• Korean Journal of Fisheries and Aquatic Sciences
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• v.34 no.6
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• pp.600-604
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• 2001

For the effective utilization of cuttle bone as a calcium powder, we examined calcination condition ($700^{\circ}C: 0\sim10\;hrs,\;800^{\circ}C:\;0\sim3\;hrs,\;900^{\circ}C:\;0\sim1\;hr\;and\;1,000^{\circ}C:\;0\sim30\;mins$) for recovery of calcium from raw cuttle bone powder (RCB) and characteristics of calcined cuttle bone powder (CCB) treated by optimal condition. During calcination of RCB, the yields was decreased, while total and soluble calcium contents and white index were increased up to constant calcination time ($8\;hrs\;at\;700^{\circ}C,\;2\;hrs\;at\;800^{\circ}C,\;45\;min\;at\;900^{\circ}C\;and\;20\;min\;at\;1,000^{\circ}C$). But, these after that almost unchanged. From these results, the optimal calcination conditions for recovery of calcium from RCB were revealed $8\;hrs\;at\;700^{\circ}C,\;2\;hrs\;at\;800^{\circ}C,\;45\;min\;at\;900^{\circ}C\;and\;20\;min\;at\;1,000^{\circ}C$. In the case of CCB treated for 2 hrs at $800^{\circ}C$, total calcium was about $70\%$, the major component was calcium oxide, and the structure consisted of porosity. The calcium solubility of CCB increased by 22 times compared to RCB. But, the pH of RCB was about 12.9. Therefore, for the effective utilization of RCB as a calcium powder, it requires a suitable modification operation for adjustment of pH ($pH\;2.0\~9.0$).

• Korean Journal of Materials Research
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• v.4 no.8
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• pp.934-944
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• 1994

Effects of residual chloride on thermal decomposition behaviour of a-stannic acid and physical properties of $SnO_{2}$ powder were observed. The powder was fabricated by hydroxide method; $\alpha$-stannic acid was precipitated by mixing acqueous solutions of $SnCl_{4}$ and $NH_{4}$OH . The precipitate was washed with $NH_{4}NO_{3}$ solution while washing was controlled to be of three grades to modify its residual chloride content. The precipitate was dried at $1100^{\circ}C$ ~ 24h and calcined in air at $500^{\circ}C$ ~ $1100^{\circ}C$ for one hour. Thermal decomposition behaviour of $\alpha$-stannic acid was examined by a DT-TGA and a FTIR. Chemical composition and physical properties of $SnO_{2}$ powder were observed by an AES, a BET and a TEM, respectively. With a reduction in chloride content, the relative crystallite size of $SnO_{2}$ powder slightly increased by a low-temperature-calcining. However, at a high calcining temperature(T), the reverse relation occured. It was suggested that chloride ion replaces part of lattice oxygen site of a-stannic acid. Also, chloride ion on the site was suggested to retard de-hydration as well as crystalization at a low T while to promote crystal growth of $SnO_{2}$ by forming oxygen vacancy at a high T.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.4 no.3
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• pp.252-261
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• 1994

The $(Ba_{1-X}Sr_X)ZrO_3$ powder showing chemically pure and fine particle size was attempted to be synthesized by the oxalate method. The objective of this study is to determine the optimum synthesis condition of stable $(Ba_{1-X}Sr_X)ZrO_3$ powder in terms of the temperatures coefficient of resonant frequency ${\tau}_f$ by examining the microstructure and dielectric properties of the synthesized powder. The six compounds (x=0, 0.2, 0.4, 0.6, 0.8, 1) of $(Ba_{1-X}Sr_X)ZrO_3$ were prepared by the oxalate method, and then calcined at $1000^{\circ}C$ to obtain the crystalline $(Ba_{1-X}Sr_X)ZrO_3$ powder. The synthesized powder showed the globular-shape and average particle size of less than $0.2 \mu\textrm{m}$. The composition of x=0.5, i.e., half of Ba was replaced by Sr, is experted to show the zero value of temperatures coefficient of capacitance ${\tau}_c$.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.1 no.1
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• pp.59-70
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• 1991

ZnO fine powder was prepared by the batch precipitation process using $ZnCl_2$ and hexamethylenetetramine solution as a mother solution. When the concentrations of $ZnCl_2$solution were $0.1mol/\ell$ and 0.05mol/-, the particles of rod shape were obtained when the conentration of $ZnCl_2$solution was $0.01mol/\ell$, the particle of plate shape was obtained. When the hexamethylenetetramine as a precipitants was used, pH was raised slow during a few minute be-cause of slow hydrolysis rate of hexamethylenetetramine. For rapid raising of pH during initial reac-tion time, $NH_4$OH was added as nucleant. When $NH_4$OH as a nucleant was added, obtained particle was shape of granular and the mean particle size was $0.41\mu\textrm{m}$. After calcination at $500^{\circ}C$ during 1hour, all of remained organic phase was removed but the shape of particles was not changed. But pa-rticles were slightly shrunk in comparision with before calcined particles.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.12 no.2
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• pp.87-90
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• 2002

$LiCoO_{2}$ powders were synthesized at various temperatures using lithium hydroxide and cobalt hydroxide as precursors prepared by precipitation process and freeze-drying. In this study, the$LiCoO_{2}$ samples were synthesized via a solid state reaction with various LiOH concentration between 10 % and 30 % excess. And $LiCoO_{2}$powders were calcined at 600~$800^{\circ}C$ in a short time. Measurements of XRD and SEM were performed to characterize the properties of the prepared materials. The effect of amount of Li ions on the structural change in powder has been examined using the XRD analysis. For the not added excess of LiOH, CoOOH phase presented in the XRD pattern of $LiCoO_{2}$ due to loss of Li ions during firing. The morphology and particle size of the powders were examined using SEM. The obtained powders are high temperature-$LiCoO_{2}$HT-LiCoO$_{2}$) and homogeneous with the range of grain size in the order of hundreds of nanometers. The effects of variation of LiOH concentration on the structural change in powder were investigated using the Rietveld analysis. As an analysis result, c/a is constant by 4.99 on all occasions. Finally, the structure of HT-$LiCoO_{2}$ was simulated by the commercial software $Creius^{2}$(Molecular Simulations, Inc.) from the results of Rietveld analysis.

• Journal of Hydrogen and New Energy
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• v.20 no.5
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• pp.432-438
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• 2009

In this paper, we synthesized LSG powder by Modified-GNP method. Lanthanum, strontium and gallium (LSG) were selected in the preparation of an oxygen-electrode (anode) for High Temperature Steam Electrolysis system (HTSE). The used amount and concentration of nitric acid were varied to find out an appropriate composition for oxygen-electrode (anode). In order to optimize the molar ratio of La and Sr, ratio of La to Sr was varied that 2:8, 5:5 and 8:2. The combined LSGs were calcined for 2 hours at $700^{\circ}C$ and were sintered in a furnace for 4 hours at $1200^{\circ}C$. The phase and crystallinity of LSG powder were determined by XRD. The surface morphology was observed through SEM photograph, and the specific surface area was investigated with BET. The thermochemical property was determined by TG/DTA. The synthesized preparation was obtained of $La_{0.8}Sr_{0.2}GaO_{3}$ formula for 3M nitric acid, which was the best perovskite phase.

• Korean Journal of Materials Research
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• v.21 no.8
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• pp.468-475
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• 2011

[ $LaMeO_3$ ](Me = Cr, Co) powders were prepared using the polymeric precursor method. The effects of the chelating agent and the polymeric additive on the synthesis of the $LaMeO_3$ perovskite were studied. The samples were synthesized using ethylene glycol (EG) as the solvent, acetyl acetone (AcAc) as the chelating agent, and polyvinylpyrrolidone (PVP) as the polymer additive. The thermal decomposition behavior of the precursor powder was characterized using a thermal analysis (TG-DTA). The crystallization and particle sizes of the $LaMeO_3$ powders were investigated via powder X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and particle size analyzer, respectively. The as-prepared precursor primarily has $LaMeO_3$ at the optimum condition, i.e. for a molar ratio of both metal-source (a : a) : EG (80a : 80a) : AcAc (8a) inclusive of 1 wt% PVP. When the as-prepared precursor was calcined at $700^{\circ}C$, only a single phase was observed to correspond with the orthorhombic structure of $LaCrO_3$ and the rhombohedral structure of $LaCoO_3$. A solid-electrolyte impedance-metric sensor device composed of $Li_{1.5}Al_{0.5}Ti_{1.5}(PO_4)_3$ as a transducer and $LaMeO_3$ as a receptor has been systematically investigated for the detection of NOx in the range of 20 to 250 ppm at $400^{\circ}C$. The sensor responses were able to divide the component between resistance and capacitance. The impedance-metric sensor for the NO showed higher sensitivity compared with $NO_2$. The responses of the impedance-metric sensor device showed dependence on each value of the NOx concentration.

• Korean Journal of Materials Research
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• v.17 no.7
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• pp.382-385
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• 2007

[ $LaFeO_3$ ] powders were prepared as the oxidation catalyst materials to reduce the emission of particulate matters from diesel engine and their catalytic effects on the oxidation of carbon were investigated. Solution combustion method was employed for the powder synthesis, which uses highly exothermic and selfsustaining reactions. In this study $LaFeO_3$ powders were synthesized at $400^{\circ}C$ as varying the ratio ($\Phi$) of fuel (citric acid) and oxidizer (metal nitrate), and their phase and carbon ignition property were examined. As $\Phi$ decreases, the crystallinity of synthesized $LaFeO_3$ powders enhanced. By calcining at $700^{\circ}C$, all the powders synthesized at various $\Phi$ fully crystallized. The calcined $LaFeO_3$ powders showed carbon ignition temperature as low as $501{\sim}530^{\circ}C$, which implied the decrease of the ignition temperature by $120{\sim}150^{\circ}C$.

• Korean Journal of Materials Research
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• v.23 no.10
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• pp.543-549
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• 2013

The purpose of this paper was to investigate the effect of a high-energy milling (HEM) process on the particle morphology and the correlation between a thermal treatment and tetragonal/monoclinic nanostructured zirconia powders obtained by a precipitation process. To eliminate chloride residue ions from hydrous zirconia, a modified washing method was used. It was found that the used washing method was effective in removing the chloride from the precipitated gel. In order to investigate the effect of a pre-milling process on the particle morphology of the precipitate, dried $Zr(OH)_4$ was milled using a HEM machine with distilled water. The particle size of the $Zr(OH)_4$ powder exposed to HEM reduced to 100~150 nm, whereas that of fresh $Zr(OH)_4$ powder without a pre-milling process had a large and irregular size of 100 nm~1.5 ${\mu}m$. Additionally, modified heat treatment process was proposed to achieve nano-sized zirconia having a pure monoclinic phase. It was evident that two-step calcining process was effective in perfectly eliminating the tetragonal phase, having a small average particle of ~100 nm with good uniformity compared to the sample calcined by a single-step process, showing a large average particle size of ~300 nm with an irregular particle shape and a broad particle size distribution. The modified method is considered to be a promising process for nano-sized zirconia having a fully monoclinic phase.

• Journal of Powder Materials
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• v.20 no.3
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• pp.210-214
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• 2013

This manuscript reports on compared color evolution about phase transformation of ${\alpha}-FeOOH@SiO_2$ and ${\beta}-FeOOH@SiO_2$ pigments. Prepared ${\alpha}$-FeOOH and ${\beta}$-FeOOH were coated with silica for enhancing thermal properties and coloration of both samples. To study phase and color of ${\alpha}$-FeOOH and ${\beta}$-FeOOH, we prepared nano sized iron oxide hydroxide pigments which were coated with $SiO_2$ using tetraethylorthosilicate and cetyltrimethyl-ammonium bromide as a surface modifier. The silica-coated both samples were calcined at high temperatures (300, 700 and $1000^{\circ}C$) and characterized by scanning electron microscopy, CIE $L^*a^*b^*$ color parameter measurements, transmission electron microscopy and UV-vis spectroscopy. The yellow ${\alpha}$-FeOOH and ${\beta}$-FeOOH was transformed to ${\alpha}-Fe_2O_3$ with red, brown at 300, $700^{\circ}C$, respectively.