• Title/Summary/Keyword: Solvothermal synthesis

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Morphological Change of $CuInSe_2$ Nanoparticles by Solvothermal Synthesis Conditions (용매열 합성조건에 따른 $CuInSe_2$ 나노입자 형상변화)

  • 김기현;전영갑;윤경훈;박병옥
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2003.11a
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    • pp.230-230
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    • 2003
  • Chalcopyrite 구조를 가진 CuInSe$_2$ (CIS) 나노입자를 유기용매인 diethylamine을 사용하여 autoclave안에서 용매열법(solvothermal method)으로 제조하였다. 180 $^{\circ}C$에서 36시간 반응시켜 길이가 10-30 nm, 폭이 5-10 nm인 rod-Eke 형상을 한 CIS 나노입자를 얻었다. 반응온도를 25$0^{\circ}C$로 증가시키고 동일한 반응시간에서 보다 미세하고 균일한 구형의 CIS 나노입자를 관찰할 수 있었다. 한편, 190 $^{\circ}C$에서 얻어진 CIS 나노입자는 36시간을 반응시킨 경우 구형으로 관찰되었으나 60시간 반응시킨 경우는 길이가 50-100 nm 인 rod-like 입자로 성장하였다. 이와 같이 반응시간과 온도를 달리하여 나노입자의 형상이 바뀌는 것을 입자성장기구의 관점에서 고찰하였다. 반응시간과 온도에 따라 얻어진 CIS 나노 입자들의 결정성, 미세구조 그리고 정량 및 정성분석을 XRD, SEM, TEM, EDS등으로 각각 행하였다.

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Application of monodisperse Fe3O4 submicrospheres in magnetorheological fluids

  • Anupama, A.V.;Kumaran, V.;Sahoo, B.
    • Journal of Industrial and Engineering Chemistry
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    • v.67
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    • pp.347-357
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    • 2018
  • Steady shear response of a magnetorheological fluid (MRF) system containing porous mono-disperse magnetite ($Fe_3O_4$) spheres synthesized by solvothermal method is demonstrated. In applied magnetic field the interaction between the spherical particles leads to form strong columnar structures enhancing the yield strength and viscosity of the MRFs. The yield strengths of the MRFs also scale up with the concentration of magnetic particles in the fluid. Considering magnetic dipolar interaction between the particles the magneto-mechanical response of the MRFs is explained. Unlike metallic iron particles, the low-density corrosion resistant soft-ferrimagnetic $Fe_3O_4$ spherical particles make our studied MRF system efficient and reliable for shock-mitigation/vibration-isolation applications.

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

  • Noh, Seung-Jun;Kim, Jinsoo
    • Korean Chemical Engineering Research
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    • v.52 no.2
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    • pp.214-218
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    • 2014
  • In this study, nanoporous $Cu_3(BTC)_2$ membranes were synthesized on macroporous alumina tube supports by solvothermal method. It is very difficult to prepare uniform and crack-free $Cu_3(BTC)_2$ layer on macroporous alumina support by in situ solvothermal method. In this study, continuous and crack-free $Cu_3(BTC)_2$ tubular membranes could be obtained by in situ solvothermal process after surface modification of alumina support. The surface modification was conducted by spraying Cu precursor solution on the alumina support heated at $200^{\circ}C$. The prepared $Cu_3(BTC)_2$ tubular membranes were characterized by XRD, FE-SEM and gas permeation experiments. $H_2$ permeance through $5{\mu}m$ thick $Cu_3(BTC)_2$ tubular membrane was calculated to be $7.8{\times}10^{-7}mol/s{\cdot}m^2{\cdot}Pa$ by single gas permeation test, with the ideal selectivities of $H_2/N_2=11.94$, and $H_2/CO_2=12.82$.

Synthesis and Hydrogen Adsorption Properties of Porous Polymer

  • Wang, Qi;Liu, Jin;Zhang, Jing;Oh, Won-Chun
    • Korean Journal of Materials Research
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    • v.26 no.6
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    • pp.332-336
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    • 2016
  • Three kinds of porous polymer were synthesized using a solvothermal of tri-4,4'-diphenylmethane diisocyanate (MDI-trimer) and different diamino monomers. The effects of the synthesis conditions and the monomer selection on the synthesis of porous polymer properties were studied. The results show that the synthesis of $NH_2$-containing monomer molecules smaller the microporous polymers was easy to implement; the specific surface areas of the polymers are related to the monomer ratio and the reaction time. The results show that the synthesized porous polymer had good hydrogen storage performance; the hydrogen storage ability improved with the addition of heterocyclic nitrogen.

Preparation and Properties of Eu3+ Doped Y2O3 Nanoparticles with a Solvothermal Synthesis Using the Ethylene Glycol (에틸렌 글리콜을 이용하여 용매열 합성으로 Eu3+가 도핑된 Y2O3 나노 입자의 제조 및 특성)

  • 신수철;조태환
    • Journal of the Korean Ceramic Society
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    • v.40 no.7
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    • pp.709-714
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    • 2003
  • Eu doped $Y_2$ $O_3$ nanoparticles were prepared with the solvothermal synthesis using the ethyleneglycol solvent at 20$0^{\circ}C$ for 3-5 h and then annealed in air at 1000-140$0^{\circ}C$ for 2-4 h. The X-ray diffraction pattern of annealed crystals at 100$0^{\circ}C$ for 2 h could be indexed as pure cubic cell of $Y_2$ $O_3$ phase with lattice parameters a=10.5856 $\AA$ which is very close to the reported data (JCPDS Card File, 41-1105 a=10.6041 $\AA$). Average size of prepared phosphor particles have about 100 nm, which were spherical morphology. The phosphor particle sizes decreased and the emission intensity increased at the annealing temperature. Though PL spectrum analysis, the 3% Eu doped $Y_{2-x}$ $O_3$:E $u_{x}$ $^{3+}$(x=0.06) phosphor showed the excitation spectrum at 250 nm wavelength and the maximum emission spectrum at 611 nm wavelength.

Preparation of Al-doped NiO via Solvothermal Synthesis and its Crystal Structural and Electrical Properties (용매열 합성법을 통하여 알루미늄을 도핑한 니켈옥사이드의 제조와 그 결정구조적, 전기적 특성)

  • Hong, Sun-Ki;Ji, Mi-Jung;Lee, Min-Jin;Jung, Sung-Hun;Seol, Kwang-Hee;Choi, Byung-Hyun
    • Korean Journal of Materials Research
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    • v.22 no.11
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    • pp.631-635
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    • 2012
  • Nickel oxide was doped with a wide range of concentrations (mol%) of Aluminum (Al) by solvothermal synthesis; single-phased nano powder of nickel oxide was generated after calcination at$900^{\circ}C$. When the concentration of Al dopant was increased, the reduced intensity was confirmed through XRD analysis. Lattice parameters of the synthesized NiO powder were decreased after treatment of the dopant; parameters were increased when the concentration of Al was over the doping limit (5 mol% Al). The binding energy of $Ni^{2+}$ was chemically shifted to $Ni^{3+}$ by doping $Al^{3+}$ ion, as confirmed by the XPS analysis. The tilted structure of the synthesized NiO with 5 mol% Al dopant and the polycrystalline structure of the $Ni_{0.75}Al_{0.25}O$ were observed by HR-TEM analysis. The electrical conductivity of the newly synthesized NiO was highly improved by Al doping in the conductivity test. The electrical conductivity values of the commercial NiO and the synthesized NiO with 5 mol% Al dopant ($Ni_{0.95}Al_{0.05}O$) were 1,400 s/cm and 2,230 s/cm at $750^{\circ}C$, respectively. However, the electrical conductivity of the synthesized NiO with 10 mol% Al dopant ($Ni_{0.9}Al_{0.1}O$) decreased due to the scattering of free-electrons caused by the large number of impurity atoms; the electrical conductivity of $Ni_{0.9}Al_{0.1}O$ was 545 s/cm at $750^{\circ}C$.

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

  • Woo, Moo Hyun;Kang, Bong Kyun;Yoon, Dae Ho
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.26 no.3
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    • pp.109-114
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    • 2016
  • Monodispersed $ZnGa_2O_4$ microspheres were synthesized by a facile two-step process consisting of a solvothermal method and calcination process. The prepared monodispersed $ZnGa_2O_4$ microspheres were aggregated into 3D microstructures by self-assembly with a large number of small $ZnGa_2O_4$ particles generated in nucleation. This nucleation and self-assembly making hierarchical microstructures were depended on the concentration of PEG (polyethylene glycol) due to CAC (critical aggregation concentration) theory. And also we controlled the amount of zinc acetate to make pure $ZnGa_2O_4$ phase. Additionally, to fix the optimized calcination condition, sample was characterized by TG-DTA to prove the thermal property in the calcination process and by FT-IR to identify the changes of functional group bonding between each element of the $ZnGa_2O_4$ precursor and oxide calcined at $900^{\circ}C$ for 1 h.

Facile Synthesis of CdTe Nanorods from the Growth of Te Nanorods

  • Xu, Weiwei;Niu, Jinzhong;Zheng, Shuang;Tian, Guimin;Wu, Xinghui;Cheng, Yongguang;Hu, Xiaoyang;Liu, Shuaishuai;Hao, Haoshan
    • Journal of the Korean Chemical Society
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    • v.61 no.4
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    • pp.185-190
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    • 2017
  • One-dimensional CdTe nanorods (NRs) are obtained by the reaction of various Cd precursors with single crystalline Te nanorod templates, which are pre-synthesized from Te precursors by a simple and reproducible solvothermal method. Throughout the process, the diffraction intensity of different crystal facets of single crystalline Te NRs varied with reaction times. Finally, by alloying Cd ions along the axial direction of Te NRs, polycrystalline cubic phase CdTe NRs with diameters of 80-150 nm and length up to $1.2-2.4{\mu}m$ are obtained. The nucleation and growth processes of Te and CdTe NRs are discussed in details, and their properties are characterized by XRD, SEM, TEM, Raman scattering, and UV-vis absorption spectra. It was found that the key elements of synthesizing CdTe NRs such as reaction temperatures and Cd sources will strongly influence the final shape of CdTe NRs.

Synthesis of CuInSe2 Nanoparticles by Solvothermal Method (용매열법을 이용한 CuInSe2 나노 입자 합성)

  • Kim Ki-Hyun;Chun Young-Gab;Park Byung-Ok;Yoon Kyung-Hoon
    • Korean Journal of Materials Research
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    • v.14 no.10
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    • pp.737-742
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    • 2004
  • $CuInSe_2$ (CIS) nanoparticles of chalcopyrite structure were directly synthesized by a solvothemal method in an autoclave with diethylamine as a solvent. A morphology change of the nanoparticles was observed as a function of reaction temperatures and times. Dense rod-type CIS nanoparticles with width of $5\sim10mm$ and length in the range of 30-80 nm were obtained at $180^{\circ}C$ for 36 hrs whereas spherical particles with diameter in the range of 5-10 nm were observed at $250^{\circ}C$ for 36 hrs. The formation of the rod-like nanoparticles in diethylamine, without double N-chelation, was explained by the Solution-Liquid-Solid (SLS) mechanism.