Hypersonic plasma particle deposition of Si–Ti–N nanostructured coatings

• Published in: Surface & coatings technology 2004-11, Vol.188, p.364-370
• Main Authors: Hafiz, J., Wang, X., Mukherjee, R., Mook, W., Perrey, C.R., Deneen, J., Heberlein, J.V.R., McMurry, P.H., Gerberich, W.W., Carter, C.B., Girshick, S.L.
• Format: Article
• Language: English
• Subjects: Hardness; Nanostructured; Plasma synthesis; Size distribution; Si–Ti–N
• ISSN: 0257-8972; 1879-3347
• DOI: 10.1016/j.surfcoat.2004.08.226

Si–Ti–N coatings with various compositions were deposited on molybdenum substrates using hypersonic plasma particle deposition (HPPD). In this method, vapor phase precursors (TiCl 4, SiCl 4 and NH 3) are dissociated in a DC plasma arc and the hot gas is quenched in a rapid nozzle expansion to nucleate nanoparticles. These nanoparticles are then accelerated in hypersonic flow, causing them to deposit by ballistic impaction on a substrate placed downstream of the nozzle. Films of 10–25 μm thickness were deposited at rates of 2–10 μm/min, depending on reactant flow rates, at substrate temperatures ranging from 200 to 850 °C. When the reactant gases were premixed the coatings consisted of nc-TiN, nc-TiSi 2, nc-Ti 5Si 3 and amorphous Si 3N 4. For the unpremixed reactants case, the coatings consisted of free Si, nc-TiN and amorphous Si 3N 4. Hardness of as-deposited films was evaluated by nanoindentation of polished film cross-sections. Measured hardness values, averaged over 10–15 locations for each film, ranged from 16–24 GPa. In separate experiments with the same conditions, particle size distributions were measured by placing a sampling probe at the same location as the film substrate. The sampled aerosol was rapidly diluted and delivered to a scanning mobility particle sizer (SMPS). In-situ particle size distribution measurements confirmed that the coatings were formed by impaction of nanoparticles in the 5–15 nm range, with higher reactant flow rates producing larger particles. Focused ion beam (FIB) milling was used to observe film cross-section and porosity. For as-deposited films containing pores, in-situ plasma sintering was used to densify the film without grain growth.