• Title/Summary/Keyword: Hydrothermal growth

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Effects of Mo co-doping into Fe doped β-Ni(OH)2 microcrystals for oxygen evolution reactions (Fe-doped β-Ni(OH)2의 산소발생반응 증가를 위한 Mo의 동시도핑효과)

  • Je Hong Park;Si Beom Yu;Tae Kwang An;Byeong Jun Kim;Jeong Ho Ryu
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.34 no.1
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    • pp.30-35
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    • 2024
  • In order to improve the efficiency of the water splitting system for hydrogen production, the high overvoltage in the electrochemical reaction caused by the catalyst in the hydrogen evolution reaction (HER) and oxygen evolution reaction (OER) must be reduced. Among them, transition metal-based compounds are attracting attention as catalyst materials that can replace precious metals such as platinum that are currently used. In this study, nickel foam, an inexpensive metal porous material, was used as a support, and Fe-doped β-Ni(OH)2 microcrystals were synthesized through a hydrothermal synthesis process. In addition, in order to improve OER properties, changes in the shape, crystal structure, and water splitting characteristics of Fe-Mo co-doped β-Ni(OH)2 microcrystals synthesized by co-doping with Mo were observed. The changes in the shape, crystal structure, and applicability as a catalyst for water splitting were examined.

Petrology of the Chaeyaksan basaltic rocks and application of hornblende geobarometer (채약산 현무암질암류의 암석학적인 특징 및 각섬석 지질압력계의 적용)

  • 김상욱;황상구;양판석;이윤종;고인석
    • The Journal of the Petrological Society of Korea
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    • v.8 no.2
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    • pp.92-105
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    • 1999
  • The Cretaceous Chaeyaksan basaltic rocks consist mainly of basaltic tuffs intercalating three layers of basalt. Stratigraphically, the rocks are located between the upper Songnaedong Formation and the lower Geoncheonri Formation and contain plagioclase, augite, hornblende, and a few olivine phenocrysts. Geochemically, they show calc-alkaline characteristics in some immobile element content, but show the alkaline suite feature in the mobile major element composition. The basalts are widely spilitized but some of them is altered to shoshonitic rocks with more calcic plagioclase, calcite, and chlorite, and adularia veinlets are common in the rocks. It is supposed that the post-eruption alteration of the rocks is done through alkali-replacement by hydrothermal solution or vapor rather than by low grade regional metamorphism. It is considered that A1 in hornblende will be available for estimating the pressure of the pre-eruption magma in the reservoir although the plagioclase of the rocks are highly albitized. The crystallization pressure was calculated as 5.7Kb by the equation of Johnson and Rutherford(l989) incorporating of the effect of overestimate of .41T in hornblende in the case of quartz-free rocks. Application of the estimated temperature, pressure and the constituent of phenocrysts of the rocks to the experimental P-T phase diagram for basalts established by Green(1982) indicates the crystallization course and succession of growth of the phenocrysts during of rising and cooling of the magma reservoir; augite + augite and olivine + augite, olivine, and hornblende -+ augite and hornblende+ augite, hornblende, and plagioclase. Such evolution course of the magma may include crystal fractionation by the phenocrysts crystallization and contamination by country rock in lower crust.

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Artificial Control of ZnO Nanorods via Manipulation of ZnO Nanoparticle Seeds (산화아연 나노핵의 조작을 통한 산화아연 나노로드의 제어)

  • Shin, Kyung-Sik;Lee, Sam-Dong;Kim, Sang-Woo
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.11a
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    • pp.399-399
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    • 2008
  • Synthesis and characterization of ZnO structure such as nanowires, nanorods, nanotube, nanowall, etc. have been studied to multifunctional application such as optical, nanoscale electronic and chemical devices because it has a room-temperature wide band gap of 3.37eV, large exiton binding energy(60meV) and various properties. Various synthesis methods including chemical vapor deposition (CVD), physical vapor deposition, electrochemical deposition, micro-emulsion, and hydrothermal approach have been reported to fabricate various kinds of ZnO nanostructures. But some of these synthesis methods are expensive and difficult of mass production. Wet chemical method has several advantage such as simple process, mass production, low temperature process, and low cost. In the present work, ZnO nanorods are deposited on ITO/glass substrate by simple wet chemical method. The process is perfomed by two steps. One-step is deposition of ZnO seeds and two-step is growth of ZnO nanorods on substrates. In order to form ZnO seeds on substrates, mixture solution of Zn acetate and Methanol was prepared.(one-step) Seed layers were deposited for control of morpholgy of ZnO seed layers by spin coating process because ZnO seeds is deposited uniformly by centrifugal force of spin coating. The seed-deposited samples were pre-annealed for 30min at $180^{\circ}C$ to enhance adhesion and crystallinnity of ZnO seed layer on substrate. Vertically well-aligned ZnO nanorods were grown by the "dipping-and-holding" process of the substrates into the mixture solution consisting of the mixture solution of DI water, Zinc nitrate and hexamethylenetetramine for 4 hours at $90^{\circ}C$.(two-step) It was found that density and morphology of ZnO nanorods were controlled by manipulation of ZnO seeds through rpm of spin coating. The morphology, crystallinity, optical properties of the grown ZnO nanostructures were carried out by field-emission scanning electron microscopy, high-resolution electron microscopy, photoluminescence, respectively. We are convinced that this method is complementing problems of main techniques of existing reports.

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Fluid Inclusion Study of the Samcheonpo Amethyst Deposit of Kyongsangnamdo, Korea (경상남도 삼천포 광산의 자수정에 대한 유체포유물 특성)

  • Bae, Yun-Sue;Yang, Kyoung-Hee
    • Journal of the Mineralogical Society of Korea
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    • v.19 no.3 s.49
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    • pp.153-162
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    • 2006
  • Fluid inclusions in amethyst from the Samcheonpo amethyst deposit of the Waryongsan area, Kyongnam generally grouped into four different types: Type I (liquid-rich and $10{\sim}23wt%$ NaCl, $Th=289{\sim}359^{\circ}C$), Type II (vapor-rich and $2{\sim}10wt%$ NaCl, $Th=304{\sim}365^{\circ}C;$), Type III (halite-bearing, $31{\sim}54wt%$ NaCl, $Th=259{\sim}510^{\circ}C;$), and Type IV ($CO_{2}-bearing\;9{\sim}13wt%\;NaCl,\;126{\sim}277^{\circ}$). Type I, II, and III inclusions are confined in the lower part of the amethyst and Type IV in the upper, which indicates significant hydrothermal activity during the earliest stage of the amethyst growth or the solidus condition of granitic rocks. The earliest fluid exsolved from the crystallizing granitic magma formed Type IIIa which is spatially associated with silicate melt inclusions. The homogenization behavior of Type IIIa inclusions by dissolution of the halite crystal after the bubble disappearance indicates that Type IIIa inclusions were trapped at some relatively elevated pressure. Exsolution of Type IIIb, I, II forming fluids with gradual decrease in their salinity was followed. The last fluid was $CO_{2}-bearing$ fluid (Type IV), which is assumed to be derived by decarbonization reactions with the surrounding sedimentary rocks. It suggests that the fine-grained granitic rocks containing the Samcheonpo amethyst crystallized at the sub-solvus condition saturated with water and exsolved abundant water.

Effect of SiC Crystal Phase on Growing ZSM-5 on the Surface of SiC (탄화규소 결정상의 종류가 탄화규소 표면에 ZSM-5가 형성되는데 미치는 영향)

  • Jung, Eunjin;Lee, Yoon Joo;Kim, Younghee;Kwon, Woo Teck;Shin, Dong-Geun;Kim, Soo Ryong
    • Korean Chemical Engineering Research
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    • v.53 no.2
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    • pp.247-252
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    • 2015
  • ZSM-5 crystals grew on the surface of ${\alpha}$-SiC and ${\beta}$-SiC particles by hydrothermal synthesis method. SiC particles which were > $50{\mu}m$ of size were used, and oxide layer were developed on the surface of the particles to induce growth of ZSM-5 from the surface. Then, synthesis time and temperature condition were considered growing ZSM-5. In this study, oxide layer was formed on ${\beta}$-SiC at $900^{\circ}C$ in air, and it was controlled to grow ZSM-5 grew from the ${\beta}$-SiC surface with $150^{\circ}C$ synthesis condition. This is due to Si-O-Si or Si-O-Al bond, which is basic framework of ZSM-5 can be easily formed, from the silicon oxide film on the surface of ${\beta}$-SiC. When the synthesis temperature was $200^{\circ}C$, the size of ZSM-5 was increased, and it covered much area of the SiC surface with better crystal shapes with longer synthesis time.

Pervaporation of n-Butanol/water Mixture through Organophilic ZSM-5 Zeolite Membrane (소수성 ZSM-5 제올라이트 분리막을 이용한 n-부탄올/물 혼합물의 투과증발)

  • Cho, Moon-Hee;Kong, Chang-In;Lee, Yong-Taek
    • Membrane Journal
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    • v.21 no.4
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    • pp.336-344
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    • 2011
  • Organophilic ZSM-5 membrane was synthesized on the inside of a porous stainless steel support by a hydrothermal secondary growth with seed crystals. They are used to separate n-butanol from its aqueous solution. Pervaporation characteristics such as a permeation flux and a separation factor are investigated as a function of the feed concentration and the operating temperature. The concentration of n-butanol was changed from 0.001 mole fraction to 0.015 mole fraction with an interval of 0.005 mole fraction; the operating temperature was controlled to be 25C, $35^{\circ}C$ and $45^{\circ}C$. When the operating temperature was $45^{\circ}C$, the flux of n-butanol significantly increased from 2 to $27g/m^2/hr$ as the mole fraction of n-butanol in the feed side increased from 0.001 to 0.015. Consequently, the concentration of n-butanol in the permeate substantially increased from 0.0016 to 0.052 mole fraction. When the feed concentration was 0.015, the flux of n-butanol significantly increased from 13 to $27g/m^2/hr$ as the operating temperature increased from $25^{\circ}C$ to $45^{\circ}C$. As a result, the concentration of n-butanol in the permeate also increased from 0.045 to 0.052 mole fraction.

Synthesis of Na-A type Zeolite From Melting Slag (소각재 용융슬래그를 이용한 제올라이트 Na-A의 합성)

  • Jang Young-Nam;Chae Soo-Chuu;Bae In-Kook;Ryou Kyung-Won
    • Journal of the Mineralogical Society of Korea
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    • v.18 no.1
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    • pp.11-17
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    • 2005
  • Na-A zeolite were synthesized from melting slag of the incinerated ash by the alkaline activation processes. The experiments were performed in stainless steel vessels, with continuous stirring during the reaction periods. The silica-rich solution, a starting material, which was the waste of crystal growth factory, contains 5.7 wt% SiO₂ and 3.2 wt% Na₂O. And NaAlO₂ was made by the reaction of aluminium dross and NaOH solution and its molar ratios were Na₂O/Al₂O₃= 1.2 and H₂O/Na₂O=9. During the residence time of 7∼8 h at 80℃, the mixing of the silica-rich solution, NaAlO₂ and melting slag yields the production of homogeneous Na-A zeolite. The optimal reactant composition in molar ratio of Na₂O:Al₂O₃:SiO₂ was 1.3∼l.4 : 0.8∼0.9 : 2 and mixing ratio of solution and slag was 1/7∼10 (g/cc). Synthesized Na-A zeolite has cubic form uniformly and its size ranges about 1 ㎛. Ca/sup 2+/ ion exchange capacity of the Na-A was about 180∼210 meq/100g, corresponding approximately 80% to the commercial detergent builder.

Synthesis of ceramic particles by hydrothermal method (수열법에 의한 세라믹분말 합성)

  • 김판채;최종건
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 1996.06b
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    • pp.219-222
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    • 1996
  • 수열법은 밀폐용기중에서 10$0^{\circ}C$이상의 가열, 가압된 수용액이 반응에 관여하는 것으로써, 수정, CaCO3, AlPO4, GaPO4 등과 같은 단결정의 육성 뿐만 아니라 균일분산계로부터 균일한 결정성의 미립자 합성에도 폭넓게 이용되고 있다. 세라믹분말의 합성에 있어서, 이 방법은 특히 형상, 입자크기의 제어가 용이할 뿐만 아니라 고상법, 졸-겔법, 공침법에서와 같은 열처리, 분쇄과정이 필요없기 때문에 고순도의 초미립자를 얻을 수 있는 장점이 있다. 근년 미국, 일본에서는 수열법을 이용한 유전, 압전체 등 세라믹분말의 일부가 공업적인 규모로 대량 생산되고 있다. 그러나 이에 대한 국내 기술은 아직 초기단계에 이르고 있는 실정이다. 따라서 본 연구실에서는 수열법에 의한 단결정 육성 (예; 자수정, CaCO3, AlPO4, GaPO4, KTP, Emerald 등), 박막제조 (예; GaP, PbTiO3, BaTiO3 등), 정제 (고령토, 장석, 도석 등), 원석처리 (진주, 인공 emerald, 비취 등) 그리고 각종 세라믹분말의 합성 등과 같은 다양한 기반기술의 축적과 동시에 공업화에 대응한 수열장치를 위하여 반응용기의 대형화, 엄밀한 밀폐방식, 실용적인 수열조건 등을 개발해 오고 있다. 본 발표에서는 현재까지의 연구개발 내용 중에서 결정성 미립자에 관련한 세라믹분말의 합성에 대한 일부의 결과들을 보고한다. 일반적으로 수열장치는 전기로, 반응용기, 온도 및 압력제어계 등을 기본으로 하고 있으며 시판용의 대부분이 교반기가 부착된 수직형 (vertical type)이다. 이와 같은 방식에 있어서는 엄밀한 밀폐가 곤란, 반응온도의 한계성 (25$0^{\circ}C$ 이하), 증진율의 한계성 (소량생산) 등과 같은 점이 있기 때문에 본 연구실에서는 개폐식 전기로내에 엄밀한 밀폐가 가능한 수평식(horizontal type)의 반응용기를 채택한 뒤 이를 회전 또는 시이소(seesaw)식으로 움직일 수 있도록 하여 연속공정화, 온도구배의 자율조절 그리고 보다 저온에서도 인위적인 이온의 확산을 효율적으로 유도할 수 있도록 하였다. 이와 같은 방식은 기존의 방식과 비교하여 반응용기 내에 응집현상과 미반응물이 존재하지 않으며 또한 단분산으로 결정성 미립자를 대량적으로 얻을 수 있는 장점이 있었다. 다음은 이상과 같이 본 연구실에서 자체 개발한 수열장치를 이용하여 PbTiO3, (Pb,La)TiO3Mn, BaTiO3, ZnSiO4:Mn, CaWO4 등과 같은 세라믹분말에 대한 합성 실험의 결과이다. 압전성, 초전성이 우수한 PbTiO3 및 (Pb,La)TiO3:Mn 분말의 수열합성은 PbO, TiO2, La2O3 등의 분말을 출발원료로 하여 합성도도 25$0^{\circ}C$부근의 알카리성 용액중에서 결정성 PbTiO3 및 (Pb,La)TiO3:Mn 미립자를 단상으로 얻었으며 입자의 형상 및 크기는 합성온도와 수열용매의 종류에 의존하였다. 유전체로서 폭넓게 응용되고 있는 BaTiO3 분말은 Ba(OH)2.8H2O, TiO2와 같은 최적의 출발원료를 선택함으로써 15$0^{\circ}C$ 부근의 저온영역에서도 용이하게 합성할 수 있었다. 특히 본 연구에서는 수용성인 Ba(OH)2.8H2O를 사용함으로써 host-guest적인 반응을 유도시키는데 있어 물의 가장 실용적이고 효과적인 수열용매임도 알았다. ZnSiO4:Mn, CaWO4, MgWO4와 같은 형광체 분말은 공업적으로 고상반응 또는 습식법에 의해 얻어지고 있으나 이들 방법에 있어서는 분쇄공정으로 인한 형광특성의 저하와 같은 문제점이 있다. 따라서 본 연구에서는 수열법을 이용하여 이들 화합물의 합성을 시도하였으며 그 결과 합성온도 30$0^{\circ}C$ 부근의 알칼리성 용액중에서 수열적으로 얻어짐을 알았다. 여기서의 합성분말을 이용하여 실제 조명램프로 제조한 결과 녹색, 청색 발광용 형광체로서 우수한 형광특성을 나타내었다. 천연에서 소량 산출되고 있는 고가의 (Li,Al)MnO2(OH)2:Co 분말은 도자기의 전사지용 청색안료로써 이용되고 있다. 본 연구실에서는 LiOH.H2O, Al(OH)3, MnO2 등의 분말을 출발원료로 하고 24$0^{\circ}C$ 온도 부근 그리고 물을 수열용매로 하여 천연산에 필적하는 (Li,Al)MnO2(OH)2:Co 분말을 인공적으로 합성하였다.

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Screening of the Antimicrobial and Antitumor Activity of Xanthium strumarium L.Extract (한국산 도꼬마리 추출물로부터 항균.항암물질의 탐색)

  • 김현수;유대식;이인선;김용원;여수환
    • KSBB Journal
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    • v.18 no.1
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    • pp.55-61
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    • 2003
  • To isolate and purify the antimicrobial and antitumor agents in Xanthium strumarium L. hydrothermal extract. The crude extract was extracted in ether or ethylacetate under neutral, acidic, and alkali conditions. The antimicrobial activity of each extract was tested against 16 strains of bacteria, 2 strains of yeast, and 2 strains of fungus. The ether neutral extract (XE-N) exhibited the strongest growth inhibition upon the 8 strains of gram-positive bacteria, 6 strains of gram-negative bacteria and Cryptococcus neoformans. Fluorescein diacetate (FDA) testing of XE-N and XEA-N showed growth inhibition of the 3 strains of E. coli, S. aureus and C. albicans even at 30 ng/mL, with the exception of p. aeruginosa. XE-N-S1 and XE-N-S3 from neutral ether extract (XE-N), XE-N-S3 from the acidic ether extract (XE-A), and XEA-N-S1 from ethylacetate (XEA-N) were purified as antimicrobial and antitumor agents. However all purified compounds decomposed with the exception of XE-N-S1. The results upon the antitumor activities of the crude extract and of its purified compounds, showed that XE-N-S1 had the best antitumor activity against HeLa cells. In terms of antitumor activity against HepG2 cells, XE-N-S1 and XE-N-S3 were superior, and against HT29 cells XE-N and XE-N-Sl were good, against Saos2, NCI H522, NCI H1703, Clone M3 cells XE-N-51 was very good, and against LN CAP cells XE-N-S3 was the best. Comparing of cellular toxicities various extracts and purified compounds with the existing antitumor agents, XE-A, XEA-A and XEA-B had the lowest toxicity, and XE-B had a lower toxicity than etoposide. XE-N-S1 and XE-N-S3 showed higher toxicities than etoposide, and the toxicity of XE-A-S3 was higher than that of etoposide, and lower than that of csplatin.