Abstract
Three types of problems related to nanometer-scale characterization are discussed with reference to heterogeneous catalysts. Changes occurring in air-sensitive samples, notably reoxidation of reduced metallic particles leading to flase size distributions, can be avoided by use of transfer devices and special preparation techniques. Specimen damage constitutes a greater problem and can only be overcome by degrading the available resolution. The possibility of correlating nanoanalysis with information obtained from larger-scale techniques is greatly enhanced by extending the use of ultramicrotome cross-sectioning, which can preserve positional information up to a millimeter scale, to this class of materials. The use of ultramicrotome sections has the added advantage of constant specimen thickness leading to increased dependability of X-ray analysis. An example is given of analysis of a bimetallic catalyst in comparison with electron probe microanalysis in which STEM confirms the EPMA results and provides in addition valuable particle-by-particle information relevant to catalytic preparation and performance.
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