• 제목/요약/키워드: Solvothermal process

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용매열 공정을 이용한 세리아(CeO2) 나노분말의 합성 및 분산거동 (Synthesis and Dispersion of Ceria(CeO2) Nanoparticles by Solvothermal Process)

  • 임태섭;옥지영;최연빈;김봉구;손정훈;정연길
    • 한국재료학회지
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    • 제30권7호
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    • pp.376-382
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    • 2020
  • CeO2 nanoparticles, employed in a lot of fields due to their excellent oxidation and reduction properties, are synthesized through a solvothermal process, and a high specific surface area is shown by controlling, among various process parameters in the solvothermal process, the type of solvent. The synthesized CeO2 nanoparticles are about 11~13 nm in the crystallite size and their specific surface area is about 65.38~84.65 ㎡/g, depending on the amount of ethanol contained in the solvent for the solvothermal process; all synthesized CeO2 nanoparticles shows a fluorite structure. The dispersibility and microstructure of the synthesized CeO2 nanoparticles are investigated according to the species of dispersant and the pH value of the solution; an improvement in dispersibility is shown with the addition of dispersants and control of the pH. Various dispersing properties appear according to the dispersant species and pH in the solution with the synthesized CeO2 nanoparticles, indicating that improved dispersing properties in the synthesized CeO2 nanoparticles can be secured by applying dispersant and pH control simultaneously.

Synthesis and Characterization of Y2O3 Powders by a Modified Solvothermal Process

  • Jeong, Kwang-Jin;Bae, Dong-Sik
    • 한국재료학회지
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    • 제22권2호
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    • pp.78-81
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    • 2012
  • $Y_2O_3$ nanomaterials have been widely used in transparent ceramics and luminescent devices. Recently, many studies have focused on controlling the size and morphology of $Y_2O_3$ in order to obtain better material performance. $Y_2O_3$ powders were prepared under a modified solvothermal condition involving precipitation from metal nitrates with aqueous ammonium hydroxide. The powders were obtained at temperatures at $250^{\circ}C$ after a 6h process. The properties of the $Y_2O_3$ powders were studied as a function of the solvent ratio. The synthesis of $Y_2O_3$ crystalline particles is possible under a modified solvothermal condition in a water/ethylene glycol solution. Solvothermal processing condition parameters including the pH, reaction temperature and solvent ratio, have significant effects on the formation, phase component, morphology and particle size of yttria powders. Ethylene glycol is a versatile, widely used, inexpensive, and safe capping organic molecule for uniform nanoparticles besides as a solvent. The characterization of the synthesized Y2O3 powders were studied by XRD, SEM (FE-SEM) and TG/DSC. An X-ray diffraction analysis of the synthesized powders indicated the formation of the $Y_2O_3$ cubic structure upon calcination. The average crystalline sizes and distribution of the synthesized $Y_2O_3$ powders was less than 2 um and broad, respectively. The synthesized particles were spherical and hexagonal in shape. The morphology of the synthesized powders changed with the water and ethylene glycol ratio. The average size and shape of the synthesized particles could be controlled by adjusting the solvent ratio.

솔보써말 방법을 이용한 구리분말 제조 및 전자파 차폐제로의 응용 (The Preparation of Copper Powder Using Solvothermal Process and Its Application as EMI Shielding Agent)

  • 이효원;김수룡;권우택;최덕균;김영희
    • 한국재료학회지
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    • 제16권5호
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    • pp.285-291
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    • 2006
  • Copper powders have been widely used in electrically conductive coatings, electrode materials et al. and are very prospective since they are cheaper than noble metal powders such as silver or palladium. In this study, copper powders for metal filler of EMI shielding have been prepared using a solvothermal process from $CuSO_4$, NaOH, Glucose, mixed solvent ($H_2O$: Ethanol) and hydrazine which was used as a reducing agent at various reaction conditions. The prepared copper powders showed finely dispersed spherical shape without agglomerate, uniform morphology, narrow size distribution, high purity and were about 400-700 nm in size. The prepared powders were characterized using XRD, SEM, TGA, XPS, particle size measurement and EMI shielding efficiency.

Consolidation of Incineration Fly Ash by Solvothermal Reaction

  • Masuda, Kaoru;Endoh, Shigehisa
    • 대한전자공학회:학술대회논문집
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    • 대한전자공학회 2001년도 The 6th International Symposium of East Asian Resources Recycling Technology
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    • pp.655-658
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    • 2001
  • The generation of fly ash tends to increase yearly so that this is currently considered a big environmental concern, which requires appropriate treatment approaches. In this research the consolidation of incineration fly ash by the hot-press solvothermal reaction was investigated to provide an alternative process for the treatment and utilization of this waste material. Results showed that at reaction conditions of 52 K treatment, 20 ㎫ pressure and 60 minutes treatment time, the resulting consolidate exhibited a compressive ness strengths of 37-40 ㎫, a tensile strength of 6.5-7.0 ㎫ and a Rockwell hardness of 20-23 RH15W. These properties are comparable to the compressive ness strength of Portland cement which ranges from 30-40 ㎫ as well as with the tensile strengths of mortar, ganite, artificial lightweight aggregate and solidified high connote whose values are 2-2.5 ㎫, 5-9 ㎫, 5-10 ㎫ and 3-5 ㎫ respectively- Furthermore, by mixing fly ash with glass at 50% ratio and then subjecting to similar treatment conditions, a consolidate with even higher tensile strength of 12.5-13.3 ㎫ and hardness of 77-80 RH15W may be achieved.

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Controlling size and magnetic properties of Fe3O4 clusters in solvothermal process

  • Madrid, Sergio I. Uribe;Pal, Umapada;Jesus, Felix Sanchez-De
    • Advances in nano research
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    • 제2권4호
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    • pp.187-198
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    • 2014
  • Magnetite nanoparticles (MNPs) of different sizes were synthesized by solvothermal process maintaining their stoichiometric composition and unique structural phase. Utilizing hydrated ferric (III) chloride as unique iron precursor, it was possible to synthesize sub-micrometric magnetite clusters of sizes in between 208 and 381 nm in controlled manner by controlling the concentration of sodium acetate in the reaction mixture. The sub-micrometer size nanoclusters consist of nanometric primary particles of 19 - 26.3 nm average size. The concentration of sodium acetate in reaction solution seen to control the final size of primary MNPs, and hence the size of sub-micrometric magnetite nanoclusters. All the samples revealed their superparamagnetic behavior with saturation magnetization ($M_s$) values in between 74.3 and 77.4 emu/g. $M_s$. The coercivity of the nanoclusters depends both on the size of the primary particles and impurity present in them. The mechanisms of formation and size control of the MNPs have been discussed.

Optimization of Reaction Conditions for High Yield Synthesis of Carbon Nanotube Bundles by Low-Temperature Solvothermal Process and Study of their H2 Storage Capacity

  • Krishnamurthy, G.;Agarwal, Sarika
    • Bulletin of the Korean Chemical Society
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    • 제34권10호
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    • pp.3046-3054
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    • 2013
  • Synthesis of Carbon Nanotube bundles has been achieved by simple and economical solvothermal procedure at very low temperature of $180^{\circ}C$. The product yield obtained was about 70-75%. The optimization of reaction conditions for an efficient synthesis of CNTs has been presented. The CNTs are obtained by reduction of hexachlorobenzene in the presence of Na/Ni in cyclohexane. The X-ray diffraction, Fourier transform infrared and Raman spectral studies have inferred us the graphene structure of the products. The CNTs formed as the bundles were viewed on scanning electron microscope, transmission electron microscope and high-resolution transmission electron microscope. These are the multiwalled CNTs with outer diameter of 5-10 nm, the inner diameter 2-4 nm and cross sectional diameter up to 5 nm. Brunauer-Emmett-Teller (BET) based $N_2$ gas adsorption studies have been made to obtain BET surface area and $H_2$ storage capacity. Effect of the experimental variables such as reaction temperature, amount of catalyst and the amount of carbon source were investigated. It is found that they affect significantly on the product nature and yield.

용매열합성법을 통한 단분산된 ZnGa2O4 구형 입자의 제조 및 특성 (Facile synthesis and characteristics of monodispersed ZnGa2O4 microsphere via solvothermal method)

  • 우무현;강봉균;윤대호
    • 한국결정성장학회지
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    • 제26권3호
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    • pp.109-114
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    • 2016
  • 용매열합성법과 하소 과정으로 이루어진 두 단계 공정을 통해 단분산된 마이크로 크기의 구형 $ZnGa_2O_4$ 입자를 합성하였다. 합성된 3차원 구조의 구형 $ZnGa_2O_4$ 입자는 핵 생성과정에서 발생된 $ZnGa_2O_4$ 핵들이 자기 조립에 의해 형성된다. 이렇게 3차원 구조의 입자를 형성하는 원리인 '핵 성성'과 '자기 조립' 과정은 계면활성제인 PEG(polyethylene glycol)의 영향을 받는다. 그 이유는 계면활성제인 PEG의 농도가 임계응집농도(critical aggregation concentration)를 결정짓기 때문이다. 그리고 $ZnGa_2O_4$ 단상 합성을 위해 원료인 zinc acetate의 양을 조절했으며, 최적의 하소 조건을 결정하고자 TG-DTA를 통해 열적 거동을 확인했다. 또한 열처리 전 모체와 $900^{\circ}C$에서 1시간의 열처리 과정을 거친 산화물을 구성하는 작용기의 변화를 규명하기 위해 FT-IR을 측정하였다.

Novel solvothermal approach to hydrophilic nanoparticles of late transition elements and its evaluation by nanoparticle tracking analysis

  • Dutilleul, Marion Collart;Seisenbaeva, Gulaim A.;Kessler, Vadim G.
    • Advances in nano research
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    • 제2권2호
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    • pp.77-88
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    • 2014
  • Solvothermal treatment of late transition metal acetylacetonates in a novel medium composed either of pure acetophenone or acetophenone mixtures with amino alcohols offers a general approach to uniform hydrophilic metal nanoparticles with high crystallinity and low degree of aggregation. Both pure metal and mixed-metal particles can be accesses by this approach. The produced materials have been characterized by SEM-EDS, TEM, FTIR in the solid state and by Nanoparticle Tracking Analysis in solutions. The chemical mechanisms of the reactions producing nanoparticles has been followed by NMR. Carrying out the process in pure acetophenone produces palladium metal, copper metal with minor impurity of $Cu_2O$, and NiO. The synthesis starting from the mixtures of Pd and Ni acetylacetonates with up to 20 mol% of Pd, renders in minor yield the palladium-based metal alloy along with nickel oxide as the major phase. Even the synthesis starting from a mixed solution of $Cu(acac)_2$ and $Ni(acac)_2$ produces oxides as major products. The situation is improved when aminoalcohols such as 2-aminoethanol or 2-dimethylamino propanol are added to the synthesis medium. The particles in this case contain metallic elements and pairs of individual metals (not metal alloys) when produced from mixed precursor solutions in this case.

표면 개질된 지지체를 이용한 Cu3(BTC)2 튜브형 분리막의 용매열 합성 및 특성분석 (Solvothermal Synthesis and Characterization of Cu3(BTC)2 Tubular Membranes Using Surface Modified Supports)

  • 노승준;김진수
    • Korean Chemical Engineering Research
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    • 제52권2호
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    • pp.214-218
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    • 2014
  • 본 연구에서는 용매열합성법(solvothermal method)을 이용하여 매크로 기공의 알루미나 튜브 지지체 위에 나노기공 $Cu_3(BTC)_2$ 분리막을 제조하였다. In-situ 용매열합성법을 이용하는 경우, 매크로 기공의 알루미나 지지체 위에 균일한 핵생성과 성장을 통해 연속적이고 균열이 없는 $Cu_3(BTC)_2$ 층을 형성하기 어렵다. 본 연구에서는 용매열합성 전에 알루미나 지지체 표면을 $200^{\circ}C$로 가열한 상태에서 Cu 전구체 용액을 분무하여 지지체 표면을 개질한 후, 용매열합성법을 수행하여 연속적이고 균열이 없는 $Cu_3(BTC)_2$ 튜브형 분리막을 제조할 수 있었다. 합성된 $Cu_3(BTC)_2$ 분리막은 XRD, FE-SEM 및 기체투과 실험 등을 통해 분석하였다. $5{\mu}m$의 두께를 가진 $Cu_3(BTC)_2$ 튜브형 분리막을 통한 단일기체 투과실험 결과, $80^{\circ}C$에서 $H_2$가 가지는 투과도는 $7.8{\times}10^{-7}mol/s{\cdot}m^2{\cdot}Pa$이고, $H_2/N_2$, $H_2/CO_2$의 이상선택도는 각각 11.94, 12.82로 계산되었다.