• Title/Summary/Keyword: Solid-state synthesis

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SYNTHESIS OF BLOCK COPOLYMERS CONTAINING POLYPEPTIDE AND ITS BIOMEDICAL APPLICATION

  • Cho, Chong-Su
    • Proceedings of the Korean Society of Sericultural Science Conference
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    • 1997.06a
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    • pp.159-169
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    • 1997
  • ABA-type(or AB) block copolymers composed of poly(${\gamma}$-alkyl L-glutamate) (PALG)[or poly(L-leucine)] as the A component and polyether[or poly (N-isopropy1 acrylamide) as the B component were synthesized by polymerization of (${\gamma}$-alkyl L-glutamate N-carboxyanhydride initiated by primary amined located at both(or one) ends of the polymer chains. Structural studies of the block copolymers were performed in the solution and solid state. Also, artificial skin, drug delivery system of the block copolymers and cell attachment onto the copolymer were carried out for biomedical applications.

Theory of Nanoparticles Mechanosynthesis

  • Urakaev, Farit Kh.
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2005.07a
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    • pp.405-406
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    • 2005
  • A theoretical investigation of the solid-phase mechanochemical synthesis of nano-sized target product on the basis of dilution of the initial powdered reagent mixture by another product of an exchange reaction is presented. On the basis of the proposed 3-mode particle size distribution in mechanically activated mixture, optimal molar ratios of the components in mixture are calculated, providing the occurrence of impact-friction contacts of reagent particles and excluding aggregation of the nanosized particles of the target reaction product. Derivation of kinetic equations for mechanochemical synthesis of nanoscale particles by the final product dilution method in the systems of exchange reactions is submitted. On the basis of obtained equations the necessary times of mechanical activation for complete course of mechanochemical reactions are designed. Kinetics of solid phase mechanosynthesis of nano-TlCl by dilution of initial (2NaCl + $Tl_2SO_4$) mixture with the exchange reaction product (diluent, $zNa_2SO_4$, $z=z^*=11.25$) was studied experimentally. Some peculiar features of the reaction mechanism were found. Parameters of the kinetic curve of nano-TlCl obtained experimentally were compared with those for the model reaction KBr + TlCl + zKCl = (z + 1) KCl + TlBr ($z=z_l^*=13.5$), and for the first time the value of mass transfer coefficient in a mechanochemical reactor with mobile milling balls was evaluated. Dynamics of the size change was followed for nanoparticle reaction product as a function of mechanical activation time.

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Fabrication of a Full-Scale Pilot Model of a Cost-Effective Sodium Nickel-Iron Chloride Battery Over 40 Ah

  • Lee, Dong-Geun;Ahn, Byeong-Min;Ahn, Cheol-Woo;Choi, Joon-Hwan;Lee, Dae-Han;Lim, Sung-Ki
    • Journal of Electrochemical Science and Technology
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    • v.12 no.4
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    • pp.398-405
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    • 2021
  • To fabricate a full-scale pilot model of the cost-effective Na-(Ni,Fe)Cl2 cell, a Na-beta-alumina solid electrolyte (BASE) was developed by applying a one-step synthesis cum sintering process as an alternative to the conventional solid-state reaction process. Also, Fe metal powder, which is cheaper than Ni, was mixed with Ni metal powder, and was used for cathode material to reduce the cost of raw material. As a result, we then developed a prototype Na-(Ni,Fe)Cl2 cell. Consequently, the Ni content in the Na-(Ni,Fe)Cl2 cell is decreased to approximately (20 to 50) wt.%. The #1 prototype cell (dimensions: 34 mm × 34 mm × 235 mm) showed a cell capacity of 15.9 Ah, and 160.3 mAh g-1 (per the Ni-Fe composite), while the #2 prototype cell (dimensions: 50 mm × 50 mm × 335 mm) showed a cell capacity of 49.4 Ah, and 153.2 mAh g-1 at the 2nd cycle.

La0.8Ca0.2CrO3 Interconnect Materials for Solid Oxide Fuel Cells: Combustion Synthesis and Reduced-Temperature Sintering

  • Park, Beom-Kyeong;Lee, Jong-Won;Lee, Seung-Bok;Lim, Tak-Hyoung;Park, Seok-Joo;Song, Rak-Hyun;Shin, Dong-Ryul
    • Journal of Electrochemical Science and Technology
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    • v.2 no.1
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    • pp.39-44
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    • 2011
  • Sub-micrometer $La_{0.8}Ca_{0.2}CrO_3$ powders for ceramic interconnects of solid oxide fuel cells were synthesized by the aqueous combustion process. The materials were prepared from the precursor solutions with different glycine (fuel)-to-nitrate (oxidant) ratios (${\phi}$). Single-phase $La_{0.8}Ca_{0.2}CrO_3$ powders with a perovskite structure were obtained after combustion when ${\phi}$ was equal to or larger than 0.480. Especially, the stoichiometric precursor with ${\phi}$ = 0.555 yielded the spherical $La_{0.8}Ca_{0.2}CrO_3$ particles with 150-250 nm diameters after calcination at $1000^{\circ}C$. When compared with the powders synthesized by the solid-state reaction, the combustion-derived, fine powders exhibited improved sinterability, leading to near-full densification at $1400^{\circ}C$ in oxidizing atmospheres. Moreover, a small quantity of glass additives was used to reduce the sintering temperature, and considerable densification was indeed achieved at temperatures as low as $1100^{\circ}C$.

One step facile synthesis of Au nanoparticle-cyclized polyacrylonitrile composite films and their use in organic nano-floating gate memory applications

  • Jang, Seok-Jae;Jo, Se-Bin;Jo, Hae-Na;Lee, Sang-A;Bae, Su-Gang;Lee, Sang-Hyeon;Hwang, Jun-Yeon;Jo, Han-Ik;Wang, Geon-Uk;Kim, Tae-Uk
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.307.2-307.2
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    • 2016
  • In this study, we synthesized Au nanoparticles (AuNPs) in polyacrylonitrile (PAN) thin films using a simple annealing process in the solid phase. The synthetic conditions were systematically controlled and optimized by varying the concentration of the Au salt solution and the annealing temperature. X-ray photoelectron spectroscopy (XPS) confirmed their chemical state, and transmission electron microscopy (TEM) verified the successful synthesis, size, and density of AuNPs. Au nanoparticles were generated from the thermal decomposition of the Au salt and stabilized during the cyclization of the PAN matrix. For actual device applications, previous synthetic techniques have required the synthesis of AuNPs in a liquid phase and an additional process to form the thin film layer, such as spin-coating, dip-coating, Langmuir-Blodgett, or high vacuum deposition. In contrast, our one-step synthesis could produce gold nanoparticles from the Au salt contained in a solid matrix with an easy heat treatment. The PAN:AuNPs composite was used as the charge trap layer of an organic nano-floating gate memory (ONFGM). The memory devices exhibited a high on/off ratio (over $10^6$), large hysteresis windows (76.7 V), and a stable endurance performance (>3000 cycles), indicating that our stabilized PAN:AuNPs composite film is a potential charge trap medium for next generation organic nano-floating gate memory transistors.

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Synthesis of Ultrafine LaAlO$_3$ Powders with Good Sinterability by Self-Sustaining Combustion Method Using (Glycine+Urea) Fuel ((Glycine+Urea) 혼합연료를 이요한 자발착화 연소반응법에 의한 우수한 소결성의 초미분체 LaAlO$_3$ 분말 합성)

  • Nam, H.D.;Choi, W.S.;Lee, B.H.;Park, S.
    • Journal of the Korean Ceramic Society
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    • v.36 no.2
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    • pp.203-209
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    • 1999
  • LaAlO3d single phase used as the butter layer on Si wafer for YBa2Cu3O7-$\delta$ superconductor application were prepared by solid state reaction method and by self-sustaining combustion process. The microstructure and crystallity of synthesiszed LaAlO3 powder studied using scanning electron microscope (SEM) and X-ray diffractometer(XRD), specific surface area and sintering characteristics fo powder were investigated by Brunauer-Emmett-Teller (BET) method and dilatometer respectively. In solid state reaction method, it is difficult to obtain LaAlO3 single phase up to 150$0^{\circ}C$ period. However, in self-sustaining combustion process, it is to easy to do it only $650^{\circ}C$. Based on the results of analysis of dilatometer it is easier to obtain high sintering density (98.87%) in self-sustaining combustion process than in the solid state reaction method. This reason is that the average particle size prepared by self-sustaining combustion process is nano crystal size and has high specific surface are value(56.54 $m^2$/g) compared with that by solid state reaction method. Also, LaAlO3 layer on the Si wafer has been achieved by screen printing and sintering method. Even though the sintering temperature is 130$0^{\circ}C$, the phenomena of silicon out diffusion in LaAlO3/Si interphase are not observed.

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Synthesis of akermanite bioceramics by solid-state reaction and evaluation of its bioactivity (고상반응법에 의한 아커마나이트 분말의 합성 및 생체활성도 평가)

  • Go, Jaeeun;Lee, Jong Kook
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.32 no.5
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    • pp.191-198
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    • 2022
  • Zirconia and titanium alloys, which are mainly used for dental implant materials, have poor osseointegration and osteogenesis abilities due to their bioinertness with low bioactivity on surface. In order to improve their surface bioinertness, surface modification with a bioactive material is an easy and simple method. In this study, akermanite (Ca2MgSi2O7), a silicate-based bioceramic material with excellent bone bonding ability, was synthesized by a solid-state reaction and investigated its bioactivity from the analysis of surface dissolution and precipitation of hydroxyapatite particles in SBF solution. Calcium carbonate (CaCO3), magnesium carbonate (MgCO3), and silicon dioxide (SiO2) were used as starting materials. After homogeneous mixing of starting materials by ball milling and the drying of at oven, uniaxial pressing was performed to form a compacted disk, and then heat-treated at high temperature to induce the solid-state reaction to akermanite. Bioactivity of synthesized akermanite disk was evaluated with the reaction temperature from the immersion test in SBF solution. The higher the reaction temperature, the more pronounced the akermanite phase and the less the surface dissolution at particle surface. It resulted that synthesized akermanite particles had high bioactivity on particle surface, but it depended on reacted temperature and phase composition. Moderate dissolution occurred at particle surfaces and observed the new precipitated hydroxyapatite particles in synthetic akermanite with solid-state reaction at 1100℃.

Novel solvothermal approach to hydrophilic nanoparticles of late transition elements and its evaluation by nanoparticle tracking analysis

  • Dutilleul, Marion Collart;Seisenbaeva, Gulaim A.;Kessler, Vadim G.
    • Advances in nano research
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    • v.2 no.2
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    • pp.77-88
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    • 2014
  • Solvothermal treatment of late transition metal acetylacetonates in a novel medium composed either of pure acetophenone or acetophenone mixtures with amino alcohols offers a general approach to uniform hydrophilic metal nanoparticles with high crystallinity and low degree of aggregation. Both pure metal and mixed-metal particles can be accesses by this approach. The produced materials have been characterized by SEM-EDS, TEM, FTIR in the solid state and by Nanoparticle Tracking Analysis in solutions. The chemical mechanisms of the reactions producing nanoparticles has been followed by NMR. Carrying out the process in pure acetophenone produces palladium metal, copper metal with minor impurity of $Cu_2O$, and NiO. The synthesis starting from the mixtures of Pd and Ni acetylacetonates with up to 20 mol% of Pd, renders in minor yield the palladium-based metal alloy along with nickel oxide as the major phase. Even the synthesis starting from a mixed solution of $Cu(acac)_2$ and $Ni(acac)_2$ produces oxides as major products. The situation is improved when aminoalcohols such as 2-aminoethanol or 2-dimethylamino propanol are added to the synthesis medium. The particles in this case contain metallic elements and pairs of individual metals (not metal alloys) when produced from mixed precursor solutions in this case.

Synthesis of BaSrSiO4 Phosphors by Solid State Reaction and Its Luminescent Properties (고상법에 의한 BaSrSiO4 형광체의 분말합성 및 발광특성)

  • Kang, Joo Young;Won, Hyeong Il;Hayk, Nersisyan;Won, Chang Whan
    • Korean Journal of Materials Research
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    • v.23 no.12
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    • pp.727-731
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    • 2013
  • In this study, green barium strontium silicate phosphor ($BaSrSiO_4:Eu^{3+}$, $Eu^{2+}$) was synthesized using a solid-state reaction method in air and reducing atmosphere. Investigation of the firing temperature indicates that a single phase of $BaSrSiO_4$ is formed when the firing temperature is higher than $1400^{\circ}C$. The effect of firing temperature and doping concentration on luminescent properties are investigated. The light-emitting property was the best when the molar content of $Eu_2O_3$ was 0.025 mol. Also, the luminescent brightness of the $BaSrSiO_4$ fluorescent substance was the best when the particle size of the barium was $0.5{\mu}m$. $BaSrSiO_4$ phosphors exhibit the typical green luminescent properties of $Eu^{3+}$ and $Eu^{2+}$. The characteristics of the synthesized $BaSrSiO_4:Eu^{3+}$, $Eu^{2+}$ phosphor were investigated using X-ray diffraction (XRD) and scanning electron microscopy. The maximum emission band of the $BaSrSiO_4:Eu^{3+}$, $Eu^{2+}$ was 520 nm.

Synthesis and Characterization of Substituted Pyridine Complexes of Molybdenum (II). Substituted Pyridinium Salts of Oxopentachloromolybdates (V) (몰리브덴의 피리딘계 착물합성과 그 성질 (제2보). 옥소오클로로몰리브덴 (V) 의 치환피리딘늄염)

  • Sang Oh Oh;Chang Su Kim
    • Journal of the Korean Chemical Society
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    • v.25 no.4
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    • pp.263-269
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    • 1981
  • The substituted pyridinium salts of oxochloromolybdates(V) have been prepared characterized by visible and infrared spectra, and magnetic moments. The electrical conductance of aqueous solutions of substituted pyridinium salts have been measured over a range of concentrations. The results indicate that the complex anions are monomeric in the solid. The magnetic moments of the complexes are similar to the spin-only values. Substituted pyridines are present as pyridinium cation in solid state.

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