Microstructures of TiN films grown by various physical vapour deposition techniques

Abstract

A study has been made of TiN coatings deposited on steel substrates by five commercially available physical vapour deposition (PVD) methods; low voltage electron beam evaporation, triode high voltage electron beam evaporation, random-arc evaporation, steered-arc evaporation and magnetron sputtering. The microstructure and substrate-film interfacial microchemistry of the films were investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM) together with energy-dispersive X-ray spectroscopy (EDX), cross-sectional transmission electron microscopy (XTEM) and scanning transmission electron microscopy (STEM) combined with EDX analyses of XTEM samples. The XRD analyses showed that all the films were in a state of compressive stress with interplanar distances as much as 1.7% higher than reference bulk values. SEM examination revealed only minor variations in surface roughness among the samples except for the arc-evaporated films which contained large droplets and craters resulting from the detachment of droplets. The number density and average sizes of droplets and craters were lower in the steered-arc sample than in the random-arc sample. XTEM analyses showed that all the films had columnar structures with clearly defined substrate-film interfacial layers. The films appeared dense except for the magnetron-sputtered sample which exhibited intercolumnar porosity. STEM-EDX analyses showed large variations in the microchemistry of the substrate-film interfacial regions which consisted, depending on the sample, of renucleated near-surface substrate grains, intentionally (or, in at least one case, unintentionally) introduced foreign material or gas-bubble-like inclusions. However, the microchemistry of these interfacial regions was, in most cases, understandable on the basis of the substrate pretreatment and/or choice of film growth parameters.