Using small‐angle scattering, together with density measurements, X‐ray diffraction, nitrogen adsorption, and both transmission and scanning electron microscopy, the microstructural evolution during sintering in nanostructured ceramic oxides has been studied. The availability of samples with sufficient size and uniformity has permitted absolute calibration of the scattering data and made possible determinations of microstructural parameters and surface areas that are statistically representative of the undisturbed nanophase morphologies. A fully quantitative microstructural model has been developed, and the effects of varying processing parameters during powder synthesis and sintering have been assessed. Predictions are made regarding the achievable sintered full‐density microstructures.

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