CVD温度对钼沉积层组织及性能的影响

介绍了化学气相沉积法(CVD)制备难熔金属钼膜层的原理和方法。以MoF_6和H_2为原料,采用化学气相沉积法在纯铜基体上沉积出难熔金属钼膜层。分析研究了沉积层的组织、结构和硬度。实验结果表明：沉积膜层显微组织随沉积温度变化而不同,沉积温度较低时,沉积层显微组织为细晶层状结构,沉积层硬度可达677×9.8 MPa：沉积温度较高时,沉积层显微组织为致密的柱状晶,硬度稍高于一般烧结钼的硬度。     

化学气相沉积难熔金属钼组织性能的研究

介绍了化学气相沉积法制备难熔金属钼膜层的原理和方法。以MoF6和H2为原料,采用化学气相沉积法在纯铜基体上沉积出难熔金属钼膜层。分析研究了沉积层的组织、结构和硬度。实验结果表明：沉积膜层显微组织随沉积温度变化而不同,沉积温度较低时沉积层显微组织为细晶层状结构,沉积层硬度可达677HV;沉积温度较高时沉积层显微组织为致密的柱状晶,硬度稍高于一般烧结钼。     

CVD温度对钨沉积层组织性能的影响

以WF6和H2为反应气体,采用化学气相沉积法在纯铜基体上沉积出难熔金属钨涂层.分析研究了沉积温度对沉积层组织、结构、表面形貌及涂层致密度、硬度、耐磨性能的影响.试验结果表明:随着温度升高,沉积速率加快,涂层组织逐渐由柱状晶转变为树枝晶,表面粗糙度显著增加,膜层致密度、硬度下降,耐磨性降低.化学气相沉积钨的最佳工艺温度范围为550～650℃.     

反应磁控溅射法制备(Ti,Al)N薄膜的力学性能

以WF6和H2为原料,采用化学气相沉积法在纯铜基体上沉积出难熔金属钨涂层。分析研究了不同沉积温度(500℃,600℃,700℃)沉积层显微组织、表面形貌、表面粗糙度及相关机制。试验分析表明:随沉积温度升高,沉积速率加快,涂层组织柱状晶生长取向趋于杂乱;沉积层表面形貌发生明显改变,表面粗糙度显著增加。杂质颗粒对沉积组织有显著的影响,造成沉积表面粗糙度显著增加。     

钽的CVD动力学规律及显微组织

简述氢气还原氯化钽化学气相沉积钽(CVD)的主要原理,研究氯化、氯气流量、氢气流量和沉积温度4个参数对沉积速率及沉积层显微组织的影响。结果表明:氯化温度对沉积速率的影响最小,沉积温度的影响最大;显微组织由小晶粒区和柱状晶区组成,沉积参数改变,柱状晶晶粒大小发生变化。     

化学气相沉积制备铂族金属涂层及难熔金属

综述了化学气相沉积(Chemical Vapor Deposition,简称CVD)技术制备高温抗氧化涂层-铂族金属(Pt、Ir)涂层及难熔金属(W、Mo、Ta、Nb、Re)的方法.并对部分有报道的沉积参数以及沉积参数对沉积层结构及性质的影响进行了介绍.     

固态输送ZrCl4低压化学气相沉积制备ZrC涂层的特征

采用ZrCl4-CH4-H2-Ar反应体系、固态输送ZrCl4粉末低压化学气相沉积(CVD)制备ZrC涂层。研究温度对低压化学气相沉积ZrC涂层物相组成、晶体择优生长、涂层表面形貌、断面结构、涂层生长速度和沉积均匀性等方面的影响。结果表明:不同温度下沉积的涂层主要由ZrC和C相组成;随着温度的升高,ZrC晶粒(200)晶面择优生长增强,颗粒直径增大,表面致密性增加,沉积速率上升;涂层断面结构以柱状晶为主;随着离进料口距离的增加,涂层的沉积速率逐渐减小;1 500℃时,沉积系统的均匀性比1 450℃时的差。     

工艺参数对CVI-TaC沉积速率的影响

利用TaCl5-Ar-C3H6-H2反应体系,采用化学气相渗透(CVI)法在炭毡中沉积TaC,并研究了CVI工艺参数如气体流速、滞留时间、沉积温度、沉积压力和H2的加入等对碳化钽在炭毡中沉积速率(用炭毡质量分数的增加来表示)的影响。研究表明:CVI-TaC受表面反应控制的最大气体流速为40 cm/s,最小滞留时间为1.2 s;沉积速率与沉积温度之间的关系不符合Arrhenius方程,沉积速率随沉积温度的升高先增加后减小,在950℃时达到最大值;在1 000℃时,CVI过程受孔隙扩散所控制;沉积速率随沉积压力的升高以及H2的加入而急剧增加。     

化学气相沉积技术及在难熔金属材料中的应用

简述了化学气相沉积技术(Chemical Vapor Deposition,简称CVD)的发展历程及其应用领域;重点阐述CVD技术在难熔金属(W、Re、Ta、Mo、Nb)相关领域的应用概况并展望了其研究前景,特别指出CVD技术在制备难熔金属合金研究上存在的挑战和机遇。     

CVD钨沉积层组织控制

以WF6和H2为反应气体,采用间断供应反应气体方法改变CVD钨沉积层显微组织形貌。研究了间断沉积工艺参数对沉积层显微组织及性能的影响,讨论了间断沉积层的表面应力状态及断口裂纹扩展情况。结果表明:采用间断化学气相沉积法钨层的显微组织随周期沉积时间的缩短,柱状晶晶粒长度尺寸变小,形态逐渐接近等轴晶;沉积层表面形貌呈圆球状,沉积层生长界面不再趋向于单一方向;钨层保持了连续CVD钨的高纯度、高密度特性。且采用间断供应反应气体沉积方法显著降低了钨制品表面的残余应力,使裂纹扩展方向发生改变,有效阻碍了裂纹的深入扩展。     

沉积温度对高性能TiAlN涂层微观结构和力学性能的影响

采用真空电弧离子镀（AIP）技术在不同沉积温度下TiAlN涂层,用于高性能制造,并研究了沉积温度与表面性能的关系。结果表明,由于离子轰击作用,表面大颗粒随沉积温度的升高而减少。随着沉积温度的升高,涂层表面的晶粒尺寸先急剧减小后逐渐增大。此外,沉积温度对合成涂层的相组成和化学成分影响不大。随着沉积温度的升高,硬度和粘结强度先迅速增加,后逐渐降低。当沉积温度在450℃左右时,沉积的TiAlN涂层硬度最高,粘结强度最大。上述现象的发生机理与沉积过程中表面与界面之间的微观组织和残余应力的变化有关。合成的涂层在高达900℃的空气中具有良好的热稳定性。     

The effect of substrate position on the microstructure and mechanical properties of SiC coatings on carbon/carbon composites

In this work, silicon carbide (SiC) coatings were produced on carbon/carbon composites using a chemical vapour deposition (CVD) method. During deposition, the temperature was fixed at 1200 °C and the coatings were produced by placing substrates at three different positions (340, 380 and 420 mm from the inlet) in the CVD reactor. The effect of substrate position on the microstructure and mechanical properties of the SiC coatings were experimentally investigated. The phase composition, surface morphology, defects and microstructure were studied using X-ray diffraction (XRD), scanning electron microscopy (SEM) and Raman Spectroscopy. The hardness and Young's modulus were measured using a nano-indentation method while fracture toughness was evaluated by micro-indentation. It was found that the deposition rate decreased linearly as substrate position moved far from the reactor inlet. In all coatings, only β-SiC phase was observed with a high density of stacking faults. It was found that the substrate position in the CVD reactor has a significant effect on the microstructure, grain size and crystallinity of the coating. At 340 and 420 mm substrate positions, a well-developed faceted microstructure with high crystallinity was observed while at 380 mm substrate position, the coating having lenticular-like fine grains with low crystallinity was obtained. The hardness values obtained from the top surface of the coatings are found to be higher than those from the cross-section, although the Young's modulus data (measured from the top surface and cross-section) were observed to be similar. At 380 mm substrate position, hardness, Young's modulus and fracture toughness were found to be the lowest compared to that of the coatings produced at 340 and 420 mm substrate positions. It is concluded that the SiC coatings with better mechanical properties can be produced by adjusting the substrate position in the CVD reactor.     

Fabrication of WC-Co/(Ti,W)C graded cemented carbide by spark plasma sintering

The WC-Co/(Ti, W)C graded cemented carbide was prepared by spark plasma sintering. The substrate is WC-8Co, and the hard layer is (Ti, W)C solid-solution. The effects of sintering temperature and holding time on the microstructure and properties of graded cemented carbide were analyzed. The hard layer is mainly formed by dissolving WC in the Co-phase and then by solid-solution reaction with TiC. As the sintering temperature increases, the migration rate of WC increases. When the holding time is 5 min, the thickness and the W content of the (Ti, W)C solid-solution hard layer increases with the increasing of sintering temperature. The thickness of the (Ti, W)C solid-solution can reach 51 ± 2 μm at the sintering temperature of 1700 °C for the holding time of 5 min. The hardness of hard layer surface increases first and then decreases with the increasing of sintering temperature. The Vickers hardness is the highest at 1600 °C, which can reach HV_0.221.53GPa. As the holding time increases, the thickness of the solid-solution hard layer increases, but the rate of growth decreases. As the thickness increases, the difference in the W element concentration between the solid-solutions of the same pitch decreases along the layer depth direction, and W element concentration in the entire hard layer increases. The oxidation behavior of graded cemented carbide at 400 °C and 600 °C was investigated. The (Ti, W)C hard layer has superior oxidation resistance relative to the WC-Co substrate.     

Mechanical Properties and Dissolution Behavior of Plasma Sprayed Wollastonite Coatings Deposited at Different Substrate Temperatures

The effect of substrate temperature on the microstructure, mechanical properties and dissolution behavior of wollastonite coatings is investigated. The crystallinity of as-deposited coatings increases with increasing substrate temperature, whereas the porosity shows only a little variable tendency. The Knoop hardness and elastic modulus increase with the substrate temperature up to 400?°C firstly, and then a decrement is observed with the temperature further increasing to 600?°C. The dissolution rate characterized by the pH changes and the ion concentration changes of Ca, Si and P in SBF decreases with the increase in the substrate temperature. It can be concluded that increasing the substrate temperature is a feasible method to improve the mechanical properties and to decrease the dissolution rate of wollastonite coatings. However, the bioactivity of coatings deposited on preheated substrates is superior to those on non-preheated ones, which presumably results from their different phase compositions.     

沉积温度对高功率脉冲磁控溅射AlCrSiN涂层结构和性能的影响*

采用高功率脉冲磁控溅射(HiPIMS)技术在不同沉积温度下制备了Al-Cr-Si-N涂层。系统研究了沉积温度对涂层结构、成分、显微形貌、力学和摩擦学性能的影响。结果表明:随着沉积温度由100℃升至350℃,涂层内部开始由非晶向纳米晶转化,300℃时出现fcc-AlN相;涂层平整性和致密性逐步改善,膜/基结合强度逐渐提高,在300℃达到最大值77 N,但温度继续升高至350℃时,严重的轰击刻蚀作用使临界载荷骤降至25 N;涂层硬度逐渐增加,在350℃达到最大值19.4GPa;涂层内应力整体呈下降趋势,由–0.8 GPa逐渐降低至–0.4 GPa左右。     

Effects of temperature on the mechanical properties of Ti6Al4V powder compacts prepared by magnetic pulse compaction

The effects of temperature (0–500°C) on the compressive strength, hardness, average relative density, and microstructure of Ti6Al4V powder green compacts prepared by magnetic pulse compaction were investigated. The results show that with increasing heating temperature, the compressive strength first increases and then decreases with the maximum value of 976.74 MPa at 400°C. The average relative density and hardness constantly increase, and their values reach 96.11% and HRA 69.8 at 500°C, respectively. The increase of partial welding is found among the junctions of particles inside the compacts; there is no obvious grain growth inside the compacts within the temperature range.     

气体流量对LPCVD ZrC涂层结构和沉积机理的影响

利用低压化学气相沉积(LPCVD)工艺,采用Zr-Br2-C3H6-H2-Ar反应体系,在1200℃下,于石墨基底表面制备了ZrC涂层。研究了气体流量对ZrC涂层微观形貌和沉积机理的影响。结果表明,随着气体流量由200 mL/min向1000 mL/min增大,涂层的沉积速率先增大后减小,在800 mL/min时达到极值,极大值为3.37×10-3g·cm-2·h-1。同时,涂层的择优取向发生了明显的变化,在600~800 mL/min范围内,涂层具有稳定且强烈的(200)晶面择优取向。XPS分析结果表明,沉积产物中的C/Zr比也随气体流量的增大,相应的由0.85快速地升高到1.49。当气体流量为200 mL/min时,涂层致密光滑,ZrC晶粒具有典型的等轴晶结构特征;当气体流量为400~800 mL/min时,涂层光滑平坦,ZrC晶粒具有规则的四面体结构;当气体流量为1000 mL/min时,涂层表面存在着大量不规则的岛状、弓状颗粒。基底表面边界层厚度的变化是影响涂层沉积过程的主要因素。     

Production and characterization of wear resistant Ti(C,N) coatings manufactured by modified chemical vapor deposition process

Wear resistant Ti(C,N) coatings were produced by changing the heating rate during the chemical vapor deposition process (CVD). The modification of the CVD process led to the formation of Ti(C,N) coatings with a particulate grain architecture consisting of two different crystallites (star-shaped and lenticular-like morphologies) co-existing in the coating layer. The microstructure formation of the Ti(C,N) layer was investigated by interrupting the CVD process at different temperatures. Depending on the deposition temperature, rounded, star-shaped and/or lenticular-like crystallites formed. The overall C/N ratio of the Ti(C,N) layer was 0.16/0.84, as determined by x-ray diffraction. TEM/EELS investigations of Ti(C,N) crystallites revealed an inhomogeneous distribution of carbon and nitrogen in the grains. Cutting tests showed outstanding wear resistance of the Ti(C,N) layers produced by the modified CVD process.     

Microstructure Characterization and Corrosion Properties of Nitrocarburized AISI 4140 Low Alloy Steel

Plasma nitrocarburizing treatments of AISI 4140 low alloy steel have been carried out in a gas mixture of 85% N₂-12% H₂-3% CO₂. All treatments were performed for 5 h at a chamber pressure of 4 mbar. Different treatment temperatures varying from 520 to 620 °C have been used to investigate the effect of treatment temperature on the corrosion and hardness properties and also microstructure of the plasma nitrocarburized steel. Scanning electron and optical microscopy, x-ray diffraction, microhardness measurement, and potentiodynamic polarization technique in 3.5% NaCl solution were used to study the treated surfaces. The results revealed that plasma nitrocarburizing at temperatures below 570 °C can readily produce a monophase ε compound layer. The compound layer formed at 620 °C is composed of two sub-layers and is supported by an austenite zone followed by the diffusion layer. The thickest diffusion layer was related to the sample treated at 620 °C. Microhardness results showed a reduction of surface hardness with increasing the treatment temperature from 520 to 620 °C. It has also been found that with increasing treatment temperature from 520 to 545 °C the corrosion resistance increases up to a maximum and then decreases with further increasing treatment temperature from 545 to 620 °C.     

Kinetics and microstructure of TiN coatings by CVD

Titanium nitride (TiN) coatings obtained by chemical vapor deposition with TiCl₄, H₂, and N₂ as gas sources at the atmospheric pressure have been examined in this study. The results showed that the deposition rate increased and reached a saturated value with increasing TiCl₄ partial pressure at different process parameters including deposition temperatures and partial pressures of H₂ and N₂. The reaction orders of TiCl₄, H₂, and N₂ were extracted by the least-square regression approximation of the experimental data. For TiCl₄ on N₂, their reaction order is influenced by the partial pressure of the other. A degraded growth rate at a high temperature of 1200°C was mainly related to the endothermic CVD TiN reaction and the hot-wall reactor. Microstructural examination by scanning electron microscope revealed the surface morphology changed with process parameters. Compositional analysis of the CVD TiN showed non-stoichiometric at low temperatures and 1200°C, but stoichiometric at 1000°C. The TiN stoichiometry could be affected by the partial pressures of N₂ and H₂.