• Title/Summary/Keyword: Hydrothermal crystallization

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Preparation of A and Y type zeolite film by hydrothermal crystallization (수열결정화법에 의한 A 및 Y형 제올라이트 박막의 제조)

  • 김건중;박노춘;안화승;남세종
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.8 no.1
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    • pp.55-63
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    • 1998
  • A and Y type zeolitic crystal films were synthesized on porous supports from the reaction mixture of 1.9 $SiO_2-1.5\;Na_2O-Al_2O_3-40\;H_2O$ and 10 $SiO_2-7\;Na_2O-Al_2O_3-280\;H_2O$ composition, respectively. The zeolite film was characterized by XRD and SEM. The crystals grown on the porous matrix were very closely bound together and the thickness of membrane was about 8-15$\mu \textrm{m}$. The densely intergrown crystals could be also synthesized by the hydrothermal treatment at $100^{\circ}C$ after pressing the reaction mixture without addition of water. A zeolite membrane crystallized as a thin film showed the selective permeability of water from water and methanol mixture through the molecular sieving activity of micropores.

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Influence of Alumina on Hydrothermal Synthesis of 11Å Tobermorite (알루미나가 11Å Tobermorite의 수열합성에 미치는 영향)

  • Yim Going;Yim Chai Suk
    • Korean Journal of Materials Research
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    • v.15 no.2
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    • pp.97-105
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    • 2005
  • [ $11\AA$ ] tobermorite$(5CaO{\cdot}6SiO_2{\cdot}5H_2O)$ is synthesized from the mixtures of calcium hydroride and quartz using alumina in a molar ratio $Ca(OH)_2/SiO_2$ of 0.8 at $180^{\circ}C$ for 8 and 24 hrs under saturated steam pressure. The influence of alumina on the formation of $11\AA$ tobermorite was investigated by X-ray diffraction, differential thermal analysis and infrared spectroscopy. $11\AA$ tobermorite containing increasingly larger amounts of aluminum showed a shift of the basal spacing from 11.3 to $11.6\AA$. In general, there was a direct linear relation between the basal spacing and added content of alumina. The differential thermal analysis curves showed that $11\AA$ tobermorite with increasing alumina contents exhibited the exothermic peak at high temperature, namely $11\AA$ tobermorite containing aluminum gave a sharp exothermic peak at temperature around $850\~860^{\circ}C$ in the case of $S_3\~S_5$. The absorption band at $1607\~1620cm^{-1}$ is attributed to the bending vibration of water, and the position of the main O-H stretching and Si-O lattice vibration of $11\AA$ tobermorite at 3500 and $965cm^{-1}$ respectively is not altered. Consequently the existence of alumina accelerates the crystallization of $11\AA$ tobermorite, and that the aluminum ion appears to substitute for the silicon ion in $11\AA$ tobermorite structure. Al-containing tobermorite is distinguished from Al-free tobermorite.

Synthesis and Characterization of Fe Doped TiO2 Nanoparticles by a Sol-Gel and Hydrothermal Process

  • Kim, Hyun-Ju;Jeong, Kwang-Jin;Bae, Dong-Sik
    • Korean Journal of Materials Research
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    • v.22 no.5
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    • pp.249-252
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    • 2012
  • Fe doped $TiO_2$ nanoparticles were prepared under high temperature and pressure conditions by mixture of metal nitrate solution and $TiO_2$ sol. Fe doped $TiO_2$ particles were reacted in the temperature range of 170 to $200^{\circ}C$ for 6 h. The microstructure and phase of the synthesized Fe doped $TiO_2$ nanoparticles were studied by SEM (FE-SEM), TEM, and XRD. Thermal properties of the synthesized Fe doped $TiO_2$ nanoparticles were studied by TG-DTA analysis. TEM and X-ray diffraction pattern shows that the synthesized Fe doped $TiO_2$ nanoparticles were crystalline. The average size and distribution of the synthesized Fe doped $TiO_2$ nanoparticles were about 10 nm and narrow, respectively. The average size of the synthesized Fe doped $TiO_2$ nanoparticles increased as the reaction temperature increased. The overall reduction in weight of Fe doped $TiO_2$ nanoparticles was about 16% up to ${\sim}700^{\circ}C$; water of crystallization was dehydrated at $271^{\circ}C$. The transition of Fe doped $TiO_2$ nanoparticle phase from anatase to rutile occurred at almost $561^{\circ}C$. The amount of rutile phase of the synthesized Fe doped $TiO_2$ nanoparticles increased with decreasing Fe concentration. The effects of synthesis parameters, such as the concentration of the starting solution and the reaction temperature, are discussed.

Synthesis of Gallosilicate(Ga-MFI} and Its Comparison with ZSM-5 (갈리실리케이트(Ga-MFI)의 합성 및 ZSM-5와의 비교)

  • Kim, Young-Kook;Hwang, Jae-Young;Kim, Myung-Soo;Park, Hong-Soo;Hahm, Hyun-Sik
    • Journal of the Korean Applied Science and Technology
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    • v.21 no.3
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    • pp.231-237
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    • 2004
  • Ga-MFI was synthesized by a hydrothermal process at atmospheric pressure. The effect of mole ratios of reactants on crystallization was also investigated thoroughly. The characteristics of synthesized Ga-MFI was compared with ZSM-5. The synthesis of Ga-MFI was carried out with five different mole-compositions of $\underline{a}SiO_2-\underline{b}Ga_2O_3-\underline{c}Na_2O-\underline{d}TPA_2o-\underline{e}H_2O$. The synthesized Ga-MFI and ZSM-5 were characterized by XRD and FT-IR. The inorganic cation ($Na^+$) and water played an important role in crystallinity and the organic cation ($TPA^+$) as a template played a great influence on yields. With the increase in the amount of $Ga^{3+}$, crystallization time was increased. With a fixed $SiO_2/Ga_2O_3$ ratio of 400, the optimum reaction condition was obtained at $H_2O/SiO_2$=30${\sim}$35, $Na_2O/SiO_2$=0.5${\sim}$0.6, and $TPA_2O/Na_2O$=1${\sim}$1.25. In these cases, the crystallinity and yield were more than 95% and 90%, respectively. By comparing IR spectrum of Ga-MFI with those of ZSM-5 and silicalite, it was found that Ga-MFI showed a unique peak at 970 $cm^{-1}$, which may be used to identify Ga-MFI from ZSM-5 and silicalite.

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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Study on the Metal Ore Deposits of Gyeongsang buk-do Area (경상북도(慶尙北道) 일원(一圓)에 부존(賦存)하고 있는 금속지하자원(金屬地下資源)의 지질광상학적(地質鑛床學的) 연구(硏究))

  • Kim, Y.K.;Lee, J.Y.;Kim, S.W.;Koh, I.S.
    • Economic and Environmental Geology
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    • v.9 no.3
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    • pp.143-156
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    • 1976
  • The Cretaceous metal ore deposits in the Gyeongsang basin of Gyeongsangbuk-do are characterized by the formation of metallogenic provinces which show zonal distribution pattern around Yeonil province where pneumatolytic type is dominated and hydrothermal type are distributed in the order of decreasing temperature type outward. Some Cretaceous granitic rocks include zoned alkali feldspars which reflect rapid variation of $H_2O$ during emplacement and crystallization of the water-saturated granitic magma. The ore deposits are considered to be originated from upward transportation of ore solution from the excess of water exhausted from uprising magma, which seems to be intimately related to the fact that the majority of the ore deposits in Daegu area are cummulated around the granites including zoned alkali feldspars. In order to collect geochemical data necessary for geochemical exploration in the study area, certain trace elements were chosen as pathfinders from monzonite and soil in the vicinity of Dalsung Tungsten Mine by studying the dispersion patterns of trace elements: Ba and Sr show trends to decrease toward ore deposit while Cu, Pb, and Mo increase. Around mining area there are distributed apparently Equisetum arvense Linne and Mentha sachinensis Kudo which may be used as index plants. In the viewpoint of geologic structure, the trends of the ore veins in contact aureole around the Palgongsan granite body correspond with the pre- and syn- plutonism joint pattern in hornfels in the area.

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Study of Preparation of BaTiO$_3$ Powder using Hydrothermal methods - Estimation of Crystallization with Concentrations (수열합성법에 의한 BaTiO$_3$ 제조 - 농도변화에 따른 결정성 평가)

  • 남성찬;최정묵;박정훈;김종기;박상도;김홍국
    • Proceedings of the Korea Society for Energy Engineering kosee Conference
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    • 2002.11a
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    • pp.165-169
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    • 2002
  • BaTiO$_3$ 분말을 Ba(OH)$_2$ㆍ8$H_2O$와 아나타제형의 TiO$_2$$\chi$$H_2O$를 이용하여 광화제 첨가 없이 열수처리에 의한 탈수(dehydration) 및 재결정화(recrystallization) 과정을 통한 수열합성법에 의해 제조하였다. Autoclave 반응기를 이용한 실험의 경우, BaTiO$_3$ 분말을 생성하기 위한 최적 반응온도 및 시간은 각각 21$0^{\circ}C$, 4시간으로 확인되었으며, 이 때 생성된 BaTiO$_3$ 분말의 크기는 0.1~0.2$mu extrm{m}$로 입도분포가 양호하였다. 그리고, 바륨과 티타늄의 농도비가 증가됨에 따라 결정화도(tetragonality)가 증가하는 경향을 나타내고 있다. 이는 반응하지 않고 남아 있는 바륨의 영향으로 생각되며, 이는 반응물의 pH와도 관련이 있다. 또한, 반응온도 및 시간도 결정화도에 커다란 영향을 미치는 변수로 주로 반응온도 및 시간이 증가함에 따라 결정화도도 함께 증가하는 추세를 나타내고 있다.

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Synthesis of KIT-1 Mesoporous Silicates Showing Two Different Macrosporous Strucrtues; Inverse-opal or Hollow Structures (거대기공 구조-역오팔 또는 중공 구조를 갖는 KIT-1 메조포러스 실리케이트의 제조)

  • Baek, Youn-Kyoung;Lee, Jung-Goo;Kim, Young Kuk
    • Journal of Powder Materials
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    • v.23 no.3
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    • pp.189-194
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    • 2016
  • We report a facile method for preparing KIT-1 mesoporous silicates with two different macroporous structures by dual templating. As a template for macropores, polystyrene (PS) beads are assembled into uniform three dimensional arrays by ice templating, i.e., by growing ice crystals during the freezing process of the particle suspension. Then, the polymeric templates are directly introduced into the precursor-gel solution with cationic surfactants for templating the mesopores, which is followed by hydrothermal crystallization and calcination. Later, by burning out the PS beads and the surfactants, KIT-1 mesoporous silicates with macropores are produced in a powder form. The macroporous structures of the silicates can be controlled by changing the amount of EDTANa4 salt under the same templating conditions using the PS beads and inverse-opal or hollow structures can be obtained. This strategy to prepare mesoporous powders with controllable macrostructures is potentially useful for various applications especially those dealing with bulky molecules such as, catalysis, separation, drug carriers and environmental adsorbents.

Crystal Growing of NaX type Zeolite

  • Ha, Jong-Pil;Seo, Dong-Nam;Kim, Seong-Yong;Jung, Mi-Jeong;Moon, In-Ho;Cho, Sang-Joon;Park, Hyun-Min;Kim, Ik-Jin
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 1999.06a
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    • pp.351-360
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    • 1999
  • A large NaX type zeolite crystal of a uniform particle size of 20${\mu}{\textrm}{m}$ are grown with various H2O content by hydrothermal reaction and added seed crystal (2~3 ${\mu}{\textrm}{m}$) to reactant solution as a function of different adding seed levels from 3 to 15 %. The result that increased purity of NaX zeolite above 95% and homogeneity of crystal size by increasing adding seed levels, also decreased crystallization time. It was explained that adding seed to synthesis solution leaded out increase of surface area of physical contact reaction and directed growth of seed crystal, so more rapid consumption of reaction gel as increase seeding levels.

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Crystal growing of NaX type zeolite

  • Ha, Jong-Pil;Seo, Dong-Nam;Jung, Mi-Jeong;Moon, In-Ho;Cho, Sang-Joon;Park, Hyun-Min;Kim, Ik-Jin
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.9 no.4
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    • pp.371-376
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    • 1999
  • A large NaX type zeolite crystal of a uniform particle size of 20$\mu\textrm{m}$ are grown with various {{{{{H}_{2}O}}}} content by hydrothermal reaction and added seed crystal (2~3$\mu\textrm{m}$) to reactant solution as a function of different adding seed levels from 3 to 15%. The result that increased purity of NaX zeolite above 95% and homogeneity of crystal size by increasing adding seed levels, also decreased crystallization time. It was explained that adding seed to synthesis solution leaded out increase of surface area for physical contact reaction and directed growth of seed crystal, so more rapid consumption of reaction gel as increase seeding levels.

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