Technique for preparation and characterization in cross-section of oral titanium implant surfaces using focused ion beam and transmission electron microscopy.

The surface properties of materials are believed to control most of the biological reactions toward implanted materials. To study the surface structure, elemental distribution, and morphology, using transmission electron microscopy (TEM) techniques, thin foils of the surface (in cross-section) are needed. These have been cumbersome to produce, in particular, from the normally irregular screw-shaped metal implants. Focused ion beam (FIB) microscopy has been developed partly for TEM sample preparation, mainly within the microelectronics industry. Our study describes a method based on FIB for producing electron transparent foils/sections from a metal implant for TEM analysis. Using a screw-shaped titanium dental implant, it was demonstrated that thin foils can be prepared with submicron specificity and from almost any surface geometry. A comparison of different lift-out techniques showed that the in situ lift-out preparation technique allowed plasma cleaning and produced particularly good samples with excellent yield. The titanium oxide on the implant surface was analyzed using energy-filtered TEM (EFTEM) and high-resolution TEM (HRTEM) and the TiO(2) rutile phase being determined via the lattice parameters. This study provides the first set of data for the optimization of a new route for preparation and analysis of biomaterial surfaces and interfaces.