• Title/Summary/Keyword: Solution ZrO2

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Synthesis of $(ZrSiO_4)$ Powders by the Sol-Gel Process -Effect of the Milling- (졸-겔법에 의한 지르콘$(ZrSiO_4)$ 분말 합성 -재분쇄(Milling)에 대한 효과-)

  • 신용철;신대용;한상목;남인탁
    • Journal of the Korean Ceramic Society
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    • v.32 no.7
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    • pp.853-857
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    • 1995
  • ZrSiO4 powders were prepared from partially hydrolyzed solution of Si(OC2H5)4 and ZrOCl2.8H2O solution by the sol-gel method and formation rate of ZrSiO4 on the reaction parameter was investigated. In order to prepare homogeneous ZrSiO4 precursor gels, the H2O/Si(OC2H5)4 molar ratio of about 2, the pH of the ZrOCl2.8H2O solution fo about 4 and stirring time of the mixed solutions of about 2 hrs were appropriate. Formation of temperature of ZrSiO4 reduced about 15$0^{\circ}C$ by milling and formation of ZrSiO4 at 1300~135$0^{\circ}C$ showed an accelerative increase through the hedvall effect by silica.

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CeO2-Promoted Highly Active Catalyst, NiSO4/CeO2-ZrO2 for Ethylene Dimerization

  • Pae, Young-Il;Shin, Dong-Cheol;Sohn, Jong-Rack
    • Bulletin of the Korean Chemical Society
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    • v.27 no.12
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    • pp.1989-1996
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    • 2006
  • The $NiSO_4/CeO_2-ZrO_2 $catalysts containing different nickel sulfate and $CeO_2$ contents were prepared by the impregnation method, where support, $CeO_2-ZrO_2$was prepared by the coprecipitation method using a mixed aqueous solution of zirconium oxychloride and cerium nitrate solution followed by adding an aqueous ammonia solution. No diffraction line of nickel sulfate was observed up to 20 wt %, indicating good dispersion of nickel sulfate on the surface of $CeO_2-ZrO_2$. The addition of nickel sulfate (or $CeO_2$) to $ZrO_2$ shifted the phase transition of $ZrO_2$ from amorphous to tetragonal to higher temperatures because of the interaction between nickel sulfate (or $CeO_2$) and $ZrO_2$. A catalyst (10-$NiSO_4/1-CeO_2-ZrO_2$) containing 10 wt % $NiSO_4$ and 1 mole % $CeO_2$, and calcined at $600{^{\circ}C}$ exhibited a maximum catalytic activity for ethylene dimerization. The catalytic activities were correlated with the acidity of catalysts measured by the ammonia chemisorption method. The role of $CeO_2$was to form a thermally stable solid solution with zirconia and consequently to give high surface area, thermal stability and acidity of the sample.

Control of Microstructures and Properties of Composites of the $Al_2O_3-ZrO_2-Spinel$ System: II. $Al_2O_3-ZrO_2-Spinel$ Composites Prepared by the Solution Infiltration Method ($Al_2O_3-ZrO_2-Spinel$계 복합체의 미세구조 및 물성제어: II. 용액침투법에 의한 $Al_2O_3-ZrO_2-Spinel$ 복합소결체)

  • 현상훈;송원선
    • Journal of the Korean Ceramic Society
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    • v.30 no.10
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    • pp.811-818
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    • 1993
  • Al2O3/ZrO2-Spinel composites were prepared by infiltrating magnesium sulfate solution into the porous preform made from Al2O3-20wt% ZrO2 composite powders derived through an emulsion route. The microstructure and composition of the modified composites could be controlled by manipulating the presingtering temperature of the preform, infiltration time, and so on. It was found that spinel phases were concentrated near the surface than in the interior of the Al2O3/ZrO2-Spinel composites infiltrated for 6hrs, while spinel phases were uniformly distributed in the comosites infiltrated for 2 days. The relative density and fracture toughness of the composite infiltrated for 6 hrs were 98.6% and 7.2MN/m3/2, respectively.

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Preparation of $ZrO_2$ Coated Graphite Powders in Aqueous and Nonaqueous Solution (수계-비수계 용매를 이용한 흑연분말의 $ZrO_2$ 수열코팅)

  • 김정환;이태근;이기강;이석근
    • Korean Journal of Crystallography
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    • v.14 no.2
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    • pp.67-72
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    • 2003
  • Graphite powders were coated with ZrO₂ by the controlled hydrolysis of a DI water, ethanol and DI water+ethanol solutions. The hydrolysis process was carried out with temperature control because of the low wettability of Zr ions to the surface of the graphite. PVA was added to the solution for the enhancement of metal ion adsorption. The surface of the graphite powders coated with ZrO₂ was observed by SEM and TEM. There are two types of ZrO₂ particles with the condition of ZrOCl₂°§8H₂O aqueous solutions were used; (a) primary particles a few nm in size and (b) secondary particles with ∼0.1 ㎛ size were obtained. The graphite powders coated in 50% ethanol-50% DI water solution of Zr(SO₄)₂ㆍ4H₂O have the relatively uniform coating layer and the starting temperature of oxidation was 100℃ higher than the raw graphite.

NiSO4 Supported on FeO-promoted ZrO2 Catalyst for Ethylene Dimerization

  • Sohn, Jong-Rack;Kim, Young-Tae;Shin, Dong-Cheol
    • Bulletin of the Korean Chemical Society
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    • v.26 no.11
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    • pp.1749-1756
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    • 2005
  • The $NiSO_4$ supported on FeO-promoted $ZrO_2$ catalysts were prepared by the impregnation method. FeOpromoted $ZrO_2$ was prepared by the coprecipitation method using a mixed aqueous solution of zirconium oxychloride and iron nitrate solution followed by adding an aqueous ammonia solution. The addition of nickel sulfate (or FeO) to $ZrO_2$ shifted the phase transition of $ZrO_2$ (from amorphous to tetragonal) to higher temperatures because of the interaction between nickel sulfate (or FeO) and $ZrO_2$. 10-$NiSO_4$/5-FeO-$ZrO_2$ containing 10 wt % $NiSO_4$ and 5 mol % FeO, and calcined at 500 ${^{\circ}C}$ exhibited a maximum catalytic activity for ethylene dimerization. $NiSO_4$/FeO-$ZrO_2$ catalysts was very effective for ethylene dimerization even at room temperature, but FeO-$ZrO_2$ without $NiSO_4$ did not exhibit any catalytic activity at all. The catalytic activities were correlated with the acidity of catalysts measured by the ammonia chemisorption method. The addition of FeO up to 5 mol % enhanced the acidity, surface area, thermal property, and catalytic activities of catalysts gradually, due to the interaction between FeO and $ZrO_2$ and due to consequent formation of Fe-O-Zr bond.

Preparation and Characteristics of Ceramic Composite Powders Coated with $Al_2O_3$: (III) Composite Powders of $Al_2O_3-ZrO_2$ ($Al_2O_3$로 피복시킨 세라믹 복합분체의 제조 및 특성: (III) $Al_2O_3-ZrO_2$ 복합분체)

  • 현상훈;이지현;송원선
    • Journal of the Korean Ceramic Society
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    • v.29 no.8
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    • pp.667-673
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    • 1992
  • The alumina-zirconia composite powders of core particle ZrO2 coated with Al2O3 were prepared by the hydrolysis-deposition of the mixed aluminum salt solution of Al2(SO4)3-Al(NO3)3-Urea. The effects of hydrolysis reaction and coating parameters on characteristics of coated powders and composites were also investigated. The degree of coating could be estimated from the ratio of tetra-/mono-ZrO2 present at the room temperature after heat-treating coated powders at 120$0^{\circ}C$ and the result of TEM observations. When the content of ZrO2 in the dispersed coating system, the coating time, and the volume ratio of water/solution were 50 mg/g, 180 min, and 5, respectively the coating efficiency was maximum (the ratio of tetra-/mono-ZrO2 was 87/13). The relative densities of coated Al2O3-ZrO2 composites sintered at 1$650^{\circ}C$ for 4 hrs were about 91~98% and the maximum ratio of tetra-/mono-ZrO2 in Al2O3-20wt% ZrO2 composites was 62/38.

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Characteristics of Nano-Sized, α-2ZrO2·P2O5 Powder Prepared by Polyvinyl Alcohol Solution Method (Polyvinyl Alcohol 용액법에 의해 제조된 나노크기 α-2ZrO2·P2O5 분말의 특성 연구)

  • Ma, Chung-Il;Lee, Sang-Jin
    • Korean Journal of Materials Research
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    • v.27 no.4
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    • pp.179-183
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    • 2017
  • $2ZrO_2{\cdot}P_2O_5$ powder, which is not synthesized by solid reaction method, was successfully synthesized through PVA solution method. In this process, the firing temperature and the PVA content strongly affected the crystallization behavior and final particle size. A stable ${\alpha}$-phase $2ZrO_2{\cdot}P_2O_5$ was synthesized at a firing temperature of $1200^{\circ}C$ and holding time of 4 h. ${\beta}$-phase $2ZrO_2{\cdot}P_2O_5$ was observed, with un-reacted $ZrO_2$ phases, for firing temperatures lower than $1200^{\circ}C$. In terms of the PVA content effect, the powder prepared with a PVA mixing ratio of 12:1 showed stable ${\alpha}$-phase $2ZrO_2{\cdot}P_2O_5$; however, the ${\beta}$-phase was found to co-exist at relatively higher PVA content. The synthesized ${\alpha}$-phase $2ZrO_2{\cdot}P_2O_5$ powder showed an average particle size of 100~250 nm and an average thermal expansion coefficient of $-2.5{\times}10^{-6}/^{\circ}C$ in the range of room temp. ${\sim}800^{\circ}C$.

A Study on Fabrication of $Al_2O_3-ZrO_2$ Inorganic Membranes (알루미나-지르코니아 세라믹 막 제조에 관한 연구)

  • 김병훈;나용한
    • Journal of the Korean Ceramic Society
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    • v.32 no.10
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    • pp.1147-1161
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    • 1995
  • When ceramic membrance was made from metal salt solution in place of metal akoxide solution, crack free and good adhesion to supporter was optimized for sol stability and good adhesion force. A starting sol was prepared from aluminum oxychloride aqueous solutjion in order to inhibit the grain growthof Al2O3 during heat treatment. The crack free dip coating can't be achieved in 1mol/ι zirconium oxychloride solution because of the high viscosity which interferes with the hydration copolymerization between Al3+ ion and Zr4+ ion. Thus Al2O3-ZrO2 sol stability and viscosity for dip coating was effective when 0.01 mol/ι zirconium oxychloride was added. The minimizing of crack and achieving better adhesion to the supporter wa obtained by microwave drying, surfactant addition and ultrasonic dip coating in wet atmosphere. The result seems to minimize the capillary force and improve the adhesive ability to supporter during the process. Where the average pore size of Al2O3-ZrO2 ultrafilter ceramic membrane measured 17 Å by the BET method and observed γ-Al2O3 phase with tetragonal zirconia after firing at 700℃.

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Fabrication of $Y_2O_3-ZrO_2$ and $CaO-ZrO_2$ Fibers by Sol-Gel Process and Their Phase Characterization by Raman Microprobe (졸-겔법에 의한 $Y_2O_3-ZrO_2$계와 $CaO-ZrO_2$계 섬유의 제조 및 Raman Microprobe에 의한 상분석)

  • 황진명;은희태;권혁기
    • Journal of the Korean Ceramic Society
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    • v.31 no.1
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    • pp.104-114
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    • 1994
  • ZrO2 fibers were fabricated by means of the Sol-Gel process using Zr(O-nC3H7)4-H2O-C2H5OH-HNO3 solution as a starting material. The optimum experimental parameters such as molar ratio of starting materials, concentration, temperature, viscosity, the amounts of stabilizer and the pH of solution were determined. The experimentally determined optimum variables which produce good ZrO2 fibers were used to manufacture the Y2O3-and CaO-ZrO2 fibers. The amounts of Y2O3 and CaO were varied within the range from 1.5~5 mol% and 3~15 mol% respectively. The phase transformation and microstructural evolution of the fabricated ZrO2 gel fibers were investigated after heat treatments up to 120$0^{\circ}C$ by X-ray diffraction, Raman microprobe spectroscopy, SEM, and specific surface area and pore volume measurements. From the analysis of X-ray diffraction and Raman spectra, the phase of heat treated Y2O3-and CaO partially stabilized ZrO2 gel fibers(Y2O3:2.5~3 mol%, CaO:6~9 mol%) were identified as a tetragonal phase up to 100$0^{\circ}C$. The maximum tensile strength of 2.5Y2O3-97.5ZrO2 and 6CaO-94ZrO2 (in mol%) fibers heat treated at 100$0^{\circ}C$ for 1 hr was found be 1.3~2 GPa with diameters of 10~20 ${\mu}{\textrm}{m}$.

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Preparation of $ZrO_2/Al_2O_3-Mullite$ Composites Using the Silica Sol Infiltration Method (실리카 졸 침투법을 이용한 $ZrO_2/Al_2O_3-Mullite$ 복합체의 제조)

  • 현상훈;최지영
    • Journal of the Korean Ceramic Society
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    • v.29 no.9
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    • pp.719-728
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    • 1992
  • ZrO2/Al2O3-Mullite composites were prepared by infiltration of the silica sol to the porous ZrO2/Al2O3 bodies. The porous ZrO2/Al2O3 bodies for infiltration were fabricated using ZrO2 (20wt%)/Al2O3 composite powders synthesized by the emulsion-hot kerosene drying method. The preparation of silica sols was conducted by the hydrolysis-peptization of an alcoholic TEOS solution. When ZrO2/Al2O3-Mullite and ZrO2/Al2O3 composites were sintered at 1$650^{\circ}C$ for 4 hrs, both of them showed an excellent sinterability. As the amount of mullite added in the composites increased, the ratio of the tetragonal phase of zirconia to the monoclinic phase at the room temperature became higher. It was known that values of the fracture toughness of the ZrO2/Al2O3-Mullite composites were about 5.48 MPa.m1/2 much larger than that of the ZrO2/Al2O3 system.

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