Fabrication of Graphene/Cu Composite by Chemical Vapor Deposition and Effects of Graphene Layers on Resultant Electrical Conductivity

Graphene(Gr)has unique properties including high electrical conductivity;Thus,graphene/copper(Gr/Cu)composites have attracted increasing attention to replace traditional Cu for electrical applications. However,the problem of how to control graphene to form desired Gr/Cu composite is not well solved. This paper aims at exploring the best parameters for preparing graphene with different layers on Cu foil by chemical vapor deposition(CVD)method and studying the effects of different layers graphene on Gr/Cu composite’s electrical conductivity. Graphene grown on single-sided and double-sided copper was prepared for Gr/Cu and Gr/Cu/Gr composites. The resultant electrical conductivity of Gr/Cu composites increased with decreasing graphene layers and increasing graphene volume fraction. The Gr/Cu/Gr composite with monolayer graphene owns volume fraction of less than 0.002%,producing the best electrical conductivity up to59.8 ×10^(6)S/m,equivalent to 104.5% IACS and 105.3% pure Cu foil.

Purification of Single-walled Carbon Nanotubes Grown by a Chemical Vapour Deposition(CVD) Method

A procedure for purification of single walled carbon nanotubes(SWNTs) grown by the chemical vapour deposition(CVD) of carbon monooxide has been developed. Based on the result from TGA/DTA of as prepared sample, the oxidation temperature was determined. The process included sonication, oxidation and acid washing steps. The purity and yield after purification were determined and estimated by TEM. Moreover, for the first time, a loop structure for CVD SWNTs has been observed.

GROWTH MECHANISM OF TiC WHISKERS PREMRED BY A MODIFIED CHEMICAL VAPOR DEPOSITION METHOD

High quality TiC whiskers have been prepared by a modified chemical vapor deposition (CVD) method using TiCl4 and CH4 as reactant gases and Ni as substrate. The deposition temperature and gas flow mies have ampreciable effect on the whisker growth.The whisker orientations and morphology are determined by X-my diffraction (XRD),scanning electron micmpmph (SEM) and transmission electron microgmph (TEM).In addition to the spherical tips, spiral growth microsteps and obvious terraces are observed at the tips and side faces of whiskers in the present eoperiment. The whiskers grow mostly along (100) direction. The whisker growth mechanism is discussed in detail.

Science Letters:Development of supported boron-doping TiO_2 catalysts by chemical vapor deposition

In this study, supported nonmetal (boron) doping TiO2 coating photocatalysts were prepared by chemical vapor deposition (CVD) to enhance the activity under visible light irradiation and avoid the recovering of TiO2. Boron atoms were successfully doped into the lattice of TiO2 through CVD, as evidenced from XPS analysis. B-doped TiO2 coating catalysts showed drastic and strong absorption in the visible light range with a red shift in the band gap transition. This novel B-TiO2 coating photocatalyst showed higher photocatalytic activity in methyl orange degradation under visible light irradiation than that of the pure TiO2 photocatalyst.

Fibrous TiO_2 prepared by chemical vapor deposition using activated carbon fibers as template via adsorption,hydrolysis and calcinations

TiO2 fibers were prepared via alternatively introducing water vapor and Ti precursor carried by N2 to an APCVD （chemical vapor deposition under atmospheric pressure） reactor at ≤200 ℃. Activated carbon fibers （ACFs） were used as templates for deposition and later removed by calcinations. The obtained catalysts were characterized by scanning electron micros- copy （SEM）, transmission electron microscopy （TEM）, Brunauer, Emmett and Teller （BET） and X-ray diffraction （XRD） analysis The pores within TiO2 fibers included micro-range and meso-range, e.g., 7 nm, and the specific surface areas for TiO2 fibers were 141 m^2/g and 148 m^2/g for samples deposited at 100 ℃ and 200℃ （using ACFI700 as template）, respectively. The deposition temperature significantly influenced TiO2 morphology. The special advantages of this technique for preparing porous nano-material include no consumption of organic solvent in the process and easy control of deposition conditions and speeds.

Synthesis of flower-like WS_(2) by chemical vapor deposition

Flower-like tungsten disulfide(WS_(2))with a diameter of 5-10μm is prepared by chemical vapor deposition(CVD).Scanning electron microscopy(SEM),energy dispersive spectrometer(EDS),Raman spectroscopy,and ultraviolet-visible(UV-vis)spectroscopy are used to characterize its morphological and optical properties,and its growth mechanism is discussed.The key factors for the formation of flower-like WS_(2)are determined.Firstly,the cooling process causes the generation of nucleation dislocations,and then the"leaf"growth of flower-like WS_(2)is achieved by increasing the temperature.

Monolayer MoS_(2)of high mobility grown on SiO_(2)substrate by two-step chemical vapor deposition

We report a novel two-step ambient pressure chemical vapor deposition(CVD)pathway to grow high-quality Mo S_(2)monolayer on the Si O_(2)substrate with large crystal size up to 110μm.The large specific surface area of the pre-synthesized Mo O_(3)flakes on the mica substrate compared to Mo O_(3)powder could dramatically reduce the consumption of the Mo source.The electronic information inferred from the four-probe scanning tunneling microscope(4P-STM)image explains the threshold voltage variations and the n-type behavior observed in the two-terminal transport measurements.Furthermore,the direct van der Pauw transport also confirms its relatively high carrier mobility.Our study provides a reliable method to synthesize high-quality Mo S_(2)monolayer,which is confirmed by the direct 4P-STM measurement results.Such methodology is a key step toward the large-scale growth of transition metal dichalcogenides(TMDs)on the Si O_(2)substrate and is essential to further development of the TMDs-related integrated devices.

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.

C-H-F氛围下金刚石薄膜的低温CVD生长过程分析

基于第一性原理的密度泛函理论对C-H-F氛围下低温CVD金刚石薄膜的生长过程进行仿真分析,计算H、F原子在氢终止金刚石表面发生萃取反应的吸附能、反应热与反应能垒,并分析CF_(3)、CF_(2)、CF 3种生长基团在带有活性位点基底上的吸附。结果表明:与H原子相比,F原子更容易在氢终止金刚石表面萃出H,并以HF形式脱附,且在C-H-F氛围下有利于在低温时产生更多的活性位点;CF_(3)、CF_(2)、CF基团在吸附后的结构和吸附能绝对值都更有利于金刚石相的生成,适当提高CF_(3)、CF_(2)、CF基团的浓度有助于实现金刚石相的更高速率生长。

一步TCVD法制备大面积碳纳米管冷阴极及其场致发射性能研究

本文提出一步热化学气相沉积法(TCVD)热解二茂铁,并直接在硅衬底上制备大面积(1 cm^(2))、高质量碳纳米管(CNTs)场致发射冷阴极阵列的制备工艺.通过调控二茂铁的热解温度(650~1000℃),获得了最佳的二茂铁的碳转化效率以及高结晶度的碳纳米管阵列.研究了不同热解温度下制备的碳纳米管微观形貌及其对场致发射性能的影响机制.场致发射实验测试表明在热解温度850℃条件下制备的碳纳米管冷阴极其开启电场(10μA/cm^(2))和阈值电场(1 mA/cm^(2))分别为1.32 V/μm和2.64 V/μm,最大电流密度为14.51 mA/cm^(2),对应的场增强因子为13267,表现出良好的场发射性能.本文提出的一步制备碳纳米管冷阴极阵列的制备方法无需任何蚀刻气体或光刻图案工艺,该方法安全、经济、可重复性好,在碳纳米管场发射冷阴极领域具有广阔的应用前景.

Effect of Substrate Temperature on the Selective Deposition of Diamond Films

Selective deposition of diamond film on patterned Si (100) substrates has been achieved by using microwave plasma chemical vapor deposition (MPCVD) method. The films have been characterized by scanning electron microscope (SEM) and Raman spectrum. The influence of substrate temperature on the nucleation behavior of diamond was discussed in detail and the optimized deposition condition has been obtained.

WC-Co硬质合金/CVD金刚石涂层刀具研究现状

化学气相沉积(Chemical vapor deposition,CVD)金刚石涂层刀具具有高硬度、优异的耐磨性、良好的冲击韧性和化学稳定性,能满足高效率、高精度的加工要求,逐渐成为切削铝和高硅铝合金、碳纤维增强复合材料及石墨等轻质量高强度难加工材料的主流涂层刀具。基于WC-Co硬质合金为基体的CVD金刚石涂层刀具在切削加工过程中容易发生CVD金刚石涂层的剥落,自主研发结合性能优良、长时间加工稳定的WC-Co硬质合金/CVD金刚石涂层刀具仍是该领域国内外发展的必然趋势。目前,研究者为了提高WC-Co硬质合金/CVD金刚石涂层刀具的结合性能,采用化学刻蚀法和机械处理法相结合去除WC-Co硬质合金基体表层中的Co粘结相,发现其能增强涂层与基体的结合强度,但基体表层Co粘结相含量的减少容易导致基体中形成脆化层,降低基体的强度和韧性。为了减少基体的强度和韧性损失,研究者在WC-Co硬质合金基体和金刚石涂层之间制备稳定的含Co中间化合物或沉积中间层,成功阻挡Co粘结相的热扩散。除了上述方法外,研究者还通过调控金刚石涂层工艺参数和结构,将微米晶与纳米晶金刚石层叠相结合,来提高金刚石涂层刀具的摩擦学性能和涂层与基体间结合强度。本文综述了WC-Co硬质合金/CVD金刚石涂层刀具的应用进展,明确了WC-Co硬质合金与CVD金刚石涂层间附着失效是刀具切削加工中最主要的失效形式,详细分析了影响附着失效的主要原因。在此基础上,着重介绍了各种优化工艺对增强涂层刀具性能影响的最新研究进展;指出了WC-Co硬质合金/CVD金刚石涂层刀具的性能受化学刻蚀、机械刻蚀、形成含钴化合物层、沉积中间层等基体前处理以及金刚石涂层工艺参数和结构的影响较大,对于不同牌号或不同厂家生产的同种牌号的WC-Co硬质合金基材,需要进行不同的表面前处理,而针对不同的切削加工材料,需要采用合适的金刚石涂层沉积工艺和结构以提高涂层与基材之间的结合强度,进而提高刀具的性能;最后提出了研制一种普适性强的基体前处理、涂层工艺和结构创新策略,以实现不同应用场景下WC-Co硬质合金/CVD金刚石涂层刀具的高效长寿命切削,可能是未来的研究方向。

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.

CVD金刚石涂层前预处理对硬质合金基体强度的影响

CVD金刚石涂层硬质合金刀具是有色金属及合金、石墨、陶瓷和碳纤维增强塑料(CFRP)等复合材料机械加工的理想刀具。但金刚石涂层前对WC-Co硬质合金基体的预处理过程在消除表面Co改善涂层附着力的同时也降低了基体强度。通过正交试验并采用SEM和EDS分析试样表面形貌和Co含量,采用XRD分析试样表层的相组成,研究了预处理对两种WC晶粒度的WC-6Co硬质合金基体强度的影响机制。结果表明:酸、碱预处理均显著降低基体强度,热处理则可消除酸碱处理对强度的不利影响。预处理对不同WC晶粒度的硬质合金基体强度的影响明显不同。粗晶硬质合金预处理后抗弯强度降低幅度更大,其抗弯强度的Weibull模数减小也更显著。相对而言,粗晶硬质合金的抗弯强度对酸腐蚀时间tC更敏感,而细晶硬质合金则受碱腐蚀时间tM的影响更大。因此,金刚石涂层前,应根据不同硬质合金基体的成分和微观结构匹配合适的预处理制度。

高速旋转垂直热壁CVD外延生长n型4H-SiC膜的研究

采用高速旋转垂直热壁化学气相沉积(CVD)设备在偏向〈1010〉晶向4°的n型4H-SiC衬底上进行了同质外延生长,在设定的工艺条件下,外延膜生长速率达到40.44μm/h,厚度不均匀性和掺杂浓度不均匀性分别达到1.37%和2.79%。AFM表征结果显示表面均方根粗糙度为0.11 nm;Leica显微镜观察显示外延膜表面光滑,生长缺陷密度很低,没有宏观台阶结构;Raman谱线清晰锐利,表现出典型的4H-SiC特征。综合分析表明,本实验使用国产的高速旋转垂直热壁CVD设备,在较高的外延生长速率下,获得了具有高厚度均匀性和高掺杂浓度均匀性的高质量4H-SiC外延膜,对目前碳化硅外延产业的发展和半导体设备的国产替代具有良好的指导作用。

雾化辅助CVD腔体的优化设计与实现

为了实现雾化辅助CVD(chemical vapor deposition,化学气相沉积)腔体的可定制性、可复用性及经济性,并满足高质量单晶氧化镓(Ga_(2)O_(3))薄膜制备的实际需求,设计开发了一种新型雾化辅助CVD腔体。该腔体主要由反应腔室模块、冷却模块和缓冲腔室模块组成。采用新型腔体和常规腔体进行了单晶Ga_(2)O_(3)薄膜制备实验,对Ga_(2)O_(3)薄膜进行了X射线衍射(X-ray diffraction,XRD)图谱分析,并采用原子力显微镜(atomic force microscope,AFM)观察其表面形貌。实验结果表明:采用新型腔体可制备出性能更优的α-Ga_(2)O_(3)、β-Ga_(2)O_(3)薄膜;采用新型腔体和常规腔体制备的α-Ga_(2)O_(3)薄膜的(006)晶面的半峰宽分别为0.172°、0.272°,表面粗糙度分别为25.6 nm和26.8 nm,可见采用新型腔体制备的α-Ga_(2)O_(3)具有更优的结晶度、表面平整性和致密度。通过新型腔体的设计,构建了更有利于单晶Ga_(2)O_(3)薄膜生长的稳定环境,为Ga_(2)O_(3)薄膜制备工艺的优化提供了可靠路径。研究结果为制备高品质金属氧化物半导体薄膜提供了参考。

CVD设备水冷循环系统的计算及设计

CVD设备水冷循环系统能防止材料在室壁上生长,使反应室得到充分及时地冷却,保证设备的安全运行。根据当前一种主流的CVD设备结构,对设备各冷却部件需要的冷却要求进行了分析计算,确定了各冷却支路需要的管径大小,提出了CVD设备水冷循环系统的结构设计方案,并根据实际运行结果验证了该水冷循环系统的合理性及可行性,满足CVD设备连续工艺对水冷循环系统的要求。

CVD SiC致密表面涂层制备及表征

考察了沉积温度、稀释气体流量对化学气相沉积(CVD)SiC涂层的显微结构及晶体结构的影响,分析得出:沉积温度为1100℃,稀释气体Ar流量<400mL/min时,制备的SiC涂层晶体结构完整、致密。在该制备工艺条件下沉积的SiC涂层密度为3.204g/cm3,显微硬度为HV4459.2,弹性模量为471GPa,涂层具有优异的光学加工性能,光学加工后表面粗糙度为0.429nm,能满足光学应用的要求。

红外用CVD ZnS多晶材料的研制

论述了制备红外用CVD ZnS多晶材料的化学气相沉积工艺和热等静压处理工艺。针对CVD ZnS多晶材料具备优良的光学和力学性能,采用化学气相沉积工艺和热等静压处理技术成功研制出大尺寸多晶材料,其最大尺寸达到250 mm×15 mm。测试了CVD ZnS样品的各项光学、力学性能指标。样品的全波段透过率均接近ZnS材料的本征水平,折射指数均匀性优于2×10-5,在1.06μm的吸收系数为2×10-3cm-1,抗弯强度达到104 MPa。