• Korean Journal of Materials Research
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• v.13 no.4
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• pp.251-258
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• 2003

The effects of the salt and the precursor pH on the synthesizing behavior and the morphology of mullite have been studied. Two kinds of mullite precursor sols were prepared by the dissolution of two kinds of salt (aluminum nitrate enneahydrate, Al($NO_3$)$_3$ㆍ$9H_2$O; type I and aluminum sulfate 14∼18 water, (SO$Al_4$)$_3$$\cdot$$14∼18H_2$O; type II) into the mixture of colloidal silica sol, respectively. Precursor pH of the sols was controlled to the acidic (pH= 1.5∼2) and basic (pH= 8.5∼9) conditions. The co-products with nitrate and sulfate were completely eliminated at $500^{\circ}C$ and $850^{\circ}C$, respectively, which was confirmed by TG/DTA results. The synthesizing temperature of mullite phase was found to be above $1200^{\circ}C$ for pH= 1.5∼2 and above $1300^{\circ}C$ for pH= 8.5∼9 in type I. However, in type II, the synthesizing temperature of mullite was decreased to $850^{\circ}C$ for pH= 1.5∼2 and $1100^{\circ}C$ for pH= 8.5∼9. The grain size of the mullite synthesized at pH= 8.5∼9 was larger than that at pH= 1.5∼2 in overall heat-treated temperatures, showing smaller grain size in type II. Aspect ratio of the mullite grains was more increased at pH= 1.5∼2 than pH= 8.5∼9 in type I, showing similar aspect ratio at both pH conditions in type II. It was found that the synthesizing temperature and grain size were predominantly governed by the initial precursor pH and decomposition of the salt, with minor effect on the grain morphology.

• Korean Journal of Materials Research
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• v.10 no.12
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• pp.845-852
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• 2000

Mesoporous ${\gamma}-Al_2O_3$ has been prepared by selective leaching of silica from calcined domestic kaolinite. From XRD and TG-DTA data, it was found that the microstructure of a spinel phase, consisting of ${\gamma}-Al_2O_3$ containing a small mount of amorphous silica, was obtained by calcining kaolinite samples at around $1000^{\circ}C$ for 24h. Porous ${\gamma}-Al_2O_3$ was prepared by selectively dissolving the amorphous silica in KOH solutions of 1~4M at temperatures of $25~90^{\circ}C$ for leaching time of 0.5~4h. In the case of the ${\gamma}-Al_2O_3$ obtained upon KOH treatment of 4M at $90^{\circ}C$ for 1h, it showed a very narrow unimodal pore size distribution, and also formed much mesopore at a diameter of around $40~80{\AA}$. The specific surface area was $250\textrm{m}^2/g$ and the total pore volume was $0.654\textrm{cm}^3/g$.

• Korean Journal of Materials Research
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• v.22 no.11
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• pp.620-625
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• 2012

A general synthetic method to make $Fe_3O_{4-{\delta}}$ (activated magnetite) is the reduction of $Fe_3O_4$ by $H_2$ atmosphere. However, this process has an explosion risk. Therefore, we studied the process of synthesis of $Fe_3O_{4-{\delta}}$ depending on heat-treatment conditions using $FeC_2O_4{\cdot}2H_2O$ in Ar atmosphere. The thermal decomposition characteristics of $FeC_2O_4{\cdot}2H_2O$ and the ${\delta}$-value of $Fe_3O_{4-{\delta}}$ were analyzed with TG/DTA in Ar atmosphere. ${\beta}-FeC_2O_4{\cdot}2H_2O$ was synthesized by precipitation method using $FeSO_4{\cdot}7H_2O$ and $(NH_4)_2C_2O_4{\cdot}H_2O$. The concentration of the solution was 0.1 M and the equivalent ratio was 1.0. ${\beta}-FeC_2O_4{\cdot}2H_2O$ was decomposed to $H_2O$ and $FeC_2O$4 from $150^{\circ}C$ to $200^{\circ}C$. $FeC_2O4$ was decomposed to CO, $CO_2$, and $Fe_3O_4$ from $200^{\circ}C$ to $250^{\circ}C$. Single phase $Fe_3O_4$ was formed by the decomposition of ${\beta}-FeC_2O_4{\cdot}2H_2O$ in Ar atmosphere. However, $Fe_3C$, Fe and $Fe_4N$ were formed as minor phases when ${\beta}-FeC_2O_4{\cdot}2H_2O$ was decomposed in $N_2$ atmosphere. Then, $Fe_3O_4$ was reduced to $Fe_3O_{4-{\delta}}$ by decomposion of CO. The reduction of $Fe_3O_4$ to $Fe_3O_{4-{\delta}}$ progressed from $320^{\circ}C$ to $400^{\circ}C$; the reaction was exothermic. The degree of exothermal reaction was varied with heat treatment temperature, heating rate, Ar flow rate, and holding time. The ${\delta}$-value of $Fe_3O_{4-{\delta}}$ was greatly influenced by the heat treatment temperature and the heating rate. However, Ar flow rate and holding time had a minor effect on ${\delta}$-value.

• Korean Journal of Materials Research
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• v.19 no.3
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• pp.163-168
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• 2009

$Eu^{3+}$-doped $Y_2O_3$ red phosphor was synthesized in a flux method using the chemicals $Y_2O_3,\;Eu_2O_3,\;H_3BO_3$ and $BaCl_2{\cdot}2H_2O$. The effect of a flux addition on the preparation of $Y_2O_3:Eu_{3+}$ red phosphor used as a cold cathode fluorescence lamp was investigated. $H_3BO_3$ and $BaCl_2{\cdot}2H_2O$ fluxes were used due to their different melting points. The crystallinity, thermal properties, morphology, and emission characteristics were measured using XRD, TG-DTA, SEM, and a photo-excited spectrometer. Under UV excitation of 254 nm, $Eu_2O_3$ 3.7 mol% doped $Y_2O_3$ exhibited a strong narrow-band red emission, peaking at 612 nm. From this result, the phosphor synthesized by firing $Y_2O_3$ with 3.7 mol% of $Eu_2O_3$, 0.25 mol% of $H_3BO_3$ and 0.5 mol% of $BaCl_2{\cdot}2H_2O$ fluxes at $1400^{\circ}C$ for 2 hours had a larger particle size of $4{\mu}m$ on average compared to the phosphor of the $H_3BO_3$ flux alone. In addition, a phosphor synthesized by the two fluxes together had a rounder corner shape, which led to the maximum emission intensity.

• Journal of the Korean Magnetics Society
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• v.2 no.1
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• pp.29-36
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• 1992

The fundamental research about the amorphous ferrite, which is expected as the important material for electronic and information imdustry in future, was carried out in this work. Because the ferromagnetic amorphous ferrites reported recently are very inferior in magnetic properties than the crystalline ferrites, the development of the more ferromagnetic amorphous ferrites is required. In order to obtain the fundamental data for the preparation of amorphous ferrites, the hand-made twin-roller quenching apparatus was used for rapid quenching. Investigation on amorphous ferrite in the system $CaO-Bi_{2}O_{3}-Fe_{2}O_{3}$ has been carried out in the composition of 10-50 mole% CaO, 10-50 mole% $Bi_{2}O_{3}$, 40-70 mole% $Fe_{2}O_{3}$. Large magnetization values were obtained near the composition of the mixture of $BiFeO_{3}$ and $CaFe_{4}O_{7}$. Especially, an amorphous ${(CaO)}_{20}{(Bi_{2}O_{3})_{15}{(Fe_{2}O_{3})}_{65}$ specimen has a magmetization value of about 21.84 emu/g at 0K(10 kOe). Fe $M\"{o}ssbauer$ absorption spectrum indicates that this specimen is compsed of two amorphous phases, antiferromagnetic phase($\alpha$-phase) and ferromagnetic phase($\beta$-phase). Crystallization of this amorphous ferrite was happened in steps-$550^{\circ}C$ and $775^{\circ}C$, then observed crystal phases were perovskite phase of $BiFeO_{3}$ and $Fe_{2}O_{3}$ phase.

• Journal of the Korean Chemical Society
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• v.64 no.5
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• pp.249-258
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• 2020

The potential use of egg shell and calcined egg shell as adsorbent was evaluated and compared to remove Cd²⁺ from aqueous solution. The samples were characterized using Thermogravimetry and Differential Thermal Analysis (TG/DTA), Scanning Electron Microscope (SEM), X-ray Diffractometer (XRD), Energy Dispersive X-ray Spectrometer (EDX) and BET Surface Analyzer. The batch-type adsorption experiment was conducted by varying diverse variables such as contact time, pH, initial Cd²⁺ concentrations and adsorbent dosage. The results showed that, under the initial Cd²⁺ concentrations ranged from 25 to 200 mg g^-1, the removal efficiencies of Cd²⁺ by egg shell powder (ESP) were decreased steadily from 96.72% to 22.89% with increase in the initial Cd²⁺ concentration at 2.5 g of dosage and 8 h of contact time. However, on the contrary to this, calcined egg shell powder (CESP) showed removal efficiencies above 99% regardless of initial Cd²⁺ concentration. The difference in the adsorption behavior of Cd²⁺ may be explained due to the different pH values of ESP and CESP in solution. Cd²⁺ seems to be efficiently removed from aqueous solution by using the CESP with a basicity nature of around pH 12. It was also observed that an optimum dosage of ESP and CESP for nearly complete removal of Cd²⁺ from aqueous solution is approximately 5.0 g and 1.0 g, respectively. Consequently, Cd²⁺ is more favorably adsorbed on CESP than ESP in the studied conditions. Adsorption data were applied by the pseudo-first-order and pseudo-second-order kinetics models and Freundlich and Langmuir isotherm models, respectively. With regard to adsorption kinetics tests, the pseudo-second-order kinetics was more suitable for ESP and CESP. The adsorption pattern of Cd²⁺ by ESP was better fitted to Langmuir isotherm model. However, by contrast with ESP, CESP was described by Freundlich isotherm model well.

• Journal of the Korea Institute of Building Construction
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• v.18 no.3
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• pp.203-210
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• 2018

Corrosion of the rebar is one of the main factors affecting the durability of reinforced concrete in the world which lead to the failure of the reinforced concrete structures. In this research, a new method of fixing $CO_2$ is practiced to improve the carbonation resistance of the concrete. Brucite($Mg(OH)_2$), a kind of common $CO_2$ fixation materials, was added into ordinary Portland cement paste. Samples containing 0%, 5%, 10%, and 15% $Mg(OH)_2$ were exposed to an accelerated carbonation curing regime with 20% concentration of $CO_2$, 60% relative humidity, and a temperature of $20^{\circ}C$ until tested at 3d, 7d, 14d and 28d. After 28d of $CO_2$ accelerated curing, in the paste containing $Mg(OH)_2$, magnesian calcite was detected by SEM-EDX. Meanwhile, the paste containing $Mg(OH)_2$ exhibit the better pore distribution than ordinary Portland cement paste and the compressive strength of the cement paste containing $Mg(OH)_2$ were more than 50Mpa.

• Journal of the Mineralogical Society of Korea
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• v.4 no.1
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• pp.1-10
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• 1991

Tosudite from the Sungsan mine, Korea is an alteration product of rhyolitic tuff in the cretaceous Hwangsan Formation. It is associated with illite, dickite, nacrite or quartz and also found in the cavities of black claystone. X-ray diffraction and chemical analyses show that the Sungsan tosudite is a lithium-bearing aluminous 1:1 regularly interstratified mineral of di, dioctahedral chlorite and smectite. Its structural formula is $(K_{0.73}Na_{0.02}Ca_{0.07})(Si1_{13.23}Al_{2.77})(Li_{0.52}Mg_{0.08}Mn_{0.01)Fe^{3+}_{0.07}Al_{12.33})O_{40}(OH)_{20}$ and it suggests that Sungsan tosudite consists of regularly interstratified Li-donbassite and beidellite. DTA and TG curves as well as IR absorption data also support such a result. Temperature of formation of tosudite is inferred to be between $110{\circ}$ and $270{\circ}C$.

• Journal of the Mineralogical Society of Korea
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• v.30 no.4
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• pp.179-186
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• 2017

This study investigated the mineralogical characteristics of lime mortars used in pointing of Namhansanseon Yeojang from Joseon dynasty. Polarization microscopy revealed quartz, feldspar, mica, pyroxene and opaque minerals in the lime mortars. XRD analysis also confirmed clay minerals chlorite and kaolin. As a result of particle size analysis of lime mortars, the particle size distribution was wide and size was not uniform. 60% of samples were corresponded to the sand area. The chemical components detected from XRF analysis, 8.71-11.18 % of Ca as the main component of lime and $SiO_2$, $Al_2O_3$, and $Fe_2O_3$ in soil minerals were main components. The lime mortars showed an endothermic peak due to decarbonization reaction of $CaCO_3$ at $750^{\circ}C$ and weight reduction rate of 10%. The microstructures were agglomerated amorphous and observed rhombohedral calcite crystals by scanning electron microscope. It is considered that the pointing of Yeojang is a mortar mixed with lime and soil. In addition the Hanbongseong Yeojang was constructed using the same materials and construction technique because the minerals composition is not different according to the Yeojang location and use.

• Korean Journal of Materials Research
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• v.22 no.7
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• pp.346-351
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• 2012

$Li_{1+x}Al_xTi_{2-x}(PO_4)_3$(LATP) is a promising solid electrolyte for all-solid-state Li ion batteries. In this study, LATP is prepared through a sol-gel method using relatively the inexpensive reagents $TiCl_4$. The thermal behavior, structural characteristics, fractured surface morphology, ion conductivity, and activation energy of the LATP sintered bodies are investigated by TG-DTA, X-ray diffraction, FE-SEM, and by an impedance method. A gelation powder was calcined at $500^{\circ}C$. A single crystalline phase of the $LiTi_2(PO_4)_3$(LTP) system was obtained at a calcination temperature above $650^{\circ}C$. The obtained powder was pelletized and sintered at $900^{\circ}C$ and $1000^{\circ}C$. The LTP sintered at $900{\sim}1000^{\circ}C$ for 6 h had a relatively low apparent density of 75~80%. The LATP(x = 0.3) pellet sintered at $900^{\circ}C$ for 6 h was denser than those sintered under other conditions and showed the highest ion conductivity of $4.50{\times}10^{-5}$ S/cm at room temperature. However, the ion conductivity of LATP (x = 0.3) sintered at $1000^{\circ}C$ decreased to $1.81{\times}10^{-5}$ S/cm, leading to Li volatilization and abnormal grain growth. For LATP sintered at $900^{\circ}C$ for 6 h, x = 0.3 shows the lowest activation energy of 0.42 eV in the temperature range of room temperature to $300^{\circ}C$.