Cubic Aluminum Nitride Coating Through Atmospheric Reactive Plasma Nitriding

Aluminum nitride is a promising material for structural and functional applications. Cubic AlN (c-AlN) is expected to have higher thermal conductivity due to their high symmetry; however, its fabrication is difficult. In this study, c-AlN was synthesized by atmospheric plasma spray process through the reaction between Al feedstock powder and nitrogen plasma. Al powders were supplied to the plasma stream by Ar carrier gas and reacted with surrounding N₂ plasma, then deposit onto substrate. The obtained coatings were c-AlN/Al mixture at 150 mm of spray distance, and the nitride content was improved by increasing the spray distance. The coatings almost consist of c-AlN at 300 mm of spray distance. The coatings thickness decreased from 100 to 10 μm with increasing spray distance from 150 to 300 mm. Using carrier gas, N₂ enable to fabricate thick c-AlN coating with hardness 1020 Hv.     

Splat Morphology and Influence of Feeding Rate During Reactive Plasma Spray of Aluminum Powder

Fabrication of aluminum nitride (AlN) coatings using conventional plasma spraying processes directly has been deemed impossible. It is attributed to the thermal decomposition of the AlN feedstock particles during spraying without a stable melting phase. Using the reactivity of the plasma (reactive plasma spraying: RPS) showed a promising consideration for in situ formation of AlN thermally sprayed coatings. Several AlN-based coatings were fabricated through the RPS of aluminum powders in the N₂/H₂ plasma. The focus of this study is in discussing the morphology of splat deposition during the nitriding of Al particles. Furthermore, the influence of the feeding rate during the RPS and nitriding of Al powders will be investigated. The nitride content, as well as the unreacted molten Al phase, strongly influences splat deposition and morphology during the RPS of Al. The collected splats can be divided into reacted, partially reacted, and unreacted splats. The reacted splats tend to show a disk or egg-shell shape. The partially reacted mainly had outside nitride shells and an unreacted molten Al part in the center. The unreacted splats tended to show a splash shape. The main controlling factor is the time of the droplet impact on the substrate during the reaction sequence. The particle size and spray distance showed significant effects on the splat formation due to their effect on the nitriding conversion and the melting behavior of the particles during RPS nitriding. The powder feeding rate was investigated through increasing the injection rate and by using a low carrier gas flow rate. Increasing the powder feeding rate significantly improved the coating thickness. However, it suppressed the nitriding conversion of the large Al particles. Thus, with increasing the amount of the powder in the plasma, the Al molten particles are easily aggregated and agglomerate together upon colliding on the substrate with an AlN shell on the surface. This prevents the N₂ from having access to all of the aggregated particles. Therefore, the fabricated coatings using large Al particles consist of surface AlN layers and the central parts of AlN and Al composite layers. On the other hand, it was possible to fabricate about 500-μm-thick AlN coatings using fine Al particles of 15 μm and increasing the feeding rate. Using the fine particles improved the nitriding reaction due to the improvement of the surface area (the reaction area). Moreover, the nitriding process of the Al particles with increasing the feeding rate was also investigated.     

Effect of Solid Shield on Coating Properties in Atmospheric Plasma Spray Process

This paper investigates the impact of shrouded shield structure on plasma spray processes and the selection of optimal shield structure. Response of plasma flame characteristics to solid shield structures is studied first, and experimental investigations are then performed for both atmospheric (APS) and shrouded (SPS) plasma spray processes. It is found that the usage of conical shield (divergence angle 5.5°) with 90 mm in length is effective to form a low-oxygen (<2%) and high-temperature (>3000 K) region in the plasma flame and this region can cover the majority area for particles passing by. The average particle temperature is higher in SPS than in APS with the given conditions, and such behavior is intensified as solid shield length increases. Using the SPS process, more disk-shaped splats are obtained, and the oxygen concentration in coating is significantly reduced. The degree of the oxidation in the coatings is further reduced as the length of the solid shield increases from 50 to 90 mm. Applying solid shield will lead to high flame temperature and low oxidation; however, the substrate overheating and velocity reduction may occur. For the cases studied, the optimal shield length is around 90 mm.     

Reactive Atmospheric Plasma Spraying of AlN Coatings: Influence of Aluminum Feedstock Particle Size

Feedstock powder characteristics (size distribution, morphology, shape, specific mass, and injection rate) are considered to be one of the key factors in controlling plasma-sprayed coatings microstructure and properties. The influence of feedstock powder characteristics to control the reaction and coatings microstructure in reactive plasma spraying process (RPS) is still unclear. This study, investigated the influence of feedstock particle size in RPS of aluminum nitride (AlN) coatings, through plasma nitriding of aluminum (Al) feedstock powders. It was possible to fabricate AlN-based coatings through plasma nitriding of all kinds of Al powders in atmospheric plasma spray (APS) process. The nitriding ratio was improved with decreasing the particle size of feedstock powder, due to improving the nitriding reaction during flight. However, decreasing the particle size of feedstock powder suppressed the coatings thickness. Due to the loss of the powder during the injection, the excessive vaporization of fine Al particles and the completing nitriding reaction of some fine Al particles during flight. The feedstock particle size directly affects on the nitriding, melting, flowability, and the vaporization behaviors of Al powders during spraying. It concluded that using smaller particle size powders is useful for improving the nitriding ratio and not suitable for fabrication thick AlN coatings in reactive plasma spray process. To fabricate thick AlN coatings through RPS, enhancing the nitriding reaction of Al powders with large particle size during spraying is required.     

Influence of Ceramic Powder Size on Process of Cermet Coating Formation by Cold Spray

Influence of the ceramic particle size on the process of formation of cermet coatings by cold spray is experimentally studied. A specially developed nozzle with separate injection of ceramic and metal powders into the gas stream is used in the experiments. The results obtained demonstrate that fine ceramic powders (Al₂O₃, SiC) produce a strong activation effect on the process of spraying soft metal (Al, Cu) and increase deposition efficiency of the metal component of the mixture compared to the pure metal spraying. At the same time, coarse ceramic powder produces a strong erosion effect that considerably reduces coating mass growth and deposition efficiency of the metal component. It is experimentally shown that the addition of fine hard powder to soft metals as Al and Cu allows to significantly reduce the “critical” temperature (the minimum gas stagnation temperature at which a nonzero particle deposition is observed) for spraying these metals.     

INITIAL ATMOSPHERIC CORROSION OF ZINC IN THE PRESENCE OF NH4C1

Influence of NH4Cl on the initial atmospheric corrosion of zinc was investigated via quartz crystal microbalance (QCM) in laboratory at 80%RH and 25℃. The results show that NH4Cl can accelerate the initial corrosion of zinc. Mass gain increase with the exposure time, but mass gain in the later doesn't change obviously due to the formation of the insoluble simonkolleite on zinc surface in the presence of NH4Cl. Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) was used to characterize the corrosion products. Zn5Cl2(OH)8·H2O, (NH4)2ZnCl4 and ZnO are the corrosion products on zinc. Brief discussion on the mechanisms of atmospheric corrosion of zinc in the presence of NH4Cl was introduced.     

粗糙铝片表面NH_4Cl晶体形核特性研究

制备了润湿特性不同的纯铝表面,并考察了以其作为基底激冷触发30%NH4Cl(质量分数)水溶液中的NH4Cl晶粒形核过程。结果表明:随在空气中暴露时间的延长,具有微纳米层级结构的纯铝表面的润湿性会由强润湿转变为不可润湿,NH4Cl晶粒在强润湿表面的形核点密度明显高于不可润湿表面。分析认为:强润湿性表面产生的毛细作用易于使溶液渗入表面结构中,因而表面凹陷能够有效地促进形核;而不可润湿表面易于存留气体,这会减少利于形核的凹陷结构,同时凹陷结构中气泡的存在使得形核功增大,导致形核困难。     

超声波作用对NH_4Cl枝晶形态影响的研究

研究了超声波功率和处理时间对饱和NH4Cl溶液结晶温度、晶粒度和二次枝晶的影响。实验中发现,在相同的结晶条件下,随着超声处理时间的延长,晶粒细化效应增强,结晶二次晶间距不断增大。同时,随着超声波功率的增加,对晶粒细化、二次晶间距的增大以及对二次晶根部的影响效应增强,但存在峰值。     

Optimization of Atmospheric Plasma Spray Process Parameters using a Design of Experiment for Alloy 625 coatings

Alloy 625 is a Ni-based superalloy which is often a good solution to surface engineering problems involving high temperature corrosion, wear, and thermal degradation. Coatings of alloy 625 can be efficiently deposited by thermal spray methods such as Air Plasma Spraying. As in all thermal spray processes, the final properties of the coatings are determined by the spraying parameters. In the present study, a D-optimal experimental design was used to characterize the effects of the APS process parameters on in-flight particle temperature and velocity, and on the oxide content and porosity in the coatings. These results were used to create an empirical model to predict the optimum deposition conditions. A second set of coatings was then deposited to test the model predictions. The optimum spraying conditions produced a coating with less than 4% oxide and less than 2.5% porosity. The process parameters which exhibited the most important effects directly on the oxide content in the coating were particle size, spray distance, and Ar flow rate. The parameters with the largest effects directly on porosity were spray distance, particle size, and current. The particle size, current, and Ar flow rate have an influence on particle velocity and temperature but spray distance did not have a significant effect on either of those characteristics. Thus, knowledge of the in-flight particle characteristics alone was not sufficient to control the final microstructure. The oxidation index and the melting index incorporate all the parameters that were found to be significant in the statistical analyses and correlate well with the measured oxide content and porosity in the coatings.

送粉等离子束表面冶金工艺及涂层强韧化机制研究

利用自行研发的送粉等离子束表面冶金涂层设备及Fe-Cr-Ni-B-Si-C系混合合金粉末在普通低碳钢表面制备了铁基复合材料涂层.采用OM、SEM、EDS、XRD等手段,研究了同步送粉等离子束表面冶金工艺参数对涂层显微组织的影响及涂层的强韧化机制.结果表明,工作电流、扫描速度以及搭接工艺是影响涂层微观组织特征的重要因素.经工艺优化后的复合材料涂层的典型微观组织由固溶了大量Cr、少量Ni、Si的极度过饱和的γ相枝晶及枝晶间复杂合金碳硼化物 γ相共晶组织构成.细晶强化、固溶强化和高硬度相的沉淀析出及其弥散强化是等离子束表面冶金复合材料涂层强韧化的3种主要机制.     

Improvement of Coating Properties in Three-Cathode Atmospheric Plasma Spraying

The main aim of this study is to improve the coating properties of three-cathode atmospheric plasma-sprayed coatings with respect to porosity and residual stresses. This was done by means of numerical simulation coupled with advanced diagnostic methods. A numerical model for the triple injection of alumina feedstock, as well as acceleration and heating of the powder particles in the characteristic threefold symmetrical plasma jet cross section produced by a three-cathode-plasma torch, was developed. The modeling results for the standard injector’s position “0” were calculated and experimentally verified by laser Doppler anemometry. Based on the criteria defined for the concentrated feedstock transport and homogeneous thermal treatment of powder particles in the plasma jet, the optimal injection position was found. In the next step, a previously developed, coupled CFD-FEM-simulation model was used for simulations of the coating build-up, describing flattening, solidification, and deformation due to shrinkage for alumina particles on a rough substrate surface.     

Challenges Upon Reactive Plasma Spray Nitriding: Al Powders and Fabrication of AlN Coatings as a Case Study

Reactive plasma spraying (RPS) is a promising technology for the in situ formation of several ceramic coatings. The focus of this paper is to summarize the state of our current knowledge about the RPS process and using the nitriding of Al particles and the fabrication of aluminum nitride coatings, as a case study. The aspects and challenges in this process such as the influence of the plasma power, in-flight time, particle size, nitriding mechanism, splat morphology, in-flight particle diagnostics, N₂ plasma gas, and the feeding rate on the RPS process are analyzed and discussed.     

ZrO2纳米粉等离子喷涂工艺及磨损性能研究

应用spraywatch热喷涂在线监测系统测定了ZrO2纳米粉等离子喷涂工艺参数与喷涂粒子温度和速度的关系；测定了涂层耐磨性，分析了涂层表面形貌、界面结合状况和物相组成；获得了涂层制备的较佳喷涂工艺参数。涂层为纳米结构，主要由四方相构成。     

Phase Formation and Transformation in Alumina/YSZ Nanocomposite Coating Deposited by Suspension Plasma Spray Process

Suspension Plasma Spray process was used for deposition of pseudo-eutectic composition of alumina-yttria-stabilized zirconia as a potential thermal barrier coating using Mettech axial III torch. Process variables including feed and plasma parameters were altered to find their effects on the formation of phases in the composite coating. The in-flight particle velocity was found to be the crucial parameter on phase formation in the resulting coatings. Low particle velocities below 650 m/s result in the formation of stable phases i.e., α-alumina and tetragonal zirconia. In contrast, high particle velocities more than 750 m/s favor the metastable γ-alumina and cubic zirconia phases as dominant structures in as-deposited coatings. Accordingly, the plasma auxiliary gas and plasma power as influential parameters on the particle velocity were found to be reliable tools in controlling the resulting coating structure thus, the consequent properties. The noncrystalline portion of the coatings was also studied. It was revealed that upon heating, the amorphous phase prefers to crystallize into pre-existing crystalline phases in the as-deposited coating. Thus, the ultimate crystalline structure can be designed using the parameters that control the particle velocity during plasma spray coating.     

反应等离子喷涂TiN/AlN涂层在润滑状态下摩擦磨损性能的研究

对用反应等离子喷涂法制备的TiN／AlN涂层在油润滑条件下的摩擦磨损特征进行了研究，并就轻、重载荷下的磨损机理进行了探讨。结果表明：油润滑条件下，涂层磨损体积显著降低。在轻载荷下，以疲劳磨损为主；在重载荷下，以脆性剥落和磨粒磨损为主。     

反应等离子喷涂TiN/AlN涂层在润滑状态下摩擦磨损性能的研究

对用反应等离子喷涂法制备的TiN/AlN涂层在油润滑条件下的摩擦磨损特征进行了研究,并就轻、重载荷下的磨损机理进行了探讨。结果表明:油润滑条件下,涂层磨损体积显著降低。在轻载荷下,以疲劳磨损为主;在重载荷下,以脆性剥落和磨粒磨损为主。     

Influence of the Spray Angle on the Characteristics of Atmospheric Plasma Sprayed Hard Material Based Coatings

This paper presents an investigation of the influence of the spray angle on thermally sprayed coatings. Spray beads were manufactured with different spray angles between 90 and 20° by means of atmospheric plasma spraying (APS) on heat-treated mild steel (1.0503). WC-12Co and Cr₃C₂-10(Ni20Cr) powders were employed as feedstock materials. Every spray bead was characterized by a Gaussian fit. This opens the opportunity to analyze the influence of the spray angle on coating properties. Furthermore, metallographic studies of the surface roughness, porosity, hardness, and morphology were carried out and the deposition efficiency as well as the tensile strength was measured. The thermally sprayed coatings show a clear dependence on the spray angle. A decrease in spray angle changes the thickness, width, and form of the spray beads. The coatings become rougher and their quality decreases.     

Influence of Powder Injection Parameters in High-Pressure Cold Spray

High-pressure cold spray systems are becoming widely accepted for use in the structural repair of surface defects of expensive machinery parts used in industrial and military equipment. The deposition quality of cold spray repairs is typically validated using coupon testing and through destructive analysis of mock-ups or first articles for a defined set of parameters. In order to provide a reliable repair, it is important to not only maintain the same processing parameters, but also to have optimum fixed parameters, such as the particle injection location. This study is intended to provide insight into the sensitivity of the way that the powder is injected upstream of supersonic nozzles in high-pressure cold spray systems and the effects of variations in injection parameters on the nature of the powder particle kinetics. Experimentally validated three-dimensional computational fluid dynamics (3D CFD) models are implemented to study the particle impact conditions for varying powder feeder tube size, powder feeder tube axial misalignment, and radial powder feeder injection location on the particle velocity and the deposition shape of aluminum alloy 6061. Outputs of the models are statistically analyzed to explore the shape of the spray plume distribution and resulting coating buildup.     

等离子喷涂工艺参数对Cr_2O_3涂层组织和磨损性能的影响

通过改变PLC控制的等离子喷涂工艺参数,研究了喷涂电流、电压、氩气流量和喷涂距离对Cr2O3涂层磨损性能和显微组织的影响。结果表明,Cr2O3粉末喷涂的最佳电流、氩气流量、电压和喷涂距离分别为450 A、45 L/min、60 V和90 mm。纳米级Cr2O3涂层形成了片状组织和纳米颗粒的混合结构,有利于涂层耐磨性和韧性的提高。