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Influence of annealing on oxidation, microstructure and mechanical properties of Ni-49Ti films

  • S. Bysakh (a1), A. Kumar (a2), S.V. Kamat (a2), S.K. Sharma (a3) and S. Mohan (a3)...

Thin films of Ni-49 at.%Ti were deposited by DC magnetron sputtering on silicon substrates at 300 °C. The as-deposited amorphous films were annealed at a vacuum of 10−6 mbar at various temperatures between 300 and 650 °C to study the effect of annealing on microstructure and mechanical properties. The as-deposited films showed partial crystallization on annealing at 500 °C. At 500 °C, a distinct oxidation layer, rich in titanium but depleted in Ni, was seen on the film surface. A gradual increase in thickness and number of layers of various oxide stoichiometries as well as growth of triangular shaped reaction zones were seen with increase in annealing temperature up to 650 °C. Nanoindentation studies showed that the film hardness values increase with increase in annealing temperature up to 600 °C and subsequently decrease at 650 °C. The results were explained on the basis of the change in microstructure as a result of oxidation on annealing.

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1.Wayman C.M.: Thermoelastic martensitic transformations and the nature of the shape memory effect, in Phase Transformations in Solids, edited by Tsakalakos T. (Mater. Res. Soc. Symp. Proc. 21, North-Holland, Amsterdam, 1984) p. 657.
2.Wolf R.H. and Heuer A.H.: TiNi (shape memory) films on silicon for MEMS applications. J. Microelectromech. Syst. 4, 206 (1995).
3.Fu Y.Q. and Du H.J.: Relaxation and recovery of stress during martensite transformation for sputtered shape memory TiNi film. Surf. Coat. Technol. 153, 100 (2002).
4.Kahn H., Huff M.A., and Heuer A.H.: The TiNi shape-memory alloy and its applications for MEMs. J. Micromech. Microeng. 8, 213 (1998).
5.Jardine A.P. and Mercado P.G.: Dynamics of thin film NiTi cantilevers on Si, in Phase Transformations in Thin Films–Thermodynamics and Kinetics, edited by Atzmon M., Greer A.L., Harper J.M.E., and Libera M.R. (Mater. Res. Soc. Symp. Proc. 311, Pittsburgh, PA, 1993) p. 161.
6.Seguin J.-L., Vendan M., Isalgue A., Esteve-Cano V., Carchano H., and Torra V.: Low temperature crystallized Ti-rich NiTi shape memory alloy films for microactuators. Sens. Actuators, A 74, 65 (1999).
7.Yang Y., Jia H.S., Zhang Z.F., Shen H.M., Hu A., and Wang Y.N.: Thin films of NiTi shape memory alloy. Mater. Lett. 22, 137 (1995).
8.Bush J.D., Johnson A.D., Lee C.H., and Stevenson D.A.: Shape memory properties in Ni–Ti sputter-deposited films. J. Appl. Phys. 68, 3224 (1990).
9.Huang X. and Liu Y.: Effect of annealing on the transformation behavior and superelasticity of NiTi shape memory alloy. Scr. Mater. 45, 153 (2001).
10.Surbled P., Clerc C., Pioufle B.L., Ataka M., and Fujita H.: Effect of the composition and thermal annealing on the transformation temperatures of sputtered TiNi shape memory alloy thin films. Thin Solid Films 401, 52 (2001).
11.Satoh G., Birnbaum A., and Yao Y.L.: Annealing effect on the shape memory properties of amorphous NiTi thin films. J. Manuf. Sci. Eng. 132, 051004 (2010).
12.Chu C.L., Wu S.K., and Yen Y.C.: Oxidation behavior of equiatomic TiNi alloy in high temperature air environment. Mater. Sci. Eng., A 216, 193 (1996).
13.Xu C.H., Ma X.Q., Shi S.Q., and Woo C.H.: Oxidation behavior of TiNi shape memory alloy at 450–750 °C. Mater. Sci. Eng., A 371, 45 (2004).
14.Ko J.H. and Lee D.B.: High temperature oxidation behavior of TiNi alloys. Mater. Sci. Forum 475479, 853 (2005).
15.Wang X.X., Mao Z.Y., Cao Z.W., Qing R.Y., Jiang X.C., and Peng S.Y.: Oxide film and its effect on shape memory effect and biocompatibility in a TiNi alloy, in Proceedings of International Symposium on Shape Memory Materials, Beijing, China, September 25–28, 1994.
16.Miyazaki S. and Ishida A.: Martensitic transformation and shape memory behavior in sputtered-deposited TiNi-base thin films. Mater. Sci. Eng., A 273275, 106 (1999).
17.Kale A., Seal S., Sobczak N., Morgie J., and Sundaram K.B.: Effect of deposition temperature on the morphology, structure, surface chemistry and mechanical properties of magnetron sputtered Ti70–Al30 thin films on steel substrate. Surf. Coat. Technol. 141, 252 (2001).
18.Huang X. and Liu Y.: Some factors affecting the properties of sputter deposited NiTi-base shape memory alloy thin films, in Smart Materials II, edited by Wilson A.R. and Varadan V.V., eds.; Proceedings of SPIE Int. Soc. Opt. Eng. Vol. 4934, (2002) p. 210.
19.Badini C. and Laurella F.: Oxidation of FeCrAl alloy: Influence of temperature and atmosphere on scale growth rate and mechanism. Surf. Coat. Technol. 135, 291 (2001).
20.Chu J.P., Lai Y.W., Lin T.N., and Wang S.F.: Deposition and characterization of TiNi-base thin films by sputtering. Mater. Sci. Eng., A 277, 11 (2000).
21.Eswar Raju K.S.S., Bysakh S., Sumesh M.A., Kamat S.V., and Mohan S.: The effect of ageing on microstructure and nanoindentation behavior of dc magnetron sputter deposited nickel rich NiTi films. Mater. Sci. Eng., A 476, 267 (2008).
22.Jarrigea I., Holligerb P., Nguyenc T.P., Ip J., and Jonnard P.: From diffusion processes to adherence properties in NiTi microactuators. Microelectron. Eng. 70, 251 (2003).
23.Fenske F., Schöpke A., Schulze S., and Selle B.: Analytical studies of nickel silicide formation through a thin Ti layer. Appl. Surf. Sci. 104105, 218 (1996).
24.Oliver W.C. and Pharr G.M.: An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments. J. Mater. Res. 7, 1564 (1992).
25.Zhang L., Xie C., and Wu J.: Oxidation behavior of sputter-deposited Ti–Ni thin films at elevated temperatures. Mater. Charact. 58, 471 (2007).
26.Otsuka K. and Ren X.: Physical metallurgy of Ti–Ni-based shape memory alloys. Prog. Mater Sci. 50, 511 (2005).
27.Chan C.M., Trigwell S., and Duerig T.: Oxidation of an NiTi alloy. Surf. Interface Anal. 15, 349 (1990).
28.Kekare S.A., Shelton D.K., and Aswath P.B.: Oxidation of high-temperature intermetallics, in The Minerals, Metals and Materials Society, (Warrendale, PA, 1993) p. 325.
29.Tall P.D., Ndiaye S., Beye A.C., Zong Z., Soboyejo W.O., Lee H.J., Ramirez A.G., and Rajan K.: Nanoindentation of Ni–Ti thin films. Mater. Manuf. Processes 22, 175 (2007).
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Journal of Materials Research
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