• 대한화학회지
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• 제30권2호
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• pp.231-236
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• 1986

수소크롬산이온에 의한 $[Mo_2O_4(C_2O_4)_2(OH_2)_2]^{2-}$의 산화는 $[Mo_2O_5(C_2O_4)_2(OH_2)_2]^{2-}$를 생성한다. 수소크롬산이온과 $[Mo_2O_4(C_2O_4)_2(OH_2)_2]^{2-}$의 반응에 대한 화학양론은 ${3Mo_2}^V+2Cr^{VI}\;{\rightleftharpoons}\;{3Mo_2}_{VI}+2Cr^{III}$와 같다. 관찰된 속도상수는 $[H+]^2$에 의존한다. $Cr^{VI}$는 Cr^V$와 $Cr^{IV}$를 거쳐서 $Cr^{III}$로 일전자씩 연속적으로 변화한다. 이들 반응에 대한 상세한 메카니즘이 제시되며 이에 대해서 논의된다.

• 한국세라믹학회지
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• 제34권10호
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• pp.1083-1091
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• 1997

반응성이 좋은 미분말의 고온 초전도상을 얻고자 액상 합성법 중의 하나인 옥살산염법을 이용하였다. 본 방법을 사용하여 합성 분체의 초기 형상과 입도를 제어하였고, 개선된 균일성을 가진 Bi(Pb)-Sr-Ca-Cu-O 초전도 분말을 제조할 수 있었다. 합성된 산화물 초전도체 분말의 특성 및 pellct으로 성형후 열처리한 시편의 미세구조와 전기적특성을 조사하였다. 또한, Tape casting법에 의해 후막을 제작하여 미세구조와 전기적 특성을 관찰하였다. 합성된 분말의 입자 크기는 100~300nm 이하의 구형이었으나 대부분이 1~3 ${\mu}{\textrm}{m}$ 크기로 응집되어 있었다. 84$0^{\circ}C$로 72시간 동안 열처리한 괴상 시편의 임계저항온도는 110K였으며, 열처리한 후막의 임계전류는 각각 0.6A, 1.9A였다.

• 방사성폐기물학회지
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• 제19권2호
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• pp.187-196
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• 2021

Chemical equilibrium calculations for multicomponent aqueous systems involving the reductive dissolution of magnetite (Fe₃O₄) with oxalic acid (H₂C₂O₄) were performed using the HSC Chemistry® version 9. They were conducted with an aqueous solution model based on the Pitzer's approach of one molality aqueous solution. The change in the amounts and activity coefficients of species and ions involved in the reactions as well as the solution pH at equilibrium was calculated while changing the amounts of raw materials (Fe₃O₄ and H₂C₂O₄) and the system temperature from 25℃ to 125℃. In particular, the conditions under which Fe₃O₄ is completely dissolved at high temperatures were determined by varying the raw amount of H₂C₂O₄ and the temperature for a given raw amount of Fe₃O₄ fed into the aqueous solution. When the raw amount of H₂C₂O₄ added was small for a given raw amount of Fe₃O₄, no undissolved Fe₃O₄ was present in the solution and the pH of the solution increased significantly. The formation of ferrous oxalate complex (FeC₂O₄) was observed. The equilibrium amount of FeC₂O₄ decreased as the raw amount of H₂C₂O₄ increased.

• 한국결정성장학회지
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• 제4권3호
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• pp.252-261
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• 1994

본 연구는 수산염법에 의해 화학적으로 균일하며 고순도인 미립의 $(Ba_{1-X}Sr_X)ZrO_3$ 분말을 합성하고 합성된 분말의 미세구조와 유전특성을 조사하여 공진주파수의 온도계수$({gamma}_f)$가 안정한 $(Ba_{1-x}Sr_x)Zr0_3$의 최적 합성조건을 규명하고자 하였다. 6가지 조성의 $(Ba{_1-X}Sr_x)ZrO_3$ (X=0, 0.2, 0.4, 0.6, 0.8, 1) 화합물을 수산염법으로 얻은 후 이를 $1000^{\circ}C$에서 하소하여 결정질 $(Ba_{1-X}Sr_X)ZrO_3$ 분말을 합성하였다. 합성한$(Ba_{1-x}Sr_x)Zr0_3$ 분말은 구형으로 $0.2 {mu}m$이하의 평균 입경을 가졌으며, ${\tau}_c$는 Ba에 대해 Sr이 0.5 정도 치환된 조성에서 0이 되는 조성을 유추할 수 있었다.

• 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.

• Korean Chemical Engineering Research
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• 제55권6호
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• pp.785-790
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• 2017

To collect zinc, Fe and Zn in spent pickling solution were extracted by using TBP (tributyl phosphate), and Zn was recovered from extracted solution to zinc oxalate particles by oxalic acid solution. The reusability of TBP solvent was also tested. The distribution coefficient of Zn was not affected by the concentration of Fe in spent pickling solution, almost constant with the values of 7.12~9.31 when extracted by TBP solvent. It was found that the extraction capacity of TBP solvent for Zn is higher than that for Fe. The extraction efficiency of Zn was higher than 95%, while most of Fe was left in aqueous phase. After the recovery, the used TBP solvent could be repeatedly reused for the extraction of Zn up to eight times. XRD analysis showed that zinc oxalate ($ZnC_2O_4$ $2H_2O$) was formed from the reaction of Zn-TBP and oxalic acid. From the results of SEM analysis, the formation of zinc oxalate particle was strongly affected by the concentration of oxalic acid. In summary, Zn in spent pickling solution was successfully separated and recovered with TBP solvent and oxalic acid solution, respectively.

• 한국전기전자재료학회논문지
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• 제14권11호
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• pp.904-911
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• 2001

High-density lead zirconate titanate(Pb(Zr$\_$0.53/Ti$\_$0.47/)O$_3$, PZT) ceramics were fabricated by a new milling-precipitation(MP) process improved from the conventional solid state process. This process was progressed by a milling impregnation through mixing ZrO$_2$ and TiO$_2$ powders with lead nitrate(Pb(NO$_3$)$_2$) water solution in zirconia ball media, and then milling precipitation was induced from precipitation of PbC$_2$O$_4$ by adding ammonium of oxalate monohydrate((NH$_4$)$_2$C$_2$O$_4$$.$H$_2$O) as a precipitant. As a result of this process, single-phase perovskite structure was formed at the calcination temperature of 750$\^{C}$ for Pb(Zr$\_$0.53/Ti$\_$0.47/)O$_3$ powders. In addition, the highest density at the sintering temperature of 1100$\^{C}$ was obtained, because of the highly sinterable PZT Powders ground through the re-milling process. Piezoelectric and dielectric properties of sintered sample were improved by MP process.

• 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 $O_2$.

• 자원리싸이클링
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• 제12권1호
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• pp.33-40
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• 2003

약 90%의 $Mn_3$$O_4$를 함유하는 고탄소폐로망간을 중저탄소폐로망간으로 제조하는 과정의 bag filter에 채집된 분진에는 소량의 Na, K, Fe, Si, Ca, Mg등의 불순물이 함유된다. 환원배소로 망간을 MnO의 상태로 만든 분진을 질산으로 침출하여 고농도 망간 침출액을 조제하고, 조제된 침출액에서 불순물을 제거하기 위한 기초실험을 하였다. 침출액중의 철 성분은 침출액의 pH를 4 이상으로 하여 수산화철 침전을 생성시킨 다음 여과에 의해 제거하므로써 여액 내의 잔류농도가 수ppm 이하가 되도록 하였고, 이 때 규소성분도 수산화철과 함께 공침시켜 10ppm 이하로 제거하였다. 4N의 질산을 사용하는 경우 질산 $1ell$ 대하여 환원된 분진 150g을 첨가하면 침출액의 pH가 4이상으로 되어 철과 규소 성분이 제거된 Mn농도가 약 10%인 침출액을 조제 할 수 있었다. 그리고 Ca 와 Mg를 옥살산염 형태로 침전시켜 제거할 목적으로 수행한 단일 옥살산염 수용액에서의 Mn과 Ca, Mg의 용해 및 침전 특성 조사에서는 수용액의 온도가 높을수록 반응속도가 빨라져 Mg의 제거에 유리하며, pH가 낮을수록 고농도의 Mn용액을 얻을 수 있으며 이 때 용액내의 Ca/Mn 및 Mg/Mn은 pH에 관계없이 일정하였다.

• 한국세라믹학회지
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• 제20권2호
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• pp.107-114
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• 1983

Formation of Strontium titanate from the products of coprecipitation takes place at 110$0^{\circ}C$ which is 200-30$0^{\circ}C$ lower than that from mechanical mixtures of $SrCO_3$ and $TiO_2$. This is apparently due to the nature of the compounds formed by the reaction of mixtures of aqueous solutions of $SrCl_2$ and $TiCl_4$ with an ammoniacal solution of ammoni-um carbonate and ammonium hydroxide. A procedure is described for preparing strontium titanyl oxalate tetrahydrate in the several mole ratio of $TiCl_4$ to $SrCl_2$. STrontium titanyl oxalates decompose to titanate at elevated temperature. The coprecipitates and the fired specimen were subjected to examined thermal and X-ray analyses and microstruc-ture by SEM.