改进化学气相沉积法在炭纤维表面生长碳纳米管(英文)

采用一种改进的化学气相沉积法在炭纤维表面制备碳纳米管。为了提高炭纤维表面的润湿性能,炭纤维在浸渍之前先在CVD设备中在真空下973 K的高温处理,然后在硝酸和浓硫酸体积比为3∶1的混合酸中酸处理30 min。而改进的化学气相沉积法关键在于让催化剂的还原步骤和碳纳米管的生长步骤同时进行。这样通过减小过渡金属元素与炭纤维之间的接触时间从而降低了它们之间的相互扩散,在确保了炭纤维本身的力学性能下降程度明显小于用普通化学气相法制备的情况下生长出长且茂密的碳纳米管阵列。另外,经过对工艺参数的优化发现当用乙醇作溶剂,Fe(NO3)3.9H2O溶度为100 mmol/L,氢气和碳源气体比值为4/1,而生长时间为30 min时得到最好的碳纳米管阵列。     

Synthesis of carbon nanowalls by hot-wire chemical vapor deposition

Carbon nanowall (CNW) is a carbon nano-material which has a wall structure that stood on substrates. CNWs can be synthesized by hot-wire chemical vapor deposition (HWCVD) using methane without hydrogen dilution. The synthesis of CNWs by HWCVD is discussed along with reviewing the experimental results. The growth of CNWs is affected by hydrogen dilution ratio and substrate surface temperature. Based on these results, it is suggested that hydrogen radical density and substrate surface temperature are the important parameters for the synthesis of CNWs. The growth process of CNWs is also discussed.     

Synthesis and characterization of carbon spheres prepared by chemical vapour deposition

Carbon spheres, with uniform diameters of about 1 μm, have been achieved via Chemical vapour deposition (CVD). The fabricated materials have been fully characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray analysis (EDX). The results show that the spheres are 95% carbon. The formation mechanism of carbon spheres has also been discussed.     

Synthesis of carbon nanofiber films and nanofiber composite coatings by laser-assisted catalytic chemical vapor deposition

Uniform carbon nanofiber films and nanofiber composite coatings were synthesized from ethylene on nickel coated alumina substrates by laser-assisted catalytic chemical vapor deposition. Laser annealing of a 50 nm thick nickel film produced the catalytic nanoparticles. Thermal decomposition of ethylene over nickel nanoparticles was initiated and maintained by an argon ion laser operated at 488 nm. The films were examined by scanning electron microscopy and by transmission electron microscopy. Overall film uniformity and structure were assessed using micro-Raman spectroscopy. Film quality was related to the experimental parameters such as incident laser power density and irradiation time. For long irradiation times, carbon can be deposited by a thermal process rather than by a catalytic reaction directly over the nanofiber films to form carbon nanocomposite coatings. The process parameters leading to high quality nanofiber films free of amorphous carbon by-products as well as those leading to nanofiber composite coatings are presented.     

Synthesis and characterization of indium nitride nanowires by plasma-assisted chemical vapor deposition

High-quality indium nitride (InN) nanowires were synthesized in a high temperature furnace on Au-coated Si substrates through the reaction of indium metal vapor with highly reactive nitrogen radicals generated by N₂ plasma. Highly-reactive nitrogen radicals provided a wide process window for the synthesis of InN nanowires by lowering the process temperature to avoid the decomposition of InN. X-ray diffraction, transmission electron microscopy and Raman spectra further showed that the as-synthesized InN nanowires were perfect single crystallites of wurtzite structure with the growth direction along [110].     

Characterization and cytocompatibility of carbon layers prepared by photo-induced chemical vapor deposition

We studied the preparation of the carbon layers on polytetrafluoroethylene (PTFE) by chemical vapor deposition from acetylene induced by UV-excimer lamp. Their surface properties and chemical structure were characterized by Atomic Force Microscopy, Scanning Electron Microscopy, Raman spectroscopy, Rutherford Backscattering Spectrometry, Elastic Recoil Detection Analysis, X-ray Induced Photoelectron Spectroscopy and others. The deposited layers could be characterized as hydrogenated amorphous carbon (a-C:H) containing additional oxygenic structures and conjugated double bonds. The cytocompatibility of the samples was tested with using of human umbilical endothelial cells (HUVEC). In comparison with pristine PTFE, the deposition resulted in drastically increased adhesion and proliferation of HUVEC.     

Multi-walled carbon nanotube growth on oxidized silicon substrates using cyclohexane precursor by chemical vapor deposition

Randomly oriented multi-walled nanotubes (MWNTs) are grown by a thermal chemical vapor deposition (CVD) process from cyclohexane precursor on a 20% copper-80% nickel (Cu-Ni) catalyst on oxidized silicon substrates. This combination of precursor and catalyst, to our knowledge, has been employed for the first time to demonstrate growth of multi-walled carbon nanotubes. The effects of annealing, gas ambient and catalyst layer thickness on the morphology of the grown carbon layers are discussed. The low resistivity values of the MWNTs grown on oxidized silicon substrates are attractive for their potential use in photonic devices and display applications.     

乙炔热裂解沉积对PAN基炭纤维性能的影响

利用有机溶剂去除PAN基炭纤维表面的集束剂与染剂.然后通过乙炔热裂解沉积对其进行表面改性,以期获得兼具高机械强度和优良导电性的高性能PAN基炭纤维.采用SEM、AFM、XRD、Raman等方法对PAN基炭纤维在改性前后的微观结构、结晶性、抗拉强度、弹性模量、导电性等进行了分析.研究结果表明采用化学气相沉积法可以提高或者明显改善石墨化处理后的PAN基炭纤维的力学性能(抗拉强度为2GPa,弹性模量为270GPa)和导电性(5×10-4Ω·cm).     

定向碳纳米管的化学气相沉积制备法

报道了一种简便有效的合成定向碳纳米管 (CNTs)的化学气相沉积 (CVD)制备方法。以铁为催化剂 ,乙炔为碳源 ,采用单一反应炉 ,直接在石英基底上沉积催化剂颗粒薄膜 ,成功合成了定向性好、管径均匀的高质量大密度的碳纳米管     

Synthesis of multi-walled carbon nanotubes by microwave plasma-enhanced chemical vapor deposition

Microwave plasma-enhanced chemical vapor deposition (MW-PECVD) has been employed to synthesize carbon nanostructures by using Fe (or Co, Ni)/γ-Al₂O₃ as catalysts and a mixture of benzene, hydrogen, and argon as precursors. By regulating the types of catalyst, the microwave incident power, the ratio and flux of the precursors, many morphologies such as ordinary geometric, helix-shaped, and planar spiral carbon nanotubes with aspect ratios of 100–1000 have been observed. Furthermore, two novel nanostructures, which are probably the missing link between onion-like carbon particles and nanotubes, have also been obtained. The striking feature of this new approach is the low synthesis temperature (<520°C) due to the non-equilibrium characteristic of microwave plasma operated at low pressure, which is crucial for some fascinating applications.     

Synthesis of sulfur-doped carbon nanotubes from sulfur powder using chemical vapor deposition

Sulfur-doped carbon nanotubes (SCNT) with high sulfur contents have been prepared using chemical vapor deposition (CVD) from sulfur powder, acetylene gas and Fe/CaCO₃ (as catalyst). In this regard, various growth's temperatures were examined to investigate its effects on the structure and the sulfur content of prepared SCNT. The best condition was obtained at 700°C and using 4 g of sulfur powder. The product was characterized using FE-SEM and EDS, which showed rode-like SCNT with about 40 nm diameter and 10.75% sulfur content. Moreover, TEM, Raman and XPS analyses were employed to obtain more details related to the product. The XPS results confirmed the presence of sulfur atoms, which covalently incorporated in the carbon framework. Finally, the catalytic ability of the product in oxygen evolution reaction was examined and the results showed high stability and low oxygen production rate for this product.     

Quantitative elucidation of the rapid growth and growth saturation of millimeter-scale vertically aligned carbon nanotubes by hot-filament chemical vapor deposition

We report the rapid synthesis of millimeter-long vertically-aligned carbon-nanotubes (VACNTs) by hot-filament chemical-vapor-deposition without the use of water vapor. The growth rate increased initially up to ~ 190 μm/min but decreased thereafter resulting in the growth of up to 2.2 ± 0.2 mm in 23 ± 2 min. A thermodynamic model driven by a carbon-concentration gradient can account for very rapid initial growth with Arrhenius-type exponential temperature dependence. Another model devised for the quantitative elucidation of the monotonic decrease in growth-rate and quasi saturation of VACNT growth confirmed that the growth kinetics of VACNTs are controlled by the concomitant contribution of a diffusion-limited precursor supply and reaction-driven catalyst deactivation.     

热化学气相沉积法在硅纳米丝上合成碳纳米管

利用热化学气相沉积法在负载不同厚度催化剂的硅纳米丝(SiNW)表面生长碳纳米管(CNTs),探讨了生长条件对所合成SiNW-CNT的结构和场发射特性的影响.这种类似树状的三维结构具有较高碳纳米管表面密度及降低的电场筛除效应等潜在优势.使用拉曼光谱( Raman)、电子显微镜(SEM)、透射电子显微镜(TEM)、能量扩散分光仪(EDS)分析了碳纳米管的结构性质,并在高真空下施加电场测得碳纳米管的场发射特性.结果表明:随硅纳米丝上负载催化剂镍膜厚度的变化,所合成碳纳米管的表面特性、结晶结构及功函数改变,导致电子发射难易程度的改变,进一步影响碳纳米管的场发射特性.     

Preparation and characterization of carbon molecular sieves from chestnut shell by chemical vapor deposition

In this study, carbon molecular sieves (CMS) were produced from chestnut shell by chemical activation process followed by chemical vapor deposition (CVD) of methane. The influences of deposition temperature (800–900?°C), time (15–60?min) and flow rate of CH₄ (100–300?mL/min) on pore development of carbon molecular sieve were investigated. The produced CMSs were characterized by several techniques such as N₂ adsorption, CO₂ adsorption, CH₄ adsorption, elemental analysis, FTIR analysis and SEM analysis. The textural analysis of the CMS samples showed the successful deposition of methane on pores of the produced activated carbon derived from chestnut shell to yield a microporous CMS with a narrow pore size distribution. The deposition temperature, time and flow rate of CH₄ were shown to strongly affect the pore structure of the CMS. The maximum CO₂ adsorption capacity (525.7?mg/g) was obtained at a deposition temperature of 850?°C, time of 30?min, and CH₄ flow rate of 100?mL/min.     

乙炔催化裂解制备碳纳米带及其结构表征

以乙炔（C2H2）为碳源,铁为催化剂,通过化学气相沉积技术在单晶硅衬底上制备了碳纳米带.采用场发射SEM、TEM、激光Raman光谱等先进分析手段对其形态和结构进行了表征.研究发现：碳纳米带是一种准二维材料,厚度约30nm,宽度在几百纳米,长度在100μm量级.碳纳米带的碳层沿着与其生长轴方向一致的（002）晶向排列,碳层的边缘都弯曲折叠成封闭结构.碳纳米带中碳层的排列不很平直,其中存在大量的层错.由此认为碳纳米带可用于能源等领域.     

沉积条件对CVD碳纤维生长的影响

用CH4、H2或包含NH3的混合气体为反应气体,利用负偏压增强热丝化学气相沉积方法在沉积有过渡层(Ta或Ti)和催化剂层(NiFe)的Si衬底上制备碳纤维,并用扫描电子显微镜研究了它们的生长和结构,结果发现不同的沉积条件对碳纤维的生长和结构有很大的影响。在无辉光放电的条件下,衬底温度较低时碳纳米管或纤维生长困难;提高衬底温度,能够弯曲生长;在辉光放电的条件下,则呈现定向生长的特点。     

A chemical method to graft carbon nanotubes onto a carbon fiber

A simple method is developed for grafting carbon nanotubes (CNTs) onto a carbon fiber surface. CNT and carbon fiber undergo an oxidation treatment. Oxidation generates oxygen, like carboxyl, carbonyl or hydroxyl groups, or amine groups on nanotubes and carbon fiber surface. Functionalized CNTs are dispersed in a solvent and deposited on carbon fibers. The bonds between CNT and carbon fiber are operated by esterification, anhydridation or amidization of the chemical surface groups. The resulting materials are characterized by scanning electron microscopy (SEM). CNTs form a 3D network around the carbon fibers. Likewise, CNT bonding between two fibers is observed.     

Hot-wire chemical vapor deposition of carbon nanotubes

Hot-wire chemical vapor deposition (HWCVD) has been employed for the continuous gas-phase generation of both carbon multi-wall and single-wall nanotube (MWNT and SWNT) materials. Graphitic MWNTs were produced at a very high density at a synthesis temperature of 600 °C. SWNTs were deposited at a much lower density on a glass substrate held at 450 °C. SWNTs are typically observed in large bundles that are stabilized by tube–tube van der Waals’ interactions. However, transmission electron microscopy analyses revealed only the presence of isolated SWNTs in these HWCVD-generated materials.     

Temperature effect on synthesis of different carbon nanostructures by sulfur-assisted chemical vapor deposition

The temperature effect on synthesizing different carbon nanostructures in the range of 820−1020 °C by sulfur-assisted chemical vapor deposition is investigated. When the growth temperature is no more than 900 °C (e.g. 820, 860, and 900 °C), carbon onions can be obtained, accompanying with some fishbone-like carbon nanofibers (CNFs), graphite sheet and carbon nanotubes (CNTs). When the growth temperature is increased to 940 °C or above (e.g. 980 and 1020 °C), the products are mainly CNTs. Furthermore, by comparing the nitrogen adsorption-desorption results of samples obtained with and without sulfur addition at each temperature, it is found that the specific surface area (SSA) of products can be remarkably enlarged after introducing small amount of sulfur during growth. This is favorable to their applications in areas like electrodes of supercapacitors, adsorbents, catalyst supports, and so on.     

Physical activation and characterization of multi-walled carbon nanotubes catalytically synthesized from methane

A series of treatment processes were employed to purify and then physically activate the multi-walled carbon nanotubes obtained using catalytic decomposition of methane. In order to characterize and compare the activation effect, the carbon fibers were also treated by the same activation processes. The results showed that the normal physical activation by CO₂ or steam has not too much effect on the surface area of purified multi-walled carbon nanotubes, in particular, the carbon nanotubes were burned when using the poignant activation conditions. However, the surface area of carbon fibers availably etched in the same activation processes is much increased. In addition, the mechanisms of physical activation on multi-walled carbon nanotubes and carbon fibers have been investigated.