• 한국세라믹학회지
• /
• 제48권5호
• /
• pp.379-383
• /
• 2011

This paper presents the synthesis of one-dimensional spinel $LiMn_2O_4$ nanostructures using a facile and scalable two-step process. $LiMn_2O_4$ nanorods with average diameter of 100 nm and length of 1.5 ${\mu}m$ have been prepared by solid-state lithiation of hydrothermally synthesized ${\beta}$-$MnO_2$ nanorods. $LiMn_2O_4$ nanowires with diameter of 10 nm and length of several micrometers have been fabricated via solid-state lithiation of ${\beta}$-$MnO_2$ nanowires. The precursors have been lithiated with LiOH and reaction temperature and pressure have been controlled. The complete structural transformation to cubic phase and the maintenance of 1-D nanostructure morphology have been evaluated by XRD, SEM, and TEM analysis. The size distribution of the spinel $LiMn_2O_4$ nanorods/wires has been similar to the $MnO_2$ precursors. By control of reaction pressure, cubic 1-D spinel $LiMn_2O_4$ nanostructures have been fabricated from tetragonal $MnO_2$ precursors even below $500^{\circ}C$.

• 한국세라믹학회지
• /
• 제35권8호
• /
• pp.843-849
• /
• 1998

Fine powders of Mn-Zn ferrite were prepared by the alcoholic dehydration method and densification beha-vior of synthesized powder was investigated. The concentration and pH of solution for optimal precipitation was 0.4M and 2.5 respectively. The spinel single phase metastable state was formed by thermal decom-position of precipitate and then spinel phase was disintegrated into hematite and spinel {{{{ { { ZnFe}_{2 }O }_{4 } }} at 600$^{\circ}C$ With increase of temperature reaction of solid solution between hematite and spinel was proceeded and resulted in the spinel single phase (Mn, Zn Fe){{{{ { {Fe }_{2 }O }_{4 } }} On account of high reactivity of uncalcined powders densification started at 200$^{\circ}C$ lower and completed at 50$^{\circ}C$ lower in comparison with calcined powders.

• Journal of Electrochemical Science and Technology
• /
• 제2권1호
• /
• pp.39-44
• /
• 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 $1100^{\circ}C$.

• 한국세라믹학회지
• /
• 제49권2호
• /
• pp.197-203
• /
• 2012

In this study, in order to improve densification of $La_{0.8}Ca_{0.2}Cr_{0.9}Co_{0.1}O_{3-\delta}$ (LCCC), which is known for one of the most proper candidate interconnector materials in the solid oxide fuel cells, $CaCrO_4$ was prepared via solid oxide synthesis route and added to the LCCC with different amount and particle sizes. As the amount of the $CaCrO_4$ increased, porosity of the sintered samples increased, and the pore size was proportional to the particle size of the $CaCrO_4$. This supports the fact that the $CaCrO_4$ phase forms liquid during sintering and permeate into the matrix leaving behind large pores. Then the liquid reacts with the matrix through the solid solution. However, when the samples were sintered with a slow ramp up rates, the porosity decreased. This is thought to be caused by the progressive solid solution of $CaCrO_4$ before the temperature reach to the melting temperature and forms a fluent amount of liquids. The sintering behavior of the LCCC with the addition of $CaCrO_4$ was analyzed through the transient liquid phase sintering on the basis of the microstructure observation and phase identification by x-ray diffraction.

• 한국전기전자재료학회:학술대회논문집
• /
• 한국전기전자재료학회 2005년도 하계학술대회 논문집 Vol.6
• /
• pp.270-271
• /
• 2005

A high Tc superconducting with a nominal composition of $Bi_2Sr_2Ca_2Cu_3O_Y$ was prepared by the citarte method. The solid precursor produced by the dehydration of the gel at $120^{\circ}C$ for 12h is not in the amorphous state as expected but in a crystalline state. X-ray diffraction peaks of nearly the same angular position as the peaks of high Tc phase were observed in the precursor. After pyrolysis at $400^{\circ}C$ and calcination at $840^{\circ}C$ for 4h, the (001)peak of the high Tc phase was cleary observed. Experimental results suggest that the intermediate phase formed before the formation of the superconducting phase may be the most important factro in determining whether it is easy to form the high Tc phase or not. because the nucleation barriers of the two superconducting phase may be altered by the variation of the crystal structures of those intermediate phase.

• 한국재료학회지
• /
• 제22권9호
• /
• pp.470-475
• /
• 2012

$La_{1-x}Sr_xMnO_3$(LSM,$0{\leq}x{\leq}0.5$) powders as the air electrode for solid oxide fuel cell were synthesized by a glycine-nitrate combustion process. The powders were then examined by X-ray diffraction(XRD) and scanning electron microscopy (SEM). The as-formed powders were composed of very fine ash particles linked together in chains. X-ray maps of the LSM powders milled for 1.5 h showed that the metallic elements are homogeneously distributed inside each grain and in the different grains. The powder XRD patterns of the LSM with x < 0.3 showed a rhombohedral phase; the phase changes to the cubic phase at higher compositions($x{\geq}0.3$) calcined in air at $1200^{\circ}C$ for 4 h. Also, the SEM micrographs showed that the average grain size decreases as Sr content increases. Composite air electrodes made of 50/50 vol% of the resulting LSM powders and yttria stabilized zirconia(YSZ) powders were prepared by colloidal deposition technique. The electrodes were studied by ac impedance spectroscopy in order to improve the performance of a solid oxide fuel cell(SOFC). Reproducible impedance spectra were confirmed using the improved cell, which consisted of LSM-YSZ/YSZ. The composite electrode of LSM and YSZ was found to yield a lower cathodic resistivity than that of the non-composite one. Also, the addition of YSZ to the $La_{1-x}Sr_xMnO_3$ ($0.1{\leq}x{\leq}0.2$) electrode led to a pronounced, large decrease in the cathodic resistivity of the LSM-YSZ composite electrodes.

• 한국분말재료학회지
• /
• 제11권1호
• /
• pp.28-33
• /
• 2004

In the present study, the focus is on the analysis of carbothermal reduction of the titanium-cobalt-oxygen based oxide powder by solid carbon for the optimizing synthesis process of ultra fined TiC/Co composite powder. The titanium-cobalt-oxygen based oxide powder was prepared by the combination of the spray drying and desalting processes using the titanium dioxide powder and cobalt nitrate as the raw materials. The titanium-cobalt-oxygen based oxide powder was mixed with carbon black, and then this mixture was carbothermally reduced under a flowing argon atmosphere. The changes in the phase structure and thermal gravity of the mixture during carbothermal reduction were analysed using XRD and TGA. The synthesized titanium-cobalt-oxygen based oxide powder has a mixture of $TiO_2$ and $CoTiO_3$. This oxide powder was transformed to a mixed state of titanium car-bide and cobalt by solid carbon through four steps of carbothermal reduction steps with increasing temperature; reduction of $CoTiO_3$ to $TiO_2$ and Co, reduction of $TiO_2$, to the magneli phase($Ti_nO_{2n-1}$, n>3), reduction of the mag-neli phase($Ti_nO_{2n-1}$, n>3) to the $Ti_nO_{2n-1}$(2$\leq$n$\leq$3) phases, and reduction and carburization of the $Ti_nO_{2n-1}$(2$\leq$n$\leq$3) phases to titanium carbide.

• 대한방사성의약품학회지
• /
• 제2권2호
• /
• pp.103-107
• /
• 2016

Solid phase extraction (SPE) purification method is the efficient and well-known tool for automated [$^{11}C$]acetate synthesis. A fully automated homemade module adopting the SPE method and 'pinch' valves was developed very economically with a universal interface board, a relay card and an open source programmable logic controller. The radiochemical yield of the optimized [$^{11}C$]acetate synthesis by this system was $58.8{\pm}2.1%$ (n=10, decay-corrected) from $15.5{\pm}0.19GBq$ of $[^{11}C]CO_2$ as starting activity, and total synthetic time was 15 minutes. HPLC analysis showed its high radiochemical purity as $97.4{\pm}1.1%$ without possible by-products.

• Advances in nano research
• /
• 제2권2호
• /
• pp.77-88
• /
• 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.

• 한국분말재료학회지
• /
• 제29권1호
• /
• pp.34-40
• /
• 2022

Recently, high-entropy carbides have attracted considerable attention owing to their excellent physical and chemical properties such as high hardness, fracture toughness, and conductivity. However, as an emerging class of novel materials, the synthesis methods, performance, and applications of high-entropy carbides have ample scope for further development. In this study, equiatomic (Hf-Ti-Ta-Zr-Nb)C high-entropy carbide powders have been prepared by an ultrahigh-energy ball-milling (UHEBM) process with different milling times (1, 5, 15, 30, and 60 min). Further, their refinement behavior and high-entropy synthesis potential have been investigated. With an increase in the milling time, the particle size rapidly reduces (under sub-micrometer size) and homogeneous mixing of the prepared powder is observed. The distortions in the crystal lattice, which occur as a result of the refinement process and the multicomponent effect, are found to improve the sintering, thereby notably enhancing the formation of a single-phase solid solution (high-entropy). Herein, we present a procedure for the bulk synthesis of highly pure, dense, and uniform FCC single-phase (Fm3m crystal structure) (Hf-Ti-Ta-Zr-Nb)C high-entropy carbide using a milling time of 60 min and a sintering temperature of 1,600℃.