Structural properties and nitrogen-loss characteristics in sputtered tungsten nitride films

• Published in: Thin solid films Vol. 372; no. 1; pp. 257 - 264
• Main Authors: Shen, Y.G, Mai, Y.W, McBride, W.E, Zhang, Q.C, McKenzie, D.R
• Format: Journal Article
• Language: English
• Published: Lausanne Elsevier B.V 01.09.2000; Elsevier Science
• Subjects: Composition and phase identification; Condensed matter: structure, mechanical and thermal properties; Cross-disciplinary physics: materials science; rheology; Deposition by sputtering; Exact sciences and technology; Magnetron sputtering; Materials science; Methods of deposition of films and coatings; film growth and epitaxy; Nitride thin films; Nitrogen; Physics; Surfaces and interfaces; thin films and whiskers (structure and nonelectronic properties); Thin film structure and morphology; Tungsten; Nitride thin films; Magnetron sputtering; Nitrogen; Tungsten; Inorganic compounds; Phase studies; Transition element compounds; Crystallization; Tungsten nitrides; Experimental study; Nonstoichiometry; Thermal stability; Columnar structure; Characterization; Thin films; Magnetrons; Chemical preparation; Chemical composition; Reactive sputtering; Microstructure; Thermal annealing
• ISSN: 0040-6090; 1879-2731
• DOI: 10.1016/S0040-6090(00)01041-5

A combination of X-ray photoelectron spectroscopy (XPS), parallel electron energy-loss spectroscopy (PEELS), X-ray diffraction (XRD), transmission electron microscopy (TEM) and transmission electron diffraction (TED) were used to investigate structural properties and nitrogen-loss characteristics of thin WN x films prepared by reactive magnetron sputtering of tungsten in an Ar–N 2 gas mixture. XRD θ−2θ scans combined with plan-view and cross-sectional TEM showed that the as-deposited WN x films were amorphous in structure . Annealing of the as-deposited films at 600°C or above resulted in crystallization of the amorphous phases, forming either a two-phase structure consisting of W 2N and b.c.c. W or a single-phase structure of W 2N, which was related to the initial nitrogen concentration in the films. The 150-nm thick crystalline films near a stoichiometry of W 2N had a columnar microstructure with an average column width of 15–20 nm near the film surface, whereas the column grains were larger for substoichiometric films. Thermal stability and nitrogen-loss characteristics of nitride films were also studied by in situ annealing in the TEM and PEELS system. The results indicate that between 600 and 800°C the W 2N phase was stable. Nitrogen in the film started to evaporate to vacuum at approximately 820°C and was fully released after 900°C annealing.