• 한국수소및신에너지학회논문집
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• 제12권1호
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• pp.65-73
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• 2001

Carbon nanotubes were prepared by catalytic decomposition of $CH_4$ using Ni-MgO catalyst at various temperatures. $H_2$ effect on crystallinity and morphology during the synthesis of carbon nanotubes was investigated. The crystallinity and morphology were characterized by SEM, TEM, XRD, TGA, and Raman spectroscopy. In addition, the hydrogen adsorption properties were evaluated by PCT measurement in a hydrogen pressure range between 1 and 120 bar. The optimal synthesis temperature of carbon nanotubes was elevated in the presence of $H_2$, although significant difference of carbon nanotube morphology was not found. It is believed that hydrogen served as self-cleaner mops the amorphous carbon on the catalyst surface. It is proved that the carbon nanotubes have multi-walled structure, short length with a outer diameter of 20 ~40nm and open tips after elimination of the catalyst. The amount of hydrogen adsorbed in carbon nanotubes is increased as the pressure of hydrogen is increased and reaches 1.3 wt % under the hydrogen pressure of 120 bar at room temperature.

• Bulletin of the Korean Chemical Society
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• 제25권10호
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• pp.1521-1524
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• 2004

The effect of $H_2$ gas on the carbon nanotubes (CNTs) synthesis with CO-$H_2$ gas mixture was investigated using mass measurements and scanning electron microscopy (SEM). The maximum weight and yield of the synthesized carbon were obtained when the mixture ratio of $H_2$: CO was 3 : 7 and 9 : 1, respectively. In case of 100% carbon monoxide (CO) without hydrogen ($H_2$) addition, the weight of carbon increased, but CNTs were not observed. The CNTs began to be made when the contents of $H_2$ reaches at least 10%, their structures became more distinct with an increase of $H_2$ addition, and then the shapes of CNTs were more thin and straight. When the contents of $H_2$ was 80% ($H_2$ : CO = 8 : 2), the shapes and growth of CNTs showed an optimal condition. On the other hand, when the contents of $H_2$ was higher than the critical value, the shapes of CNTs became worse due to transition into inactive surface of catalyst. It was considered that the inactive surface of catalyst resulted from decrease of carbon (C) and $H_2$ concentration by facilitation of methane ($CH_4$) gasification reaction (C + 2$H_2$ ${\rightarrow}$ $CH_4$) between C and $H_2$ gases. It was also found that H2 addition had an influence considerably on the shape and structure of CNTs.

• 한국재료학회:학술대회논문집
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• 한국재료학회 2011년도 추계학술발표대회
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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.

• Bulletin of the Korean Chemical Society
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• 제25권5호
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• pp.617-619
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• 2004

As an pretreatment, a Fe$(NO_3)_3{\cdot}9H_2O-Al(OH)_3$mixture was ground by a high energy mill and used as a supported catalyst for the growth of carbon nanotubes by a thermal CVD. The crystal structure of the catalyst disordered by the grinding influenced significantly the synthesis of carbon nanotubes in a thermal CVD.

• Transactions on Electrical and Electronic Materials
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• 제9권2호
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• pp.62-66
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• 2008

We report on the growth mechanism of vertically aligned carbon nanotubes (VACNTs) using ultra thin Ni catalysts and direct current plasma enhanced chemical vapor deposition (PECVD) system. The CNTs were grown with -600 V bias to substrate electrode and catalyst thickness variation of 0.07 nm to 3 nm. The CNT density was reduced with catalyst thickness reduction and increased growth time. Cone like CNTs were grown with ultra thin Ni thickness, and it results from an etch of carbon network by reactive etchant species and continuous carbon precipitation on CNT walls. Vertically aligned sparse CNTs can be grown with ultra thin Ni catalyst.

• 전기학회논문지
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• 제62권6호
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• pp.782-785
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• 2013

Multi-walled carbon nanotubes were synthesized on Ni catalyst using thermal chemical vapor deposition. By introducing ammonia gas during the CNT synthesis process, clean and vertically aligned CNTs without impurities could be prepared. As the ammonia gas increased a partial pressure of hydrogen in the mixed gas during the CNT synthesis process, we could control the CNT synthesis rate appropriately. As the ammonia gas has an etching ability, amorphous carbon species covering the catalyst particles were effectively removed. Therefore catalyst particles could maintain their catalytic state actively during the synthesis process. Finally, we could obtain clean and vertically aligned CNTs by introducing $NH_3$ gas during the CNT synthesis process.

• 대한전기학회:학술대회논문집
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• 대한전기학회 2006년도 제37회 하계학술대회 논문집 C
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• pp.1378-1379
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• 2006

Carbon nanotubes (CNTs) with few defects and very small amount of amorphous carbon coating have been synthesized by catalytic decomposition of acetylene in $H_2$ over well-dispersed metal particles supported on MgO. The yield, quality and diameters of CNTs were obtained by control of catalyst metal compositions to be used. The optimization condition of carbon nanotubes with high yield is when Co and Mo are in a 1:1 ratio and Fe metal contents to Co is increased on magnesium oxide support. It is also found that the diameter of the as-prepared CNTs can be controlled mainly by adjusting the molar ratio of Fe-Mo, Co-Fe, and Co-Mo versus the MgO support. Our results indicated that desired diameter distribution of CNTs is obtained by choosing or combining the catalyst to be employed.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2000년도 하계학술대회 논문집
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• pp.328-331
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• 2000

Carbon nanotube(CNT) was successfully grown on Ni-W alloyed substrate by applying PECVD technique(Plasma Enhanced Chemical Vapor Deposition). As a catalyst, Ni-W alloyed substrate was prepared by mechanical alloying method. In order to find the optimum growth condition, initially two different types of gas mixtures such ac $C_2$H$_2$-H$_2$and $C_2$H$_2$-MH$_3$were systematically investigated by adjusting results on the mixing ratio in temperature range of 500 to 80$0^{\circ}C$. In this work, we will report the preliminary results on the CNT processed by PECVD, which were characterized by XRD, SEM and TEM. Finally we will evalute the effect on CNT growth by changing many processing parameters, such as typical gas, mixing ratio between 2 mixture, plasma power and etc.

• 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.

• Carbon letters
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• 제14권2호
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• pp.99-104
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• 2013

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.