Version November 16, 2009.ppt

Electron probe microanalysisEPMA EPMA of Particles What’s the point? Bulk vs particle Normal EPMA assumes that the electron beam is exciting a homogeneous volume, i.e. there is no difference either laterally or vertically. Thus, the matrix correction is being applied in a uniform matter, and there is one applicable f(rz) profile for each element. However, particles create many difficulties, including: The Good, the Bad, the Ugly Most operators of electron microprobes, using WDS, understand the difficulties of trying to do EPMA on non-flat surfaces (particles). However, the real problem is that there are probably 100 EDS systems on SEMs for every 1 WDS on an electron microprobe. And with SEMs and EDS systems so easy to operate, a large number of users make major errors without knowing it, assuming whatever the software spits out as a composition is really what it is. After these slides, you should know the difference between the GOOD, the BAD, and the UGLY… particle analyses. Size: “Mass Effect” Size: Absorption Effect Absorption effect of non-flat upper surface: there is a different path length from the normal flat geometry. In this case, the emergent x-rays will travel ~50% shorter distance in the material, and thus have ~50% of the absorption, and all else being equal, will yield a K-ratio twice as large as it would be if it were larger and had a flat polished surface. Size - Detector-sample Geometry EDS (shown to right): Variable effect of geometry of trajectory between beam impact area on non-uniform surface and the location of the detector. K-ratios from point 1 could be significantly different than those from point 3, despite the sphere being of uniform composition. WDS: Could be as bad, with up to 5 spectrometers positioned at 5 different orientations EDS vs WDS For all the problems cited, EDS has an advantage over WDS for “particle analysis” in that the spectrometer is in a constant position relative to the sample and beam “landing spot”, whereas WDS