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Elemental dispersive x-ray (EDX) composition distribution mapping using a scanning electron microscope (SEM) provides information about samples that is complementary to that obtained from X-ray diffraction. Examples are given (e.g., Ba and Cu maps of YBa2Cu3O7 − δ, see figure) to demonstrate the usefulness of this technique in evaluating the homogeneity of sol-gel products and in elucidating elemental zoning (see also cover picture).