NEW POSSIBILITIES FOR X-RAY DIFFRACTOMETRY

Bernd Hasse – Incoatec, Geesthacht, Germany

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B. Hasse – PPXRD 2009, Glasgow2/22

Bright sealed tube for ultimate convenience

Incoatec Microfocus Source – IµS

The source

• Point focus sealed tube

• Cu, Mo, Cr, or Ag anode

• High brilliance

• Low power: 30 W

• Air-cooled

• Tube change as easy as for conventional sealed-tubes

• 3 Years warranty

B. Hasse – PPXRD 2009, Glasgow3/22

Optimized Optics in Incoatec‘s new very stable and easy-to-align housing

Incoatecs Microfocus Source – IµS

The optics and housing

• New family of 2D beam shapingMontel Optics: The Quazar Optics

• 2D focusing or collimating or hybrid (f+c)

• Patented housing with optional motors

• Stable positioning

B. Hasse – PPXRD 2009, Glasgow4/22

New Equipment for Diffractometry

Microfocus Source IµS

Optics with Housing

Sample stage

2D detector(VÅNTEC 2000)

Bruker D8 GADDSwith IµSTM

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IµSTM & VÅNTEC-2000

• symmetrical reflection

• 600 sec collection time

• sample to detector 15 cm

Sample: quartz powder

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D8 Discover with GADDS

IµSTM & VÅNTEC-2000

°2θ

The five fingers of quartz

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IµSTM for XRD with focusing optics

• measurements in transmission geometry

• with Bruker D8 GADDS and VÅNTEC 2000

B. Hasse – PPXRD 2009, Glasgow8/22

IµS (Cu-Kα) with focusing optics vs. classical setup

IµS – 2D focussing optics

• Spotsize 230 µm

• 0.3 mm snout

• small slice for integration to obtain better resolution (poor detector calibration)

15 sec collection time

Ibuprofen / measured in transmission geometry / Sample-Detector distance 290 mm

Sealed Tube – 1D collimating optics

• 0.3 mm collimator

120 sec collection time

B. Hasse – PPXRD 2009, Glasgow9/22

IµSTM focusing onto the detector: LaB6

FW HM of LaB6 sample fitted with PV function

403938373635343332313029282726252423222120

105,000100,000

95,00090,00085,00080,00075,00070,00065,00060,00055,00050,00045,00040,00035,00030,00025,00020,00015,00010,000

5,0000

-5,000

0.09174322 0.07588469 0.08700313

60 seconds, 292 mm sample-detector

FWHM: 0.08°2θ

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D8 DISCOVER with GADDS HTS (IµS):Combinatorial Screening Reflection & Transmission

B. Hasse – PPXRD 2009, Glasgow11/22

IµS (Cu-Kα) with collimating optics for SAXS measurementsSilver behanate (H3C-(CH2)20-COOAg) / Bruker AXS NANOSTAR / 3-Pinhole-geometry / 1000 s exposure time / 1035 mm detector distance

q

Total Intensity: 17.000 cps (IµS @ 30W)

For comparison:Sealed tube with cc-Göbel mirrors @ 1.4 kW: 3.300 cps

B. Hasse – PPXRD 2009, Glasgow12/22

IµS with a marDTB

B. Hasse – PPXRD 2009, Glasgow13/22

ASS with Cu-Kα

Whole tabletExposure time: 300 sFocusing onto the detector

B. Hasse – PPXRD 2009, Glasgow14/22

Temperature-dependent Phase Transition in Copper phthalocyanine

N

N

N

N

N

N

N NCu

• Heating from 30 °C to 350 °C with a rate of 0.75 K/min• Exposure time per frame: 240 s• Operation mode of mar345: 100 µm x 100 µm @ 240 mm

R.E. Dinnebier, M. Müller, MPI for Solid State Research, Stuttgart

B. Hasse – PPXRD 2009, Glasgow15/22

Results• Reaction Temperature:

- TR = 295 °C (Lab data)- TR = 275 °C (Synchrotron data)

• Activation Energy: - EA = 254 kJ·mol-1 (Lab data)- EA = 245 kJ·mol-1 (Synchrotron data)Calculated with the non-isothermal Avrami-theorie- EA = 241 kJ·mol-1 (isothermal investigation)

R.E. Dinnebier, M. Müller, MPI for Solid State Research, Stuttgart

B. Hasse – PPXRD 2009, Glasgow16/22

IµS (Mo-Kα) with focusing optics: LaB6

Frame integrated with Powder3DIPProfile Matching with FullProf

<FWHM> = 0.13°2θ

Sample-Detector Distance: 260 mm2θ: 30°Slitsize: 0.2 x 0.2 mm²Spot size: 110 µmExposure time: 1200 s

B. Hasse – PPXRD 2009, Glasgow17/22

Ibuprofen with Mo-Kα

Whole tablet in blister packExposure time: 120 sFocusing onto the detector

**

***

B. Hasse – PPXRD 2009, Glasgow18/22

Comparison of IµS (Mo-Kα) and IµS (Ag-Kα)

Mo Ag

End of measurement range for Mo-Kα

Sample: LaB6Exposure Time:

300 sDetector-Distance:

200 mm

B. Hasse – PPXRD 2009, Glasgow19/22

IµS (Ag-Kα) with focusing optics: Pigment Red 170 in diamond anvil cell

Exposure time: 1200 s

M. Schmidt, Uni Frankfurt/M; K. Friese, A. Grzechnik, Uni Bilbao

B. Hasse – PPXRD 2009, Glasgow20/22

Summary (1): XRD with IµS

Incoatec Microfocus Source IµS

• Microfocus Source• 30 W, air-cooled• New 2D - Quazar

Multilayer Optics• Low maintenance• for Cu, Mo, Cr, and Ag

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• 2D focusing beam• XRD in transmission• Well plate screening• Position sensitive

measurements• Single crystal

diffraction

Summary (2): XRD with IµS

• 1D collimating beam +1D focusing beam

• XRD in reflection• Texture• Phase identification

• 2D collimating beam• SAXS• Texture

Acknowledgement

All colleagues @ Incoatec GmbH

M. Schmidt, Frankfurt/M, Germany

K. Friese, A. Grzechnik, Uni Bilbao, Spain

R.E. Dinnebier, M. Müller, MPI for Solid State Research,Stuttgart, Germany

All colleagues from Bruker AXS