• Title/Summary/Keyword: Solid-state synthesis

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A Study on the Microstructures and Ionic Conductivity of Li1.3Al0.3Ti1.7(PO4)3 with Different Synthesis Routes (합성 방법에 따른 Li1.3Al0.3Ti1.7(PO4)3 소결체의 미세 구조 및 이온전도 특성 연구)

  • Seul Ki Choi;Jeawon Choi;MinHo Yang
    • Journal of Powder Materials
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    • v.30 no.2
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    • pp.107-115
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    • 2023
  • Li1.3Al0.3Ti1.7(PO4)3(LATP) is considered a promising material for all-solid-state lithium batteries owing to its high moisture stability, wide potential window (~6 V), and relatively high ion conductivity (10-3-10-4 S/cm). Solid electrolytes based on LATP are manufactured via sintering, using LATP powder as the starting material. The properties of the starting materials depend on the synthesis conditions, which affect the microstructure and ionic conductivity of the solid electrolytes. In this study, we synthesize the LATP powder using sol-gel and co-precipitation methods and characterize the physical properties of powder, such as size, shape, and crystallinity. In addition, we have prepared a disc-shaped LATP solid electrolyte using LATP powder as the starting material. In addition, X-ray diffraction, scanning electron microscopy, and electrochemical impedance spectroscopic measurements are conducted to analyze the grain size, microstructures, and ion conduction properties. These results indicate that the synthesis conditions of the powder are a crucial factor in creating microstructures and affecting the conduction properties of lithium ions in solid electrolytes.

Sol-gel Synthesis and Properties of Phosphate Ceramics

  • Lee, Burtrand I.;Cao, Zhicheng;Samuels, Willam D.;Exarhos, Gregory J.
    • The Korean Journal of Ceramics
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    • v.6 no.4
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    • pp.390-395
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    • 2000
  • Silicon, titanium, zirconium phosphates were synthesized by starting with appropriate chemical precursors in a solution. The synthetic procedure, chemical and physical structures were examined by FT-IR, liquid and solid state NMR, TGA, SEM, XRD, etc. The phosphates were examined for thermal and electrical properties. Advantages of the synthesis technique and the data on unique structures and thermal properties are reported.

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Soft Solution Processing : Low-Energy Direct Fabrication of Advanced Inorganic Materials

  • Masahiro Yoshimura;한규승;Wojciech Suchanek
    • Bulletin of the Korean Chemical Society
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    • v.20 no.8
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    • pp.875-878
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    • 1999
  • A new concept ??soft solution processing?? has been introduced to fabricate advanced solid state materials in an economical, environmentally friendly, and energy and material efficient way. The prepared films show the desired and prospective properties despite of low temperature synthesis and no post-synthesis annealing. Successful examples demonstrate that soft solution processing is capable of preparing advanced materials with planned properties through the easy control of reaction conditions in a suitable aqueous solution in a single synthetic step without huge energy consumption and without any sophisticated equipment.

Eutectic Ceramic Composites by Melt-Solidification

  • Goto, Takashi;Tu, Rong
    • Journal of the Korean Ceramic Society
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    • v.56 no.4
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    • pp.331-339
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    • 2019
  • While high-temperature ceramic composites consisting of carbides, borides, and nitrides, the so-called ultra-high-temperature ceramics (UHTCs), have been commonly produced through solid-state sintering, melt-solidification is an alternative method for their manufacture. As many UHTCs are binary or ternary eutectic systems, they can be melted and solidified at a relatively low temperature via a eutectic reaction. The microstructure of the eutectic composites is typically rod-like or lamellar, as determined by the volume fraction of the second phase. Directional solidification can help fabricate more sophisticated UHTCs with highly aligned textures. This review describes the fabrication of UHTCs through the eutectic reaction and explains their mechanical properties. The use of melt-solidification has been limited to small specimens; however, the recently developed laser technology can melt large-sized UHTCs, suggesting their potential for practical applications. An example of laser melt-solidification of a eutectic ceramic composite is demonstrated.

Study on the Synthesis by Milling and Solid-State Reaction Method and Electrochemical Properties of LiNiO2 (기계적 혼합과 고상법에 의한 LiNiO2의 합성과 전기화학적 특성)

  • Kim, Hunuk;Youn, SunDo;Lee, Jaecheon;Park, HyeRyoung;Song, Myoungyaup
    • Journal of the Korean Ceramic Society
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    • v.42 no.5 s.276
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    • pp.319-325
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    • 2005
  • [ $LiNiO_2$ ] was synthesized by the solid-state method after mixing $LiOH{\cdot}H_2O$ and $Ni(OH)_2$ with SPEX mill. The optimum condition for the synthesis of $LiNiO_2$ was the calcination at $750^{\circ}C$ for 30h in $O_2$ stream after milling for 1 h. The $LiNiO_2$ synthesized under this condition showed relatively large value of $I_{003}/I_{104}$ and relatively small value of R-factor. When $LiNiO_2$ was cycled in 2.7$\~$4.15 V at 0.1C-rate, the first discharge capacity was not very large (145.8 mAh/g) but it showed good cycling performance. When $LiNiO_2$ was cycled in 2.7$\~$4.2 V at 0.1C-rate, the first discharge capacity was large but ,it showed poor cycling performance probably because of the transition of H2 hexagonal structure to H3 hexagonal structure. In addition, when $LiNiO_2$ was cycled in 1.0$\~$4.8 V at 1/24C- rate, the first discharge capacity was very large (257.7 mAh/g) and the discharge capacity increased with the number of cycles.

Synthesis and Photoluminescence Studies on Sr1-xBaxAl2O4 : Eu2+, Dy3+

  • Ryu, Ho-Jin;Singh, Binod Kumar;Bartwal, Kunwar Singh
    • Journal of the Korean Ceramic Society
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    • v.45 no.3
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    • pp.146-149
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    • 2008
  • Strontium-substituted $Sr_{1-x}Ba_xAl_2O_4:Eu^{2+},\;Dy^{3+}$ compositions were prepared by the solid state synthesis method. These compositions were characterized for their phase, crystallinity and morphology using powder x-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. Photoluminescence properties were investigated by measuring excitation spectra, emission spectra and decay time for varying Ba/Sr concentrations. Photoluminescence results show higher luminescence and long decay time for $Sr_{1-x}Ba_xAl_2O_4:Eu^{2+},\;Dy^{3+}$(x=0). This is probably due to the influence of the 5d electron states of $Eu^{2+}$ in the crystal field. Long persistence was observed for these compositions due to $Dy^{3+}$ co-doping.

Dry Media Reaction Procedure for Synthesis of α,β-Unsaturated Acids, α-Cyanoacrylonitriles and α-Cyanoacrylates via Knoevenagel Condensation Using NaHSO4·SiO2 Catalyst (NaHSO4·SiO2 촉매를 이용한 Knoevenagel 축합을 거친α,β의 불포화산, α-Cyanoacrylonitriles와 α-Cyanoacrylates의 합성을 위한 무수조건하의 반응 절차)

  • Gopalakrishnan, M.;Sureshkumar, P.;Kanagarajan, V.;Thanusu, J.;Thirunavukkarasu, S.
    • Journal of the Korean Chemical Society
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    • v.51 no.4
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    • pp.346-351
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    • 2007
  • Efficient stereoselective synthesis of α,β-Unsaturated acids, α-Cyanoacrylonitriles and α-Cyanoacrylates has been carried out in the presence of NaHSO4·SiO2 under solvent?free conditions with an E-geometry.

Leucite Synthesis from Solid-State Sintering (고상법에 의한 Leucite 합성)

  • Yoon, Dong-Sup;Lee, Byung-Ha
    • Journal of the Korean Ceramic Society
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    • v.42 no.4
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    • pp.282-286
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    • 2005
  • Leucite crystal has been utilized for dental porcelain due to its high thermal expansion coefficient to meet its counter metal side. Many industrial applications of leucite from the incongruently melting of potassium feldspar are used and its minimum temperature of crystallization is $1150^{\circ}C$. This study aimed to get leucite crystal from lower temperature through congruently melting, and the starting materials are taken from K-feldspar mainly, and aluminum hydroxide and potassium carbonate are additionally supplied to meet stoichiometry of leucite. We report that the leucite crystal can be synthesized in congruently melting from the temperature $950^{\circ}C$ through solid-state sintering with k-feldspar, potassium carbonate and aluminum hydroxide.

In-situ Synthesis of Cu-TiB2 Nanocomposite by MA/SPS

  • Kwon, Young-Soon;Kim, Ji-Soon;Kim, Hwan-Tae;Moon, Jin-Soo;D.V Dudina;O.I. Lomovsky
    • Journal of Powder Materials
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    • v.10 no.6
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    • pp.443-447
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    • 2003
  • Nano-sized $TiB_2$ was in situ synthesized in copper matrix through self-propagating high temperature synthesis (SHS) with high-energy ball milled Ti-B-Cu elemental mixtures as powder precursors. The size of $TiB_2$ particles in the product of SHS reaction decreases with time of preliminary mechanical treatment ranging from 1 in untreated mixture to 0.1 in mixtures milled for 3 min. Subsequent mechanical treatment of the product of SHS reaction allowed the $TiB_2$ particles to be reduced down to 30-50 nm. Microstructural change of $TiB_2$-Cu nanocomposite during spark plasma sintering (SPS) was also investigated. Under simultaneous action of pressure, temperature and electric current, titanium diboride nanoparticles distributed in copper matrix move, agglomerate and form a interpenetrating phase composite with a fine-grained skeleton.