Oxide scales formation in nano-crystalline TiAlCrSiYN PVD coatings at elevated temperature

Nano-crystalline TiAlCrSiYN plasma vapor deposited (PVD) coatings were developed for oxidation and wear protection at elevated temperatures. Compositional tuning of the coatings was performed to enhance oxidation protection at elevated temperatures.The oxidation kinetics of the coatings has been studied over 180 h at 900 °C in air. Post-oxidation microstructural examinations of specimens were performed using transmission electron microscopy (TEM), secondary electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX) and glow discharge optical emission spectroscopy (GDOES). Micro mechanical characteristics of the coating were studied using a micro materials nanotest system. Wear resistance of the coatings were studied during turning of Inconel 718.Experimental results clearly indicate that the aluminum-rich PVD TiAlCrSiYN coatings with 60 at.% of Al can improve oxidation resistance of titanium aluminide alloy at the temperature 900 °C as well as wear resistance during machining of Inconel 718. It was shown that during oxidation, continuous protective alumina-based oxide films form on the surface. These oxides are predominantly (Al,Cr)₂O₃-based films. Self-healing behavior of the TiAlCrSiYN coatings was observed in its ultra-fine nano-crystalline structure.     

Microstructure evolution and thermal stability of an Fe-based amorphous alloy powder and thermally sprayed coatings

High velocity oxy-fuel (HVOF) thermal spraying has been used to produce coatings of an Fe–18.9%Cr–16.1%B–4.0%C–2.8%Si–2.4%Mo–1.9%Mn–1.7%W (in at.%) alloy from a commercially available powder (Nanosteel SHS7170). X-ray diffraction (XRD), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM) were employed to investigate the powder, as-sprayed coatings and annealed coatings which had been heated to temperatures in the range of 550–925 °C for times ranging from 60 to 3900 min. Microhardness changes of the coatings were also measured as a function of annealing time and temperature. The powder was found to comprise amorphous and crystalline particles; the former had a maximum diameter of around 22 μm. The coating was composed of splat like regions, arising from rapid solidification of fully molten powder, and near-spherical regions from partially melted powder which had a largely retained its microstructure. The amorphous fraction of the coating was around 50% compared with 18% for the powder. The enthalpies and activation energies for crystallization of the amorphous phase were determined. Crystallization occurred in a two stage process leading to the formation of α-Fe (bcc), Fe_1.1Cr_0.9B_0.9 and M₂₃C₆ phases. DSC measurements showed that the first stage occurred at 650 °C. Annealing the coating gave a hardening response which depended on temperature and time. The as-sprayed coating had a hardness of 9.2 GPa and peak hardnesses of 12.5 and 11.8 GPa were obtained at 650 and 750 °C, respectively. With longer annealing times hardness decreased rapidly from the peak.     

Hot corrosion behavior of detonation gun sprayed Cr3C2–NiCr coatings on Ni and Fe-based superalloys in Na2SO4–60% V2O5 environment at 900 °C

The present work investigates the hot corrosion resistance of detonation gun sprayed (D-gun) Cr₃C₂–NiCr coatings on Superni 75, Superni 718 and Superfer 800 H superalloys. The deposited coatings on these superalloy substrates exhibit nearly uniform, adherent and dense microstructure with porosity less than 0.8%. Thermogravimetry technique is used to study the high temperature hot corrosion behavior of bare and Cr₃C₂–NiCr coated superalloys in molten salt environment (Na₂SO₄–60% V₂O₅) at high temperature 900 °C for 100 cycles. The corrosion products of the detonation gun sprayed Cr₃C₂–NiCr coatings on superalloys are analyzed by using XRD, SEM, and FE-SEM/EDAX to reveal their microstructural and compositional features for elucidating the corrosion mechanisms. It is shown that the Cr₃C₂–NiCr coatings on Ni- and Fe-based superalloy substrates are found to be very effective in decreasing the corrosion rate in the given molten salt environment at 900 °C. Particularly, the coating deposited on Superfer 800 H showed a better hot corrosion protection as compared to Superni 75 and Superni 718. The coatings serve as an effective diffusion barrier to preclude the diffusion of oxygen from the environment into the substrate superalloys. It is concluded that the hot corrosion resistance of the D-gun sprayed Cr₃C₂–NiCr coating is due to the formation of desirable microstructural features such as very low porosity, uniform fine grains, and the flat splat structures in the coating.     

Evolution of microstructure and hardness of AE42 alloy after heat treatments

The AE42 magnesium alloy was developed for high pressure die casting (HPDC) from low-aluminum magnesium alloys. In this alloy the rare earth (RE) elements were shown to increase creep resistance by forming Al_xRE_y intermetallics along the grain boundaries. The present work investigates the microstructure of squeeze cast AE42 magnesium alloy and evaluates its hardness before and after heat treatments. The change in hardness is discussed based on the microstructural observations. Some suggestions are given concerning future design of alloy compositions in order to improve high temperature creep properties even further. It is shown that the microstructure of the squeeze-cast AE42 alloy is stable at high temperature 450 °C. The subsequent solution and ageing treatments have a limited effect on the hardness. The weak age-hardening is attributed to the precipitation of small amount of Mg₁₇Al₁₂-phase with the use of about 0.7 wt.% aluminum. The heat treatment to achieve a maximum increase in the hardness is: solution treatment at 450 °C for 5–10 h followed by an ageing treatment at 190–220 °C for about 5 h.     

Mechanical properties and scratch test resistance of nickel-boron coated aluminium alloy after heat treatments

Electroless nickel-boron deposits were synthesized on aluminium alloys and submitted to heat treatments under neutral (95% Ar + 5% H₂) atmosphere. Two set of treatment conditions were used: 1 h at 400 °C and 4 h at 180 °C. Micro- and nanohardness measurements were carried out on the free surface of the sample and on polished cross-sections. A comparative hardness study was conducted to assess the influence of load, indent position (free surface or cross section), and heat treatment on the results of the indentation tests. Scratch tests were made on selected coatings to assess their adhesive properties and scratch resistance. Roughness measurements were carried out on the coatings before and after heat treatments. The samples were also investigated by XRD (X-ray Diffraction), SEM (Scanning electron microscopy) and optical microscopy to link their mechanical properties to their composition, structure and morphology.     

Investigation on the Electrical Properties of Vacuum Cold Sprayed SiC-MoSi2 Coatings at Elevated Temperatures

SiC-MoSi₂ composite powders was prepared by wet milling with MoSi₂ powders and SiC loose grinding ball in alcohol solution. Vacuum cold spray (VCS) process was used to deposit SiC-MoSi₂ electric conducting composite coatings. The microstructure of the VCS SiC-MoSi₂ composite coatings were characterized by scanning electron microscopy. The electrical resistance of the coatings was measured using a four-point probe method. The effects of the deposition parameters on the electrical resistivity of the composite coatings were investigated. The electrical properties of the coatings at elevated temperatures in air and Ar gas atmospheres were also explored. The results show that the electrical resistivity of SiC-MoSi₂ coatings decreases with increasing He gas flow rates ranged from 3 to 6 L/min. The electrical resistivity increases with the increase in heat treatment temperature due to “pesting” behavior of MoSi_2. The electric conductive property of the VCS SiC-MoSi₂ coating is significantly improved after heat treatment at 1000 °C for 3 h in Ar protective atmosphere without oxidation. A minimum resistivity of the heat treated coating is 0.16 Ω · cm.     

Abrasive wear resistance of electroless Ni-P coated aluminium after post treatment

Electroless nickel (EN) coatings are recognised for their hardness and wear resistance in automotive and aerospace industries. In this work, electroless Ni-P coatings were deposited on aluminium alloy substrate LM24 (Al-9 wt.% Si alloy) and the effect of post treatment on the wear resistance was studied. The post treatments included heat treatment and lapping with two different surface textures. Scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), X-ray diffraction (XRD) and micro-abrasion tester were used to analyse morphology, structure and abrasive wear resistance of the coatings. Post heat treatment significantly improved the coating density and structure, giving rise to enhanced hardness and wear resistance. Microhardness of electroless Ni-P coatings with thickness of about 15 μm increased due to the formation of Ni₃P after heat treatment.     

The Effect of Post-Heat Treatment on Microstructure of 316L Cold-Sprayed Coatings and Their Corrosion Performance

The combined effects of process gases and post-heat treatment temperature on the microstructure of 316L cold-sprayed coatings on Al5052 substrates have been investigated in this study. The stainless steel coatings were subjected to heat treatment at four different temperatures (250, 500, 750, and 1000 °C) to study the effect of heat treatment. In addition, the corrosion performances of the coatings at different process temperatures have been compared using the potentiodynamic scanning technique. Microstructural characterization of the coatings was carried out using scanning and transmission electron microscopy and x-ray diffraction. The results of present study showed that cold-sprayed stainless steel coatings processed with helium exhibited higher corrosion resistance than those of coatings sprayed with nitrogen process gas. This could partially be attributed to the reduction in porosity level (4.9%) and improvement of particle-particle bonding. In addition, evaluation of the mechanical and microstructural properties of the coatings demonstrated that subsequent heat treatment has major influence on the deposited layers sprayed with He process gas.     

Effects of iron catalyst on the formation of crystalline domain during carbonization of electrospun acrylic nanofiber

To investigate the effects of introducing the iron compound on the carbonization behavior polyacrylonitile (PAN)-based electrospun nanofibers were carbonized with or without iron(III) acetylacetonate (AAI) over the temperature range of 900–1500 °C in nitrogen atmosphere. The morphological characteristics of the carbon nanofibers were investigated using X-ray diffractometer (XRD), Raman spectroscopy, field emission scanning electron microscopy, and transmission electron microscopy. The electrical conductivity of the carbon nanofiber web was measured by four-point probe method. The iron catalyst had a profound effect on the crystal structure of the carbonized nanofiber. In the presence of AAI the nanofibers carbonized at 1300 °C developed graphite structure, which could be obtained at the temperature higher than 2000 °C in the absence of the catalyst. The in-plane size of the graphite crystals (L_a) was measured to be about 6.5 nm by Raman spectroscopy and the (0 0 2) spacing by XRD was 0.341 nm.     

Effects of TiN film coating on electrochemical behaviors of nanotube formed Ti-xHf alloys

Ti-xHf (x=10%, 20%, 30% and 40%, mass fraction) alloys were prepared by arc melting, and the microstructure was controlled for 24 h at 1 000 °C in argon atmosphere. The formation of nanotube was conducted by anodizing on Ti-Hf alloys in 1.0 mol/L H₃PO₄ electrolytes with small amounts of NaF at room temperature. And then TiN coatings were coated by DC-sputtering on the anodized surface. Microstructures and nanotube morphology of the alloys were examined by field emission scanning electron microscopy(FE-SEM) and X-ray diffractometry(XRD). The corrosion properties of the specimens were examined through potentiodynamic test (potential range from −1 500 to 2 000 mV) in 0.9 % NaCl solution by potentiostat. The microstructure shows the acicular phase and α′ phase with Hf content. The amorphous oxide surface is transformed to crystalline anatase phase. TiN coated nanotube surface has a good corrosion resistance.     

Effects of Arc Spray Process Parameters on Corrosion Resistance of Ti Coatings

In order to improve the corrosion resistance of carbon steel structures in marine environment, Ti wires were sprayed to a steel substrate using arc spray technique, and orthogonal experimental design was used to investigate the effects of the fluctuation in the main parameters of spray process on the microstructure and the corrosion resistance of sprayed coatings. The results show that the corrosion resistance of sprayed coatings is very sensitive to spray process parameters, corrosion current density can decrease from 997.7 to 5.08 μA cm⁻² by optimizing process parameters. The coatings are composed of TiN and Ti₂O, and the corrosion resistance of coatings can be improved with the decrease in the contents of oxides. The spray distance should be exactly monitored and controlled in arc spray process because of its great effects on the quality of sprayed coatings.     

The effects of heat treatment and gas atmosphere on the thermal conductivity of APS and EB-PVD PYSZ thermal barrier coatings

The effects of heat treatment and gas atmosphere on thermal conductivity of atmospheric plasma sprayed (APS) and electron beam physical vapor deposited (EB-PVD) partially Y₂O₃ stabilized ZrO₂ (PYSZ) thermal barrier coatings (TBCs) were investigated. Two-layer samples that had an EB-PVD coating deposited on bond coated nickel-base superalloy IN625 substrates, free-standing APS and EB-PVD coatings as well as a quasi-free-standing EB-PVD PYSZ coating (coating on semitransparent sapphire) were included in the study. Thermal diffusivity measurements for determining thermal conductivity were made from room temperature up to 1150 °C in vacuum and under argon gas using the laser flash technique. To investigate the effect of heat treatment on thermal conductivity, coatings were annealed at 1100 °C in air. For both the APS and EB-PVD PYSZ coatings the first 100 h heat treatment caused a significant increase in thermal conductivity that can be attributed to microstructural changes caused by sintering processes. Compared to the measurements in vacuum, the thermal conductivity of APS coatings increased by about 10% under argon gas at atmospheric pressure, whereas for the EB-PVD coatings, the influence of gas on thermal conductivity was relatively small. The effect of gas on the thermal conductivity of APS and EB-PVD PYSZ coatings can be attributed to amount, shape, and spatial arrangement of pores in the coating material.     

Syntheses and mechanical properties of Mo-Si-N coatings by a hybrid coating system

In this work, comparative studies on microstructure and mechanical properties between Mo₂N and Mo-Si-N coatings were conducted. Ternary Mo-Si-N coatings were deposited on steel substrates (AISI D2) and Si wafers by a hybrid method, where arc ion plating (AIP) technique was combined with a magnetron sputtering technique. Instrumental analyses of X-ray diffractometer (XRD), high-resolution transmission electron microscopy (HRTEM), and X-ray photoelectron spectroscopy (XPS) revealed that the Mo-Si-N coatings must be a composite consisting of fine Mo₂N crystallites and amorphous Si₃N₄. The hardness value of Mo-Si-N coatings significantly increased from 22 GPa of Mo₂N coatings to about 37 GPa with Si content of 10 at.% due to the refinement of Mo₂N crystallites and the composite microstructure characteristics. The average friction coefficient of the Mo-Si-N coatings gradually decreased from 0.65 to 0.4 with increasing Si content up to 15 at.%. The effects of Si content on microstructure and mechanical properties of Mo-N coatings were systematically investigated.     

Effect of Thermal Aging on Microstructure and Functional Properties of Zirconia-Base Thermal Barrier Coatings

Thermal barrier coating (TBCs) systems made of plasma sprayed zirconia are commonly used in gas turbine engines to lower metal components surface temperature and allow higher combustion temperature that results in higher fuel efficiency and environmentally cleaner emissions. Low thermal conductivity and long service life are the most important properties of these coatings. The objective of this work was to study the influence of a long-term heat treatment (i.e., 1200 °C/2000 h) on different characteristics of atmospheric plasma sprayed TBCs. Two zirconia feedstock materials were evaluated, namely, yttria partially stabilized zirconia and dysprosia partially stabilized zirconia. Several spray conditions were designed and employed to achieve different coating morphologies. Microstructure analyses revealed that the coating microstructure was significantly dependent on both operating conditions and heat treatment conditions. Significant changes in coatings porosity occurred during heat treatment. The lowest thermal conductivity was reached with the dysprosia partially stabilized zirconia material. Heat treatment affected TBCs adhesion strength as well.     

Microstructure and Wear Resistance Evolution of HVOFSprayed WC-（W,Cr）2C-Ni Coating with Post Heat Treatment In Air Atmosphere

WC-(W,Cr)2C-Ni coating was prepared on 1Cr18Ni9Ti stainless steel and C-276 Ni-base Hastelloy by high velocity oxy-fuel(HVOF)spraying.The effect of post heat treatment in air atmosphere on the microstructure,phase composition,microhardness,fracture toughness,and wear resistance of HVOF-sprayed WC-(W,Cr)2C-Ni coating was investigated.The microstructure and phase composition of the coatings were analyzed by means of field emission scanning electron microscopy(FESEM)and X-ray diffraction(XRD).The microhardness and fracture toughness of the coatings were measured using a microhardness tester and a Vickers hardness tester.Moreover,dry friction and wear behavior of the coatings sliding against Si3N4 ball was investigated using an oscillating friction and wear tester;and the worn surfaces of the coatings were analyzed by means of scanning electron microscopy(SEM).It was found that heat treatment within 500-800°C resulted in crystallization of amorphous phase in as-sprayed coating,generating nanoscale new phases such as NiWO4,CrWO4 and Cr2WO6.Besides,heat treatment led to increase of the microhardness of as-sprayed coating,and the highest microhardness was obtained after heat treatment at 800°C.The fracture toughness and wear resistance of the as-sprayed coating increased with increasing heat treatment temperature up to 700°C but tended to decrease with further elevating temperature.In other words,the mechanical properties and wear resistance of the as-sprayed coatings were worsened owing to excessive growth of oxidation grains and depletion of ductile Ni binder after heat treatment above 700°C.Thus it was suggested that as-sprayed ceramic composite coating should be post heat treated in air at a moderate temperature of 700°C so as to achieve the optimized mechanical properties and wear resistance.     

On the Early Stage Isothermal Oxidation of APS CoNiCrAlY Coatings

The aim of this study is to analyze the evolution of microstructural and room temperature mechanical properties of air plasma sprayed (APS) CoNiCrAlY coatings before and after early stage high-temperature oxidation. To this purpose, selected samples were isothermally heat treated at 1110 °C for different durations. Phase analysis and oxide scale characterization were performed using x-ray diffraction. Morphological and microstructural features of as-sprayed and oxidized CoNiCrAlY coatings were analyzed by scanning electron microscopy and energy dispersive x-ray spectroscopy. After heat treatment, a duplex oxide scale, composed of an inner α-Al₂O₃ layer and an outer spinel-type oxide layer, was observed on coating top-surface. The nanoindentation technique was employed to study the evolution of the mechanical properties. An increase in Young’s modulus and hardness with increasing the aging time was observed, this effect was mainly addressed to the partial densification of coating microstructure.     

电弧喷涂锡基巴氏合金涂层的组织与性能

针对电弧喷涂巴氏合金涂层组织与铸造组织的显著差异,借助于扫描电子显微镜、能谱分析和X射线衍射分析涂层的微观组织结构;测试了巴氏合金涂层在钢铁基体上的结合强度,研究了涂层与碳钢及铸铁组成摩擦副时的磨损表现.结果表明,电弧喷涂巴氏合金涂层的组织细小、均匀,SnSb和Cu6Sn5化合物的形态趋于不规则的块状或近于球形;施加过渡底层可以使涂层更可靠地与钢铁基体结合;在润滑条件下,涂层表现出比铸造合金更好的耐摩性能.     

Influence of liquid nitrogen quenching on the evolution of metastable phases during plasma spraying of (ZrO2–5 wt.% Y2O3)–20 wt.% Al2O3 coatings

The preparation of nanostructured (ZrO₂–5 wt.% Y₂O₃)–20 wt.% Al₂O₃ coatings by atmospheric plasma spraying of commercially available micron-scale powders is reported. Materials were prepared by means of a standard spraying technique and by using an improved technique that allows for the quenching of the material using liquid nitrogen-cooled substrates. Quenching leads to the controlled formation of metastable phases. The influence of liquid nitrogen cooling on the formation of the metastable phases was studied by X-ray diffraction under a grazing incidence angle of 1°. A significant increase in the amount of the metastable zirconia phase and a more homogeneous composition along the thickness were found compared to the regularly sprayed coatings. All materials were subjected to a thermal treatment for 1 h at 1400 °C to study the evolution of stable phases.     

Oxidation behavior at 300–1000 °C of a (Mo,W)Si2-based composite containing boride

The oxidation behavior of a (Mo,W)Si₂ composite with boride addition was examined at 300–1000 °C for 24 h in dry O₂. The oxidation kinetics was studied using a thermobalance, and the oxide scales were analyzed using a combination of electron microscopy (SEM/EDX, FIB, BIB) and XRD. Accelerated oxidation was found to occur between 500 °C and 675 °C, with a peak mass gain at 625 °C. The rapid oxidation is attributed to the vaporization of molybdenum oxide that leaves a porous and poorly protective silica layer behind. At higher temperature (700–1000 °C) a protective scale forms, consisting of a dense SiO₂/B₂O₃ glass.     

Nano-phenomena during exposure of plasma-sprayed ceria stabilised zirconia coatings to oxygen rich environments

Plasma-sprayed zirconia coatings are widely used for oxidation protection. Up-to-date, microstructural stabilisation of such coatings is mainly achieved with yttrium oxide; however recent scientific attempts indicated that ceria stabilised zirconia coatings could be a very promising alternative. In the present work, a coating of this kind has been deposited onto a Ni-based superalloy with the interference of a NiCrAlY bond coating by plasma spraying. Its oxidation resistance was estimated with thermogravimetric analysis with exposure at 1100 °C in air. The microstructure of the as-sprayed coating was studied with X-ray diffraction and electron microscopy before and after oxidation. From this examination it was deduced that ceria stabilised zirconia (CSZ) coating is rather stable at the temperature under question. However reduction of ceria takes place at larger exposure periods.