It's cute (可爱)……… But does it DO anything??.

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Presentation transcript:

It's cute (可爱)……… But does it DO anything??

Powder diffraction - applications Qualitative analysis - what IS this stuff?!! Every material has a unique x-ray powder pattern Every PHASE has a unique powder pattern This image, taken under a microscope, shows that a 'duplex stainless steel' has two phases - austenite (AUS) & ferrite (FE) AUS FE This is the X-ray diffraction pattern

Powder diffraction - applications Qualitative analysis - what IS this stuff?!! The X-ray diffraction pattern tells us this AUS FE How?

Powder diffraction - applications Qualitative analysis - what IS this stuff?!! We use the Powder Diffraction File database (the PDF) and a search system History 1938 Hanawalt paper on first database and search method 1941 ASTM committee publishes database on cards 1969 JCPDS incorporated; publishes the JCPDF

Powder diffraction - applications Qualitative analysis - what IS this stuff?!! We use the Powder Diffraction File database (the PDF) and a search system History 1938 Hanawalt paper on first database and search method 1941 ASTM committee publishes database on cards 1969 JCPDS incorporated; publishes the JCPDF 1977 JCPDS became the International Centre for Diffraction Data (ICDD) - currently publishing various databases, including the new PDF-4, with diffraction and structure data for >240,000 phases

Powder diffraction - applications Qualitative analysis - what IS this stuff?!! Make d, I list: 2.080 100 1 1.081 30 6 2.025 100 2 1.040 12 1.798 45 4 1.018 20 8 1.433 20 0.907 35 5 1.272 26 7 0.898 3 1.170 50 3 0.830 14 Do search/match

Powder diffraction - applications Qualitative analysis - what IS this stuff?!! Example of page of search manual for Hanawalt manual search/match

Powder diffraction - applications Qualitative analysis - what IS this stuff?!! Do search/match Make d, I list: 2.080 100 1 1.081 30 6 2.025 100 2 1.040 12 1.798 45 4 1.018 20 8 1.433 20 0.907 35 5 1.272 26 7 0.898 3 1.170 50 3 0.830 14 1 2 3 - no match 1 2 4 - no match 1 2 x - no match 1 3 4 - no match 1 3 5 - no match 1 3 x - no match 1 4 5 - no match 1 4 6 - MATCH!

Powder diffraction - applications 1. Qualitative analysis Quantitative analysis Crystal structure determination Crystallite size Microstrain Residual macrostresses ?

stress = modulus x strain Powder diffraction - applications 1. Qualitative analysis Quantitative analysis Crystal structure determination Crystallite size Microstrain Residual macrostresses stress = modulus x strain  = E  (Hooke's law)

Powder diffraction - applications Residual stress Reflections shift position (d-values change under stress)

Powder diffraction - applications Residual stresses

Residual stress Suppose isotropic solid loaded in uniaxial tension Can measure change in interplanar spacing for planes reflecting as above d = (d - do)/ do - this is the strain   = (1/E) ( - ( + )) -  is Poisson's ratio  = - (1/E)  - so, can get stress 

 =  (1 + )/E sin2  /E)( +  Residual stress Biaxial & triaxial stress states more complicated Stress state resolved differently along different directions in sample, so peak shifts change w/ direction       =  (1 + )/E sin2  /E)( +  

Residual stress Measurement procedure - classical technique - sin2  Diffractometer must have two more rotations - and       

Residual stress Measurement procedure - classical technique - sin2     

 =  (1 + )/E sin2  /E)( +  Residual stress Measurement procedure - classical technique - sin2  slope  =  (1 + )/E sin2  /E)( +   sin2  Need E,  - measure or calculate

Powder diffraction - applications 1. Qualitative analysis Quantitative analysis Crystal structure determination Crystallite size Microstrain Residual macrostresses Thin films

Powder diffraction - applications Thin films

Powder diffraction - applications Thin films

Powder diffraction - applications Thin films

Powder diffraction - applications Thin films

Powder diffraction - applications Thin films Can rotate film and still get reflection

Powder diffraction - applications Thin films

Powder diffraction - applications 1. Qualitative analysis Quantitative analysis Crystal structure determination Crystallite size Microstrain Residual macrostresses Thin films Crystallinity 9. Studies of phase diagrams A. Phase boundaries B. Solid solutions C. Phase transitions 10. Studies of chemical reactions and identification of reaction products. 11. Determination of grain sizes. 12. Preferred orientation in polycrystalline bodies. 13. Many more