• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.25 no.4
• /
• pp.166-171
• /
• 2015

In this study, using solid-state and flux, $Y_3Al_5O_{12}:Er^{3+}\;(YAG:Er^{3+})$ powders were successfully synthesized at low temperatures. To analyze the crystallinity of powders according to the synthesis or non-synthesis of powders and powder calcination temperatures, X-ray diffraction (XRD) was measured. In the case of pure YAG, when YAG was analyzed using the general solid-phase method, it was calcined for 12 hours at $1400^{\circ}C$ and pure YAG phase could be obtained. But when $BaF_2$ was added to YAG, YAG was synthesized at lower temperature (1000^{\circ}C$). It was thus found that the synthesis temperature could be lowered by about $400^{\circ}C$. Also, when BaF2 with an optimal concentration was added to $YAG:Er^{3+}$, the particle shape and size according to synthesis temperatures were surveyed, and corresponding luminous intensity was discussed.

• Bulletin of the Korean Chemical Society
• /
• v.30 no.8
• /
• pp.1719-1723
• /
• 2009

The LiFeP$O_4$ powder was synthesized by using the solid state reaction method with Fe($C_2O_4){\cdot}2H_2O,\;(NH_4)_2HPO_4,\;Li_2CO_3$, and chitosan as a carbon precursor material for a cathode of a lithium-ion battery. The chitosan added LiFePO4 powder was calcined at 350 ${^{\circ}C}$ for 5 hours and then 800 ${^{\circ}C}$ for 12 hours for the calcination. Then we calcined again at 800 ${^{\circ}C}$ for 12 hours. We characterized the synthesized compounds via the crystallinity, the valence states of iron ions, and their shapes using TGA, XRD, SEM, TEM, and XPS. We found that the synthesized powders were carbon-coated using TEM images and the iron ion is substituted from 3+ to 2+ through XPS measurements. We observed voltage characteristics and initial charge-discharge characteristics according to the C rate in LiFeP$O_4$ batteries. The obtained initial specific capacity of the chitosan added LiFeP$O_4$ powder is 110 mAh/g, which is much larger than that of LiFeP$O_4$ only powder.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.9 no.5
• /
• pp.510-515
• /
• 1999

Synthesize of anatase type $TiO_2$ from $TiCl_4$ solution was studied. KOH was used on dehydration reaction of $TiCl_4$ solution. Products of dehydration reaction was calcined at 300, 500, 700, 900, $1000^{\circ}C$ during 1hour. Calcined products was studied by XRD, DTA, and FT-IR for effect of calcined temperature. The results are as follow. \circled1 Product pf dehydration reaction at$ 90^{\circ}C$ was semicrystalline anatase type $TiO_2$ because it has a peak vary broad and low at the position of anatase crysral XRD pattern. \circled2 Pure titanium oxide semi-crystalline products were produced at acid pH condition which convert to anatase crystal at $300^{\circ}C$ and to rutile crystal at $700^{\circ}C$. \circled3 The chemical composition of semicrystalline products which was produce at alkali pH conditions, were potasium titante. Potasium-titanate semi-crystalline products crystallized at 630~$640^{\circ}C$ \circled4 The transition temperature of potassium dopped titanium oxide semi-crystalline products was increased with the contents of potasium. \circled5 The optimum synthesise condition of anatase $TiO_2$ products from $TiCl_4$ and KOH are pH 3~5 and $300^{\circ}C$ calcination.

• Korean Chemical Engineering Research
• /
• v.51 no.4
• /
• pp.426-431
• /
• 2013

Nanosized $TiO_2$ particles were prepared from titanium (IV) sulfate solution using base solutions at low reaction temperature ($95^{\circ}C$) and atmospheric pressure by hydrothermal precipitation method without calcination. The effects of preparation conditions, such as kind of base solutions (NaOH, $NH_4OH$, Monoethanolamine, Diethanolamine, Triethanolamine) and surfactants (CTAB, Span 20, SDBS), concentration of surfactants, temperature and pH, on the physical properties of $TiO_2$ particles have been investigated by XRD, SEM and Zeta-potential meter. Absorption area was also investigated by DRS in order to confirm the photocatalytic activity of the nanosized $TiO_2$ particles. It was turned out that, among base solutions, NaOH provides the smallest $TiO_2$ particles with excellent crystallinity. And cationic surfactant (CTAB) prepared smaller $TiO_2$ particles than any other surfactants. When CTAB is added in the concentration ratio of $Ti(SO_4)_2$:CTAB=10:1, $TiO_2$ particles with particle diameter of 5.8 nm were prepared. This is approximately 1/10 of that prepared without CTAB.

• Korean Chemical Engineering Research
• /
• v.44 no.2
• /
• pp.172-178
• /
• 2006

Mesoporous silicate materials have been used as adsorbents for the removal of heavy metals from water by introducing functional groups such as thiol and amine. In this research, it was investigated whether surfactants used as templating agents in synthetic processes can act as adsorption sites for heavy metals. Three mesoporous silicates-SBA-15, MCM-41, and HMS were synthesized using, respectively, block copolymer, hexadecyltrimethylammoniumbromide (HDTMA), and dodecyamine as surfactants. X-ray diffraction and $N_2$ gas adsorption analysis confirmed that the mesoporous silicates were well prepared and FT-IR spectra resulted in the existence of the surfactants in as-synthesized mesoporous silicates and the removal of surfactants after calcination. The interactions between $Pb^{2+}$ ions and the mesoporous silicate materials with/without surfactants were observed. In adsorption kinetic experiments, it revealed that the calcined mesoporous silicates and the surfactant-loaded SBA-15 almost had no adsorption capacity for $Pb^{2+}$ ions. In contrast, the surfactant-loaded MCM-41 and HMS showed, respectively, the adsorption capacities of 26.60 and 115.16 mg/g which were acquired through the fits of adsorption kinetic data to the pseudo second order kinetic model. The adsorption capacities were comparable to those of other mesoporous adsorbents for heavy metals.

• Proceedings of the Korea Association of Crystal Growth Conference
• /
• 1996.06b
• /
• pp.259-279
• /
• 1996

최근 정보·전자산업의 발전으로 고 신뢰성 전자재료에 대한 수요가 증대되고 있으며 이러한 첨단산업의 기반의 될 신소재 중 전자세라믹스가 차지하는 비중이 그 대부분을 차지하고 있으며 이에 대한 수요와 기대가 점점 커지고 있다. 이러한 전자세라믹스는 유전재료, 자성재료, 압전재료, 도전성 재료 등으로 나뉘게 된다. 어떠한 분류에 들어가든 그 조성은 금속의 산화물 형태가 일반적이며 미세한 분말의 성형체를 소결(sintering) 함으로써 최종제품으로 완성된다. 이러한 전잣라믹스가 최근 요구되는 고 신뢰성, 고 밀도화를 달성하기 위해선 원료 분말 제조단계부터 제어가 필요하다. 원료분말의 균일·균질성과 그 입도는 소결특성 뿐만아니라 전기적 특성에도 큰 영향을 미치기 때문이다. 세라믹스의 분말제조 방법 중 일반적으로 사용되는 방법으로는 고상 산화물을 혼합하여 하소(calcination)한 후 분쇄하는 '고상합성법'과 금속의 염 또는 alkoxide 용액을 이용하여 화학적으로 제조하는 '습식 화학적 합성법'이 있다. 고상합성법은 합성온도가 높고 기계적 분쇄와 혼합에 의존하므로 균일·균질성이 떨어지고 분말크기를 1㎛ 이하로 만들기 힘들다. 반면에 습식화학적 합성법은 기계적인 분쇄와 혼합에선 얻을 수 없는 원자 혹은 분자단위의 균일한 혼합과 submicron 이하의 미세한 분말을 얻을 수 있다. 따라서 이러한 습식 화학적 합성으로 얻은 분말을 사용하면 미세한 입자의 특성으로 인해 소결온도를 낮출 수 있으며 균일한 미세구조와 균질한 조성을 갖게되어 기계적·전기적 물성증진도 가져올 수 있게 된다. 습식 화학적 분말합성법은 전술하였듯이 alkoxide의 가수분해를 이용하는 sol-gel 법과 금속의 염(salt) 용액을 이용하여, 화학적으로 화합물 침전을 얻거나 또는 공침전물(coprecipitate) 형태의 분말을 얻는, 침전법으로 나뉠 수 있다. 침전법의 근본원리는 pH 및 pCO3 등에 따른 이온종의 용해도 차이를 이용하는 것으로써 각 이온종에 따른 solubility product(ksp)를 이용하여 설명된다. 본 연구에서는 침전법을 사용한 Ba-, Pb-계 전자세라믹스의 분말합성에 대한 이론적 고찰과 공정개발 및 실험을 통한 물성증진 효과에 대해 알아보았다. 본 실험상의 전자세라믹스 조성은 강유전체, 세라믹반도체, 압효과에 대해 알아보았다. 본 실험상의 전자세라믹스 조성은 강유전체, 세라믹 반도체, 압전재료로 널리 사용되는 BaTiO3, PZT(PbZrO3-PbTiO3)와 수직 자기기록매체로 큰 가능성이 있으며 hard ferrite로 널리쓰이는 Ba-feerite(BaFe12O19)로써 수산화물 형태의 침전에 대한 기구(mechanism)와 물성에 대해 살펴보았다. 이러한 침전법에 의한 분말합성 과정에는 소결체의 물성에 영향을 미치는 pH 조절제나 원료에서 혼입될 수 있는 Na+, K+, Cl-, SO4- 등의 제거(washing 혹은 filtering)가 필수적이다. 그러나 침전법에서 얻게 되는 분말은 매우 미세하여 colloid를 형성하게 되며, 이러한 colloid 상태의 미세한 침전입자가 filtering media에 끼이게 되어 견고하면서도 상당한 부피를 가지는 filter cake을 형성하기 때문에 filtering에 많은 시간과 다량의 filtering agent (본 실험의 경우엔 증류수)가 필요하게 된다. 따라서 이러한 문제점을 해결하기 위하여 colloid 상태의 침전물을 얼렸다 녹이는 freezing process를 개발, 적용하여 그 원리 및 효과, 그로인한 분말형태를 관찰하여 보았다.

• Korean Journal of Optics and Photonics
• /
• v.16 no.2
• /
• pp.168-173
• /
• 2005

Ag-doped $TiO_2$ thin films were prepared by RF magnetron co-sputtering method, and their physical and chemical properties were examined as a function of calcination temperature. XRD results showed that the crystallite size of Ag-doped films was smaller than that of the $TiO_2$ thin films. SEM results showed that the particle size of $Ag/TiO_2$ film was smaller and more uniform than pure $TiO_2$ film. The films had high transparency in the visible range. The films calcined at $600^{\circ}C$ were the anatase phase, and the films calcined at $900^{\circ}C$ were a mixture of anatase and rutile phases. The absorption edge of films calcined at $900^{\circ}C$ was red-shifted. This is due to the augmented absorption resulting from the phase transformation from anatase to rutile phase. And the transmittance of films decreased by the light scattering and absorption in the films. Photocatalytic activity of $Ag/TiO_2$ thin films was higher than that of the pure $TiO_2$ thin films.

• Journal of the Mineralogical Society of Korea
• /
• v.22 no.4
• /
• pp.371-383
• /
• 2009

Crystallinity and textural relations, which are crucial in terms of the quality concept of high-purity limestone, have not been effectively applicable to the limestone evaluation as crude ore due to the difficulties in precise measurements. To overcome the above, as a new method of ore characterization, a measurement of shape factor and grain boundary frequency utilizing the image analysing system was adopted in this study. Some domestic limestones used for lime manufacturing were investigated by such a quality evaluation method, and its results are discussed and correlated each other samples. As the result, even though calcite contents of crude ore, i.e., limestone grade and its crystal size are similar, quality of manufactured lime is remarkably different depending on the degree of shape factor and grain boundary frequency. In other words, as the more irregular in crystal shape and the higher the grain boundary frequency, the manufactured quick lime became more superior in all terms of lime quality such as rate of calcination, porosity, reactivity, sintering and decrepitation effect. However, because the quick lime become easily overheated in case of relatively higher degree in shape factor and grain boundary effect, a technology minimizing heating time is necessary for the manufacturing of high quality lime. In limestone industry, such a ore characterization method will be much more reasonable than the conventional method by measurement of mean size, because the method may collectively comprise crystal shape and other textural factors which can not be numerically evaluated in the past.

• Transactions of the Korean hydrogen and new energy society
• /
• v.27 no.5
• /
• pp.517-525
• /
• 2016

The present work investigates the effect of $K_2CO_3$ catalyst on steam gasification of Kideco coal and the deactivation of the catalyst due to thermal exposure and interaction with coal ash. The gasification reactivity at $700^{\circ}C$ is highly enhanced by $K_2CO_3$, which is not deactivated by the heat treatment at $T{\leq}800^{\circ}C$. TGA and XRD results prove minor decomposition of $K_2CO_3$ after the calcination at $800^{\circ}C$. $K_2CO_3$ is, however, evaporated at the higher temperature. Assuming the conversion of $K_2CO_3$ into $K_2O$ by the decomposition and into $K_2O{\cdot}2.5SiO_2$ and $KAlO_2$ by the interaction with coal ash, the reactivity of the gasification is evaluated in the presence of $K_2O$, $K_2O{\cdot}2.5SiO_2$ and $KAlO_2$. Among them, $K_2O$ is the most active, but much lower in the activity than $K_2CO_3$. XRD results show that $K_2CO_3$ could react readily with the ash above $700^{\circ}C$.

• Korean Chemical Engineering Research
• /
• v.54 no.2
• /
• pp.152-156
• /
• 2016

Experimental research on the preparation of photocatalyst for the decomposition of brilliant blue FCF ($C_{37}H_{31}O_9N_2S_3Na_2$) was performed. $TiO_2$ and ZnO powders were prepared from titanium (IV) sulfate and zinc acetate at low reaction temperature and atmospheric pressure by hydrothermal precipitation method without calcination. In addition, $TiO_2$ was prepared with cationic surfactant CTAB (Hexadecyltrimethyl ammonium bromide) at the same conditions. The physical properties of prepared $TiO_2$ and ZnO, such as crystallinity, average particle size and absorbance, were investigated by XRD, Zeta-potential meter and DRS. And, the photocatalytic degradation of brilliant blue FCF has been studied in the batch reactor under UV radiation. For the photocatalysts prepared without CTAB, $TiO_2$ has smaller particle size and larger absorbance and photocatalytic reaction rate than ZnO. And $TiO_2$, prepared with CTAB whose concentration is 1/10 of that of precursor, shows 15% higher than that prepared without CTAB in final photocatalytic degradation ratio of brilliant blue FCF.