High Count Rate Electron Probe Microanalysis

Reducing the measurement uncertainty of quantitative analyses made using electron probe microanalyzers (EPMA) requires a careful study of the individual uncertainties from each definable step of the measurement. Those steps include measuring the incident electron beam current and voltage, knowing the angle between the electron beam and the sample (takeoff angle), collecting the emitted x rays from the sample, comparing the emitted x-ray flux to known standards (to determine the k-ratio) and transformation of the k-ratio to concentration using algorithms which includes, as a minimum, the atomic number, absorption, and fluorescence corrections. This paper discusses the collection and counting of the emitted x rays, which are diffracted into the gas flow or sealed proportional x-ray detectors. The representation of the uncertainty in the number of collected x rays collected reduces as the number of counts increase. The uncertainty of the collected signal is fully described by Poisson statistics. Increasing the number of x rays collected involves either counting longer or at a higher counting rate. Counting longer means the analysis time increases and may become excessive to get to the desired uncertainty. Instrument drift also becomes an issue. Counting at higher rates has its limitations, which are a function of the detector physics and the detecting electronics. Since the beginning of EPMA analysis, analog electronics have been used to amplify and discriminate the x-ray induced ionizations within the proportional counter. This paper will discuss the use of digital electronics for this purpose. These electronics are similar to that used for energy dispersive analysis of x rays with either Si(Li) or Ge(Li) detectors except that the shaping time constants are much smaller.