• Title/Summary/Keyword: low-temperature hydrothermal synthesis

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Hydrothermal Synthesis of 6mol% Yttria Stabilized Cubic ZrO2 Nano Powders (이트리아 안정화 지르코니아 나노 분말 합성)

  • Lee, Jae-Hoon;Bae, Sung-Hwan
    • Korean Journal of Materials Research
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    • v.27 no.8
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    • pp.445-450
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    • 2017
  • YSZ (Yttria-stabilized zirconia) is a ceramic material that is used for electronic and structural materials due to its excellent mechanical properties and specific electrical characteristics according to the Yttrium addition. Hydrothermal synthesis has several advantages such as fine particle size, uniform crystalline phase, fast reaction time, low process temperature and good dispersion condition. In order to synthesize YSZ nanoparticles with high crystallinity, hydrothermal synthesis was performed at various concentrations of NaOH. The hydrothermal process was held at a low temperature ($100^{\circ}C$), with a short process time (2,4,8 hours); the acidity or alkalinity of solution was controlled in a range of pH 2~12 by addition of NaOH. The optimum condition was found to be pH 12, at which high solubility levels of Y(OH) and Zr(OH) were reported. The synthesized nano powder showed high crystallinity and homogenous composition, and uniform particle size of about 10 nm.

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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Magnetic Properties of Micron Sized Fe3O4 Crystals Synthesized by Hydrothermal Methods (수열합성을 이용하여 제작한 Fe3O4 결정입자의 자기적 특성)

  • Lee, Ki-Bum;Nam, Chunghee
    • Journal of Powder Materials
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    • v.26 no.6
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    • pp.481-486
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    • 2019
  • Iron oxides currently attract considerable attention due to their potential applications in the fields of lithiumion batteries, bio-medical sensors, and hyperthermia therapy materials. Magnetite (Fe3O4) is a particularly interesting research target due to its low cost, good biocompatibility, outstanding stability in physiological conditions. Hydrothermal synthesis is one of several liquid-phase synthesis methods with water or an aqueous solution under high pressure and high temperature. This paper reports the growth of magnetic Fe3O4 particles from iron powder (spherical, <10 ㎛) through an alkaline hydrothermal process under the following conditions: (1) Different KOH molar concentrations and (2) different synthesis time for each KOH molar concentrations. The optimal condition for the synthesis of Fe3O4 using Fe powders is hydrothermal oxidation with 6.25 M KOH for 48 h, resulting in 89.2 emu/g of saturation magnetization at room temperature. The structure and morphologies of the synthesized particles are characterized by X-ray diffraction (XRD, 2θ = 20°-80°) with Cu-kα radiation and field emission scanning electron microscopy (FE-SEM), respectively. The magnetic properties of magnetite samples are investigated using a vibrating sample magnetometer (VSM). The role of KOH in the formation of magnetite octahedron is observed.

Properties of Cement Mortar as Particle Size and Hydrothermal Synthesis Temperature Using Scheelite Tailing (중석 광미를 사용한 시멘트 모르타르의 입도 및 수열합성온도별 물리적 특성)

  • Chu, Yong Sik;Seo, Seong Gwan;Choi, Sung Bum;Kim, Gyoung man;Hong, Seok Hwan
    • Resources Recycling
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    • v.28 no.6
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    • pp.46-53
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    • 2019
  • Cement mortar was hydrothermal-synthesized with particle size of tailings using scheelite tailings deposited without proper treatment, and its physical properties were investigated. The mixing ratios of water-cement and sand-cement were fixed at 75 % and 400 %, respectively, during preparing cemnt mortar, and the sand was replaced by the tailings at 0 ~ 50 %. The particle size of tailings was controlled at 9.3 ~ 53.0 ℃, and the hydrothermal temperature was kept at 60 ~ 180 ℃ for 6 hours after the temperature increased to pretermined temperature with 2 ℃ heating rate. The compressive strength increased with increasing hydrothermal temperature. The compressive strengths were 55.2 MPa and 54.5 MPa when the mortars were prepared with 30 % low arsenic and high arsenic tailings after 60 min grinding. The compresiive strenght was enhanced 300 % compared with reference sample.

Cost effective and low energy consuming hydrothermal synthesis of Ni based MOF

  • Israr, Farrukh;Kim, Duk Kyung;Kim, Yeongmin;Oh, Seung Jin;Ng, Kim Choon;Chun, Wongee
    • Journal of Energy Engineering
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    • v.24 no.2
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    • pp.51-54
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    • 2015
  • The mesoporous metal organic framework structure of Ni-BTC was successfully synthesized in a low temperature and short operation time via hydrothermal synthesis process. Such operational route virtuously consumed less electrical and thermal energy. It proved time saving along with acceptable product yield (38%). The product was characterized through FESEM, FT-IR, XRD and $N_2$ gas adsorption measurement. Hightemperature stability of synthesized MOF was gauged by diffraction indexing of XRD patterns of as synthesized and heat treated samples of MOFs. The mathematically calculated particle size of Ni-BTC was found to be 42nm.

Hydrothermal Synthesis and Characterization of BaTiO3 Fine Powders (BaTiO3 미세 분말의 수열합성 및 특성분석)

  • Park, Jung-Hoon;Park, Sangdo
    • Korean Chemical Engineering Research
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    • v.45 no.5
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    • pp.448-454
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    • 2007
  • Hydrothermal synthesis was conducted with starting material as Barium hydroxide and hydrous titania ($TiO_2{\cdot}xH_2O$) to obtain barium titanate fine Powder. The conversion, crystal structure and properties of as-prepared powder were investigated according to reaction temperature, time and concentration. The effect of variables on conversion was in order of time < temperature < concentration and the maximum conversion reached to 99.5% in the case of hydrothermal synthesis at $180^{\circ}C$ for 2 h with 2.0 M reactant concentration. At low concentration such as 0.25 M, formation of unreacted $BaCO_3$ and $TiO_2$ was not inevitable at even high reaction temperature and these components converted into $BaTi_2O_5$ at high temperature and remained as impurity. As concentration of reactant increased, the size of as-synthesized $BaTiO_3$ powder deceased and Ba/Ti molar ratio approached into 1, showing Ba/Ti ratio of $1{\pm}0.005$ for reaction at $180^{\circ}C$ for 2 h with 2.0 M concentration.

Growth Characteristics of the ZnO Nanowires Prepared by Hydrothermal Synthesis Technique with Applied DC Bias (DC 바이어스를 인가하여 수열합성법으로 성장시킨 ZnO 나노와이어의 성장 특성)

  • Lim, Young-Taek;Shin, Paik-Kyun
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.27 no.5
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    • pp.317-321
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    • 2014
  • Hydrothermal synthesis technique could be carried out for growth of ZnO nanowires at relatively low process temperature, and it could be freely utilized with various substrates for fabrication process of functional electronic devices. However, it has also a demerit of relatively slow growth characteristics of the resulting ZnO nanowires. In this paper, an external DC bias of positive and negative 0.5 [V] was applied in the hydrothermal synthesis process for 2~8 [h] to prepare ZnO nanowires on a seed layer of AZO with high electrical conductivity. Growth characteristics of the synthesized ZnO nanowires were analyzed by FE-SEM. Material property of the grown ZnO nanowires was examined by PL analysis. The ZnO nanowires grown with positive bias revealed distinctively enhanced growth characteristics, and they showed a typical material property of ZnO.

Synthesis of zeolite A membranes on alumina support by hydrothermal reaction (수열반응에 의한 알루미나 지지체에 제올라이트 A 박막의 합성)

  • Ko, Tae-Seog
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.17 no.3
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    • pp.95-101
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    • 2007
  • The synthesis of NaA zeolite membrane on a porous alumina support from clear solution by using hydrothermal reaction was investigated. Effects of reaction temperature, reaction time and seeding for transformation of zeolite A membrane and powder which are produced in the reactor were monitored through X-ray diffraction (XRD) analysis and scanning electron microscopy (SEM). The transformation process of producing Zeolite A membrane starts from the formation of the compact and continuous membrane on the surface of porous support from clear solution. The large Zeolite A poly-crystal was then farmed through the dissolution process. Finally, the process was advanced from sodalite to amorphous. In case of powder, sodalite is formed in the early stage of reaction because of surrounding space difference between membrane and powder crystal. Discrete surrounding space of powder crystal makes easy to transform to sodalite. From Zeolite A to amorphous through transformed product was rapidly advanced at high temperature while the membrane with somewhat low coverage was obtained at low temperature. A compact and continuous zeolite A membrane was synthesized at $120^{\circ}C$ in 12-hour period.

The Synthesis of Kaolinitic Clay Minerals from Domestic Diatomite by Hydrothermal Process (국내산 규조토의 수열반응에 의한 Kaolinite질 인공점토의 합성에 관한 연구)

  • 김남일;박계혁;정창주
    • Journal of the Korean Ceramic Society
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    • v.31 no.11
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    • pp.1401-1413
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    • 1994
  • The synthesis of kaolinite mineral from domestic diatomite for silica resource, commercial vailable gibbsite or alumina for alumina resource were made under various hydrothermal treatment, and the sythetic effect of acidic mineralizers, temperature treatment with time duration, particle size of alumina on formation of kaolinite mineral and the plastic properties of synthesized kaolinite were investigated. The various acidic mineralizers which are HCl, HNO3, H2SO4 and Oxalic acid were employed for hydrothermal reaction in the range of 0.01 mol/ι to 2 mol/ι concentration of each mineralizers. It was found that HCl in the level of 1 mol/ι solution produced highly yields of well-crystallized and platy form kaolinite mineral and gave the most effective extraction of iron oxide, compared to that of others, that HNO3 produced highly yield of kaolinite but lower extraction of iron oxide, that H2SO4 produced low yield of kaolinite and formed alunite mineral, and that oxialic acid formed spherical crystalline kaolinite and gave low extraction of iron oxide. Moreover, it showed that kaolinite minerals were well synthesized in a wide range of less than 2 mol/ι acids, but were poorly synthesized at more than 2 mol/ι acids. However, boehmite and kaolinite were coexistently formed in the temperature range of 18$0^{\circ}C$ and 20$0^{\circ}C$ when the calcined diatomite and gibbsite were involved. The well-ordered kaolinite mineral as a platy form was highly synthesized in the temperature range of 220 and 24$0^{\circ}C$, when the same marterials as above were used with treatment of 1 mol/ι HCl solution. The results also revealed that the size of crystalline platy form kaolinite, synthesized from alumina and calcined diatomite with treatment in 1 mol/ιHCl solution at 24$0^{\circ}C$, was much larger than that of gibbsite and calcined diatomite shown previously, and that kaolinite and corundum minerals were coexistently formed under any hydrothermal treatment conditions. The plasticity of synthesized kaolinite from under 2 ${\mu}{\textrm}{m}$ alumina and calcined diatomite was very poor, and that of the synthesized kaolinite from raw diatomite and gibbsite gave higher than that of calcined diatomite and gibbsite.

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Synthesis of Zeolite from Sewage Sludge Incinerator Fly Ash by Hydrothermal Reaction in Open System (Open System 수열반응을 통한 하수슬러지 소각 비산재의 Zeolite 합성가능성)

  • Lee, Je-Seung;Eom, Seok-Won;Choi, Han-Young
    • Journal of Environmental Health Sciences
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    • v.33 no.4
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    • pp.317-324
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    • 2007
  • The sewage treatment sludge disposal has become a serious environmental problem because of restricted direct land-filling and oceandumping in spite of their large amounts discharged. So the recycling of sewage treatment sludge is very useful alternative for waste management. Here, we studied the feasibility of zeolite synthesis in open system from the sewage treatment sludge incinerator fly ash by means of hydrothermal synthesis. We considered the concentration of NaOH, reaction time, reaction temperature and reaction step as synthesis variables. The phase of zeolite products was identified by X-ray diffractometer(XRD) and ammonium ion exchange test was performed for the raw fly ash and two zeolite products(Z-3 and Z-5). In leaching test of the raw fly ash, hazard metal is detected very low level compared with regulatory leaching test standard. But in total recoverable test, the total contents of the fly ash were very high in terms of the standard for waste-derived fertilizer. Through hydrothermal reaction, small amount of zeolite P was synthesied in 1 N of NaOH solution and relatively large amount of hydroxysodalite was synthesied in 3 N and 5 N of NaOH solution with similar peak intensity. Addition of an aging step in the synthesis didn't increase the amount of zeolite phase. Maximum $NE_4^+-N$ exchange capacity is 1.49 mg $NH_4^+-N/g$ in Z-3 and 1.38 mg $NH_4^+-N/g$ in Z-5. Most of the ammonium ion is exchanged in 30 minutes and disorption did not occur until 5 hours.