An automated particle analysis routine is implemented on an electron microprobe for analyzing the chemical composition and projective area of populations of individual silver halide microcrystals. An LN2 cryostage is used to prevent material degradation due to reaction with the impinging electron beam. The background in the EDX spectra is lowered by depositing the microcrystals on a carbon-coated copper grid, mounted in a transmission holder. The ILα/AgLα net X-ray intensity ratio, obtained from a spectrum-fitting algorithm, is used to determine the crystal composition by means of a standard-based calibration curve. The uncertainty on the concentration measurement of individual microcrystals is calculated using the uncertainties on the net X-ray counts and the uncertainties on the calibration curve. The area measurement is optimized by introducing a gray value histogram correction on each individual measurement. Overlapping microcrystals are scrapped from the analysis by defining a maximum shape factor, against which the shape factor of the microcrystal is tested. To minimize problems with drift of the cryostage, spectrum acquisition is carried out immediately after a single microcrystal has been located, based on the backscattered electron image. Several applications are discussed.

SummarySilver halide microcrystals are usually composed of different phases with varying halide compositions. These microcrystals can be sectioned with an ultramicrotome with a certain thickness in a specific direction. The scanning electron microscopical analysis of these sections provides information on the internal halide profile.During sample sectioning, many deformations can be induced in the material, and usually dominate the different scanning electron images.By acquiring X-ray maps, it is possible to locate the different phases in the sections. This technique, however, is very time-consuming, and can only be used when the local halide variations are very high.When an EDX line scan is acquired over the section, information on the position of the phases with different halide composition is obtained in a reasonable time, and shows no dependence on the section deformations. From this knowledge, several positions on the section are selected where local X-ray analyses are performed. After quantifying the results, the internal halide distribution is obtained. The analytical lateral resolution is about 30 nm for sections Ϸ100 nm thick.

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