(Ti1−XAlX)N coatings were deposited by plasma enhanced chemical vapor deposition (PECVD) method using a gas mixture of TiCl4, AlCl3, NH3, H2 and Ar. X‐ray diffraction and transmission electron microscopy were used to investigate the structure of the deposited (Ti1−XAlX)N coatings. They showed single phase NaCl‐structure up to X=0.8, while a mixed phase of NaCl type (Ti0.2Al0.8)N and AlN with würtzite‐structure was observed for 0.8<X<1.0. The lattice parameter changed linearly with the function X (d=4.241−0.197 X Å) in the single phase region. Metastable AlN particles with an NaCl structure and a lattice parameter of 4.03 Å were found on AlN coatings produced by PECVD using AlCl3, NH3 and H2. It was assumed that the formation of (Ti1−XAlX)N solid solution in a wide concentration range occurred due to the metastable AlN. When (Ti1−XAlX)N coatings were heat‐treated at 1000 °C, AlN with a stable würtzite structure precipitated. However, the broadened x‐ray diffraction peak and the diffuse transmission electron microscopy diffraction patterns indicated that the amount of precipitation was not the same for each (Ti1−XAlX)N grain.

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