Microstructural characterization of radio frequency and direct current plasma-sprayed Al2O3 coatings

Microstructures of radio frequency (RF) and direct current (DC) plasma-sprayed Al₂O₃ coatings deposited onto steel substrates were characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), electron microprobe analysis (EMPA), polarizing optical microscopy (OM), and transmission electron microscopy (TEM). Because RF and DC plasmas produce different particle heating and acceleration, the morphology, phase structure, and fracture modes of the coatings vary substantially. In the case of RF coatings, a clear lamellar microstructure with relatively thick lamellae was observed, which is due to the large particles and the low particle velocities, with α-Al₂O₃ as the predominant phase and with delamination type of fracture detected on the fracture surface. In contrast, the DC coatings consisted of predominantly metastable γ-Al₂O₃ as well as amorphous phases, with a mixed fracture mode of the coating observed. In spite of limited interfacial interdiffusion detected by EMPA, TEM showed an interfacial layer existing at the interface between the coating and the substrate for both cases. For RF coatings, the interfacial layer on the order of 1 μm was composed of three sublayers, each of which was different in composition and morphology. However, the interfacial layer for the DC coating consisted primarily of an amorphous phase, containing both coating and substrate materials with or without platelike microcrystals; although in some regions a thick amorphous Al₂O₃ layer was in direct contact with the substrate.     

Influence of hydrogen on the microstructure of plasma-sprayed yttria-stabilized zirconia coatings

The influence of secondary hydrogen and current on the deposition efficiency (DE) and microstructure of yttria-stabilized zirconia (YSZ) coatings was evaluated. To better understand the influence of the spray process on coating consistency, a YSZ powder, −125 +44 μm, was sprayed with nitrogen/hydrogen parameters and a 9 MB plasma gun from Sulzer Metco. DE and coating porosity, which were produced using two different spray gun conditions yielding the same input power, were compared. Amperage was allowed to vary between 500 and 560 A, and hydrogen was adjusted to maintain constant power, while nitrogen flow was kept at a fixed level. Several power conditions, ranging from 32 to 39 kW, were tested. Different injection geometries (i.e., radial with and without a backward component) were also compared. The latter was found to produce higher in-flight temperatures due to a longer residence time of the powder particles in the hotter portion of the plasma. Porosity was based on cross-sectional micrographs. In-flight particle temperature and velocity measurements were also carried out with a special sensor for each condition. Test results showed that DE and coating density could vary significantly when a different hydrogen flow rate was used to maintain constant input power. On the other hand, DE was found to correlate very well with the temperature of the in-flight particles. Therefore, to obtain more consistent and reproducible DE and microstructures, it is preferable to maintain the in-flight particle temperature around a constant value instead of keeping a constant input power by adjusting the secondary hydrogen flow rate.     

The electrical insulation behavior and sealing effects of plasma-sprayed alumina–titania coatings

Two commercial sealants based on polymers were studied and the electrical insulation properties of ceramic coatings were tested, before and after the impregnation treatment, using a plasma-sprayed Al₂O₃–13% TiO₂ coating as the reference coating. The second part of this paper reports on the effects of curing temperature and exposure time of the sealants on the penetration depth of the ceramic coating. The preliminary test results with a DC puncture tester imply that the dielectric breakdown voltage mechanism of plasma-sprayed ceramic coatings has been determined to be a corona mechanism. Dielectric breakdown voltage of the as-sprayed and as-ground samples have shown a linear trend with regard to the thickness, showing an average dielectric strength of 20 kV/mm for the thickness scale studied. The penetration depth of sealants to the ceramic coating can be clearly recognized with addition of fluorescent dye (EpoDye). It is also shown that grinding the coating before sealing and adding fluorescent dye (EpoDye) does not affect the penetration depth of sealants. For epoxy-based sealant, the effects of temperature on the penetration depth of the sealant show that an optimum temperature can be determined. The balance between the beneficial and the detrimental effects is obtained at approximately 100°C. Moreover, the effect of curing time on the penetration depth is beneficial. However, for urethane-based sealant, it seems that the impregnation process may be complex because of the high pressures of entrapped gases occurring during the process. Although the penetration of sealant to the ceramic coating has reached over 300 μm, the effects of curing time and temperature have not been clearly established.     

Transmission electron microscopy observation of microstructure of plasma-sprayed nanostructured zirconia coating

Nanostructured zirconia coatings deposited by plasma spraying technique were observed using transmission electron microscopy (TEM). It was found that the as-sprayed nanostructured zirconia coating had bimodal microstructures in terms of grain size distribution in the direction parallel to substrate surface. One was in the range 30–120 nm, which was the dominative structure of the coating, and the other was about 150–400 nm. The cross-section micrograph of the plasma sprayed nanostructured zirconia coating revealed that the coating still exhibited lamellar structure with columnar grains extending through its thickness. In conjunction with partially molten zirconia grains, amorphous regions were found. Domain structure and superlattice structure were observed in the plasma-sprayed nanostructured zirconia coating. The formations of the domain and superlattice structures are discussed in this paper.     

Comparison of plasma-sprayed alumina coatings by RF and DC plasma spraying

Splat size and shape- factor distributions for plasma- sprayed alumina particles on various substrates were studied using a setup derived from the line- scan test. Direct- current (dc) and radiofrequency (rf) plasma torches were used to study the influence of particle velocity at impact. The influence of substrate temperature prior to spraying also was studied. Splats collected on smooth substrates kept below 100 °C were extensively fingered and had poor substrate contact. When the substrates were heated to 300 °C before spraying, the splats became disk- shaped and their substrate contact was very good. Similar results were obtained for rough substrates. Coating adhesion decreased with particle velocity and was lower for the dc plasma torch when using larger particles, which did not melt as well as smaller ones. Melting and adhesion were much improved with the rf torch.     

Cross-sectional analysis on microstructure of plasma-sprayed HA＋TiO2 composite coatings on titanium substrate

The cross-sectional analysis on hydroxyapatite (HA) coating and HA TiO2 composite coating was conducted by using electron probe microanalyser (EPMA). The results reveal that annealing at 650℃ leads to the cracking within the HA coating or along the coating/substrate interface. The ribbon-like regions in HA coating are verified to contain less PO4^4- groups resulted from the high temperature melting of HA particles in plasma flame. From the viewpoint of microstructural observation, it can be concluded that the addition of TiO2 into HA coating can effectively strengthen and toughen the whole coating system with a shift of the well-bonded interface from the THA (top HA) coating/HTBC (HA TiO2 bond coat) interface in the as-sprayed THBC (top HA-HTBC) coating to the HTBC/Ti substrate interface in the heat treated THBC coating. The THA coating bonds well to Ti substrate per-haps via its TiO2 hobnobbing with the Ti oxides formed on the Ti substrate.     

Effect of annealing treatment on the microstructure and properties of cold-sprayed Cu coating

Copper (Cu) coating was deposited by cold spraying, and the electrical resistivity of the coating in both directions parallel and perpendicular to the coating surface was measured to investigate the anisotropy of the coating. Annealing treatment was applied to the coating to examine its effect on the microstructure and properties of the cold-sprayed Cu coating. The examination of coating microstructure evidently revealed that the coating was constituted by the flattened particles, and the interfaces were clearly observed between the deposited particles. The anisotropy in microstructure and electrical resistivity was present in cold-sprayed Cu coating. The electrical resistivity of the as-sprayed coating was higher than that of Cu bulk. Moreover, the electrical resistivity along the direction parallel to the coating surface was lower than that along the perpendicular direction. It was found that annealing treatment led to the enhancement of particle interface bonding and evident recry stallization of the elongated grains and remarkable grain growth as well. The annealed coating presented equiaxed grain structures similar to the annealed Cu bulk with particle interfaces almost disappearing under certain annealing conditions. The coalescence of voids or pores in the coating was clearly observed at high annealing temperatures. Moreover, the annealed coating yielded an electrical resistivity and microhardness comparable to Cu bulk. The original version of this paper was published in the CD ROM Thermal Spray Connects: Explore Its Surfacing Potential, International Thermal Spray Conference, sponsored by DVS, ASM International, and HW International Institute of Welding, Basel, Switzerland, May 2–4, 2005, DVS-Verlag GmbH, Düsseldorf, Germany.     

Al_2O_3含量对Al_2O_3-Al复合涂层组织和摩擦磨损性能的影响

通过改变喷涂粉末中Al2O3和Al的比例,在AZ91D镁合金表面制备不同Al2O3含量的等离子喷涂Al2O3-Al复合涂层。对复合涂层的显微组织、硬度和摩擦磨损性能进行表征,研究Al2O3含量对涂层组织和磨损性能的影响。结果表明,涂层组织为带状Al2O3分布在致密的Al基体上,Al2O3内可见细微的片层结构,且层与层间存在一定的孔隙。复合涂层中Al平均硬度62HV,Al2O3平均硬度达1380 HV。摩擦磨损实验证实,复合涂层具有较小的摩擦系数和较低磨损量,大大改善了镁合金表面的抗磨损性能。涂层中Al2O3体积少于Al时,Al2O3增加使涂层的抗磨效果增强。涂层中Al2O3体积超过Al后,涂层的孔隙增多、涂层变脆,其耐磨损性能下降。     

Deposition and properties of high-velocity-oxygen-fuel and plasma-sprayed Mo-Mo2C composite coatings

Molybdenum thermal-spray coatings, dispersion strengthened by molybdenum oxides and molybdenum carbides, play an important role in industrial tribological applications. Traditionally, they have been prepared by plasma and wire flame spraying. High porosity and lower cohesion strength limit their application in situations where both galling and abrasion wear is involved. In this study, high-velocity-oxygen-fuel (HVOF) deposition of molybdenum and molybdenum carbide coatings was attempted. Deposition was achieved for all powders used. Composition, microstructure, mechanical, and wear properties of the HVOF synthesized coatings were evaluated and compared with plasma-sprayed counterparts. The HVOF coatings possessed a very good abrasion resistance, whereas plasma deposits performed better in dry sliding tests. Measurements showed a close relationship between the coating surface hardness and its abrasion resistance. Results also suggested correlation between molybdenum carbide distribution in the molybdenum matrix and the sliding friction response of Mo-Mo₂C coatings.     

电弧喷涂4Cr13涂层的组织与性能研究

研究了喷砂粗化、喷涂打底涂层、电拉毛三种表面预处理工艺下电弧喷涂4Cr13涂层的组织与性能.利用扫描电镜、能谱仪等手段对涂层组织和断口形貌进行分析,同时对涂层的显微硬度和结合强度进行了测试.结果表明:电弧喷涂4Cr13涂层组织呈现出典型的层状结构.不同的表面预处理工艺对涂层的结合强度影响显著,喷砂粗化并喷涂打底涂层能使...     

Development and microstructure optimization of atmospheric plasma-sprayed NiO/YSZ anode coatings for SOFCs

In this paper, preparation and characterization of porous anode layers with uniform phase distribution are discussed for solid oxide fuel cell (SOFC) application. The Ni/8YSZ cermet coatings were fabricated by atmospheric plasma spray (APS) process using oxidized nickel coated graphite (Ni-graphite) and 8 mol% yittria — stabilized zirconia (8YSZ) blend as feedstock. To control the microstructure of the coating, the nickel coated graphite with low density was used as a starting feedstock instead of conventional pure nickel (Ni) powder. To balance the conductivity, uniform porosity, and structural stability of the coatings, the effects of process parameters such as hydrogen gas flow rate, stand off distance and pore formation precursor (graphite) addition on the microstructures of the resulting coatings are investigated. The results show that the anode coatings with high conductivity, structural stability and porosity could be deposited with moderate hydrogen gas flow rate and short stand off distance.     

退火温度对磁控溅射Mo薄膜结构和性能的影响

采用磁控溅射技术在石英基体上制备了厚度为600 nm的Mo薄膜,并在不同温度下(400～ 900℃)对其进行退火处理.通过XRD、SEM、四探针测试仪对Mo薄膜的结构和性能进行了分析.结果表明,随着退火温度的升高,(110)晶面择优取向特性增强.Mo薄膜在退火温度为800℃时电阻率达到最小值3.56×10-5 Ω·cm,在900℃退火时薄膜出现宽度约为50 nm的微裂纹且薄膜电阻率较大.     

The deformation and cooling of ceramic particles sprayed with a thermal radio-frequency plasma under atmospheric conditions

Common thermal-spray techniques use the strong acceleration of powder particles to produce dense ceramic coatings with high bond strength. The residence time of the powder particles within the plasma jet is correspondingly low, and only relatively small particles can be molten. In this work, on the contrary, an inductively coupled radio-frequency (RF) inductively coupled plasma (ICP) torch was used to spray large oxide-ceramic powder particles under atmospheric conditions. The slow plasma flow of a RF plasma leads to large residence times of the powder particles, so that the powder size of the feedstock can be 100 μm and more. It was observed that these particles will not be strongly accelerated in the plasma and that their velocity at the moment of impact is in the range of 10 to 20 m/s. Ceramic coatings were ICP sprayed with a low porosity and a high bond strength, similar to direct current (DC) or high-velocity-oxygen-fuel (HVOF) sprayed coatings. The morphology of ICP-sprayed particles on smooth steel surfaces, as a function of the surface temperature, is described and compared with DC plasma-sprayed splats. Furthermore, the degree of deformation was measured and determined by different models, and the pronounced contact zones formed between the pancake and the substrate were investigated. The ICP-sprayed ceramic coatings show some special properties, such as the absence of metastable crystalline phases, which are common in other spray technologies.     

烧结工艺对ZnO压敏陶瓷微观结构与电学性能影响

以ZnO粉末为主要原料,添加TiO2、Bi2O3、MnO2、Co2O3、Sb2O3为组元,在不同烧结温度(1100~1250℃)与保温时间(1.0~2.5h)下制备ZnO压敏陶瓷。采用SEM观察陶瓷形貌,利用压敏电阻直流参数仪测试陶瓷的电学性能,研究烧结温度与保温时间对陶瓷结构和性能的影响。结果表明,随烧结温度升高,压敏电压、漏电流逐渐降低,而非线性系数先减小后增加。制备ZnO压敏陶瓷的适宜烧结温度与保温时间分别为1250℃、1h,压敏电压为17.0V/mm、漏电流为0.014mA、非线性系数为14.2,陶瓷内部晶粒可长大至128.7μm。     

The relationship between the microstructure and thermal diffusivity of plasma-sprayed tungsten coatings

Tungsten and tungsten alloy coatings are candidate materials for plasma facing components of divertor plates in future fusion reactors. In normal operation, the sprayed coatings will be submitted to intense heat fluxes and particle bombardment. This work investigated the relationship between the microstructure of plasma-sprayed tungsten coatings and their thermal diffusivity as determined by the laser flash method. The microstructural investigation was carried out on copper-infiltrated coatings. Such a preparation technique permitted the measurement of the total true contact area between the lamellae within the tungsten coatings. The spraying atmosphere was found to strongly influence the interfacial contact between lamellae and coating thermal diffusivity.     

Effects of deposition parameters on microstructure and thermal conductivity of diamond films deposited by DC arc plasma jet chemical vapor deposition

The uniform diamond films with 60 mm in diameter were deposited by improved DC arc plasma jet chemical vapor deposition technique. The structure of the film was characterized by scanning electronic microcopy(SEM) and laser Raman spectrometry. The thermal conductivity was measured by a photo thermal deflection technique. The effects of main deposition parameters on microstructure and thermal conductivity of the films were investigated. The results show that high thermal conductivity, 10.0 W/(K-cm), can be obtained at a CH4 concentration of 1.5% (volume fraction) and the substrate temperatures of 880-920 ℃ due to the high density and high purity of the film. A low pressure difference between nozzle and vacuum chamber is also beneficial to the high thermal conductivity.     

爆炸喷涂Al-Cu-Cr准晶涂层的组织及硬度研究

为了研究热喷涂工艺对爆炸喷涂Al-Cu-Cr准晶涂层组织和硬度的影响规律，采用三种爆炸喷涂工艺参数在Q235A低碳钢基体上制备涂层，借助XRD、SEM和OM等技术手段对粉末和涂层的组织结构进行分析，并检测涂层横截面的孔隙率和显微硬度。结果表明，用于喷涂的A165Cu20Cr15准晶粉末中含有二十面体准晶相i-A165Cu24Cr11和极少量具有单斜结构的晶体相θ-Al13Cr2（即Al83Cu4Cr13）；而爆炸喷涂涂层中除i和θ两相外，生成了新相——体心立方结构的α-Al69Cu18Cr13（准晶i的晶体类似相）和Al2O3相。涂层呈典型层状结构，其它条件不变的情况下，涂层中各晶体相与准晶相i最强峰衍射强度的比值α／i、θ/i和Al2O3／i随爆炸喷涂工作气体流速的成比例提高而增加，同时涂层截面的孔隙率下降而显微硬度HV0.1升高。     

Suspension DC plasma spraying of thick finely-structured ceramic coatings: Process manufacturing mechanisms

Due to the large volume fraction of the internal interfaces and reduced size of stacking defects, thick (from 20 to 100 µm) nano- or sub-micron structured coatings exhibit better properties than conventional micron structured ones (e.g. higher coefficients of thermal expansion, lower thermal diffusivity, higher hardness and toughness, better wear resistance, among other coating characteristics and functional properties). They could hence offer pertinent solutions to numerous emerging applications, in particular for energy production, energy saving, diffusion and environmental barriers, etc.Suspension plasma spraying (SPS) permits to manufacture such finely-structured layers and consists in mechanically injecting within the plasma flow a liquid suspension of sub-micrometric-sized or nano-sized particles through an injector of diameter of the order of one hundred micrometers. Upon penetration within the DC plasma jet, two phenomena occur sequentially: droplet fragmentation and then solvent evaporation. Particles are then processed by the plasma flow (heat and momentum transfers) prior to their impact, flattening and solidification upon the surface to be covered.Compared to plasma spraying of micrometer-sized particles (APS), SPS exhibit several major differences : i) a more pronounced sensitivity to electric are root fluctuation requiring to operate the spray gun in a relatively stable mode (take over) unless to process inhomogeneously the suspension which would results in heterogeneous coating structure; ii) a shorter spray distance (since small particles decelerate faster than bigger ones) leading to higher thermal flux transmitted from the plasma flow to the substrate (5 to 10 times higher than conventional plasma spraying); iii) an emphasized thermophoresis effect; iv) a typical cohesive structure made of the stacking of granular and flattened particles with low density of stacking defects.This paper aims at presenting recent developments carried-out on this process in terms of process optimization and coating manufacturing mechanisms.     

Simultaneous independent measurement of splat diameter and cooling time during impact on a substrate of plasma-sprayed molybdenum particles

In thermal spray processes, the coating structure is the result of flattening and cooling of molten droplets on the substrate. The study of the cooling time and evolution of the splat size during impact is then of the highest importance to understand the influence of the spray parameters and substrate characteristics on the coating structure. Measurement of particle temperature during impact requires the use of a high-speed two-color pyrometer to collect the thermal emission of the particle during flattening. Simultaneous measurement of the splat size with this pyrometer is difficult since the size of the particle can change as it cools down. To measure the splat size independently, a new measurement technique has been developed. In this technique, the splat size is measured from the attenuation of the radiation of a laser beam illuminating the particle during impact. Results are presented for plasma-sprayed molybdenum particles impacting on a glass substrate at room temperature. It is shown that the molybdenum splat reaches its maximum extent about 2 μs after the impact. In this work, we show that this increase of the splat surface is followed by a phase during which the splat size decreases significantly during 2 to 3 μs.     

Effects of silver powder particle size on the microstructure and properties of Ag-Yb<Subscript>2</Subscript>O<Subscript>3</Subscript> electrical contact materials prepared by spark plasma sintering

Ag-Yb₂O₃ electrical contact materials were fabricated by spark plasma sintering (SPS). The effects of silver powder particle size on the microstructure and properties of the samples were investigated. The surface morphologies of the sintered samples were examined by optical microscope (OM), and the fracture morphologies were observed by scanning electron microscopy (SEM). The physical and mechanical properties such as density, electrical resistivity, microhardness, and tensile strength were also tested. The results show that the silver powder particle size has evident effects on the sintered materials. Comparing with coarse silver powder (5 μm), homogeneous and fine microstructure was obtained by fine silver powder (≤0.5 μm). At the same time, the electrical conductivity, microhardness, and tensile strength of the sintered samples with fine silver powder were higher than those of the samples with coarse silver powder. However, silver powder particle size has little influence on the relative densities, which of all samples (both by fine and coarse silver powders) is more than 95%. The fracture characteristics are ductile.