• Korean Journal of Materials Research
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• v.14 no.10
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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.

• Journal of the Korean Society for Heat Treatment
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• v.15 no.1
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• pp.16-20
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• 2002

In conventional metallothermic reduction(MR) for obtaining tantalum powder in batch-type operation, it is difficult to control morphology and location of deposits because the reaction occurs by direct physical contact between reductants and feed materials. On the other hand, a electronically mediated reaction(EMR) is capable to overcome these difficulties through the reaction by electron transfer and have a merit of continuous process. In this study an MR and EMR method has been applied to the production of a tantalum powder by sodium reduction of $K_2TaF_7$. As the reduction temperature increases, the particle size and yield of tantalum powder obtained by MR and EMR method is increased.

• Korean Journal of Materials Research
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• v.14 no.12
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• pp.857-862
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• 2004

Production of titanium powder directly from tantalum oxides ($TiO_2$) pellet through an electronically mediated reaction (EMR) by calciothermic reduction has been investigated. Feed material ($TiO_2\;pellet$) and reductant (Ca-Ni alloy) were charged into electronically isolated locations in a molten calcium chloride ($CaCl_2$) bath at $950^{\circ}C$. The current flow through an external circuit between the feed (cathode) and reductant (anode) locations was monitored during the reduction of $TiO_2$. The current approximately 3.2A was measured during the reaction in the external circuit connecting cathode and anode location. After the reduction experiment, pure titanium powder with low nickel content was obtained even though Ca-Ni alloy was used as a reductant. These results demonstrate that titanium powder can be produced without direct physical contact between the feed and reductant. In certain experimental conditions, pure titanium powder with approximately $99.5\;mass\%$ purity was successfully obtained.

• Journal of Powder Materials
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• v.10 no.6
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• pp.395-405
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• 2003

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 $K_2$TaF$_{7}$. 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.

• Journal of Powder Materials
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• v.14 no.3 s.62
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• pp.173-179
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• 2007

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 $K_2TaF_7$ 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 $({\sim}34{\mu}m)$, while those prepared via EMR were of uniform $(13{\mu}m)$. In the MR process, the Ta powder recovery rate increased from 37% to 83% at 1123K in constrat with EMR process.

• Journal of Powder Materials
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• v.11 no.4
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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.

• Journal of Powder Materials
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• v.14 no.3 s.62
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• pp.190-196
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• 2007

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 $K_2TaF_7$ 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.