• Title/Summary/Keyword: Hydrothermal crystallization

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The Effects of Temperature and Pressure on Synthesis of Zeolite 4A from Coal Fly Ash by Hydrothermal Reaction (석탄 비산회로부터 수열법에 의한 제올라이트 4A의 합성시 온도와 압력의 영향)

  • Yoon, Cheol;Yeon, Ik-Jun;Kim, Kwang-Yul
    • Journal of the Korean Applied Science and Technology
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    • v.16 no.3
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    • pp.217-221
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    • 1999
  • This study was carried out to synthesis the zeolite using the bituminous coal fly ash emitted from power plant that occurs several environmental problems. In spite of fly ash has contained high content of $SiO_2$ and $Al_2O_3$, it disposed mainly landfill. If the effective methods to recover the $SiO_2$ and $Al_2O_3$ were developed, the fly ash could be utilized valuable raw materials. In this study, fly ash was used as raw material to synthesize the zeolite by pressurized hydrothermal reaction. Also, experimental parameters included temperature($70{\sim}110^{\circ}C$, and pressure($140{\sim}200$ psi) of crystallization were investigated. The more crystallization pressure was increased, the more Zeolite 4A was synthesized at 70 and $90^{\circ}C$. Zeolite 4A of metastable phase tend to be transformed into sodalite of stable phase at $110^{\circ}C$.

Mineral Phases and Phase Diagram of Hydrothermal Alteration Zone in Geodo Mine, Korea (거도광산 열수변질대의 광물상과 상평형 연구)

  • 최진범;김수진
    • Journal of the Mineralogical Society of Korea
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    • v.16 no.1
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    • pp.49-63
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    • 2003
  • Rare and unusual occurrence of hydrothermal minerals were found in Geode mine area. They are developed in the late stage of hydrothermal alteration of earlier skarns and later by the open-space filling crystallization. The alteration of earlier skarns of clinopyroxene, garnet, and plagioclase formed mainly chlorite or sometimes uncommon hydrothermal minerals of prehnite, illite, and pumpellyite. Open-space filling crystallization characterized by hydrothermal minerals developedin open sapce or good are prehnite, pumpellyite, clinozoisite, illite, and Ca-zeolites of stilbite annstellerite. Mineral phases and paragenesis are examined in detail by microscopy, XRD, SEM, and EPMA. Using the Schreinemaker's method, equibrium reactions among these minerals are establishedand isothemal-isobaric phase diagrams of $\mu$$H_2O$-$\mu$$CO_2$cot are plotted. Hydrothermal minerals such asprehnite, pumpellyite, clinozoisite, illite, and some chlorite were ffrmed under high partial pressure of $CO_2$with relatively low $H_2$O fugacity. Later, stilbite and calcite in association with illite crystallized under relatively both high partial Pressure of $CO_2$and high $H_2$O fugacity.

The Sannae-Eonyang Granitic Rocks and Hydrothermal System, Southeastern Kyongsang Basin

  • Yang, Kyoung-Hee;Lee, Joon-Dong
    • Economic and Environmental Geology
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    • v.33 no.1
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    • pp.19-30
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    • 2000
  • The Sannae-Eonyang granitic rocks are a large fossil hydrothermal system containing the Sannae Mo-W fissure-vein type and the Eonyang amethyst deposits in the southeastern Kyongsang Basin. They evolved through similar stages showing the similarities in chemical and mineralogical compositions, fractionation trends and early magmatic fluids. Major, trace and rare earth element(REE) variations can be accounted for fractional crystallization combined with variable degrees of metasomatism. Based on the aqueous fluids exsolved directly from the crystallizing melt, the Sannae-Eonyang granitic rocks were emplaced at similar depth or pressure conditions. High temperature fluid interaction with the granitic rocks affects the elements such as K, Na, Rb, Ba, Sr, Eu, and heavy REE (HREE) mostly through feldspar re-equilibration. Although hydrothermal fluids produced partly positive Eu anomalies and HREE depletion in the granitic rocks at the Sannae Mo-W mine, the chemical concentrations defining fractionnation trends have survived the effects of alteration. Aqueous fluids exsolved from the crystallizing melt appears to be widespread, whereas fluids of moderate to low salinity and low-density with relatively high homogenization temperatures and $Co_2$-rich fluids appear to be mainly restricted and responsible for Mo-W and amethyst mineralization, respectively. Hydrothermal system of the Sannae-Eonyang granitic rocks represents repeated fluid events; from exsolution of aqueous fluids from the crystallizing melt, through fluid immiscibility and meteoric convection to later mineralization.

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On the Possibility of Bulk Large Diamond Single Crystal Synthesis with Hydrothermal Process

  • Andrzej M. Szymanski
    • Journal of the Mineralogical Society of Korea
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    • v.10 no.1
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    • pp.18-32
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    • 1997
  • Analysis of geological data, relating to occurrence and formation of diamonds as well as host rocks, inclined author to have different outlook on the diamond genesis and to establish a proposition on their formation at pneumatolytic-hydrothermal conditions near superficial Earth zones. Based on that theoretical foundations and experimental works, the first low-pressure and low-temperature hydrothermal diamond synthesis from water solution in pressure autoclave was executed. As a result, the natural diamond seed crystal grew bigger ad coupling of the synthetic diamond single-crystalline grains were obtained. SEM documentation proofs that parallely paragenetic crystallization of quartz and diamond, and nucleation of new octahedral diamond crystals brush take place on the seed crystal surface. Forecast of none times growth of diamond industrial application at 2000 and seventeen times at 2010 with reference to 1995, needs technology of large and pure single-crystals diamond synthesis. Growth of the stable and destressed diamond single-crystals in the pseudo-metastable diamond plot, may be realized with processes going through the long time and with participation of free radicals catalysts admixtures only. Sol-gel colloidal processes are an example of environment which form stable crystals in thermodynamically unstable conditions through a long time. Paper critically discusses a whole way of studies on the diamond synthesis, from high-pressure and high-temperature processes through chemical vapour deposition up to hydrothermal experiments.

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Synthesis of Nanoparticles via Surface Modification for Electronic Applications

  • Lee, Burtrand I.;Lu, Song-Wei
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 2000.06a
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    • pp.35-58
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    • 2000
  • The demand for sub-micrometer or nanometer functional ceramic powders with a better suspension behavior in aqueous media in increasing. Redispersible barium titanate (BT) nanocrystals, green light emitting Mn2+ doped Zn$_2$SiO$_4$ and ZnS nanoparticle phosphors were synthesized by a hydrothermal method or chemical precipitation with surface modification. The nanoparticle redispersibility for BT was achieved by using a polymeric surfactant. X-ray diffraction(XRD) results indicated that the BT particles are of cubic phase with 80 nm in size. XRD results of zinc silicate phosphor indicate that seeds play an important role in enhancing the nucleation and crystallization of Zn$_2$SiO$_4$ crystals in a hydrothermal condition. This paper describes and discuss the methods of surface modification, and the resulting related properties for BT, zinc silicate and zinc sulfide.

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Preparation and Magnetic Properties of Ba-Ferrite Particles Using the Supercritical Water Crystallization Method

  • Nam, Sung-Chan;Kim, Kun-Joong;Park, Sang-Do
    • Proceedings of the Korean Magnestics Society Conference
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    • 2000.09a
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    • pp.433-440
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    • 2000
  • Barium ferrite particles were synthesized from Ba(NO$_3$)$_2$, Fe(NO$_3$)$_3$ and KOH mixed solutions using hydrothermal crystallization in supercritical water. The experimental apparatus for production of barium ferrite is a flow-type apparatus. Fine barium ferrite particles were produced because supercritical water causes the metal hydroxides to be rapidly dehydrated before significant growth takes place. The effects of Fe/Ba ratio and reaction time on the formation, particle size, and magnetic properties of barium ferrite were studied. When Fe/Ba ratio were varied from 0.5 to 12, single-phase barium ferrite powder was only produced in the range of 0.5〈Fe/Ba〈2. Also, with elevating reaction time, the BaO.6Fe$_2$O$_3$ particle size grew smaller. Especially, uniform barium hexaferrite particles of size 100-200nm were obtained at 80sec. In this study, therefore, single-phase barium ferrite particles are highly stable and can be produced continuously in a reaction time of less then 2min.

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Hydrothermal crystallization and secondary synthesis of vanadium containing zeolites (바나듐함유 제올라이트의 수열결정화 및 2차처리합성)

  • Kim, Geon-Joong
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.7 no.3
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    • pp.437-448
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    • 1997
  • The substitution of vanadium atoms into the zeolite framework structure could be applied to the large pore zeolites by means of modified treatments as well as direct hydrothermal synthesis. The incorporation of V into the zeolite framework was demonstrated by instrumental analysis techniques. The result of X-ray diffraction analysis showed that the unit cell parameters increased after incorporation of vanadium into the zeolitic lattice, indicating that the replacement of Si by the larger V atoms could cause a slight expansion in the unit cell. In addition, the results of FTIR, Uv-Vis and Si-MAS-NMR spectra strongly support the incorporation of V into the zeolite framework. Acid leaching of aluminum in zeolites can provide a vacant position in the lattice for the insertion of vansdium by secondary hydrothermal treatment.

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Electrochemical properties of $LiFePO_4$ cathode materials by hydrothermal route

  • Jin, Bo;Li, Hu;Park, Kyung-Hee;Gu, Hal-Bon;Park, Bok-Kee
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2007.06a
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    • pp.363-364
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    • 2007
  • Phospho-olivine $LiFePO_4$ cathode materials were prepared by hydrothermal reaction at different temperatures. The structural performance of $LiFePO_4$ powders were characterized by X-ray diffraction (XRD). $LiFePO_4$/Li batteries were characterized electrochemically by charge/discharge experiments. The XRD results demonstrate that $LiFePO_4$ powder has an orthorhombic olivine-type structure with a space group of Pnmb. Among the synthesized cathode materials, $LiFePO_4$synthesized at $170^{\circ}C$ and subsequently annealed at $500^{\circ}C$ shows the best electrochemical properties. It shows initial discharge capacity of $167\;mAh\;g^{-1}$ (98% of the theoretical capacity) close to the theoretical capacity of $LiFePO_4$ ($170\;mAh\;g^{-1}$) at 0.1 C rate, which is ascribed to the enhanced degree of crystallinity, better phase purity, more spherical and more finely dispersed nanoparticles, crystallization and activation of small amount impurity.

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Synthesis and crystallization of nanosized zirconia powder using hydrothermal process (수열반응에 의한 나노 지르코니아 분말의 합성 및 결정화)

  • 노희진;이종국;서동석;황규홍
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.12 no.3
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    • pp.126-132
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    • 2002
  • The nanocrystalline zirconia powder with anisotropic shapes was synthesized by hydrothermal treatment of the tetragonal zirconia prepared by aging the zirconium hydroxide precipitate, which was obtained from the reaction between $ZrOCl_2{\cdot}8H_2O$ and KOH solutions under the fixed pH of 13.5, at $100^{\circ}C$ for 24 h. With increasing the hydrothermal reaction temperature and time, the fraction of tetragonal phase with spherical zirconia decreased, whereas, relatively the fraction of monoclinic phase with spindle-like and rod shape zirconia increased. As increased concentration of the NaOH solution it promoted the particle size to become larger and the crystalline phase to transform tetragonal to monoclinic. However, the specific surface area at the early stage of the reaction increased and subsequently decreased because of grain growth in powder with longer reaction time.

Synthesis of FAU(Faujasite)-type Zeolite with Variation of Synthesis Condition (합성조건의 변화에 따른 FAU(Faujasite)형 제올라이트의 합성)

  • 임형미;김봉영;남중희;안병길;오성근;정상진
    • Journal of the Korean Ceramic Society
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    • v.40 no.2
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    • pp.132-138
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    • 2003
  • The effect of synthesis condition, type of starting materials, mole ratio, mixing. aging, and crystallization temperature and time, on the size of FAU-type zeolite has been studied. Different mixing route may lead to the different phase of zeolite even with the same starting materials. In general, the size of particles is smaller after aging, especially at lower aging temperature. Two step mixture gel preparation method resulted to not only the reduction of crystallization time but also that of particle size, but without the aging of two mixture gels before the preparation of the overall gel in the second step, only the crystallization time was reduced, not the particle size. The FAU-type zeolite with average particle size 0.4$\mu$m and BET surface area 838 $m^2$/g was obtained from starting materials of liquid sodium silicate, sodium aluminate, and sodium hydroxide with two step preparation of mixture gel, aging of the mixture gels in two steps, which effectively reduced the crystallization time and particle size.