• Carbon letters
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• 제28권
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• pp.72-80
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• 2018

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 $CaCO_3$ 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 ($700^{\circ}C$), time (55 min), argon flow rate ($230.37mL\;min^{-1}$) and acetylene flow rate ($150mL\;min^{-1}$) 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.

• 한국분말재료학회지
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• 제15권6호
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• pp.496-502
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• 2008

Aluminum nitride (AlN) powders were prepared by the chemical vapor synthesis (CVS) process in the $AlCl_{3}-NH_{3}-N_{2}$ system. Aluminum chloride ($AlCl_3$) as the starting material was gasified in the heating chamber of $300^{\circ}C$. Aluminum chloride gas transported to the furnace in $NH_{3}-N_{2}$ atmosphere at the gas flow rate of 200-400ml/min. For samples synthesized between 700 and $1200^{\circ}C$, the XRD peaks corresponding to AlN were comparatively sharp and also showed an improvement of crystallinity with increasing the reaction temperature. In additions, the average particle size of the AlN powders decreased from 250 to 40 nm, as the reaction temperature increased.

• 한국정밀공학회지
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• 제24권6호
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• pp.113-120
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• 2007

Chemical vapor deposition (CVD) is one of the various synthesis methods that have been employed for carbon nanotube (CNT) growth. In particular, Ren et al reported that large areas of vertically aligned multi-wall carbon nanotubes could be grown using a direct current (dc) PECVD system. The synthesis of CNT requires a metal catalyst layer, etchant gas, and a carbon source. In this work, the substrates consists of Si wafers with Ni-deposited film. Ammonia $NH_3$) and acetylene ($C_2H_2$) were used as the etchant gases and carbon source, respectively. Pretreated conditions had an influence on vertical growth and density of CNTs. And patterned growth of CNTs could be achieved by lithographical defining the Ni catalyst prior to growth. The length of single CNT was increased as niclel dot size increased, but the growth rate was reduced when nickel dot size was more than 200 nm due to the synthesis of several CNTs on single Ni dot. The morphology of the carbon nanotubes by TEM showed that vertical CNTs were multi-wall and tip-type growth mode structure in which a Ni cap was at the end of the CNT.

• 한국재료학회지
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• 제28권5호
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• pp.279-285
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• 2018

Graphene is an interesting material because it has remarkable properties, such as high intrinsic carrier mobility, good thermal conductivity, large specific surface area, high transparency, and high Young's modulus values. It is produced by mechanical and chemical exfoliation, chemical vapor deposition (CVD), and epitaxial growth. In particular, large-area and uniform single- and few-layer growth of graphene is possible using transition metals via a thermal CVD process. In this study, we utilize polystyrene and boron oxide, which are a carbon precursor and a doping source, respectively, for synthesis of pristine graphene and boron doped graphene. We confirm the graphene grown by the polystyrene and the boron oxide by the optical microscope and the Raman spectra. Raman spectra of boron doped graphene is shifted to the right compared with pristine graphene and the crystal quality of boron doped graphene is recovered when the synthesis time is 15 min. Sheet resistance decreases from approximately $2000{\Omega}/sq$ to $300{\Omega}/sq$ with an increasing synthesis time for the boron doped graphene.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2009년도 제38회 동계학술대회 초록집
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• pp.80-80
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• 2010

Graphene has attracted tremendous attention for the last a few years due to it fascinating electrical, mechanical, and chemical properties. Up to now, several methods have been developed exclusively to prepare graphene, which include micromechanical cleavage, polycrystalline Ni employing chemical vapor deposition technique, solvent thermal reaction, thermal desorption of Si from SiC substrates, chemical routes via graphite intercalation compounds or graphite oxide. In particular, polycrystalline Ni foil and conventional chemical vapor deposition system have been widely used for synthesis of large-area graphene. [1-3] In this study, synthesis of mono-layer graphene on a Ni foil, the mixing ratio of hydrocarbon ($CH_4$) gas to hydrogen gas, microwave power, and growth time were systemically optimized. It is possible to synthesize a graphene at relatively lower temperature ($500^{\circ}C$) than those (${\sim}1000^{\circ}C$) of previous results. Also, we could control the number of graphene according to the growth conditions. The structural features such as surface morphology, crystallinity and number of layer were investigated by scanning electron microscopy (SEM) and atomic force microscopy (AFM), transmission electron microscopy (TEM) and resonant Raman spectroscopy with 514 nm excitation wavelength. We believe that our approach for the synthesis of mono-layer graphene may be potentially useful for the development of many electronic devices.

• 한국재료학회지
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• 제22권3호
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• pp.130-135
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• 2012

We present a method of graphene synthesis with high thickness uniformity using the thermal chemical vapor deposition (TCVD) technique; we demonstrate its application to a grid supporting membrane using transmission electron microscope (TEM) observation, particularly for nanomaterials that have smaller dimensions than the pitch of commercial grid mesh. Graphene was synthesized on electron-beam-evaporated Ni catalytic thin films. Methane and hydrogen gases were used as carbon feedstock and dilution gas, respectively. The effects of synthesis temperature and flow rate of feedstock on graphene structures have been investigated. The most effective condition for large area growth synthesis and high thickness uniformity was found to be $1000^{\circ}C$ and 5 sccm of methane. Among the various applications of the synthesized graphenes, their use as a supporting membrane of a TEM grid has been demonstrated; such a grid is useful for high resolution TEM imaging of nanoscale materials because it preserves the same focal plane over the whole grid mesh. After the graphene synthesis, we were able successfully to transfer the graphenes from the Ni substrates to the TEM grid without a polymeric mediator, so that we were able to preserve the clean surface of the as-synthesized graphene. Then, a drop of carbon nanotube (CNT) suspension was deposited onto the graphene-covered TEM grid. Finally, we performed high resolution TEM observation and obtained clear image of the carbon nanotubes, which were deposited on the graphene supporting membrane.

• Journal of Electrical Engineering and Technology
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• 제7권6호
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• pp.983-989
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• 2012

The purpose of this paper is to decide the optimum synthesis conditions of polycrystalline diamond films according to the ratio of gas mixture. Diamond films were deposited with cyclo-hexane as a carbon precursor by the microwave plasma enhanced chemical vapor deposition process. The optimum oxygen ratio to cyclo-hexane was reached about 125 % under the fixed 0.3% c-hexane in hydrogen. Oxygen plays a role in etching the graphitic components of carbon sp2 bond effectively. By OES measurement, the best synthesis conditions found out about 12.5 % and 15.75 %, which is the emission intensity ratios of CH(B-X) and $H{\beta}$ on $H{\alpha}$, respectively. Also, the electron temperature was similar about 5,000 to 5,200 K in this work.

• 한국재료학회:학술대회논문집
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• 한국재료학회 2012년도 춘계학술발표대회
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• pp.90.2-90.2
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• 2012

Graphene has recently attracted significant attention because of its unique optical and electrical properties. For practical device applications, special attention has to be paid to the synthesis of high-quality graphene on large-area substrates. Graphene has been synthesized by eloborated mechanical exfoliation of highly oriented pyrolytic graphite, chemical reduction of exfoliated grahene oxide, thermal decomposition of silicon carbide, and chemical vapor deposition (CVD) on Ni or Cu substrates. Among these techniques, CVD is superior to the others from the perspective of technological applications because of its possibility to produce a large size graphene. PECVD has been demonstrated to be successful in synthesizing various carbon nanostructures, such as carbon nanotubes and nanosheets. Compared with thermal CVD, PECVD possesses a unique advantage of additional high-density reactive gas atoms and radicals, facilitating low-temperature, rapid, and controllable synthesis. In the current study, we report results in synthesizing of high-quality graphene films on a Ni films at low temperature. Controllable synthesis of quality graphene on Cu foil through inductively-coupled plasma CVD (ICPCVD), in which the surface chemistry is significantly different from that of conventional thermal CVD, was also discussed.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2011년도 제41회 하계 정기 학술대회 초록집
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• pp.381-381
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• 2011

The influence of the water vapor on the growth of single-walled carbon nanotubes (SWCNTs) was investigated. SWCNTs were synthesized by catalytic chemical vapor deposition of acetylene over Fe-Mo/MgO catalyst with injection of water vapor. The morphologies and structures of the water-assisted SWCNTs were investigated according to the growth conditions such as water vapor concentrations, flow rate of the gas, furnace temperature, and growth time. Water-assisted SWCNTs exhibited large bundle morphological features with well-alignment of each CNT, while SWCNTs synthesized in the absence of water vapor showed entangled CNT with the random orientation. We also found that the diameter of the SWCNT bundle could be controlled by the growth condition. In our optimal growth condition, the product yield and the purity were 300 wt. % and 75%, which were 7.5 and 2.5 times higher than those of SWCNTs synthesized without water vapor, respectively. More detail discussion will be offered at the poster presentation.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2004년도 제26회 학술발표회 초록집
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• pp.89-89
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• 2004