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Silicon crystals containing aluminum have been annealed at various temperatures within the range 700° to 1350°C, particular emphasis being given to the range 1200° to 1300°C. Precipitation, which occurs during the heat treatment in the bulk crystal and on various structural defects, has been detected by transmission optical microscopy. A lowering of the aluminum concentration in the neighborhood of the precipitate particles after heating at 1250°C has been revealed at the surface by a novel technique involving the etching of crystals which also contain phosphorus, where internal cylindrical and planar p‐n junctions are formed round individual dislocations and grain boundaries, respectively. At this temperature, no precipitation is observed on dislocations in plastically deformed crystals. The precipitation of aluminum is interpreted in terms of a chemical reaction involving the coprecipitation of oxygen and possibly carbon.