• Title/Summary/Keyword: Solid state synthesis

Search Result 356, Processing Time 0.034 seconds

Synthesis and Characterization of V2O - Doped Karrooite Brown Pigments (V2O5가 고용된 Karrooite계의 Brown색 안료합성과 특성)

  • Kim, Gum-Sun;Lee, Byung-Ha
    • Journal of the Korean Ceramic Society
    • /
    • v.48 no.4
    • /
    • pp.303-306
    • /
    • 2011
  • [ $V_2O_5$ ]doped Karrooite pigments were synthesized by the solid state method to get stabilized brown pigment in oxidation and reduction atmosphere. Optimum substitution condition and limited dopant with $V_2O_5$ for Karrooite pigment was investigated. With calcination at $1250^{\circ}C{\sim}1400^{\circ}C$, compositions were designed varying $V_2O_5$ molar ratio by increasing 0.02mole to the formula $Mg_1-xTi_2-xM_{2x}O_5$(x = 0.01~0.09 mole). Synthesized pigments were analyzed by XRD, Raman spectroscopy and UV-vis. When $V_2O_5$ was doped from 0.01 to 0.05 mole, single phase of Karrooite was observed at temperature $1300^{\circ}C$ and soaking time 4h by Raman spectroscopy. However, it was found that excess $VO_2$ peak appeared with 0.07 and 0.09 mole of $V_2O_5$ doped to $MgTi_2O_5$. This result indicated that the maximum limit of solid solution is 0.05 mole $V_2O_5$. Karrooite pigments were applied as a ceramic pigment to achieve brown colors in lime magnesia glaze and lime barium graze at both of oxidation and reduction atmosphere. CIE color coordinates are $L^*$ = 40.34, $a^*$ = 9.94, $b^*$ = 21.40 in lime magnesia glaze.

Properties of Low Temperature Sintering of La0.8Sr0.2Ga0.8Mg0.2-xZnxO2.8 (X = 0.0 - 0.05) Electrolyte (La0.8Sr0.2Ga0.8Mg0.2-xZnxO2.8(X=0.0~0.05) 전해질의 저온 소결 특성)

  • Lim, Kyoung Tae;Lee, Chung Hwan;Yu, Ji Haeng;Peck, Dong-Hyun;Baik, Kyeong Ho
    • Journal of the Korean Ceramic Society
    • /
    • v.51 no.3
    • /
    • pp.208-217
    • /
    • 2014
  • $La_{0.8}Sr_{0.2}Ga_{0.8}Mg_{0.2-x}Zn_xO_{2.8}$(LSGMZ, X=0-0.05) was prepared using a solid state reaction method. Two secondary phases ($LaSrGaO_4$ and $LaSrGa_3O_7$) of powders were identified by X-ray diffraction analysis. The relative amount of these secondary phases depended on the calcination conditions (temperature and time) and Zn content. The sintering density of LSGMZ was enhanced by increasing the Zn content and calcination temperature at the low sintering temperatures ($1250-1300^{\circ}C$). The relationship between the sintering density of LSGMZ and the synthesis conditions was discussed considering the phase analysis results.

Synthesis and Characterization of LSCF/CGO Composite Cathode for SOFC (SOFC용 LSCF/CGO 공기극의 제조 및 특성연구)

  • Park, Jae-Layng;Lim, Tak-Hyoung;Lee, Seung-Bok;Park, Seok-Joo;Shin, Dong-Ryul;Han, Kyoo-Seung;Song, Rak-Hyun
    • Journal of Hydrogen and New Energy
    • /
    • v.21 no.1
    • /
    • pp.19-25
    • /
    • 2010
  • Composites of LSCF($La_{0.6}Sr_{0.4}Co_{0.2}Fe_{0.8}O_{3-\delta}$) and CGO (gadolinium doped ceria)-based ceramics are logical candidate cathode materials with CGO electrolytes. LSCF with perovskite structure was synthesized and investigated by Solid State Reaction (SSR) method used as cathode materials for SOFC (solid oxide fuel cell). The optimized temperature was $1100^{\circ}C$ to synthesize $La_{0.6}Sr_{0.4}Co_{0.2}Fe_{0.8}O_{3-\delta}$ with rhombohedral structure. The polarization resistance of the LSCF/CGO (50:50 wt.%) was smaller than that of other composite cathodes. The analysis of the EIS data of LSCF/CGO suggests that the diffusion and adsorption-desorption of oxygen can be the key process in the cathodic reaction.

Electrical Properties of Bi-doped Apatite-type Lanthanum Silicates Materials for SOFCs (중·저온 영역 SOFC용 고체 전해질로의 응용을 위한 Bi가 첨가된 아파타이트형 란타늄 실리케이트의 전기적 특성)

  • Kim, Dae-Young;Jeong, Gwang-Ho;Lee, Sung-Gap
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
    • /
    • v.25 no.6
    • /
    • pp.486-490
    • /
    • 2012
  • $La_{7.33}Bi_2(SiO_4)_6O_2$ specimens were fabricated by standard solid-state synthesis route for solid oxide electrolytes. The calcined powders exhibited uniform particles with a mean particle size of about $28{\mu}m$. The room-temperature structure of $La_{7.33}Bi_2(SiO_4)_6O_2$ specimens was analyzed as hexagonal, space group P63 or P63/m, and the unit cell volume increased with increase a sintering temperature. The specimens sintered at $1,175^{\circ}C$ showed X-ray patterns of homogeneous apatite single phase without the second phase such as $La_2Si_2O_7$ and $La_2SiO_5$. The specimen sintered at $1,175^{\circ}C$ showed the maximum sintered density of 5.49 $g/cm^3$. Increasing the sintering temperature, total conductivities increased, activation energy decreased and the values were $1.98{\times}10^{-5}Scm-1$ and 1.23 eV, respectively.

Crack propagation behavior of in-situ structural gradient Ni/Ni-aluminide//Ti/Ti-aluminide laminate materials (Ni/Ni-aluminide//Ti/Ti-aluminide 구조경사형 층상재료의 균열 전파 거동)

  • Chung, D.S.;Kim, J.K.;Cho, H.
    • Journal of the Korean Crystal Growth and Crystal Technology
    • /
    • v.15 no.6
    • /
    • pp.269-275
    • /
    • 2005
  • Ni/Ni-aluminide/Ti/Ti-aluminide laminate composite, considered as a functionally gradient material, was manufactured by thin foil hot press technique. Thick intermetallic layers of NiAl and $TiAl_3$ were formed by a self-propagating high-temperature synthesis (SHS) reaction, and thin continuous taters of $Ni_3Al$ and TiAl were formed by a solid-state diffusion. Fracture resistance with loading along the crack arrester direction is higher than crack divider direction due to the interruption of crack growth in metal layers. The $Ni_3Al$ and NiAl intermetallic layer showed cleavage and intergranular fracture behavior, respectively, while the fracture mode of $TiAl_3$ layer was found to be an intragranular cleavage. The debonding between metal and intermetallic layer and the pores were observed in the Ni/Ni-aluminide layers, resulting in the lower fracture resistance. With the results of acoustic emission (AE) source characterization the real time of failure and the effect of AE to crack growth could be monitored.

Fabrication of ZrB2-based Composites for Ultra-high Temperature Materials (초고온 소재용 ZrB2계 복합소재의 제조)

  • Kim, Seong-Won;Chae, Jung-Min;Lee, Sung-Min;Oh, Yoon-Suk;Kim, Hyung-Tae;Nahm, Sahn
    • Journal of Powder Materials
    • /
    • v.16 no.6
    • /
    • pp.442-448
    • /
    • 2009
  • $ZrB_2$-based composites are candidate materials for ultra-high temperature materials (UHTMs). $ZrB_2$ has become an indispensable ingredient in UHTMs, due to its high melting temperature, relatively low density, and excellent resistance to thermal shock or oxidation. $ZrB_2$ powders are usually synthesized by solid state reactions such as carbothermal, borothermal, or combined carbothermal reaction. SiC is added to this system in order to enhance the oxidation resistance of $ZrB_2$. In this study, $ZrB_2$?based composites were successfully synthesized and densified through two different processing paths. $ZrB_2$ or $ZrB_2$ 25 vol.%SiC was fully synthesized from oxide starting materials with reducing agents after heat treatment at 1400$^{\circ}C$. Besides, $ZrB_2$?20 vol.%SiC was fully densified with $B_4C$ as a sintering additive after hot pressing at 1900$^{\circ}C$. The synthesis mechanism and the effect of sintering additives on densification of $ZrB_2$ ?SiC composites were also discussed.

Synthesis and Luminescence Properties of Lanthanide Complexes of a Novel Polyaminopolycarboxylate Ligand

  • Tang, Chang-Quan;Tang, Rui-Ren;Tang, Chun-Hua;Zeng, Zhi-Wen
    • Bulletin of the Korean Chemical Society
    • /
    • v.31 no.5
    • /
    • pp.1283-1288
    • /
    • 2010
  • A novel polyaminopolycarboxylate ligand with many coordination sites, N,N,$N^1,N^1,N^2,N^2$-[( 2,4,6-tri(aminomethyl)-pyridine]hexakis(acetic acid) (TPHA), was designed and synthesized and its lanthanide complexes $Na_6Tb_2$(TPHA)$Cl_6{\cdot}14H_2O$, $Na_6Eu_2$(TPHA)$Cl_6{\cdot}8H_2O$, $Na_6Gd_2$(TPHA)$Cl_6{\cdot}11H_2O$ and $Na_6Sm_2$(TPHA)$Cl_6{\cdot}9H_2O$ were successfully prepared. The ligand and the complexes were characterized by elemental analysis, IR, mass, NMR and TG-DTA. The TG-DTA studies indicated that the complexes had a high thermal stability, whose initial decomposition temperature was over $270^{\circ}C$. The luminescence properties of the complexes in solid state were investigated and the results suggested that $Tb^{3+}$ and $Eu^{3+}$ ions could be sensitized efficiently by the ligand, especially the Tb(III) complex displayed a very strong luminescence intensity (> 10000) and only displayed characteristic metal-centered luminescence. Also, the correlative comparison between the structure of ligand and luminescence properties showed how the number of the coordination atoms of ligand can be a prominent factor in the effectiveness of ligand-to-metal energy transfer.

Preparation and Luminescence Properties of $Y_{2-x}Gd_xO_3:Eu$ Phosphors by Pechini Method (페치니법에 의한 $Y_{2-x}Gd_xO_3:Eu$ 형광체의 제조와 발광 특성)

  • Lee, Dong-Kyu;Lee, Jin-Hwa;Ahn, Byung-Chul;Jun, Sang-Bae
    • Journal of the Korean Applied Science and Technology
    • /
    • v.23 no.3
    • /
    • pp.207-214
    • /
    • 2006
  • $Y_{2-x}Gd_xO_3:Eu$, phosphors for plasma display panel(PDP), were prepared by Pechini method which use yttriun chloride, gadolinium chloride, and europium oxide as starting materials. This method is a different way to the synthesis of europium(Eu)-doped phosphors, and it consists of the formation of a polymeric resin obtained by polyesterification between metal chelate compounds and a polyfunctional alcohol. This needs lower temperature than solid-state synthetic method. The prepared $Y_{2-x}Gd_xO_3:Eu$ phosphor particles had spherical shape and coherence. The luminescence intensity of $Y_{2-x}Gd_xO_3:Eu$ phosphor particles increased according to the increase of gadolinium(Gd) content(to 0.8mol%), and $Y_{1.2}Gd_{0.8}O_3:Eu$ phosphors had the highest luminescence intensity under vacuum ultra violet(VUV) excitation. The optimum concentration of Eu in the phosphor and optimum calcination temperature was 3wt% and $1100^{\circ}C$. The prepared phosphors were consist of particle, and its size was between 100nm and 150nm. Among the different polyfunctional alcohols, diethylene glycol(DEG) improved the luminescence intensities of phosphors more than other additives. The Pechini method proved that it is demonstrated to be suitable for the synthesis of phosphors used in PDP.

Synthesis of $LiCoO_{2}$ powders from precursors prepared by precipitation process

  • Park, Cheong-Song;La, Jung-In;Kim, Do-Youn
    • Journal of the Korean Crystal Growth and Crystal Technology
    • /
    • v.12 no.2
    • /
    • pp.87-90
    • /
    • 2002
  • $LiCoO_{2}$ powders were synthesized at various temperatures using lithium hydroxide and cobalt hydroxide as precursors prepared by precipitation process and freeze-drying. In this study, the$LiCoO_{2}$ samples were synthesized via a solid state reaction with various LiOH concentration between 10 % and 30 % excess. And $LiCoO_{2}$powders were calcined at 600~$800^{\circ}C$ in a short time. Measurements of XRD and SEM were performed to characterize the properties of the prepared materials. The effect of amount of Li ions on the structural change in powder has been examined using the XRD analysis. For the not added excess of LiOH, CoOOH phase presented in the XRD pattern of $LiCoO_{2}$ due to loss of Li ions during firing. The morphology and particle size of the powders were examined using SEM. The obtained powders are high temperature-$LiCoO_{2}$HT-LiCoO$_{2}$) and homogeneous with the range of grain size in the order of hundreds of nanometers. The effects of variation of LiOH concentration on the structural change in powder were investigated using the Rietveld analysis. As an analysis result, c/a is constant by 4.99 on all occasions. Finally, the structure of HT-$LiCoO_{2}$ was simulated by the commercial software $Creius^{2}$(Molecular Simulations, Inc.) from the results of Rietveld analysis.

A Synthesis of Mullite and Cordierite Ceramics by Solution-Polymerzation Route Based on PVA (PVA를 이용한 Solution-Polymerzation 합성법에 의한 Mullite, Cordierite 세라믹스의 합성)

  • 이용석;이병하
    • Journal of the Korean Ceramic Society
    • /
    • v.41 no.2
    • /
    • pp.151-157
    • /
    • 2004
  • Because of the excellent thermal and chemical properties of mullite and cordierite as the stable oxide ceramic materials, they were widely used from engineering materials to electronic materials. Notwithstanding of their high demands, mullite was synthesised because it is not existed in nature. It is also difficult to produce cordierite of fine powder with high purity due to the narrow range of synthetic temperature. Mullite was synthesised by solid state reaction. However, synthesized mullite has been inhomogeneous. Because of the facts, various synthetic methods have been studied so far including sol-gel method. The purpose of this study is to synthesis mullite and cordierite of fine powder with high purity at the lower temperature by solution-polymerization route using PVA as a polymer carrier, which is an economical method by using low cost materials. As a result, mullite and cordierite were produced with mono crystal phase at 1200$^{\circ}C$ and 1250$^{\circ}C$, respectively, and their surface area over 20 ㎡/g.