Surface and Coatings Technology 182 (2004) 204–214 0257-8972/04/$ - see front matter  2003 Elsevier B.V. All rights reserved. doi:10.1016/j.surfcoat.2003.08.052 Comparative investigation of Ti–Si–N films magnetron sputtered using Ti Si qTi and Ti Si qTiN targets 53 53 D.V. Shtansky *, I.V. Lyasotsky , N.B. D’yakonova , F.V. Kiryukhantsev-Korneev , S.A. Kulinich , a, b b a a E.A. Levashov , J.J. Moore a c Moscow State Institute of Steel and Alloys, Leninsky pr. 4, 164, Moscow 119049, Russia a I.P. Bardin Central Research Institute for the Iron and Steel Industry, 2 Baumanskaya Street, 9y23, Moscow 107005, Russia b nd ACSEL Laboratory, Colorado School of Mines, Golden, CO 80401, USA c Received 8 April 2003; accepted in revised form 14 August 2003 Abstract A comparative investigation of Ti–Si–N films deposited by DC magnetron sputtering (MS) of composite Ti Si qTi and 53 Ti Si qTiN targets in an argon atmosphere or reactively (RMS) in a gaseous mixture of ArqN is presented. The targets were 53 2 manufactured by means of self-propagating high-temperature synthesis. The microstructure, phase and chemical composition of Ti–Si–N films were studied by means of X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy and Auger electron spectroscopy. The films were characterized in terms of their hardness, elastic modulus, elastic recovery and surface topography. Measurements of hardness were performed by the method of sclerometry (hardness under failure) and by load–depth-sensing nanoindentation (hardness under elastic and plastic deformation). The friction coefficient of Ti–Si–N films against hard metal was also determined. Results obtained show that the Ti–Si–N films deposited in pure Ar using Ti Si qTiN 53 target consist of nanocrystalline TiN in an amorphous a-TiSi matrix. The volume fraction of the fcc phase increased as the x substrate temperature or bias voltage was raised. The films deposited by sputtering of Ti Si qTiN target in Ar and by sputtering 53 of Ti Si qTi target in Arq14% N were characterized by the presence of planar (100) texture. This preferred orientation, 53 2 however, becomes less pronounced as the nitrogen partial pressure is raised up to 14% and 24%, respectively. The Ti–Si–N films consist of crystalline grains, 2–15 nm in size, elongated in the direction of film growth. When N was added to the gas discharge 2 during deposition, the TiN grain size slightly increased. The lattice parameter was calculated from X-ray diffraction spectra to a(0.431–0.432nm (MS) and a(0.428–0.430nm (RMS) thatishigherthanthatofthebulkTiN (0.424 nm).Thefilmsshowed hardness less than 35 GPa and Young’s modulus in the range of 220–250 GPa. Friction coefficient values between approximately 0.5 and 0.6 were recorded.  2003 Elsevier B.V. All rights reserved. Keywords: Magnetron sputtering; SHS composite targets; Ti–Si–N coatings; Nanostructured thin films; Structure; Hardness; Young’s modulus; Wear 1. Introduction Ti–Si–N thin films are of interest because of their high hardness w1,2x, thermal stability w1x, oxidation resistance w2x, and diffusion barrier performance w3x.Si- doped TiN films also exhibit superior performance over binary nitrides in tribological applications. The structure of Ti–Si–N films was shown to consist of nanocrystal- line titanium nitride (TiN) in an amorphous matrix. Both physical vapor deposition (PVD) and chemical *Corresponding author. Tel.: q7-95-230-4535; fax: q7-95-236- 5298. E-mail address: shtansky@shs.misis.ru (D.V.Shtansky). vapor deposition (CVD) techniques have been success- fully applied in a large number of studies. The TiNya- Si N nanocomposites were prepared by means of 34 plasma-induced CVD from TiCl and Si N w4x. PVD 4 34 was applied to produce Ti–Si–N films by reactive magnetron sputtering of high-purity Ti and Si targets w5–7x, TiSi target w8x, Ti Si target w3,9,10x, TiSi and 53 2 Ti Si targets w3x.Morerecently,hybridsystemscombin- 3 ingarcplatingandsputteringtechniques w11x andCVDy PVD w12x have been employed. Despite the availability of numerous literature data, a number of problems remain unsolved. Veprek and co- workers w13x reported the deposition of Ti–Si–N films