Influence of annealing temperature on microstructure evolution of TiAlSiN coating and its tribological behavior against Ti6Al4V alloys

TiAlSiN multicomponent coating, owing to its high hardness and excellent high temperature resistance, was widely used in the cutting field of difficult-to-cut materials such as titanium alloys. For machining titanium alloys, high temperature is easy to gather on the tool chips and deteriorate the cutting tools. Moreover, high temperature will also promote the microstructure evolution and make the wear mechanism more complex. In this paper, TiAlSiN coatings were deposited on cemented carbides and annealed at 400 °C, 600 °C and 800 °C respectively for 60 min in air, followed by reciprocating friction tests against Ti6Al4V counterparts. AFM, SEM, EDS and XPS were applied to investigate the microstructure evolution and tribological behavior of TiAlSiN coating after high temperature annealing. The results demonstrated that the oxidation resistance of TiN phase in TiAlSiN coating was worse than Si₃N₄ and AlN phases. These nitrides can be oxidized to TiO₂, SiO_x and AlO_x under 600 °C, and the depth of oxide layer was increased with the rising annealing temperature, resulting in the coarsened microstructure. The wear mechanisms of as-deposited TiAlSiN coating were oxidation wear and adhesion wear. With the rising annealing temperature, abrasive wear was gradually enhanced. For the TiAlSiN coating annealed at 800 °C, abrasive wear became the dominant wear mechanism.     

High temperature friction and wear behavior of MoS<Subscript>2</Subscript>/Nb coating in ambient air

MoS₂ coatings are well-known for their solid lubricant properties and used as self-lubricants in vacuum and inert gas environments, and such coatings are not used in atmospheric conditions because of their deteriorating tribology. The tribological performance of MoS₂ solid lubricant coatings in the different atmospheres has been improved by the codeposition of a small amount of another metal. In this study, the tribological behavior of MoS₂/Nb coatings was investigated in ambient air at temperatures up to 500°C by using high-temperature pin-on-disc tribo testers and alumina balls as counterfaces. MoS₂/Nb coatings were deposited on silicon wafers and AISI 52100 steel substrate by closed-field unbalanced magnetron sputtering. The structural analyses of the coatings were performed using X-ray diffraction and scanning electron microscopy techniques. The hardness was measured using a microhardness tester.     

High-temperature oxidation behavior of the SiC layer of TRISO particles in low-pressure oxygen

Surrogate tristructural-isotropic (TRISO)-coated fuel particles were oxidized in 0.2 kPa O₂ at 1200–1600°C to examine the behavior of the SiC layer and understand the mechanisms. The thickness and microstructure of the resultant SiO₂ layers were analyzed using scanning electron microscopy, focused ion beam, and transmission electron microscopy. The majority of the surface comprised smooth, amorphous SiO₂ with a constant thickness indicative of passive oxidation. The apparent activation energy for oxide growth was 188 ± 8 kJ/mol and consistent across all temperatures in 0.2 kPa O₂. The relationship between activation energy and oxidation mechanism is discussed. Raised nodules of porous, crystalline SiO₂ were dispersed across the surface, suggesting that active oxidation and redeposition occurred in those locations. These nodules were correlated with clusters of nanocrystalline SiC grains, which may facilitate active oxidation. These findings suggest that microstructural inhomogeneities such as irregular grain size influence the oxidation response of the SiC layer of TRISO particles and may influence their accident tolerance.     

Characterization of Yb2SiO5-based environmental barrier coating prepared by plasma spray–physical vapor deposition

Due to the high-input power compared to atmospheric plasma spraying (APS), plasma spray-physical vapor deposition (PS-PVD) can primarily achieve a splat-like deposition, allowing for the preparation of high-density environmental barrier coatings (EBCs). In this paper, dense Yb₂SiO₅-based coatings are prepared by PS-PVD at different substrate temperatures. It was found that the coating deposited at the substrate temperature of 700 °C contained a large amount of silicon-rich amorphous phase. When the substrate temperature increased to 1100 °C and a slow cooling process after deposition was involved, a coating with high crystallinity of ～77% and low porosity of less than ～2% was achieved. Phase evolution of the coatings was studied by a semi-in-situ high-temperature X-ray diffractometer. During the heating process, metastable phases X1-Yb₂SiO₅ and α-Yb₂Si₂O₇ emerged and transformed into stable phases following high-temperature treatment. Furthermore, the effects of long-term thermal aging at 1300 °C on the microstructure, phase composition, thermal conductivity, and hardness of the coating prepared at the substrate temperature of 1100 °C were found to be limited.     

Effect of MoS2 content on friction and wear properties of Mo and S co-doped CrN coatings at 25–600 °C

With increasingly harsh working environments for mechanical systems and the rapid development of various high-tech industries, requirements for the stable operation of mechanical systems are increasing in a wide temperature range. Mo and S co-doped CrN coatings with different MoS₂ contents were prepared via unbalanced magnetron sputtering to provide better friction properties to the coatings at high temperatures. Scanning electron microscopy and nanoindentation were adopted to analyze the microstructure and mechanical performance. The mechanical performance of the coatings was enhanced by increasing the MoS₂ content, however, excessive MoS₂ reduced the mechanical properties of the coatings. Besides, the adhesion of the coatings first increased and then decreased rapidly with the increase of the MoS₂ content. In addition, the residual stress of the coating first decreased and then increased upon increasing the MoS₂ content. The high-temperature tribological behavior of the coatings was measured from room temperature (25 °C) to 600 °C. The CrN/MoS₂-0.6A coating was found to exhibit low friction and wear coefficient at room temperature and relatively good comprehensive properties at high temperature. This study provides a feasible design for engineering applications and lays the foundations for the preparation of coatings with superior high-temperature friction properties.     

Microstructure,mechanical, tribological,and oxidizing properties of AlCrSiN/AlCrVN/AlCrNbN multilayer coatings with different modulated thicknesses

Multilayer structure design is one of the most promising methods for improving the comprehensive performance of AlCrN-based hard coatings applied to cutting tools. In this study, four types of AlCrSiN/AlCrVN/AlCrNbN multilayer coatings, with different modulated thicknesses, were deposited to investigate their microstructure, mechanical, tribological, and oxidizing properties. All multilayer coatings exhibited grain growth along the crystallographic plane of (200) with a NaCl-type face-centered cubic (FCC) structure. The results show that, as the modulation thickness decreases from ～35 nm to ～10 nm, (1) the grain refinement effect is increasingly evident; (2) all multilayer coatings show a hardness of >30 GPa and an elastic modulus of >300 GPa. Both the ability to resist elastic strain to failure and the plastic deformation of multilayer coatings increase. In addition, their resistance to cracking reduces; (3) the wear rates of these multilayer coatings reduce successively from 1.78 × 10^?16 m³ N^?1 m^?1 to 7.7 × 10^?17 m³ N^?1 m^?1. This is attributed to an increase in self-lubricating VO_x and a decrease in adhesives from the counterparts; (4) the best high-temperature oxidation resistance was obtained for the multilayer coating with a modulated thickness of ～15 nm.     

Phase, microstructure, and oxidation resistance of yttrium silicates coatings prepared by a hydrothermal electrophoretic deposition process for C/C composites

Oxidation-resistant yttrium silicates coatings for SiC precoated carbon/carbon composites were prepared by a novel hydrothermal electrophoretic deposition process. Sonochemical-synthesized yttrium silicates nanocrystallites, isopropanol, and iodine were respectively used as source materials, solvent, and charging agent during the deposition. Phase compositions, surface and cross-section microstructures of the as-prepared multilayer coatings were characterized by an X-ray diffractometer (XRD) and a scanning electron microscopy (SEM). The influence of deposition temperatures on the phase, microstructure, and oxidation resistance of the multilayer coated C/C composites was particularly investigated. Results show that the as-prepared outer coatings are composed of yttrium silicates crystallites with a main phase of Y₂Si₂O₇ and Y₂SiO₅. The thickness and density of the yttrium silicates coatings are improved with the increase of deposition temperature. Compared with SiC coating prepared by pack cementation, the multilayer coatings prepared by pack cementation with a later hydrothermal electrophoretic deposition process exhibit better antioxidation properties. The as-prepared multilayer coatings can effectively protect C/C composites from oxidation at 1773 K in air for 35 h with a weight loss of 0.32 × 10⁻³ g/cm².     

Investigation of the conditions for synthesis of Ce<Subscript>0.9</Subscript>Y<Subscript>0.1</Subscript>O<Subscript>2</Subscript> dense coatings

The conditions for preparation of Ce_0.9Y_0.1O₂ (CYO) oxide coatings on La_0.8Sr_0.2MnO₃ (LSM) ceramic substrates by screen printing were investigated. The CYO compound was synthesized by the pyrolysis of polymer-salt composites with the aim of producing submicron powders with a uniform size distribution. Transmission electron microscopy of the microstructure of the CYO compound synthesized with ethylene glycol revealed that the synthesis product consists of ultrafine crystalline particles with an average size of 5–15 nm. The use of CYO nanopowders made it possible to prepare rather dense single-layer coatings on LSM substrates. It was demonstrated that annealing of the coatings at high temperatures leads to the recrystallization and coarsening of particles.     

High pressure sintering of cubic boron nitride compacts with Al and AlN

Cubic boron nitride (cBN) compacts, using 15 wt.% Al and 20 wt.% AlN respectively as additives, were sintered in the temperature range of 1300–1700 °C for 20 min under high pressure of 5.0 GPa. The hardness, microstructure, phase composition and cutting performance of the high pressure sintered samples were investigated. A liquid phase sintering and reaction process was observed in the cBN–Al system, which leads to the formation of AlN and AlB₂ as confirmed by X-ray diffraction (XRD) in the sintered compacts. Scanning electron microscopy (SEM) analysis shows that the samples have a homogeneous microstructure. The hardness decreases with increase of sintering temperature and reaches the highest Vickers hardness of 32.1 GPa at 1350 °C. While in the cBN–AlN system, AlN grains agglomerate heavily at temperature below ~ 1500 °C. As the sintering temperature increasing, Al₂O₃ appeared and the AlN agglomeration disappeared gradually. A highest cBN–AlN composite hardness of 29 GPa was achieved when sintered at 1600 °C. Turning tests showed that cBN compacts with 15 wt.% Al as the additive has a longer tool life as compared to that with 20 wt.% AlN. Our results indicated that cBN–Al system is more favourable to obtain well-sintered cBN compacts comparing with the cBN–AlN system.     

Thermal stability and oxidation resistance of V-alloyed TiAlN coatings

V-containing nitride coatings recently attract a wide range of research interests owing to their excellent tribological properties. To evaluate their comprehensive properties, a comparative study on the intrinsic thermal stability and oxidation resistance of TiAlN and TiAlVN coatings are conducted here. Ti_0.56Al_0.44N, Ti_0.50Al_0.44V_0.06N, and Ti_0.40Al_0.50V_0.10N coatings, deposited by cathodic arc evaporation, exhibit a single-phase face-centered cubic structure with a hardness of 28.9–29.8 GPa. The V-containing coatings show a pronounced age-hardening upon annealing, which contributes to a hardness increase of 3.7 and 4.8 GPa at 800 °C for Ti_0.50Al_0.44V_0.06N and Ti_0.40Al_0.50V_0.10N, respectively, corresponding to 2.9 GPa for Ti_0.56Al_0.44N. Also, alloying with V retards the formation of wurtzite AlN upon annealing, especially in Ti_0.50Al_0.44V_0.06N, and thus contributes to a higher hardness above 30 GPa even annealing at 1100 °C, while the hardness of Ti_0.56Al_0.44N significantly reduces to 27.8 ± 0.6 GPa. However, alloying with V into TiAlN leads to an earlier formation of rutile TiO₂ and also Ti-rich oxide top-layer on the outside surface instead of dense Al₂O₃, and thus degrades the oxidation resistance. When exposed to air at 700 °C for 10 h, the Ti_0.50Al_0.44V_0.06N and Ti_0.40Al_0.50V_0.10N coatings suffer from a severe oxidation, whereas only a compact oxide scale with a thickness of ~ 80 nm for Ti_0.56Al_0.44N is formed.     

Wear behaviors and high-temperature oxidation resistance properties of tantalum carbide layer

A TaC/Ta₂C bilayer is obtained by vacuum carburizing technology and characterized by scanning electron microscopy, X-ray photoelectron spectroscopy (XPS), X-ray diffraction, the nano-indentation, friction and wear test, high-temperature oxidation experiment. XPS analyses indicate that the carburized layer is composed of intermediate layer Ta₂C and outer-layer TaC. The total thickness of the carburized layer is approximately 20 μm. The nano-indentation hardness of the carburized layer along the depth direction varies from 14.632 to 35.832 GPa. The formation of the hard phase in carbide considerably improves the wear resistance of pure Ta. The high-melting-point ceramic phase in carbide improves the high-temperature oxidation resistance of pure Ta, thereby making it serve in high-temperature air environment for a short time.     

Characterization of wollastonite coatings prepared by sol–gel on Ti substrate

Wollastonite coatings were prepared by sol–gel on Ti substrate and their microstructures have been studied. The phase compositions and the surface morphologies of these coatings were examined by X-ray diffraction and scanning electron microscopy. Thermal behavior of dried gel was examined by differential scanning calorimetry (DSC) and thermogravimetry (TG). There are many cracks among coatings and particles with size about 200–300 nm distributing inside cracks. DSC and TG results show that the glass transformation temperature of dried gel is about 850°C. After calcined at temperature 900°C, the phase of coatings consists of wollastonite, SiO₂, and CaSi₂O₅.     

Effect of Annealing Temperature and Alumina Particles on Mechanical and Tribological Properties of Ni-P-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> Composite Coatings

In this study, the effect of annealing temperature and alumina particles on micro-hardness, corrosion, wear, and friction of Ni-P-Al₂O₃ composites coating is studied. The electroless nickel composite coating with various alumina particle content is deposited on a mild steel substrate. The corrosion behaviour and tribological behaviour (wear and friction) of the composite coated samples are investigated and compared with Ni-P coated samples. The micro-hardness, wear resistance, and corrosion resistance of the composite coating improved significantly after heat treatment (400 °C) and in the presence of alumina particles. The composite coating deposited with alumina particle concentration of 10 g/L in an electroless bath and heat treated at 400 °C shows excellent results compared to Ni-P, as-deposited Ni-P-Al₂O₃ coating and coatings heat treated at different annealing temperature (200 °C, 300 °C, and 500 °C). Microstructure changes and composition of the composite coatings due to incorporation of alumina particles and heat treatment are studied with the help of SEM (scanning electron microscopy), EDX (energy dispersive X-ray analysis and XRD (X-ray diffraction analysis).     

Complex study of protective Cr3C2–NiAl coatings deposited by vacuum electro-spark alloying,pulsed cathodic arc evaporation,magnetron sputtering,and hybrid technology

Coatings were obtained by vacuum electro-spark alloying (VESA), pulsed cathodic arc evaporation (PCAE), magnetron sputtering (MS) techniques and VESA-PCAE-MS hybrid technology using Cr₃C₂–NiAl electrodes. The structure of the coatings was analyzed using scanning and transmission electron microscopy, X-ray diffraction and energy-dispersive spectroscopy. Mechanical properties were determined by nanoindentation, while tribological properties were assessed using pin-on-disk tribometer. Corrosion resistance was estimated by voltammetry in 1 N H₂SO₄ and 3.5%NaCl solutions. Oxidation resistance tests were performed at 800°С in air. The VESA coating had the highest thickness, low friction coefficient and high wear resistance. PCAE coating demonstrated the highest hardness (24 GPa) and elastic recovery (59%), oxidation resistance and superior corrosion resistance both in 1 N H₂SO₄ (i_corr = 70 μА/cm²) and 3.5%NaCl (i_corr = 0.74 μА/cm²) solutions. The MS coating had average mechanical properties and low corrosion current density (71 μА/cm²) in 1 N H₂SO₄. Deposition of coatings using VESA-PCAE-MS hybrid technology led to an increase in corrosion and oxidation resistance at least by 1.5 times in comparison with the VESA coating.     

High-temperature oxidation induced layering process for Si–C–B–N ceramic fibers with SiC nanograins

High-temperature oxidation resistance is important for Si–C–B–N ceramic fibers when reinforcing ceramic matrix composites with superior reliability and faulting tolerance. At present, few studies have investigated on the high-temperature oxidation behavior of Si–C–B–N fibers, limiting their further applications. In this work, we analyzed the high-temperature oxidation process of Si–C–B–N ceramic fibers with SiC nanograins (SiBCN-SiCn fibers) at 1000–1500 °C in air. SiBCN-SiCn fibers stated to be oxidized at 1000 °C, with the formation of thin oxide layer. After oxidizing at 1300 °C, obvious oxide layer that mainly consisted of amorphous SiO₂ could be detected. Further oxidizing at 1500 °C caused the thickness increment of oxide layer, which could inhibit the oxidation products (CO, N₂) to release away from the fibers. The remained CO and N₂ may react with SiC nanograins to form SiO₂ and graphite-like g-C₃N₄, causing the formation of additional transition layer. Our finding may support useful information for the applications of SiBCN-SiCn fibers under harsh environment.     

Effect of Fe catalyst thickness and C2H2/H2 flow rate ratio on the vertical alignment of carbon nanotubes grown by chemical vapour deposition

Carbon nanotubes (CNTs) were fabricated by Chemical Vapour Depositon using a C₂H₂/H₂ mixture. They were grown on Si/SiO₂ substrate with Fe film as catalyst, deposited using thermal evaporation technique. The aim of this work is to emphasize the role of the Fe catalyst thickness and the C₂H₂/H₂ flow rate ratio to grow vertically aligned CNTs by thermal CVD. In order to investigate these aspects, four Fe metal films with thickness of 2.5, 3.5, 7.5 and 16 nm were deposited on Si/SiO₂ substrate and CNTs were grown with different C₂H₂/H₂ flow rate ratios, from 5/95 to 30/70 by thermal CVD at 750 °C. Results showed that CNTs were not vertically aligned with 16 nm catalyst thickness for all flow rate ratios, while CNTs were always vertically aligned for iron thickness less than 3.5 nm and vertically aligned only for a C₂H₂/H₂ flow rate ratio greater than 20/70 for the 7.5 nm catalyst thickness. Morphology and structural information about CNTs and Fe metal clusters were provided by field emission gun-scanning electron microscopy (FEG-SEM), atomic force microscopy (AFM) and high resolution transmission electron microscopy (HRTEM). Our results also indicate that for each flow rate ratio exists a critical thickness of iron catalyst under which vertically aligned CNTs are obtained.     

Fabrication of oxide-based near infrared-shielding coatings for a smart window to prevent infrared-induced photoaging in human skin

Oxide-based near infrared (IR)-shielding coatings consisting of quarter‐wave stacks of oxygen-deficient tantalum oxide (Ta₂O_5?x) and silicon oxide (SiO₂) multilayers and tin-doped indium oxide (In₂O₃) (ITO) films with the thicknesses of 200–600 nm can block the passage of IR-A (wavelength: 760–1400 nm) and IR-B (wavelength: 1400–3000 nm) radiation, respectively. In this study, the optical properties and microstructure of these oxide-based IR-shielding coatings were investigated. Transmission electron microscopy images indicated that amorphous Ta₂O_5?x/amorphous SiO₂ multilayers were uniform and dense. ITO films were found to be highly crystalline and show carrier concentrations of up to 7.1 × 10²⁰ cm^?3, resulting in the strong IR-B optical absorption due to the plasma excitation of the free carriers. Oxide-based IR-shielding coatings with an ITO thickness of 420 nm were found to have near-IR shielding rates of >90% and an average visible light transmittance of >70%. The effects of IR on human keratinocytes were studied to evaluate the IR-induced photoaging in human skin. It was found that the downregulation of cellular proliferation and the enhancement of senescence-associated β-galactosidase activity induced by IR irradiation were significantly inhibited by oxide-based IR-shielding coatings. Thus, this study provides a facile method for the development of coatings for smart windows with high IR-shielding ability and high visible light transmittance.     

Two‐Step Carbothermal Synthesis of AlN–SiC Solid Solution Powder Using Combustion Synthesized Precursor

In the present work, a two‐step carbothermal reduction method is employed to prepare the AlN–SiC solid solution (AlN–SiCss) powders by using a combustion synthesized precursor. The precursor is prepared by low‐temperature combustion synthesis (LCS) method using a mixed solution of aluminum nitrate, silicic acid, polyacrylamide, glucose, and urea. The synthesized LCS precursor exhibits a porous and foamy uniform mixture of Al₂O₃ + SiO₂ + C consisting of flaky particles. The carbothermal reduction in the LCS precursor is carried out in two steps. First, the precursors are calcined at 1600°C in argon for 3 h. Subsequently, the precursors are further calcined at 1600°C–1900°C in nitrogen for 3 h. The results indicate that the precursor calcined at and above 1850°C in nitrogen for 3 h yields the single‐phase AlN–SiCss powders. The synthesized AlN–SiCss powder exhibits near‐spherical particles with diameter of 200–500 nm. The experimental and thermodynamical results reveal that the formation of AlN–SiCss occurs via the diffusion of AlN into SiC by virtue of formation of a highly defective β′ intermediate during the second step reaction.     

Nanocasting Synthesis of Ultrafine WO<Subscript>3</Subscript> Nanoparticles for Gas Sensing Applications

Ultrafine WO₃ nanoparticles were synthesized by nanocasting route, using mesoporous SiO₂ as a template. BET measurements showed a specific surface area of 700 m²/gr for synthesized SiO_2, while after impregnation and template removal, this area was reduced to 43 m²/gr for WO3 nanoparticles. HRTEM results showed single crystalline nanoparticles with average particle size of about 5 nm possessing a monoclinic structure, which is the favorite crystal structure for gas sensing applications. Gas sensor was fabricated by deposition of WO₃ nanoparticles between electrodes via low frequency AC electrophoretic deposition. Gas sensing measurements showed that this material has a high sensitivity to very low concentrations of NO₂ at 250°C and 300°C.     

Superior high-temperature oxidation resistance of magnetron sputtered Hf–B–Si–C–N film

A hard and optically transparent amorphous Hf₇B₂₃Si₁₇C₄N₄₅ film with a contamination level less than 4 at%, prepared by reactive pulsed dc magnetron sputtering, was subjected to systematic investigation of high-temperature oxidation behavior in air up to 1700 °C. We focus on thermogravimetric analysis of the film in air and on the evolution of the film structure, microstructure and elemental composition with an annealing temperature ranging from 1100 °C to 1700 °C. The film exhibits a superior oxidation resistance up to 1600 °C due to a formation of a nanocomposite protective oxide layer on the surface above 1000 °C. The layer consists of monoclinic and tetragonal (or orthorhombic) HfO₂ nanocrystallites surrounded by a SiO₂-based amorphous matrix, most probably containing boron. The HfO₂ nanocrystallites exhibit a gradient in size with a dense population of small (a couple of nm) crystallites next to the interface and larger but dispersed crystallites close to the surface.