• 한국재료학회지
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• 제13권12호
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• pp.806-811
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• 2003

Ultrafine TaC powders were synthesised by spray drying using tantalum oxalate solution. The spray dried powders were spherical shape and less than 30 $\mu\textrm{m}$ in size. The powders calcined at 500 and X$700^{\circ}C$ showed amorphous structures and $Ta_2$$O_{5}$ phase was obtained by calcining at $700^{\circ}C$. The particle size and shape remains constant after calcination. The calcined spherical powders were composed of an agglomerate of primary particles under 50 nm in size. The complete formation of TaC could be achieved by heat treatment at $1050^{\circ}C$ for 6 hrs. The observed size of TaC powders by TEM was less than 200 nm.

• 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.

• Nuclear Engineering and Technology
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• 제51권8호
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• pp.1957-1963
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• 2019

A UVC photo-Fenton advanced oxidation process (AOP) was studied to develop a process for the decomposition of oxalic acid waste generated in the chemical decontamination of nuclear power plants. The oxalate decomposition behavior was investigated by using a UVC photo-Fenton reactor system with a recirculation tank. The effects of the three operational variables-UVC irradiation, H₂O₂ and Fenton reagent-on the oxalate decomposition behavior were experimentally studied, and the behavior of the decomposition product, CO₂, was observed. UVC irradiation of oxalate resulted in vigorous CO₂ bubbling, and the irradiation dose was thought to be a rate-determining variable. Based on the above results, the oxalate decomposition kinetics were investigated from the viewpoint of radical formation, propagation, and termination reactions. The proposed UVC irradiation density model, expressed by the first-order reaction of oxalate with the same amount of H₂O₂ consumption, satisfactorily predicted the oxalate decomposition behavior, irrespective of the circulate rate in the reactor system within the experimental range.

• 한국전기전자재료학회논문지
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• 제15권1호
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• pp.46-55
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• 2002

10mo1% Gd$_2$O$_3$ doped CeO$_2$ fine powders were synthesized by the oxalate coprecipitation method. The characteristics and sintering behavior of fine powders were investigated. The oxalate precipitates had the specific surface area of 150$m^2$/g, and appeared to be fine and spherical primary particles with a size of approximately 5.5nm. The decomposition of the precipitates occurred from a temperature around 30$0^{\circ}C$ and it was completed below 40$0^{\circ}C$, resulted in the formation of the oxide. The calcination temperature of the fine powders was suitable at 77$0^{\circ}C$. By introducing fine powders washed with alcohol and ball-milling process after calcination, the sintered body was possible to attain the value of 97% of the theoretical density at low temperature of 130$0^{\circ}C$

• 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.

• 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.

• Bulletin of the Korean Chemical Society
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• 제35권6호
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• pp.1832-1836
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• 2014

A deep understanding of the metallic silver catalysts formation process on oxide support and the formation mechanism is of great scientific and practical meaning for exploring better catalyst preparing procedures. Herein the thermal decomposition process of supported silver catalyst with silver oxalate as the silver precursor in the presence of ethylenediamine and ethanolamine is carefully investigated by employing a variety of characterization techniques including thermal analysis, in situ diffuse reflectance infrared Fourier transform spectroscopy, scanning electron microscopy, and X-ray diffraction. The formation mechanism of supported silver particles was revealed. Results showed that formation of metallic silver begins at about $100^{\circ}C$ and activation process is essentially complete below $145^{\circ}C$. Formation of silver was accompanied by decomposition of oxalate group and removal of organic amines. Catalytic performance tests using the epoxidation of ethylene as a probe reaction showed that rapid activation (for 5 minutes) at a relatively low temperature ($170^{\circ}C$) afforded materials with optimum catalytic performance, since higher activation temperatures and/or longer activation times resulted in sintering of the silver particles.

• 자원환경지질
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• 제45권2호
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• pp.89-104
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• 2012

본 연구에서는 제주도 토양 중 화산쇄설암과 현무암을 모재로 발달하는 두 Andisol 토양의 Al 용해도 특성을 규명하고자 하였다. 토양 A층은 높은 유기물함량과 $Al_{pyrophosphate}/Al_{oxalate}$ 비를 나타내는 반면, 토양 Bo층은 낮은 유기물함량과 $Al_{pyrophosphate}/Al_{oxalate}$ 비를 나타낸다. 이는 반응성 Al이 A층에서는 대부분이 유기물과 결합한 형태로 존재하고 있는 반면, 토양 Bo층에서는 무기질의 광물과 결합하고 있음을 지시한다. Acid-oxalate 용해처리, 그리고 150 및 $350^{\circ}C$ 열처리 전후의 FT-IR 스펙트럼 비교, 투과전자현미경(TEM)을 이용한 관찰결과, 토양 Bo층에 상당량의 이모골라이트(Imogolite)가 존재함을 확인하였다. 이들 시료에 대한 Al-용해도 특성규명을 위한 Batch 평형실험결과, 토양 Bo층에서의 Al-용해도는 ITM(Imogolite-type material)과 Al hydroxy-interlayered aluminosilicate에 의한 Simultaneous equilibrium보다는 ITM의 Congruent dissolution model을 따르는 것으로 나타났다. 투석과 Aging과정 후의 용해도 특성 변화는 PI(Proto imogolite) sol의 생성이 되고, 이들의 이모골라이트로의 상전이가 Al-용해도에 영향을 주었음을 지시한다. 이러한 결과는, 실내실험 결과를 보완해주는 것으로, 제주도 Andisol토양에서의 Al-용해도 특성이 ITM에 의한 Congruent dissolution에 의해 조절되고 있음을 지시한다.

• 공업화학
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• 제16권4호
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• pp.496-501
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• 2005

Iron계 금속 촉매의 존재 하에서 ABS의 열분해 거동을 TGA (Thermogravimetric Analysis)를 통해서 조사하였다. Iron계 금속 촉매(ferric nitrate nonahydrate, ammonium ferric sulfate dodecahydrate, iron sulfate hydrate, ammonium ferric oxalate, iron(II) acetate, iron(II) acetylacetonate 및 ferric chloride)는 ABS의 열분해 과정에서 화학반응을 야기하여, 질소분위기에서 촤(char)형성이 관찰되었으며, $600^{\circ}C$에서 3~23 wt%의 비휘발성 촤를 형성하였다. 이와 같은 질소분위기에서의 ABS의 촤 생성은 iron계 금속 촉매의 가교효과(crosslinking effect)로 추정된다. 한편, 공기분위기에서는 생성된 촤가 고온 산화반응에 의해서 열분해되었다.

• 한국세라믹학회지
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• 제43권10호
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• pp.666-672
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• 2006

GDC20($Ce_{0.8}Gd_{0.2}O_{1.9}$) powder was synthesized by oxalate co-precipitation and milling and its thermal decomposition, phase formation, and sinterability were investigated. As-prepared precipitates were non-crystalline due to the milling process and completely decomposed at 400$^{\circ}C$ The powder calcined at 800$^{\circ}C$ for 2 h contained fine p]sty particles with an average size of 0.69 $\mu$m. Attrition milling of the calcined powder for 2 h had a little milling effect, resulting in a slight decrease in the particle size to 0.45 $\mu$m. The milled powder consisted of small spherical primary particles and some large particles, which had been agglomerated during calcination. Due to the excellent sinterability of the powder, sintering of the powder compacts for 4 h showed relative densities of 78.7% at 1000$^{\circ}C$ and 97.8% at 1300$^{\circ}C$, respectively. Densification was found to almost complete at temperature above 1200$^{\circ}C$ and a dense and homogeneous microstructure was obtained. A rapid grain growth occurred between 1200$^{\circ}C$ and 1300$^{\circ}C$. Grains in 0.1$\sim$0.5 $\mu$m sizes at 1200$^{\circ}C$ grew to 0.2$\sim$2 $\mu$m and their size distribution became broader at 1300$^{\circ}C$.