Application Report Dr. Ya-Ching Yang phone: (02)86981212 #205 email: yaching.yang@bruker.com.tw

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

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)

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

APPLICATION 1 Fluorescence Powder

Phase Identification in DIFFRAC.EVA

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.

APPLICATION 2 Lanthanide Powder

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.

Phase Identification in DIFFRAC.EVA

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

APPLICATION 3 Mg2Si Alloy

Quantitative Analysis in TOPAS

Quantitative Analysis in TOPAS

APPLICATION 4 Lithium Battery Material

Quantitative Analysis in TOPAS

Quantitative Analysis in TOPAS

Quantitative Analysis in TOPAS

APPLICATION 5 Silicon Ingot Powder

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.

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.

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.

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.

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.

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.

APPLICATION 6 Refractory Material

Quantitative Analysis in TOPAS

Quantitative Analysis in TOPAS

Quantitative Analysis in TOPAS 高溫時，Corundum相消失

APPLICATION 7 MLCC (Multilayer Ceramic Capacitor) Material

Quantitative Analysis in TOPAS

Quantitative Analysis in TOPAS

APPLICATION 8 Fuel Cell Material

Phase Identification in DIFFRAC.EVA

Quantitative Analysis in TOPAS

Quantitative Analysis in TOPAS

LMSR Structure

APPLICATION 9 ZnO Powder

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

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

APPLICATION 10 Bio Material

Phase Identification in DIFFRAC.EVA 34-0010 -Ca5(PO4)3(OH)-SG: P63/m (176) ,a=9.41480, c=6.87910 09-0169-Ca3(PO4)2, SG: R-3c (167) ,a=10.42900,c=37.38000

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

TOPAS analysis Amorphous phase contents around 45%

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

APPLICATION 11 Thin Film Application

Phase Identification in DIFFRAC.EVA CIGS/Mo/Glass

Phase Identification in DIFFRAC.EVA ITO/Glass

Samples Before Laser Annealing GST/Glass

Samples After Laser Annealing GST/Glass

Search/Match Results by DIFFRAC.EVA GST/Glass

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

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