• 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.

• Bulletin of the Korean Chemical Society
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• v.24 no.5
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• pp.664-666
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• 2003

• 한국신재생에너지학회:학술대회논문집
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• 2009.06a
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• pp.134-137
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• 2009

Commercially available elemental powders of Cu, Zn, Sn and Se were employed for crystallizing a stannite-type $Cu_2ZnSnSe_4$ compound by means of solid state reaction. $Cu_2ZnSnSe_4$ reaction chemistry was also modeled based on differential-thermal analysis and X-ray powder diffraction results. It was observed that Se tends to react preferably with Cu to form CuSe and $CuSe_2$ phases at low reaction temperature. The formation of $Cu_5Zn_8$ intermetallic phase was found to be the intermediate reaction path for the binary ZnSe formation. A solid state reaction at $320^{\circ}C$ reacted elemental powderst obinary selenides of CuSe, ZnSe and SnSe completely. The crystallization of $Cu_2ZnSnSe_4$ was was detected to begin at $300^{\circ}C$ and its weight fraction increased with an increase of reaction temperature, which most probably formed from the reaction between $Cu_2SnSe_3$ and ZnSe.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.16 no.6
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• pp.256-259
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• 2006

The amorphous $SiO_x$ nanowires were synthesized by the vapor phase epitaxy (VPE) method. $SiO_x$ nanowires were formed on silicon wafer of temperatures ranged from $800{\sim}1100^{\circ}C$ and nickel thin film was used as a catalyst for the growth of nanowires. A vapor-liquid-solid (VLS) mechanism is responsible for the catalyst-assisted amorphous $SiO_x$ nanowires synthesis in this experiment. The SEM images showed cotton-like nanostructure of free standing $SiO_x$ nanowires with the length of more than about $10{\mu}m$. The $SiO_x$ nanowires were confirmed amorphous structure by TEM analysis and EDX spectrum reveals that the nanowires consist of Si and O.

• Bulletin of the Korean Chemical Society
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• v.35 no.8
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• pp.2381-2384
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• 2014

A solid-phase synthetic approach is reported for the synthesis of an ascorbic acid (ASA)-dipeptide conjugate that exhibited enhanced antioxidant activity. The N-terminal amino group of dipeptide (Ala-Ala) on a resin support was first activated by 1,1'-carbonyldiimidazole (CDI), and then reacted with an ASA derivative. The addition of a base, triethylamine (TEA), promoted nucleophilic acylation of ASA derivative and yielded a desired product (ASA-Ala-Ala) with enhanced purity, when cleaved from the resin. Compared to the approach where a C3 hydroxyl group of ASA was first activated with CDI and then reacted with the amino group of dipeptide on the resin, this new approach allowed a significant reduction of a total reaction time from 120 h to 8 h at $25^{\circ}C$. As-prepared ASA-dipeptide conjugate (ASA-Ala-Ala) showed improved antioxidant activity compared to ASA.

• Applied Biological Chemistry
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• v.34 no.4
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• pp.334-338
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• 1991

Synthesis of $(D-Phe^7\;-Leu^8)$ bradykinin and bradykinin by solid phase method using a new reaction vessel was carried out. Coupling was performed by dicyclohexylcarbodiimide. After cleavage with dried HBr the peptides were purified by high pressure liquied chromatography. Their purify was assayed by paper and thin layer chromatography, melting point and amino acid analysis. $(D-Phe^7\;-Leu^8)$ bradykinin and bradykinin were incubater in vitro endopeptidase $({\alpha}-chymotrysis)$ and exopeptidase(carboxypeptidase A, leucine aminopeptidase) in order to study the degradation pattern of peptides. $(D-Phe^7\;-Leu^8)$ bradykinin and bradykinin were rapidly degradated by ${\alpha}-chymotrypsin$ and carboxypeptidase A $(D-Phe^7\;-Leu^8)$ bradykinin and bradykinin coution$(D-Phe^7\;-Leu^8)$ bradykinin and bradykinin contain imino peptide bound from proline at N-terminal and therefore they were not attacted by leucine aminopeptidase.

• 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.

• Progress in Superconductivity and Cryogenics
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• v.25 no.4
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• pp.10-13
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• 2023

To confirm the room-temperature superconductivity at ambient pressure as claimed in recent arXiv preprints by Lee et al., we followed the original authors' systematic solid-state synthesis recipe to reproduce Cu-doped Pb-apatite, known as LK-99. Using X-ray diffraction and Raman spectroscopy, we identified inclusion of various impurities alongside the apatite phase in our sample. While the sample exhibited an overall semiconducting behavior in electrical transport, an intriguing resistivity anomaly at 380 K was observed, possibly originating from a structural phase transition of the Cu_2-δS impurity. Based on the transport and magnetization measurements, we conclude that the sample is a non-magnetic semiconductor, with absence of superconductivity.

• 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.

• Journal of the Korean Ceramic Society
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• v.23 no.1
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• pp.33-43
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• 1986

The synthesis of high-purity AlN by a vapor-phase reaction was investigated using the $NH_3-AlCl_3-H_2$ reacting system. The theoretical yields of AlN were determined from th thermodynamic equilibrium composi-tions. It was shown that the yields above 90% could by obtained even in the range of relatively low temper-ature of 600-1200K. The reaction temperature and the initial amounts/ratios of the reacting gases showed significant effects on the yields but the total pressure did not. The experimental results showed that a high-purity AlN having a needle shape was the only product as a solid phase and its amount produced increased with the reaction temperature. While the degree of agglmera-tion of the synthesized AlN increased with the reaction temperature the size of each particle consisting of the agglomerates was independent of the temperature but grew from 0.09 to 0.115${\mu}{\textrm}{m}$ with the flow rate of NH3. These experimental results were compared with the theoretical aspects for the synthesis of a high-purity AlN.