• Bulletin of the Korean Chemical Society
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• 제19권11호
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• pp.1185-1188
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• 1998

Layered nanocomposite, SiO2/TiO2 sol pillared clay, has been prepared by the ion exchange reaction of Na' ion in montmorillonite with positively charged mixed SiO2/TiO2 sol. The nanosized sol particles were synthesized by mixing SiO2 sol solution with TiO2 one, which is obtained by acidic hydrolysis of TEOS and TiCl4, respectively. From powder XRD, the basal spacing (d001) of the sample calcined at 400 ℃ was found to be ca. 60 Å, due to the multistacking of nanosized SiO2 and TiO2 sol particles, which was confirmed by the pore size analysis from 129Xe NMR and micropore analysis calculated from nitrogen adsorption. The BET specific surface area shows the value of 684 m2g-1 (Langmuir 1115 m2g-1), which is the highest among various pillared clays ever reported previously, and the total porosity is found to be 0.51 mlg-1, and the pores are mainly composed of micropore with a size of ca. 11.8 Å. This result agrees with the adsorption capacity obtained from water adsorption. According to diffuse reflectance ultraviolet-visible spectroscopy, it is found that the TiO2 particles stabilized in the interlayer space of montmorillonite are quantum-sized of ca. 20 Å.

• 한국분말재료학회지
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• 제24권6호
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• pp.457-463
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• 2017

Nanosized $Gd_2O_3:Eu^{3+}$ red phosphor is prepared using a template method from metal salt impregnated into a crystalline cellulose and is dispersed using a bead mill wet process. The driving force of the surface coating between $Gd_2O_3:Eu^{3+}$ and mica is induced by the Coulomb force. The red phosphor nanosol is effectively coated on mica flakes by the electrostatic interaction between positively charged $Gd_2O_3:Eu^{3+}$ and negatively charged mica above pH 6. To prepare $Gd_2O_3:Eu^{3+}$-coated mica ($Gd_2O_3:Eu/mica$), the coating conditions are optimized, including the stirring temperature, pH, calcination temperature, and coating amount (wt%) of $Gd_2O_3:Eu^{3+}$. In spite of the low luminescence of the $Gd_2O_3:Eu/mica$, the luminescent property is recovered after calcination above $600^{\circ}C$ and is enhanced by increasing the $Gd_2O_3:Eu^{3+}$ coating amount. The $Gd_2O_3:Eu/mica$ is characterized using X-ray diffraction, field emission scanning electron microscopy, zeta potential measurements, and fluorescence spectrometer analysis.

• 한국분말재료학회지
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• 제29권3호
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• pp.207-212
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• 2022

Nanosized rutile titanium dioxide (TiO₂) is used in inorganic pigments and cosmetics because of its high whiteness and duality. The high quality of the white pigments depends on their surface coating technique via the solgel process. SiO₂ coatings are required to improve the dispersibility, UV-blocking, and whiteness of TiO₂. Tetraethyl orthosilicate (TEOS) is an important coating precursor owing to its ability to control various thicknesses and densities. In addition, we use Na₂SiO₃ (sodium silicate) as a precursor because of its low cost. Compared to TEOS, which controls the pH using a basic catalyst, Na₂SiO₃ controls the pH using an acid catalyst, giving a uniform coating. The coating thickness of TiO₂ is controlled using a surface modifier, cetrimonium bromide, which is used in various applications. The shape and thickness of the nanosized coating layer on TiO₂ are analyzed using transmission electron microscopy, and the SiO₂ nanoparticle behavior in terms of the before-and-after size distribution is measured using a particle size analyzer. The color measurements of the SiO₂ pigment are performed using UV-visible spectroscopy.

• 한국분말재료학회지
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• 제19권2호
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• pp.122-126
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• 2012

The Fe-based self-fluxing alloy powders and TiC particles were ball-milled and subsequently compacted and sintered at various temperatures, resulting in the TiC particle-reinforced Fe self-fluxing alloy hybrid composite, and the microstructure and micro-hardness were investigated. The initial Fe-based self-fluxing alloy powders and TiC particles showed the spherical shape with a mean size of approximately 80 ${\mu}m$ and the irregular shape of less than 5 ${\mu}m$, respectively. After ball-milling at 800 rpm for 5 h, the powder mixture of Fe-based self-fluxing alloy powders and TiC particles formed into the agglomerated powders with the size of approximately 10 ${\mu}m$ that was composed of the nanosized TiC particles and nano-sized alloy particles. The TiC particle-reinforced Fe-based self-fluxing alloy hybrid composite sintered at 1173 K revealed a much denser microstructure and higher micro-hardness than that sintered at 1073 K and 1273 K.

• 한국결정성장학회지
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• 제20권6호
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• pp.283-288
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• 2010

나노 크기의 NiO 분말을 Ni 산성염과 Ni 염기성염을 혼합하여 제조하는 방법에서 원료가 생성되는 NiO와 이의 환원으로 생성되는 Ni 결정 특성에 미치는 영향을 연구하였다. 산성염으로는 Ni formate를 염기성염으로는 수산화 Ni과 염기성 Ni 탄산염을 사용하였다. 혼합비는 산성염 1당량에 염기성염 9당량을 사용하였으며, 탄산염을 사용한 경우 $750^{\circ}C$/2 h 하소에서도 ~100 nm의 구형의 NiO 분말을 얻었으며, 수산화 염을 사용한 경우는 $600^{\circ}C$/2 h에서는 ~100 nm의 유사 구형의 NiO가 생성되나, $750^{\circ}C$ 열처리에서는 100~600 nm의 유사 입방체 분말을 얻었다. 수산화 염을 사용한 경우에는 탄산염을 사용한 경우에 비하여 수소가스에 의한 환원이 훨씬 빠르게 진행되어 necking이 일어나며 소결이 이루어져 다공체를 형성하였다. 이들 특성을 TG/DSC, XRD, SEM으로 분석하였다.

• 한국분말재료학회지
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• 제26권5호
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• pp.410-414
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• 2019

The hydrogen reduction behavior of the $CuO-SCo_3O_4$ powder mixture for the synthesis of the homogeneous Cu-15at%Co composite powder has been investigated. The composite powder is prepared by ball milling the oxide powders, followed by a hydrogen reduction process. The reduction behavior of the ball-milled powder mixture is analyzed by X-ray diffraction (XRD) and temperature-programmed reduction at different heating rates in an Ar-10%H2 atmosphere. The scanning electron microscopy and XRD results reveal that the hydrogen-reduced powder mixture is composed of fine agglomerates of nanosized Cu and Co particles. The hydrogen reduction kinetics is studied by determining the degree of peak shift as a function of the heating rate. The activation energies for the reduction of the oxide powders estimated from the slopes of the Kissinger plots are 58.1 kJ/mol and 65.8 kJ/mol, depending on the reduction reaction: CuO to Cu and $SCo_3O_4$ to Co, respectively. The measured temperature and activation energy for the reduction of $SCo_3O_4$ are explained on the basis of the effect of pre-reduced Cu particles.

• 한국분말재료학회지
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• 제15권6호
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• pp.450-457
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• 2008

The objectives of this study were the development of a synthesis technique for highly active nanosized ITO powder and the understanding of the reaction mechanisms of the ITO precursors. The precipitation and agglomeration phenomena in ITO and $In_{2}O_{3}$ precursors are very sensitive to reaction temperature, pH, and coexisting ion species. Excessive $Cl^-$ ion and $Sn^{+4}$ ions had a negative effect an synthesizing highly active powders. However, with a relevant stabilizing treatment the shape and size of ITO and $In_{2}O_{3}$ precursors could be controlled and high density sintered products of ITO were obtained. By applying the reprecipitation process (or stabilization technique), highly active ITO and $In_{2}O_{3}$ powders were synthesized. Sintering these powders at $1500^{\circ}C$ for 5 hours produced 97% dense ITO bodies.

• 한국분말재료학회지
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• 제11권2호
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• pp.124-129
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• 2004

Nanosized WC and WC-Co powders were synthesised by chemical vapor condensation(CVC) process using the pyrolysis of tungsten hexacarbonyl(W(CO)$_6$) and cobalt octacarbonyl(Co$_2$(CO)$_8$). The microstructural changes and phase evolution of the CVC powders during post heat-treatment were studied using the XRD, FE-SEM, TEM, and ICP-MS. CVC powders were consisted of the loosely agglomerated sub-stoichimetric WC$_{1-x}$ and the long-chain Co nanopowders. The sub-stochiometric CVC WC and WC-Co powders were carburized using the mixture gas of CH$_4$-H$_2$ in the temperature range of 730-85$0^{\circ}C$. Carbon content of CVC powder controlled by the gas phase carburization at 85$0^{\circ}C$ was well matched with the theoretical carbon sioichiometry of WC, 6.13 wt％. During the gas phase carburization, the particle size of WC increased from 20 nm to 40 nm and the long chain structure of Co powders disappeared.

• 한국분말재료학회지
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• 제29권3호
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• pp.247-251
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• 2022

This study demonstrates the effect of the compaction pressure on the microstructure and properties of pressureless-sintered W bodies. W powders are synthesized by ultrasonic spray pyrolysis and hydrogen reduction using ammonium metatungstate hydrate as a precursor. Microstructural investigation reveals that a spherical powder in the form of agglomerated nanosized W particles is successfully synthesized. The W powder synthesized by ultrasonic spray pyrolysis exhibits a relative density of approximately 94% regardless of the compaction pressure, whereas the commercial powder exhibits a relative density of 64% under the same sintering conditions. This change in the relative density of the sintered compact can be explained by the difference in the sizes of the raw powder and the densities of the compacted green body. The grain size increases as the compaction pressure increases, and the sintered compact uniaxially pressed to 50 MPa and then isostatically pressed to 300 MPa exhibits a size of 0.71 m. The Vickers hardness of the sintered W exhibits a high value of 4.7 GPa, mainly due to grain refinement.

• 한국재료학회지
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• 제12권12호
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• pp.947-954
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• 2002

HCl concentration and reaction time are the decisive factors in determining the structure of precipitates in the process of synthesis of $TiO_2$ particles from aqueous $TiOCl_2$ solution by precipitation and the volumetric proportion of brookite phase in $TiO_2$ particles can be controlled by these two factors. As reaction rate increases with increase of reaction temperature, the reaction time, at which maximum volumetric proportion of brookite phase in $TiO_2$ particles was obtained, was reduced. The brookite was transformed directly to rutile phase with only increase of reaction time. And precipitation was delayed with increase of HCl concentration because the amount of $H_2$O, which is necessary source of oxygen for conversion of $Ti^{+4}$ to $TiO_2$, was relatively reduced with increase of that. Brookite in the mixture phase powder was finally transformed to rutile phase via anatase through heat-treatment.