直流、射频磁控溅射制备钌薄膜的微观结构及电学性能分析

为了探索直流和射频磁控溅射制备钌薄膜的微观结构及性能差异,进而指导薄膜制备工艺优化。采用直流和射频磁控溅射法在SiO2/Si(100)衬底上沉积不同时间和温度的钌薄膜;通过高分辨场发射扫描电镜、X射线衍射仪、原子力显微镜、四探针等方法研究不同溅射电源下制备的钌薄膜的微观结构和电学性能。结果表明,在相同溅射条件下,DC-Ru薄膜的结晶性优于RF-Ru薄膜;其厚度大于RF-Ru薄膜,满足tDC≈2tRF;其沉积速率高于RF-Ru薄膜,满足vDC≈2vRF。然而,其电阻率却高于RF-Ru薄膜,这主要得益于RF-Ru薄膜的致密度较高,从而降低了电子对缺陷的散射效应。     

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.     

Microstructures and erosion resistance of plasma-sprayed WCp/NiCrBSi composite coatings

WCp/NiCrBSi composite coatings have been deposited by plasma spraying with the mixed powders of WC-12Ni and NiCrBSi. The coatings consist mainly of WC, γ-Ni, Ni3B, CrB, Cr2B, M7C3, M23C6 and W2C phases. The W2C content increases with increasing WC mass fraction in the powders. The porosity and microhardness of the coatings are related to the coating WC content. The excessive WC results in decreasing the microhardncss due to increasing the porosity. The WCp/ NiCrBSi coating with 35 % WC mass fraction powder has more excellent erosion resistance. With an increase of impact angles from 15°to 90°the erosion rate of the coating increases, the erosion rate at 15°impact angle being approximately two times lower than that at 90°impact angle. Based on the wear morphology of the coatings at different impact angles, the wear mechanisms were discussed.     

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.     

Y2O3掺杂ZrSiO4涂层的微观组织和相结构研究

本文采用大气等离子喷涂成功制备了ZrSiO4及Y2O3掺杂ZrSiO4涂层,研究了Y2O3掺杂后ZrSiO4涂层微观组织结构、力学性能,并研究了涂层在1300 ℃下的烧结行为。结果表明,等离子喷涂ZrSiO4涂层主要由ZrSiO4、t-ZrO2、少量的m-ZrO2及无定型SiO2组成,而等离子喷涂ZrSiO4-5%Y2O3涂层主要由c-ZrO2、少量ZrSiO4相及无定型SiO2组成。相较于ZrSiO4涂层,Y2O3掺杂略微提高了ZrSiO4-5%Y2O3涂层的硬度和断裂韧性。在1300 ℃高温烧结48 h后等离子喷涂ZrSiO4涂层中(t,m)-ZrO2和无定型SiO2反应生成重新ZrSiO4相,该反应伴随着体积收缩,使得涂层中存在着大量孔隙和裂纹。相较于纯ZrSiO4涂层, ZrSiO4-5%Y2O3涂层中主要是c-ZrO2相和ZrSiO4相,添加Y2O3有助于涂层中的ZrO2保持在立方相（c-ZrO2）,提高了ZrO2的高温相稳定性。     

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.     

等离子喷涂和激光熔覆热障涂层隔热性能比较

采用多种方法制备不同类型的Al2O3-13％TiO2热障涂层,即等离子喷涂常规涂层、纳米结构涂层及激光熔覆纳米结构涂层．在分析三类涂层微观组织的基础上,对其隔热性能进行了比较．结果表明,即等离子喷涂常规陶瓷涂层呈典型的层状堆积特征,纳米结构涂层都为特殊的两相结构,其中部分熔化区由类似的残留纳米粒子组成,等离子喷涂纳米结构涂层的完全熔化区为片层状结构,而相应的激光熔覆涂层的完全熔化区则为细小等轴晶．在相同条件下,等离子喷涂纳米结构热障涂层具有最好的隔热性能,而激光熔覆纳米结构涂层的隔热性能要好于等离子喷涂常规涂层．     

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.     

横纵磁场下铁基合金堆焊层组织性能的对比分析

将Fe5自熔合金采用等离子弧堆焊设备堆焊到低碳钢表面,在堆焊的过程中施加直流横向和直流纵向磁场,并调节磁场参数和堆焊工艺参数,对不同参数下堆焊试样进行硬度和磨损试验,采用显微电镜和扫描电镜对堆焊层显微组织进行分析,研究两种磁场状态下堆焊层组织、性能的差异性,并对其中的机理进行探究.结果表明,直流横向磁场和直流纵向磁场均可提高硬质相的形核率,改善堆焊层的组织性能;横向磁场作用下堆焊层中硬质相杂乱分析,而纵向磁场使堆焊层中的硬质相以规则的"六边形"出现,这使得横向磁场对提高堆焊层的硬度较明显,纵向磁场对提高堆焊层耐磨性效果明显.     

电接触强化对Ni/Cu复合镀层组织与性能的影响

利用电刷镀在铸铁表面制备了厚度在1 mm左右的Ni/Cu复合镀层,并对镀层进行了电接触强化试验。利用场发射电镜(FESEM)、维氏硬度计分析了电接触强化对镀层组织性能的影响。试验结果表明,电接触强化改善了镀层表面和内部质量,减少了镀层内部裂纹、孔洞等缺陷。同时,电接触强化使镀层和基体之间产生了部分镶嵌熔融。电接触强化改变了Ni层与Cu层的组织结构,使镀层组织更加致密紧实,Cu层和Ni层之间发生了塑性变形,产生了一定的镶嵌。强化后镀层表面及截面硬度都有所提升。镀层与基体之间形成的硬化层硬度远大于基体硬度,电接触强化提高了镀层与基体之间的结合力。     

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。     

纳米氧化锆热障涂层组织结构和抗热冲击性能分析

采用大气等离子喷涂技术制备了纳米氧化锆热障涂层和常规热障涂层.利用FESEM和XRD对纳米氧化锆热障涂层的组织结构和物相组成进行分析.系统研究了两种热障涂层的抗热冲击性能.微观组织分析结果表明,纳米氧化锆热障涂层展现出独特的纳米—微米复合结构,包括柱状晶和未熔融或部分熔融纳米颗粒.非平衡四方相是涂层的主要物相.抗热冲击性能试验结果表明,纳米氧化锆热障涂层拥有更为优越的抗热冲击性能,这主要得益于其相对致密的结构以及微裂纹、纳米晶粒、小孔径孔隙的应力缓释作用.热应力失效是涂层失效的主要原因.     

等离子喷涂Al-Mo涂层的高温硫化和氧化行为研究

烧嘴是水煤浆气化系统的重要部件。运行过程中的高温硫化经常导致烧嘴提前失效,进而影响设备的安全稳定运行。本文采用等离子喷涂方法制备了Mo为粘结层的Al-Mo涂层,测量其在973 K, 1073 K and 1173 K的硫化和氧化行为,并与Mo涂层和Inconel合金进行比较。结果表明Al-Mo涂层的高温硫化抗力和氧化抗力均优于Mo涂层,高温硫化抗力优于Inconel合金。该涂层的提出为喷嘴失效问题的解决提供了便捷、有效的技术方案。     

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...     

三种热障涂层的组织性能

采用等离子喷涂技术制备了三种不同材料的热障涂层(TBC),对涂层进行了组织性能的分析比较.结果表明,Al-1075的TBC结合强度最高,为 24.66 MPa,具有良好的抗热震性能;KF-230的TBC结合强度最低,为 16.06 MPa;LG-210的TBC结合强度居中,抗热震性能最差.分析认为,氧化物层(TGO)在热障涂层中的失效起至关重要的作用,TGO是裂纹的产生源,是裂纹扩展的通道,是热障涂层系统中的最薄弱环节.因此抑制TGO是提高涂层结合强度、改善涂层抗热震性能的重要措施.     

等离子喷涂过程中粒子的氧化及其对涂层性能的影响

利用粒子收集装置和附加氩气保护罩,研究了铁粒子和NiCoCrAlY粒子在等离子喷涂过程中的氧化行为及其对涂层性能的影响.结果表明,粒子在飞行过程中存在对流氧化和扩散氧化两种氧化机制,粒子的氧化方式取决于离开喷嘴的距离;离开喷嘴距离越长,粒子氧化越严重;采用附加氩气保护罩能明显减少喷涂过程中外界空气对粒子的氧化,降低涂层孔隙率,提高NiCoCrAlY涂层的抗高温氧化性能.

Abstract：

The oxidation mechanisms of iron particles and NiCoCrAlY particles during plasma spraying process and its effect on the sprayed coatings were investigated by the in-flight particles collection setup and the gas shrouding. The results show that there are two oxidation mechanisms during in-flight oxidation: one is the diffusion oxidation; the other is the convective oxidation, which are decided by the distance from the spraying particles to the nozzle. The oxidation content increases with the increasing of the standoff distance. The shrouded gas can decrease the oxidation content of inflight particles and increase the oxidation resistance of NiCoCrAIY coatings.