Synthesis of carbon nanotube array using corona discharge plasma-enhanced chemical vapor deposition

A corona discharge phasma-enhanced chemical vapor deposition with the features of atmospheric pressure and low temperature has been developed to synthesize the carbon nanotube array ,The array was synthesized from methane and hydrogen mixture in anodic aluminum oxide template channels in that cobalt was electrodeposited at the bottom.The characterization results by the scanning electron microscopy,transmission electron microscopy,energy dispersive X-ray spectroscopy and Raman spectroscopy indicate that the array consists of carbon nanotubes with the diameter of about 40 nm and the length of more than 4 μm, and the carbon anotubes are mainly restrained within the channels of templates.     

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.     

Synthesis of carbon nanotube arrays using ethanol in porous anodic aluminum oxide template

Carbon nanotube (CNT) arrays confined by porous anodic aluminum oxide (AAO) template were synthesized using ethanol as reactant carbon source at low pressure. Images by scanning electron microscope (SEM) and low magnification transmission electron microscopy (TEM) show that these CNTs have highly uniform outer diameter and length, absolutely controlled by the diameter and depth of nano-channel arrays of the AAO. High resolution transmission electron microscopy (HRTEM) imaging indicates that the graphitization of the CNT walls is better than the results reported on this kind of template-based CNT arrays, although it is not so good as that of multiwalled carbon nanotubes (MWCNTs) synthesized by catalysis. CNTs synthesized using acetylene as reactant gas show much less graphitization than those prepared using ethanol by comparing the results of HRTEM and Raman spectroscopy. The etchingeffects of decomposed OH radicals on the amorphous carbon and the roughness of AAO nano-channel arrays on the CNTs growth were employed to explain the graphitization and growth of the CNTs.     

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.     

Synthesis of ordered Si nanowire arrays in porous anodic aluminum oxide templates

Highly ordered polycrystalline Si nanowire arrays were synthesized in porous anodic aluminum oxide (AAO) templates by the chemical vapor deposition (CVD) method. The morphological structure, the crystal character of Si nanowire arrays and the individual nanowire were analyzed by the transmission electron microscopy (TEM), scanning electron microscopy (SEM), atom force microscopy (AFM) and the X-ray diffraction spectrum (XRD), respectively. It is shown that most fabricated silicon nanowires (SiNWs) tend to be assembled parallelly in bundles and constructed with highly orientated arrays. This method provides a simple and low cost fabricating craftwork and the diameters and lengths of SiNWs can be controlled, the large area Si nanowire arrays can be achieved easily under such a way. The curling and twisting SiNWs are fewer than those by other synthesis methods.     

Preparation of double-walled carbon nanotubes

Double-walled carbon nanotubes were prepared using the floating chemical vapor deposition with methane as carbon source and adding small amount of sulfur into the ferrocene catalyst. The optimized technological parameters are: the reaction temperature is 1200℃; the catalyst vapor temperature is 80℃; the flow rate of argon is 2000 SCCM; the flow rate of methane is 5 SCCM. The purified DWNTs under these optimized technological parameters have high purity above 90 wt%.     

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.     

采用热丝化学气相沉积法制备SiCN薄膜的研究

采用热丝化学气相沉积(HFCVD)系统,在单晶Si衬底上制备SiCN薄膜。所采用的源气体为高纯的SiH4,CH4和N2。用原子力显微镜(AFM)、X线衍射谱(XRD)和X线光电子能谱(XPS)对样品进行表征与分析。研究结果表明:SiCN薄膜表面由许多粒径不均匀、聚集紧密的SiCN颗粒组成;薄膜虽然已经晶化,但晶化并不充分,存在着微晶和非晶成分,通过Jade软件拟合计算出薄膜的结晶度为48.72%;SiCN薄膜不是SiC和Si3N4的简单混合,薄膜中Si,C和N这3种元素之间存在多种结合态,主要的化学结合状态为Si—N,Si—N—C,C—N,N=C和N—Si—C键,但是,没有观察到Si—C键,说明所制备的薄膜形成了复杂的网络结构。     

直流辉光放电等离子体增强化学气相法制备金刚石及氮化碳薄膜

采用直流辉光放电等离子体增强化学气相沉积(PECVD)技术方法 ,在Si(100)衬底上制备了金刚石薄膜 ,并在此基础上合成了含有少量晶态颗粒的非晶氮化碳薄膜     

碳纳米管的合成与制备

金属纳米颗粒和碳纳米管是两种重要的纳米材料,要实现碳纳米管的大批量制备,必须首先解决催化剂连续投放问题和催化剂与产物及时导出的问题.通过特殊的反应装置和工艺可以实现碳纳米管的连续制备,从而达到低成本大批量制备碳纳米管的目的.本文采用一个简单的方法合成了铁钴(Fe/Co)纳米颗粒,并采用化学气相沉积法实现了碳纳米管的批量合成,纳米颗粒的尺寸分布均匀,碳纳米管管径均匀、高纯度、结构完美.合成的碳纳米管机械强度高,同时还有独特的金属或半导体导电性.     

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.      

Synthesis of nano onion-like fullerenes by using Fe/Al2O3 as catalyst by chemical vapor deposition

Nano-carbon materials were synthesized by the catalytic decomposition of acetylene at 400℃ by using Fe/Al₂O₃ as catalyst. The product was refluxed in 36% concentrated HCl at 60℃ for 48 h in order to remove the catalyst support. The samples were examined by scanning and high resolution transmission electron microscopy, energy dispersive spectroscopy and X-ray diffraction. The results show that nano onion-like fullerenes encapsulating a Fe₃C core were obtained. These had a structure of stacked graphitic fragments, with diameters ranging from 15―50 nm. When the product was further heat- treated at 1100℃ for 2 h, nano onion-like fullerenes with a clear concentric graphitic layer structure were obtained. The growth mechanism of nano onion-like fullerenes encapsulating metal cores is suggested to follow a vapor-solid growth model.     

氧化热处理对不锈钢基碳纳米管结构及其电化学检测性能的影响

采用化学气相沉积法,以不锈钢基体中的Fe、Ni等成分为催化剂,直接在其表面生长碳纳米管并进行氧化热处理。采用场发射扫描电镜观察制备的碳纳米管形貌及尺寸,并采用接触角测量方法检测试样亲水性质,结合透射电镜、拉曼光谱和XPS检测分析氧化热处理引起的碳管形貌和特征差异,最后考察尿酸在碳纳米管电极上的电化学响应。结果表明,氧化热处理使碳纳米管平滑的表面变得粗糙,暴露出了更多的边平面结构,并且碳纳米管从疏水变为超亲水状态,使其在电化学反应过程中电极表面能够更好地与溶液中的物质接触,有利于材料电化学性能的提高;以经过氧化热处理的碳纳米管为电极,能够在大量抗坏血酸存在的条件下选择性地测定尿酸。     

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．     

压强对PECVD制备碳纳米管的影响

采用等离子体增强化学气相沉积技术(PECVD),以C2H2、H2和N2为反应气体,在镀Ni催化剂的Si基底上成功制备出多壁碳纳米管薄膜.并通过扫描电镜拍摄其表征,系统、深入地研究了沉积压强对碳管形貌的影响.结果表明:沉积压强对催化剂的刻蚀和碳纳米管薄膜的形成起着重要作用,获得定向性良好、分布均匀、密度适中的碳纳米管的最佳沉积压强是300 Pa.     

CoFe2O4纳米管的合成与表征

利用阳极氧化铝模板,用化学方法合成了CoFe2O4纳米管.X射线衍射结果表明,纳米管由无择优取向的、立方尖晶石结构的多晶CoFe2O4构成.电子显微镜显示,纳米管管径约300 nm,管壁厚度约100 nm,由约30 nm的CoFe2O4颗粒组成.进一步的磁性测量表明,纳米管阵列无明显的各向异性,其矫顽力约1 kOe,磁滞回线的方形度约0.37.     

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.     

催化剂的合成方法及配比对CVD法制备碳纳米管的影响

用离子注入法、简单混合法和水热晶化法分别制备了片状负载型系列、粉状混合型系列及粉状负载型系列催化剂.用3种系列催化剂通过CVD法分别制备了碳纳米管粗产物,用TEM和SEM检测手段对粗产物形貌进行了观察.结果表明,片状负载型催化剂:当Fe(Ⅱ)离子注入能量为25 keV、剂量为1×1016cm-2时其催化活性较高,制得的碳纳米管含量较多,管径均匀(约20 nm),但粗产物数量少;粉状混合型催化剂(Co/石墨):当纳米Co粉比例为15%时具有一定的催化活性,CVD法制备碳管有少量管径不一的碳管生成;水热法合成的粉状负载型催化剂(NiO/SiO2)分散性好、催化活性高,当硅-镍比为1:12时制备的碳纳米管含量高,管径细而均匀(10～16 nm),并且粗产物数量较多.     

Synthesis of LiFePO4 in situ vapor-grown carbon fiber （VGCF） composite cathode material via microwave pyrolysis chemical vapor deposition

One of the most important factors that limits the use of LiFePO 4 as cathode material for lithium ion batteries is its low electronic conductivity.In order to solve this problem,LiFePO 4 in situ vapor-grown carbon fiber (VGCF) composite cathode material has been prepared in a single step through microwave pyrolysis chemical vapor deposition.The phase,microstructure,and electrochemical performance of the composites were investigated.Compared with the cathodes without in situ VGCF,the initial discharge capacity of the composite electrode increases from 109 to 144 mA h g-1 at a 0.5-C rate,and the total electric resistance decreases from 538 to 66.The possible reasons for these effects are proposed.     

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.