• Title/Summary/Keyword: hydride formation

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A study on crystal growth and properties of high quality DAST (고품질 DAST 결정성장과 특성에 관한 연구)

  • 윤선웅;연석주;김종흠
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.14 no.1
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    • pp.12-16
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    • 2004
  • In this study, we have investigated the development of the crystal growth stability and reproducibility for large and high-quality DAST. DAST crystal were grown from a saturated methanol solution by a slow cooling method and DAST was synthesized by the condensation of 4-methyl-n-methyl pyridinum tosylate, which was prepared from 4-pocoline and methyl toluenesulponate and 4-N-dimethyl amino-bezaldehyde in the presence of piperidine. We had synthesized DAST crystals in dry Argon atmosphere in order to avoid the formation of hydride organge co-crystals, DAST$.$$H_2O$. Since DAST molecules crystallize in a humid atmosphere, crystal structure become centrosymmetric, and then second order NLO (nonlinear optical) properties would be disappeared. We fixed the growth orientation of DAST crystal (001) surface. The crystal growth was proceeded at a cooling rate of $H_2O$/day and the cooling period is for 4 days. The dimensions of seed crystal was $2.5\times 3.6\times0.4\textrm{mm}^3$ and we have obtained a DAST crystal with the dimension of $10\times 10.5\times3.0\textrm{mm}^3$. The color of grown DAST crystal is red and it's surface appears to be metallic green.

Kinetics and Mechanism of the Oxidation of Substituted Benzyl Alcohols by Cr(VI)-Heterocyclic Complex (2,4'-Bipyridinium Chlorochromate) (크롬(VI)-헤테로고리 착물(2,4'-비피리디늄 클로로크로메이트)에 의한 치환 벤질 알코올류의 산화반응에서 속도론과 메카니즘)

  • Park, Young Cho;Kim, Young Sik
    • Applied Chemistry for Engineering
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    • v.25 no.6
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    • pp.648-653
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    • 2014
  • Cr(VI)-heterocyclic complex (2,4'-bipyridinium chlorochromate) was synthesized by the reaction between heterocyclic compound(2,4'-bipyridine) and chromium trioxide, and characterized by IR and ICP analysis. The oxidation of benzyl alcohol using 2,4'-bipyridinium chlorochromate in various solvents showed that the reactivity increased with the increase of the dielectric constant (${\varepsilon}$), in the order : N,N-dimet-hylformamide (DMF) > acetone > chloroform > cyclohexene. In the presence of DMF solvent with acidic catalyst such as hydrochloric acid (HCl solution), 2,4'-bipyridinium chlorochromate oxidized benzyl alcohol (H) and its derivatives (p-$CH_3$, m-Br, m-$NO_2$). Electron-donating substituents accelerated the reaction rate, whereas electron acceptor groups retarded the reaction rate. The Hammett reaction constant (${\rho}$) was -0.67 (303 K). The observed experimental data have been rationalize the proton transfer occurred followed the formation of a chromate ester in the rate-determining step.

The Effect of Planetary Ball Mill Process on the Hydrogenation Behavior of Mg2NiHx (Mg2NiHx 수소화거동에 미치는 기계적합금화 공정의 영향)

  • Lim, Jae-Won;Ha, Won;Hong, Tae-Whan;Kim, Shae-Kwang;Kim, Young-Jig;Park, Hyun-Soon
    • Transactions of the Korean hydrogen and new energy society
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    • v.10 no.2
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    • pp.131-139
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    • 1999
  • The objective of this works was to synthesize the$Mg_2Ni$ hydrogen storage materials economically and to eliminate the intial activation process. $Mg_2NiH_x$ was mechanically alloyed under purified hydrogen gas atmosphere using pure Mg and Ni chips. M.A(Mechanical Alloying) was carried out using planetary ball mill for times varying from 12h to 96h under 20bars of hydrogen gas pressure. $Mg_2NiH_x$ started to form after 48h and the homogeneous $Mg_2NiH_x$ composites was synthesized after 96h. From TG analysis, the dehydriding reaction of $Mg_2NiH_x$ started at around $200^{\circ}C$. The result of P-C-T at $300^{\circ}C$ revealed the hydrogen storage capacity of $Mg_2NiH_c$ reached 3.68 wt% and the effective hydrogen storage was 2.38 wt%. The enthalpy difference of absorption-desorption cycling for the hydride formation and the hysteresis were reduced and the plateau flatness and the sloping were improved according to M.A time.

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Effects of Nickel and Iron Oxide Addition by Milling under Hydrogen on the Hydrogen-Storage Characteristics of Mg-Based Alloys

  • Song, Myoung Youp;Baek, Sung Hwan;Park, Hye Ryoung;Mumm, Daniel R.
    • Korean Journal of Metals and Materials
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    • v.50 no.1
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    • pp.64-70
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    • 2012
  • Samples of pure Mg, 76.5 wt%Mg-23.5 wt%Ni, and 71.5 wt%Mg-23.5 wt%Ni-5 wt%$Fe_2O_3$ were prepared by reactive mechanical grinding and their hydriding and dehydriding properties were then investigated. The reactive mechanical grinding of Mg with Ni is considered to facilitate nucleation and to shorten diffusion distances of hydrogen atoms. After hydriding-dehydriding cycling, the 76.5 wt%Mg-23.5 wt%Ni and 71.5 wt%Mg-23.5 wt%Ni-5 wt%$Fe_2O_3$ samples contained $Mg_2Ni$ phase. In addition to the effects of the creation of defects and the decrease in particle size, the addition of Ni increases the hydriding and dehydriding rates by the formation of $Mg_2Ni$. Expansion and contraction of the hydride-forming materials (Mg and $Mg_2Ni$) with the hydriding and dehydriding reactions are also considered to increase the hydriding and dehydriding rates of the mixture by forming defects and cracks leading to the fragmentation of particles. The reactive mechanical grinding of Mg-Ni alloy with $Fe_2O_3$ is considered to decrease the particle size.

Nano-thick Nickel Silicide and Polycrystalline Silicon on Polyimide Substrate with Extremely Low Temperature Catalytic CVD (폴리이미드 기판에 극저온 Catalytic-CVD로 제조된 니켈실리사이드와 실리콘 나노박막)

  • Song, Ohsung;Choi, Yongyoon;Han, Jungjo;Kim, Gunil
    • Korean Journal of Metals and Materials
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    • v.49 no.4
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    • pp.321-328
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    • 2011
  • The 30 nm-thick Ni layers was deposited on a flexible polyimide substrate with an e-beam evaporation. Subsequently, we deposited a Si layer using a catalytic CVD (Cat-CVD) in a hydride amorphous silicon (${\alpha}$-Si:H) process of $T_{s}=180^{\circ}C$ with varying thicknesses of 55, 75, 145, and 220 nm. The sheet resistance, phase, degree of the crystallization, microstructure, composition, and surface roughness were measured by a four-point probe, HRXRD, micro-Raman spectroscopy, FE-SEM, TEM, AES, and SPM. We confirmed that our newly proposed Cat-CVD process simultaneously formed both NiSi and crystallized Si without additional annealing. The NiSi showed low sheet resistance of < $13{\Omega}$□, while carbon (C) diffused from the substrate led the resistance fluctuation with silicon deposition thickness. HRXRD and micro-Raman analysis also supported the existence of NiSi and crystallized (>66%) Si layers. TEM analysis showed uniform NiSi and silicon layers, and the thickness of the NiSi increased as Si deposition time increased. Based on the AES depth profiling, we confirmed that the carbon from the polyimide substrate diffused into the NiSi and Si layers during the Cat-CVD, which caused a pile-up of C at the interface. This carbon diffusion might lessen NiSi formation and increase the resistance of the NiSi.

A Study on Electrolysis of Heavy Water and Interaction of Hydrogen with Lattice Defects in Palladium Electrodes (팔라디움전극에서 중수소의 전기분해와 수소와 격자결함의 반응에 관한 연구)

  • Ko, Won-Il;Yoon, Young-Ku;Park, Yong-Ki
    • Nuclear Engineering and Technology
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    • v.24 no.2
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    • pp.141-153
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    • 1992
  • Excess tritium analysis was peformed to verify whether or not cold fusion occurs during electrolysis of heavy water in the current density range of 83~600 mA/$\textrm{cm}^2$ for a period of 24 ~ 48 hours with use of palladium electrodes of seven different processing treatments and geometries. The extent of recombination of D$_2$ and $O_2$gases in the electrolytic cell was measured for the calculation of accurate enthaplpy values. The behavior and interaction of hydrogen atoms with defects in Pd electrodes were examined using the Sieverts gas charging and the positron annihilation(PA) method. Slight enrichment of tritium observed was attributed to electrolytic enrichment but not to the formation of a by-product of cold fusion. The extent of recombination of D$_2$and $O_2$gases was 32%. Hence the excess heat measured during the electrolysis was considered to be due to the exothermic reaction of recombination but not to nuclear fusion. Lifetime results from the PA measurements on the Pd electrodes indicated that hydrogen atoms could be trapped at dislocations and vacancies in the electrodes and that dislocations were slightly more preferred sites than vacancies. It was also inferred from R parameters that the formation of hydrides was accompanied by generation of mostly dislocations. Doppler broadening results of the Pd electrodes indicated that lattiec defect sites where positrons were trapped first increased and then decreased, and this cycle was repeated as electrolysis continued. It can be inferred from PA measurements on the cold-rolled Pd and the isochronally annealed Pd hydride specimens that microvoid-type defects existed in the hydrogen-charged electrode specimen.

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The molten KOH/NaOH wet chemical etching of HVPE-grown GaN (HVPE로 성장된 GaN의 용융 KOH/NaOH 습식화학에칭)

  • Park, Jae Hwa;Hong, Yoon Pyo;Park, Cheol Woo;Kim, Hyun Mi;Oh, Dong Keun;Choi, Bong Geun;Lee, Seong Kuk;Shim, Kwang Bo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.24 no.4
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    • pp.135-139
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    • 2014
  • The hydride vapor phase epitaxy (HVPE) grown GaN samples to precisely measure the surface characteristics was applied to a molten KOH/NaOH wet chemical etching. The etching rate by molten KOH/NaOH wet chemical etching method was slower than that by conventional etching methods, such as phosphoric and sulfuric acid etching, which may be due to the formation of insoluble coating layer. Therefore, the molten KOH/NaOH wet chemical etching is a better efficient method for the evaluation of etch pits density. The grown GaN single crystals were characterized by using X-ray diffraction (XRD) and X-ray rocking curve (XRC). The etching characteristics and surface morphologies were studied by scanning electron microscopy (SEM). From etching results, the optimum etching condition that the etch pits were well independently separated in space and clearly showed their shape, was $410^{\circ}C$ and 25 min. The etch pits density obtained by molten KOH/NaOH wet chemical etching under optimum etching condition was around $2.45{\times}10^6cm^{-2}$, which is commercially an available materials.

Mechanistic Studies on the Reactions of 1-[(Aryl)(phenylseleno)methyl]benzotriazoles and 6-Aryl-6-(benzotriazol-1-yl)-1-hexenyl Phenyl Selenides with Tributyltin Hydride (1-[(아릴)(페닐셀레노)메틸]벤조트리아졸과 셀렌화 6-아릴-6-(벤조트리아졸-1-일)-1-헥센일 페닐의 삼부틸틴 수소화물과의 반응메카니즘에 관한 연구)

  • Kang, Yoon Ho;Kim, Kyong Tae
    • Journal of the Korean Chemical Society
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    • v.43 no.1
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    • pp.74-84
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    • 1999
  • Most of the reactions involving benzotriazoles as a synthetic auxiliary have been explained by ionic mechanisms, whereas benzotriazole-mediated radical reactions have received little attention. The reaction of 1-[(aryl)(phenylseleno)methyl]benzotriazole with $Bu_3$SnH in the presence of AIBN in benzene at reflux gave 2-aminodiphenyl selenide (16-29%), 2-aminobiphenyl (9-15%), diphenyl diselenide (30-93%), 1-(arylmethyl) benzotriazole (9-39%) and tributyltin-phenyl selenide (10-36%), whereas the compounds were treated with excess molar amount of $Bu_3$SnH in the absence of AIBN to afford N-(arylmethyl)anilines (44-66%) along with diphenyl diselenide (53-100%), benzotriazole (27-35%) and 1-(arylmethyl)benzotriazole (16-33%). Similarly, treatment of 6-aryl-6-(benzotriazol-1-yl)-1-hexenyl phenyl selenides with $Bu_3$SnH in the presence of AIBN gave 6-aryl-6-phenylamino-1-hexene (9-31%) and 1-aryl-1-oxo-5-pentene (15-44%). A mechanism for the formation of the products is proposed.

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Effects of acid-treatment conditions on the surface properties of the RBM treated titanium implants (산-처리 조건이 RBM처리한 티타늄 임플란트의 표면 특성에 주는 영향)

  • Lee, Han-Ah;Seok, Soohwang;Lee, Sang-Hyeok;Lim, Bum-Soon
    • Korean Journal of Dental Materials
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    • v.45 no.4
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    • pp.257-274
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    • 2018
  • The purpose of this study was to evaluate the effect of acid-treatment conditions on the surface properties of the RBM (Resorbable Blast Media) treated titanium. Disk typed cp-titanium specimens were prepared and RBM treatments was performed with calcium phosphate ceramic powder. Acid solution was mixed using HCl, $H_2SO_4$ and deionized water with 4 different volume fraction. The RBM treated titanium was acid treated with different acid solutions at 3 different temperatures and for 3 different periods. After acid-treatments, samples were cleaned with 1 % Solujet solution for 30 min and deionized water for 30 min using ultrasonic cleanser, then dried in the electrical oven ($37^{\circ}C$). Weight of samples before and after acid-treatment were measured using electric balance. Surface roughness was estimated using a confocal laser scanning microscopy, crystal phase in the surface of sample was analyzed using X-ray diffractometer. Surface morphology and components were evaluated using Scanning Electron Microscope (SEM) with Energy Dispersive X-ray spectroscopy (EDX) and X-ray Photoemission Spectroscopy (XPS). Values of the weight changes and surface roughness were statistically analyzed using Tukey-multiple comparison test (p=0.05). Weight change after acid treatments were significantly increased with increasing the concentration of $H_2SO_4$ and temperature of acid-solution. Acid-treatment conditions (concentration of $H_2SO_4$, temperature and time) did not produce consistent effects on the surface roughness, it showed the scattered results. From XRD analysis, formation of titanium hydrides in the titanium surface were observed in all specimens treated with acid-solutions. From XPS analysis, thin titanium oxide layer in the acid-treated specimens could be evaluated. Acid solution with $90^{\circ}C$ showed the strong effect on the titanium surface, it should be treated with caution to avoid the over-etching process.