• Title/Summary/Keyword: Solid-State Reaction

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Solid-State $^{51}V$ NMR and Infrared Spectroscopic Study of Vanadium Oxide Supported on $TiO_2-ZrO_2$

  • Park, Eun Hui;Lee, Man Ho;Son, Jong Rak
    • Bulletin of the Korean Chemical Society
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    • v.21 no.9
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    • pp.913-918
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    • 2000
  • Vanadium oxide catalyst supported on TiO2-ZrO2 has been prepared by adding Ti(OH)4-Zr(OH)4 powder to an aqueous solution of ammonium metavanadate followed by drying and calcining at high temperatures. The char-acterization ofthe prepared catalysts was performed using solid-state 51V NMR and FTIR.In thecase ofcalci-nation temperature at 773 K, vanadium oxide was in a highly dispersed state for the samples containing low loading V2O5 below 25 wt %, but for samplescontaining high loading V2O5 equal to or above 25 wt %, vana-dium oxidewas well crystallized due to the V2O5 loading exceeding the formation of monolayer on the surface of TiO2-ZrO2.The ZrV2O7 compound was formed through the reactionof V2O5 and ZrO2 at 773-973 K, where-as the V3Ti6O17 compound was formedthrough the reaction of V2O5 and TiO2 at 973-1073 K. The V3Ti6O17 compound decomposed to V2O5 and TiO2 at 1173 K, which were confirmed by FTIR and 51V NMR.

Optical Properties of Y3Al5O12;Ce3+,Pr3+ Transparent Ceramic Phosphor for High Power White Lighting (고출력 백색 광원용 Y3Al5O12;Ce3+,Pr3+ 투명 세라믹 형광체의 광학특성)

  • Kang, Taewook;Lim, Seokgyu;Kim, Jongsu;Jeong, Yongseok
    • Korean Journal of Materials Research
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    • v.29 no.2
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    • pp.116-120
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    • 2019
  • We prepared $Y_3Al_5O_{12};Ce^{3+},Pr3^{+}$ transparent ceramic phosphor using a solid state reaction method. By XRD pattern analysis and SEM measurement, our phosphors reveal an Ia-3d(230) space group of cubic structure, and the transparent ceramic phosphor has a polycrystal state with some internal cracks and pores. In the Raman scattering measurement with an increasing temperature, lattice vibrations of the transparent ceramic phosphor decrease due to its more perfect crystal structure and symmetry. Thus, low phonon generation is possible at high temperature. Optical properties of the transparent ceramic phosphor have broader excitation spectra due to a large internal reflection. There is a wide emission band from the green to yellow region, and the red color emission between 610 nm and 640 nm is also observed. The red-yellow phosphor optical characteristics enable a high Color Rendering Index (CRI) in combination with blue emitting LED or LD. Due to its good thermal properties of low phonon generation at high temperature and a wide emission range for high CRI characteristics, the transparent ceramic phosphor is shown to be a good candidate for high power solid state white lighting.

Growth Mechanism and Crystal Ordering of Spherulitic Patterns in a Belousov-Zhabotinsky Type Reaction System

  • Yadav, Narendra;Majhi, S.S.;Srivastava, P.K.
    • Bulletin of the Korean Chemical Society
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    • v.33 no.10
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    • pp.3397-3406
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    • 2012
  • Three types of spherulitic morphologies have been investigated in dual substrate mode of Belousov-Zhabotinsky (BZ) type reaction system. Prior to growth of spherulites, three distinct patterning behaviors have been observed sequentially during the reaction process. Initial and the early-phase of reaction showed the emergence of concentric ring-like wave patterns. A colloidal-state of reaction consists of numerous fine solid particles, which forms primarily some nucleation centers of dendritic characters. The nucleation centers were found to grow in sizes and shapes with the progress of reaction. It leads to growth of dendritic-like spherulitic crystal patterns. The resultant spherulites showed transitions in their morphologies, including sea-weeds and rhythmic spherulitic crystal patterns, by the effects substituted organic substrate and in the higher concentration of bromate-initiator respectively. The branching mechanism and crystal ordering of spherulitic textures were studied with help of optical microscope (OPM) and scanning electron microscope (SEM). Characteristics of crystal phases were also evaluated using X-ray diffraction (XRD) and differential thermal analysis (DTA). Results indicated that the compositions of reactants and crystal orderings were interrelated with morphological transitions of spherulites as illustrated and described.

Synthesis of Li2MnSiO4 by Solid-state Reaction (고상반응법을 이용한 Li2MnSiO4 합성)

  • Kim, Ji-Su;Shim, Joong-Pyo;Park, Gyung-Se;Sun, Ho-Jung
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.25 no.5
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    • pp.398-402
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    • 2012
  • Synthesis of $Li_2MnSiO_4$ was attempted by the conventional solid-state reaction method, and the phase formation behavior according to the change of the calcination condition was investigated. When the mixture of the three source materials, $Li_2O$, MnO and $SiO_2$ powders, were used for calcination in air, it was difficult to develop the $Li_2MnSiO_4$ phase because the oxidation number of $Mn^{2+}$ could not be maintained. Therefore, two-step calcination was applied: $Li_2SiO_3$ was made from $Li_2O$ and $SiO_2$ at the first step, and $Li_2MnSiO_4$ was synthesized from $Li_2SiO_3$ and MnO at the second step. It was easy to make $Li_2MnSiO_3$ from $Li_2O$ and $SiO_2$. $Li_2MnSiO_4$ single phase was developed by the calcination at $900^{\circ}C$ for 24 hr in Ar atmosphere as the oxidation of $Mn^{2+}$ was prevented. However, the $Li_2MnSiO_4$ was ${\gamma}-Li_2MnSiO_4$, one of the polymorph of $Li_2MnSiO_4$, which could not be used as the cathode materials in Li-ion batteries. By applying the additional low temperature annealing at $400^{\circ}C$, the single phase ${\beta}-Li_2MnSiO_4$ powder was synthesized successfully through the phase transition from ${\gamma}$ to ${\beta}$ phase.

Preparation and characterization of CoAl2O4 blue ceramic nano pigments by attrition milling (어트리션밀을 이용한 CoAl2O4 나노 무기 안료의 제조 및 특성 평가)

  • Lee, Ki-Chan;Yoon, Jong-Won;Kim, Jin-Ho;Hwang, Kwang-Taek;Han, Kyu-Sung
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.23 no.5
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    • pp.255-264
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    • 2013
  • Cobalt aluminate ($CoAl_2O_4$) is a highly stable pigment with excellent resistance to light, weather, etc., which has resulted in widespread use as a ceramic pigment. Due to the unique optical characteristics, $CoAl_2O_4$ is generally used as a coloring agent to decorate porcelain products, glass, paints and plastics. Here, $CoAl_2O_4$ pigments were synthesized by polymerized complex method and solid state reaction. Then $CoAl_2O_4$ pigment were grinded using the attrition milling with 1 mm size zirconia ball for 3 hours. The attrition milling process was performed at the constant speed of 800 rpm and ball to powder weight ratio (BPR) was 100 : 1. The characteristics of synthesized pigment were analyzed by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), particle size analyser (PSA) and CIE $L^*a^*b^*$. The XRD patterns of $CoAl_2O_4$ show single phase spinel structure. The particle size of $CoAl_2O_4$ measured by FE-SEM, TEM and PSA analysis was in the range of 100~200 nm. The blue color of obtained $CoAl_2O_4$ pigments could be confirmed through CIE $L^*a^*b^*$ measurement.

Synthesis and Biocompatibility of the Hydroxyapatite Ceramic Composites from Tuna Bone(I) - The Sintering Properties of Hydroxyapatite and Hydroxyapatite- Containing Wollastonite Crushed with Dry Milling Process - (참치 뼈를 이용한 Hydroxyapatite 세라믹 복합체의 합성 및 생체 친화성(제1보)-건식법으로 분쇄한 Hydroxyapatite 및 Wollastonite가 첨가된 소결체의 특성-)

  • Kim, Se-Kwon;Lee, Chang-Kook;Byun, Hee-Guk;Jeon, You-Jin;Lee, Eung-Ho;Choi, Jin-Sam
    • Applied Chemistry for Engineering
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    • v.8 no.6
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    • pp.994-999
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    • 1997
  • The sintering properties of hydroxyapatite isolated from tuna bone and hydroxyapatite-containing wollastonite sintered by solid-state reaction was investigated. As the sinterability of hydroxyapatite dependent upon the particle size by dry milling, it showed a sintering. But the hydroxyapatite-containing wollastonite was appeared good sinterability. On X-ray measurements, the major phases of hydroxyapatite-containing wollastonite by solid state reaction at $1250^{\circ}C$ were identified as hydroxyapatite and pseudowollastonite(${\alpha}-CaSiO_3$). And the phases appeared as whitlockite [$Ca_3(PO_4)_2$] by decomposition of hydroxyapatite at higher temperature above $1250^{\circ}C$. The shapes of microstructure on SEM images changed from porous to dense bulk by elevating temperature. The mean bending strength of hydroxyapatite-containing wollastonite sintered by solid-state reaction at $1300^{\circ}C$ was about 18 MPa, it was close to the cancellous bone's maximum strength, 20 MPa.

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Characteristics and thermal stability of SrAl2O4: Eu2+, Dy3+ long afterglow phosphors synthesized solid state reaction and polymerized complex method (고상반응법과 착체중합법으로 합성된 SrAl2O4: Eu2+, Dy3+ 축광성 형광체의 특성 및 열적 안정성 평가)

  • Kim, Tae-Ho;Hwang, Hae-Jin;Kim, Jin-Ho;Hwang, Kwang-Taek;Han, Kyu-Sung
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.26 no.5
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    • pp.193-200
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    • 2016
  • Characteristics of $SrAl_2O_4:Eu^{2+}$, $Dy^{3+}$ phosphorescent phosphors synthesized by solid state reaction and polymerized complex method were comparatively analyzed. In order to evaluate thermal stability of $SrAl_2O_4:Eu^{2+}$, $Dy^{3+}$ phosphorescent phosphors at high temperature, phosphorescent properties of $SrAl_2O_4:Eu^{2+}$, $Dy^{3+}$ were investigated with thermal treatment at $1250^{\circ}C$ under reducing atmosphere, which was the general heat treatment conditions for ceramic manufacturing process. The phosphorescent properties of thermally treated $SrAl_2O_4:Eu^{2+}$, $Dy^{3+}$ phosphors synthesized by solid state reaction and polymerized complex method were investigated. The crystal structure and crystallite size were observed through XRD analysis. Microstructure and particle size of thermally treated $SrAl_2O_4:Eu^{2+}$, $Dy^{3+}$ phosphors were analyzed by SEM and PSA. Photoluminescence and afterglow characteristics of thermally treated $SrAl_2O_4:Eu^{2+}$, $Dy^{3+}$ phosphorescent phosphors were measured by spectrofluorometer.

Surface Modification Reaction of Photocatalytic Titanium Dioxide with Triethoxysilane for Improving Dispersibility

  • Lee, Myung-Jin;Kim, Ji-Ho;Park, Young-Tae
    • Bulletin of the Korean Chemical Society
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    • v.31 no.5
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    • pp.1275-1279
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    • 2010
  • We have carried out the surface modification of photocatalytic $TiO_2$ with triethoxysilane through dehydrogenation reaction and characterized the modified photocatalyst by spectroscopic methods, such as FT-IR, solid-state $^{29}Si$ MAS NMR, XPS, and XRF, etc. We also examined photocatalytic activity of the immobilized photocatalytic titanium dioxide with triethoxysilane by decolorization reaction of dyes such as cong red and methylene blue under visible light. Dispersion test showed that the photocatalytic titanium dioxide immobilized with triethoxysilane group has kept higher dispersibility than titanium dioxide itself. No appreciable precipitation takes place even after standing for 24 h in the 4:6 mixture ratio of ethanol and water.

Preparation of Fine Alumina Powder

  • Soh, Dea-Wha;Jeon, Yong-Woo;N., Korobova
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2002.07b
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    • pp.670-673
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    • 2002
  • Powder synthesis using the alkoxy precursor technique exhibits processing flexibility not available in traditional high temperature solid-state reaction. With proper process control, impurities can be reduced to very low levels. The major distinction of the present work lies in the method of accomplishing the hydrolysis reaction. In the present case, water is not added to the system. Instead the metal alkoxide/alcohol solution is heated to a temperature at which water is formed through dehydration of the alcohol solvent, causing precipitation of the corresponding metal oxide (hydroxide). The present method provides a means of producing amorphous alumina.

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Reaction Path of Cu2ZnSnS4 Nanoparticles by a Solvothermal Method Using Copper Acetate, Zinc Acetate, Tin Chloride and Sulfur in Diethylenetriamine Solvent

  • Chalapathy, R.B.V.;Jung, Gwang Sun;Ko, Young Min;Ahn, Byung Tae;Kown, HyukSang
    • Current Photovoltaic Research
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    • v.1 no.2
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    • pp.109-114
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    • 2013
  • $Cu_2ZnSnS_4$ (CZTS) nanoparticles were synthesized by a solvothermal method using copper (II) acetate, zinc acetate, tin chloride, and sulfur in diethylenetriamine solvent. Binary sulfide particles such as CuS, ZnS, SnS, and $SnS_2$ were obtained at $180^{\circ}C$; single-phase CZTS nanoparticles were obtained at $280^{\circ}C$. CZTS nanoparticles with spherical shape and grain size of 40 to 60 nm were obtained at $280^{\circ}C$. In the middle of 180 and $280^{\circ}C$, CZTS and ZnS phases were found. The time variation of reaction at $280^{\circ}C$ revealed that an amorphous state formed first instead of binary phases and then the amorphous phase was converted to crystalline CZTS state; it is different reaction path way from conventional solid-state reaction path of which binary phases react to form CZTS. CZTS films deposited and annealed from single-phase nanoparticles showed porous microstructure and poor adhesion. This indicates that a combination of CZTS and other flux phase is necessary to have a dense film for device fabrication.