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.

<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

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.

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.

GENETIC OPTIMIZATION OF HOT FILAMENT PARAMETERS IN HFCVD SYSTEM

In HFCVD system the substrate temperature is a key factor which deeply affects the quality of diamond films. Th e magnitude and the variation of the substrate temperature must be limited in a suitable range to deposit diamond films of uniform thickness over large areas. In this paper, the hot filament parameters are investigated on the basi s of GAs to realize a good substrate temperature profile. Computer simulations d emonstrate that on parameters optimized by GAs a uniform substrate temperatur e field can be formed over a relatively large circle area with R s=10 cm.

Si-doped diamond films prepared by chemical vapour deposition

The effects of Si doping on morphology, components and structure characteristics of CVD diamond films were studied. Si-doped CVD diamond films were deposited on Si substrate by adding tetraethoxysilane （TEOS） into acetone as source of reactant gas. The morphology and microstructure of diamond films were characterized by scanning electron microcopy （SEM）. The crystalline quality of diamond films was studied by Raman spectroscopy and X-ray diffractometry （XRD）. The surface roughness of the films was evaluated with surface profilometer. The results suggest that Si doping tends to reduce the crystallite size, enhance grain refinement and inhibit the appearance of （11 I） facets. Raman spectra indicate that Si doping can enhance the formation of sp2 phase in diamond films. Moreover, Raman signal of SiC was detected, which suggests the existence of Si in the diamond films. Smooth fine-grained diamond （SFGD） film was synthesized at Si to C ratio of 1%.

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。

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

Boron-substituted carbon powder, B x C1?x with x up to 0.17, has been successfully synthesized by hot filament chemical vapor deposition. The boron concentration in prepared B x C1?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 approximately at 620°C and has a higher oxidation resistance than carbon.

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.

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.

Effect of deposition parameters on micro-and nano-crystalline diamond films growth on WC-Co substrates by HFCVD

The characteristics of hot filament chemical vapor deposition（HFCVD） diamond films are significantly influenced by the deposition parameters, such as the substrate temperature, total pressure and carbon concentration. Orthogonal experiments were introduced to study the comprehensive effects of such three parameters on diamond films deposited on WC-Co substrates. Field emission scanning electron microscopy, atomic force microscopy and Raman spectrum were employed to analyze the morphology, growth rate and composition of as-deposited diamond films. The morphology varies from pyramidal to cluster features with temperature decreasing. It is found that the low total pressure is suitable for nano-crystalline diamond films growth. Moreover, the substrate temperature and total pressure have combined influence on the growth rate of the diamond films.

Effects of deposition parameters on HFCVD diamond films growth on inner hole surfaces of WC-Co substrates

Deposition parameters that have great influences on hot filament chemical vapor deposition (HFCVD) diamond films growth on inner hole surfaces of WC?Co substrates mainly include the substrate temperature (t), carbon content (φ), total pressure (p) and total mass flow (F). Taguchi method was used for the experimental design in order to study the combined effects of the four parameters on the properties of as-deposited diamond films. A new figure-of-merit (FOM) was defined to assess their comprehensive performance. It is clarified thatt,φandp all have significant and complicated effects on the performance of the diamond film and the FOM, which also present some differences as compared with the previous studies on CVD diamond films growth on plane or external surfaces. Aiming to deposit HFCVD diamond films with the best comprehensive performance, the key deposition parameters were finally optimized as:t=830 °C,φ=4.5%,p=4000 Pa,F=800 mL/min.

Preparation, characterization and electrochemical properties of boron-doped diamond films on Nb substrates

A series of boron-doped polycrystalline diamond films were prepared by hot filament （HF） chemical vapor deposition on Nb substrates. The effects of B/C ratio of reaction gas on film morphology, growth rate, chemical bonding states, phase composition and electrochemical properties of each deposited sample were studied by scanning electron microscopy, Raman spectra, X-ray diffraction, microhardness indentation, and electrochemical analysis. Results show that the average grain size of diamond and the growth rate decrease with increasing the B/C ratio. The diamond films exhibit excellent adhesion under Vickers microhardness testing （9.8 N load）. The sample with 2% B/C ratio has a wider potential window and a lower background current as well as a faster redox reaction rate in H2SO4 solution and KFe（CN）6 redox system compared with other doping level electrodes.

CVD金刚石膜研究进展

金刚石由于其优异的声、光、电、热和力学性能,是重要的功能材料之一。金刚石的制备方法主要有高温高压方法和低压化学气相沉积方法。化学气相沉积法因制备得到的样品质量高、面积大,设备简单、可规模化等特性,是合成金刚石膜的重要方法。为了实现低合成压力条件下的金刚石膜的均匀、快速、大尺寸、高质量生长,目前研究人员在金刚石低压生长的控制方面做出了深入的研究。文章综述了近年来化学气相沉积法(包括热丝CVD法、离子体增强CVD法、燃烧火焰CVD法)生长金刚石膜的研究进展,包括金刚石膜的生长机理、关键设备、关键工艺参数等。此外,还详细讨论了生长过程中的关键工艺参数与金刚石膜生长速率和质量的关系,这些对化学气相沉积制备金刚石膜的研究、生产至关重要。

Amorphous SiO_2 interlayers for deposition of adherent diamond films onto WC-Co inserts

Amorphous Si O2（a-Si O2） films were synthesized on WC-Co substrates with H2 and tetraethoxysilane（TEOS） via pyrolysis of molecular precursor.X-ray diffraction（XRD） pattern shows that silicon-cobalt compounds form at the interface between a-Si O2 films and WC-Co substrates.Moreover,it is observed by transmission electron microscope（TEM） that the a-Si O2 films are composed of hollow mirco-spheroid a-Si O2 particles.Subsequently,the a-Si O2 films are used as intermediate films and chemical vapor deposition（CVD） diamond films are deposited on them.Indentation tests were performed to evaluate the adhesion of bi-layer（a-Si O2 ＋ diamond） films on cemented carbide substrates.And the cutting performance of bi-layer（a-Si O2 ＋ diamond） coated inserts was evaluated by machining the glass fiber reinforced plastic（GFRP）.The results show that a-Si O2 interlayers can greatly improve the adhesive strength of diamond films on cemented carbide inserts;furthermore,thickness of the a-Si O2 interlayers plays a significant role in their effectiveness on adhesion enhancement of diamond films.

Effect of deposition temperature on properties of boron-doped diamond films on tungsten carbide substrate

Boron-doped diamond(BDD)films were deposited on the tungsten carbide substrates at different substrate temperatures ranging from 450 to 850°C by hot filament chemical vapor deposition(HFCVD)method.The effect of deposition temperature on the properties of the boron-doped diamond films on tungsten carbide substrate was investigated.It is found that boron doping obviously enhances the growth rate of diamond films.A relatively high growth rate of 544 nm/h was obtained for the BDD film deposited on the tungsten carbide at 650°C.The added boron-containing precursor gas apparently reduced activation energy of film growth to be 53.1 kJ/mol,thus accelerated the rate of deposition chemical reaction.Moreover,Raman and XRD analysis showed that heavy boron doping(750 and 850°C)deteriorated the diamond crystallinity and produced a high defect density in the BDD films.Overall,600-700°C is found to be an optimum substrate temperature range for depositing BDD films on tungsten carbide substrate.