• Title/Summary/Keyword: Complex Sol-Gel Process

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Preparation by the double extraction process with preliminary neutron irradiation of yttria or calcia stabilised cubic zirconium dioxide microspheres

  • Brykala, Marcin;Walczak, Rafal;Wawszczak, Danuta;Kilim, Stanislaw;Rogowski, Marcin;Strugalska-Gola, Elzbieta;Olczak, Tadeusz;Smolinski, Tomasz;Szuta, Marcin
    • Nuclear Engineering and Technology
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    • v.53 no.1
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    • pp.188-198
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    • 2021
  • A modern approach to nuclear energy involves reprocessing like transmutations of spent nuclear fuel products to reduce their radiotoxicity and time needed for their storage. For this purpose, they are immobilized in inert matrices made of zirconia and can be "burned" in fast neutron reactor or Accelerator Driven System. These matrices in spherical form can be obtained by sol-gel process. The paper presents a method of microspheres fabrication based on the combined Complex Sol-Gel Process and double extraction process consisting in the preparation of zirconium-ascorbate sol and simultaneous extraction of water and nitrates. The procedure allows obtaining gel microspheres with a diameter of 50 ㎛, which after heat treatment are processed into the final product. The synthesis of zirconia microspheres with Yttrium by internal gelation process is well known for over a decade now. However, the explanation and characterization of synthesis of such material by extraction of water process is rarely found. Parameters such as: pH, viscosity, shape, sphericity and crystal structure have been determined for synthesized products and semi-products. In addition, preliminary research consisting in irradiation of the obtained materials in fast and thermal neutron flux was carried out. The obtained results are presented and described in this work.

Preparation of $\gamma-LiAlO_2$ Short Fibers by the Sol-Gel Method (졸-겔법에 의한 $\gamma-LiAlO_2$ 단섬유의 제조)

  • 현상훈;이재현;홍성안
    • Journal of the Korean Ceramic Society
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    • v.33 no.10
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    • pp.1079-1088
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    • 1996
  • Discontinuous ${\gamma}$-LiAlO2 fibers for fiber-reinforcing MCFC matrixes have been produced by the sol-gel process using the centrifugal spinning apparatus of the Rotary type. Gel fibers could be obtained through spinning of stable LiAlO2 complex polymetric sols under the optimum spinning conditions (hollow-disc rotating velocity 9000 rpm sol feeding rate of 4ml/min flowing N2 temperature of 4$0^{\circ}C$ and flowing N2 pressure of 4 bar). It was found that defect free and densified ${\gamma}$-LiAlO2 fibers with the relative density of 98% and the mean diameter of 4.7${\mu}{\textrm}{m}$ were prepared when the spinned fibers were heat-treated to 100$0^{\circ}C$ on the specified heating schedule. in particular the mean diameter and length of fibers could be controlled by the pressure of flowing N2 and the chopping-sieving method respectively.

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Preparation and Characteristics of $\gamma-LiAlO_2$ Fibers by the Sol-Gel Method (졸-겔 법에 의한 $\gamma-LiAlO_2$ 화이버의 제조 및 특성)

  • 현상훈;홍성안;신현철
    • Journal of the Korean Ceramic Society
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    • v.32 no.2
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    • pp.197-208
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    • 1995
  • ${\gamma}$-LiAlO2 fibers for fiber reinforced molten carbonate fuel cell (MCFC) matrix have been produced from LiAlO2 complex polymeric sols using the sol-gel process. The stable and spinnable LiAlO2 sols could be synthesized by mixing LiNO3 alcohol solutions in aluminum complex polymeric sols prepared through the condensationpolymerization reaction of 1 more of aluminum tri-sec-butoxide with 0.55 mole of mixed chelates (mole ratio of acetylaceton/triethanolamine=0.25/0.3). It was found that the viscosity range for fiber-spinning should be higher than 30 poise. The defect-free flexible ${\gamma}$-LiAlO2 fibers with the average tensile strength of 350 MPa could be obtained when the spinned fibers were heat-treated to 120$0^{\circ}C$ on the specified heating schedule after dried at room temperature.

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The Preparation of Alumina Fiber by Sol-Gel Method (I) Rheological Properties (졸겔법에 의한 알루미나 섬유의 제조 (I) 유동학적 특성분석)

  • 최용수;이종혁;이해욱;김창은
    • Journal of the Korean Ceramic Society
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    • v.32 no.1
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    • pp.17-24
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    • 1995
  • The TEA complex polymeric sol was prepared by the alkoxide sol-gel method. The purpsoe of this experiment was to vefity the particle shape in the sol from the investigation of the rheological properties. TEA retarded hydrolysis rate by the reaction with alkoxide enough to make a stable transparent sol in the wide range of composition. From the results of the viscosity change with time, the optimum mole ratio for spinning was selected as 0.5 mole of TEA, 3 mole of H2O and the optimum viscosity was 104 cPs. The rheological behavior of the sol showed that the particle shape in the sol was linear, which was adequate for fiber drawing.

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Thin Oxide Functional Films by Metal Alkoxide Method

  • Natalya, Korobova
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2000.07a
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    • pp.9-16
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    • 2000
  • A survey over the role of sol-gel processing and metal alkoxides in the thin film preparation is given. The basic chemistry of the sol-gel process is complex due to the different reactivities of the network forming and the wide variety of reaction parameters. Despite the important progress in the investigations of the mechanisms of thin film formation, a direct relation of reaction parameters to functional oxide properties is still very difficult.

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Fabrication of Hollow Micro-particles with Nonspherical Shapes by Surface Sol-gel Reaction (표면 솔-젤 반응을 활용한 마이크로미터 크기의 비구형상 공동 입자의 제조)

  • Cho, Young-Sang;Jeon, Seog-Jin;Yi, Gi-Ra
    • Korean Chemical Engineering Research
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    • v.45 no.6
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    • pp.611-618
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    • 2007
  • We demonstrate the sol-gel coating technique of colloidal clusters for producing hollow micro-particles with complex morphologies. Cross-linked amidine polystyrene (PS) microspheres were synthesized by emulsifier-free emulsion copolymerization of styrene and divinylbenzene. The amidine PS particles were self-organized inside toluene-in-water emulsion droplets to produce large quantities of colloidally stable clusters. These clusters were coated with thin silica shell by sol-gel reaction of tetraethylorthosilicate (TEOS) and ammonia, and the organic polystyrene cores were removed by calcination at high temperature to generate nonspherical hollow micro-particles with complex morphologies. This process can be used to prepare hollow particles with shapes such as doublets, tetrahedra, icosahedra, and others.

Preparation of Alumina by the Sol-Gel Process(I) - Characteristics of Polymeric Alumina Sol (졸겔법에 의한 알루미나의 제조(I) - 중합 알루미나 졸의 특성)

  • 이해욱;김구대;정형진;김창은
    • Journal of the Korean Ceramic Society
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    • v.28 no.1
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    • pp.60-66
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    • 1991
  • The polymeric alumina sol was prepared by partial hydrolysis of aluminum sec-butoxide reacted with acetylacetone and its characteristics was investigated. The effects of alcohol solvent, acetylacetone, and acid concentration to the sol were investigated. FT-IR and Al27-MASNMR were used to study hydrolysis and polymerization reaction of aluminum complex. Synthesized sol showed the characteristics of polymeric alumina sol. To make a clear polymeric alumina sol, the optimum contents of acetylacetone, H2O and alcohol solvent were 0.4-0.6 mole, 0.25-1.25 mole, 3-5 mole per one mole alkoxide respectively. As a result of the Al27-MASNMR analysis, it was noted that hexa-penta-coordinated Al were main structure.

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Characteristics of La0.2Ca0.8MnO3 Powder and Pellet Prepared by Sol-Gel Process (졸-겔법으로 합성한 La0.2Ca0.8MnO3의 분말과 펠렛의 특성)

  • Jung, Miewon;Lee, Jiyun;Kim, Hyunjung
    • Applied Chemistry for Engineering
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    • v.16 no.1
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    • pp.150-152
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    • 2005
  • $La_{0.2}Ca_{0.8}MnO_3$ colossal magnetoresistance (CMR) powders and pellets were synthesized by sol-gel process involving a stable metal chelate complex with acetylacetone. The structural changes of reaction mixture were monitored by FT-IR spectroscopy and X-ray diffractometry. The microstructure of sintered samples and the cation composition of gel powder were studied by FE-SEM/EDS and ICP-AES. The magnetic property was investigated as a function of temperature.

Synthesis of Silver-doped Silica-complex Nanoparticles for Antibacterial Materials

  • Shin, Yu-Shik;Park, Mira;Kim, Hak-Yong;Jin, Fan-Long;Park, Soo-Jin
    • Bulletin of the Korean Chemical Society
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    • v.35 no.10
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    • pp.2979-2984
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    • 2014
  • Silver nanoparticles have been synthesized by liquid-phase and alcohol reduction methods. Silver-doped silica-complex nanoparticles were prepared using a sol-gel process. The formation, structure, morphology, and particle size of the nanoparticles have been studied using several techniques. Silver nanoparticles of size of 30-40 nm were formed successfully by alcohol reduction. TEM images show that both the concentration and the molecular weight of polyvinyl pyrrolidone (PVP) considerably affect the size of the emerging silver nanoparticles. The number of silver-doped silica-complex particles increased by a mercapto-group treatment that showed a narrower size distribution than that of silica treated with amino groups. The silver/polyester and silver-doped silica/polyester masterbatch chips showed excellent antibacterial activity against Staphylococcus aureus and Escherichia coli.

The synthesis of Highly Crystalline and monodisperse maghemite and zirconia Nanocrystallites without size-selection process

  • Park, Jong-Nam;Joo, Jin;Yoo, Tae-kyung;Na, Hyun-Bin;Lee, Soo-Sung;Park, Hyun-Min;Kim, Young-Woon;Hyun, Taek-Hwan
    • Proceedings of the Korea Crystallographic Association Conference
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    • 2003.05a
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    • pp.20-20
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    • 2003
  • A new and simple method has been developed to synthesize highly crystalline and monodisperse maghemite (γ-Fe₂O₃) and zirconia (ZrO₂) nanocristallites. High temperature aging of metal-surfactant complex was founded to generate monodisperse nanoparticles, wherein the nuclei were prepared by the thermal decomposition of iron-oleate complex in case of iron oxide and nonhydrolytic sol-gel reaction in case of zirconia respectively. By varying the experimental conditions, in other words concentration of surfactants, kind of metal precursor, reaction temperature and so on, the diameter of spherical nanoparticles could be controlled at various size. The synthesized nanoparticles were characterized by electron diffraction, X-ray diffraction, and low- and high-resolution transmission electron microscope.

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