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Formation process of AlN from urea and aluminum chloride hexa‐hydrate (N/Al = 60) under nitrogen is investigated. An aluminum hexa‐urea complex crystallizes on mixing the two raw materials at room temperature. The complexes react with excess urea and/or its decomposed products, such as biuret above 160°C, and form an amorphous phase containing Al,N,C, and O around 400°C after releasing volatile products...