Nitride films are deposited from a single equiatomic AlCrMoSiTi target by reactive DC magnetron sputtering. The influence of the substrate bias and deposition temperature on the coating structure and properties are investigated. The bias is varied from 0 to − 200 V while maintaining a substrate temperature of 573 K. And the temperature is changed from 300 to 773 K whilst maintaining a substrate bias of − 100 V. From X-ray diffraction analysis, it is found that all the as-deposited coatings are of a single phase with NaCl-type FCC structure. This is attributed to the high mixing entropy of AlN, CrN, MoN, SiN, and TiN, and the limited diffusion kinetics during coating growth. Specific aspects of the coating, namely the grain size, lattice constant and compressive stress, are seen to be influenced more by substrate bias than deposition temperature. In fact, it is possible to classify the deposited films as large grained (~ 15 nm) with a reduced lattice constant (~ 4.15 A) and low compressive residual stresses for lower applied substrate biases, and as small grained (~ 4 nm) with an increased lattice constant (~ 4.25 A) and high compressive residual stresses for applied biases of − 100 V or more. A good correlation between the residual stress and lattice constant under various deposition conditions is found. For the coatings deposited at − 100 V, and at temperatures above 573 K, the hardness could attain to the range of 32 to 35 GPa. Even after annealing in vacuum at 1173 K for 5 h, there is no notable change in the as-deposited phase, grain size or lattice constant of the coatings but an increase in hardness. The thermal stability of microstructure is considered to be a result of the high mixing entropy and sluggish diffusion of these multi-component coatings. For the anneal hardening it is proposed that the overall bonding between target elements and nitrogen is enhanced by thermal energy during annealing.

Influence of substrate bias, deposition temperature and post-deposition annealing on the structure and properties of multi-principal-component (AlCrMoSiTi)N coatings

The phase stability of Al-containing cubic transition metal (TM) nitrides, where Al substitutes for TM (i.e. TM1−xAlxN), is studied as a function of the TM valence electron concentration (VEC). X-ray diffraction and thermal analyses data of magnetron sputtered Ti1−xAlxN, V1−xAlxN and Cr1−xAlxN films indicate increasing phase stability of cubic TM1−xAlxN at larger Al contents and higher temperatures with increasing TM VEC. These experimental findings can be understood based on first principle investigations of ternary cubic TM1−xAlxN with TM = Sc, Ti, V, Cr, Y, Zr and Nb where the TM VEC and the lattice strain are systematically varied.However, our experimental data indicate that, in addition to the decomposition energetics (cubic TM1−xAlxN → cubic TMN + hexagonal AlN), future stability models have to include nitrogen release as one of the mechanisms that critically determine the overall phase stability of TM1−xAlxN.

https://iopscience.iop.org/article/10.1088/0022-3727/43/3/035302/pdf

Experimental and computational study on the phase stability of Al-containing cubic transition metal nitrides

This paper reviews a Plasma Enhanced Magnetron Sputtering (PEMS) technology and a series of studies of Ti– Si–C–N nanocomposite coatings deposited using this technique. The PEMS technology is discussed briefly and compared with conventional magnetron sputter deposition. In PEMS, an electron source is used to generate plasma in addition to the magnetron plasma for both ion cleaning of the surfaces before deposition and enhanced ion bombardment during the deposition. The coatings thus obtained are very dense with nearly no columnar structure. Using this technology, many Ti–Si–C–N coatings have been prepared. These coatings are found to be nanocomposite coatings composed of nanocrystalline TiCN with grain sizes of 4.7– 100 nm in a matrix of amorphous SiC x N y . Their hardness ranges from 25 to 43 GPa and has a Si concentration up to about 3.5 at.%. They exhibit erosion resistance over 100 times better than the uncoated Ti–6Al–4V substrate. It has been observed that the toughness of the coating, or the resistance to crack formation and propagation, evaluated using H 3 / E ⁎ 2 , correlates well with the coating erosion resistance. The relationship among the processing parameters and the coating microstructure, nanohardness, adhesion, and erosion resistance are discussed. In addition, single and multilayered coatings have also been compared. These coatings are intended to be used against severe sand erosion for gas turbine compressor blades and vanes.

Plasma enhanced magnetron sputter deposition of Ti–Si–C–N based nanocomposite coatings

TiAlN based nanoscale multilayer coatings designed to adapt their tribological properties at elevated temperatures

Hard coatings based on ternary Ti–Al–N and Cr–Al–N are commercial products currently employed in many industrial applications due to their outstanding chemical and physical properties, including high hardness and toughness and thermal as well as chemical stability. In this chapter the current understanding of mechanisms relevant for the thermal and chemical stability of these coating systems will be summarized based on state-of-the-art experimental and computational data.

Synthesized by low-temperature (substrate temperatures below 500 °C) plasma-assisted vapor deposition (PVD) techniques, ternary Ti1−xAlxN, Cr1−xAlxN, and related coatings form metastable solid solutions. Depending on the chemical composition (and the deposition parameters used, like substrate temperature, gas pressure, and ion bombardment), the coatings crystallize in a face centered cubic (fcc) NaCl-type (c) or a hexagonal close packed (hcp) wurtzite-type (w) phase. For the main engineering applications, the cubic modification is preferred due to the superior mechanical, tribological, and oxidation properties. For example, the hardness of as-deposited c-Ti1−xAlxN and c-Cr1−xAlxN coatings, with AlN content (x) close to its metastable cubic solubility limit of x ∼ 0.7, can be as high as 37 and 30 GPa, respectively. During thermal treatments above the deposition temperature (e.g., during cutting application), the coatings undergo various processes to reach equilibrium. While for single-phase cubic Ti1−xAlxN the decomposition into the stable phases c-TiN and w-AlN occurs across the formation of cubic Al-rich and Ti-rich domains, the decomposition of Cr1−xAlxN is driven by nucleation and growth of w-AlN as well as by the release of N2 starting at temperatures around 1000 °C. The combination of experimental (e.g., x-ray diffractometry, calorimetry, nanoindentation, scanning and transmission electron microscopy, and atom probe tomography) with computational (e.g., density functional theory and continuum mechanics) studies allows for identifying, describing, and understanding the mechanisms and processes that govern the thermally induced decomposition. Thermal stability is discussed for Ti1−xAlxN-based coating systems, while chemical stability is analyzed for Cr1−xAlxN-based coating systems. Furthermore, the influence of alloying elements such as Y, Nb, Ta, Zr, and Hf on the phase formation, structure, mechanical, and thermal properties of these ternary Ti1−xAlxN and Cr1−xAlxN coatings is discussed.

Protective Transition Metal Nitride Coatings

Inductively coupled plasmas (ICPs) were generated to assist magnetron sputtering. By bombarding the growing film with a high-density (∼2.0 mA/cm 2 ) low-energy (∼22 eV) ion flux, Ti-Si-N films containing 0-12 at.% Si were deposited on Si(100) substrates at low deposition temperature (<150 °C). The residual compressive stresses of these films were measured to be lower than 1.5 GPa. Film hardness was significantly enhanced by the addition of a small amount of Si and attained a maximum value of 48 GPa at approximately 5.8 at.% Si. From X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) results, the superhard Ti-Si-N films were characterized as having a nanocomposite structure, consisting of nanocolumns of TiN crystallites with amorphous Si 3 N 4 inside the column boundaries. The hardest Ti-Si-N film exhibited a pronounced TiN(200) texture. No refinement of crystallite size by the addition of Si was observed in the present series of Ti-Si-N films. Thus, the hardness enhancement was attributed to nanocomposite effect.

Structure and properties of Ti-Si-N films prepared by ICP assisted magnetron sputtering

Inductively coupled plasmas (ICPs) were sustained by an internal antenna with insulating coverage to assist conventional magnetron sputtering process. This enabled to irradiate the growing films on the grounded Si (100) substrates with high-density low-energy ion flux. The surface mobility of adatoms could be enhanced markedly but without producing significant forward ion recoils or implantation, and then low-stressed, superhard nanocomposite Ti-Si-N could be synthesized at low deposition temperature by the ICP assisted magnetron sputtering.

Low-temperature synthesis of superhard ti-si-n nanocomposite films

Pseudobinary Zr–Al–N films were synthesized by an inductively combined rf-plasma-assisted magnetron sputtering for the purpose of examining the prediction on the phase change in the T (transition metal)–Al–N pseudobinary system based on band parameters. Phase change from B1 structure to B4 was not verified by XRD and FTIR methods. Microhardness of these films showed a maximum hardness of about 46 GPa at the content of 30% AlN and then decreased drastically to about 28 GPa at the content of 35% AlN. The AlN content for the drastic change showed good agreement with the critical content predicted based on band parameters. Under the assumption that the drastic change of microhardness corresponds to the B1–B4 phase change, it is interpreted that appearance of two XRD peaks near 2θ=32° and 2θ=38° is attributed to the formation of the Zr–Al–N films with B1 structure. On the other hand, single XRD peak 2θ=38° in the Zr–Al–N film with ZrN/AlN=65:35 is assigned to B4 phase. Further, the existence of some amount of the B4 phase in the Zr–Al–N film with ZrN/AlN=70:30–80:20 is suggested from broadness in XRD peaks.

Characterization of Zr–Al–N films synthesized by a magnetron sputtering method

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Structure and properties of Ti-Si-N films prepared by ICP assisted magnetron sputtering

Low-temperature synthesis of superhard ti-si-n nanocomposite films

Characterization of Zr–Al–N films synthesized by a magnetron sputtering method