Growth of carbon nanotubes directly on a nickel surface by thermal CVD

A simple method of growing carbon nanotubes directly on nickel substrate without chemical pretreatment is reported. It is demonstrated that carbon nanotubes growth is directly affected by the roughness on the surface. Carbon nanotubes density is large in each growth zone observed on the surface; these zones being spread sparsely for coarse roughness of the surface. The density of carbon nanotubes decreases and the number of growth zones increases as the roughness on the surface is reduced. The above trend was not affected with C₂H₂ flow time changing from 10 to 2 min. A similar result was obtained using a Ni alloy as substrate, but the effect of surface roughness on the growth of CNTs was less pronounced. The CNTs grown on the Ni alloy were free of amorphous carbon and uniformly distributed.     

Effect of fuel structure on synthesis of carbon nanotubes in diffusion flames

Carbon nanotubes (CNTs) were synthesized on nickel nitrate coated nickel foam in co-flow diffusion flames. Two different fuel structures, methane and ethylene, were used to synthesize CNTs. The effect of fuel structure on CNTs was systematically studied. Results showed that carbon nanomaterials, including nanotubes and nanofibers, were successfully synthesized in all conditions in methane flames, while, in ethylene flames, bamboo-like CNTs were synthesized in limited conditions. It was also found that carbon nanomaterials synthesized in ethylene flames had more defects than that of in methane flames. In addition, metal nickel nanoparticles acted as catalysts in the synthesis of CNTs, and carbon nanomaterials diameter was dependent on the catalyst particle size. Flame-synthesized CNTs were based on the vapor-liquid-solid mechanism, and a “recursive growth mechanism” for CNTs growth was proposed, which would be more conducive to the understanding of CNTs growth mechanism. This method offers another possibility for low-cost, large-scale synthesis of carbon nanomaterials.     

Application of the Taguchi analytical method for optimization of effective parameters of the chemical vapor deposition process controlling the production of nanotubes/nanobeads

Seven variable parameters of the chemical vapor deposition system have been optimized with the help of the Taguchi analytical method for getting a desired product, e.g., carbon nanotubes or carbon nanobeads. It is observed that almost all selected parameters influence the growth of carbon nanotubes. However, among them, the nature of precursor (racemic, R or Technical grade camphor) and the carrier gas (hydrogen, argon and mixture of argon/hydrogen) seem to be more important parameters affecting the growth of carbon nanotubes. Whereas, for the growth of nanobeads, out of seven parameters, only two, i.e., catalyst (powder of iron, cobalt, and nickel) and temperature (1023 K, 1123 K, and 1273 K), are the most influential parameters. Systematic defects or islands on the substrate surface enhance nucleation of novel carbon materials. Quantitative contributions of process parameters as well as optimum factor levels are obtained by performing analysis of variance (ANOVA) and analysis of mean (ANOM), respectively.     

Synthesis of individual ultra-long carbon nanotubes and transfer to other substrates

In this article, we report the synthesis of ultra-long carbon nanotubes (CNTs) by thermal chemical vapour deposition method. Ultra-long, individual and aligned CNTs were directly grown on a flat silicon substrate. The orientation of the nanotubes was found parallel to the gas flow direction. The ultra-long CNTs were grown with different transition metallic salts, such as nickel chloride, iron (III) chloride, cobalt acetate and ruthenium acetate, as the catalysts. The influence of the growth conditions, such as growth temperature, reactive gas flow on the length and alignment of the CNTs was studied in detail. By using different catalysts, ultra-long single-walled carbon nanotubes (SWCNTs) or multi-walled carbon nanotubes (MWCNTs) were successfully grown. These ultra-long CNTs were transferred to other substrates by two methods. (1) The first method is to use polydimethylsiloxane as a stamp. (2) The second method is to use KOH as an etching agent. The diameter and length of the CNTs were characterised by transmission electron microscope, scanning electron microscope, atomic force microscope and Raman spectroscopy. The results indicate that the length of the CNTs can reach up to 4?mm. The diameter of the SWCNTs is in the range of 0.7–2.1?nm and the diameter of the MWCNTs is approximately 150?nm.     

Nano-octopus: a new form of branching carbon nanofiber

A new multibranched octopus-type structure of carbon nanofibers is synthesized from a natural precursor, camphor, by a thermal chemical vapor deposition technique. An alloy of Cu:Ni catalyst is prepared by electrochemically coating nickel on a copper sheet, with nickel sulfate as an electrolyte, and heating that nickel-coated copper sheet to a higher temperature. Deposition of carbon on these substrates leads to the formation of a branched nanostructure in the temperature range of 923 K to 1023 K. The fiber diameter increases from 30 nm to 250 nm with increasing pyrolysis temperature. Detailed morphology and the internal structure of these fibers are studied by scanning and transmission electron microscopy.     

Synthesis of carbon nanotubes using SBA-15 as a template by the reaction of methane and carbon dioxide

Multiwalled carbon nanotubes (CNTs) were synthesized using Ni loaded mesoporous SBA-15 as a template by reaction of methane and carbon dioxide. The influences of nickel content on the selectivity and crystallinity of CNTs were investigated. It can be seen that the crooked CNTs with a diameter varied from 9.9, 12.5 to 36.5 nm with creasing content of Ni from 5, 15, and 30 wt%/SBA-15. A uniform diameter and good quality CNTs were obtained in our system.     

Carbon nanotubes synthesis in microwave plasma torch at atmospheric pressure

Well aligned multi-walled carbon nanotubes were synthesized at atmospheric pressure using a microwave plasma torch on silicon substrates with silicon oxide buffer layer and catalyst overlayer in the mixture of argon, hydrogen and methane. Iron or nickel was used as catalysts. The optimum substrate temperature for the deposition on Si/SiO₂/Fe substrates was about 970 K. In this case SEM micrographs of the deposits revealed a presence of vertically aligned nanotubes with the diameters around 15 nm. TEM micrographs showed a presence of amorphous carbon particles in the samples and some defects in the wall structure of the produced nanotubes. In Raman spectra two peaks at 1332 and 1584 cm⁻¹ were observed. The CNTs were also synthesized on the substrates without SiO₂ buffer layer but their quality was lower. The synthesis with Ni instead of Fe catalyst required lower temperature and the alignment of the nanotubes was worse. The deposition process was monitored by optical emission spectroscopy. Atomic lines of hydrogen and argon, an emission of CN due to a presence of nitrogen impurities from atmosphere, a weak molecular band of CH and strong C₂ emission were detected in the spectra.     

Chemical vapor deposition of carbon nanotube layers on aluminum foil

A novel technique has been demonstrated for direct chemical vapor deposition of carbon nanotubes (CNTs) on aluminum foil. It has been shown that the foil surface acquires catalytic properties after being held in an aqueous nickel nitrate solution for a certain time. CNTs were deposited by the catalytic pyrolysis of ethanol vapor. The hybrid materials thus prepared have the form of aluminum foil coated with “carbon wool” from CNTs on both sides. The layers have good adhesion to the aluminum substrate, which allows it to be deformed without causing the CNT layer to peel off. Such material is potentially attractive, in particular, for the fabrication of supercapacitors.     

Synthesis of CNTs via ethanol decomposition over ball-milled Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> coated copper sheets

Carbon nanotubes (CNTs) were synthesized on ball-milled Fe₂O₃ coated copper sheets by the catalytic decomposition of ethanol vapor at 650°C. TEM, SEM, and EDX revealed the presence of 30–50 nm diameter multiwalled carbon nanotubes with catalytic particles at their tips. CNTs, α-Fe, and Fe₃C were detected by XRD. Raman and TG analyses show that the product is CNTs with less than 10 wt % residues. The carbon yield was the maximum at 354 wt %. The text was submitted by the authors in English.     

The effect of temperature on the growth of carbon nanotubes on copper foil using a nickel thin film as catalyst

Growth of carbon nanotubes (CNTs) on bulk copper foil substrates has been achieved by sputtering a nickel thin film on Cu substrates followed by thermal chemical vapor deposition. The characteristics of the nanotubes are strongly dependent on the Ni film thickness and reaction temperature. Specifically, a correlation between the thin film nickel catalyst thickness and the CNT diameter was found. Two hydrocarbon sources investigated were methane and acetylene to determine the best conditions for growth of CNTs on copper. These results demonstrate the effectiveness of this simple method of directly integrating CNTs with highly conductive substrates for use in applications where a conductive CNT network is desirable.     

氮掺杂碳纳米管的无金属催化剂合成和表征

采用爆炸辅助化学气相沉积法, 以碳纳米管(CNTs)作催化剂, 三聚氰胺作碳源和氮源, 无金属催化剂合成出氮掺杂碳纳米管(CN_x). 通过TEM、EDS、Mapping、XPS、Raman和TG测试手段对CN_x进行了表征. 结果表明, CNx具有竹节状结构, 其掺氮量高达17at%, 且氮元素分布均匀. 氮元素以石墨型和吡啶型掺杂在石墨层中, 由于大量氮元素掺杂造成纳米管石墨化程度降低, 抗氧化能力减弱.     

燃料和基板对火焰法制备一维碳纳米材料的影响

以乙醇、甲醇及液化石油气为碳源，低碳钢及含Ni合金钢等为基板，采用火焰法成功地制备出了一维碳纳米材料，包括碳纳米管（CNTs）和一种新的“实心”碳纳米纤维（CNFs）。利用场发射枪高分辨扫描电镜（SEM）、透射电镜（TEM）和激光Raman光谱对碳纳米材料的结构进行了表征。发现基板材料决定燃烧生成物的性质，含Fe元素及其化合物的基板材料倾向于合成“实心”碳纳米纤维，而含Nj元素及其化合物的基板材料倾向于合成“空心”的碳纳米管，认为这是由于碳与Fe的亲和力比Ni大而造成的。不同碳源对一维碳纳米材料的形态也有影响，这与它们的含碳量和燃烧热等不同有关。     

堇青石载镍催化剂对燃烧合成碳纳米管的影响

借助于硝酸镍溶液, 利用浸渍法在堇青石表面均匀负载镍催化剂颗粒, 在甲烷扩散火焰中活化并催化生成碳纳米 管. 实验结果表明, 生成的多壁碳纳米管直径为30～50nm, 长度约为十几微米, 空腔比较小, 管壁石墨结晶结构良好.提高浸渍液浓度, 催化剂颗粒尺寸明显变大, 但对碳纳米管的形态影响比较小. 延长浸渍时间, 可使催化剂颗粒密度提高, 碳纳米管出现成束生长现象. 结合碳管成核生长过程和火焰燃烧的特点, 探讨了催化剂对于碳纳米管生长的影响机制.     

Direct synthesis of Y-junction carbon nanotubes by microwave-assisted pyrolysis of methane

Both Y-junction carbon nanotubes and individual carbon nanotubes were synthesized without any additive catalyst by microwave decomposition of methane. Detailed microstructures of as-synthesized products have been characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman spectroscopy. The results show that these Y-junction CNTs possess an internal bamboo-shaped structure, and some three dimensional multi-terminal junctions are also observed on CNTs. As gas flow rate decreased to 15 sccm, only individual nanotubes could be obtained. A possible mechanism is proposed for the synthesis of the Y-junction carbon nanotubes on these observations. This technique may also have great potential in making other nano-structured carbon materials on a large scale and at low cost.     

Synthesis and characterization of carbon nanotubes via ultrasonic spray pyrolysis method on zeolite

Ultrasonic spray pyrolysis method for the synthesis of carbon nanotubes (CNTs) has been investigated with zeolite supporting material. Single wall carbon nanotubes (SWCNTs) were obtained at 850 °C in nitrogen environment. Such deposition system makes it possible to grow CNTs without reducing agent at atmospheric pressure in a simple setup. Iron and cobalt acetate were used as catalyst and ethanol as carbon source for the synthesis of CNTs. Results show that nature of zeolite and cobalt concentration play important roles for SWCNTs production. Interestingly, we notice that in catalyst particles of sharp shape, nucleation of a nanotubes cap occurs dominantly in the forward direction.     

乙醇催化燃烧法制备竹节形碳纳米管

乙醇催化燃烧法可以方便的制备出碳纳米管和碳纳米纤维。介绍采用该方法制备出一种独特的竹节形的碳纳米管，利用乙醇作为碳源和燃料，提供材料生长所需的能量；利用Cu薄片作为基底；利用FeCl3或Fe（NO3）3作为催化剂先体。通过扫描电子显微镜（SEM），透射电子显微镜（TEM），对黑色絮状的沉积产物进行表征。实验结果表明，产物中的碳纳米管具有较好的竹节形结构。实验也表明制备的竹节形碳纳米管的形貌和微结构与其独特的制备条件有关，如：火焰的抖动，催化剂先体溶液的浓度，制备时间等。并对竹节形碳纳米管的形貌和生长机制进行了详细的讨论。     

Cold-wall CVD carbon nanotube synthesis on porous alumina substrates

Carbon nanotubes were synthesized by chemical vapor deposition (CVD) using ethanol vapor as carbon source. Catalysts were Co and Mo metallic particles obtained from the corresponding acetates dissolved in ethanol. Acetate solutions are deposited on porous alumina substrates by dip coating. A dense array of aligned carbon nanotubes perpendicular to the substrate surface grow with 20 min exposure to ethanol vapor flow for substrate temperatures between 650 and 830 °C. Sample analysis is performed with scanning electron microscopy and Raman spectroscopy.     

碳纳米管对Fe-P非晶的力学性能和晶化行为影响的研究

采用快速凝固技术制备了碳纳米管／铁碳非晶复合材料,并对其组织、力学性能和热稳定性进行了研究检测结果表明,碳纳米管在非晶基体中的弥散存在,使得非晶抗拉强度提高,晶化激活能增加,晶化特征温度明显提高,加入２Ｗ／％碳纳米管,使铁磷非晶的室温抗拉强度提高了１２０％,晶化激活能增加了约４０％,晶化开始温度提高了约１００Ｋ,此外,在温度高于其晶化温度约２００Ｋ时,碳纳米管和非晶基体界面间发生了固相反应。     

Solvent-free microwave-assisted synthesis of tenorite nanoparticle-decorated multi-walled carbon nanotubes

Copper-decorated carbon nanotubes (CNTs) have important applications as precursors for ultra-conductive copper wires. Tenorite-decorated CNTs (CuO-CNTs) are ideal candidates and are currently developed using laborious processes. For this reason, we have developed a facile and scalable method for the synthesis of CuO-CNTs from copper acetate. It was found that the optimal loading of copper acetate onto the CNTs was 23.1 wt% and that three 1-minute microwave treatments were sufficient for the decomposition of copper acetate to copper oxide. The loading of copper oxide onto the nanotubes was confirmed using X-ray photoelectron spectroscopy, energy-dispersive X-ray spectroscopy and thermogravimetric analysis. The materials were characterised using X-ray diffraction and scanning electron microscopy.     

Self-assembled interconnection by bamboo-like carbon nanotubes

Carbon nanotubes (CNTs) could be formed on Si substrate using nickel catalyst under microwave plasma-enhanced chemical vapor deposition system. Under the high, negative-bias voltage (−400 V) condition, we found the formation of the carbon nanotube islands and the bamboo-like carbon nanotube interconnection lines. Most of the bamboo-like carbon nanotubes connected with the carbon nanotubes themselves, which indicates the self-assembled characteristics of the carbon nanotube interconnection lines. The self-assembled characteristics of the bamboo-like carbon nanotube interconnection lines were evaluated using computer-aided image analysis.