The purpose of this study is to investigate the densification behavior and the corresponding microstructural evolution of tantalum and tantalum-tungsten alloy powders for explosively formed liners. The inherent inhomogeneous microstructures of tantalum manufactured by an ingot metallurgy might degrade the capability of the warhead. Therefore, to overcome such drawbacks, powder metallurgy was incorporated into the near-net shape process in this study. Spark plasma-sintered tantalum and its alloys with finer particle sizes exhibited higher densities and lower grain sizes. However, they were contaminated from the graphite mold during sintering. Higher compaction pressures in die and isostatic compaction techniques also enhanced the sinterability of the tantalum powders; however, a full densification could not be achieved. On the other hand, the powders exhibited full densification after being subjected to hot isostatic pressing over two times. Consequently, it was found that the hot isostatic-pressed tantalum might exhibit a lower grain size and a higher density as compared to those obtained in previous studies.

Metallic tantalum powder is manufactured by reducing tantalum oxide (Ta2O5) with magnesium gas at 1,073–1,223 K in a reactor under argon gas. The high thermodynamic stability of magnesium oxide makes the reduction reaction from tantalum oxide into tantalum powder possible. The microstructure after the reduction reaction has the form of a mixture of tantalum and magnesium oxide, and the latter could be entirely eliminated by dissolving in weak hydrochloric acid. The powder size in SEM microstructure for the tantalum powder increases after acid leaching in the range of 50–300 nm, and its internal crystallite sizes are observed to be 11.5 to 24.7 nm with increasing reduction temperatures. Moreover, the optimized reduction temperature is found to be 1,173 K as the minimum oxygen concentration is approximately 1.3 wt.%.

A bulk-type Ta material is fabricated using the kinetic spray process and its microstructure and physical properties are investigated. Ta powder with an angular size in the range 9-37 μm (purity 99.95%) is sprayed on a Cu plate to form a coating layer. As a result, ~7 mm-sized bulk-type high-density material capable of being used as a sputter material is fabricated. In order to assess the physical properties of the thick coating layer at different locations, the coating material is observed at three different locations (surface, center, and interface). Furthermore, a vacuum heat treatment is applied to the coating material to reduce the variation of physical properties at different locations of the coating material and improve the density. OM, Vickers hardness test, SEM, XRD, and EBSD are implemented for analyzing the microstructure and physical properties. The fabricated Ta coating material produces porosity of 0.11~0.12%, hardness of 311~327 Hv, and minor variations at different locations. In addition, a decrease in the porosity and hardness is observed at different locations upon heat treatment.

The effect of heat treatment environment on the microstructure and properties of tantalum coating layer manufactured by kinetic spraying was examined. Heat treatments are conducted for one hour at 800oC, 900oC, and 1000oC in two different environments of vacuum and Ar gas. Evaluation of microstructure and physical properties are conducted. High density α- tantalum single phase coating layer with a porosity of 0.04% and hardness of 550 Hv can be obtained. As heat treatment temperature increases, porosity identically decreases regardless of heat treatment environment (vacuum and Ar gas). Hardness of heat treated coating layer especially in Ar gas environment deceases from 550 Hv to 490 Hv with increasing heat treatment temperature. That in vacuum environment deceases from 550 Hv to 530 Hv. The boundary between particles became vague as heat treatment temperature increases. Oxygen distribution of tantalum coating layer is minute after heat treatment in vacuum environment than Ar gas environment.

Tantalum nitrides () have been developed to substitute the Cd based pigments for non-toxic red pigment. Various doping elements were doped to reduce the amount of high price Tantalum element used and preserve the red color tonality. Doping elements were added in the synthesizing process of precursor of amorphous tantalum oxides and then Tantalum nitrides doped with various elements were obtained by ammonolysis process. The average particle size of final nitrides with secondary phases was larger than the nitride without the secondary phases. Also secondary phases reduced the red color tonality of final products. On the other hand, final nitrides without secondary phase had orthorhombic crystal system and presented good red color. In other words, in the case of nitrides without secondary phases, doping elements made a solid solution of tantalum nitride. In this context, doping process controlled the ionic state of nitrides and the amount of oxygen/nitrogen in final nitrides affected the color tonality.

Colored tantalum oxy-nitride (TaON) and tantalum nitride () were synthesized by ammonolysis. Oxygen deficient tantalum oxides () were produced by a titration process, using a tantalum chloride () precursor. The stirring speed and the amount of were important factors for controling the crystallinity of tantalum oxides. The high crystallinity of tantalum oxides improved the degree of nitridation which was related to the color value. Synthesized powders were characterized by XRD, SEM, TEM and Colorimeter.

In this study, tantalum (Ta) compacts were fabricated in a spark plasma sintering (SPS) process and their microstructure and mechanical properties were investigated. Ta compacts with a density of 99% were successfully fabricated by controlling the sintering conditions of the current and the temperature. The density and hardness were increased as the sintering temperature increased. The Ta2C compound was observed at the surface of the compacts due to the contact between the Ta powder and graphite mold during the sintering process. The main fracture mode showed a mixed type with intergranular and transgranular modes having some roughness.

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.

Ultrafine TaC-5%Co composite powders were synthesized by spray conversion process using tantalum oxalate solution and cobalt nitrate hexahydrate(Co( . 6). The phase of Ta-Co oxide powders had amorphous structures after calcination below 50 and changed , and phase by heating above . 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. The complete formation of TaC could be achieved at 105 for 6 hours. The observed size of TaC-Co composite powders by TEM was smaller than 200 nm.