High-Temperature Oxidation of Nickel-Based Cermet Coatings Containing WC and Al<Subscript>2</Subscript>O<Subscript>3</Subscript> Nanosized Particles

This paper investigates the high-temperature oxidation of cermet coatings composed of two types of nanosized particles (WC and a mixture of WC and Al₂O₃) incorporated in nickel and produced by co-electrodeposition. For this purpose, high-temperature oxidation tests were conducted at three temperatures (500, 600, and 700 °C) in dry air with 6 time intervals up to 96 h and mass changes at each specific time interval was measured. Statistical techniques were used to calculate the oxidation rate constants (k) and growth-rate time constants (a) for all coatings. The confidence intervals associated with tests were also calculated. The results showed linear to sub-parabolic oxidation rates for coatings composed of only WC particles and sub-liner to liner oxidation rates for coating with both WC and Al₂O₃ particles. The reduction in oxidation rates for coatings with both WC and Al₂O₃ particles were correlated to the addition of Al₂O₃ particles in the matrix.     

Oxidation behaviour of Nimonic 263 in high-temperature supercritical water

The oxidation tests of the Nimonic 263 alloy exposed to deaerated supercritical water at 600–700°C under 25?MPa were carried out for up to 1000?h. Oxidation rate increased with an increase in temperature. The microstructure and phase composition of oxide scale were analysed by scanning electron microscopy/energy dispersive X-ray spectroscopy, X-ray diffraction and X-ray photoelectron spectroscopy. It can be seen that a complex oxide structure formed on the surface of Nimonic 263 including an outer layer of Ni–Fe/Ni–Cr spinel oxide, Ni/Co hydroxide and TiO₂ and an inner layer of a mixture of NiCr₂O₄ and Cr₂O₃ while the innermost layer is made up of Cr₂O₃. The MoO₃ can be observed at 600°C but disappeared with the increasing temperature. The growth mechanism of oxide scale was discussed.     

Oxidation Mechanisms of Copper and Nickel Coated Carbon Fibers

Differential-Thermal Analysis (DTA) and X-ray diffraction analysis were applied to determine the mechanisms of high-temperature oxidation of copper- and nickel-coated carbon fibers. Both kinds of coatings were deposited by electroless plating onto the fiber surface. The as-deposited copper film was crystalline, whereas the nickel coating consisted of an amorphous Ni–P alloy. Coated fibers were heated from room temperature to 900 °C in air at 10 °C min^?1. For the copper coating, the main oxidation product formed at low temperatures was Cu₂O, while at higher temperatures was CuO. The crystallization of Ni–P took place at 280–360 °C with the formation of Ni and Ni₃P. The final compounds were NiO, Ni₂P and Ni₃(PO₄)₂. After complete oxidation of the carbon fibers, copper and nickel-oxidized microtubes were obtained. Besides, while copper reduced the temperature of the fiber oxidation, nickel coatings increased the minimum temperature needed for this reaction.     

Corrosion Inhibition of 304 Stainless Steel by Nano-Sized Ti/Silicone Coatings in an Environment Containing NaCl and Water Vapor at 400–600°C

The corrosion behavior of 304 stainless steel (SS) and its corrosion inhibition by brushing nano-sized Ti/silicone coatings on its surface in an environment containing a solid NaCl deposit and water vapor at 400–600°C was studied. Results indicated that water vapor or NaCl, especially water vapor plus NaCl accelerated the corrosion of the steel markedly. The corrosion scales of the uncoated steel had a duplex structure at 400–500°C and internal oxidation occurred for the uncoated steel at 600°C in an environment containing NaCl and water vapor. The corrosion of the 304SS was inhibited efficiently by the coatings at 400–500°C, and the coated steel suffered corrosion to some extent and most of the coatings were destroyed at 600°C. X-ray diffraction (XRD) indicated that the corrosion products of the uncoated steel were mainly Fe₂O₃, Cr₂O₃, NiO or Na₂CrO₄, and the coatings consisted mainly of TiO₂ and SiO₂ after exposure at 400–500°C. The good corrosion resistance of the nano-sized Ti/silicon coatings was attributed to the formation of SiO₂, and TiO₂ that resulted from the decomposition of the organic components in the coating and fast oxidation of nano-Ti powder respectively during the experiments, TiO₂ mixed together with SiO₂ and formed a new coating on the steel surface that played an important role in the protection of the steel.     

Oxidation of X20 in Water Vapour: The Effect of Temperature and Oxygen Partial Pressure

The oxidation behaviour of X20 in various mixtures of water, oxygen, and hydrogen was investigated at temperatures between 500 °C and 700 °C (time: 336 h). The samples were characterised using reflected light microscopy and scanning electron microscopy equipped with energy dispersive spectroscopy. Double-layered oxides developed during oxidation under all conditions. The morphology of the oxide layers was strongly influenced by temperature, whereas the influence of the oxidising environment appeared to be less pronounced, as long as it contained water vapour. The inner layer consisted of converted M₂₃C₆ embedded in Fe–Cr spinel after oxidation at 500 and 600 °C, while alternating layers of Cr-rich and Cr-poor oxide were observed after oxidation at 700 °C. An internal oxidation zone developed during oxidation at 500 and 600 °C, with its depth influenced by the oxidising environments. The results are discussed based on the various hypotheses of the accelerating effect of water vapour that have been put forth in the literature.     

The Effect of Colored Titanium Oxides on the Color Change on the Surface of Ti-5Al-5Mo-5V-1Cr-1Fe Alloy

In the present investigation, a color change on the surface of Ti-5Al-5Mo-5V-1Cr-1Fe alloy was studied through thermal oxidation experiments in the temperature range of 100-1000 °C with an interval of 50 °C. The phase composition and morphology of oxide layer were characterized by x-ray diffraction and light optical microscopy, respectively. The result shows that the achieved colors after thermal oxidation followed a chromatic scale which went from silver white to light yellow to golden yellow to blue and then to light green and brownish black. The color change on the alloy mainly resulted from the different colored titanium oxides in the oxide layer. The silver white, yellow, and blue on the alloy with the oxidation temperature below 600 °C were the results of TiO₂ white tint, TiO golden tint, and Ti₂O₃ blue color, respectively. The light green was the mixed color of TiO golden tint and Ti₂O₃ blue color in the oxidation temperature range of 600-700 °C. However, at the oxidation temperatures exceeding 750 °C, the color turned to be brownish black. It might be associated with the thick, porous, and multilayered oxide layer. Consequently, it can be suggested that the illustration of the color change is vitally necessary for assessing the quality of the final workpieces according to the color change on titanium alloys.     

Cyclic Oxidation Behavior of the Ti–6Al–4V Alloy

The cyclic oxidation behavior of the Ti–6Al–4V alloy has been studied under heating and cooling conditions within a temperature range from 550 to 850 °C in air for up to 12 cycles. The mass changes, phase, surface morphologies, cross-sectional morphologies and element distribution of the oxide scales after cyclic oxidation were investigated using electronic microbalance, X-ray diffractometry, scanning electron microscopy and energy dispersive spectroscopy. The results show that the rate of oxidation was close to zero at 550 °C, obeyed parabolic and linear law at 650 and 850 °C, respectively, while at 750 °C, parabolic—linear law dominated. The double oxide scales formed on surface of the Ti–6Al–4V alloy consisted of an inner layer of TiO₂ and an outer layer of Al₂O₃, and the thickness of oxide scales increased with an increasing oxidation temperature. At 750 and 850 °C, the cyclic oxidation resistance deteriorated owing to the formation of voids, cracks and the spallation of the oxide scales.     

低氧分压下NiTi记忆合金氧化行为的研究

本文研究了NiTi形状记忆合金在H₂-H₂O气氛下400-700 °C的氧化行为。合金的氧化过程遵循立方规律,氧化激活能127.52 kJ/mol。氧化显著降低了试样表面的Ni含量。400 °C氧化的试样,其表面形貌与其他试样不同,并且氧化膜较薄,截面结构无法用SEM分析。500 °C、600 °C、700 °C氧化的试样,表面有两种形貌的氧化物,一种是颗粒状氧化物,另一种是晶须状氧化物。截面分析表明,氧化膜分为两层,上层由TiO₂构成,下层由Ni₃Ti构成,两层界面处有孔洞生成。     

Oxidation behavior of porous Ti3SiC2 prepared by reactive synthesis

High-purity porous Ti₃SiC₂ with a porosity of 54.3% was prepared by reactive synthesis and its oxidation behavior was evaluated under air in the temperature range from 400 to 1000 °C. Thermogravimetric analysis and differential scanning calorimetry (TG-DSC), scanning electron microscope (SEM), X-ray diffractometometry (XRD), energy dispersive spectrometer (EDS), Raman spectrum, BET surface area analysis, and pore-parameter testing were applied to the studies of the oxidation kinetics, phase composition, micro morphology, and porous structure parameters of porous Ti₃SiC₂ before and after oxidation. The results showed that the formation of TiO₂ oxidized products with different modifications was the primary factor influencing the oxidation resistance and structural stability of porous Ti₃SiC₂. Cracks were observed in the samples oxidized in the full temperature range of 400-1000 °C because of the growth stress and thermal stress. At 400-600 °C, anomalous oxidation with higher kinetics and the aberrant decrement in pore size and permeability were attributed to the occurrence of severe cracking caused by the formation of anatase TiO₂. At raised temperatures over 600 °C, the cracking phenomena were alleviated by the formation of rutile TiO₂, but the outward growth of the oxide scales detrimentally decreased the connectivity of porous Ti₃SiC₂.     

Phase composition,morphology and element contents of micro-arc oxidation ceramic coatings on Ti–6Al–4V alloy under different calcination conditions

Compound ceramic coatings with the main crystalline of Al_2TiO_5(in the as-prepared coating without treatment) were prepared in situ on the surface Ti–6Al–4V alloy by means of pulsed bipolar micro-arc oxidation in Na AlO_2 solution. For the purpose of studying the antioxidation properties of the samples, the coated samples treated in argon and the as-coated samples were calcined in air at 1000 °C. And the related characteristics were investigated by X-ray diffraction(XRD), scanning electron microscopy(SEM) and X-ray fluorescence(XRF) spectroscopy, respectively. The results show that, when it was calcined in air for 1 h, Al_2TiO_5in the as-prepared coating decomposed and transformed into α-Al_2O_3 and rutile TiO_2.However, after almost 4 h in argon, Al_2TiO_5in the asprepared coating decomposed and the final coating surface contents are completely α-Al_2O_3, and those of the middle interface are mainly Al_2O_3 and Ti_2O_3. The morphologies of the coatings after calcination in argon and air are different.High-temperature oxidation occurred violently in the alloy substrate without coatings. Furthermore, the weight gain curves of the as-prepared samples and the coated samples treated in argon both show a parabolic shape.     

Hot Corrosion Behavior of Inconel 625 Superalloy in Eutectic Molten Nitrate Salts

Corrosion resistance of Inconel 625 Ni-based superalloy was studied in a molten nitrate salt consisting of 40 KNO₃–60 NaNO₃ (wt%) at 500 and 600 °C. Open-circuit potential, potentiodynamic polarization, electrochemical impedance spectroscopy and gravimetric tests were used to evaluate the degradation mechanism and corrosion behavior of the alloy. Surface morphology and chemical analysis of corrosion products were characterized by means of scanning electron microscopy and energy-dispersive X-ray spectrometry. The weight-loss curves showed that with the increase in temperature, the oxidation rate and mass gain increased; the relationship between the mass gain and time was close to the parabolic oxidation law. The electrochemical corrosion results confirmed that during the exposure of Inconel 625 alloy to the molten salts, nickel dissolves as a result of non-protective NiO layer formed. The formation of a non-protective oxide layer with low barrier property was responsible for observing the weak corrosion resistance of the alloy at high temperatures (500 and 600 °C). Cyclic polarization tests showed a positive hysteresis confirming the nucleation and growth of stable pits on the surface of Inconel 625 at high anodic overpotentials. Sodium nitrite acts as an efficient pitting inhibitor for this case. In this way, the sodium nitrite with the concentration of 0.1 molal was found to have an optimum inhibition effect on pit nucleation at 600 °C.     

钼添加对CrN涂层抗氧化性能的影响

研究钼添加对CrN涂层微观结构和抗氧化性能的影响,采用反应磁控溅射法在硅片和高速钢片上制备不同Mo含量的Cr-Mo-N涂层,并在500~800 ℃的高温空气中退火1 h,用X射线衍射（XRD）、拉曼光谱和扫描电子显微镜（SEM）对涂层退火前后的微观形貌进行表征。沉积的CrN和Cr-Mo-N涂层均表现出基于CrN晶格的B1面心立方相（fcc）。Mo离子取代Cr-N晶格中的Cr离子,形成Cr-Mo-N固溶体。在600 ℃时,XRD和拉曼光谱表明,Mo含量较高的Cr-Mo-N涂层中形成MoO₃相,表面较粗糙,含氧量较高。在700 ℃时,CrN涂层由于内应力的作用,其横截面形貌为疏松的柱状晶,并有一定的多孔区,而Cr-Mo-N涂层则为致密的柱状晶结构。低Mo含量（<17at%）的Cr-Mo-N涂层比CrN涂层具有更好的抗氧化性。     

An Investigation into the Nature of the Oxide Layer Formed on Kovar (Fe–29Ni–17Co) Wires Following Oxidation in Air at 700 and 800 °C

This work provides new insight and evidence that challenges and extends the accepted view of the oxidation behaviour of Kovar (ASTM-15). Specimens of 2 mm diameter Kovar wire were oxidised in air at 700 or 800 °C for 10 min. The resulting oxide layers were analysed by X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy with energy-dispersive X-ray spectroscopy, scanning transmission electron microscopy and Raman spectroscopy. Oxide layers of approximately 2 and 4 µm thickness were formed at 700 and 800 °C, respectively. These were found to contain iron, cobalt and traces of nickel. The combination of analysis techniques revealed that the oxide contains Fe₂O₃ in addition to (Fe, Co, Ni)₃O₄, a spinel oxide, in contrast to the combinations of Fe₃O₄, Fe₂O₃ and FeO that are typically reported. The oxide layer was found to be complex, consisting of multiple layers with different compositions, which is overlooked in the existing literature.     

Microstructure Evolution During Steam Oxidation of a Nb Stabilized Austenitic Stainless Steel

The oxidation behaviour of TP 347H FG in mixtures of water, oxygen, and hydrogen was investigated at 500, 600, and 700 °C for a fixed oxidation time of 336 h. The samples were characterised using X-ray diffraction, reflective light and electron microscopy methods. Thin discontinuous double-layered oxide scales developed during oxidation at 500 °C, whereas continuous double-layered oxide scales covered the entire sample surface after oxidation at 600 and 700 °C. The major part of the inner oxide layer developed within the former alloy grains, whereas a Fe–Cr spinel formed along the former alloy grain boundaries. Transmission electron microscopy and electron energy loss spectroscopy investigations revealed that the part of the scale that grows into the alloy grains consists of particles of Fe–Cr spinel embedded in a metallic Fe–Ni matrix, which indicates that this part of the scale grows by an internal oxidation mechanism. The thickness of the inner oxide zone at high humidity (46%) is not significantly affected by the type of carrier gas used, whereas this thickness at low humidity (8% H₂O) is sensitive for the carrier gas and increases in the following order: air < Ar+7% H₂ < Ar, indicating that the presence of oxygen or hydrogen in addition to a relatively low content of water vapour counteracts the effect of water vapour on the development of the inner oxide zone.     

Roasting reaction of ferrous sulfide

The rate and mechanism of oxidation of ferrous sulfide have been studied by means of the spring balance and X-ray diffraction analysis over the temperature range from 500° to 700°C. The complete oxidation to oxides begins at 600°C. At the initial stage of oxidation, a slight increase of weight was found. It was observed by X-ray that the deficiency of iron ion in FeS occurs in this stage. This is interpreted as follows: iron ion reacts with oxygen by migrating from the interior of FeS crystal to the surface, without evolution of SO₂, until the deficiency of iron attains to a limiting value. Above 600°C the rate of oxidation does not change with temperature, so the rate-determining factor is diffusion of gas. Since the observed rate of oxidation depends upon the amount of the sample, the diffusion in the bed of the sample may determine the rate.     

Corrosion Resistance of APS- and HVOF-Sprayed Coatings in the Al2O3-TiO2 System

In this article, the results of corrosion investigations performed on thermally sprayed ceramic coatings with different compositions in the Al₂O₃-TiO₂ system (Al₂O₃, Al₂O₃-3%TiO₂, Al₂O₃-40%TiO₂, and TiO _x ) are presented. The coatings were deposited on corrosion-resistant steel substrates using atmospheric plasma spraying (APS) and high-velocity oxy-fuel (HVOF) spraying processes and characterized by means of optical microscopy, scanning electron microscopy (SEM), and x-ray diffraction (XRD). The corrosion properties were investigated in 1 N solutions of NaOH and H₂SO₄, at room temperature, 60 °C, and 85 °C, as well as in hydrothermal conditions with deionized water at 100 °C and 200 °C. The corrosion stability of the coatings depended on coating characteristics (spraying method, microstructure, and crystalline phase composition) and the corrosive environment (media, test temperature, and duration). In contrast to expectations, APS-sprayed coatings were found to be more corrosion-resistant than the HVOF-sprayed coatings. Addition of TiO₂ to Al₂O₃ increased the corrosion stability, especially for the HVOF-sprayed coatings. In this work, TiO _x coatings were found to be more corrosion-resistant than the Al₂O₃-based coatings.     

Effect of Nd2O3 Additive on Microstructure and Tribological Properties of Plasma-Sprayed NiCr-Cr2O3 Composite Coatings

Four types of NiCr-Cr₂O₃ composite coatings doped with different mass fraction of Nd₂O₃ were deposited by atmospheric plasma spraying. The microstructure and phase composition of as-sprayed coatings were analyzed by scanning electron microscope (SEM) and X-ray diffraction (XRD). Furthermore, their friction and wear behaviors at 20 and 600 °C under unlubricated condition were evaluated using CSM high temperature tribometer. The results showed that Nd₂O₃ could refine microstructure of NiCr-Cr₂O₃ composite coating and make Cr₂O₃ distribution more uniform in the coating, which leads to the increase of average microhardness. In addition, NiCr-Cr₂O₃ composite coatings doped with Nd₂O₃ had better wear resistance than that without Nd₂O₃ at experimental temperatures. Especially, the coating containing 8 wt.% Nd₂O₃ showed the best wear resistance at 20 and 600 °C, which was attributed to the refined microstructure and improved microhardness. At 20 °C, the wear mechanism of the coating was abrasive wear, brittle fracture and splat detachment. At 600 °C, the wear mechanism was adhesion wear and plastic deformation.     

Cyclic Oxidation Behavior of IN 718 Superalloy in Air at High Temperatures

Ni-base superalloy IN 718 was cyclically oxidized in laboratory air at temperatures ranging from 750 to 950 °C for up to 12 cycles (14 h/cycle). The kinetic behaviour as well as the surface morphology, and the oxide phases of the scales were characterized by means of weight gain measurements, cyclic oxidation kinetics, scanning electron microscopy equipped with energy dispersive spectroscopy (SEM-EDS), and X-ray diffraction (XRD) analysis techniques. The results showed that as the oxidation temperature increased, the oxidation rate, the external scale thickness, and internal oxidation zone increased. It was suggested that the oxidation rate was controlled by the diffusion of substrate elements in the alloy and the inward diffusion of oxygen through the oxide scale. The oxidation kinetics followed a sub-parabolic rate law and, the activation energy of oxidation was 249 ± 20 kJ mol^?1. The scaling process was controlled mainly by the diffusion of chromium, titanium, manganese, and oxygen ions through the chromia scale. IN 718 showed low weight gain and very slow reaction rates of substrate elements at 750 °C. At 850 °C, a continuous and very thin oxide scale was formed. At 950 °C, XRD and EDS-elemental mapping analysis revealed that a complex oxide scale had formed. It consisted of an outermost layer of TiO₂?CMnCr₂O₄ spinels, inner layer of Cr₂O₃, and the inner most layer composed of Ni₃Nb enriched with Nb, Ti and Al oxides underneath the chromia layer. The oxide scale at this temperature seemed to be thicker layer, significant spallation and volatilization had apparently occurred, and greater internal corrosion was identified. The doping effect of titanium was observed, where it was found to be diffused through the chromia scale to form TiO₂ at the oxide-gas interface as well as internally and at the oxide alloy interface. The amount of rutile (TiO₂) at the oxide surface increased with temperature. In view of Mn contents in the alloy, the manganese?Cchromium spinel oxide was inferred to have played an important role in cyclic oxidation behaviour of IN 718, where the change in oxidation kinetic was noted. The Al contents would cause internal Al-rich oxide formation at grain boundaries.     

The Influence of Temperature on Frictional Behavior of Plasma-Sprayed NiAl-Cr2O3 Based Self-Adaptive Nanocomposite Coatings

Frictional behavior of nano and hybrid-structured NiAl-Cr₂O₃-Ag-CNT-WS₂ adaptive self-lubricant coatings was evaluated at a range of temperatures, from room temperature to 700 °C. For this purpose, hybrid structured (HS) and nanostructured (NS) composite powders with the same nominal compositions were prepared by spray drying and heat treatment techniques. A series of HS and NS coating samples were deposited on steel substrate by an atmospheric plasma spraying process. The tribological behavior of both coatings was studied from room temperature to 700 °C at 100° intervals using a custom designed high temperature wear test machine. Scanning electron microscopy was employed for the evaluation of the composite coatings and worn surfaces. Experimental results indicated that the hybrid coating had inferior tribological properties when compared to the nanostructured coating, showing the attractive frictional behavior on the basis of low friction and high wear resistance; the NS coating possessed a more stable friction coefficient in the temperature range of 25-700 °C against alumina counterface. Microstructural examinations revealed more uniformity in NS plasma-sprayed coatings.     

Investigation of the surface properties of heat treated electroless Ni–P coating

Electroless nickel phosphorus (Ni–P) coatings were synthesised from an acid chloride electrolyte. The synthesised coatings were heat treated at different temperatures, and the surfaces of the heat treated coating were characterised using scanning electron microscopy and X-ray diffraction. Adhesion, wettability, hardness and corrosion behaviour of the coatings were measured. The surface morphology showed the formation of a nano crystalline nickel matrix under heat treated condition. X-ray diffraction analysis of the heat treated samples revealed the recrystallisation of nickel and formation of Ni₃P phase in the coatings. The wettabilty study showed that the as-deposited Ni–P coating is hydrophobic and wettability increases to a maximum of 70.8° contact angle for heat treated temperature of 400°C due to nano crystalline formation. The Rockwell C adhesion test revealed the presence of micro cracks with increase in heat treatment temperature, however the failure is within the acceptability limit. The micro hardness of the Ni–P coating increased with increase in heat treatment temperature. Corrosion potential of the Ni–P coating shifted to a positive potential under heat treated conditions owing to oxidation and precipitation of Ni₃P phase. Decreased corrosion rate and corrosion current density (7.37–0.21?µA?cm^?2) is attributed to heat treatment at 400°C.