1. The probe Some material used from:

2. EPMA - electron probe microanalysis Probe signals

3. EPMA - electron probe microanalysis 'New' signal - cathodoluminescence visible and near-visible radiation 'New' signal - cathodoluminescence visible and near-visible radiation Application: identify impurities in semiconductors

4. EPMA - electron probe microanalysis The instrument

5. EPMA - electron probe microanalysis Measuring x-ray wavelengths In Braggs' law, keep d constant (d is known) use single crystal (remember monochromator) In Braggs' law, keep d constant (d is known) use single crystal (remember monochromator) = 2d sin  Measure  to get - identify & quantify element Use curved single crystal for focusing Use curved single crystal for focusing

6. EPMA - electron probe microanalysis Measuring x-ray wavelengths Focusing or Rowland circle radius kept constant. Vary  by translating crystal away from specimen & rotating. Counter moved to stay near focus point on circle. Focusing or Rowland circle radius kept constant. Vary  by translating crystal away from specimen & rotating. Counter moved to stay near focus point on circle.

7. EPMA - electron probe microanalysis Qualitative Identify and characterize phases (shape, size, surface relief, etc.) Elements present in each phase Identify and characterize phases (shape, size, surface relief, etc.) Elements present in each phase Quantitative Complete chemical analysis on a sub-micro scale Elemental concentration mapping Complete chemical analysis on a sub-micro scale Elemental concentration mapping

8. EPMA - electron probe microanalysis Interaction volume details

9. EPMA - electron probe microanalysis Interaction volume Depth increases with accelerating voltage decreases with at. no. Depth increases with accelerating voltage decreases with at. no.

10. EPMA - electron probe microanalysis Interaction volume Diameter increases with probe current

11. EPMA - electron probe microanalysis Matrix corrections for quantitative x-ray analysis For a each element: C/C° ~ I/I° = k or: C/C° = k ZAF For a each element: C/C° ~ I/I° = k or: C/C° = k ZAF C = concn in specimen C° = concn in std I = intensity from specimen I° = intensity from std C = concn in specimen C° = concn in std I = intensity from specimen I° = intensity from std ZAF = matrix corrections Z - at. no. A - absorption F - fluorescence ZAF = matrix corrections Z - at. no. A - absorption F - fluorescence

12. EPMA - electron probe microanalysis Atomic no. correction Function of electron backscattering factor & electron stopping power - depend upon the average at. nos. of unknown and standard Function of electron backscattering factor & electron stopping power - depend upon the average at. nos. of unknown and standard Varies with composition and accelerating voltage

13. EPMA - electron probe microanalysis Absorption correction

14. EPMA - electron probe microanalysis Absorption correction A varies with , takeoff angle, accelerating voltage

15. EPMA - electron probe microanalysis Fluorescence correction electrons ––> primary fluorescent x-rays ––> secondary fluorescent x-rays

16. EPMA - electron probe microanalysis Fluorescence correction electrons ––> primary fluorescent x-rays ––> secondary fluorescent x-rays Varies with composition and accelerating voltage

17. EPMA - electron probe microanalysis Can't calculate ZAFs unless concns known. Use k values (I/I° = k) to estimate compositions of each element. Then calculate ZAFs, and refine by iteration Can't calculate ZAFs unless concns known. Use k values (I/I° = k) to estimate compositions of each element. Then calculate ZAFs, and refine by iteration

18. EPMA - electron probe microanalysis Micro scale elemental analysis

19. EPMA - electron probe microanalysis Micro scale elemental analysis Pd on particles

20. EPMA - electron probe microanalysis Micro scale elemental analysis

21. EPMA - electron probe microanalysis Micro scale elemental analysis