• 한국분말재료학회지
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• 제10권4호
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• pp.255-261
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• 2003

Ultrafine TaC-5%Co composite powders were synthesized by spray conversion process using tantalum oxalate solution and cobalt nitrate hexahydrate(Co($(NO_3)_2$ . 6$H_2O$). The phase of Ta-Co oxide powders had amorphous structures after calcination below 50$0^{\circ}C$ and changed $Ta_2O_5$, $TaO_2$ and $CoTa_2O_6$ phase by heating above $600^{\circ}C$. The calcined Ta-Co oxide powders were spherical agglomerates consisted of ultrafine primary particles <50 nm in size. By carbothermal reaction, the TaC phase began to form from 90$0^{\circ}C$. The complete formation of TaC could be achieved at 105$0^{\circ}C$ for 6 hours. The observed size of TaC-Co composite powders by TEM was smaller than 200 nm.

• Bulletin of the Korean Chemical Society
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• 제14권1호
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• pp.38-42
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• 1993

Factor analysis was applied to study the thermal decomposition of barium titanyl oxalate (BTO) which is used as the precursor of barium titanate. BTO was synthesized in $H_2O$ solvent and calcined at various temperatures. The X-ray diffraction patterns were obtained to make the data matrix of peak intensity vs. 2${\theta}$. Abstract factor analysis and target transformation factor analysis were applied to this data matrix. It has been found that the synthesized BTO consists of the crystals of $BaC_2O_4{\cdot}0.5H_2O\;and\;BaC_2O_4{\cdot}2H_2O$ as well as the amorphous solid of TiO-oxalate. The results also indicate that the BTO was transformed via $BaCO_3\;to\;BaTiO_3\;and\;Ba_2TiO_4$ during the thermal decomposition.

• 한국해양공학회지
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• 제11권1호
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• pp.44-48
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• 1997

During studies of the ripening reaction of titanium oxalate, a new crystalline phase has been found. The crystal system was determined to be orthormbic with space group $C222_1$. The unit cell parameters were refined to a=10.503(2)$\AA$ b=15.509(3)$\AA$ c=9.7000(1)$\AA$. The chemical formula of the crystal is Ti$_{2}$O$_{2}$(C$_{2}$O$_{4}$)(OH)$_{2}$. H$_{2}$O. When heated to temperatures between 31$0^{\circ}C$ and 38$0^{\circ}C$, the material became amorphous. Heated above 41$0^{\circ}C$ converted it into anatase-type titanium dioxide.

• 대한화학회지
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• 제33권1호
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• pp.65-69
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• 1989

방사성 바륨 또는 방사성 란탄 추적자를 함유하고 있는 Ba(NO$_3)_2$ 와 TiO(NO$-3)_2$의 무기혼합용액을 옥살산의 에탄올 용액으로 적정하므로써 바륨티탄닐의 옥살산 염을 합성하였고, 이를 1000$^{\circ}$C에서 하소시켜 BaTiO$_3$를 만들었다. 옥살산염의 분석결과는 BaTiO(C$_2O_4)_2{\cdot}4H_2O$이며, 무기혼합용액중 Ba/Ti의 몰비가 0.950∼1.05 범위 내에서 화학양론적 결합으로 합성됨을 방사성 바륨 추적자의 도움으로 쉽게 확인하였고, Perovskite형의 구조임을 XRD로 확인하였다. 그리고 란탄 첨가제가 침전에 화학적으로 균일하게 혼입됨은 방사성 란탄의 추적자 실험으로 발견하였다. 이와 같은 실험적 사실로부터 침전물의 구성 성분의 결합이 분자준위에서 일어나고 또 티탄산바륨이 단일상의 결정임을 설명하였다.

• 한국세라믹학회지
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• 제27권2호
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• pp.274-282
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• 1990

SnO2 powder was prepared by hydroxide method and oxalate method. In hydroxide method, the pH dependence of powder characteristics was investigated by using buffer solution. As increasing the pH of solution, SnO2 powder size was decreased because nucleation rate was inctreased by more supersaturation of solution. Also, we found that the powder by our method has larger specific surface area in comaprison with other method. And the degree of agglomeration of precipitate with the change of precipitation temperature was investigated in oxalate method. The SnC2O4 was angular shape precipitate, and the size of the SnC2O4 was increased with the increase of precipitation temperature in methanol solvent.

• 한국세라믹학회지
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• 제47권2호
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• pp.183-188
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• 2010

$Ce_{0.8}Gd_{0.2}O_{1.9}$(GDC20) powder was synthesized by milling of $CeO_2$ slurry and Gd oxalate precipitation. The mixture of $CeO_2$ powder and Gd precipitates calcined at $600^{\circ}C$ for 2 h showed the particle size distribution similar to that of $CeO_2$ powder, which had been milled during the synthesis process. Attrition milling of the calcined powder with an average particle size of $0.36\;{\mu}m$ for 2 h resulted in a decrease in the particle size to $0.24\;{\mu}m$. Although the milled powder consisted of small particles(<$1\;{\mu}m$), a small amount of fine platy $Gd_2O_3$ particles, which had been survived in the milling process, was observed. Sintering of the powder compacts for 4 h showed relative densities of 80.7% at $1300^{\circ}C$ and 97% at $1400^{\circ}C$, respectively. Densification was found to almost complete at $1500^{\circ}C$, resulting in a dense and homogeneous microstructure with a relative density of 99.5%.

• 자연과학논문집
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• 제1권
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• pp.47-59
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• 1987

티타닐 옥살산 바륨 사 수화물(BaTiO($$C_2$$O_4$)_2$ $4H_2$O) 의 분해반응을 열중량 분석법 (TG), 미분 열중량 분석법 (DTG) 그리고 시차 열분석법 (DTA) 를 이용하여 반응기구를 조사 하였다. 중간 생성물과 생성기체는 적외선 분광법과 X-ray회절법을 이용하여 확인하였다. 열분해 과정은 탈수 과정을 포함하여 5단계 분해과정으로 진행하였으며 1단계 분해과정은 탈수과정이며 일부 옥살산기의 분해과정이 함께 일어나게 된다. 2단계 분해과정에서는 1/2몰의 일산화 탄소가 방출되었다. 옥살산기의 분해는 $260~460^{\circ}C$의 온도범위에서 완전히 일어나고 분해하는 시료의 중간체에 자유로운 이산화 탄소기를 가지는 탄산화물을 생성하게 된다. 중간 생성체인 탄산화물의 최종분해는 $650~750^{\circ}C$에서 일어나며 티탄산 바륨 ($BaTiO_3$)이 생성된다.

• 한국세라믹학회지
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• 제31권8호
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• pp.835-840
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• 1994

In this study, the synthesis of Ba2Ti9O20 powder having chemically homogeneous and highly pure fine particle size distribution was attempted by the oxalate method. And the effects of ZrO2 addition was investigated. The four compositions (X=0, 0.028, 0.048, 0.068) of Ba2(Ti9-x, Zrx)O20 were prepared by precipitation reaction of BaCl2, TiCl4, and ZrOCl2, with oxalic acid and NH4OH acting as a precipitating agent and a pH regulator respectively, in aqueous solution. In case of 4.8 mol% ZrO2 addition, the single phase Ba2Ti9O20 was obtained at 120$0^{\circ}C$ and its dielectric properties was excellent showing K=40.5, Q=4621 at 5.4 GHz.

• The Korean Journal of Ceramics
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• 제4권3호
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• pp.213-221
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• 1998

$BaCe_{0.9}Gd_{0.1_O_{2.95}$ powder was synthesized by oxalate coprecipitation method. Precipitate with a stoichimetric ratio of the cations was prepared by adding a mixture of Ba, Ce and Gd nitrate solution to an oxalic acid solution at pH 4. Reaction between the constituent oxides to form a perovskite phase was initiated at $800^{\circ}C$ and a single phase $BaCe_{0.9}Gd_{0.1_O_{2.95}$ powder having good sinterability was obtained after calcination at $1000^{\circ}C$. Sintering green compacts of this powder for 6 h showed a considerable densification to start at $1100^{\circ}C$ and resulted in 93% and 97% relative densities at $1300^{\circ}$ and at $1450^{\circ}C$, respectively. Whereas the power compacts prepared by solid state reaction had lower relative densities, 78% at $1300^{\circ}$and 90% at $1450^{\circ}C$. Fine particles of $CeO_2$ second phase were observed in the surface of the sintered compacts. This was attributed to the evaporation of BaO from the surface that had been exposed during thermal etching.

• 한국결정성장학회지
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• 제10권3호
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• pp.239-244
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• 2000

$LiMn_2$$O_4$Spine에 Li 과량 및 Mn 대신 Co를 일부 치환시킨 $_{1+x}$ Co$_{y}$ Mn$_{2-y}$ $O_4$(0$\leq$x$\leq$0.2,y=0,1/9,1/6) spinel에 대한 합성온도 결정, 상의 생성 등 고온 상평형에 대해 연구하였다. 고온 합성에 따른 제 2상의 생성을 방지하기 위해 저온합성이 가능한 습식화학적 합성법중 하나인 oxalate 침전법을 사용하여 $600^{\circ}C$ 이하에서 단일상의 spinel로 합성하였다. 이렇게 합성된 분말에 대해 TG-DTA분석 및 고온에서 급냉한 분말에 대한 XRD분석을 통해 질량(산소)의 증감에 연관된 가역적인 상전이 온도인 $T_1$, $T_2$및 $T_{2'}$ 들을 확인하였으며, 첨가된 Li의 양과 치환된 Co의 양에 따른 격자상수, 상전이 온도의 변화, 고온상의 안정성 등에 대해 연구하였다. 본 연구를 통해 Li$_{1+x}$ Co$_{y}$ Mn$_{2-y}$ $O_4$spinel의 합성온도 및 냉각속도 둥 합성과정 결정에 필요한 결과들을 얻을 수 있었다.