Characterization of Nanocomposite Coatings in the System Ti–B–N by Analytical Electron Microscopy and X-Ray Photoelectron Spectroscopy

 Superhard nanocomposite coatings of different composition in the quasi-binary system TiN–TiB₂ were deposited onto stainless steel sheets by means of unbalanced DC magnetron co-sputtering using segmented TiN/TiB₂ targets. The chemistry and microstructure of a TiB_0.6N_0.7 coating was investigated using X-ray and electron diffraction, photoelectron spectroscopy, energy-filtering transmission electron microscopy, and electron energy-loss spectrometry. High resolution elemental mapping of the elements Ti, B, N, and O with energy-filtering TEM reveals a homogeneous distribution on the nanometer scale. X-Ray and electron diffraction exhibit only TiN crystallites of nanometer size, but no information on the boron-rich phase. The near-edge fine structures of the BK and NK ionization edges in the EELS spectra of the Ti–B–N coatings were used to derive information on the phases by comparing the edges with those of reference compounds. It was found that the TiN nanocrystals occur together with TiO _x particles; the grains are embedded in a strongly disordered or quasi-amorphous matrix consisting mainly of TiB₂ particles and, near the steel substrate, also boron oxide (B₂O₃).