• Title/Summary/Keyword: Sol-gel preparation

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Effects of Thermal Treatment Conditions on the Powder Characteristics of Uranium Oxide in HTGR Fuel Preparation (고온가스로용 핵연료 제조에서 열처리 조건이 우라늄산화물 입자 특성에 미치는 영향)

  • Kim, Yeon-Ku;Jeong, Kyung-Chai;Oh, Seung-Chul;Suhr, Dong-Soo;Cho, Moon-Sung
    • Journal of Powder Materials
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    • v.16 no.2
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    • pp.115-121
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    • 2009
  • The effects of thermal treatment conditions on ADU (ammonium diuranate) prepared by SOL-GEL method, so-called GSP (Gel supported precipitation) process, were investigated for $UO_2$ kernel preparation. In this study, ADU compound particles were calcined to $UO_3$ particles in air and Ar atmospheres, and these $UO_3$ particles were reduced and sintered in 4%-$H_2$/Ar. During the thermal calcining treatment in air, ADU compound was slightly decomposed, and then converted to $UO_3$ phases at $500^{\circ}C$. At $600^{\circ}C$, the $U_3O_8$ phase appeared together with $UO_3$. After sintering of theses particles, the uranium oxide phases were reduced to a stoichiometric $UO_2$. As a result of the calcining treatment in Ar, more reduced-form of uranium oxide was observed than that treated in air atmosphere by XRD analysis. The final phases of these particles were estimated as a mixture of $U_3O_7$ and $U_4O_9$.

Effects of Surface Characterization of γAl2O3 Particles by Aging in the Sol Preparation (졸 합성시 숙성이 γAl2O3 입자의 표면특성에 미치는 영향)

  • Yoo, Seung-Joon;Kwak, Dong-Heui;Kim, Hyeong-Gi;Hwang, Un-Yeon;Park, Hyung-Sang;Yoon, Ho-Sung;Jang, Hee Dong
    • Korean Chemical Engineering Research
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    • v.46 no.3
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    • pp.545-549
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    • 2008
  • The surface characteristics of calcined ${\gamma}-Al_2O_3$ particles as well as ${\gamma}-AlO$(OH) sol particles were controlled by aging in the boehmite sol preparation. As a result of the study, the IEPs of ${\gamma}-AlO$(OH) particles were decreased from pH 9.25 to pH 8.70 and those of the calcined ${\gamma}-Al_2O_3$ particles were decreased from pH 9.90 to pH 8.86 by the increase of the aging times. As a result of the acidic and basic characterization of the calcined ${\gamma}-Al_2O_3$ particles by the aging, the amount of acid sites was decreased from 0.1367 mmol/g to 0.0783 mmol/g by the increase of the aging times and Hammett acidity, $H_o$ was showed the acidic strength of 4.8 or above. On the other hand, the amount of basic sites was decreased from 0.4399 mmol/g to 0.3074 mmol/g by the increase of the aging times. Based on these results, we proposed the fact that the aging step in the sol-gel process was an important step to control the surface characterization of ${\gamma}-Al_2O_3$ particles including acidity and basicity.

Photoelectrochemical and Hydrogen Production Characteristics of CdS-TiO2 Nanocomposite Photocatalysts Synthesized in Organic Solvent (유기용매상에서 제조된 수소제조용 CdS-TiO2 나노복합 광촉매의 특성 연구)

  • Jang, Jum-Suk;So, Won-Wook;Kim, Kwang-Je;Moon, Sang-Jin
    • Transactions of the Korean hydrogen and new energy society
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    • v.13 no.3
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    • pp.224-232
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    • 2002
  • CdS-$TiO_2$ nano-composite sol was prepared by the sol-gel method in organic solvents at room temperature and further hydrothermal treatment at various temperatures to control the physical properties of the primary particles. Again, CdS-$TiO_2$ composite particulate films were made by casting CdS-$TiO_2$ sols onto $F:SnO_2$ conducting glass and then heat-treatment at $400^{\circ}C$. Physical properties of these 61ms were further controlled by the surface treatment with $TiCl_4$, aqueous solution. The photo currents and hydrogen production rates measured under the experimental conditions varied according to the $CdS/[CdS+TiO_2]$ mole ratio and the mixed-sol preparation method. For $CdS-TiO_2$ composite sols prepared in IPA, CdS particles were homogeneously surrounded by $TiO_2$ particles. Also, the surface treatment with $TiCl_4$ aqueous solution caused a considerable improvement in the photocatalytic activity, probably as a result of close contacts between the primary particles by the etching effect of $TiCl_4$. It was found that the photoelectrochemical performance of these particulate films could be effectively enhanced by this approach.

Preparation and Characterization of BaTiO3 Powders and Thin films (티탄산바륨 분말과 박막의 제조 및 특성 연구)

  • Jung, Miewon;Son, Hyunjin;Lee, Jiyun;Kim, Hyunjung
    • Analytical Science and Technology
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    • v.17 no.2
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    • pp.173-179
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    • 2004
  • The $BaTiO_3$ powders and thin films were prepared by an alkoxide modified sol-gel process (polymerization-complex route) using ethylene glycol. The stable starting (Ba-Ti)-mixed metal organic sol was made by addition of acetylacetone. The $BaTiO_3$ powders, which had a particle size of 40~77 nm, were crystallized from an amorphous to a tetragonal phase on annealing at 700 and $1100^{\circ}C$ for 1 h. From FT-IR, solid-state $^{13}C$ CP/MAS NMR spectroscopy and X-ray diffractometry, the trace of the Ba-Ti-oxycarbonate phase first appeared at $400^{\circ}C$. Hydrolyzed sol was spin coated on a quartz wafer at 3500 rpm for 60 s and pyrolyzed at $1100^{\circ}C$ for 1 h. After heat treatment, the coated layer became dense and smooth.

Preparation and Characterization of La0.8Ca0.2MnO3 (La0.8Ca0.2MnO3의 합성 및 특성연구)

  • 정미원;이지윤;김현정
    • Journal of the Korean Ceramic Society
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    • v.40 no.5
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    • pp.434-440
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    • 2003
  • The powders of L $a_{0.8}$C $a_{0.2}$Mn $O_3$ Colossal Magnetoresistance (CMR) materials were synthesized by sol-gel process. Lanthanum(H), Calcium(II) and Manganese(III) 2,4-Pentanedionate were dissolved in a mixed binary solution consisted of propionic acid and methanol with PEG (15 wt%) aqueous solution. The progress of reactions was monitored by FT-IR spectroscopy. The Lao scao.2Mn03 gel powders were annealed at various temperatures. The structural changes were investigated by FT-IR, CP/MAS $^{ 13}$C solid state NMR spectroscopy and XRD. The thermochemical property, particle characterization, microstructure of sintered sample, and cation composition of gel powder were studied by TG/DTA, FE-SEM and ICP-AES. The magnetic characterizations were identified through measurement of magnetic moment by VSM.

UO2 Kernel Particle Preparation for HTGR Nuclear Fuel (고온가스로용 핵연료 UO2 Kernel 입자제조)

  • Jeong, Kyung-Chai;Kim, Yeon-Ku;Oh, Seung-Chul;Cho, Moon-Sung
    • Journal of the Korean Ceramic Society
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    • v.44 no.8
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    • pp.437-444
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    • 2007
  • The broth solution was prepared by the mixing of an uranyl nitrate, THFA, PVA, and water. The uranium concentration of the broth solution was $0.5{\sim}0.8$ mole-U/L and the viscosity of it was $30{\sim}80cSt$. The droplets of this broth solution were farmed in air and ammonia by the vibrating nozzle with the frequency of 100 Hz at the amplitude of $100{\sim}130V$. The diameter of the droplet was about $1900{\mu}m$ from using the nozzle diameter of 1 mm. The diameter of the aged gel was about $1400{\mu}m$ after aging in ammonia solution at $60{\sim}80^{\circ}C$, and the dried gel with the diameter of about $900{\mu}m$ was obtained after drying at room temperature or partially vacuum condition. The diameter of the calcined $UO_3$ microsphere after calcination at $600^{\circ}C$ appeared about $800{\mu}m$ in air atmosphere. Although the droplets of the same sizes were formed, the calcined microspheres of different sizes were manufactured in the case of the broth solutions of the different uranium concentration. The droplets of the desired diameters were obtained by the change of the nozzle diameters and the broth flow rates.

Adipic Acid Assisted Sol-Gel Synthesis of Li1+x(Mn0.4Ni0.4Fe0.2)1-xO2 (0 < x < 0.3) as Cathode Materials for Lithium Ion Batteries

  • Karthikeyan, Kaliyappan;Amaresh, Samuthirapandian;Son, Ju-Nam;Kim, Shin-Ho;Kim, Min-Chul;Kim, Kwang-Jin;Lee, Sol-Nip;Lee, Yun-Sung
    • Bulletin of the Korean Chemical Society
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    • v.34 no.1
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    • pp.89-94
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    • 2013
  • Layered $Li_{1+x}(Mn_{0.4}Ni_{0.4}Fe_{0.2})_{1-x}O_2$ (0 < x < 0.3) solid solutions were synthesized using solgel method with adipic acid as chelating agent. Structural and electrochemical properties of the prepared powders were examined by means of X-ray diffraction, Scanning electron microscopy and galvanostatic charge/discharge cycling. All powders had a phase-pure layered structure with $R\bar{3}m$ space group. The morphological studies confirmed that the size of the particles increased at higher x content. The charge-discharge profiles of the solid solution against lithium using 1 M $LiPF_6$ in EC/DMC as electrolyte revealed that the discharge capacity increases with increasing lithium content at the 3a sites. Among the cells, $Li_{1.2}(Mn_{0.32}Ni_{0.32}Fe_{0.16})O_2$ (x = 0.2)/$Li^+$ exhibits a good electrochemical property with maximum initial capacity of 160 $mAhg^{-1}$ between 2-4.5 V at 0.1 $mAcm^{-2}$ current density and the capacity retention after 25 cycles was 92%. Whereas, the cell fabricated with x = 0.3 sample showed continuous capacity fading due to the formation of spinel like structure during the subsequent cycling. The preparation of solid solutions based on $LiNiO_2-LiFeO_2-Li_2MnO_3$ has improved the properties of its end members.

Low Temperature Preparation of Transparent Glass-Ceramic Using Metal-Alkoxides (1) Synthesis and Properties of Porous Monolithic Gel in Li2O·1.7Al2O3·8.6SiO2 (금속 알콕시드를 이용한 투명 결정화유리의 저온 합성 (1) Li2O·1.7Al2O3·8.6SiO2 다공성 겔체의 합성)

  • Chun, Kyung-Soo;Tak, Joong-Jae
    • Applied Chemistry for Engineering
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    • v.18 no.6
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    • pp.568-574
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    • 2007
  • Crack-free dried gel monoliths of the composition $Li_2O1{\cdot}7Al_2O_3{\cdot}8.6SiO_2$ have been prepared as a precursor of transparent glass-ceramic by the hydrolysis and polycondensation of mixed metal alkoxides in solutions containing N,N-dimethylformamide as the drying control chemical additive, alcohols, and water. It was investigated that activation energy for gelation according to the variation of water concentration ranged from 13 to 14 kcal/mol. Only when the amount of water for gelation was 3 times higher than the stoichiometric amount, monolithic dry gels were successfully prepared after drying at $70{\sim}75^{\circ}C$ and at a rate of 0.1~0.3%/h. The specific surface area, the pore volume, the average pore diameters of dried gel at $180^{\circ}C$ were about $239.40m^2/g$, 0.001~0.03 mL/g, and $145.62{\AA}$, respectively. It showed that the dried monolithic gel had a porous body. The DTA curve had the first exothermic peak around $800^{\circ}C$ and the 2nd peak around $980^{\circ}C$, which may correspond to crystallization of the gel.

Preparation of Al2O3-coated TiO2 Electrode for Recombination Blocking of Photoelectron in Dye-Sensitized Solar Cells (염료감응형 태양전지의 광전자 재결합 방지를 위한 Al2O3 코팅 TiO2 전극 제조)

  • Hwang, Kyung-Jun;Yoo, Seung-Joon;Jung, Sung-Hoon;Kim, Sun-Il;Lee, Jae-Wook
    • Applied Chemistry for Engineering
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    • v.21 no.2
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    • pp.162-168
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    • 2010
  • To increase the energy conversion efficiency of dye sensitized solar cells (DSSCs), it has been widely studied how to effectively transferred the electron generated from the adsorbed dye to the $TiO_{2}$ electrode for avoiding the recombination of injected electrons and iodide ions ($I^-/I_3^-$). For the blocking of the recombination, in this study, $Al_2O_3$-coated $TiO_{2}$ electrode was prepared and applied for DSSCs. In especial, the optimal preparation conditions of $Al_2O_3$ coated onto $TiO_{2}$ porous film was proposed for higher energy conversion efficiency. As a result, the solar cells fabricated from $Al_2O_3$-coated (i.e., particle size of bohemite sol : 100 nm) $TiO_{2}$ electrodes showed superior conversion efficiency (9.0%) compared to the bare $TiO_{2}$ electrodes (7.5%).

Preparation of High-Transmittance Glass Thin Films by the Sol-Gel Process (졸-겔법을 이용한 고투과율 유리 박막의 제조)

  • Hwang, Kyuseog;Song, Jongeun;Lee, Hyungmin;Lim, Yongmu;Kim, Sangmoon;Shim, Moonsik;Yun, Yeomhum
    • Journal of Korean Ophthalmic Optics Society
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    • v.4 no.1
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    • pp.45-49
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    • 1999
  • To prepare high-transmittance films, thin films were fabricated on the microscope slide glasses with silicon alkoxides and boric acids as starting materials by using a dip-coating technique. Thicknesses of the thin films were controled as viscosity of the sol used and composition of the $B_2O_3$ was changed at 5, 10, 15 and 20 mol%. Transmittance at visible range and IR transmittance of the films according to the composition were measured, and refractive index of the films were analyzed also. Maximum transmittance at visible range and minimum refractive index were obtained at 15 mol% $B_2O_3$. We will discuss a decrease of the transmittance at 20 mol% on the basis of the refractive index.

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