ICMCTF2000 Session B2: Chemical Vapor Deposition Techniques

Thursday, April 13, 2000 8:30 AM in Room Royal Palm Salon 1-3

Thursday Morning

Time Period ThM Sessions | Abstract Timeline | Topic B Sessions | Time Periods | Topics | ICMCTF2000 Schedule

Start Invited? Item
8:30 AM B2-1 Injection MOCVD : Ferroelectric Thin Films And Functional Oxide Superlattices.
F. Weiss, J.P. Senateur, J. Lindner, C. Dubourdieu, V. Galindo (LMGP-ENSPG-INPG, France); A. Abrutis (Vilnius University, Lithuania)
MOCVD is a suitable technique for the synthesis of functional metal oxide thin films. When gaseous precursors are available the process is generally simple (SiO2 DRAMs or compound semiconductors). In the case of solid precursors (necessary e.g. for the new Bax√sub 1-xTiO3 DRAM generation) one has to overcome a precursor delivery problem. In the present paper, Injection-MOCVD was proved to be an efficient method, not only to grow single layers, but also heterostructures and superlattices of functional oxide materials. We report on the deposition of BST films and BaTiO3/SrTiO3 superlattices (BTO/STO) obtained by injection MOCVD. In a first time, BST films were deposited on various substrates such as LaAlO3(LAO), SrTiO3:Nb(STO:Nb) and Al2O3(0001), resulting in epitaxial films in the case of STO or LAO substrates and highly textured films in the case of Al2O3 substrates. The good crystallinity of the films obtained was evidenced using X-ray analysis. Concerning the dielectric properties of the BST films deposited on STO:Nb one can mention that the Tc values were found to be the same as those for bulk materials. Further superlattices have been obtained by combining ferroelectric, magnetic (CMR) and superconducting (HTS) oxides. Typical results of these superlattices will be reported.
9:10 AM B2-3 Single-phased Hard Coatings of the Metastable Cr3(C0.8N0.2)2 Ternary Phase Grown by Low Pressure MOCVD
F. Maury (CNRS/INPT, Ecole Nationale Superieure de Chimie, France); F. Ossola (CNR, Italy); F. Senocq (CNRS/INPT, Ecole Nationale Superieure de Chimie, France)

The ternary phase Cr3(C0.8N0.2)2 is known to be stabilized both at high temperature and under a high pressure of nitrogen. Therefore it is unstable in the typical conditions of the vapor deposition processes, i.e. moderate temperature and normal or low total pressure, and so far, the potentiality of this ternary phase to be used as metallurgical coatings has not been investigated. We report in this contribution a novel deposition process of this ternary phase on various substrates including steel.

Single-phased coatings of Cr3(C0.8N0.2)2 have been deposited by combining an MOCVD process and an annealing post-treatment. The films were grown in the temperature range 683-793 K by low pressure MOCVD using Cr(NEt2)4) as single-source precursor. As-deposited films are very smooth and x-ray amorphous. A relatively low amount of nitrogen is uniformly incorporated into the film. The nitrogen content is nearly independent on the growth conditions and it amounts the value of the ternary phase (about 7 at. %). The as-deposited films crystallize upon annealing at 873 K under vacuum to form the orthorhombic Cr3(C0.8N0.2)2 phase. No evidence for additional phases has been found. Both as-deposited and annealed coatings exhibit a high hardness and a good adhesion on stainless steel substrates. The hardness slightly increases upon crystallization to reach typically 17 GPa. Preliminary properties of this metastable carbonitride phase are reported and its potentialities as hard metallurgical coating are discussed.

9:30 AM B2-4 A Study of Microstructures of Ti(C,N) Coatings Deposited by CVD
N.Y. Yoshikawa (Toshiba Tungaloy Col, Ltd., Japan); I.Y. Yazaki, T.S. Saito (Toshiba Tungaloy Co., Ltd., Japan)
Ti(C,N) coating deposited by CVD is widely used as a wear protective layer of cemented carbide cutting tools. Properties of the CVD coated cemented carbide tools depend on adhesion strength, coating thickness, and microstructures of the coatings, however there are not so many reports about them. In this study, the microstructures of the Ti(C,N) coating are focused and the effects of the microstructures on the properties of the coated cemented carbide tools are discussed. The difference between a conventional granular structure and a developing columnar structure is described.
10:30 AM B2-7 Duplex Processes: New Developments in the Combination of Technologies
F. Schuster (CEA-Grenoble, France)
High resistance surface treatments against corrosion, wear and fatigue can be achieved by several new combinations of single processes. The goal of this work is to present the new developments in the field of duplex processes. Several combined processes for steels and non ferrous metals are reviewed. The combination of low frequency PACVD (DLC, TiN, TiAlN), MOCVD (CrC, CrN) and plasma nitriding or carburizing , of low frequency PACVD (DLC, SiOx...) and PVD(CrN...) in a single device are presented. Some industrial examples highlight the great potential of such combined processes. Different multilayer architectures obtained with these two duplex and hybrid technologies reveal promising results in terms of wear and corrosion behaviour.
11:30 AM B2-10 Study of the Effects of Metal Ion Post-implantation on the Near Surface Properties of TiN Deposited by CVD
A.J. Perry (A.I.M.S. Consulting, Switzerland); R.R. Manory, L. Ward, P. Kavouri (Royal Melbourne Institute of Technology, Australia)

In contrast to the effect of nitrogen ion implantation, where changes in properties are related [1] to the chemical and tribological character of the implanted zone (i.e. the near-surface zone where the implanted ions reside), metal ion implantation hardens the substrate and enhances wear resistance to depths well beyond that zone -- this is known as the 'long range effect'. As shown recently, the extent of this hardening depends on the conditions generated in the implanted zone during the implantation process [2].

In the present study, the surface topography and residual stress in TiN deposited by CVD and subjected to a metal ion implantation post-treatment are presented covering the range from Al to W ions. Coatings made by CVD were chosen because of their low residual stress (0 - 0.5 GPa tensile). The surface topography is discussed in terms of Ra values determined by profilometry and by AFM and studied by fractal analysis. It is found that the residual stress increases with ion beam energy but that there is no concomitant change in the coefficient of friction, the surface roughness nor in the surface topography caused by the associated sputter loss. The stress in the implanted zone is shown to correlate directly with the stress generated in the material affected by the long range effect, in accordance with the mechanism proposed recently [2]. 1 R.R. Manory et al., Surf. Coat. Technol., 114 (1999) 137. 2 Y.P. Sharkeev et al., Vacuum, 52 (1999) 247.

11:50 AM B2-11 Plasma-Enhanced CVD of (Ti,Al)N Films from Chloridic Precursors in a DC Glow Discharge
R. Prange, R. Cremer, D. Neuschütz (LTH, RWTH Aachen, Germany)
Metastable Ti1-xAlxN films have been deposited from gaseous mixtures of TiCl4-AlCl3-N2-H2-Ar in a pulsed DC glow discharge at 510 °C. When the discharge voltage was kept constant, the Al content x of the films increased linearly with the AlCl3/TiCl4-ratio in the feed gas. Increasing the discharge voltage also increased the Al content. Up to compositions of Ti0.09Al0.91N the layers remained single-phase cubic with a strong [100] texture. Films with a higher Al content consisted of two phases and their cubic phase showed a weak [111] texture. The lattice parameter of the homogeneous cubic films decreased with increasing Al content in accordance with Vegard´s law. Films with a low Al content exhibited a columnar morphology, while the films with high Al contents had a fine grained structure. Increasing the discharge voltage also caused the grain size to decrease. The microhardness of the single-phase coatings increased with increasing Al content up to 3947 HV 0.05 for x = 0.83, while the two-phase layers showed hardness values around 5000 HV 0.05. The metastable films began to decompose at temperatures between 750 and 800 °C, depending on the Al content. The decomposition of the films with an Al/Ti ratio below 1 caused the lattice parameter of the cubic phase to increase and the microhardness to decrease. Films with high Al contents did not show any increase in the lattice parameter after annealing and their microhardness strongly increased. Investigation of the oxide layer formed on a Ti0.21Al0.79N film after annealing in air at 800 °C showed that an amorphous alumina layer with a thickness of approximately 100 nm was formed on the surface, preventing further oxidation. The films with high Al content exhibited advantageous tribological properties with friction coefficients of 0.5. Thus, they seem to be especially well suited for an application on cutting and metal working tools.
Time Period ThM Sessions | Abstract Timeline | Topic B Sessions | Time Periods | Topics | ICMCTF2000 Schedule