detector distance 29 cm 120 sec collection time IµS XRD 2 focusing optic 2mm X 2mm on sample, and 200 um spot focused on detector Sample-detector distance 15 cm 15 sec collection time

14 Ibuprofen, measured in transmission Comparison IµS - Sealed tube Lin (Counts) Theta - Scale File: ibuprofen trans 300 col va_00 [001].raw - Step: Step time: 120. s File: ibuprofen_3.raw - Step: Step time: 15. s (*) - Ibuprofen - C13H18O2 - Sealed tube - Sample-Detector distance 29cm - 0.3mm collimator - Vantec 2000 detector - IµS with optic focused on detector. Resolution is comparable to a measurement with 300μm collimator at 30cm distance. - Better relative intensities because of improved crystallite statistics

15 Comparison: Gabapentin IµS & VÅNTEC-2000 vs. Classical set-up Sealed Tube Sample-Detector distance 29cm 0.3mm collimator VÅNTEC-2000 detector 120 sec collection time IµS XRD 2 focusing optic 2mmX2mm on sample, and 200um spot on detector 15 sec collection time

16 Gabapentin, Measured in Transmission Lin (Counts) Theta - Scale Step: Step time: 120. s - File: gabapentin 25 cm trans_00 [001].raw Step: Step time: 15. s - File: gabapentin_2.raw - Sample-detector distance 29 cm - 0.3mm collimator - VÅNTEC-2000 detector - IµS with optics focused on detector. Resolution is comparable to a measurement with 300 μm collimator at 30 cm distance.

17 Comparison for Screening Applications Sealed tube system with primary beam monochromator, collimator and VÅNTEC-2000 detector Resolution depends on collimator size and detector distance loss of intensity for good resolution, 2 frames may be necessary Poor crystallite statistics that gets worse for smaller collimators Better resolution possible with 0.1 collimator or below Microsource with optic focused on VÅNTEC-2000 detector Resolution depends on sampledetector distance, one frame has enough coverage for pharmaceutical applications, even if good resolution is required Larger sample area is irradiated Better crystallite statistics and intensities, if enough sample is present Resolution depends on focusing length of optic

18 Sample: Diclofenac Sodium Salt - Sample-detector distance 29 cm - Measurement time: 100 sec mm collimator - VÅNTEC-2000 detector

19 Sample: Diclofenac Sodium Salt 3000 Lin (Counts) Sample-detector distance 29 cm - Measurement time: 100 sec mm collimator - VÅNTEC-2000 detector Theta - Scale DSS [001] - File: DSS_01 [001].raw (Q) - Diclofenac sodium - C14H10Cl2NNaO2 - Y: % - d x by: 1. - WL:

20 Sample: Naproxen - Sample-detector distance 29 cm - Measurement time: 100 sec mm collimator - VÅNTEC-2000 detector

21 Sample: Naproxen Lin (Counts) Sample-detector distance 29 cm - Measurement time: 100 sec mm collimator - VÅNTEC-2000 detector naproxen [001] - File: naproxen_01 [001].raw (C) - Naproxen - C14H14O3 2-Theta - Scale

22 Sample: Ibuprofen Tablet in Transmission - Sample-detector distance 29 cm mm collimator sec measurement time

23 Comparison of Ibuprofen Brands Lin (Counts) Measurement of whole tablets in transmission Comparison of integrated data Promising configuration for QC applications of final products File: ibuprofen_tablet_01 [001].raw File: walgrenn_ibuprofen_tablet_01 [001].raw (*) - Ibuprofen - C13H18O (N) - beta-lactose - C12H22O11 2-Theta - Scale

24 Non-Ambient Scans of PbO Particles Temperature: 50ºC to 600ºC Ramp rate: 30ºC/min Temperature step: 50ºC/frame Data collection: 120 seconds/frame

25 PbO Sample Integrated Oatterns Lin (Counts) Theta - Scale 900 Lin (Counts) Theta - Scale PbO - File: PbO_ raw - Temp.: 50 C PbO - File: PbO_ raw - Temp.: 100 C PbO - File: PbO_ raw - Temp.: 150 C PbO - File: PbO_ raw - Temp.: 200 C PbO - File: PbO_ raw - Temp.: 250 C PbO - File: PbO_ raw - Temp.: 300 C

26 PbO Sample Integrated Pattern Lin (Counts) Lin (Counts) Theta - Scale Theta - Scale PbO - File: PbO_ raw - Temp.: 350 C PbO - File: PbO600_01.raw - Temp.: 600 C PbO - File: PbO_ raw - Temp.: 400 C PbO - File: PbO_ raw - Temp.: 450 C PbO - File: PbO_ raw - Temp.: 500 C PbO - File: PbO_ raw - Temp.: 550 C

27 IμS for SAXS Experiments with D8 System

28 Experimental setup VÅNTEC-2000 detector was positioned such that the source to detector distance equals the focal distance of the optics. E31 focusing optics was used. A 2 mm wide stripe of lead tape was mounted directly at the detector face as a beam stop. The sample was positioned right after the optics exit. The beam size at the optics exit is supposed to be around 1 mm (because 1mm slits were used to eliminate single reflected beam and the white beam) The beam size at the focal position is supposed to be around 0.15mm Samples measured: AgBh (also used for calibration) Glassy Carbon Duck tendon

29 Silver Behenate Sample Measured intensity I(q) 1e+6 1e+5 1e+4 1e+3 1e+2 Raw data Strong reflections are visible from the Silver Behanate The experimental beamstop in the center is clearly visible. An intermediate radius (between min and max) was used for the calibration of the sample to detector distance. Sample to detector distance was cm Measurement time: 30 s 1e q [Å -1 ]

30 Glassy Carbon Intensity [a.u.] GC The 2D scattering image of glassy carbon The graph shows the background corrected profile after integration in a chi direction of 120 deg. The background was measured under the same conditions. Measurement time: 10 sec The profile of GC looks as expected. Benefits: linear intensity range 2 theta range The minimum q value corresponds to a real space dimension of about 230 Å q [Å -1 ]

31 Duck Tendon 2e+5 Raw data 2D Scattering pattern of duck tendon The integration was performed in a narrow section (30 deg in chi) Peaks of the collagen fibers are visible but the air scattering background dominates. Measured intensity I(q) 2e+5 1e+5 5e q [Å -1 ]

32 Summary - IµS is the ideal X-ray source for many spot-focus applications - Parallel or focusing optics for reflection or transmission geometry are available - For measurements, the X-ray flux density is about 5 to 1000 times higher than conventional seal tube with Single Göbel mirror optics depending on the configuration and sample properties - IµS and VÅNTEC-2000 is an ideal configuration for combinatorial screening applications in transmission (more sample volume irradiated, better 2 theta coverage, intensity and resolution) - IµS is also a very promising source for small angle scattering applications.

33 Incoatec GmbH: INnovative COAting TEChnologies Spin-off of the GKSS Research Center Geesthacht, near Hamburg Founded as joint venture with Bruker AXS in 2002 > 12 years of experience in X-ray optics and > 18 years of experience in thin film technology 1/13

34 Products & Services Multilayer mirrors (WDXRF, TXRF, Goebel, Montel) Customized coatings for synchrotron mirrors < 150 cm Incoatec s Microfocus Source IµS TM Upgrades of existing equipment 2/13

35 Incoatec Microfocus Source IµS TM The source Point focus source Spot size < 50 µm High brilliance Low power: 30 W Air-cooled No maintenance Easy tube change 3-year warranty Bright sealed tube for ultimate convenience 3/13

36 Incoatec Microfocus Source IµS TM The optics Latest generation of 2D beam shaping Montel Optics: The Quazar TM Optics 2D focusing or collimating or hybrid Patented easy-to-align housing with optional motors Very stable Optimized optics in Incoatec s new very stable and easy-to-align housing 4/13

37 How to improve the power density of a source? Reduce the focal spot - Increase the ratio of circumference to area of focal spot (1 / r) - Improve sideways heat dissipation Use rotating anodes - Rotate away the hot spot Do both 5/13

38 Power Densities Conventional sealed tube IµS Microstar rotating anode Power (W) 1, ,700 Focal size (mm 2 ) 0.4 x x x 1.5 Power density (W/mm 2 ) 469 5,429 18,000 6/13

39 Why improve the power density? Power density is proportional to brightness (brilliance) Brightness = flux density / divergence High brightness means higher flux density at lower divergence 7/13

40 Rotating anode mains cable IµS mains cable 8/13

41 Why IµS? Low power consumption; no maintenance; air cooled High brightness means higher flux density at lower divergence Compact tube design makes shorter distances between tube focus and optics possible This leads to a more efficient use of the X-rays emitted by a source (large capturing angles) 9/13

42 Capturing Angle Minimum d-spacing = 3 nm Minimum distance to source = 30 mm capturing angle (mrad^2) cm optics 10 cm optics 15 cm optics distance between source and mirror center (mm) 10/13

43 IµS models - Optics with 5 x 5 mrad 2 divergence for high flux density - Single crystal diffraction - Transmission powder diffraction - Optics with 1 x 1 mrad 2 divergence and moderate flux density - Small angle scattering - Optics with 1 x 5 mrad 2 divergence ( hybrid ) - Reflection powder diffraction - (high resolution) microdiffraction 11/13 Brightness = flux density / divergence

44 Single Crystal Diffraction with IµS TM Chemical Crystallography (Mo-K α, optic 5 mrad) Flux density: > 4x of 2 kw ST system* and > 1.2x of 4 kw RAG system* FWHM = 0.12 focus fold (integrated) intensity gain over 2 kw ST system* Excellent for small crystals Biological Crystallography (Cu-K α, optic 5 mrad) Flux density: > 1.5x of 4 kw RAG system** FWHM = 0.25 focus S-SAD Phasing, Protein screening Small molecule crystallography: ~ 10 2 (integrated) intensity gain over 1.5 kw ST system* Glucose 80 s/ : 1.50 Å 20 s/ : 1.41 Å 12/13 * plus graphite monochromator ** plus 1 st gen. multilayer mirrors

45 More XRD 2 Fabline and µ-hrxrd SAXS; Nanostar 13/13