Structure,Composition, and Properties of Arc PVD Mo–Si–Al–Ti–Ni–N Coatings

Using an arc physical vapor deposition process, we have produced nanostructured Mo–Si–Al–Ti–Ni–N coatings with a multilayer architecture formed by Mo₂N, AlN–Si₃N₄, and TiN–Ni and a crystallite size on the order of 6–10 nm. We have studied the physicomechanical properties of the coatings and their functional characteristics: wear resistance, adhesion to their substrates, and heat resistance. According to high-temperature (550°C) wear testing and air oxidation (600°C) results, the coatings studied here are wearand heat-resistant under appropriate temperature conditions. Their properties are compared to those of Mo–Si–Al–N coatings.     

Creep of silicon nitride-titanium nitride composites

The effect of particulate TiN additions (0–50 wt%) on creep behaviour of hot-pressed (5 wt%Y₂O₃ + 2 wt%Al₂O₃)-doped silicon nitride (HPSN)-based ceramics was studied. Creep was measured using a four-point bending fixture in air at 1100–1340 °C. At 1100 °C, very low creep rates of HPSN with 0–30 wt% TiN are observed at nominal stresses up to 160 MPa. At 1200 °C the creep rate is slightly higher, and at 1300 °C the creep rate is increased by three orders of magnitude compared to 1100 °C and rupture occurs after a few hours under creep conditions. It was established that the formation of a TiN skeleton could detrimentally affect the creep behaviour of HPSN. An increase in TiN content leads to higher creep rates and to shorter rupture times of the samples. Activation energies of 500–1000 kJ mol^?1 in the temperature range of 1100–1340 °C at 100 MPa, and stress exponentsn?4 in the stress range 100–160 MPa at 1130–1200 °C were calculated. Possible creep mechanisms and the effect of oxidation on creep are discussed.     

New intelligent multifunctional SiO2/VO2 composite films with enhanced infrared light regulation performance,solar modulation capability,and superhydrophobicity

Abstract

Highly transparent, energy-saving, and superhydrophobic nanostructured SiO₂/VO₂ composite films have been fabricated using a sol–gel method. These composite films are composed of an underlying infrared (IR)-regulating VO₂ layer and a top protective layer that consists of SiO₂ nanoparticles. Experimental results showed that the composite structure could enhance the IR light regulation performance, solar modulation capability, and hydrophobicity of the pristine VO₂ layer. The transmittance of the composite films in visible region (T_lum) was higher than 60%, which was sufficient to meet the requirements of glass lighting. Compared with pristine VO₂ films and tungsten-doped VO₂ film, the near IR control capability of the composite films was enhanced by 13.9% and 22.1%, respectively, whereas their solar modulation capability was enhanced by 10.9% and 22.9%, respectively. The water contact angles of the SiO₂/VO₂ composite films were over 150°, indicating superhydrophobicity. The transparent superhydrophobic surface exhibited a high stability toward illumination as all the films retained their initial superhydrophobicity even after exposure to 365 nm light with an intensity of 160 mW^.cm^?2 for 10 h. In addition, the films possessed anti-oxidation and anti-acid properties. These characteristics are highly advantageous for intelligent windows or solar cell applications, given that they can provide surfaces with anti-fogging, rainproofing, and self-cleaning effects. Our technique offers a simple and low-cost solution to the development of stable and visible light transparent superhydrophobic surfaces for industrial applications.     

TiN as a high temperature diffusion barrier for arsenic and boron

The use of TiN thin films as high temperature diffusion barrier layers for arsenic and boron was investigated. The TiN films are formed by reactive evaporation at room temperature and then annealed at a higher temperature. TiN and TiN/TiSi₂ films are placed between heavily doped polycrystalline silicon films and single-crystal silicon substrates of opposite doping polarity for secondary ion mass spectrometry analysis and electrical measurements of Schottky and ohmic contacts respectively. The results indicate that TiN is a good diffusion barrier for arsenic at 900°C. The effectiveness of this property is degraded as the temperature exceeds 900°C and it becomes ineffective at 1000°C. TiN is a better diffusion barrier for boron than for arsenic. It allows limited diffusion of boron at temperatures of up to 1000°C. The TiN/TiSi₂ composite forms good ohmic contacts when the substrates are heavily doped. The ohmic contacts can survive after annealing at temperatures of up to 1000°C. It also forms good Schottky contacts when the substrates are lightly doped. The Schottky contacts can survive after annealing at temperatures of up to 950°C in one case and of up to 1000°C in another case.     

Author index

Films of TiC, TiN and their composite were prepared on molybdenum by a reactive sputtering method with CH₄ and N₂ as the reactive gases and argon as the sputtering gas and applying bias potentials to the substrate material.The films were characterized by X-ray photoelectron spectroscopy and Auger electron spectroscopy. The quantitative chemical composition of the TiC and TiN coatings was determined as a function of the partial pressures of CH₄ (P_CH4) and N₂ (P_N2) during the reactive sputtering. For the TiC coating the most suitable P_CH4 range which gives the stoichiometric composition (carbon-to-titanium ratio, 0.8–1.0) without impurities was found to be (2–5) × 10^?4 Torr (substrate temperature, 300 °C; bias potential, ? 300 V). For the TiN coating the structure and composition of the films prepared by reactive sputtering were observed to depend greatly on the condition of applying the bias potential. The suitable P_N2 range which gives golden films of the stoichiometric composition was higher than 1 × 10^?4 Torr (substrate temperature, 200–300 °C; bias potential from ?75 to ?200 V).On the basis of these experimental studies of TiC and TiN coatings successive coatings of TiC and TiN were deposited onto a molybdenum substrate to achieve higher thermal stability and better adhesion to the substrate. The successive coating method is a promising technique for use in fusion reactors.     

Oxidation resistance of TiN,CrN, TiAlN and CrAlN coatings deposited by lateral rotating cathode arc

In this paper, four kinds of hard coatings, TiN, CrN, TiAlN and CrAlN (with Al/Ti or Al/Cr atomic ratio around 1:1), were deposited on stainless steel substrates by a lateral rotating cathode arc technique. The as-deposited coatings were annealed in ambient atmosphere at different temperatures (500–1000 °C) for 1 h. The evolution of chemical composition, microstructure, and microhardness of these coatings after annealing at different temperatures was systematically analyzed by energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD) and nanoindentation experiments. The oxidation behaviour and its influence on overall hardness of these four coatings were compared. It was found that the ternary TiAlN and CrAlN coatings have better oxidation resistance than their binary counterparts, TiN and CrN coatings. The Cr-based coatings (CrN and CrAlN) exhibited evidently better oxidation resistance than the Ti-based coatings (TiN and TiAlN). TiN coating started to oxidize at 500 °C. After annealing at 700 °C no N could be detected by EDX, indicating that the coating was almost fully oxidized. After annealed at 800 °C, the coating completely delaminated from the substrate. TiAlN started to oxidize at 600 °C. It was nearly fully oxidized (with little residual nitrogen detected in the coating by EDX) and partially delaminated at 1000 °C. Both CrN and CrAlN started to oxidize at 700 °C. CrN was almost fully oxidized (with little residual nitrogen detected in the coating by EDX) and partially delaminated at 900 °C. The oxidation rate of the CrAlN coating is quite slow. After annealing at 1000 °C, only about 19 at.% oxygen was detected and the coating showed no delamination. The Ti-based (TiN and TiAlN) coatings were not able to retain their hardness at higher temperatures (≥ 700 °C). On the other hand, the hardness of CrAlN was stable at a high level between 33 and 35 GPa up to an annealing temperature of 800 °C and still kept at a comparative high value of 18.7 GPa even after annealed at 1000 °C, indicating a very promising applicability of this coating for high speed dry machining and other applications under high temperature environments.     

Mit TiN-Partikeln Lasermodifizierte Al2O3-Keramik im reversierenden Gleitkontakt unter Variation der Luftfeuchte und Temperatur

With TiN particles lasermodified Al₂O₃ ceramic under oscillating sliding contact at different humidities and temperatures A slightly porous, commercially available alumina ceramic was surface modified up to 170 μm thickness by adding TiN particles. The multiphase surface structure of this laser treated ceramic consisted of about 12 vol.% TiN, 16 vol.% grain boundary phase and 72 vol.% Al₂O₃. Tribological tests on the modified ceramic and for reference also on a highly dense alumina and titania were carried out in oscillating sliding contact against Al₂O₃ balls. In these tests, the temperature of the specimens was varied between 28°C and 500°C. At room temperature the relative humidity of the surrounding air was changed between 3% and 70% and additional tests were run by using distilled water as interfacial medium. The resulting multiphase microstructure showed substantially reduced friction and wear at different temperatures and also above relative humidities of about 35% at room temperature compared with the highly dense, commercially available alumina.     

Microstructural study of oxidation of carbon-rich amorphous boron carbide coating

Carbon-rich amorphous boron carbide (B _x C) coatings were annealed at 400°C, 700°C, 1000°C and 1200°C for 2 h in air atmosphere. The microstructure and composition of the as-deposited and annealed coatings were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), micro-Raman spectroscopy and energy dispersive X-ray spectroscopy (EDS). All of the post-anneal characterizations demonstrated the ability of carbon-rich B _x C coatings to protect the graphite substrate against oxidation. Different oxidation modes of the coatings were found at low temperature (400°C), moderate temperature (700°C) and high temperature (1000°C and 1200°C). Finally, the feasibility of the application of carbon-rich BxC instead of pyrolytic carbon (PyC) as a fiber/matrix interlayer in ceramics-matrix composites (CMCs) is discussed here.     

Novel system (K2TiF6-N2-Ti) to synthesize rod-like TiN nanopowders

ABSTRACT

A direct approach to synthesize rod-like TiN nanopowders by the reaction system (K₂TiF₆-N₂-Ti) is reported in this paper. Within a tube furnace, a solid precursor (K₂TiF₆) is thermally decomposed at 640°C producing TiO₂ (sea-urchin-like rutile microstructures), K₃TiOF₅ (by-product), and fluorine which moves toward a titanium foil by the effect of an N₂ flow synthesizing titanium fluoride species (TiF₄ and TiF₃). The titanium foil is located at different temperatures from 500°C to 900°C. Due to the fact that the quantity of fluorine is limited, the titanium fluoride species eventually become titanium nitrides. The effect of reaction temperature and time was studied and based on an analysis of variance, temperature was found to be the most important factor regarding to the phase composition of TiN nanostructures and also to the real production rate. The highest values of powder production rate (1.29) (the highest possible) and phase concentration (>98% TiN) were found at 800°C. Likewise, the reaction time was the most important factor in regard to obtaining the smallest particles (～16 nm) at 2.5 h.     

Effect of laser glazing on the thermo-mechanical properties of plasma-sprayed LaTi2Al9O19 thermal barrier coatings

Conventional duplex (DL) and functionally graded (FG) LaTi₂Al₉O₁₉ (LTA) coatings were deposited over C263 nickel alloy by air plasma spray (APS) and compared with subsequent laser glazing processes. The effect of laser glazing on adhesion strength and thermal barrier performance was investigated. The thermal barrier effect was measured using the temperature difference technique involving infrared (IR) rapid heater and the adhesion strength was measured using the scratch tester. The surface morphology and microstructure were analyzed by optical microscopy (OM), Scanning Electron Microscope (SEM) and 3D profilometer. Based on the experimental results, the laser glazing showed a remarkable temperature drop after IR rapid heating. The changes in porosity and grain refinement make more contributions to the temperature drop of the laser-glazed coatings than that of as-sprayed coatings. The temperature drop is about 110°C for laser-glazed LTA FG coating after 100?s of IR flash, while the drop in DL as-sprayed coating is 60°C compared to the base material.