• Title/Summary/Keyword: Solid state synthesis

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Synthesis and Mechanism of Ni-Doped Hibonite Blue Pigments (Ni-Doped Hibonite 파란색 안료의 합성과 발색기구)

  • Kim, Gumsun;Lee, Byung-Ha
    • Korean Journal of Materials Research
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    • v.24 no.1
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    • pp.43-47
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    • 2014
  • NiO-doped hibonite pigments were synthesized by the solid state method to get stabilized blue color pigment in both oxidation and reduction atmospheres. Optimum substitution condition with NiO for hibonite blue pigment was investigated. Experimental results were comparable to those of previous cobalt-minimization studies performed with other phosphate- or oxide-based cobalt-containing ceramic pigments (having olivine ($Co_2SiO_4$), spinel ($CoAl_2O_4$), or with co-doped willemite ($(Co,Zn)_2SiO_4$) structures). Composition was designed varying the NiO molar ratio increasing with $SnO_2$. The optimum substitution content is 0.93 mole NiO with 0.75mole $SnO_2$. The characteristics of the synthesized pigment were analyzed by XRD, Raman spectroscopy, SEM, and UV-vis. Synthesized pigment was applied to a lime-barium glaze with 10 wt% each and fired at an oxidation atmosphere of $1250^{\circ}C/1h$ and a reducing atmosphere $1240^{\circ}C/1h$. Blue color was obtained with $L^*a^*b^*$ values at 43.39, -6.78, -18.20 under a reducing atmosphere and 41.66, -6.36, -14.7 under and oxidation atmosphere, respectively.

A Water-Soluble Polyimide Precursor: Synthesis and Characterization of Poly(amic acid) Salt

  • Lee, Myong-Hoon;Jun Yang
    • Macromolecular Research
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    • v.12 no.3
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    • pp.263-268
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    • 2004
  • We have synthesized a water-soluble polyimide precursor, poly(amic acid) amine salt (PAD), from pyromellitic dianhydride (PMDA), 4,4'-oxydianiline, and N,N -dimethylethanolamine (DMEA) and have investigated in detail its properties with respect to the degree of salt formation (D$\_$sf/). The maximum value of D$\_$sf/ we obtained upon precipitation of the precursor solution into acetone was 79%. We synthesized a PAD having a D$\_$sf/ of 100% (PAD100) by the solid state drying of an organic solution. The precursors showed different solubility depending on the D$\_$sf/ to make up to 4 wt% solutions in water containing a small amount of DMEA. PAD100 is completely soluble in pure water. We investigated the imidization behavior of PAD in aqueous solution using various spectroscopic methods, which revealed that PAD 100 has faster imidization kinetics relative to that of the poly(amic acid)-type precursors. The resulting polyimide films prepared from an aqueous precursor solution possess almost similar physical and thermal properties as those prepared from N-methyl-2-pyrrolidone(NMP) solution. Therefore, we have demonstrated that PAD can be used as a water-based precursor of polyimide; this procedure avoids the use of toxic organic solvents, such as NMP.

Study on the Synthesis by Mechanical Grinding and Solid-State Reaction Method and the Electochemical Properties of $LiNiO^2$ (기계적 혼합과 고상법에 의한 $LiNiO^2$의 합성과 전기화학적 특성 연구)

  • 윤순도;이재천;박혜령;송명엽
    • 한국전기화학회:학술대회논문집
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    • 2004.06a
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    • pp.281-286
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    • 2004
  • [ $LiOH{\cdot}H^2O$ ]와 $Ni(OH)^2$를 기계적으로 혼합하여 고상법으로 $LiNiO^2$를 합성하고, $LiNiO^2$의 전기화학적 특성을 조사하였다. 기계적 혼합을 위해 SPEC mill을 사용하였으며, 1시간 동안 milling하여 공기 중 $450^{\circ}C$에서 5시간 동안 전처리한 후 $750^{\circ}C$에서 30시간 동안 산소를 흘려주면서 하소한 시료가 가장 좋은 전기화학적 특성을 나타내었다. $2.7\~4.15V$에서 0.1C로 충${\cdot}$방전시 초기방전용량은 그다지 높지 않았으나(145.8mAh/g) 좋은 싸이클 성능을 나타내었으며, $2.7\~4.2V$에서 0.1C로 충${\cdot}$방전시 높은 초기방전용량(164.7mAh/g)을 나타내었으나 싸비클 성능은 그리 좋지 않았는데, 이는 충${\cdot}$방전시 육방구조$(H^2)$에서 육방구조$(H^3)$로의 상전이가 영향을 주는 것으로 사료된다. 초기방전용량과 방전용량은 Cation mixing을 나타내는 $I^{003}/I^{104}$값보다 hexagonal ordering을 나타내는 R-factor에 더 의존하는 것으로 사료된다.

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The structure analysis of $Y_1Ba_2Cu_3O_x$ high Tc superconductor based on rietveld method (리트벨트 해석법을 이용한 $Y_1Ba_2Cu_3O_x$ 고온 초전도체의 구조분석)

  • 채기병;소대화
    • Electrical & Electronic Materials
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    • v.8 no.6
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    • pp.780-786
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    • 1995
  • For the execution of RIETAN program adopting Rietveld Analysis Method, the sample superconductor is made according to the solid state synthesis method at 920.deg. C for 24hrs, and was examined for the optimization of parameters needed to analyze Rietveld method with the input of the measured pattern data after measuring the pattern resulted from the X-ray diffraction. It was proven that the lattice constant of the superconductor which was consisted of Pmmm orthorhombic crystal structure in the analyzed space group correspond to the presented theoretical lattice constant a=3.8887(8).angs., b=3.8238(4).angs., c=11.7079.angs.. Therefore, it was examined and confin-ned that the R factor, which was compensated after analyzing the structure of superconductor resulted from this experimented data with the computer simulation, was refined to $R_{wp}$=8.83[%], $R_{P}$=6.47[%], $R_{I}$=10.08[%], $R_{F}$=7.19[%], $R_{E}$=3.76[%]. On the basis of these experimental data, the significant parameter such as the scale factor(S) and the zero point shift(Z) and FWHM value(U,V,W) were optimized as follows; S=2.0827E-3, Z=0.2146, U=4.2761E-2, V=1.7983E-2, and W=2.6768E-2.2.2.2.2.2.

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Synthesis and Piezoelectric Properties of PZT Ceramics will Improved Process (공정개선을 통한 PZT 세라믹스의 합성 및 압전특성)

  • 윤철수;송태권;박태곤;박인용;김명호
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.14 no.11
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    • pp.904-911
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    • 2001
  • High-density lead zirconate titanate(Pb(Zr$\_$0.53/Ti$\_$0.47/)O$_3$, PZT) ceramics were fabricated by a new milling-precipitation(MP) process improved from the conventional solid state process. This process was progressed by a milling impregnation through mixing ZrO$_2$ and TiO$_2$ powders with lead nitrate(Pb(NO$_3$)$_2$) water solution in zirconia ball media, and then milling precipitation was induced from precipitation of PbC$_2$O$_4$ by adding ammonium of oxalate monohydrate((NH$_4$)$_2$C$_2$O$_4$$.$H$_2$O) as a precipitant. As a result of this process, single-phase perovskite structure was formed at the calcination temperature of 750$\^{C}$ for Pb(Zr$\_$0.53/Ti$\_$0.47/)O$_3$ powders. In addition, the highest density at the sintering temperature of 1100$\^{C}$ was obtained, because of the highly sinterable PZT Powders ground through the re-milling process. Piezoelectric and dielectric properties of sintered sample were improved by MP process.

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SYNTHESIS OF METASTABLE ALLOYS BY ION MIXING IN THE BINARY METAL SYSTEMS AND THEORETICAL MODELLING

  • Liu, B.X.;Zhang, Z.J.;Jin, O.;Pan, F.
    • Journal of the Korean Vacuum Society
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    • v.4 no.S2
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    • pp.148-155
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    • 1995
  • (1) The metastable crystalline(MX) phases formed by ion mixing are classified into 5 types, i.e. the super-saturated solid solutions and the enlarged HCP-I phases reported earlier, and the newly observed FCC-I phases in hcp-based alloys, The FCC-ll and HCP-ll phases in bcc-based alloys. The growth kinetics of the MX phases is discussed. (2) The interfacial free energy in the multilayered films was found to play an important role in ion beam mixing(IM) induced amorphization. By adding sufficient interfaces, amorphous alloys were obtained even in the systems with rather positive heat of formation. (3) Gibbs free energy diagrams of some representative systems were constructed, by calculating the free energy curves of all the competing phases. Steady-state thermal annealing was conducted and the results confirmed the relevance of the constructed diagrams, which were inturn employed to interpret the MX phase formation as well as the glass forming ability upon IM in the binary metal systems.

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Synthesis of Lu3Al5O12:Ce3+ Nano Phosphor by Coprecipitation Method, and Their Optical Properties (공침법을 이용한 Lu3Al5O12:Ce3+ 나노 형광체 합성과 광학적 특성 분석)

  • Kang, Taewook;Kang, Hyeonwoo;Kim, Jongsu;Kim, Gwangchul
    • Journal of the Semiconductor & Display Technology
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    • v.18 no.4
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    • pp.51-56
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    • 2019
  • LuAG:Ce(Lu3Al5O12:Ce3+) nano phosphor were synthesized by applying the coprecipitation method. It is used to increase the color rendering of phosphor ceramic plate for high power LEDs and laser lighting. Internal quantum efficiency and absorption of LuAG:Ce nano phosphor are 51.5 % and 64.4 %, respectively, which is higher than the previously studied nano phosphors. The maximum absorption wavelength of this phosphor is 450 nm blue light, and the emission wavelength is 510 nm. The emission wavelength shifted to longer wavelength when the concentration of Ce increased in the heat treatment of the reducing atmosphere. Thermal quenching of LuAG nano phosphor was 70 % at 200 ℃, it was explained by their significant quenching of all raman scattering modes, implying the restriction of electron-phonon couplings caused by their defects.

Fabrication and Characterization of Ytterbium Silicates for Environmental Barrier Coating Applications (환경차폐코팅용 이터븀 실리케이트의 제조와 물성평가)

  • Choi, Jae-Hyeong;Kim, Seongwon
    • Journal of Surface Science and Engineering
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    • v.54 no.6
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    • pp.331-339
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    • 2021
  • Environmental barrier coatings(EBCs) are applied to the SiC/SiC ceramic matrix composites(CMCs) in order to protect CMCs from being corroded with water vapor by combustion gas in gas turbine engines. Ytterbium silicates, such as ytterbium monosilicate and ytterbium disilicate, are ones of the candidate materials for EBCs due to their excellent resistance to water vapor corrosion as well as thermal-expansion match with SiC. In this study, ytterbium silicates are fabricated with 2-step solid-state synthesis targeting ytterbium disilicate. After synthesizing ytterbium monosilicate, the mixtures of ytterbium monosilicate and SiO2 are heat-treated and densified by using pressureless sintering or hot pressing with a variety of heating conditions. The phase formation, thermal expansion, and oxidation behavior are examined with fabricated specimens. The final densified bodies are found to be composites between ytterbium monosilicate and ytterbium disilicate with different ratios, which results in 4.43 to 6.72×10-6/K range of coefficients of thermal expansion. The probability of these ytterbium silicates for EBC applications is also discussed.

Silicatein: Biosilicification and Its Applications (실리카테인: 생규화 및 응용)

  • Yang, Byeongseon;Yun, Jin Young;Cha, Hyung Joon
    • Journal of Marine Bioscience and Biotechnology
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    • v.10 no.2
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    • pp.34-43
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    • 2018
  • Silicon has become of increasing importance as the basic element of many high-technology products. Its synthesis is very difficult requiring high temperature solid-state reactions (> $1000^{\circ}C$) or lower temperature methods ($100-200^{\circ}C$) involving hydrothermal and solvothermal reactions under extreme pH conditions. In nature, on the other hand, a wide range of living organisms have collectively evolved the means of biosilicification at the astounding rate of gigatons/year. This is impressive because biosilicification in these organisms occurs under mild physiological conditions. Marine sponges possess the ability to sequester soluble silicon sources from their environments and assemble them into intricate 3D architecture. The advent of molecular biology has recently made it possible to glean molecular information about biosilicification from these systems and it turned out that enzyme silicatein is the core of biosilicification. In this review, biosilicification regulated by silicatein and its mechanism are described. Also, production of silicatein through recombinant technology and several applications of recombinant silicatein are described including immobilization of silicatein, formation of Au or Ag nanoparticles on nanowires, nanolithography approaches, core-shell materials, encapsulation, bone replacement materials, and microstructured optical fibers.

Synthesis and Luminescence of Sr2Si5N8:Eu2+ Red Phosphor for High Color-Rendering White LED (고연색 LED용 적색 Sr2Si5N8:Eu2+ 형광체의 합성 및 발광특성 연구)

  • Lee, Sung Hoon;Kim, Jong Su;Kang, Tae Wook;Ryu, Jong Ho;Lee, Sang Nam
    • Journal of the Semiconductor & Display Technology
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    • v.16 no.4
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    • pp.11-15
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    • 2017
  • Red phosphors, $Sr_2Si_5N_8:Eu^{2+}$, were synthesized as a single-phase crystal structure by optimizing carbon and $Eu^{2+}$ contents in a carbothermal reduction nitridation method. With increasing $Eu^{2+}$ contents, the photoluminescence spectra were red-shifted from 600 nm peak for 1 mol% for to 700 nm for 7 mol%. It was suggested that this red shift is attributed to the energy transfer from one low-energy sited $Eu^{2+}$ (1) to other high-energy sited $Eu^{2+}$ (2). Finally, the best red sample (620 nm emission peak and 80 nm half width for 3 mole% of $Eu^{2+}$) was packaged on a Blue LED together with two additional green and yellow phosphors, the fabricated White LED showed a high color-rendering index of 90 and white color coordinates of x= 0.321 and y = 0.305.

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