• 제목/요약/키워드: $\DeltaO_3$ value

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FeC2O4·2H2O의 열처리 조건이 Fe3O4-δ 형성에 미치는 영향 (Effects of Heat Treatment Conditions of FeC2O4·2H2O on the Formation of Fe3O4-δ)

  • 오경환;박원식;이상인;서동수
    • 한국재료학회지
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    • 제22권11호
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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.

N2분위기에서 FeC2O4·2H2O의 열분해에 의한 Fe3O4-δ합성 (Synthesis of Fe3O4-δ Using FeC2O4·2H2O by Thermal Decomposition in N2 Atmosphere)

  • 박원식;오경환;안석진;서동수
    • 한국재료학회지
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    • 제22권5호
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    • pp.253-258
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    • 2012
  • Activated magnetite ($Fe_3O_{4-{\delta}}$) was applied to reducing $CO_2$ gas emissions to avoid greenhouse effects. Wet and dry methods were developed as a $CO_2$ removal process. One of the typical dry methods is $CO_2$ decomposition using activated magnetite ($Fe_3O_{4-{\delta}}$). Generally, $Fe_3O_{4-{\delta}}$ is manufactured by reduction of $Fe_3O_4$ by $H_2$ gas. This process has an explosion risk. Therefore, a non-explosive process to make $Fe_3O_{4-{\delta}}$ was studied using $FeC_2O_4{\cdot}2H_2O$ and $N_2$. $FeSO_4{\cdot}7H_2O$ and $(NH_4)_2C_2O_4{\cdot}H_2O$ were used as starting materials. So, ${\alpha}-FeC_2O_4{\cdot}2H_2O$ was synthesized by precipitation method. During the calcination process, $FeC_2O_4{\cdot}2H_2O$ was decomposed to $Fe_3O_4$, CO, and $CO_2$. The specific surface area of the activated magnetite varied with the calcination temperature from 15.43 $m^2/g$ to 9.32 $m^2/g$. The densities of $FeC_2O_4{\cdot}2H_2O$ and $Fe_3O_4$ were 2.28 g/$cm^3$ and 5.2 g/$cm^3$, respectively. Also, the $Fe_3O_4$ was reduced to $Fe_3O_{4-{\delta}}$ by CO. From the TGA results in air of the specimen that was calcined at $450^{\circ}C$ for three hours in $N_2$ atmosphere, the ${\delta}$-value of $Fe_3O_{4-{\delta}}$ was estimated. The ${\delta}$-value of $Fe_3O_{4-{\delta}}$ was 0.3170 when the sample was heat treated at $400^{\circ}C$ for 3 hours and 0.6583 when the sample was heat treated at $450^{\circ}C$ for 3 hours. $Fe_3O_{4-{\delta}}$ was oxidized to $Fe_3O_4$ when $Fe_3O_{4-{\delta}}$ was reacted with $CO_2$ because $CO_2$ is decomposed to C and $O_2$.

활성화된(Fe1-xMnx)3O4-δ과 (Fe1-xCox)3O4-δ의 이산화탄소 분해 특성 (CO2 Decomposition Characteristics of Activated(Fe1-xMnx)3O4-δ and (Fe1-xCox)3O4-δ)

  • 박원식;오경환;이상인;서동수
    • 한국재료학회지
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    • 제23권4호
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    • pp.219-226
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    • 2013
  • Activated magnetite ($Fe_3O_{4-{\delta}}$) has the capability of decomposing $CO_2$ proportional to the ${\delta}$-value at comparatively low temperature of $300^{\circ}C$. To enhance the $CO_2$ decomposition capability of $Fe_3O_{4-{\delta}}$, $(Fe_{1-x}Co_x)_3O_{4-{\delta}}$ and $(Fe_{1-x}Mn_x)_3O_{4-{\delta}}$ were synthesized and then reacted with $CO_2$. $Fe_{1-x}Co_xC_2O_4{\cdot}2H_2O$ powders having Fe to Co mixing ratios of 9:1, 8:2, 7:3, 6:4, and 5:5 were synthesized by co-precipitation of $FeSO_4{\cdot}7H_2O$ and $CoSO_4{\cdot}7H_2O$ solutions with a $(NH_4)_2C_2O_4{\cdot}H_2O$ solution. The same method was used to synthesize $Fe_{1-x}Mn_xC_2O_4{\cdot}2H_2O$ powders having Fe to Mn mixing ratios of 9:1, 8:2, 7:3, 6:4, 5:5 with a $MnSO_4{\cdot}4H_2O$ solution. The thermal decomposition of synthesized $Fe_{1-x}Co_xC_2O_4{\cdot}2H_2O$ and $Fe_{1-x}Mn_xC_2O_4{\cdot}2H_2O$ was analyzed in an Ar atmosphere with TG/DTA. The synthesized powders were heat-treated for 3 hours in an Ar atmosphere at $450^{\circ}C$ to produce activated powders of $(Fe_{1-x}Co_x)_3O_{4-{\delta}}$ and $(Fe_{1-x}Mn_x)_3O_{4-{\delta}}$. The activated powders were reacted with a mixed gas (Ar : 85 %, $CO_2$ : 15 %) at $300^{\circ}C$ for 12 hours. The exhaust gas was analyzed for $CO_2$ with a $CO_2$ gas analyzer. The decomposition of $CO_2$ was estimated by measuring $CO_2$ content in the exhaust gas after the reaction with $CO_2$. For $(Fe_{1-x}Mn_x)_3O_{4-{\delta}}$, the amount of $Mn^{2+}$ oxidized to $Mn^{3+}$ increased as x increased. The ${\delta}$ value and $CO_2$ decomposition efficiency decreased as x increased. When the ${\delta}$ value was below 0.641, $CO_2$ was not decomposed. For $(Fe_{1-x}Co_x)_3O_{4-{\delta}}$, the ${\delta}$ value and $CO_2$ decomposition efficiency increased as x increased. At a ${\delta}$ value of 0.857, an active state was maintained even after 12 hours of reaction and the amount of decomposed $CO_2$ was $52.844cm^3$ per 1 g of $(Fe_{0.5}Co_{0.5})_3O_{4-{\delta}}$.

$La(Ba)Ga(Mg)O_3_\delta$계 Perovskite 산화물의 생성상 및 산소이온전도 (Phase Formation and Oxygen Ion Conduction of $La(Ba)Ga(Mg)O_3_\delta$ Perovskite Oxide System)

  • 이기태;김신;이홍림
    • 한국세라믹학회지
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    • 제36권10호
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    • pp.1056-1061
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    • 1999
  • Phase formation and oxygen ion conduction of La(Ba)Ga(Mg)O3-$\delta$ system was studied, BaLaGa3O7 and BaLaGaO4 formed as a secondary phase above the solubility limit of Ba2+ in La3+ sites. The oxygen ionic conductivity of La(Ba)Ga(Mg)O3-$\delta$ was 0.1 S/cm 80$0^{\circ}C$ The activation energy of the oxygen ion conduction was dependent on temperature. This value was higher at low temperature than at high temperature.

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전자빔 증발법에 의한 박막형 고온초전도체의 $CeO_2$ 버퍼층 증착 연구 (Research for Deposition of $CeO_2$ Buffer Layer on Coated Conductor by Electron Beam Evaporation)

  • 이종범;박신근;김혜진;문승현;이희균;홍계원
    • Progress in Superconductivity
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    • 제11권2호
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    • pp.123-127
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    • 2010
  • The properties of buffer layer for thermal and chemical stability in coated conductor is a very important issue. $CeO_2$ has desirable thermal and chemical stability as well as good lattice match. In this study, $CeO_2$ was deposited by electron beam deposition. The MgO(001) single crystal and LMO buffered IBAD substrate(LMO/IBAD-MgO/$Y_2O_3/Al_2O_3$/Hastelloy) were used as substrates, which have $\Delta\phi$ values of ${\sim}8.9^{\circ}$. The epitaxial $CeO_2$ films was deposited with high deposition rate of $12{\sim}16\;{\AA}/sec$. During deposition, the change of oxygen partial pressure(${\rho}O_2$) does not cause change in c-axis texture. In case of $CeO_2$ on MgO single crystal, the substrate temperature was optimized at $750^{\circ}C$ with superior $\Delta\phi$ and $\Delta\omega$ value. Otherwise, In case of LMO buffered IBAD substrate, It was optimized at $650^{\circ}C$ with increasing its deposition thickness of $CeO_2$, which was finally obtained with best $\Delta\phi$ value of $5.5^{\circ}$, $\Delta\omega$ value of $2^{\circ}$ and Ra value of 2.2 nm.

Color alterations of a PMMA resin for fixed interim prostheses reinforced with silica nanoparticles

  • Kotanidis, Alexandros;Kontonasaki, Eleana;Koidis, Petros
    • The Journal of Advanced Prosthodontics
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    • 제11권4호
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    • pp.193-201
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    • 2019
  • PURPOSE. The aim of the present study was to evaluate the color changes of an autopolymerizing PMMA resin used for interim fixed restorations, reinforced with $SiO_2$ nanoparticles. MATERIALS AND METHODS. Silica nanoparticles were blended with the PMMA resin powder through high-energy ball milling. Four shades of PMMA resin were used (A3, B3, C3, D3) and total color differences were calculated through the equations ${\Delta}E_{ab}=[({\Delta}L*)^2+({\Delta}a*)^2+({\Delta}b*)^2]^{1/2}$ and ${\Delta}E_{00}=[(\frac{{\Delta}L^{\prime}}{K_LS_L})^2+(\frac{{\Delta}C^{\prime}}{K_CS_C})^2+(\frac{{\Delta}H^{\prime}}{K_HS_H})^2+R_T(\frac{{\Delta}C^{\prime}}{K_CS_C})(\frac{{\Delta}H^{\prime}}{K_HS_H})]^{1/2}$. Statistically significant differences between ${\Delta}E_{ab}$ and the clinically acceptable values of 3.3 and 2.7 and those between ${\Delta}E_{00}$ and the clinically acceptable value of 1.8 were evaluated with one sample t-test (P<.05). Differences among the different shades were assessed through One-Way ANOVA and Bonferroni multiple comparison tests. RESULTS. Significantly lower values were detected for all groups concerning ${\Delta}E_{ab}$ compared to the intraorally clinical acceptable values of 3.3 and 2.7. Significantly lower mean values were detected for groups B3, C3, and D3, concerning ${\Delta}E_{00}$ compared to the intraorally clinical acceptant value of 1.8. Color pigments in red-brown (A3) and red-grey (D3) shades affect the total color change to a greater extent after the reinforcement with $SiO_2$ nanoparticles compared to the red-yellow (B3) shade. CONCLUSION. Within the limitations of this in vitro study, it can be suggested that reinforcing PMMA with $SiO_2$ nanoparticles at 0.25 wt% slightly affects the optical properties of the PMMA resin without being clinically perceivable.

NiZn 페라이트의 저온 소결 특성에 관한 연구 (A Study on Properties of Low Temperature Sintering in the NiZn Ferrite System)

  • 고상기;김병호;김경용
    • 한국세라믹학회지
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    • 제34권10호
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    • pp.1074-1082
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    • 1997
  • Microstructure and permeability as a function of sintering temperature and composition were studied on the Ni$\delta$Cu0.4-$\delta$Zn0.6Fe2O4 ($\delta$=0, 0.1, 0.2, 0.3, 0.4) which was prepared by Cu2+ substitution for Ni2+ in Ni.0.4Zn0.6Fe2O4, then followed by 8 wt% CuO and 1wt% Bi2O3 as sintering aids. It was found that NiCuZn ferrite in which Cu2+ is substituted for Ni2+ is more effective in reduction of sintering temperature than Ni.0.4Zn0.6Fe2O4, containing CuO as a sintering aid. The specimen $\delta$=0.2 sintered at 90$0^{\circ}C$ for 2hr exhibited the highest initial permeability value ($\mu$o=280 at 1Mhz), but the real permeability decreased at the frequency under 10 MHz. EPMA analysis showed that Ni$\delta$Cu0.4-$\delta$Zn0.6Fe2O4 ($\delta$=0.4), sintered at 95$0^{\circ}C$ for 2hrs consisted of three phase regions of Ni.0.3Cu0.1Zn0.6Fe2O4 region, Cu and Bi liquid existed at the 3-point boundary, although the stabilization energy of Ni2+ is higher than that of Cu2+ in B site.

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$Bi_2O_3$ 첨가에 의한 Ca[($Li_{1/3}Nb_{2/3}$)$_{1-x}$$Ti_{x}$$O_{3-{\delta}}$ 세라믹스의 마이크로파 유전 특성 (Microwave Dielectric Properties of Ca[($Li_{1/3}Nb_{2/3}$)$_{1-x}$$Ti_{x}$]$O_{3-{\delta}}$ with $Bi_2O_3$ Additives)

  • 하종윤;최지원;이동윤;윤석진;최두진;김현재
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2002년도 하계학술대회 논문집
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    • pp.131-134
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    • 2002
  • The effect of the addition on the densification, low temperature sintering, and microwave dielectric properties of the Ca[($Li_{1/3}Nb_{2/3}$)$_{1-x}$$Ti_{x}$]$O_{3-{\delta}}$/(CLNT) was investigated. $Bi_2O_3$ additives improved the dencification and reduced the sintering temperature from $1150^{\circ}C$ to $900^{\circ}C$ of CLNT microwave dielectric ceramics. As increasing $Bi_2O_3$ contents, the dielectric constants and bulk density were increased. The quality factor, however, was decreased slighty. The temperature coefficients of the resonant frequency shifted positive value as increasing $Bi_2O_3$ contents. The dielectric properties of Ca[($Li_{1/3}Nb_{2/3}$)$_{1-x}$$Ti_{x}$]$O_{3-{\delta}}$ and Ca[($Li_{1/3}Nb_{2/3}$)$_{0.8}Ti_{0.2}$]$O_{3-{\delta}}$ with 5wt% $Bi_2O_3$ sintered at $900^{\circ}C$ for 3h were $\varepsilon_{r}$=20, 35 Q.$f_{0}$=6500, 11,000 GHz, $\tau_{f}$=4, 13 ppm/$^{\circ}C$, respectively.

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중·저온형 고체산화물 연료전지 공기극 물질로 사용되는 이중층 페로브스카이트와 컴플렉스 페로브스카이트의 전기 전도도 비교 (Comparison of Electrical Conductivities in Complex Perovskites and Layered Perovskite for Cathode Materials of Intermediate Temperature-operating Solid Oxide Fuel Cell)

  • 김정현
    • 한국세라믹학회지
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    • 제51권4호
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    • pp.295-299
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    • 2014
  • Electrical conductivities of complex perovskites, layered perovskite and Sr doped layered perovskite oxides were measured and analyzed for cathode materials of Intermediate Temperature-operating Solid Oxide Fuel Cells (IT-SOFCs). The electrical conductivities of $Sm_{1-x}Sr_xCoO_{3-\delta}$ (x = 0.3 and 0.7) exhibit a metal-insulator transition (MIT) behavior as a function of temperature. However, $Sm_{0.5}Sr_{0.5}CoO_{3-\delta}$ (SSC55) shows metallic conductivity characteristics and the maximum electrical conductivity value compared to the values of $Pr_{0.5}Sr_{0.5}CoO_{3-\delta}$ (PSC55) and $Nd_{0.5}Sr_{0.5}CoO_{3-\delta}$ (NSC55). The electrical conductivity of $SmBaCo_2O_{5+\delta}$ (SBCO) exhibits a MIT at about $250^{\circ}C$. The maximum conductivity is 570 S/cm at $200^{\circ}C$ and its value is higher than 170 S/cm over the whole temperature range tested. $SmBa_{0.5}Sr_{0.5}Co_2O_{5+\delta}$ (SBSCO), 0.5 mol% Sr and Ba substituted at the layered perovskite shows a typically metallic conductivity that is very similar to the behavior of the SSC55 cathode, and the maximum and minimum electrical conductivity in the SBSCO are 1280 S/cm at $50^{\circ}C$ and 280 S/cm at $900^{\circ}C$.

무정광산의 금-은 광화작용 (Gold-Silver Mineralization of the Mujeong Mine, Korea)

  • 김상중
    • 자원환경지질
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    • 제32권3호
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    • pp.237-245
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    • 1999
  • The Mujeong au-Ag hydrothermal vein type deposits occur within the Teriary igneous rocks of the Janggi basin. Ore minerals consist of pyrite, pyrrhotite, sphalertite, chalcopyrite, galena, cosalite, lillianite, argentite and electrum, and associated with epidotization, sericitization and pyritization. Fluid inclusion studies reveal that ore fluids were low saline with a simple NaCl-$H_{2}O$ system. Fluid inclusion data indicate that homogenization temperatures and salinities of fluid are 150 to $340^{\circ}C$ and 1.0 to 6.5wt.% NaCl equivalent, respectively. Sulfur isotope compositions of sulfied minerals ( ${\delta}^{34}S$=6.2 to 9.6$\textperthousand$) indicate that the ${\delta}^{34}S_{H2S}$ value of ore fluids was about 10.4$\textperthousand$. This ${\delta}^{34}S_{H2S}$ value is likely consistent with and hydrothermal sulfur, whereas the fluids were highly influenced by mixing with meteoric water. Measured and calculated oxygen and hydrogen isotope values (${\delta}^{18}O_{H2O}$=-2.7 to 3.4 $\textperthousand$, ${\delta}D_{H2O}$ = -83.6 to -52.7 $\textperthousand$) of ore forming fluids suggest mixing with hydrothermal and meteoric water. Equilibrium thermodynamic interpretation by mineral assemblages and chemistry indicates that sulfur fugacities (-log $fs_2$) ore forming fluids range from 9.0 to 12.6 atm stage II.

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