1. Application Report Dr. Ya-Ching Yang phone: (02)86981212 #205

2. Experiments with New D2 PHASER
The measurements were made with the D2 Phaser diffractometer (θ-θ).
Every samples were measured in the Bragg-Brentano geometry.
The LynxEye fast linear detector was used for all measurements.
The powder samples were prepared in a standard PMMA sample holder (cavity diameter 25 mm and 1 mm depth).
The bulk samples were prepared in a standard PMMA sample holder (cavity diameter 40 mm and 5 mm depth).
The few amount powder samples & thin film samples were prepared in a standard Si low background sample holder.
PMMA sample holder
Si Low Background Sample Holder

3. Configuration of the diffractometer
Bragg-Brentano Geometry
Goniometer
D2 PHASER Theta/Theta
Measurement circle
300 mm
Tube
300W Cu ceramic sealed tube
Tube power
30 KV / 10 mA
Primary optics
0.6° Fixed divergence slit
2.5° Soller Slits
Air scatter screen
Secondary optics
Ni filter
Detector
LynxEye detector (5° opening)

4. The LynxEye fast linear detector
Silicon strip technology Active area 14.4mm x 16mm, 192 Si channels of 75m each
Suitable for wavelengths ranging from Cu to Cr
>98% efficiency for Cu radiation
Energy resolution ~ 25%
Max. Count rate, global: >108 cps
Max. Count rate, local: >7x105 cps
Dynamic range > 7 106cps
Maintenance free
Can withstand the primary beam
Angular resolution comparable to a scintillation detector with 0.1mm receiving slit
LynxEye TM detector

5. APPLICATION 1 Fluorescence Powder

6. Phase Identification in DIFFRAC.EVA

7. Quantitative Analysis in TOPAS
A phase quantification (based on the Rietveld method, see next slides) was performed using the TOPAS software.
The final phase ratio (in wt%) is displayed on the picture.

8. APPLICATION 2 Lanthanide Powder

9. Sample 1110.raw – XRD patterns
The sample was measured from 20o(2θ) to 90°(2θ) with a step size of 0.02°(2θ) .
The counting time was 0.5 sec per step.

10. Phase Identification in DIFFRAC.EVA

11. Quantitative Analysis in TOPAS
Blue: raw data
Red: calculated curve

12. APPLICATION 3 Mg2Si Alloy

13. Quantitative Analysis in TOPAS

14. Quantitative Analysis in TOPAS

15. APPLICATION 4 Lithium Battery Material

16. Quantitative Analysis in TOPAS

17. Quantitative Analysis in TOPAS

18. Quantitative Analysis in TOPAS

19. APPLICATION 5 Silicon Ingot Powder

20. Sample Si3N4_1
A phase identification was performed with the Diffrac.EVA software in combination with the PDF4+ database.
Obviously, the sample contains two allotropic (alpha and beta) forms of Si3N4.

21. Sample Si3N4_1
Adjusting the height of the sticks to the measured intensity, a semi-quantitative estimation of the phase is automatically performed (based on I/Icor coefficients).
The sample contains about 88.8 wt% alpha-Si3N4 and 11.2 wt% beta-Si3N4.

22. Quantitative Analysis in TOPAS
A phase quantification (based on the Rietveld method, see next slides) was performed using the DiffracPlus TOPAS software.
The final phase ratio (in wt%) is displayed on the picture. It is in very good agreement with semi-quantitative result.

23. Sample SiC
A phase identification was performed with the Diffrac.EVA software in combination with the PDF4+ database.
The sample contains two allotropic forms of SiC: 6h and 15R.
Traces of quartz and silicon could also be detected.

24. Sample SiC
Adjusting the height of the sticks to the measured intensity, a semi-quantitative estimation of the phase is automatically performed (based on I/Icor coefficients).
The sample contains about 85 wt% SiC-6H, 14.3 wt% SiC-15R and traces of quartz and silicon.

25. Quantitative Analysis in TOPAS
A phase quantification (based on the Rietveld method, see next slides) was performed using the DiffracPlus TOPAS software.
The final phase ratio (in wt%) is displayed on the picture. It is in good agreement with semi-quantitative result.

26. APPLICATION 6 Refractory Material

27. Quantitative Analysis in TOPAS

28. Quantitative Analysis in TOPAS

29. Quantitative Analysis in TOPAS
高溫時，Corundum相消失

30. APPLICATION 7 MLCC (Multilayer Ceramic Capacitor) Material

31. Quantitative Analysis in TOPAS

32. Quantitative Analysis in TOPAS

33. APPLICATION 8 Fuel Cell Material

34. Phase Identification in DIFFRAC.EVA

35. Quantitative Analysis in TOPAS

36. Quantitative Analysis in TOPAS

37. LMSR Structure

38. APPLICATION 9 ZnO Powder

39. Crystallite Calculation in TOPAS
Crystallite size determined by whole pattern with structure is ~110 Å

40. Crystallite Calculation in TOPAS
Crystallite size determined by single line profile fitting with FP is ~135 Å

41. APPLICATION 10 Bio Material

42. Phase Identification in DIFFRAC.EVA
Ca5(PO4)3(OH)-SG: P63/m (176) ,a= , c=
Ca3(PO4)2, SG: R-3c (167) ,a= ,c=

43. TOPAS analysis
Peak phase analysis with FPA function Great GOF and its Rwp down to 7.8%(<10%)

44. TOPAS analysis
Amorphous phase contents around 45%

45. TOPAS Analysis
Deconvolution of Ca5(PO4)3(OH) Phase
CS:247.9nm

46. APPLICATION 11 Thin Film Application

47. Phase Identification in DIFFRAC.EVA
CIGS/Mo/Glass

48. Phase Identification in DIFFRAC.EVA
ITO/Glass

49. Samples Before Laser Annealing
GST/Glass

50. Samples After Laser Annealing
GST/Glass

51. Search/Match Results by DIFFRAC.EVA
GST/Glass

52. Comparison of Four Thin Film Diffractions GST/Polymer
Film thickness 50nm
Measuring Condition:
Sample
1.raw
2.raw
3.raw
4.raw
Step size
0.1o
0.05o
Exposure time
0.5 sec
1 sec
2 sec