A process known as the MR and EMR combination process is able to overcome the shortcomings of the MR (metallothermic reduction) and EMR (electronically mediated reaction) process. The effects of as the raw material, sodium as the reducing agent and KCl/KF as the diluent on the characteristics of tantalum powder are investigated. In this study, a MR-EMR combination process has been employed to tantalum powder on the location of reductant. The excess of reductant were varied from 25, 50 to 75 wt%. The total charge and external circuit decreases as the amount of reductant increases. The average particle size increases with increasing the amount of reductant.
In the metallothermic reduction (MR) process used to obtain tantalum powder in one batch, it is difficult to control the morphology and location of the tantalum deposits. On the other hand, an electronically mediated reaction (EMR) process is capable of overcoming this difficulty. The effect of using as the raw material and sodium as the reducting agent on the characteristics of tantalum powder are investigated. As the temperature of the reduction varied from 1023K to 1223K, the powder particles obtained with MR were relatively large , while those prepared via EMR were of uniform . In the MR process, the Ta powder recovery rate increased from 37% to 83% at 1123K in constrat with EMR process.
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 TaF 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.
In the conventional metallothermic reduction (MR) process for obtaining tantalum powder in batch-type operation. it is difficult to control morphology and location of deposits. On the other hand, a electronically mediated reaction (EMR) process is capable to overcome these difficulties and has a merit of continuous process, but it has the defect that the reduction yield is poor. MR-EMR combination process is a method that is able to overcome demerits of MR and EMR process. In this study, a MR-EMR combination process has been applied to the production of tantalum powder by sodium reduction of TaF. The total charge passed through external circuit and average particle size (FSSS) were increased with increasing reduction temperature. The proportion of fine particle (-325 mesh) was decreased with increasing reduction temperature. The yield was improved from 65% to 74% with increasing reduction temperature. Considering the charge, impurities, morphology, particle size and yield, an reduction temperature of 1,123 K was found to be optimum temperature for MR-EMR combination process.s.
This study examined the correlation of various operational factors including reaction temperature and the quantity of reductant and diluent with the characteristics of powder using TaF as feed materials, Na as a reductant and KCl/KF as a diluent. Also to control the particle size and shape, external supply system developed, it can provide a feed material and a reductant at a fixed quantity and evaluated the characteristics of tantalum powder. When the external supply system was applied instead of the batch type process that charges feed material, reductant and diluent at the same time, it was possible to induce regular reduction reaction between feed material and reductant, which increased the recovery rate and reduced the mixture of impurities. In particular, the application of the external supply system enabled the control of reaction temperature and reaction speed according to the feeding rate of feed material during reduced reaction, and resultantly it enabled the manufacturing of granular-shaped powder with a regular granularity of 2∼3 and purity of 99.5%.%.
Pure tantalum powder has been produced by combining Na as a reducing agent, TaF 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) was effective in removing heavy metal impurities such as Fe, Cr and Ni, 8% HSO + 8% (SO) in removing fluorides such as K and F from non-reactive feed material, and 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.e.
Pure tantalum powder has been produced by combining Na as a reducing agent, 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 and the amount of the additional reductant from +5% of the theoretical amount used for the reduction of the entire . 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 to and a particle size distribution which is below 325 mesh in fined powder increases from 71% to 83%. The average size of Tantalum powder, , was close to that of the commercial powders(). Also under this condition, impurities contained in the powder were within the range allowed for the commercial Ta powders.
황산구리 전해욕에 분산제인 콜로이달 실리카(SiO2현탁액)를 첨가시키는 분산도금의 방법과 Au pre-coating을 이용하여 음극에 석출하는 전해 석출물의 결정구조, 표면형상, 결정방향 등의 변화를 검토하였다. 실리카 분산 및 Au pre-coating에 의하여 전해 석출피막의 결정입자가 미세화 되고, 균일하게 성장됨은 물론, 결정 수가 증가하였다. 콜로이달 실리카의 분산 효과에 의해서 전해 석출피막의 경도가 대략 15%까지 상승하였다. 또한 콜로이달 실리카를 분산시킨 구리 전착층의 X-선 회절패턴이 (111)면, (200)면과 (311)면이 거의 소멸되어 우선 방위가 (111)에서 (110)면으로 변화되었다.
6.5wt%Si강판을 낮은 철손실, 고투자율 그리고 자왜가 거의 0으로 우수한 자성재료로 잘 알려져 있다. 본 실험에서는 화학기상증착 (Chemical Vapor Deposition)으로 6.5wt%Si 강판을 만들었다 이 과정은 튜브 노내에서 실리콘의 함량이 낮은 Si강판에 SiCl4가스를 반응시킨다. 이때 SiCl4가스에서 분해된 Si의 원자들은 모재인 강판 표면에 증착되어 표면층에 Si가 풍부한 층을 형성한다. 마지막으로 고온에서 확산과정을 통하여 모재 내부로부터 실리콘의 함량이 균일한 강판을 얻을 수 있다. 0.5mm두께를 갖은 6.5wt%Si 강판의 철손실은 고주파수에서 약 8.92W/kg를 나타냈으며 투자율은 53,300으로 일반 실리콘강판, 즉 2.5wt%Si강판의 투자율 37,100보다 약 두배 가량 증가하였다. 또한 기계적인 특성을 평가하기 위해서 일반 0.5wt%Si강판과 773K의 온도에서 수시간 열처리한 강판을 인장실험 하였다. 따라서 수 시간 열처리한 시편에서 연신율이 증가함을 알 수 있었으며 파단면을 관찰한 결과 입 계파단면이 현저히 감소했음을 알았다
Fe기 비정질합금에서 과냉각액체영역의 유무에 따른 열적 안정성을 비교평가하기 위하여 결정화온도 이하에서 유리천이가 나타나지 않는 Fe80P6C12B12합금과 52K의 과냉각 액체영역을 갖는 Fe73P11C6B4AI4Ge2 glassy 합금을 열분석하였다. 등온결정화에 의한 열분석의 결과 JMA plot의 n값은 Fe80P6C12B12합금이 1.8-2.2이고 과냉각 액체영역을 갖는 Fe73P11C6B4AI4Ge2 합금이 2.5-4.0으로서 후자의 경우가 열적으로 안정하였다. 결정화의 양상은 Fe80P6C12B12 합금의 경우 핵생성속도가 일정할 때 확산율속에 의해 결정입자가 성장하는 반면 Fe73P11C6B4AI4Ge2 glassy합금의 경우 핵생성속도가 일정할 때 계면입자가 성장한다. Fe73P11C6B4AI4Ge2 합금 및 Fe80P6C12B12 합금의 결정화에 필요한 활성화에너지, 핵생성 및 성장에 필요한 활성화에너지는 각각 371, 353kJ/mol, 그리고 324, 301KJ/mol 및 301, 273KJ/mol로서 과냉각 액체영역을 갖는 합금이 열적으로 안정하다고 판단된다.