Friction Behaviors of the Hot Filament Chemical Vapor Deposition Diamond Film under Ambient Air and Water Lubricating Conditions

The friction behavior of the hot filament chemical vapor deposition（HFCVD） diamond film plays a critical role on its applications in mechanical fields and largely depends on the environment. Studies on the tribological properties of HFCVD diamond films coated on Co-cemented tungsten carbide （WC-Co） substrates are rarely reported in available literatures, especially in the water lubricating conditions. In this paper, conventional microcrystalline diamond（MCD） and fine-grained diamond（FGD） films are deposited on WC-Co substrates and their friction properties are evaluated on a reciprocating ball-on-plate tribometer, where they are brought to slide against ball-bearing steel and copper balls in dry and water lubricating conditions. Scanning electron microscopy（SEM）, atomic force microscopy（AFM）, surface profilometer and Raman spectroscopy are adopted to characterize as-deposited diamond films; SEM and energy dispersive X-ray（EDX） are used to investigate the worn region on the surfaces of both counterface balls and diamond films. The research results show that the friction coefficient of HFCVD diamond films always starts with a high initial value, and then gradually transits to a relative stable state. For a given counterface and a sliding condition, the FGD film presents lower stable friction coefficients by 0.02-0.03 than MCD film. The transferred materials adhered on sliding interface are supposed to have predominate effect on the friction behaviors of HFCVD diamond films. Furthermore, the effect of water lubricating on reducing friction coefficient is significant. For a given counterpart, the stable friction coefficients of MCD or FGD films reduce by about 0.07-0.08 while sliding in the water lubricating condition, relative to in dry sliding condition. This study is beneficial for widespread applications of HFCVD diamond coated mechanical components and adopting water lubricating system, replacing ofoil lubricating, in a variety of mechanical processing fields to implement the green production process.

Characterization of atomic-layer MoS_2 synthesized using a hot filament chemical vapor deposition method

Atomic-layer MoS_2 ultrathin films are synthesized using a hot filament chemical vapor deposition method. A combination of atomic force microscopy（AFM）, x-ray diffraction（XRD）, high-resolution transition electron microscopy（HRTEM）, photoluminescence（PL）, and x-ray photoelectron spectroscopy（XPS） characterization methods is applied to investigate the crystal structures, valence states, and compositions of the ultrathin film areas. The nucleation particles show irregular morphology, while for a larger size somewhere, the films are granular and the grains have a triangle shape. The films grow in a preferred orientation（002）. The HRTEM images present the graphene-like structure of stacked layers with low density of stacking fault, and the interlayer distance of plane is measured to be about 0.63 nm. It shows a clear quasihoneycomb-like structure and 6-fold coordination symmetry. Room-temperature PL spectra for the atomic layer MoS_2 under the condition of right and left circular light show that for both cases, the A1 and B1 direct excitonic transitions can be observed. In the meantime, valley polarization resolved PL spectra are obtained. XPS measurements provide high-purity samples aside from some contaminations from the air, and confirm the presence of pure MoS_2. The stoichiometric mole ratio of S/Mo is about 2.0–2.1, suggesting that sulfur is abundant rather than deficient in the atomic layer MoS_2 under our experimental conditions.

FABRICATION OF DIAMOND TUBES IN BIAS-ENHANCED HOT-FILAMENT CHEMICAL VAPOR DEPOSITION SYSTEM

Deposition of diamond thin films on tungsten wire substrate with the gas mixture of acetone and hydrogen by using bias-enhanced hot filament chemical vapor deposition（CVD）with the tantalum wires being optimized arranged is investigated.The self-supported diamond tubes are obtained by etching away the tungsten substrates.The quality of the diamond film before and after the removal of substrates is observed by scanning electron microscope（SEM）and Raman spectrum.The results show that the cylindrical diamond tubes with good quality and uniform thickness are obtained on tungsten wires by using bias enhanced hot filament CVD.The compressive stress in diamond film formed during the deposition is released after the substrate etches away by mixture of H2O2 and NH4 OH.There is no residual stress in diamond tube after substrate removal.

Formation and Transport of Atomic Hydrogen in Hot-Filament Chemical Vapor Deposition Reactors

In this paper we focus on diamond film hot-filament chemical vapor deposition reactors where the only reactant is hydrogen so as to study the formation and transport of hydrogen atoms. Analysis of dimensionless numbers for heat and mass transfer reveals that thermal conduction and diffusion are the dominant mechanisms for gas-phase heat and mass transfer, respectively. A simplified model has been established to simulate gas-phase temperature and H concentration distributions between the filament and the substrate. Examination of the relative importance of homogeneous and heterogeneous production of H atoms indicates that filament-surface decomposition of molecular hydrogen is the dominant source of H and gas-phase reaction plays a negligible role. The filament-surface dissociation rates of H2 for various filament temperatures were calculated to match H-atom concentrations observed in the literature or derived from power consumption by filaments. Arrhenius plots of the filament-surface hydrogen dissociation rates suggest that dissociation of H2 at refractory filament surface is a catalytic process, which has a rather lower effective activation energy than homogeneous thermal dissociation. Atomic hydrogen, acting as an important heat transfer medium to heat the substrate, can freely diffuse from the filament to the substrate without recombination.

<100> Textured Diamond Film on Silicon Grown by Hot Filament Chemical Vapor Deposition

The <100> textured growth of diamond film on HF eroded silicon wafer has been studied by HFCVD. The evolution of grain size and sudece morphology vs deposition time is presented and the <100> textured thick diamond film (80μm) with smooth surface, desirable for practical application in many fields is obtained

Synthesis and Growth Mechanism of Carbon Filaments by Chemical Vapor Deposition without Catalyst

Carbon filaments with diameter from several to hundreds deposition of methane without catalyst. The morphology micrometers were synthesized by chemical vapor microstructure and mechanical properties of the carbon filament were investigated by scanning electronic microscopy, optical microscopy, X-ray diffraction and mechanical testing. The results show that the carbon filament is inverted cone shape and grows up along the gas flow direction. The stem of it is formed of annular carbon layers arranged in a tree ring structure while the head is made up of concentrical layers. The tensile strength of the carbon filament is increased after graphitization for the restructuring and growing large of graphene. The growth mechanism of carbon filament was proposed according to the results of two series of experiments with different deposition time and intermittent deposition cycles.

Study of filament performance in heat transfer and hydrogen dissociation in diamond chemical vapor deposition

Hot-filament chemical vapor deposition ( HFCVD) is a promising method for commercial production of diamond films. Filament performance in heat transfer and hydrogen decomposition in reactive environment was investigated. Power consumption by the filament in vacuum, helium and 2% CH4/H2 was experimentally determined in temperature range 1300℃-2200℃. Filament heat transfer mechanism in C-H reactive environment was calculated and analyzed. The result shows that due to surface carburization and slight carbon deposition, radiation in stead of hydrogen dissociation, becomes the largest contributor to power consumption. Filament-surface dissociation of H2 was observed at temperatures below 1873K, demonstrating the feasibility of diamond growth at low filament temperatures. The effective activation energies of hydrogen dissociation on several clean refractory flaments were derived from power consumption data in literatures. They are all lower than that of thermal dissociation of hydrogen revealing the nature of catalytic dissociation of hydrogen on filament surface. Observation of substrate temperature suggested a weaker role of atomic hydrogen recombination in heating substrates in C-H environment than in pure hydrogen.

Friction and Cutting Properties of Hot-Filament Chemical Vapor Deposition Micro-and Fine-grained Diamond Coated Silicon Nitride Inserts

The micro-crystalline diamond (MCD) and fine-grained diamond (FGD) films are deposited on commercial silicon nitride inserts by the hot-filament chemical vapor deposition (HFCVD) method. The friction andcutting properties of as-deposited MCD and FGD films coated silicon nitride (Si3N4) inserts are comparatively investigated in this study. The scanning electron microscopy (SEM) and Raman spectroscopy are adopted to studythe characterization of the deposited diamond films. The friction tests are conducted on a ball-on-plate typereciprocating friction tester in ambient air using Co-cemented tungsten carbide (WC-Co), Si3N4 and ball-bearing steel (BBS) balls as the mating materials of the diamond films. For sliding against WC-Co, Si3N4 and BBS,the FGD film presents lower friction coeffcients than the MCD film. However, after sliding against Si3N4, the FGD film is subject to more severe wear than the MCD film. The cutting performance of as-deposited MCD and FGD coated Si3N4 inserts is examined in dry turning glass fiber reinforced plastics (GFRP) composite materials,comparing with the uncoated Si3N4 insert. The results indicate that the lifetime of Si3N4 inserts can be prolonged by depositing the MCD or FGD film on them and the FGD coated insert shows longer cutting lifetime than the MCD coated one.

Synthesis and oxidation behavior of boron-substituted carbon powders by hot filament chemical vapor deposition

Boron-substituted carbon powder, BxC1-x with x up to 0.17, has been successfully synthesized by hot filament chemical vapor deposition. The boron concentration in prepared BxC1-x samples can be controlled by varying the relative proportions of methane and diborane. X-ray diffraction, transmission electron microscopy, and electron energy loss spectrum confirm the successful synthesis of an amorphous BC5 compound, which consists of 10―20 nm particles with disk-like morphology. Thermogravimetry measurement shows that BC5 compound starts to oxidize ap-proximately at 620℃ and has a higher oxidation resistance than carbon.

Friction and Wear Performances of Hot Filament Chemical Vapor Deposition Multilayer Diamond Films Coated on Silicon Carbide Under Water Lubrication

Tribological properties of chemical vapor deposition (CVD) diamond films greatly affect its application in the mechanical field. In this paper, a novel multilayer structure is proposed, with which multilayer diamond films are deposited on silicon carbide by hot filament CVD (HFCVD) method. The different micrometric diamond grains are produced by adjusting deposition parameters. The as-deposited multilayer diamond films are characterized by scanning electron microscope (SEM) and white-light interferometry. The friction tests performed on a reciprocating ball-on-plate tribometer suggest that silicon carbide presents the friction coefficient of 0.400 for dry sliding against silicon nitride (Si3N4) ceramic counterface. With the water lubrication, the corresponding friction coefficients of silicon carbide and as-deposited multilayer diamond films further reduce to 0.193 and 0.051, respectively. The worn surfaces indicate that multilayer diamond films exhibit considerably high wear resistance.

Simulation of Temperature Distribution in Hot Filament Chemical Vapor Deposition Diamond Films Growth on Si C Seals

In this study, the temperature and gas velocity distributions in hot filament chemical vapor deposition(HFCVD) diamond film growth on the end surfaces of seals are simulated by the finite volume method. The influence of filament diameter, filament separation and rotational speed of the substrates is considered. Firstly,the simulation model is established by simplifying operating conditions to simulate the temperature and gas velocity distributions. Thereafter, the deposition parameters are optimized as 0.6 mm filament diameter, 18 mm filament separation and 5 r/min rotational speed to get the uniform temperature distribution. Under the influence of the rotational speed, the difference between temperature gradients along the directions perpendicular to the filament and parallel to the filament becomes narrow, it is consistent with the actual condition, and the maximum temperature difference on the substrates decreases to 7.4?C. Furthermore, the effect of the rotational speed on the gas velocity distribution is studied. Finally, diamond films are deposited on the end surfaces of Si C seals with the optimized deposition parameters. The characterizations by scanning electron microscopy(SEM) and Raman spectroscopy exhibit a layer of homogeneous diamond films with fine-faceted crystals and uniform thickness. The results validate the simulation model.

Preparation of Large-Scale Double-Side BDD Electrodes and Their Electrochemical Performances

Boron doped diamond(BDD)performs well in electrochemical oxidation for organic pollutants thanks to its wide electrochemical window and superior chemical stability.We presented a method to obtain well-adherent large-scale BDD/Nb electrode by the modified hot filament chemical vapor deposition system(HFCVD).SiC particles were sand blasted to enhance the adhesion of BDD coating.The BDD coating was then deposited on both sides of Nb which was placed vertically and closely with filament grids on both sides.The BDD/Nb electrodes had no deformation because the thermal deformations of the BDD films on both sides of the Nb substrate conteracted each other during cooling process after deposition.The surface morphology and purity of the BDD/Nb electrode were analyzed by Raman and scanning elestron microscope(SEM)techniques.Scratch test was used to investigate the adhesion of BDD films.The electrochemical performances were measured by cyclic voltammetry test.The BDD electrode at the B/C ratio of 2 000×10^(-6) held a higher oxygen evolution potential thanks to its high sp3 carbon content.Accelerated life test illustrated that the sandblasting pretreatment obviously enhanced the adhesion of BDD coating which resulted in a longer service duration than the un-sandblasted one.

Si_(3)N_(4)基底表面粗糙度对HFCVD法制备金刚石薄膜摩擦学性能的影响

采用热丝化学气相沉积法(hot filament chemical vapour deposition,HFCVD)在不同表面粗糙度的Si3N4基底表面制备金刚石薄膜,并对薄膜的特性进行检测与分析。利用场发射电子扫描显微镜、原子力显微镜检测植晶后的Si3N4基底表面以及制备的金刚石薄膜表面形貌;利用多功能摩擦磨损实验机、探针式轮廓仪,在干摩擦条件下,测试金刚石薄膜的摩擦系数及磨损率。综合基底粗糙度对植晶质量的影响、金刚石薄膜表面形貌与摩擦磨损检测实验结果,确定了Si3N4基底表面粗糙度对金刚石薄膜耐磨性的影响。结果表明:基底表面粗糙度会影响植晶的均匀性及致密性,进而影响金刚石颗粒在基底表面的生长,同时基底的表面形貌也会复映在金刚石薄膜表面。表面粗糙度为0.15μm和0.20μm的基底所制备的金刚石薄膜拥有较好的耐磨性,可得到最低的磨损率1.75×10^(−7)mm^(3)/(m·N)和最低的摩擦系数0.078。

Effects of Hot Wire Temperature on Properties of GeSi:H Films with High Hydrogen Dilution by Hot-Wire Chemical Vapor Deposition

GeSi:H films are prepared by hot-wire chemical vapor deposition(CVD) with high hydrogen dilution, DH=98%. Effects of hot wire temperature(Tw) on deposition rate, structural properties and bandgap of GeSi:H films are studied with surface profilemeter, Raman spectroscopy, Fourier transformed infrared spectroscopy, and UV-VIS-NIR spectrophotometer. It is found that the deposition rate(Rd) goes up with increasing of Tw, but increasing rate of Rd declines when Tw≥1 550 ℃. High Tw is beneficial to the formation of Ge-Si, but it has little effect on relative contents of the hydrogen bonds(Ge-H, Si-H, etc.) in the films. In the Tw range of 1 400-1 850 ℃, the maximum bandgap of the GeSi:H films is 1.39 eV at Tw =1 450 ℃ and the band gap decreases with Tw increasing when Tw≥1 450 ℃.

多片式衬底HFCVD系统沉积金刚石颗粒物理场的仿真优化

探索热丝化学气相沉积(hot filament chemical vapor deposition,HFCVD)合成高效优质的金刚石已成为研究热点。采用可提高金刚石颗粒单次沉积产量的新型多片式栅状衬底,应用FLUENT流体仿真软件,在原有单个出气口数量及进气总流量保持不变的情况下,优化传统模型,将单个进气口拆分成5个大小相等的进气口,对影响金刚石单晶颗粒均匀性的进气口数量和排布方式工艺参数进行仿真,对比分析HFCVD系统内气体的物理场。结果显示:4组优化模型均提高了衬底温度及流速的均匀性,有利于金刚石单晶颗粒的均匀生长,但对其沉积速率影响不显著;进一步分析优化模型的温度场,发现5个进气口及单个出气口分别位于反应腔体顶部和底部的中间位置时系统的温度差最低,最满足金刚石单晶颗粒在多片式硅衬底上均匀生长的条件。HFCVD金刚石单晶颗粒沉积试验验证了仿真结果的正确性。

Effect of hydrogen on low temperature epitaxial growth of polycrystalline silicon by hot wire chemical vapor deposition

Polycrystalline silicon （poly-Si） films were prepared by hot-wire chemical vapor deposition （HWCVD） at a low substrate temperature of 525 ℃. The influence of hydrogen on the epitaxial growth of ploy-Si films was investigated. Raman spectra show that the poly-Si films are fully crystallized at 525 ℃ with a different hydrogen dilution ratio （50%-91.7%）. X-ray diffraction, grazing incidence X-ray diffraction and SEM images show that the poly-Si thin films present （100） preferred orientation on （100） c-Si substrate in the high hydrogen dilution condition. The P-type poly-Si film prepared with a hydrogen dilution ratio of 91.7% shows a hall mobility of 8.78 cm2/（V-s） with a carrier concentration of 1.3 × 10^20 cm^-3, which indicates that the epitaxial poly-Si film prepared by HWCVD has the possibility to be used in photovoltaic and TFT devices.

Si3N4工程陶瓷基底金刚石涂层生长规律及性能

为了避免氮化硅材料因产生裂纹或延伸破裂等造成的失效,利用热丝化学气相沉积法(Hot filament chemical vapor deposition,HFCVD)在氮化硅基底上沉积具有高硬度的金刚石涂层,采用单因素影响试验,分别探究碳源浓度、腔室压力、基底温度对金刚石成膜过程的影响机制,探究微米和纳米金刚石涂层的最优生长工艺参数。利用拉曼光谱仪(Raman)、X射线衍射仪(XRD)、扫描电子显微镜(SEM)和原子力显微镜(AFM)对不同参数制备出的金刚石的形核、表面形貌、薄膜质量、表面粗糙度等进行表征,利用洛氏硬度计分析膜基结合力。结果表明,腔室压力越大,活性物质到达基底的动能越小,不利于金刚石的成核和生长。生长速率和表面粗糙度主要受甲烷浓度的影响:甲烷浓度从1%到7%,生长速率从0.84μm/h上升到1.32μm/h;表面粗糙度Ra从53.4 nm降低到23.5 nm;甲烷浓度过高导致涂层脱落严重,膜基结合力变差;晶面形貌和金刚石含量受到基底温度的影响较为明显,随着温度升高,金刚石质量提高。综合基底温度、腔室压力对金刚石涂层的影响,确定最佳生长温度为900℃,气压为1 kPa。调节甲烷浓度1%为微米金刚石;甲烷浓度5%为纳米金刚石。研究方法可以优化在陶瓷基底上制备具有优异性能的金刚石薄膜的制备参数。

热丝化学气相沉积法制备单晶金刚石的试验研究

热丝化学气相沉积法沉积区域可达12英寸(30.48 cm),其具备大批量生产单晶金刚石的潜力。采用尺寸为3 mm×3 mm×1 mm,(100)取向的单晶金刚石为基体,利用热丝化学气相沉积法以甲烷和氢气为前驱体,同时通入少量氮气进行同质外延生长。结果表明,在热丝温度为2200℃、碳源浓度为4%、腔体气压为4 kPa的条件下,单晶金刚石以3.41μm/h的速度生长,表面无多晶、破口、孔洞等缺陷;外延层X射线衍射光谱在(400)面处峰值的半高宽为0.11°,低于基体的半高宽0.16°,证明外延层具有较高的晶体质量;氮气的引入可以提升单晶金刚石的生长速度,同时降低外延层的晶体质量,较高的氮气浓度还会使得单晶金刚石的生长模式转为岛状生长。

HFCVD衬底三维温度场有限元法模拟

热丝化学气相沉积(Hot filament chemical vapor deposition,HFCVD)方法制备金刚石薄膜设备简单,成本低廉,适合大面积金刚石膜的产业化生产,其中衬底温度是沉积高质量CVD金刚石膜的重要参数之一。基于此,首先分析大面积HFCVD系统的热交换过程,建立大面积HFCVD系统衬底温度场的三维有限元模型。与传统纯热辐射模型相比,本模型更加接近实际系统,并较好符合试验测定的结果。根据三维有限元模型开展对大面积HFCVD系统衬底温度场的有限元仿真研究,得到HFCVD系统衬底温度场的三维分布规律,并讨论热丝直径、热丝温度、热丝根数、热丝-衬底距离和水冷散热系数等对衬底温度大小及均匀性的影响。仿真结果表明,在适宜金刚石膜生长的参数范围内,热丝参数和衬底接触热阻对衬底温度大小有显著影响,由于衬底内部的三维热传导使得衬底温度场更加均匀,各参数对衬底温度场的均匀性影响不大。研究结果为高质量制备金刚石膜提供理论基础。

沉积参数对WC-Co基体内孔HFCVD金刚石薄膜生长的影响（英文）

在内孔HFCVD金刚石薄膜沉积过程中,沉积温度(t)、碳源浓度(φ)、总反应压力(ρ)和气体总流量(F)等沉积参数对金刚石薄膜的生长具有显著影响。采用Taguchi方法系统研究这4个关键参数对内孔HFCVD金刚石薄膜性能的综合影响,并且通过自定义的品质因数(figure-of-merit,FOM)评价金刚石薄膜的综合性能。沉积温度、碳源浓度和总反应压力对于内孔HFCVD金刚石薄膜的各项性能及FOM均存在显著影响,并且与平片或外表面沉积存在一定的差异。根据上述影响性分析的结果,以获得最佳的内孔HFCVD金刚石薄膜综合性能为优化目标所确定的最优化沉积参数为:t=830℃,φ=4.5%,ρ=4000 Pa,F=800 mL/min。