微波等离子体化学气相沉积法低温制备直纳米碳管膜

Among the three main methods for the synthesis of carbon nanotubes (CNTs)， chemical vapor deposition (CVD) has received a great deal of attention since CNTs can be synthesized at significantly low temperature. Plasma chemical vapor deposition methods can synthesize CNTs at lower temperature than thermal CVD. But in the usual catalytic growth of CNTs by CVD， CNTs are often tangled together and have some defects. These will limit the property research and potential applications. How to synthesize the straight CNTs at low temperature becomes a challenging issue. In this letter， straight carbon nanotube (CNT) films were achieved by microwave plasma chemical vapor deposition (MWPCVD) catalyzed by round Fe-Co-Ni alloy particles on Ni substrate at 610℃. It was found that， in our experimental condition， the uniform growth rate along the circumference of round alloy particles plays a very important role in the growth of straight CNT films. And because the substrate is conducting， the straight CNT films grown at low temperature may have the benefit for property research and offer the possibility to use them in the future applications.     

微波等离子体化学气相沉积法低温合成纳米碳管

纳米碳管的低温合成是纳米碳管合成的一个重要研究方向。在众多的合成方法 中,化学气相沉积法,特别是等离子体化学气相沉积法在纳米碳管的低温合成方面 意义重大。本研究利用溶胶-凝胶法结合等离子体还原,获得了负载在SiO_2上的纳 米金属钻颗粒。以甲烷为碳源、氢气为载气,在纳米金属钴颗粒的催化作用下,利 用微波等离子体化学气相沉积法在低于500 ℃ 的温度条件下合成了纯度较高的纳 米碳管。     

纳米碳管电极的制备与电化学检测性能研究

纳米碳管由于其独特的物理和化学性能及广阔的应用前景而备受关注,其相关研究涉及到众多领域[1￣3]。在电化学分析领域,与其它碳电极材料相比,纳米碳管电极具有较大的电极表面积和较高的电子传递速率,其使用能增大响应电流、降低检出限,是目前电化学分析电极中一个十分引人注目     

活性炭上化学气相沉积法生长纳米碳纤维

利用流化床技术,以天然气为碳源,负载于活性炭上的纳米镍粒子为催化剂,在750 ℃下采用化学气相沉积法制备了气相生长纳米碳纤维(VGCNFs)/活性炭(AC)复合物。通过对样品进行XRD、激光拉曼光谱、扫描电镜和氮吸附检测,发现VGCNFs生长在活性炭的各个侧面上,以顶部生长模式为主,纤维的直径在40～120 nm之间,由于粗糙的纤维表面和石墨片层的翘曲而缺陷较多。VGCNFs/AC复合物与原料活性炭相比,BET比表面积从2 367 m²·g^-1降到了1 474     

MWPCVD低温合成纳米碳管的生长机理

The synthesis of carbon nanotubes (CNTs) at low temperature has received a great deal of attention and be-comes a challenging issue. But few model which accounts for the growth of CNTs is suited for the synthesis of CNTs by microwave plasma chemical vapor deposition (MWPCVD) at low temperature because most researchers conclude that the growth mechanism is determined by the catalyst-supporter interaction while ignored the diffusion of carbon in the catalyst. In this paper, under the catalytic effect of cobalt supported by SiO₂ and Al₂O₃, CNTs are synthe-sized by MWPCVD at about 500℃, and tip-growth, the model which accounts for the catalytic growth of CNTs is outlined. It is the temperature difference between the upper and bottom of the catalytic particle that results in the diffusion of carbon atoms from upper to the bottom, and precipitation of saturated carbon on the bottom surface to form CNTs.     

化学气相沉积法制备氧化锡自组装纳米结构

采用化学气相沉积法在镀有5-10 nm厚金膜的SiO2衬底上, 通过控制生长条件, 实现了二氧化锡纳米结构的自组装生长, 成功制备出了莲花状和菊花状的二氧化锡自组装纳米结构. 利用扫描电子显微镜、X射线衍射等表征分析手段对样品的表面形貌、结构及成份进行表征和研究. 并在此基础上, 讨论了两种自组装纳米结构的生长机制.     

化学气相沉积法制备氮化钛

本文以氮化钛的CVD制备为例,说明了源物质的选择对CVD过程的影响.在此基础上,综述了化学气相沉积技术在材料制备领域的最新进展.     

含钴介孔分子筛催化热解乙醇制备纳米碳管

以CTAB为模板剂,硅酸钠、氯化钴为原料,通过水热法合成含钴介孔分子筛(Co-MCM-41)。以所合成的Co-MCM-41做催化剂,采用化学气相沉积(CVD)法催化热解乙醇制备纳米碳管。通过XRD、FT-IR、TEM、N2吸附-脱附和Raman光谱等分析手段对所合成的介孔分子筛和纳米碳管进行了表征。结果表明:合成的Co-MCM-41样品具有MCM-41的介孔结构,比表面积较大且介孔有序性较好。以所合成的含钴介孔分子筛催化热解乙醇制备出管径均匀、管壁较厚、顶端开口的多壁纳米碳管。     

纳米碳管的制备及其在化学电源中的应用

本文介绍了纳米碳管制备技术的最新研究成果，并对其嵌锂行为，储氢及电催化性能进行了重点讨论，纳米碳管作为一种新型的纳米电极材料，有可能在锂离子电池，镍氢电池，燃料电池等化学电源中得到广泛的应用。     

催化剂活性组分及温度对化学气相沉积法制备碳纳米管的影响

通过XRD、DTA和TEM方法 ,研究了不同温度下催化剂活性组分Co和Ni对化学气相沉积(CVD)法制备碳纳米管的影响。结果表明 ,在最佳反应温度 ( 65 0℃ )下 ,碳纳米管在催化剂Co Al2 O3 上的产率为 45 7g 1 0 0g·cat,高于在Ni Al2 O3 上的产率 3 42g 1 0 0g·cat。XRD分析表明 ,相对于催化剂Co Al2 O3 ,在Ni Al2 O3 上制备的碳纳米管石墨化程度更高。当合成温度从 65 0℃增加到 75 0℃时 ,在催化剂Co Al2 O3 和Ni Al2 O3 上生成的多壁碳纳米管的 ( 0 0 2 )晶面的层间距分别从 3 45 和 3 42 减小到 3 3 9 和3 3 7 。进一步分析发现 ,在焙烧或催化反应过程中 ,Co、Ni与γ Al2 O3 之间存在相互作用且生成了新相物质 ,其衍射峰分别为 2θ=5 1 5 6°和 2θ=5 1 97°     

Synthesis of Carbon Nanotubes by Catalytic Chemical Vapor Deposition Using Hydrogen Storage Alloy as A Catalyst

Carbon nanotubes, which was discovered by Iijima1 in 1991, is the most typical one-dimensional nano-material with the micrometers order in length and nanometers order in diameter. CNTs are composed of graphitic sheets rolled into closed concentric cylinders, and classed into single wall nanotubes and multi-wall nanotubes. CNTs can offer many significant advantages over most existing materials. Since its discovery, unprecedented interest has been stimulated because of its significance both in…     

Structural Study of Micro and Nanotubes Synthesized by Rapid Thermal Chemical Vapor Deposition

The structures of micro and nanotubes obtained by pyrolysis of hydrocarbons, hold onto silicon (Si) substrates, are reported in this work. The tubes fabrication experiments were carried out by Rapid Thermal Chemical Vapor Deposition (RTCVD) using propane (C₃H₈) as carbon (C) precursor. Selection of parameters such as temperature of deposition, vacuum conditions or surface cleaning leads to the creation of tubular structures. Transmission electron microscopy (TEM), scanning electron microscopy (SEM), selected area electron diffraction (SAED) and energy dispersive X-ray measurements (EDX) are the microbeam techniques that allow to characterize the tubes found in the studied specimens. Different tube configurations such as isolated nanorods, Y-type junctions or fiber-like layers are evidenced. Metallic catalysis seems to be the mechanism involved in the wires formation since Fe particles are present inside the CNT tubes. Other poly-crystalline inclusions are also evidenced by SAED. The composition of the nanotubes changes from tip to tail in an amorphous matrix. The growth mechanisms leading to tube formation are described.     

An Investigation of the Plasma Composition in Plasma-enhanced Hot Filament Catalytic Chemical Vapor Deposition of Carbon Nanotubes

A mixture of acetylene, hydrogen and ammonia (C₂H₂/H₂/NH₃) is used to produce carbon nanotubes (CNTs) by a plasma-enhanced catalytic chemical vapor deposition process either without (PE CCVD) or with hot filaments-assistance (PE HF CCVD). A mathematical model based on Chemkin^™ computer package is used for analyzing specific conditions of nanotube synthesis. Simulations are compared with optical emission spectroscopy (OES) measurements. Morphological and structural investigations on the grown carbon nanostructures are also performed using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). It was shown that the significant change in the density and the morphology of the CNTs grown in the presence of NH₃ could be mainly explained by the gas phase formation of CN and HCN. Both species display a high etching activity, whereas the species C, CH, CH₂, CH₂(S), C₂ and C₂H are expected to be the most probable carbon nanotube precursors.     

纳米CaCO3负载过渡金属CVD法制备多壁碳纳米管的研究

以纳米碳酸钙粉体为载体,用浸渍法制备了可用于化学气相沉积(CVD)法制备碳纳米管的高产率催化剂.应用FESEM,HRTEM,TEM,XRD和激光拉曼谱对产物进行了表征.结果表明,由于纳米碳酸钙具有较大的比表面积,可高密度地承载催化剂活性组分.在碳纳米管生长初期,处于缓慢分解状态的纳米碳酸钙才能有效地起到载体作用,且反应温度为700～750℃时,碳纳米管的产率较高.Fe-Co双金属催化剂在700℃,催化生长60min后,可增重10倍,而且产物中无定形碳含量极少.纳米碳酸钙载体易于提纯,用质量分数为30%的硝酸超声提纯粗产品1h,可使纯度提高到97%,且不破坏碳纳米管结构.     

催化辅助爆炸法合成碳纳米管

报道了以三硝基苯酚(苦味酸,C₆H₃N₃O₇)、乙酸钴[Co(Ac)₂]和菲(C₁₄H₁₀)作为爆炸物,通过热引发方式使其在不锈钢耐高压容器中发生爆炸反应来制备多壁碳纳米管.利用TEM,HRTEM和XRD等手段对碳纳米管和催化剂的形貌和结构进行表征,综合TEM和TG测试结果确定产物中碳纳米管的含量.结果表明,随着反应条件的变化,可获得外径分布在20～40nm范围内,管长为数十微米的多壁碳纳米管.金属钴催化剂在爆炸过程中原位生成.苦味酸装填密度的增大有利于碳纳米管含量的提高,优化条件(苦味酸的装填密度为0.2g/cm³)后碳纳米管的含量可达70%左右.     

不同碳源催化化学气相沉积制备自支撑C/Ni-Fiber复合电极材料的电容脱盐性能

以甲烷、乙烯、乙醇和正丁醇为碳源,通过催化化学气相沉积在具有三维开放网络结构的烧结8μm-Ni金属纤维上沉积碳的方法,制备了以金属Ni纤维网络为集流极、沉积碳为离子存储库的薄层大面积自支撑C/Ni-fiber复合电极材料.用扫描电子显微镜（SEM）、透射电子显微镜（TEM）、热重分析（TGA）、X射线衍射（XRD）、N₂-吸脱附等温线和循环伏安与电化学阻抗谱对电极材料进行了表征,并考察了其作为电极的电容脱盐性能.乙烯、甲烷、正丁醇和乙醇为碳源的沉积碳形态分别为鱼骨状碳纳米管（CNTs）、石墨烯面取向与轴平行的CNTs、棒状和蠕虫状碳纳米纤维（CNFs）.C/Ni-fiber复合电极材料对NaCl的电吸附容量顺序为:乙烯>正丁醇>甲烷>乙醇,这与复合电极的电化学特性、孔结构和碳的纳米结构相关.在1.2 V的工作电压下,以乙烯为碳源制备的C/Ni-fiber复合电极材料对水溶液中NaCl(100 mg·L^-1)的电吸附容量达159μmol·g^-1.     

微波等离子体辅助化学气相沉积法低温合成定向碳纳米管阵列

自碳纳米管被发现以来[1] ,这种准一维纳米新材料由于其优异的力学、电学、储氢等理化性质而显示出非常重要的理论研究与实际应用价值[2 ,3] .碳纳米管阵列更可作为场致发射器件 ,有望应用于冷阴极平板显示器或纳米电子学等前沿领域[4 ] ,成为碳纳米管研究中的热点 .在已有报道的多种制备碳纳米管阵列的方法中 ,以孔性硅或孔性 Al2 O3作为模板剂 ,通过化学气相沉积制备的方法较为普遍[5～ 7] ,但此类方法往往需要在较高温度 (高于 70 0℃[6 ,7] )下进行 ,对于碳纳米管阵列最诱人的应用前景之一平板显示器而言 ,要求在显示玻璃表面直接生长…     

分叉碳纳米管的催化生长

Branching carbon nanotubes were synthesized by pyrolysis of acetylene at 700℃ over oxygen-free copper and γ-Al₂O₃-supported Cu unitary or Cu/Fe binary catalysts. The morphologies of the as-grown products were charac-terized by transmission electron microscopy. The results indicated that the branching structures were closely related to the Cu component of the catalysts. We proposed that the special electronic structure (3d¹⁰4s¹) of Cu play the crucial role in the formation of the heptagon defects related to the branching structures.