• Journal of Hydrogen and New Energy
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• v.25 no.5
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• pp.475-481
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• 2014

Ammonia borane ($NH_3BH_3$), as a source material for energy generation and hydrogen storage, has attracted growing interest due to its high hydrogen content. We have investigated the synthesis of ammonia borane from sodium borohydride ($NaBH_4$) and ammonium chloride ($NH_4Cl$) utilizing a low-temperature process. From our results, we obtained a maximum synthetic yield of 98.2% of ammonia borane complex. The diammoniate diborane (DADB) was detected in about 5~10mol% with in the solid ammonia borane by solid-state $^{11}B$-NMR analysis. The synthesized solid ammonia borane products were studied to characterize hydrogen release upon thermal dehydrogenation.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.08a
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• pp.252.1-252.1
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• 2013

Hexagonal boron nitride (h-BN) is a two dimensional material which has high band-gap, flatness and inert properties. This properties are used various applications such as dielectric for electronic device, protective coating and ultra violet emitter so on. 1) In this report, we were growing h-BN sheet directly on sapphire 2"wafer. Ammonia borane (H3BNH3) and nickel were deposited on sapphire wafer by evaporate method. We used nickel film as a sub catalyst to make h-BN sheet growth. 2) During annealing process, ammonia borane moved to sapphire surface through the nickel grain boundary. 3) Synthesized h-BN sheet was confirmed by raman spectroscopy (FWHM: ~30cm-1) and layered structure was defined by cross TEM (~10 layer). Also we controlled number of layer by using of different nickel and ammonia borane thickness. This nickel film supported h-BN growth method may propose fully and directly growing on sapphire. And using deposited ammonia borane and nickel films is scalable and controllable the thickness for h-BN layer number controlling.

• Advances in Energy Research
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• v.4 no.2
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• pp.177-187
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• 2016

Ammonia borane $NH_3BH_3$ solubilized in organic solvent is a potential liquid-state chemical hydrogen storage material. In this study, metal acetylacetonates like $Fe(O_2C_5H_7)_3$, $Co(O_2C_5H_7)_2$, $Ni(O_2C_5H_7)_2$, $Pd(O_2C_5H_7)_2$, $Pt(O_2C_5H_7)_2$ and $Ru(O_2C_5H_7)_3$ are considered for assisting dehydrocoupling of ammonia borane in diglyme (0.135 M) at $50^{\circ}C$. The molar ratio between ammonia borane and metal acetylacetonate is fixed at 100. A protocol for the separation of the soluble and insoluble fractions present in the slurry is proposed; it consists in using acetonitrile to make the precipitation of metal-based compounds easier and to solubilize boron-based intermediates/products. The nature of the metal does not affect the dehydrocoupling mechanisms, the $^{11}B\{^1H\}$ NMR spectra showing the formation of the same reaction intermediates. The aforementioned metal acetylacetonates do mainly have effect on the kinetics of dehydrocoupling. Dehydrocoupling takes place heterogeneously and dehydrogenation of ammonia borane in these conditions leads to the formation of polyborazylene via intermediates like e.g., B-(cyclodiborazanyl) amine-borane and borazine. Our main results are reported and discussed herein.

• Journal of Hydrogen and New Energy
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• v.19 no.4
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• pp.299-304
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• 2008

Thermal decomposition of Ammonia Borane have been investigated with various analytical methods including TGA, TP-MS, DSC. By-products such as aminoborane and borazine were identified during hydrogen release by TGA, TP-MS analysis. $H_2$ release amount was measured at each temperature isothermally, which resulted in 7 wt% $H_2$ release at 130$^{\circ}C$. Moreover, higher temperature enhanced hydrogen release kinetics leading to shortened induction period from 20 min at 95$^{\circ}C$ to 0 min at 130$^{\circ}C$. Melting and decomposition at close temperature (4$^{\circ}C$ difference) caused the formation of thin foam during hydrogen release. Suppression of by-products and thin foam formation during hydrogen release is suggested as critical issues to realize chemical hydrogen storage system with ammonia borane.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.08a
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• pp.285-285
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• 2013

Recently, hexagonal boron nitride (h-BN), which is III-V compound of boron and nitride by strong covalent sp2 bonds has gained great interests as a 2 dimensional insulating material since it has honeycomb structure with like graphene with very small lattice mismatch (1.7%). Unlike graphene that is semi-metallic, h-BN has large band gap up to 6 eV while providing outstanding properties such as high thermal conductivity, mechanical strength, and good chemical stability. Because of these excellent properties, hBN can potentially be used for variety of applications such as dielectric layer, deep UV optoelectronic device, and protective transparent substrate. Low pressure and atmospheric pressure chemical vapor deposition (LPCVD and APCVD) methods have been investigated to synthesize h-BN by using ammonia borane as a precursor. Ammonia borane decomposes to polyiminoborane (BHNH), hydrogen, and borazine. The produced borazine gas is a key material that is a used for the synthesis of h-BN, therefore controlling the condition of decomposed products from ammonia borane is very important. In this paper, we optimize the decomposition of ammonia borane by investigating temperature, amount of precursor, and other parameters to fabricate high quality monolayer h-BN. Synthesized h-BN is characterized by Raman spectroscopy and its absorbance is measured with UV spectrophotometer. Topological variations of the samples are analyzed by atomic force microscopy. Scanning electron microscopy and Scanning transmission Electron microscopy are used for imaging and analysis of structures and surface morphologies.

• 한국신재생에너지학회:학술대회논문집
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• 2010.11a
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• pp.111.2-111.2
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• 2010

One-dimensional nanostructures such as carbon nanotubes could be ideal templates for formation of metallic nanoparticles. Furthermore, bimetallic component nanoparticles have recently been interesting issues for having high catalytic activity. This work provides both a facile method to synthesize bimetallic catalysts via N atoms of carbon nanotubes and also a picture about how to design the optimal bimetallic catalyst for hydrogen generation from the hydrogen storage material. In principle, the ratio of one component to another component could be generically extended to fabricate the high-performance bimetallic catalysts on host nanostructures. Indeed, we demonstrate that the bimetallic catalyst composed of the optimum composition results in the excellent hydrogen generation property from an aqueous borane ammonia solution, thus being capable of satisfying the Depart of Energy in USA target required for many advanced applications even with the small amount of our bimetallic catalysts attached onto the N-doped carbon nanotubes. This high hydrogen generation rate is found to be attributed to the optimal distance between active Pt and cheap Ni atoms for effective hydrogen generation.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.02a
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• pp.617-617
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• 2013

최근 그래핀 연구와 더불어 2차원 구조의 나노소재에 대한 관심이 급증하면서 육각형의 질화붕소(hexagonal boron nitride; h-BN) 박막(nanosheet) [1]이나 붕소 탄화질화물(boron caronitride; BCN) 박막 [2,3]과 같은 2차원 구조체에 대한 연구가 활발히 진행되고 있다. 그 중 BCN은 반금속(semimetal)인 흑연(graphite)과 절연체인 h-BN이 결합된 박막으로 원소의 구성 비율에 따라 전기적 특성을 제어할 수 있다는 장점이 있다. 따라서 다양한 나노소자로의 응용을 위한 연구가 활발히 진행되고 있다. 본 연구에서는 폴리스틸렌(polystyrene, PS)과 보레인 암모니아(borane ammonia)를 고체 소스로 이용하여 열화학기상증착법으로 BCN 박막을 SiO2 기판 위에 직접 합성하였다. SEM과 AFM 관측을 통해 합성된 BCN 박막의 두께가 약 10 nm이며, RMS roughness가 0.5~2.6 nm로 매우 낮은 것을 확인하였다. 합성과정에서 PS의 양을 조절하여 BCN 박막의 탄소의 밀도를 성공적으로 제어하였으며, 이에 따라 전기적인 특성이 제어되는 양상을 확인하였다. 또한 합성온도 변화에 따른 BCN 박막의 전기적인 특성이 제어되는 양상을 확인하였다. 추가적으로 같은 방법을 이용하여 BCN 박막을 Cu 위에서 합성하여 SiO2 기판위에 전사하였다. 합성된 BCN 박막의 구조적 특징과 화학적 조성 및 결합 상태를 투과전자현미경(transmission electron microscopy), X-선 광전자 분광법(X-ray photoelectron spectroscopy), 라만 분광법(Raman spectroscopy)을 통해 조사하였고, 이온성 용액법(ionic liquid) [4]을 이용하여 전계효과 특성을 측정하였다.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.08a
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• pp.255-255
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• 2013

최근 그래핀 연구와 더불어 2차원 구조의 나노소재에 대한 관심이 급증하면서 육각형의 질화붕소(hexagonal boron nitride; h-BN) 박막(nanosheet)이나 붕소 탄화질화물(boron caronitride; BCN) 박막과 같은 2차원 구조체에 대한 연구가 활발히 진행되고 있다. 그 중 BCN은 반금속(semimetal)인 흑연(graphite)과 절연체인 h-BN이 결합된 박막으로 원소의 구성 비율에 따라 전기적 특성을 제어할 수 있다는 장점이 있다. 따라서 다양한 나노소자로의 응용을 위한 연구가 활발히 진행되고 있다. 본 연구에서는 폴리스틸렌(polystyrene, PS)과 보레인 암모니아(borane ammonia)를 고체 소스로 이용하여 열화학 기상증착법을 이용하여 BCN 박막를 SiO2 기판 위에 직접 합성하였다. SEM과 AFM 관측을 통해 합성된 BCN 박막을 확인하였으며, RMS roughness가 0.5~2.6 nm로 매우 낮은 것을 확인하였다. 합성과정에서 PS의 양을 조절하여 BCN 박막의 탄소의 밀도를 성공적으로 제어하였으며, 이에 따라 전기적인 특성이 제어되는 양상을 확인하였다. 또한 합성온도 변화에 따른 BCN 박막의 전기적인 특성이 제어되는 양상을 확인하였다. 추가적으로 같은 방법을 이용하여 BCN 박막을 Ni 위에서 합성하여 SiO2 기판위에 전사 하였다. 합성된 BCN 박막의 구조적 특징과 화학적 조성 및 결합 상태를 투과전자현미경(transmission electron microscopy), X-선 광전자 분광법(X-ray photoelectron spectroscopy)을 통해 조사하였다.

• Journal of the Korean Magnetic Resonance Society
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• v.14 no.1
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• pp.38-44
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• 2010

In liquids NMR, $^{1}H$ is the most widely observed nucleus, which is not the case in solids NMR. The reason is due to the strong homo-dipolar interactions between the hydrogen atoms which mask the useful chemical shift information. Therefore we must remove the strong homo-dipolar interactions in order to get structural information, which can be investigated by the isotropic chemical shift. There are two ways of obtaining it. One is the ultra-fast MAS of ca. 70 kHz spinning speed, which has become available only recently. The other way is devising a pulse sequence which can remove the strong homo-dipolar interaction. In the latter way, MAS with a moderate spinning rate of a few kHz, is enough to remove the chemical shift anisotropy. In this report, 1D-CRAMPS and 2D MASFSLG techniques are utilized and their results will be compared. This kind of highresolution $^{1}H$ NMR for solids, should become a valuable analytical tool in the understanding and the developing of a new class of hydrogen storage materials. Here ammonium borane $-NH_{3}BH_{3}$, whose hydrogen content is high, is used as a sample.

• Proceedings of the Korean Vacuum Society Conference
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• 2016.02a
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• pp.344.2-344.2
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• 2016

Fully and partially grown hexagonal boron nitride (h-BN) on Cu foil, synthesized by chemical vapor deposition method, was studied using Raman and SEM measurements. Fully and partially grown samples were successfully made from borane-ammonia complex to controlling pressure and growth time. The fully grown h-BN and partially grown h-BN exhibits a ~ 1370 cm-1 B-N vibrational mode (E2g). Especially, well-aligned triangular h-BN monolayer was observed on some domain of Cu foil using SEM measurements.