• Korean Journal of Materials Research
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• v.21 no.2
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• pp.78-82
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• 2011

Mono- and few-layer graphenes were grown on Ni thin films by rapid-thermal pulse chemical vapor deposition technique. In the growth steps, the exposure step for 60 s in $H_2$ (a flow rate of 10 sccm (standard cubic centimeters per minute)) atmosphere after graphene growth was specially established to improve the quality of the graphenes. The graphene films grown by exposure alone without $H_2$ showed an intensity ratio of $I_G/I_{2D}$ = 0.47, compared with a value of 0.38 in the films grown by exposure in H2 ambient. The quality of the graphenes can be improved by exposure for 60 s in $H_2$ ambient after the growth of the graphene films. The physical properties of the graphene films were investigated for the graphene films grown on various Ni film thicknesses and on 260-nm thick Ni films annealed at 500 and $700^{\circ}C$. The graphene films grown on 260-nm thick Ni films at $900^{\circ}C$ showed the lowest $I_G/I_{2D}$ ratio, resulting in the fewest layers. The graphene films grown on Ni films annealed at $700^{\circ}C$ for 2 h showed a decrease of the number of layers. The graphene films were dependent on the thickness and the grain size of the Ni films.

• Journal of Information Display
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• v.2 no.3
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• pp.54-59
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• 2001

The role of $NH_3$ for vertical alignment of CNTs was investigated. The direct cause of the alignment was a dense distribution of catalytic metal particles, but which was kept catalytically active during the growth process by $NH_3$. This allows a dense nucleation of the CNTs, and consequently, assists vertical alignment through entanglement and mechanical leaning among the tubes. The CNTs grow in a base growth mode. Several evidences were presented including a direct cross-sectional TEM observation. Since Ni is consumed both by silicide reaction and by capture in the growing tube, the growth stops when Ni is completely depleted. This occurs faster for smaller particles, and thus a longer growth results in thin bottom with poor adhesion.

• Korean Journal of Materials Research
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• v.11 no.8
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• pp.697-702
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• 2001

Effects of ammonia treatment on the morphologies of the catalytic metal films and carbon nanotubes subsequently synthesized via a thermal chemical vapor deposition method were investigated. An optimally controlled thermo-chemical process of ammonia treatment gave rise to a morphology of a dense distribution of vertically aligned carbon nanotubes. $NH_3$ treatment is a crucial key process to obtain vertically aligned carbon nanotubes. However, it was realized by a simple $NH_3$ treatment during synthesis at temperatures of $800-900^{\circ}C$ without any extra process. The structure and morphology of carbon nanotubes were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman spectroscopy.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2005.11a
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• pp.99-100
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• 2005

We have grown carbon nanotubes (CNTs) with a microwave plasma chemical vapor deposition (MPECVD) method, which has been regard as one of the most promising candidates for the synthesis of CNTs due to the vertical alignment, the low temperature and the large area growth. We use methane ($CH_4$) and hydrogen ($H_2$) gas for the growth of CNTs. 60 nm thick Ni catalytic layer were deposited on the TiN coated glass substrate by RF magnetron sputtering method. In this work, we report the effects of pressure on the growth of CNTs. We have changed pressure of processing (10 $\sim$ 20 Torr) deposition of CNTs. SEM (Scanning electron microscopy) images show diameter, length and cross section state CNTs.

• Transactions on Electrical and Electronic Materials
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• v.9 no.2
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• pp.52-56
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• 2008

Carbon nanotube films were fabricated by the catalytic CVD method. Plasma processed time effects on the field emission property were studied. The atomic structure was observed by using X-ray photoelectron spectroscopy (XPS). The surface composition changes were observed on the plasma processed CNT films. The O1s/C1s signal ratio and the Fls/Cls signal ratio changed from 1.1 % to 24.65 % and from 0 % to 3.1 % with plasma process time, respectively. We could guess it from these results that the Ar plasma process could change the surface composition effectively. In the case of the original-CNT film, no carbon shift was observed. In the case of the Ar plasma processed CNT films, however the oxygen related carbon shifts were observed. This oxygen related carbon shift at higher binding energy implies the increment of amount of the oxygen. It's possible that the increment of these bonds between carbon and oxygen results in the improvement of field emission performance.

• The Transactions of The Korean Institute of Electrical Engineers
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• v.62 no.3
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• pp.376-379
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• 2013

Multi-walled carbon nanotubes (MWCNTs) were synthesized using catalytic chemical vapor deposition (CVD) method. Oxygen plasma treatment was applied to modify surface state of the CNTs synthesized for improvement of field emission performance. Surface state of the plasma treated CNTs was studied by X-ray photoelectron spectroscopy (XPS). The surface states of the CNTs were changed as a function of plasma treatment time. The oxygen related carbon shift was moved toward higher binding energy with the plasma treatment time. This result implies that the oxygen plasma treatment changes the surface state effectively. While any shift in carbon 1s peak was not detected for the as grown CNTs, oxygen related carbon shift was detected for the plasma treated CNTs. Carbon shift implies that closed CNT tips were opened by the oxygen plasma and reacted with oxygen species. Since the field emission occurs at pentagons or dangling bonds of the CNT tips, the increase of carbon-oxygen bonds plays an important role in field emission behavior by increasing the number of electron emission sites resulting in improvement of the field emission performance.

• Journal of the Korean institute of surface engineering
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• v.50 no.6
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• pp.516-522
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• 2017

We report the growth of carbon nanotubes (CNT) on Invar-42 plates using coal tar pitch (CTP) by chemical vapor deposition (CVD) method. The solid phase CTP is used as an inexpensive carbon source since it produces a bunch of hydrocarbon gases such as $CH_4$ and other $C_xH_v$ by thermal decomposition over $450^{\circ}C$. The Invar-42 is a representative Ni-based ferrous alloy and can be used repetitively as a substrate for CNT growth because Ni and Fe are used as very active catalytic elements. We changed mixing ratio of carrier gases, argon and hydrogen, and temperature of growth region. It was found that the optimum gas ratio and temperature for high quality CNT growth are $Ar:H_2=400:400$ sccm and $1000^{\circ}C$, respectively. In addition, the carbon nanoball (CNB) was also obtained by just changing the mixing ratio to $Ar:H_2=100:600$ sccm. Finally, CTP can be employed as a versatile carbon source to produce various carbon-based nanomaterials, such as CNT and CNB.

• Journal of the Korean Vacuum Society
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• v.20 no.2
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• pp.155-163
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• 2011

Carbon nanotubes (CNT) have been attracted much attention since they have been expected to be used in various areas by virtue of their outstanding physical, electrical, and chemical properties. In order to make full use of their prominent electric conductivity in some areas such as electron emission sources, device interconnects, and electrodes in energy storage devices, direct growth of CNT with vertical alignment is definitely beneficial issue because they can maintain mechanical stability and high conductivity at the interface between substrates. Here, we report direct growth of vertically aligned CNT (VCNT) on Cu foils using thermal chemical vapor deposition and characterize the field emission property of the VCNT. The VCNT's height was controlled by changing the growth temperature, growth time, and catalytic layer thickness. Optimum growth condition was found to be $800^{\circ}C$ for 20 min with acetylene and hydrogen mixtures on Fe catalytic layer of 1 nm thick. The diameter of VCNT grown was smaller than that of usual multi walled CNT. Based on the result of field emission characterization, we concluded that the VCNT on Cu foils can be useful in various potential applications where high conductivity through the interface between CNT and substrate is required.

• Proceedings of the Materials Research Society of Korea Conference
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• 2011.10a
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• pp.17.2-17.2
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• 2011

Double-walled carbon nanotubes (DWCNTs) were grown with vertical alignment on a Si wafer by using catalytic thermal chemical vapor deposition. This study investigated the effect of pre-annealing time of catalyst on the types of CNTs grown on the substrate. The catalyst layer is usually evolved into discretely distributed nanoparticles during the annealing and initial growth of CNTs. The 0.5-nm-thick Fe served as a catalyst, underneath which Al was coated as a catalyst support as well as a diffusion barrier on the Si substrate. Both the catalyst and support layers were coated by using thermal evaporation. CNTs were synthesized for 10 min by flowing 60 sccm of Ar and 60 sccm of H2 as a carrier gas and 20 sccm of C2H2 as a feedstock at 95 torr and $750^{\circ}C$. In this study, the catalyst and support layers were subject to annealing for 0~420 sec. As-grown CNTs were characterized by using field emission scanning electron microscopy, high resolution transmission electron microscopy, Raman spectroscopy, and atomic force microscopy. The annealing for 90~300 sec caused the growth of DWCNTs as high as ~670 ${\mu}m$ for 10 min while below 90 sec and over 420 sec 300~830 ${\mu}m$-thick triple and multiwalled CNTs occurred, respectively. Several radial breathing mode (RBM) peaks in the Raman spectra were observed at the Raman shifts of 112~191 cm-1, implying the presence of DWCNTs, TWCNTs, MWCNTs with the tube diameters 3.4, 4.0, 6.5 nm, respectively. The maximum ratio of DWCNTs was observed to be ~85% at the annealing time of 180 sec. The Raman spectra of the as-grown DWCNTs showed low G/D peak intensity ratios, indicating their low defect concentrations. As increasing the annealing time, the catalyst layer seemed to be granulated, and then grown to particles with larger sizes but fewer numbers by Ostwald ripening.

• Journal of Powder Materials
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• v.22 no.2
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• pp.122-128
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• 2015

In this study, titanium(Ti) meshes and porous bodies are employed to synthesize carbon nanotubes(CNTs) using methane($CH_4$) gas and camphene solution, respectively, by chemical vapor deposition. Camphene is impregnated into Ti porous bodies prior to heating in a furnace. Various microscopic and spectroscopic techniques are utilized to analyze CNTs. It is found that CNTs are more densely and homogeneously populated on the camphene impregnated Ti-porous bodies as compared to CNTs synthesized with methane on Ti-porous bodies. It is elucidated that, when synthesized with methane, few CNTs are formed inside of Ti porous bodies due to methane supply limited by internal structures of Ti porous bodies. Ti-meshes and porous bodies are found to be multi-walled with high degree of structural disorders. These CNTs are expected to be utilized as catalyst supports in catalytic filters and purification systems.