• Journal of Powder Materials
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• v.18 no.4
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• pp.347-358
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• 2011

Two different schemes were adopted to fabricate ordered macroporous structures with face centered cubic lattice of air spheres. Monodisperse polymeric latex suspension, which was synthesized by emulsifier-free emulsion polymerization, was mixed with metal oxide ceramic nanoparticles, followed by evaporation-induced self-assembly of the mixed hetero-colloidal particles. After calcination, inverse opal was generated during burning out the organic nanospheres. Inverse opals made of silica or iron oxide were fabricated according to this procedure. Other approach, which utilizes ceramic precursors instead of nanoparticles was adopted successfully to prepare ordered macroporous structure of titania with skeleton structures as well as lithium niobate inverted structures. Similarly, two different schemes were utilized to obtain disordered macroporous structures with random arrays of macropores. Disordered macroporous structure made of indium tin oxide (ITO) was obtained by fabricating colloidal glass of polystyrene microspheres with low monodispersity and subsequent infiltration of the ITO nanoparticles followed by heat treatment at high temperature for burning out the organic microspheres. Similar random structure of titania was also fabricated by mixing polystyrene building block particles with titania nanoparticles having large particle size followed by the calcinations of the samples.

• Journal of the Korean Chemical Society
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• v.56 no.4
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• pp.484-490
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• 2012

The tin (IV) oxide nanoparticles are prepared by controlled precipitation method and calcined at temperatures of $200-600^{\circ}C$. The prepared $SnO_2$ nanoparticles characterized by XRD patterns, TEM image, IR and UV-Vis spectra. The XRD patterns and TEM image show the tetragonal structure and spherical morphology for $SnO_2$ nanoparticles, respectively. The photocatalytic activity of the prepared $SnO_2$ nanoparticles studied in degradation reaction of methylene blue (MB). The results show the size of nanoparticles, band-gap energy and photocatalytic activity of $SnO_2$ depends on the calcinations temperature. The $SnO_2$ nanoparticles calcined at $500^{\circ}C$ indicated the highest photoreactivity. Also, the zero-valent tin (ZVT) nanoparticles with tetragonal structure are prepared by a reducing agent and used as a catalyst in degradation of MB. In basic pH of 11, the degradation >95% of MB at time 150 min obtained at presence of ZVT nanoparticles.

• Resources Recycling
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• v.17 no.5
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• pp.52-59
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• 2008

Sol-gel process applied in this study was carried out by chelation of metal ions and citric acid. From the results of thermal gravimetric analysis and XRD analysis of gel powder obtained through sol-gel and heat treatment, gel powders are mostly amorphous, and crystallize completely at $900^{\circ}C$, and the crystalline structure of YAG increases with increasing calcinations temperature. Since YAG prepared by sol-gel & calcinations process was porous, and the sape and size was irregular and nonuniform, the shape and size of YAG powder had to be controlled. Therefore the effects of organic materials such as ethylene glycol and surfactant on the crystalline structure of YAG powder were investigated. Polyesterification of ethylene glycol and citric acid separated reaction area of metal ions in the solution and decreased the size of YAG primary particles. The addition of Igepal 630 as surfactant formed the droplet in the solution, and increased the size of primary particles which forms the aggregate of YAG In order to obtain monodispersed YAG particles of uniform size, gel powder prepared with organic materials had to be milled before calcination. And milling process was very important for obtaining YAG of uniform size.

• Journal of the Korean Magnetic Resonance Society
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• v.9 no.2
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• pp.138-154
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• 2005

Vanadium-incorporated aluminophosphate molecular sieve $VO^{2+}-SAPO-5$ was studied by electron spin resonance (ESR) and electron spin echo modulation (ESEM) spectroscopies to determine the vanadium structure and interaction with various adsorbate molecules. It was found that the main species at low concentration of vanadium is a monomeric vanadium units in square pyramidal or distorted octahedral coordination, both in oxidation state (IV) for the calcined hydrated material and in oxidation state (V) for the calcined material. After calcinations in $O_2$ and exposure to moisture, only species A is observed with reduced intensities. It is suggested as a $VO(H_2O)_3^{2+}$ complex coordinated to two framework oxygen bonded aluminum. When calcined, hydrated $VO^{2+}-}SAPO-5$ is dehydrated at elevated temperature, a species loses its water ligands and transforms to $VO^{2+}$ ions coordinated to two framework oxygens (species B). Species B reduces its intensity, significantly after treatment with $O_2\;at\;600^{\circ}C$ for 5 h, thus suggesting oxidation of $V^{4+}\;to\;V^{5+}$. When dehydrated $VO^{2+}-SAPO-5$ contacts with $D_2O$ at room temperature, the EPR signal of species A is observed. Thus species assumed as a $VO^{2+}(O_f)_2(D_2O)_3$, by considering two framework oxygens. Adsorption of deuterated ethanol, propanol on dehydrated $VO^{2+}_{-}SAPO-5$ result in another new vanadium species E and F, respectively, which are identified as a $VO^{2+}-(CH_3CH_2OD)_3,\;VO^{2+}-(CH_3CH_2CH_2OD)_2$ complex. When deuterated benzene is adsorbed on dehydrated $VO^{2+}-SAPO-5$, another new vanadium species G, identified as a $VO^{2+}-(C_6D_6)$ is observed. Possible coordination geometries of these various complexes are discussed.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.22 no.1
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• pp.35-40
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• 2009

Lead free positive temperature coefficient of resistivity (PTCR) ceramics based on $BaTiO_3-(Bi_{0.5}Na_{0.5})TiO_3$ solid solution were prepared by a conventional solid state reaction method. The phase structure was showed single phase with perovskite structure regardless calcinations temperature and $Ba_{1-x}(Bi_{0.5}Na_{0.5})_xTiO_3$ structure was transformed from tetragonal to orthorhombic phase at $x{\geq}0.15$ mole. The XRD peaks with $45^{\circ}{\sim}46^{\circ}$ shifted in right the influence of crystal structure change and the intensity of peak was decreased with additive $(Bi_{0.5}Na_{0.5})TiO_3$. The curie temperature risen with additive $(Bi_{0.5}Na_{0.5})TiO_3$ but disappeared for $(Bi_{0.5}Na_{0.5})TiO_3$ addition more than 0.15 mole in TMA. In relative permittivity, the curie temperature by the transform of ferroelectric phase risen with additive $(Bi_{0.5}Na_{0.5})TiO_3$ but decreased in relative permittivity. Also, the peak of new curie temperature showed the sample containing $0.025{\sim}0.045$ mole of $(Bi_{0.5}Na_{0.5})TiO_3$ near $70^{\circ}C$ caused by phase transform from ferroelectric to ferroelectric and the peak of new curie temperature disappeared at 0.045 mole of $(Bi_{0.5}Na_{0.5})TiO_3$. In our study, it was found that the PTCR in $BaTiO_3-(Bi_{0.5}Na_{0.5})TiO_3$ system was possible for $0{\sim}0.025$ mole of $(Bi_{0.5}Na_{0.5})TiO_3$ and the maximum curie temperature by phase transition showed about at $145^{\circ}C$.

• Journal of the Korean Ceramic Society
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• v.42 no.8 s.279
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• pp.561-566
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• 2005

For the homogeneous dispersion of $ZrO_2$ particles in $Al_2O_3/ZrO_2$ceramics, Zr-precusors were mixed with oxide $Al_2O_3$powders by chemical routes such as partial precipitation or partial polymerization of Zr-nitrate solutions. In case of the mechanical mixing of ultrafine $Al_2O_3$ and $ZrO_2$ oxide powders, relatively homogeneous dispersion was difficult to achieve so that the particle size and distributions of $ZrO_2$ were relatively inhomogeneous after sintering at high temperature. But when the Zr-Y-hydroxide were co-precipitated to ultrafine $Al_2O_3$ oxide powders followed by calcinations, homogeneous dispersion of nano-sized $ZrO_2$ particles in $Al_2O_3/ZrO_2$ composite ceramics were obtained. But because of the coalescence of dispersed $ZrO_2$ particles, dispersed $ZrO_2$ was grown up to more than 0.2${mu}m$ (200 nm) when sintered at the temperature of higher than $1500^{\circ}C$ But when the sintering temperature was kept to lower than $1400^{\circ}C$ by using nano-sized $\alpha-alumina$, the particle size of dispersed $ZrO_2$ could be sustained below 0.1 ${\mu}m$. But the coalescence of dispersed $ZrO_2$ between $Al_2O_3$ particles could not be avoided so that the mechanical properties were not enhanced contrary to the expectations. So Zr-polyester precursors were precipitated and coated to the surface of ultrafine $\alpha-alumina$ powders by the polymerization of Ethylene Glycol with Citric Acid and Zirconium Nitrate. By this dispersion much more uniform dispersion of $ZrO_2$ was achieved at $1450\~1600^{\circ}C$ of sintering temperature ranges. And due to especially discrete dispersion of $ZrO_2$ between $Al_2O_3$ particles, their mechanical strength was more enhanced than mechanical mixing or hydroxide precipitation methods.

• The Journal of Engineering Research
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• v.2 no.1
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• pp.139-145
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• 1997

The effect of Ba addition on the thermal stabilization of $\gamma$-$Al_2O_3$ powders were studied. Ba additive was introduced into $\gamma$-$Al_2O_3$ powders by wet impregnation of $Ba(No_3)_3$.$6H_2O$. Ba additive was proved to be effective on the thermal stabilization of $\gamma$-$Al_2O_3$ powders by suppression of sintering. The optimum content of Ba was determined by 5 mol%, through the calcinations temperature range. It is suggested that the main reason of thermal stabilizaton is the substitution effect of large $Ba^{2+}$ ions into the $\Al^{3+}$ sites, which suppressed the surface diffusion of $\Al^{3+}$ ions.

• Journal of the Mineralogical Society of Korea
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• v.22 no.2
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• pp.107-114
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• 2009

In present study, an alternative process for manufacturing ultra marine blue by using kaolin, sulfur, sodium carbonate, silica, and rosin was investigated. From the experiments, it was found in the reductive calcination process that the temperature variation with the bed height of input materials is relatively high due to the inadequate thermal conductivity of them. It was also found that the color of the ultramarine blue manufactured is sensitive for the shape of the input materials and the calcinations conditions, and specially the heating rate is very important to form ultramarine. For manufacturing green ultramarine by using sulfur, sodium carbonate, silicon, and pine resin, an optimum condition was investigated to be the heating rate region below $0.6^{\circ}C/min$, the reaction temperature of $850^{\circ}C$ and the reaction time of 4 hr. At the oxidative calcination process to manufacture ultra marine blue from green ultramarine, the optimum flow rate of air is $500{\sim}550\;{\ell}/kg$ (green ultramarine) and the reaction temperature is $500{\sim}550^{\circ}C$.

• Journal of Biosystems Engineering
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• v.39 no.3
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• pp.227-234
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• 2014

Purpose: The aim of this research was to develop and evaluate natural hydroxyapatite (HA) ceramics produced from the heat treatment of pig bones. Methods: The properties of natural HA ceramics produced from pig bones were assessed in two parts. Firstly, the raw materials were characterized. A temperature of $1,200^{\circ}C$ was chosen as the calcination temperature. Fine bone powders (BPs) were produced via calcinations and a milling process. Sintered BPs were then characterized using field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), X-ray fluorescence spectroscopy (XRF), energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared (FTIR) spectroscopy, and a 2-year in vitro degradability test. Secondly, an indirect cytotoxicity test was conducted on human osteoblast-like cells, MG63, treated with the BPs. Results: The average particle size of the BPs was $20{\pm}5{\mu}m$. FE-SEM showed a non-uniform distribution of the particle size. The phase obtained from XRD analysis confirmed the structure of HA. Elemental analysis using XRF detected phosphorus (P) and calcium (Ca) with the Ca/P ratio of 1.6. Functional groups examined by FTIR detected phosphate ($PO{_4}^{3-}$), hydroxyl ($OH^-$), and carbonate ($CO{_3}^{2-}$). The EDX, XRF, and FTIR analysis of BPs indicated the absence of organic compounds, which were completely removed after annealing at $1,200^{\circ}C$. The BPs were mostly stable in a simulated body fluid (SBF) solution for 2 years. An indirect cytotoxicity test on natural HA ceramics showed no threat to the cells. Conclusions: In conclusion, the sintering temperature of $1,200^{\circ}C$ affected the microstructure, phase, and biological characteristics of natural HA ceramics consisting of calcium phosphate. The Ca-P-based natural ceramics are bioactive materials with good biocompatibility; our results indicate that the prepared HA ceramics have great potential for agricultural and biological applications.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.18 no.5
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• pp.200-204
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• 2008

Mechano Chemical Process (MCP) skips the calcinations steps at an intermediate temperature that is always required in the conventional solid-state reaction because forming phase from raw powder is activated by mechanical energy. In this study, we prepared (Pb, La)$TiO_3$ nanopowder with perovskite structure by only high energy MCP. Especially, the PLT nanopowder was synthesized without any thermal treatment using oxides, not salts as raw powder. This process is also very simple due to dry milling method, unnecessary to dry of powder. The oxide powder was milled up to 12 hr at intervals of an hour using MCP and the pure PLT phase of perovskite structure was formed after milling time of 3 hr. And the average particle size was 20 nm with narrow distribution after milling time of 3 hr from raw powder of several $\mu m$ with inhomogeneous distribution.