• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.7 no.3
• /
• pp.428-436
• /
• 1997

Hexacelsian ($BaO{\cdot}Al_2O_3{\cdot}2SiO_2$) powder was prepared by a solution-polymerization route employing PVA solution as a polymeric carrier. A fine amorphous-type hexacelsian powder with an average particle size of 0.8 $\mu \textrm{m}$ and a BET specific surface area of $63 \textrm{m}^2$/g was made by a ball-milling the powder precursor for 12 h after calcination at $800^{\circ}C$ for :1 h. A densified hexacelsian was obtained through sintering at $1550^{\circ}C$ for 2 h under an air atmosphere. The $\alpha\longleftrightarrow\beta$ and $\beta\longleftrightarrow\gamma$ displacive phase transformation in polycrystalline hexacelsia,n was examined by using dilatometry and differential scanning calorimtry. The reconstructive transformation between hexacelsian and celsian was obtained by annealing at $1600^{\circ}C$ for 72h. Volume contraction of 5.6% was accompanied by the reconstructive transformation.

• Korean Journal of Materials Research
• /
• v.12 no.10
• /
• pp.784-790
• /
• 2002

For mass product of nanocrystalline ZnO ultrafine powders, self-sustaining combustion process(SCP) and ultrasonic spray combustion method(USCM) were applied at the same time. Ultrasonic spray gun was attached on top of the vertical type furnace. The droplet was sprayed into reaction zone of the furnace to form SCP which produces spherical shape with soft agglomerate crystalline ZnO particles. To characterize formed particles, fuel and oxidizing agent for SCP were used glycine and zinc nitrate or zinc hydroxide. Respectively, with changing combustion temperature and mixture ratio of oxidizing agent and fuel, the best ultrasonic spray conditions were obtained. To observe ultrasonic spray effect, two types of powder synthesis processes were compared. One was directly sprayed into furnace from the precursor solution (Type A), the other directly was heated on the hot plate without using spray gun (Type B). Powder obtained by type A was porous sponge shape with heavy agglomeration, but powder obtained using type B was finer primary particle size, spherical shape with weak agglomeration and bigger value of specific surface area. 9/ This can be due to much lower reaction temperature of type B at ignition time than type A. Synthesized nanocrystalline ZnO powders at the best ultrasonic spray conditions have primary particle size in range 20~30nm and specific surface area is about 20m$^2$/g.

• Proceedings of the Korean Powder Metallurgy Institute Conference
• /
• 1996.11a
• /
• pp.6-6
• /
• 1996

Ceramic based nanocomposite, in which nano-sized ceramics and metals were dispersed within matrix grains and/or at grain boundaries, were successfully fabricated in the ceramic/cerarnic and ceramic/metal composite systems such as $Al_2O_3$/SiC, $Al_2O_3$/$Si_3N_4$, MgO/SiC, mullite/SiC, $Si_3N_4/SiC, $Si_3N_4$/B, $Al_2O_3$/W, $Al_2O_3$/Mo, $Al_2O_3$/Ni and $ZrO_2$/Mo systems. In these systems, the ceramiclceramic composites were fabricated from homogeneously mixed powders, powders with thin coatings of the second phases and amorphous precursor composite powders by usual powder metallurgical methods. The ceramiclmetal nanocomposites were prepared by combination of H2 reduction of metal oxides in the early stage of sinterings and usual powder metallurgical processes. The transmission electron microscopic observation for the $Al_2O_3$/SiC nanocomposite indicated that the second phases less than 70nm were mainly located within matrix grains and the larger particles were dispersed at the grain boundaries. The similar observation was also identified for other cerarnic/ceramic and ceramiclmetal nanocornposites. The striking findings in these nanocomposites were that mechanical properties were significantly improved by the nano-sized dispersion from 5 to 10 vol% even at high temperatures. For example, the improvement in hcture strength by 2 to 5 times and in creep resistance by 2 to 4 orders was observed not only for the ceramidceramic nanocomposites but also for the ceramiclmetal nanocomposites with only 5~01%se cond phase. The newly developed silicon nitride/boron nitride nanocomposites, in which nano-sized hexagonal BN particulates with low Young's modulus and fracture strength were dispersed mainly within matrix grains, gave also the strong improvement in fracture strength and thermal shock fracture resistance. In presentation, the process-rnicro/nanostructure-properties relationship will be presented in detail. The special emphasis will be placed on the understanding of the roles of nano-sized dispersions on mechanical properties.

• Journal of Powder Materials
• /
• v.23 no.4
• /
• pp.311-316
• /
• 2016

$Ni(OH)_2$ hollow spheres have been prepared by solvent displacement crystallization using a micro-injection device, and the effect of process parameters such as concentration and the relative ratio of the injection speed of the precursor solution, which is an aqueous solution of $NiSO_4{\cdot}6H_2O$, to isopropyl alcohol of displacement solvent have been investigated. The crystal phases after NaOH treatment are in the ${\beta}-phase$ for all process parameters. A higher concentration of $NiSO_4{\cdot}6H_2O$ aqueous solution is injected by a micro-injection device and bigger $Ni(OH)_2$ hollow spheres with a narrower particle size distribution are formed. The crystallinity and hardness of the as-obtained powder are so poor that hydrothermal treatment of the as-obtained $Ni(OH)_2$ at $120^{\circ}C$ for 24 h in distilled water is performed in order to greatly improve the crystallinity. It is thought that a relative ratio of the injection speed of $NiSO_4{\cdot}6H_2O$ to that of isopropyl alcohol of at least more than 1 is preferable to synthesize Ni(OH)2 hollow spheres. It is confirmed that this solution-based process is very effective in synthesizing ceramic hollow spheres by simple adjustment of the process parameters such as the concentration and the injection speed.

• Korean Journal of Materials Research
• /
• v.8 no.12
• /
• pp.1082-1089
• /
• 1998

To obtain fine dispersion of Ag particles in $YBa_2$$Cu_3$$O_{7-y}$ (123) superconductors, 123 samples were made by pyrophoric synthetic method using malic acid and the subsequent solid- state reaction. As the pyrophoric synthetic powder was used as a precursor material, fine 123 powder of submicron size was produced in a short reaction time. The added $Ag_2$O was converted to metallic Ag during Pyrophoric reaction and it accelerated both the formation of 123 phase and the grain growth via the enhanced mass transfer. The Ag particles of the sample sintered using the pyrephoric synthetic powder were more finely dispersed in the 123 matrix, compared to those of the sample sintered using the mechanically mixed powder, attributing to the improvement of the superconducting properties.

• Journal of Powder Materials
• /
• v.28 no.2
• /
• pp.143-149
• /
• 2021

In this study, (GaN)_1-x(ZnO)_x solid solution nanoparticles with a high zinc content are prepared by ultrasonic spray pyrolysis and subsequent nitridation. The structure and morphology of the samples are investigated by X-ray diffraction (XRD), field-emission scanning electron microscopy, and energy-dispersive X-ray spectroscopy. The characterization results show a phase transition from the Zn and Ga-based oxides (ZnO or ZnGa₂O₄) to a (GaN)_1-x(ZnO)_x solid solution under an NH3 atmosphere. The effect of the precursor solution concentration and nitridation temperature on the final products are systematically investigated to obtain (GaN)_1-x(ZnO)_x nanoparticles with a high Zn concentration. It is confirmed that the powder synthesized from the solution in which the ratio of Zn and Ga was set to 0.8:0.2, as the initial precursor composition was composed of about 0.8-mole fraction of Zn, similar to the initially set one, through nitriding treatment at 700℃. Besides, the synthesized nanoparticles exhibited the typical XRD pattern of (GaN)_1-x(ZnO)_x, and a strong absorption of visible light with a bandgap energy of approximately 2.78 eV, confirming their potential use as a hydrogen production photocatalyst.

• Korean Chemical Engineering Research
• /
• v.53 no.5
• /
• pp.597-602
• /
• 2015

Characteristics of continuous preparation of ZnO powder were investigated in a micro drop/bubble fluidized reactor of which diameter and height were 0.03 m and 1.5 m, respectively. The flow rate of carrier gas for transportation of precursors to the reactor was 6.0 L/min and the concentration of Zn ion in the precursor solutions was 0.4 mol/L, respectively. Effects of reaction temperature (973 K~1,273 K) and flow rate of micro bubbles (0~0.4 L/min) on the pore characteristics of prepared ZnO powder were examined. The optimum reaction temperature for the maximum porosity in the ZnO powder was 1,073 K within this experimental condition. The mean size of ZnO powder prepared continuously in the reactor decreased but the surface of the powder became smooth, with increasing reaction temperature. The injection of micro bubbles into the reactor could enhance the formation of pores in the powder effectively, and thus the mean BET surface area could be increased by up to 58%. The mean size of prepared ZnO powder was in the range of $1.25{\sim}1.75{\mu}m$ depending on the reaction temperature.

• Progress in Superconductivity and Cryogenics
• /
• v.18 no.4
• /
• pp.9-14
• /
• 2016

The effect of the size and shape of magnesium(Mg) powder on the formation of $MgB_2$ and the critical current density($J_{c,}$) of $MgB_2$ bulk was studied. As a precursor for the formation of $MgB_2$, Mg and $MgB_4$ powder, which was synthesized through the reaction of boron (B) with Mg powders, was used. $MgB_4$ was mixed with Mg powders of various sizes, pressed into pellets and heat-treated at $650^{\circ}C-750^{\circ}C$ in flowing argon gas. The XRD analysis of the heat-treated $MgB_2$ samples showed that the volume fraction of $MgB_2$ was the highest as 92.74 % when spherical Mg powder with an average size of $25.7{\mu}m$ was used, whereas the volume fraction was the lowest as 79.64 % when plate-like Mg powder with a size of $34.1{\mu}m$ was used. The superconducting transition temperature ($T_c$) of $MgB_2$ was not sensitive to the characteristics of the Mg powders used. All of the prepared $MgB_2$ samples showed a high $T_c$ of 38.3 K and a small superconducting transition width of 0.2 K-0.5 K. $J_c$ (5 K and 1 T) of $MgB_2$ was the highest as $3.93{\times}10^4A/cm^2$ when spherical Mg powder with a size of $25.7{\mu}m$ was used, whereas $J_c$ was the lowest as $2.18{\times}10^4A/cm^2$when plate-like Mg powder with a size of $34.1{\mu}m$ was used. The relationship between the $J_c$ of $MgB_2$ and the characteristics of the Mg powders used was explained in terms of the volume fraction of $MgB_2$ and the apparent density of the $MgB_2$ pellets.

• Transactions of the Korean hydrogen and new energy society
• /
• v.28 no.1
• /
• pp.70-76
• /
• 2017

To synthesize copper nanoparticle a thermal decomposition was adopted. And to solve the problem of surface oxidation of the synthesized copper powder an electroless Ag plating method was used. The size and shape of synthesized Cu nanoparticle were affected by the size of copper oxalate used as a precursor, reaction solvent, reaction temperature and amount of reducing agent. Especially reaction solvent is dominant factor to control shape of Cu nano-particle which can have the shapes of sphere, polygon and rod. In case of glycerol, it produced spherical shape of about 500 nm in size. Poly ethylene produced uniform polygonal shape in about 700 nm and ethylene glycol produced both of polygon and rod having size range between 500 and 1500 nm. The silver coated copper powder showed a high electrical conductivity.

• Journal of Powder Materials
• /
• v.27 no.2
• /
• pp.132-138
• /
• 2020

A facile one-pot wet chemical process to prepare pure anatase TiO₂ hollow structures using ammonium hexafluorotitanate as a precursor is developed. By defining the formic acid ratio, we fabricate TiO₂ hollow structures containing fluorine on the surface. The TiO₂ hollow sphere is composed of an anatase phase containing fluorine by various analytical techniques. A possible formation mechanism for the obtained hollow samples by self-transformation and Ostwald ripening is proposed. The TiO₂ hollow structures containing fluorine exhibits 1.2 - 2.7 times higher performance than their counterparts in photocatalytic activity. The enhanced photocatalytic activity of the TiO₂ hollow structures is attributed to the combined effects of high crystallinity, specific surface area (62 ㎡g^-1), and the advantage of surface fluorine ions (at 8%) having strong electron-withdrawing ability of the surface ≡ Ti-F groups reduces the recombination of photogenerated electrons and holes.