The surface of carbon films deposited with inverted plasma fireballs is analysed in this paper. Measurements were conducted with Raman spectroscopy, atomic force microscopy and nanoindentation. The latter was used to obtain Young’s modulus as well as Martens and Vickers hardness. The roughness of the film was measured by atomic force microscopy and its thickness was measured. It was shown with Raman spectroscopy that the films are homogeneous in terms of atomic composition and layer thickness over an area of about 125 × 125 mm. Furthermore, it was demonstrated that inverted plasma fireballs are a viable tool for obtaining homogeneous, large area carbon films with rapid growth and very little energy consumption. The obtained films show very low roughness.

Carbon nanotube fiber is a promising material in electrical and electronic applications, such as, wires, cables, batteries, and supercapacitors. But the problem of joining carbon nanotube fiber is a main obstacle for its practical development. Since the traditional joining methods are unsuitable because of low efficiency or damage to the fiber structure, new methods are urgently required. In this study, the joining between carbon nanotube fiber was realized by deposited nickel–copper doublelayer metal via a meniscus-confined localized electrochemical deposition process. The microstructures of the double-layer metal joints under different deposition voltages were observed and studied. It turned out that a complete and defect-free joint could be fabricated under a suitable voltage of 5.25 V. The images of the joint cross section and interface between deposited metal and fiber indicated that the fiber structure remained unaffected by the deposited metal, and the introduction of nickel improved interface bonding of double-layer metal joint with fiber than copper joint. The electrical and mechanical properties of the joined fibers under different deposition voltages were studied. The results show that the introduction of nickel significantly improved the electrical and mechanical properties of the joined fiber. Under a suitable deposition voltage, the resistance of the joined fiber was 37.7% of the original fiber, and the bearing capacity of the joined fiber was no less than the original fiber. Under optimized condition, the fracture mode of the joined fibers was plastic fiber fracture.

To improve the pyrolytic carbon (PyC) deposition rate of Carbon/Carbon (C/C) composites prepared by the traditional chemical vapor infiltration (CVI) method, the 3D Ni/wood-carbon (3D Ni/C) catalyst was introduced into the CVI process. The effects of catalyst on the density of C/C composites were studied, and the deposition rate and morphologies of PyC were investigated after catalytic CVI. The morphologies of catalyst and PyC were characterized by scanning electron microscope and polarized light microscopy. The catalytic deposition mechanism of PyC was studied by density functional theory. The experimental results show that the initial carbon deposition efficiency of the catalytic pyrolysis process was 3–4 times that of the noncatalytic process. The catalyst reduced the energy barrier in the first step of deposition reaction from 382.55 to 171.67 kJ/mol according to simulation results. The pyrolysis reaction energy with Ni catalyst is reduced by 54% than that without the catalyst.

Continuous synthesis of high-crystalline carbon nanotubes (CNTs) is achieved by reconfiguring the injection part in the reactor that is used in the floating catalyst chemical vapor deposition (FC-CVD) process. The degree of gas mixing is divided into three cases by adjusting the configuration of the injection part: Case 1: most-delayed gas mixing (reference experiment), Case 2: earlier gas mixing than Case 1, Case 3: earliest gas mixing. The optimal synthesis condition is obtained using design of experiment (DOE) in the design of Case 1, and then is applied to the other cases to compare the synthesis results. In all cases, the experiments are performed by varying the timing of gas mixing while keeping the synthesis conditions constant. Production rate (Case 1: 0.63 mg/min, Case 2: 0.68 mg/min, Case 3: 1.29 mg/min) and carbon content (Case 1: 39.6 wt%, Case 2: 57.1 wt%, Case 3: 71.6 wt%) increase as the gas-mixing level increases. The amount of by-products decreases stepwise as the gas-mixing level increases. The IG/ID ratio increases by a factor of 7 from 10.3 (Case 1) to 71.7 (Case 3) as the gas-mixing level increases; a high ratio indicates high-crystalline CNTs. The radial breathing mode (RBM) peak of Raman spectrograph is the narrowest and sharpest in Case 3; this result suggests that the diameter of the synthesized CNTs is the most uniform in Case 3. This study demonstrates the importance of configuration of the injection part of the reactor for CNT synthesis using FC-CVD.

Carbon short fibers/copper composites with different carbon short fiber contents up to 15 wt.% as reinforcements are prepared to investigate the influence of the carbon short fiber surface coating on the microstructure, density, and electrical properties of the carbon short fibers/copper composites. The carbon short fibers were surface treated by acid functionalization followed by alkaline treatment before the coating process. It was observed from the results that coated type copper nanoparticles were deposited on the surface of the carbon short fibers. The surface treated carbon short fibers were coated by copper using the electroless deposition technique in the alkaline tartrate bath by using formaldehyde as a reducing agent of the copper sulfate. The produced coated carbon short fibers/copper composite powders were cold compacted at 600 MPa, and then sintered at 875 °C for 2 h under (hydrogen/nitrogen 1:3) atmosphere. A reference copper sample was also prepared by the same method to compare between the properties of pure copper and the carbon short fibers/copper composites. The phase composition, morphology, and microstructure of the prepared carbon short fibers/copper composite powders as well as the corresponding carbon short fibers/copper composites were investigated using X-ray diffraction analysis (XRD) and scanning electron microscope (SEM) equipped with an energy-dispersive spectrometer (EDS), respectively. The density and the electrical resistivity of the sintered composites were measured. It was observed from the results that the density was decreased; however, the electrical resistivity was increased by increasing the carbon short fibers wt.%.

In this study, an empirical relationship between the energy band gap of multi-walled carbon nanotubes (MWCNTs) and synthesis parameters in a chemical vapor deposition (CVD) reactor using factorial design of experiment was established. A bimetallic (Fe-Ni) catalyst supported on CaCO3 was synthesized via wet impregnation technique and used for MWCNT growth. The effects of synthesis parameters such as temperature, time, acetylene flow rate, and argon carrier gas flow rate on the MWCNTs energy gap, yield, and aspect ratio were investigated. The as-prepared supported bimetallic catalyst and the MWCNTs were characterized for their morphologies, microstructures, elemental composition, thermal profiles and surface areas by high-resolution scanning electron microscope, high resolution transmission electron microscope, energy dispersive X-ray spectroscopy, thermal gravimetry analysis and Brunauer-Emmett-Teller. A regression model was developed to establish the relationship between band gap energy, MWCNTs yield and aspect ratio. The results revealed that the optimum conditions to obtain high yield and quality MWCNTs of 159.9% were: temperature (700ºC), time (55 min), argon flow rate (230.37 mL min–1) and acetylene flow rate (150 mL min–1) respectively. The developed regression models demonstrated that the estimated values for the three response variables; energy gap, yield and aspect ratio, were 0.246 eV, 557.64 and 0.82. The regression models showed that the energy band gap, yield, and aspect ratio of the MWCNTs were largely influenced by the synthesis parameters and can be controlled in a CVD reactor.

Carbon nanofibers (CNF) are widely used as active agents for electrodes in Li-ion secondary battery cells, supercapacitors, and fuel cells. Nanoscale coatings on CNF electrodes can increase the output and lifespan of battery devices. Atomic layer deposition (ALD) can control the coating thickness at the nanoscale regardless of the shape, suitable for coating CNFs. However, because the CNF surface comprises stable C–C bonds, initiating homogeneous nuclear formation is difficult because of the lack of initial nucleation sites. This study introduces uniform nucleation site formation on CNF surfaces to promote a uniform SnO2 layer. We pretreat the CNF surface by introducing H2O or Al2O3 (trimethylaluminum + H2O) before the SnO2 ALD process to form active sites on the CNF surface. Transmission electron microscopy and energy-dispersive spectroscopy both identify the SnO2 layer morphology on the CNF. The Al2O3-pretreated sample shows a uniform SnO2 layer, while island-type SnOx layers grow sparsely on the H2Opretreated or untreated CNF.

Multiwall carbon nanotubes (MWCNT) with two different (L/D) aspect ratios (7±2 μm/140±30 nm and 0.5–2 μm/8–15 nm) were surface treated using nitric acid (HNO3) and polyethyleneimine (PEI) prior to their deposition on carbon fibers (CF). Before the hierarchical reinforcement with CF-MWCNT, the CFs were treated with 3-glycidoxypropyltrimethoxysilane, a coupling agent (Z6040) and with poly(amidoamine) (PAMAM) a dendrimer containing an ethylenediamine core and amine surface groups. The MWCNT were deposited on the CF using two methods, by electrostatic attraction and by chemical reactions. The changes in the CF surface morphology after the MWCNT deposition were analyzed using SEM, which revealed a higher density and uniform coverage for the PAMAM-treated CF and the short MWCNTs. The interfacial adhesion of the composite materials was evaluated using the single fiber fragmentation technique. The results indicated an improvement in the interfacial shear strength with the addition of the short-MWCNTs treated with acid solutions and grafted onto the surface of the CF fiber using electrostatic attraction.

In this study, we investigate the effect of the diffusion barrier and substrate temperature on the length of carbon nanotubes. For synthesizing vertically aligned carbon nanotubes, thermal chemical vapor deposition is used and a substrate with a catalytic layer and a buffer layer is prepared using an e-beam evaporator. The length of the carbon nanotubes synthesized on the catalytic layer/diffusion barrier on the silicon substrate is longer than that without a diffusion barrier because the diffusion barrier prevents generation of silicon carbide from the diffusion of carbon atoms into the silicon substrate. The deposition temperature of the catalyst and alumina are varied from room temperature to 150°C, 200°C, and 250°C. On increasing the substrate temperature on depositing the buffer layer on the silicon substrate, shorter carbon nanotubes are obtained owing to the increased bonding force between the buffer layer and silicon substrate. The reason why different lengths of carbon nanotubes are obtained is that the higher bonding force between the buffer layer and the substrate layer prevents uniformity of catalytic islands for synthesizing carbon nanotubes.

In this study, Fe-Ni bimetallic catalyst supported on kaolin is prepared by a wet impregnation method. The effects of mass of kaolin support, pre-calcination time, pre-calcination temperature and stirring speed on catalyst yields are examined. Then, the optimal supported Fe-Ni catalyst is utilised to produce multi-walled carbon nanotubes (MWCNTs) using catalytic chemical vapour deposition (CCVD) method. The catalysts and MWCNTs prepared using the optimal conditions are characterized using high resolution transmission electron microscope (HRTEM), high-resolution scanning electron microscope (HRSEM), electron diffraction spectrometer (EDS), selected area electron diffraction (SAED), thermogravimetric analysis (TGA), Brunauer-Emmett-Teller (BET), and X-ray diffraction (XRD). The XRD/EDS patterns of the prepared catalyst confirm the formation of a purely crystalline ternary oxide (NiFe2O4). The statistical analysis of the variance demonstrates that the combined effects of the reaction temperature and acetylene flow rate predominantly influenced the MWCNT yield. The N2 adsorption (BET) and TGA analyses reveal high surface areas and thermally stable MWCNTs. The HRTEM/HRSEM micrographs confirm the formation of tangled MWCNTs with a particle size of less than 62 nm. The XRD patterns of the MWCNTs reveal the formation of a typical graphitized carbon. This study establishes the production of MWCNTs from a bi-metallic catalyst supported on kaolin.

The feasibility of obtaining graphitic carbon films on targeted substrates without a catalyst and transfer step was explored through the pyrolysis of the botanical derivative camphor. In a horizontal quartz tube, camphor was subjected to a sequential process of evaporation and thermal decomposition; then, the decomposed product was deposited on a glass substrate. Analysis of the Raman spectra suggest that the deposited film is related to unintentionally doped graphitic carbon containing some sp-sp 2 linear carbon chains. The films were transparent in the visible range and electrically conductive, with a sheet resistance comparable to that of graphene. It was also demonstrated that graphitic films with similar properties can be reproduciblyobtained, while property control was readily achieved by varying the process temperature.

High-quality β-silicon carbide (SiC) coatings are expected to prevent the oxidation degradation of carbon fibers in carbon fiber/silicon carbide (C/SiC) composites at high temperature. Uniform and dense β-SiC coatings were deposited on carbon fibers by low-pressure chemical vapor deposition (LP-CVD) using silane (SiH4) and acetylene (C2H2) as source gases which were carried by hydrogen gas. SiC coating layers with nanometer scale microstructures were obtained by optimization of the processing parameters considering deposition mechanisms. The thickness and morphology of β-SiC coatings can be controlled by adjustment of the amount of source gas flow, the mean velocity of the gas flow, and deposition time. XRD and FE-SEM analyses showed that dense and crack-free β-SiC coating layers are crystallized in β-SiC structure with a thickness of around 2 micrometers depending on the processing parameters. The fine and dense microstructures with micrometer level thickness of the SiC coating layers are anticipated to effectively protect carbon fibers against the oxidation at high-temperatures.

We investigated the effects of parametric synthesis conditions of catalysts such as sintering temperature, sorts of supports and compositions of catalysts on alignment and length-control of carbon nanotubes (CNTs) using catalyst powders. To obtain aligned CNTs, several parameters were changed such as amount of citric acid, calcination temperature of catalysts, and the sorts of supports using the combustion method as well as to prepare catalyst. CNTs with different lengths were synthesized as portions of molybdenum and iron using a chemical vapor deposition reactor. In this work, the mechanisms of alignment of CNTs and of the length-control of CNTs are discussed.

Graphene has been synthesized on 100- and 300-nm-thick Ni/SiO2/Si substrates with CH4 gas (1 SCCM) diluted in mixed gases of 10% H2 and 90% Ar (99 SCCM) at 900˚C by using inductively-coupled plasma chemical vapor deposition (ICP-CVD). The film morphology of 100-nm-thick Ni changed to islands on SiO2/Si substrate after heat treatment at 900˚C for 2 min because of grain growth, whereas 300-nm-thick Ni still maintained a film morphology. Interestingly, suspended graphene was formed among Ni islands on 100-nm-thick Ni/SiO2/Si substrate for the very short growth of 1 sec. In addition, the size of the graphene domains was much larger than that of Ni grains of 300-nm-thick Ni/SiO2/Si substrate. These results suggest that graphene growth is strongly governed by the direct formation of graphene on the Ni surface due to reactive carbon radicals highly activated by ICP, rather than to well-known carbon precipitation from carbon-containing Ni. The D peak intensity of the Raman spectrum of graphene on 300-nm-thick Ni/SiO2/Si was negligible, suggesting that high-quality graphene was formed. The 2D to G peak intensity ratio and the full-width at half maximum of the 2D peak were approximately 2.6 and 47cm-1, respectively. The several-layer graphene showed a low sheet resistance value of 718Ω/sq and a high light transmittance of 87% at 550 nm.

Diamond-like carbon (DLC) films have been widely used in many industrial applications because of their outstanding mechanical and chemical properties like hardness, wear resistance, lubricous property, chemical stability, and uniformity of deposition. Also, DLC films coated on paper, polymer, and metal substrates have been extensively used. In this work, in order to improve the printing quality and plate wear of polymer printing plates, different deposition conditions were used for depositing DLC on the polymer printing plates using the Pulsed DC PECVD method. The deposition temperature of the DLC films was under 100˚C, in order to prevent the deformation of the polymer plates. The properties of each DLC coating on the polymer concave printing plate were analyzed by measuring properties such as the roughness, surface morphology, chemical bonding, hardness, plate wear resistance, contact angle, and printing quality of DLC films. From the results of the analysis of the properties of each of the different DLC deposition conditions, the deposition conditions of DLC + F and DLC + Si + F were found to have been successful at improving the printing quality and plate wear of polymer printing plates because the properties were improved compared to those of polymer concave printing plates.

The properties of pyrolytic carbon (PyC) deposited from C2H2 and a mixture of C2H2/C3H6 on ZrO2 particles in a fluidized bed reactor were studied by adjusting the deposition temperature, reactant concentration, and the total gas flow rate. The effect of the deposition parameters on the properties of PyC was investigated by analyzing the microstructure and density change. The density could be varied from 1.0 g/cm3 to 2.2 g/cm3 by controlling the deposition parameters. The density decreased and the deposition rate increased as the deposition temperature and reactant concentration increased. The PyC density was largely dependent on the deposition rate irrespective of the type of the reactant gas used.

The synthetic behaviors of carbon nanotubes (CNTs) by Fe/MgO catalysts were investigated in 0~90 wt.% range of MgO mixture ratios by catalytic chemical vapor deposition (CCVD) process. The CNTs were synthesized with 40 minutes of synthetic time, and 923 K of synthetic temperature using 0.1 L/min of ethylene gas and 1.0 L/min of hydrogen gas as synthetic and carrier gas, respectively. As the increase of synthetic temperatures and times, the diameters of CNTs become thicker. The carbon yield showed in a parabolic curve as MgO content increased and the maximum carbon yield was obtained at 30 wt.% of MgO. There were no obvious changes in the diameters of CNTs respect to the change of MgO content. Fe/MgO CNTs showed good crystalinity by High Resolution Transmission Electron microscope (HR-TEM) analysis. The behaviors of Fe/MgO CNTs have a tendency of depending on synthetic time and temperature rather than MgO content.

Synthesis gas is a high valued compound as a basic chemicals at various chemical processes. Synthesis gas is mainly produced commercially by a steam reforming process. However, the process is highly endothermic so that the process is very energy-consuming process. Thus, this study was carried out to produce synthesis gas by the partial oxidation of methane to decrease the energy cost. The effects of reaction temperature and flow rate of reactants on the methane conversion, product selectivity, product ratio, and carbon deposition were investigated with 13wt% Ni/MgO catalyst in a fluidized bed reactor. With the fluidized bed reactor, CH4 conversion was 91%, and Hz and CO selectivities were both 98% at 850℃ and total flow rate of 100 mL/min. These values were higher than those of fixed bed reactor. From this result, we found that with the use of the fluidized bed reactor it was possible to avoid the disadvantage of fixed bed reactor (explosion) and increase the productivity of synthesis gas.