History
The first reported preparation was in 1857 by Henri Etienne Sainte-Claire Deville and Friedrich Wöhler. In their method, silicon was heated in a crucible placed inside another crucible packed with carbon to reduce permeation of oxygen to the inner crucible. They reported a product they termed silicon nitride but without specifying its chemical composition. Paul Schuetzenberger first reported a product with the composition of the tetranitride, Si3N4, in 1879 that was obtained by heating silicon with brasque (a paste made by mixing charcoal, coal, or coke with clay which is then used to line crucibles) in a blast furnace. In 1910, Ludwig Weiss and Theodor Engelhardt heated silicon under pure nitrogen to produce Si3N4. E. Friederich and L. Sittig made Si3N4 in 1925 via carbothermal reduction under nitrogen, that is, by heating silica, carbon, and nitrogen at 1250–1300 °C.
Silicon nitride remained merely a chemical curiosity for decades before it was used in commercial applications. From 1948 to 1952, the Carborundum Company, Niagara Falls, New York, applied for several patents on the manufacture and application of silicon nitride. By 1958 Haynes (Union Carbide) silicon nitride was in commercial production for thermocouple tubes, rocket nozzles, and boats and crucibles for melting metals. British work on silicon nitride, started in 1953, was aimed at high-temperature parts of gas turbines and resulted in the development of reaction-bonded silicon nitride and hot-pressed silicon nitride. In 1971, the Advanced Research Project Agency of the US Department of Defense placed a US$17 million contract with Ford and Westinghouse for two ceramic gas turbines.
Even though the properties of silicon nitride were well known, its natural occurrence was discovered only in the 1990s, as tiny inclusions (about 2×0.5 microns in size) in meteorites. The mineral was named nierite after a pioneer of mass spectrometry, Alfred O. C. Nier. This mineral might have been detected earlier, again exclusively in meteorites, by Soviet geologists.
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