化学气相沉积技术和无机膜

综述了化学气相沉积技术在无机分离膜领域中的应用和发展近况，报道了作者所在实验室近几年来的研究进展，并从无机分离膜的超薄化、实用化出发，列举了该领域有待进行的科学和技术基础研究课题。     

射频等离子体化学气相沉积择优取向膜的研究

用射频等离子体沉积择优取向的ＴｉＮ膜，用Ｘ－衍射的方法分析影响取向的原因。     

化学气相沉积金刚石膜的光学性质

多晶金刚石膜的光学性质与工艺参数密切相关．采用一较为完备的金刚石透过率模型，研究了一系列金刚石膜在中远红外区的光学性质．并得出了不同衬底预处理方法和反应室中甲烷分压对CVD膜的平均透过率、表面粗糙度、非金刚石相含量、各种成分的吸收系数等光学性质的影响，计算结果与实测结果一致．     

CVD金刚石膜反应器内气相化学的理论研究进展

综述CVD金刚石膜沉积过程中反应器内气相化学的理论研究进展,阐述不同条件下反应器内的气相化学反应模型、反应机理及各种数值仿真方法,总结这些气相反应的选取及所对应的动力学机理。研究结果表明:CVD金刚石膜反应器内的气相化学是一个十分复杂的过程,与双碳组元相比,单碳组元对膜沉积的贡献较大,在组元C2H2,C2,CH3,C和CH中,决定膜生长的组元由具体操作条件而定。对CVD金刚石膜反应器内气相化学的研究结果不但可以为探讨膜生长机理的表面化学提供准确输入,还可为高效、优质膜的获得提供理论依据。     

中频等离子体化学气相沉积法制备ZnO薄膜

ZnO是一种多功能材料,目前处于世界范围的研究热潮中。为了拓展和改善ZnO的应用,采用中频等离子体化学气相沉积法(MF-PCVD)制备了ZnO薄膜,并研究了衬底温度对晶型和成膜速率的影响．     

用热解化学气相沉积方法合成金刚石膜

众所周知,金刚石不仅是最好的超硬耐磨材料,而且也是一种理想的功能材料。 1976年苏联科学家Derjaguin等人用化学输运反应方法首次在非金刚石衬底上合成出金刚石膜,1981年Spitsyn等人对该金刚石膜的合成机理进行了探讨。由于低压法合成金刚石可以在大面积的各种衬底上沉积出粒状或膜状金刚石,因此它将为金刚石在电子工业,光学工业和空间技术等重要领域的广泛应用开拓了崭新的局面。     

放电电流对热阴极等离子体化学气相沉积金刚石膜影响

建立了快速沉积高品质金刚石膜的热阴极辉光放电等离子体化学气相沉积新方法. 相对于常规冷阴极辉光放电而言,热阴极辉光放电是一种新型放电形式,具有许多新的特性,其中重要一点是具有较高的放电电流(6.0～10.0 A). 较高的放电电流既是热阴极辉光放电本身的突出特点,同时对于化学气相沉积金刚石膜工艺也产生重要影响. 实验研究了放电电流于金刚石膜沉积速率、表面形貌和热导率的影响,发现由于放电电流影响辉光放电的等离子体区和阳极区,进而对金刚石膜的沉积速率和品质有很大影响. 特别是通过放电电流的提高,可以有效地提高金刚石膜的品质,这对于制备优质金刚石膜产品有重大意义.     

化学气相沉积（CVD）金刚石薄膜的主要制备方法及应用

介绍了化学气相沉积金刚石薄膜的主要制备方法：热灯丝法、微波法、等离子体喷射法、火焰燃烧法。 Ｃ Ｖ Ｄ 金刚石膜的应用。     

化学气相沉积法制备碳纳米管及场发射性质的研究

讨论了化学气相沉积法制备碳纳米管的方法及过程,通过扫描电子显微镜(SEM)和透射电子显微镜(TEM)发现制备的碳纳米管的外直径在30-100nm之间;在10-5Pa高真空的条件下测定了碳纳米管薄膜的场发射性质,并比较了样品的老炼过程对场发射性质的影响.     

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     

化学浴沉积法制备纳米氧化亚铜薄膜

用改进后的化学浴沉积法制备了纳米Cu2O薄膜,并对成膜条件及膜的性能进行了研究．结果表明：化学浴沉积法改进后有利于制备高质量的纳米Cu2O薄膜;最佳反应温度为60～70C,此温度范围内Cu2O薄膜的膜厚随着循环次数线性增加．制备的薄膜纯度较高．表面较平整和致密,Cu2O粒径为14～22nm,其禁带宽度为2．01eV．     

铁-钴复合粉体的化学沉积法制备

化学镀易于控制金属相的含量,工艺简单、成本低廉,得到的镀层均匀且与基体结合力好,是制备高性能的复合粉末的一种有前途的方法.本文采用化学镀的方法,在铁粉表面包覆一层金属钴,既对原铁粉进行表面改性,又制备了钴包铁复合粉末.实验结果表明：在pH值为8,氯化钴为25 g/L,次亚磷酸钠为25 g/L,柠檬酸钠为25 g/L,硫酸铵为63 g/L时,15 g/L的铁粉装载量可以得到最佳的镀覆效果.     

Synthesis of few layer single crystal graphene grains on platinum by chemical vapour deposition

The present competition of graphene electronics demands an ef fi cient route which produces high quality and large area graphene. Chemical vapour deposition technique, where hydrocarbons dissociate in to active carbon species and form graphene layer on the desired metal catalyst via nucleation is considered as the most suitable method. In this study, single layer graphene with the presence of few layer single crystal graphene grains were grown on Pt foil via chemical vapour deposition. The higher growth temperature changes the surface morphology of the Pt foil so a delicate process of hydrogen bubbling was used to peel off graphene from Pt foil samples with the mechanical support of photoresist and further transferred to Si O2/Si substrates for analysis. Optical microscopy of the graphene transferred samples showed the regions of single layer along with different oriented graphene domains. Two type of interlayer stacking sequences, Bernal and twisted, were observed in the graphene grains.The presence of different stacking sequences in the graphene layers in fl uence the electronic and optical properties; in Bernal stacking the band gap can be tunable and in twisted stacking the overall sheet resistance can be reduced. Grain boundaries of Pt provides low energy sites to the carbon species, therefore the nucleation of grains are more at the boundaries. The stacking order and the number of layers in grains were seen more clearly with scanning electron microscopy. Raman spectroscopy showed high quality graphene samples due to very small D peak. 2D Raman peak for single layer graphene showed full width half maximum(FWHM) value of 30 cm-1. At points A, B and C, Bernal stacked grain showed FWHM values of 51.22, 58.45 and 64.72 cm-1, while twisted stacked grain showed the FWHM values of 27.26, 28.83 and 20.99 cm-1,respectively. FWHM values of 2D peak of Bernal stacked grain showed an increase of 20–30 cm-1 as compare to single layer graphene which showed its dispersive nature and con fi rmed Bernal sequence. On the other hand, the slightest decrease in FWHM values of 2D peak in twisted grain comparing to single layer con fi rmed the twisted sequence of grains. Atomic force microscopy analysis showed an increasing trend in grain height pro fi le with an increase in the number of layers.     

玻璃陶瓷基板上铜薄膜的化学气相沉积

使用低介电常数基板和高电导率、高抗电迁移的金属Cu进行布线,可以提高高密度电子封装的传输速度和可靠性。采用乙酰丙酮铜作为前驱体,在常压下利用化学气相沉积技术对玻璃陶瓷基板进行Cu薄膜金属化。利用热重分析、X射线衍射和扫描电子显微镜等技术对前驱体、Cu薄膜进行分析观察。结果表明:影响Cu导体的电阻的主要因素是沉积温度。在温度为290～310℃,N2气流量为200～350mL/min和H2气流量为450～600mL/min的条件下,获得了致密的Cu薄膜,Cu导体方块电阻为25mΩ。     

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.      

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．     

Fabrication of copper nanorods by low-temperature metal organic chemical vapor deposition

Copper nanorods have been synthe-sized in mesoporous SBA-15 by a low-temperature metal organic chemical vapor deposition (MOCVD) employing copper (II) acetylacetonate, Cu(acac)2, and hydrogen as a precursor and reactant gas, re- spectively. The hydrogen plays an important role in chemical reduction of oganometallic precursor which enhances mass transfer in the interior of the SBA-15 porous substrate. Such copper nanostructures are of great potentials in the semiconductor due to their unusual optical, magnetic and electronic properties. In addition, it has been found that chemically modi- fying the substrate surface by carbon deposition is crucial to such synthesis of copper nanostructures in the interior of the SBA-15, which is able to change the surface properties of SBA-15 from hydrophilic to hydrophobic to promote the adsorption of organic cupric precursor. It has also been found that the copper nanoparticles deposited on the external sur- face are almost eliminated and the copper nanorods are more distinct while the product was treated with ammonia. This approach could be achieved under a mild condition: a low temperature (400℃) and vac-uum (2 kPa) which is extremely milder than the con- ventional method. It actually sounds as a foundation which is the first time to synthesize a copper nanorod at a mild condition of a low reaction temperature and pressure.     

离子束辅助沉积制备氮化钽薄膜

利用离子束辅助沉积（ＩＢＡＤ）技术制备ＴａＮ薄膜；掠入谢的Ｘ射线衍射和透射电镜观察结果显示，薄膜晶粒细小、结构致密，是面心立方结构。     

化学法制备高纯碲过程中杂质元素脱除的热力学分析

通过对Te(Ⅳ)-Pb(Ⅱ)-Cu(Ⅱ)-As(Ⅲ)-H2O和Te(Ⅳ)-MeS-H2O系热力学分析,得到溶液中Te(Ⅳ),Pb(Ⅱ),Cu(Ⅱ)和As(Ⅲ)离子总浓度与溶液pH值、温度以及溶液中S2-浓度的关系。热力学分析结果表明:采用硫化物沉淀法可以深度净化Na2TeO3溶液,去除其中大部分重金属离子及砷离子,确定理论上去除Na2TeO3溶液中Pb(Ⅱ),Cu(Ⅱ)和As(Ⅲ)离子的最佳pH值为11左右。采用硫化物沉淀法对Na2TeO3溶液中Pb(Ⅱ),Cu(Ⅱ)和As(Ⅲ)离子的净化实验验证了热力学分析的正确性,通过实验使粗TeO2中的Pb,Cu和As杂质的质量分数由0.273 0%,0.165 9%和0.280 0%分别降低到3.24×10-4%,1.00×10-4%和1.30×10-3%,但S2-浓度过量对As的去除不利。实验确定硫化沉淀法去除杂质离子的最佳条件是:pH=11,温度为373 K,反应时间为50 min。     

CVD法制备SiO2薄膜工艺条件的研究

在Al2 O3 陶瓷基片上以正硅酸乙酯 (TEOS)为原料 ,高纯氮气作载气 ,采用低压冷壁式设备和化学气相沉积(CVD)方法制备SiO2 薄膜 ,研究了基片温度、TEOS温度和沉积时间对SiO2 薄膜沉积速率的影响 .采用XRD ,XPS和SEM技术对SiO2 薄膜的组成和结构进行了分析