• 제목/요약/키워드: low-temperature hydrothermal synthesis

검색결과 52건 처리시간 0.027초

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

  • 이재훈;배성환
    • 한국재료학회지
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    • 제27권8호
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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
    • 한국광물학회지
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    • 제10권1호
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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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수열합성을 이용하여 제작한 Fe3O4 결정입자의 자기적 특성 (Magnetic Properties of Micron Sized Fe3O4 Crystals Synthesized by Hydrothermal Methods)

  • 이기범;남충희
    • 한국분말재료학회지
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    • 제26권6호
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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.

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

  • 추용식;서성관;최성범;김경만;홍석환
    • 자원리싸이클링
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    • 제28권6호
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    • pp.46-53
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    • 2019
  • 본 연구에서는 국내에 적절한 환경처리 없이 방치되어 있는 중석광미를 활용하여, 중석 광미 입도별 시멘트 모르타르 제조 후 수열합성온도별 물리적 특성을 확인하였다. 시멘트 모르타르 혼합 시 물-시멘트비는 75 %로, 모래-시멘트비는 400 %로 고정하였으며, 광미는 모래(모래 중량 대비 0 ~ 50 % )를 치환하여 사용하였다. 저비소 및 고비소 광미의 입경은 9.3 ~ 53.0 ㎛로 제어하였고 수열합성온도는 승온 속도 2 ℃로 고정하여 60 ~ 180 ℃에서 6시간 동안 유지하였다. 수열합성 온도가 증가에 따라 압축강도는 상승하였으며, 60분 분쇄 저비소 및 고비소 광미를 30 % 혼합 시 압축강도는 각각 55.2 MPa 및 54.5 MPa로, 비교시편 보다 300 % 이상 향상되는 결과를 도출하였다.

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
    • 에너지공학
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    • 제24권2호
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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.

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

  • 박정훈;박상도
    • Korean Chemical Engineering Research
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    • 제45권5호
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    • pp.448-454
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    • 2007
  • 미세 $BaTiO_3$ 분말의 합성을 위해 함수 티타니아와 수산화바륨을 원료로 수열합성 실험을 수행하여, 반응시간, 온도, 농도 변화에 따른 전화율, 결정구조 및 생성 분말의 물성을 조사하였다. 전화율에 미치는 영향은 시간 < 온도 < 농도 순이었으며, 2.0 M의 원료를 $180^{\circ}C$에서 2 h 수열합성 시킬 때 최대 전화율을 99.5%를 얻을 수 있었다. 낮은 농도(0.25 M)에서는 고온에서도 미반응 $BaCO_3$와 미반응 $TiO_2$ 생성을 피할 수 없었으며, 이 미반응 물질들은 고온에서 $BaTi_2O_5$를 생성시켜 불순물로 존재하였다. 농도를 높일수록 합성 $BaTiO_3$ 분말의 크기는 작아졌으며, 분말의 Ba/Ti 비도 1에 접근하였다. 2.0M 이상의 농도에서는 $180^{\circ}C$, 2 h 반응에서 Ba/Ti 비는 $1{\pm}0.005$ 이였다.

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

  • 임영택;신백균
    • 한국전기전자재료학회논문지
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    • 제27권5호
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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.

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

  • 고태석
    • 한국결정성장학회지
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    • 제17권3호
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    • pp.95-101
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    • 2007
  • 수열합성 장치를 이용하여 종자 결정이 도포된 알루미나 지지체 위에 제올라이트 박막을 합성하였다. X-선 회절 분석과 전자현미경 사진을 이용하여 반응기 내에 생성된 제올라이트 A 분말과 제올라이트 A박막의 생성과 전이 생성물에 대해 합성온도, 합성시간, 종자결정의 영향에 대해서 고찰하였다. 제올라이트 A박막의 생성은 지지체 표면에 도포된 종자 결정에서 치밀한 연속적인 박막이 형성된 다음 용해과정을 거쳐 결정의 크기가 큰 다결정 층을 형성하고, 최종적으로 소다라이트를 거쳐 무정형으로 진행하였다. 반면에 분말에서는 반응초기부터 소다라이트가 관찰되는데 고정된 제올라이트 A 박막과 다르게 결정주위의 공간적인 차이에 의해 소다라이트가 생성하기에 용이한 공간을 갖기 때문에 소다라이트가 쉽게 생성되는 것으로 생각된다. 합성온도가 높으면 짧은 시간 내에 전이 생성물을 거쳐 무정형으로 진행하였고 온도가 낮으면 합성 시간이 길고 피복도가 다소 낮은 제올라이트 A 박막을 얻었다. $120^{\circ}C$, 12시간에서 피복도가 높은 치밀한 제올라이트 A박막을 합성하였다.

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

  • 김남일;박계혁;정창주
    • 한국세라믹학회지
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    • 제31권11호
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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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Open System 수열반응을 통한 하수슬러지 소각 비산재의 Zeolite 합성가능성 (Synthesis of Zeolite from Sewage Sludge Incinerator Fly Ash by Hydrothermal Reaction in Open System)

  • 이제승;엄석원;최한영
    • 한국환경보건학회지
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    • 제33권4호
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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.