TiN hard coating as a candidate reference material for surface metrology in chemistry: characterization and quantification by bulk and surface analyses techniques

This study presents the synthesis and characterization of TiN hard coatings as a candidate reference material for surface metrology in chemistry. TiN coatings were grown on a silicon wafer with (111) orientation using dc reactive magnetron sputtering. X-ray diffraction confirms that the diffraction phase of TiN coatings is polycrystalline, electron microscopy demonstrates that the TiN coatings presents pyramidal-shaped grains ranging from sub-micrometer to nano-size scale and with an average thickness of 666 nm. According to micro Raman results, the presence of LO phonon modes confirms that the TiN coatings are crystalline in nature and no impurities are detected. The mechanical properties at the nanoscale are evaluated using resonance tracking acoustic force atomic microscopy. The chemical composition of the TiN reveals a close 1:1 atomic ratio. The ANOVA is used to evaluate the homogeneity of the TiN via a homogeneity test according to the ISO Guide 35:2017, while, regarding the chemical composition of the Ti, the Fisher’s test demonstrates that the batch can be considered as homogeneous.