Multi-walled carbon nanotubes produced by hydrogen DC arc discharge at elevated environment temperature

Multi-walled carbon nanotubes (MWCNTs) were synthesized by hydrogen DC arc discharge at elevated environment temperature. The sample collected from the soot on the inner wall of the arc discharge furnace was investigated using TEM, HRTEM and X-ray diffraction. The results show that environment temperature has a significant effect on the formation of MWCNTs in the soot in hydrogen atmosphere as well as the diameter of the tubes. When environment temperature in the furnace is higher than about 500 °C, MWCNTs can be formed on the furnace walls with a great quantity.     

Synthesis of high quality single-walled carbon nanotubes by arc discharge method in large scale

Single-walled carbon nanotubes (SWNTs) were synthesized by a novel method. The dc arc discharge in H₂-Ar gas atmosphere with Fe₃O₄ as catalyst was used. The morphology and structures of the as-prepared SWNTs were characterized by SEM, HRTEM and Raman spectroscopy techniques. The results indicated that this new catalyst could be used to produce SWNTs with high purity and yield in large scale. The purity and yield of the SWNTs synthesized from these new catalysts were affected by the mixture buffer gas. Based on the overall ease and low-cost advantages of these new catalysts, these results suggest a potential opportunity for cost-effective and commercial production of SWNTs.     

Synthesis of carbon nanotubes by arc discharge in open air

In this work Carbon nanotubes have been synthesized by arc discharge in open air. A TIG welding ac/dc inverter was used as the power source for arc discharge. During each run of the arc discharge based synthesis, the anode was a low purity (approximately 85% C by weight) graphite rod. The effect of varying the atmosphere on the yield of soot of the carbon nanotube containing carbon soot has been studied. Various soots were produced, purified by oxidation and characterized to confirm formation of carbon nanotubes and their relative quality, using transmission electron microscopy, Raman spectroscopy, and XRD. It was found that the yield of soot formed on the cathode is higher when synthesis is carried out in open air than when carried out in a flowing argon atmosphere. When synthesized in open air, using a 7.2-mm-diameter graphite rod as anode, the yield of soot was around 50% by weight of the graphite consumed. Current and voltage for arcing were at identical starting values in all the experiments. This modified method does not require a controlled atmosphere as in the case of a conventional arc discharge method of synthesis and hence the cost of production may be reduced.     

Coral-like amorphous carbon nanotubes synthesized by a modified arc discharge

A coral-like amorphous carbon nanotube was prepared by a modified arc discharging furnace in hydrogen atmosphere with a mixture of Mo-Co₂O₃-Mg powders as catalyst at 600°C. This carbon nanotube presented a microscopic coral-like by SEM observation and amorphous structure of nanotubes by HRTEM observation. The XRD diffraction and Raman pattern presented noncrystal characteristics compared to the normal graphite structure. We believed that these results may be affected by the “synergistic” effect of catalyst, atmosphere, and temperature in the synthesis process. The possible explanations to the formation mechanism of this novel carbon nanotube have also been proposed.     

不同压力下碳纳米管的电弧法合成及其表征

采用电弧放电法在氦气/乙炔混合气氛中,在不同压力下合成了碳纳米管.运用场发射扫描电镜、场发射透射电镜、X-射线衍射仪和拉曼光谱对碳纳米管的形貌进行了表征.采用可见发射光谱对碳纳米管的形成过程进行了原位诊断研究.场发射扫描电镜结果表明,在氦气/乙炔气氛中合成的碳纳米管的长度大于50微米,许多碳颗粒沉积在碳纳米管壁上.场发射透射电镜结果表明,在0.100MPa下合成的碳纳米管的壁厚明显大于0.035MPa下合成的碳纳米管的壁厚.可见发射光谱诊断结果表明,CH和C2物种可能作为碳纳米管形成的前驱体,其中,以H原子作为无定形炭的刻蚀物种.阳极消耗速率和产物在阴极的沉积速率随着反应器中压力的增加而增加.因此,可以通过加强阳极和乙炔的蒸发速率及CH和C2物种的沉积速率而增加碳纳米管的形成速率.     

Catalyst effect on the preparation of single-walled carbon nanotubes by a modified arc discharge

Single-walled carbon nanotubes (SWCNTs) were prepared by a modified arc discharge furnace using 500?Torr helium as buffer gas at 600?°C. The effect of the catalyst type on the production of SWCNTs was studied by transmission electron microscopy, X-ray diffraction and Raman spectroscopy. The experimental results indicated that the catalyst composition plays an important role in the production rate and purity of the SWCNTs product. Fe-Ni-Mg and Co-Ni powder catalysts demonstrated excellent catalytic effect at a catalyst content of 3?wt%. The soot production rate was up to 15?g/hr and the mean diameter of SWCNTs was about 1.3?nm.     

电弧放电法制备煤基炭纳米纤维及开口竹节状碳纳米管

以中国白杨树无烟煤为原料,添加一定量煤焦油和沥青黏结剂制成炭棒作为阳极,采用直流电弧法制备竹节状碳纳米管及炭纳米纤维.用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、能量散射谱(EDS)和X射线衍射(XRD)等技术对产物进行表征.结果表明:在较低氦气压力下(0.020MPa),采用不添加任何催化剂的无烟煤基炭棒进行电弧放电,在剩余阳极上制备得到竹节状碳纳米管和炭纳米纤维.所得竹节状碳纳米管多为开口状,直径在50nm左右;炭纳米纤维宏观上成绒毛球形,纤维的直径在30nm～50nm之间.     

The preparation of carbon nanotubes by dc arc discharge using a carbon cathode coated with catalyst

Carbon nanotubes (CNTs) were grown using a dc arc discharge process and relevant process parameters were investigated. Unlike the usual process in which a carbon anode is filled with metal catalyst powder, CNTs were prepared using a carbon cathode on which the metal catalyst had been deposited using an electroplating system. Various transition metals were investigated. The results show that multi walled carbon nanotubes (MWNTs) and single walled carbon nanotubes (SWNTs) can both be synthesized using this technique. SWNTs are detected in the soot sample collected around the cathode, whereas the MWNTs are detected mainly in the deposit sample collected from the central area of the cathode. The CNT yield varies depending on the catalyst used and the properties of a good catalyst are discussed.     

低压空气中直流电弧法制备单壁碳纳米管

本文以Fe-S为催化剂、低压空气为缓冲气体采用直流电弧放电法首次大量合成低成本、高质量的单壁碳纳米管。实验结果表明在电弧放电过程中通过控制空气流量,使得电弧腔室压强保持在6～12 KPa为最优制备条件。采用扫描电子显微镜(SEM)和透射电子显微镜(TEM)对样品的形貌和结构进行表征,结果表明该方法所制备的单壁碳纳米管具有较高结晶度,管壁表面光滑、其直径为1.5～6.0 nm.采用低压空气电弧放电法有望成为低成本、大量制备高质量单壁碳纳米管的重要技术手段之一。     

Carbon nanotubes and diamond-like carbon films produced by cathodic micro-arc discharge in aqueous solutions

This letter reports the synthesis of carbon nanotubes and diamond-like carbon films using cathodic micro-arc discharge in aqueous solutions. The conditions and mechanisms for the growth of these structures were briefly discussed based on the experimental observations.     

Influence of the solution temperature on carbon nanotube formation by arc discharge method

Carbon nanotubes (CNTs) represent an important group of nanomaterials with attractive geometrical, electrical and chemical properties and are synthesised using a variety of techniques. In this study, CNTs are fabricated by arc discharge in liquid with a fully automatic setup, while this system is equipped with a heat exchange system. This fully automatic setup enables the controlling of gap between the two electrodes and temperature of the media. Furthermore, this system can cool down the solution that is heated due to arc and keep the temperature of solution constant during the arc discharge. The temperature of the solution affects the synthesising and structuring of CNTs. In this study, CNTs are fabricated between two graphite electrodes, which are submerged in LiCl (0.25?N) and with a voltage of 25?V, while Ni and Mo are used as catalysts. For comparative study, CNTs are synthesised under different thermal conditions, below zero, at environment temperature and at high temperature (up to 80°C), and the results are analysed, compared and discussed. The scanning electron microscopy, transmission electron microscopy and Raman spectroscopy are employed to study the morphology of these carbon nanostructures. The general impact of the solution temperature upon nanoproduct structures will be discussed.     

Conversion of toluene into carbon nanotubes using arc discharge plasmas in solution

In order to form nanocarbon materials, an arc discharge plasma method in hydrocarbon solvent is developed. In the case that the arc discharge is performed in toluene with nickel electrodes, tube-like nanocarbons were formed from toluene. The catalysis of the metal electrodes is found to be an important factor for the formation of the nanocarbons by the arc discharge in toluene. This method has a possibility of forming carbon nanotubes from liquid state solvents as a new carbon source by using catalyst ingredient as discharge electrodes.     

Synthesis of straight multi-walled carbon nanotubes by arc discharge in air and their field emission properties

The possibility of preparing straight multi-walled carbon nanotubes (MWCNTs) on a large scale is demonstrated using direct current arc discharge with a rotating graphite anode in low pressure air. The process is time-saving, economical, and non-hazardous. It is found that the optimum air pressure for the highest yield of MWCNTs is about 60 Torr. Investigation of the internal organization of the cathode deposit reveals that many columns about 40 μm in diameter are closely packed and mechanically stable. The highest content of MWCNTs is found in the intercolumnar spaces between columns. Emitters made of the cathode deposits that contain a large number of straight nanotubes exhibit outstanding field emission properties. The turn-on electric field decreases from 1.44 to 0.93 V/μm and the field enhancement factor β increases from about 3,190 to 7,830 only after simple burning at 750 °C for 30 min in air. The results indicate that MWCNTs prepared by arc discharge in air are promising for field emission application.     

STM investigation of carbon nanotubes connected by functional groups

Chemical functionalization of carbon nanotubes (CNTs) is essential for many applications. Attachment of functional groups to nanotubes can dramatically increase the solubility of the nanotube material. Sidewall functional groups should react with polymers and improve the mechanical properties of nanocomposites. Tubes interconnected by chemical bonds will have a reduced contact resistance and can be used for interconnection purposes in nanoscale circuits. Carbon nanotubes covered with functional groups attached to their exterior wall were analyzed using scanning tunneling microscopy (STM) and TEM. The functionalization was carried out in three steps: acid treatment in H₂SO₄/HNO₃ (3:1) mixture, reaction with SOCl₂ and reaction with diaminopropanol (DAP). The binding force between the nanotubes connected by functional groups and the mechanical stability of the connection was investigated.     

Fabrication of high quality carbon nanotubes with a simple ethanol-assisted arc discharge process

In this paper, a simplified ethanol-assisted arc discharge method was developed for the fabrication of multi-wall carbon nanotubes in high quality. Carbon nanotubes with high purity (80-90%) were obtained through controlling the current (15-25 V, 10-25 A) and ethanol concentration (70-100%). The products were characterized using transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and Raman spectrometry.     

以煤为碳源直流电弧法制备单壁纳米碳管绳

以太西无烟煤为碳源，以稀土氧化物La2O3和过渡金属Ni为催化剂制备复合的煤基炭棒，采用直流电弧放电技术，成功实现了单壁纳米碳管绳的批量制备。用TEM和Raman光谱技术对纳米碳管绳产品进行了分析表征。结果表明：太西煤是制备单壁纳米碳管的合适碳源；电弧放电得到的煤基单壁纳米碳管的直径分布在2．01nm-1．80nm之间；双金属催化剂Ni-La在单壁纳米碳管的形成过程中存在协同作用，其催化活性优于其中的单一组分。     

A novel method to produce large amount single-walled carbon nanotubes by arc discharging

A new method to produce large quantities of single-walled carbon nanotubes (SWCNTs) with high purity is developed. Using several composite graphite rods containing Y and Ni powder as the anode, and a high purity graphite hemisphere as the cathode, a cloth-like deposit could be obtained by dc arc-discharge in helium at high temperature. The deposit contained about 50% SWCNTs. In this way, more than one gram deposit could be produced in a few minutes. The structure and morphology of the SWCNTs were then examined using transmission electron microscopy, Raman spectroscopy, and thermogravimetric analysis. The article is published in the original.     

Multi-walled carbon nanotubes grow under low pressure hydrogen,air, and argon ambient by arc discharge plasma

Multi-walled carbon nanotubes (MWCNTs) were grown on cathode deposit by arc discharge plasma under H₂, Ar, and air ambient environment. The influence of ambient gas pressure on the structure and physical properties of carbon nanotube were compared. Herein, we highlight the influence of ambient environment and pressure to grow high quality carbon nanotubes. Field emission scanning electron microscopy, transmission electron microscopy, Raman spectroscopy, and X-ray diffraction were used for structural characterization and yield determination. The result revealed that background gas and pressure were crucial factor for growing highly crystalline and highly graphitic with I_D/I_G ratio 0.237 obtained for MWCNTs' synthesized in H₂ environment with extreme low defects.     

The effect of sulfur on the structure of carbon nanotubes produced by a floating catalyst method

The effect of sulfur on the structures (shell number and diameter distribution) of carbon nanotubes (CNTs) was investigated in detail using high resolution transmission electronic microscopy (HRTEM) and Raman spectroscopy. Single-walled (SWNTs), double-walled (DWNTs), and multi-walled carbon nanotubes (MWNTs) with different diameter distributions were obtained only by increasing the sulfur addition amount with methane as carbon source. A similar structure change was found for ethanol as carbon source with changing the sulfur addition amount. These results indicate that addition of sulfur is necessary to enhance the growth of SWNTs and DWNTs, independent of the carbon source for our method. Based on the growth parameter study, HRTEM observations and kinetic considerations, the role of sulfur in the nucleation and growth of CNTs was discussed.