常压化学气相沉积ZrC涂层动力学与组织结构

以ZrCl4-CH4-H2-Ar为反应体系,采用常压化学气相沉积(APCVD)法在1 473～1 873 K制备ZrC涂层,用X线衍射和扫描电镜分析涂层的相成分、ZrC晶粒择优生长及微观形貌,研究ZrC涂层沉积动力学和涂层组织结构.研究结果表明:随沉积温度的升高,APCVD ZrC涂层的沉积速率增大,ZrC微晶表观尺寸也相应增大;1 473～1 673 K沉积时,化学气相沉积过程的表观活化能为71.69 kJ/mol,沉积过程由化学动力学控制;1 673～1 873 K沉积时,过程的表观活化能为14.28 kJ/mol,沉积过程由扩散控制.沉积温度由1 473 K上升至1 673 K时,ZrC晶粒的择优生长取向出〈220〉转变为〈200〉,ZrC涂层组织为典型的针状晶结构,涂层较疏松、粗糙;1 873 K沉积时,ZrC晶粒呈短柱状,ZrC涂层致密平整,且沉积速率最高.     

流化床-化学气相沉积法制备金属涂层包覆燃料颗粒

含有Nb、Zr、W等金属包覆层的包覆型燃料颗粒是一种新型的燃料元件形式,在核工业中有重要应用。该文利用流化床-化学气相沉积(FB-CVD)法,制备得到了含有金属包覆层的新型包覆颗粒,研究了热态输运与冷态输运2种方式对金属卤化物前驱体的载带,最终成功制备得到了纯相金属Nb与金属Zr包覆层。实验结果表明,金属包覆层可有效提升包覆颗粒整体的力学性能。该文还研究了沉积温度、前驱体输运、包覆层氧化等不同因素对沉积速率的影响。结果表明:CVD制备的金属包覆层可有效提升包覆颗粒整体的压碎强度,但抗氧化性较差,不适用于直接在氧化环境下制备与使用,可作为包覆颗粒的中间涂层。     

等离子化学气相沉积硬膜技术研究

用等离子体化学气相沉积（ＰＣＶＤ）技术制备了ＴｉＮ、ＴｉＣ、Ｔｉ（ＣＮ）和（ＴｉＳｉ）Ｎ膜及其组合的多层膜。ＰＣＶＤ具有很好的覆盖性，ＰＣＶＤ－ＴｉＮ具有很好的耐磨、蚀性，膜与基体结合良好，因而用ＰＣＶＤ法在高速钢刀具、模具及轴承上沉积ＴｉＮ可大大提高其使用寿命。ＰＣＶＤ－ＴｉＮ和Ｔｉ（ＣＮ）膜无明显柱状晶，其显微硬度高于ＴｉＮ亦可用于高速钢刀具、模具上提高其使用寿命。ＰＣＶＤ－（ＴｉＳｉ）Ｎ，晶     

微波等离子体化学气相沉积合成TiN超细颗粒

热力学计算表明，Ｈ２，Ｎ２的过量有助于提高ＴｉＮ的产率，但能耗也相应增加。为此考察了温度，流量，ＴｉＣｌ４携带量，混合方式对产物性能的影响。结果表明，流量增加，温度升高，ＴｉＣｌ４携带量增加，混合愈好，则产物粒径愈小。在此基础上采用微波等离子体化学气相沉积法，合成了粒径为１２３－２８４ｎｍ的ＴｉＮ超细颗粒     

硬质合金上化学气相沉积Tic和TicxNy的研究

在TiCl_4-C_6H_5CH_3-H_2和TiCl_4-C_6H_5-H_2-N_2体系中,以YG_8硬质合金为基体,用化学气相沉积(CVD)法,研究了温度,反应物输入浓度对沉积TiC和TiC_xN_y涂层的沉积速度,显微硬度和形貌的影响。结果表明:TiC沉积速度,显微硬度随沉积温度升高而增大,对TiC沉积层的形貌也有较大的影响。TiC和TiC_xN_y的沉积速度、显微硬度随反应物摩尔比(m_c/Ti)增加到某一最大值后又下降;m_c/Ti=1时,TiC硬度呈最佳值。m_c/Ti=0.87时,TiC_xN_y硬度出现最大值。此外,还对基体一涂层间是否出现η相进行了分析。并测定了在1223～1323K间TiC沉积反应的表观活化能为157.9kJ/mol。     

化学气相沉积金刚石薄膜的表面过程

采用简单表面反应模式，对化学气相沉积金刚石薄膜的表面动力学过程进行了研究，得到了金刚石薄膜的沉积速率公式，揭示了影响薄膜生长的因素并由此讨论了金刚石薄膜生长的机制和规律。     

无氢化学气相沉积碳化钛

本文介绍了一种新的化学气相沉积碳化钛方法。用此法对几种常用的工具材料进行了沉积处理,并用金相观察、X射线结构分析、X射线光谱显微分析等手段测定了碳化钛沉积层的组织、结构和性能。应用此法于模具和某些易磨损机件上可较大地提高机件的使用寿命,且方法本身安全、经济,在一般的热处理设备条件下即能进行。     

沉积位置对化学气相沉积SiC涂层微观组织的影响

利用化学气相沉积法在C／C复合材料表面制备了SiC涂层，并借助扫描电子显微镜和X射线衍射等手段对不同位置沉积产物的微观形貌、相组成以及厚度进行了测试，推导出了沉积位置与反应气源过饱和度的定性关系，分析了反应气源过饱和度对SiC涂层形貌、晶粒尺寸以及涂层厚度的影响．研究结果表明：沿着沉积炉内气体流动的方向，反应气源的过饱和度逐渐降低，沉积所得pSiC涂层形貌由颗粒状向须状转变，晶粒尺寸与涂层厚度逐渐减小。     

高温气冷堆包覆燃料颗粒的化学气相沉积

我国正在建造１０ＭＷ高温气冷堆，包覆燃料颗粒的研制是高温气冷堆的关键技术之一。ＴＲＩＳＯ型包覆燃料颗粒是由燃料核芯、疏松热解碳层、内致密热解碳层、碳化硅层和外致密热解碳层组成。采用化学气相沉积方法，选用乙炔、丙烯、甲基三氯硅烷和氢气作为反应气体，在直径为５５ｍｍ锥形流化床包覆炉中制备包覆燃料颗粒。本文系统地研究了工艺参数和性能之间的关系，摸索出疏松热解碳层、致密热解碳层和碳化硅层的最佳包覆工艺条件，总结出经验公式，用扫描电镜观察了包覆燃料颗粒的微观结构，制备出满足设计要求的ＴＲＩＳＯ型包覆燃料颗粒。     

Chemical vapor deposition growth behavior of graphene

The optimized growth parameters of graphene with different morphologies,such as dendrites,rectangle,and hexagon,have been obtained by low-pressure chemical vapor deposition on polycrystalline copper substrates.The evolution of fractal graphene,which grew on the polycrystalline copper substrate,has also been observed.When the equilibrium growth state of graphene is disrupted,its intrinsic hexagonal symmetry structure will change into a non-hexagonal symmetry structure.Then,we present a systematic and comprehensive study of the evolution of graphene with different morphologies grown on solid copper as a function of the volume ratio of methane to hydrogen in a controllable manner.Moreover,the phenomena of stitching snow-like graphene together and stacking graphene with different angles was also observed.     

碳化锆/锆涂层炭纤维的制备及其拉伸性能研究

在一定反应温度范围内以熔盐为介质通过炭纤维与金属锆反应制备出碳化锆/锆涂层炭纤维,并在反应温度为800℃时,研究反应时间对碳化锆/锆涂层炭纤维表面相组成、形貌及其拉伸性能的影响。结果表明,800℃可制备均匀致密的碳化锆/锆涂层;且随着反应时间的延长,碳化锆/锆涂层厚度略有增加;涂层后炭纤维的拉伸强度和拉伸模量比原炭纤维的相应值略有减小。     

Catalyst enhanced chemical vapor deposition of nano-particle nickel films on teflon surface

Films formed with nanosized nickel particles on teflon surface were prepared by means of catalyst enhanced chemical vapor deposition (CECVD) with Ni(dmg)₂, Ni(acac)₂, Ni(hfac)₂, Ni(TMHD)₂, and Ni(cp)₂ as precursors, and complexes Pd(hfac)₂, PdCl₂ and Pd(η ³-2-methylallyl)acac as catalyst under carrier gas (H₂). The film growth rate depends on the precursors and substrate temperature. The chemical value, purity and surface morphology of the Ni particle films were characterized by X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The films obtained were shiny with silvery color, and consisted of grains with a particle size of 50–140 nm. The Ni was metallic of which the purity was about 90%–95% from XPS analysis. SEM micrograph showed that the film had good morphology.      

温度对氮化锆膜微观性能的影响研究

本文以直流脉冲离子源辅助中频磁控溅射方式,在常温和低热条件下在玻璃衬底上制备氮化锆膜,通过扫描电镜和纳米压痕仪对薄膜的表面形貌、显微硬度、表面粗糙度的变化情况进行了研究。结果表明：增加薄膜的沉积温度,导致膜层硬度的降低;膜层中晶粒尺寸增大;微观粗糙度增加;晶粒之间的间隙明显减小;晶粒之间出现明显的镶嵌现象。     

单源化学气相沉积法制备In2O3纳米线

以乙酰丙酮合铟[In（acac）3]（acac=acetylacetonate）作为单源前驱体,Au为催化剂,采用化学气相沉积法,于较低温度（550℃）下成功制得了In2O3纳米线．用X射线粉末衍射（XRD）、扫描电镜（SEM）、透射电镜（TEM）和能量分散光谱（EDS）对In2O3纳米线进行了表征;制得的In2O3纳米线具有单晶结构,平均直径约为80nm,长度达十几微米,其生长服从气一液一固机理．光致发光研究发现,In2O3纳米线在483nm处有一个强的发射峰,这可归因于氧空位的存在．     

Well-aligned carbon nanotube array membrane synthesized in porous alumina template by chemical vapor deposition

A new simple approach was devetoped for preparing wetl-aligned and monodispersed carbon nanotube (CNT) array membrane within the cylindrical pores of anodic aluminum oxide (AAO) template by chemical vapor deposition (CVD). Acetylene and hydrogen were used in the CVD process with Fe-catalyzer at 700°C under 250 Pa. Scanning etectron microscope (SEM) and transmission etectron microscope (TEM) were employed to characterize the resulting highly-oriented uniform hollow tube array which had a diameter of about 250 nm, a tube density of 5.3x10⁸ cm² and a length of about 60 μm. The length and diameter of the tubes depend on the thickness and pore diameter of the template. The growth properties of the CNT array film can be achieved by controlling the structure of the template, the particle size of Fe-catalyzer, the temperature in the reactor, the flow ratio and the deposition time. The highly-oriented and uniform CNT array membrane fabricated by this simple method is very much useful in a variety of applications.     

合成参数对MOCVD法生长氧化锌纳米针的影响

使用脉冲液滴注入式MOCVD,在金膜裹覆的MgO(100)衬底上于500℃合成氧化锌纳米针.纳米针为晶态并且在XRD谱线上主要呈现ZnO的4个衍射强峰(100)、(002)、(101)及(004).金没有起到催化剂的作用,在较薄(2.4nm)金膜上生长的纳米针密度较高且直径较小.500℃是ZnO纳米针较佳的合成温度,在温度不低于550℃时合成的是片状ZnO.每周期前驱体的注入剂量对纳米针的形貌有显著影响.充足的注入剂量(6.8mg/周期)能够保证纳米针合成,而较低的注入剂量(3.4mg/周期)将会合成较短且直径较小的纳米针.     

Progress of graphene growth on copper by chemical vapor deposition: Growth behavior and controlled synthesis

Recently,chemical vapor deposition (CVD) on copper has been becoming a main method for preparing large-area and highquality monolayer graphene.In this paper,we first briefly introduce the preliminary understanding of the microstructure and growth behavior of graphene on copper,and then focus on the recent progress on the quality improvement,number of layers control and transfer-free growth of graphene.In the end,we attempt to analyze the possible development of CVD growth of graphene in future,including the controlled growth of large-size single-crystal graphene and bilayer graphene with different stacking orders.     

化学气相淀积反应器内TiCl_4氧化反应动力学

采用原位红外测试技术,在线观测了化学气相淀积反应器内TiCl_4的均相氧化反应。捕获了两种重要活性中间体TiCl_3和TiOCl_2,从而导出该反应的机理模型。并采用尾气红外定量分析方法得到了TiCl_4氧化反应的动力学方程及反应活化能。反应活化能:66.8 kJ/mol,指前因子:2.45×10~2/s。