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Calibration of RHEED patterns for the appraisal of titania surface crystallography

T. Tao, R. Walton, H.K. Edwards, M.W. Fay1, D.M. Grant and P.D. Brown 1. School of Mechanical, Materials and Manufacturing Engineering, 2. The Nottingham Nanotechnology and Nanoscience Centre, University of Nottingham, University Park, Nottingham, NG7 2RD, UK
emxtt@nottingham.ac.uk Keywords: TiO2, RHEED

Titanium and its alloys are commonly used as biomaterials due to their various beneficial surface properties, especially the formation of chemically stable passivating oxide films which can provide for excellent corrosion resistance and reduce metal ion release. Titanium oxide is a ceramic layer consisting typically of TiO2 which can exhibit different polymorphs for different annealing conditions [1]. A range of titanium samples annealed at different temperatures and for different time periods have been appraised for the dynamic evolution of the titanium oxide near surface structure. Information on the near surface crystal structure of the TiO2/Ti surfaces was acquired using reflection high energy electron diffraction (RHEED). Additionally, the complementary technique of secondary electron imaging (SEI) using an FEI, XL30 SEM has been used to give further insight into the development of those titanium oxide surfaces. Illustration of the results of the combined RHEED & SEI characterisation of the sample set is shown in Figure 1. As the annealing temperature increases, the crystal structure of titanium oxide changes from amorphous, through polycrystalline anatase, to a mixture of anatase and rutile, and finally to polycrystalline rutile (Figure 1a). As the annealing time period increases, larger grain sizes and slightly preferred orientation of the grains become apparent (Figure 1b). Cross-sectional TEM is required to investigate the depth profile of the oxides formed on the Ti samples. For a Ti sample annealed at 900 C for 45 mins, crosssectional TEM (XTEM) analysis was performed to identify the sub-oxides below the surface. Figure 2 illustrates bright field TEM images from the cross sectioned sample with associated selected area electron diffraction patterns. Figure 2 (a) indicates a total oxide thickness of ~ 7 m in this instance and varying levels of electron transparency and porosity in the coating. Based on the analysis of the diffraction patterns, Figure 2 (b) shows an area encompassing (i) an upper coating, correlated almost exclusively with rutile; (ii) a lower coating, showing good correlation with rutile and a little evidence of Ti2O; and (iii) the substrate, being single crystal -Ti.
1. 2. E. Lautenschlater & P. Monaghan. Titanium and titanium alloys as dental materials. Biomaterials, 1993. 27: p. 245-253 Acknowlegement: this work was supported by the EPSRC under grant EP/E015379/1.

M. Luysberg, K. Tillmann, T. Weirich (Eds.): EMC 2008, Vol. 1: Instrumentation and Methods, pp. 753754, DOI: 10.1007/978-3-540-85156-1_377, Springer-Verlag Berlin Heidelberg 2008