• Journal of the Korean Ceramic Society
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• v.31 no.8
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• pp.893-901
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• 1994

In this study, AlN powder of fine particle size and of high purity was synthesized by the carbothermal reduction-nitridation of monodisperse, spherical Al(OH)3 which had been prepared by sol-gel method using Al(O-sec-C4H9)3 as the starting material. Depending on the mixing order and kinds of reducing agents, the optimum condition for the preparation of AlN was determined as follows. AlN single-phase was produced by the carbothermal reduction-nitridation of (1) Benzene-washed Al(OH)3 and the reducing agent, carbon, which was mixed in a ball mill: for 5 hours at 140$0^{\circ}C$ under NH3 atmosphere; (2) The mixture prepared by hydrolysis of alkoxide solution into which carbon had been dispersed beforehand: for 5 hours at 135$0^{\circ}C$ ; (3) Al(OH)3 Poly(furfuryl alcohol) composite powder: for 2.5 hours at 135$0^{\circ}C$; (4) The mixture of Al(OH)3 and polyacrylonitrile: for 5 hours at 140$0^{\circ}C$. Addition of CaF2 increased the nitridation rate when carbon or polyacrylonitrile was used as the reducing agent; but it had no effect on the nitridation rate when furfuryl alcohol was used as the reducing agent.

• Journal of Powder Materials
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• v.18 no.5
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• pp.449-455
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• 2011

In this study, p-type $(AgSbTe_2)_{15}(GeTe)_{85}$: TAGS-85 compound powders were prepared by gas atomization process, and then their microstructures and mechanical properties were investigated. The fabricated powders were of spherical shape, had clean surface, and illustrated fine microstructure and homogeneous $AgSbTe_2$ + GeTe solid solution. Powder X-ray diffraction results revealed that the crystal structure of the TAGS-85 sample was single rhombohedral GeTe phase, which with a space group $R_{3m}$. The grain size of the powder particles increased while the micro Vickers hardness decreased with increasing annealing temperature within the range of 573 K and 723 K due to grain growth and loss of Te. In addition, the crystal structure of the powder went through a phase transformation from rhombohedral ($R_{3m}$) at low-temperature to cubic ($F_{m-3m}$) at high-temperature with increasing annealing temperature. The micro Vickers hardness of the as-atomized powder was around 165 Hv, while it decreased gradually to 130 Hv after annealing at 673K, which is still higher than most other fabrication processes.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.4 no.2
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• pp.178-189
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• 1994

Fine $BaTiO_3$ powder was synthesized from the various starting solution with 0.05 M by ultrasonic spray pyrolysis method. The conditions of synthesis were fixed on flow rate was 0.5 cm/sec, low temperature furnace was $300^{\circ}C$, and high temperatures furnace was $700^{\circ}C$. The formation procedure was investigated directly by SEM with the collected particle from the each reaction step. Also, the trace of particle in reaction tube was researched theoretically. Fine $BaTiO_3$ was synthesized only in the case of nitrate aqueous solution. The synthesized $BaTiO_3$ powder was porous and spherical which was consist of primary particle at the size of 19.1 nm. The formation procedure was as follows : the particle size decreased in drying step and then increased in initial thermal decomposition step. Finally, particle size was decreased to $0.42 {mu}m$. The trace of particle in reaction tube was also theoretically simulated and discussed.

• Korean Journal of Materials Research
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• v.25 no.11
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• pp.602-606
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• 2015

Porous W with spherical and directionally aligned pores was fabricated by the combination of sacrificial fugitives and a freeze-drying process. Camphene slurries with powder mixtures of $WO_3$ and spherical PMMA of 20 vol% were frozen at $-25^{\circ}C$ and dried for the sublimation of the camphene. The green bodies were heat-treated at $400^{\circ}C$ for 2 h to decompose the PMMA; then, sintering was carried out at $1200^{\circ}C$ in a hydrogen atmosphere for 2 h. TGA and XRD analysis showed that the PMMA decomposed at about $400^{\circ}C$, and $WO_3$ was reduced to metallic W at $800^{\circ}C$ without any reaction phases. The sintered bodies with $WO_3$-PMMA contents of 15 and 20 vol% showed large pores with aligned direction and small pores in the internal walls of the large pores. The pore formation was discussed in terms of the solidication behavior of liquid camphene with solid particles. Spherical pores, formed by decomposition of PMMA, were observed in the sintered specimens. Also, microstructural observation revealed that struts between the small pores consisted of very fine particles with size of about 300 nm.

• Journal of the Korean Ceramic Society
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• v.43 no.10 s.293
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• pp.666-672
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• 2006

GDC20($Ce_{0.8}Gd_{0.2}O_{1.9}$) powder was synthesized by oxalate co-precipitation and milling and its thermal decomposition, phase formation, and sinterability were investigated. As-prepared precipitates were non-crystalline due to the milling process and completely decomposed at 400$^{\circ}C$ The powder calcined at 800$^{\circ}C$ for 2 h contained fine p]sty particles with an average size of 0.69 $\mu$m. Attrition milling of the calcined powder for 2 h had a little milling effect, resulting in a slight decrease in the particle size to 0.45 $\mu$m. The milled powder consisted of small spherical primary particles and some large particles, which had been agglomerated during calcination. Due to the excellent sinterability of the powder, sintering of the powder compacts for 4 h showed relative densities of 78.7% at 1000$^{\circ}C$ and 97.8% at 1300$^{\circ}C$, respectively. Densification was found to almost complete at temperature above 1200$^{\circ}C$ and a dense and homogeneous microstructure was obtained. A rapid grain growth occurred between 1200$^{\circ}C$ and 1300$^{\circ}C$. Grains in 0.1$\sim$0.5 $\mu$m sizes at 1200$^{\circ}C$ grew to 0.2$\sim$2 $\mu$m and their size distribution became broader at 1300$^{\circ}C$.

• Journal of the Korean Ceramic Society
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• v.30 no.4
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• pp.325-331
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• 1993

Aqueous solutions of metallic salts, ZrO(NO3)2.2H2O and Y(NO3)3.5H2O were used as raw materials to synthesize crystalline submicron spherical powders of Zr0.94Y0.06O1.97 with tetragonal crystal phase. Each aqueous solution was mixed on the magnetic stirrer to homogenize for 12 hours. The concentration of the mixed solutionwas changed from 0.01mol/$\ell$ to 0.1mol/$\ell$ calculated as the concentration of Zr0.94Y0.06O1.97. Ultrafine droplets of starting mixed solution were sprayed by the ultrasonic vibrator and carried into the furnace kept at 55$0^{\circ}C$, $650^{\circ}C$, 75$0^{\circ}C$ and 85$0^{\circ}C$ using carrier gas of air (10$\ell$/min) and pyrolysed to form Y-TZP fine powders. The results of this exeriment were as follows. 1) Synthesized powders were nonagglomerated and spherical type. 2) Particle size distribution was narrow between 0.1${\mu}{\textrm}{m}$ and 1${\mu}{\textrm}{m}$. 3) Forming reaction Y-TZP was finished above synthetic temperature 75$0^{\circ}C$. 4) As the synthetic temperature rised from 55$0^{\circ}C$ to 85$0^{\circ}C$, the mean particle size decreased from 0.35${\mu}{\textrm}{m}$ to 0.22${\mu}{\textrm}{m}$ in the concentration of starting solution with 0.02mol/$\ell$. 5) At 75$0^{\circ}C$ of synthetic temperature, the concentration changes of starting solution from 0.01mol/$\ell$ to 0.1mol/$\ell$ increased the mean particle size from 0.24${\mu}{\textrm}{m}$ to 0.38${\mu}{\textrm}{m}$. 6) Chemical compositions of each synthesized particle were homogeneous nearly.

• Resources Recycling
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• v.27 no.6
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• pp.44-52
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• 2018

In this study, copper was recovered from copper containing sludge by selectively controlling electro-refining process conditions in copper sulfate electrolyte solution. Electro-refining process was performed by LSV (Linear Sweep Voltammetry) result according to copper sulfate electrolyte solution concentration, applied current density, additive type and concentration. SEM (Scanning Electron Microscope) and PSA (Particle Size Analyzer) were used to analyze the shape and size of copper powder. In the 0.1 ~ 0.4 M copper sulfate electrolyte solution without organic additives, the copper powder size decreased as the applied current density became closer to the limiting current density and the copper powder size tended to decrease in 0.2 ~ 0.3 M copper sulfate electrolyte solution. In addition, when the shape and size of the copper powder were analyzed by adding various types and concentrations of organic additives to the previous experimental, fine spherical copper powder having the smallest size (nm) was obtained under the condition of cellulose type additive 2,000 ppm.

• Resources Recycling
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• v.9 no.4
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• pp.16-27
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• 2000

In order to produce raw material powder of advanced magnetic material by spray roasting process, newly modified spray roasting system was developed in this work. In this spray roasting system, raw material solution was effectively atomized and sprayed into the reaction furnace. Also, uniform temperature distribution inside reaction furnace made thermal decomposition process fully completed, and produced powder was effectively collected in cyclone and bag filter. This system equipped with apparatus which can purify hazard produced gas. In this study complex acid solution was prepared by dissolution of mill scale and ferro-Mn into the acid solution, and the pH of this complex acid solution was controlled about to 4. It was conformed that mill scale and ferro-Mn containing a lot of impurities such as $SiO_2$, P and Al could be used as raw material by reducing the impurities content of complex acid solution below 20 ppm. Complex oxide powder of Fe-Mn system was produced by spraying purified complex acid solution into the spray roaster through nozzle, and the variations of produced powder characters were studied by changing he reaction conditions such as reaction temperature, the injection velocity of solution and air, nozzle tip size and concentration of solution. The morphology of produced powder had spherical shape under the most experimental conditions, and concentration of solution. The morphology of produced powder has spherical shape under the most experimental conditions, and the composition and the particle size distribution were almost uniform, which tells the excellence of this spray roasting system. The grain size of most produced powder was below 100 nm. From the above results, it will be possible to produce ultra fine oxide powder from the chloride of Fe, Mn, Ni, Cu and rare earth by using this spray roasting system, and also to produce ultra fine pure metal powder by changing reaction atmosphere.

• Journal of Powder Materials
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• v.13 no.6 s.59
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• pp.396-400
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• 2006

The Ti-Ni alloy nanopowders were synthesized by a levitational gas condensation (LGC) by using a micron powder feeding system and their particulate properties were investigated by x-ray diffraction (XRD), transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) method. The starting Ti and Ni micron powders $150{\mu}m$ were incorporated into the micron powder feeding system. An ingot type of the Ti-Ni ahoy was used as a seed material for the levitation and evaporation reactions. The collected powders were finally passivated by oxidation. The x-ray diffraction experiments have shown that the synthesized powders were completely alloyed with Ti and Ni and comprised of two different cubic and monoclinic crystalline phases. The TEM results showed that the produced powders were very fine and uniform with a spherical particle size of 18 to 32nm. The typical thickness of a passivated oxide layer on the particle surface was about 2 to 3 nm. The specific surface area of the Ti-Ni alloy nanopowders was $60m^2/g$ based on BET method.

• Journal of the Korean Ceramic Society
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• v.34 no.10
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• pp.1083-1091
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• 1997

As one of the chemical powder fabrication methods, the powder preparation method by using oxalate has the following advantages; (1) easy to control the chemical stoichiometry, (2) easy to fabricate homogeneous and fine particles, and (3) easy to be thermaly decomposed at low temperature. In the present study, the initial morphology and size distribution of the powder were controlled and the homogeniaty was improved. By carefully controlling the pH with NH4OH, the Bi(Pb)-Sr-Ca-Cu-O superconducting powders were prepared and investigated for their properties. The microstructures and the superconducting properties of the pelletized samples were investigated. Also, the microstructures and electrical properties of the samples prepared by tape casting method were investigated. The fabricated powders were spherical with less than 400 nm, but most of them were agglomerated to be 1~3 ${\mu}{\textrm}{m}$ in size. The critical temperature of the pelletized sample annealed at 84$0^{\circ}C$ for 72 hours in air was 110K. And the critical currents of annealed samples in air prepared by tape casting process for 24 hours and 72 hours were 0.6 A (Jc=600A/$\textrm{cm}^2$) and 1.9A (Jc=1, 900A/$\textrm{cm}^2$) respectively.