This paper presents the results of the investigation of the grain structure formation in the intermetallic compound Ni3Al under conditions of its high-temperature synthesis under pressure in a powder mixture of nickel and aluminum of stoichiometric composition and the effect of grain size on the strength properties of the synthesized intermetallic compound. The grain structure was investigated by optical metallography, transmission electron microscopy, and EBSD analysis; the ultimate tensile strength of the intermetallic compound was investigated under the tension of the samples in the temperature range from 20 to 1000 °C. It was found that with a decrease in the grain size, not only does the tensile strength of the intermetallic compound multiply increases but also on the anomalous temperature dependence of the intermetallic compound strength there is a significant shift in the maximum strength value to the region of higher temperatures.
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