• 자원리싸이클링
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• 제21권3호
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• pp.74-83
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• 2012

희토류 금속의 제련은 광석에서부터 파분쇄, 선별과정을 거쳐 정광을 만들고, 정광 중의 희토류 성분을 추출하고 성분별로 분리하는 분리정제공정을 거쳐 희토류산화물이나 염화물과 같은 희토류화합물을 제조한 다음 희토류화합물에서 금속을 추출해내는 환원과정을 거친다. 본 고에서는 대표적 희토류 광물로서 불탄산염계광물인 바스트나사이트(bastnasite, ((RE)($CO_3$)F)와 인산염계 광물인 모나자이트(monazite,(RE)($PO_4SiO_4$))의 분해 침출과 분리정제 방법에 대해서 간략히 기술하고, 분리공정의 산물인 희토류화합물에서부터 범용 희토류금속 제조법으로 사용되고 있는 금속열환원법과 용융염전해법에 대하여 개략적인 내용을 소개하였다.

• 한국분말재료학회지
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• 제20권1호
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• pp.43-47
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• 2013

The extraction of metallic pure vanadium powder from raw oxide has been tried by Mg-reduction. In first stage, $V_2O_5$ powders as initial raw material was reduced by hydrogen gas into $V_2O_3$ phase. $V_2O_3$ powder was reduced in next stage by magnesium gas at 1,073K for 24 hours. After reduction reaction, the MgO component mixed with reduced vanadium powder were dissolved and removed fully in 10% HCl solution for 5 hours at room temperature. The oxygen content and particle size of finally produced vanadium powders were 0.84 wt% and 1 ${\mu}m$, respectively

• 한국재료학회지
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• 제11권12호
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• pp.1052-1056
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• 2001

Pure tantalum powder has been produced by sodium as a reluctant, $K_2TaF_7$as a feed material and KCl/KF as a diluent in an inconel stainless steel bomb by the metallothermic reduction. The influence of experimental variable, such as temperature of reduction on the yield and characteristics of the Ta powder has been studied. As the temperature of the reduction was varied from$ 800{\circ}C~980{\circ}C$, the yield of tantalum powder increased from 41% to 56%. However no appreciable improvement was observed above$920{\circ}C$. The fraction of fine Ta Powder decreased appreciably with the increase of temperature, and particle size was$2~3{\mu}m$at reduction temperature of$920{\circ}C$.Therefore a reduction temperature of$920{\circ}C$was optimally fixed for subsequent runs.

• Nuclear Engineering and Technology
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• 제53권6호
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• pp.1931-1938
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• 2021

Uranium ingot is produced by metallothermic reduction of uranium tetrafluoride using magnesium or calcium as reductant. Presence of oxygen containing compounds viz. uranyl fluoride and uranium oxide in the starting uranium fluoride has a significant effect on the firing time, final temperature of the charge, slag-metal separation and hence the metal recovery. As reported in the literature, the maximum tolerable limit for uranyl fluoride in the UF₄ is 2.5 wt% and limit for uranium oxide content is in the range 2-3 wt%. No theoretical or experimental basis is available till date for these limits. Analyses have been carried out in this study to understand the effect of UO₂F₂ concentration in the starting fluoride on the final temperature of the products and thus the reduction characteristics. UF₄ having uranyl fluoride concentration, less than as well as more than 2.5 wt%, have been investigated. Thermodynamic calculations have been carried out to arrive at a general expression for the final temperature attained by the products during calciothermic reduction of UF₄. Finally, an upper limit for the oxygen containing impurities has been estimated using the CaO-CaF₂ phase diagram.

• 한국분말재료학회지
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• 제26권4호
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• pp.334-339
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• 2019

To meet the current demand in the fields of permanent magnets for achieving a high energy density, it is imperative to prepare nano-to-microscale rare-earth-based magnets with well-defined microstructures, controlled homogeneity, and magnetic characteristics via a bottom-up approach. Here, on the basis of a microstructural study and qualitative magnetic measurements, optimized reduction conditions for the preparation of nanostructured Sm-Co magnets are proposed, and the elucidation of the reduction-diffusion behavior in the binary phase system is clearly manifested. In addition, we have investigated the microstructural, crystallographic, and magnetic properties of the Sm-Co magnets prepared under different reduction conditions, that is, $H_2$ gas, calcium, and calcium hydride. This work provides a potential approach to prepare high-quality Sm-Co-based nanofibers, and moreover, it can be extended to the experimental design of other magnetic alloys.

• 한국재료학회지
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• 제14권10호
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• pp.719-724
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• 2004

Production of fine tantalum powder by calciothermic reduction of tantalum oxides ($Ta_{2}O_5$) pellet through an electronically mediated reaction (EMR) has been investigated. $Ta_{2}O_5$ pellet feed and reductant calcium-nickel (Ca-Ni) alloy were charged into electronically isolated locations in a molten $CaCl_2$ bath. The current flow through an external path between the feed (cathode) and reductant (anode) locations was monitored. The current approximately 4.7A was measured during the reaction in the external circuit connecting cathode and anode location. Tantalum powder with approximately 99 $mass\%$ purity was readily obtained after each experiment. Tantalum powder by EMR using $Ta_{2}O_5$ pellet feed was fine compared with that of metal powder by metallothermic reduction and EMR using $Ta_{2}O_5$ powder feed.

• 한국분말재료학회지
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• 제10권5호
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• pp.344-347
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• 2003

Pure tantalum powder has been produced by combining Na as a reducing agent, $K_2$TaF$_{7}$ as feed material, KCl and KF as a diluent in a stainless steel (SUS) bomb, using the method of metallothermic reduction. And we examined various types of after-treatment that affect the high purification of powder. A significant amount of impurities contained in recovered powder was removed in various conditions of acid washing. In particular, 20% (HCl + HNO$_3$) was effective in removing heavy metal impurities such as Fe, Cr and Ni, 8% H$_2$SO$_4$ + 8% $Al_2$(SO$_4$)$_3$ in removing fluorides such as K and F from non-reactive feed material, and 2% $H_2O$$_2$ + 1 % HF in removing oxides that formed during reaction. Significant amounts of oxygen and part of light metal impurities could be removed through deoxidation and heat treatment process. On the other hand, because it is difficult to remove completely heavy metal impurities such as Fe, Cr, and Ni through acid washing or heat treatment process if their contents are too high, it is considered desirable to inhibit these impurities from being mixed during the reduction process as much as possible.

• 한국분말재료학회지
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• 제9권5호
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• pp.315-321
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• 2002

Pure tantalum powder has been produced by combining Na as a reducing agent, $K_2TaF_{7}$ as feed material, KCl and KF as a diluent in a stainless steel(SUS) bomb, using the method of metallothermic reduction. The present study investigated the effect of the amount of the diluent and reaction temperature on the characteristics of tantalum powder in the production process. The temperature applied in this study $850^{\circ}C$ and the amount of the additional reductant from +5% of the theoretical amount used for the reduction of the entire $K_2TaF_{7}$. The results showed that as the amount of the diluent increased, the reaction temperature became lower because the diluent prevented a temperature rise. Also, according to the mixture ratio of the feed materials and the diluent changed from 1 : 0.25 to 1 : 2, the particle size decreased from $5\mutextrm{m}$ to $1\mutextrm{m}$ and a particle size distribution which is below 325 mesh in fined powder increases from 71% to 83%. The average size of Tantalum powder, $2-4\mutextrm{m}$, was close to that of the commercial powders($2-5\mutextrm{m}$). Also under this condition, impurities contained in the powder were within the range allowed for the commercial Ta powders.

• 한국표면공학회지
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• 제42권5호
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• pp.227-231
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• 2009

The niobium capacitor showed somewhat more unstable characteristics than the commercial tantalum capacitors, but is nonetheless considered applicable as a future substitute for tantalum capacitors. In this study, niobium powder was fabricated by metallothermic reduction process using $K_2NbF_7$ as the raw materials, KCl and KF as the diluents and Na as the reducing agent. The niobium particle size greatly decreased from 0.7um to 0.2 um as the amount of diluent increased. However if a higher surface area of powder is required, more diluents need to be used in the said method in order to produce niobium powder. The niobium powder morphology and particle size are very sensitive to a amount of sodium excess. The particle size of niobium powder increased with a increasing amount of sodium excess. When more diluent and sodium are used, the niobium powder will be contaminated with more impurities such as Fe, Cr, Ni so on.

• 한국분말재료학회지
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• 제11권4호
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• pp.333-340
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• 2004

In this study, tantalum powder has been producted by MR-EMR combination process. MR-EMR combination process is a method that is able to improve demerits of MR(metallothermic reduction) and EMR(electronically mediated reaction) process. This study examined the characteristics of powder with the amount of reductant excess using $K_2$TaF$_{7}$ as feed materials, Na as a reductant and KCl/KF as a diluent. In addition, this study examined acid treatment that affect the high purification of powder. The impurities contained in powder was removed in various conditions of acid treatment. The total charge passed through external circuit and average particle size(FSSS) were increased with increasing amount of sodium excess. The proportion of fine particle(-325mesh) was decreased with increasing amount of sodium excess. The yield was improved from 70％ to 76% with increasing amount of sodium excess. Considering the impurities, charge, morphology, particle size and yield, an amount of sodium excess of 10wt% were found to be optimum conditions for MR-EMR combination process.s.