Tantalum producers

The first commercial use of tantalum was as filaments ia iacandescent lamps but it was soon displaced by tungsten. Tantalum is used ia chemical iadustry equipment for reaction vessels and heat exchangers ia corrosive environments. It is usually the metal of choice for heating elements and shields ia high temperature vacuum sintering furnaces. In 1994, over 72% of the tantalum produced ia the world went iato the manufacturiag of over 10 x 10 soHd tantalum capacitors for use ia the most demanding electronic appHcations. 

The high Ni impurity content is significant and results from the dissolution of the inner current lead made from Ni which diffused through pores of the ceramic anode body. The increased content of Ca in tantalum produced in electrolysis of CaCl2 CaO melt is connected with the entrainment of complex oxides containing CaO. A great advantage of the electrolysis process with a ceramic anode over that with a carbon anode is the production of tantalum with a relatively low carbon content. 

Gr. Tantalos, mythological character, father of Niobe) Discovered in 1802 by Ekeberg, but many chemists thought niobium and tantalum were identical elements until Rowe in 1844, and Marignac, in 1866, showed that niobic and tantalic acids were two different acids. The early investigators only isolated the impure metal. The first relatively pure ductile tantalum was produced by von Bolton in 1903. Tantalum occurs principally in the mineral columbite-tantalite. 

Separation of tantalum from niobium requires several complicated steps. Several methods are used to commercially produce the element, including electrolysis of molten potassium fluorotantalate, reduction of potassium fluorotantalate with sodium, or reacting tantalum carbide with tantalum oxide. Twenty five isotopes of tantalum are known to exist. Natural tantalum contains two isotopes. 

Terbium has been isolated only in recent years with the development of ion-exchange techniques for separating the rare-earth elements. As with other rare earths, it can be produced by reducing the anhydrous chloride or fluoride with calcium metal in a tantalum crucible. Calcium and tantalum impurities can be removed by vacuum remelting. Other methods of isolation are possible. 

Fused Salt Electrolysis. Only light RE metals (La to Nd) can be produced by molten salt electrolysis because these have a relatively low melting point compared to those of medium and heavy RE metals. Deposition of an alloy with another metal, Zn for example, is an alternative. The feed is a mixture of anhydrous RE chlorides and fluorides. The materials from which the electrolysis cell is constmcted are of great importance because of the high reactivity of the rare-earth metals. Molybdenum, tungsten, tantalum, or alternatively iron with ceramic or graphite linings are used as cmcible materials. Carbon is frequently used as an anode material. 

Other Metals. AH the sodium metal produced comes from electrolysis of sodium chloride melts in Downs ceUs. The ceU consists of a cylindrical steel cathode separated from the graphite anode by a perforated steel diaphragm. Lithium is also produced by electrolysis of the chloride in a process similar to that used for sodium. The other alkaH and alkaHne-earth metals can be electrowon from molten chlorides, but thermochemical reduction is preferred commercially. The rare earths can also be electrowon but only the mixture known as mischmetal is prepared in tonnage quantity by electrochemical means. In addition, beryIHum and boron are produced by electrolysis on a commercial scale in the order of a few hundred t/yr. Processes have been developed for electrowinning titanium, tantalum, and niobium from molten salts. These metals, however, are obtained as a powdery deposit which is not easily separated from the electrolyte so that further purification is required. 

Electrolytic Capacitors. Tantalum, because of its high melting point of 2850°C, is produced as a metal powder. As such, it is molded, sintered, and worked to wire and fod, and used to budd certain types of tantalum capacitors (51). Other capacitors are made by compacting and sintering the tantalum powder. 

The reaction of finely ground ores and an excess of carbon at high temperatures produces a mixture of metal carbides. The reaction of pyrochlore and carbon starts at 950°C and proceeds vigorously. After being heated to 1800—2000°C, the cooled friable mixture is acid-leached leaving an insoluble residue of carbides of niobium, tantalum, and titanium. These may be dissolved in HF or may be chlorinated or burned to oxides for further processing. 

Nitric acid reacts with all metals except gold, iridium, platinum, rhodium, tantalum, titanium, and certain alloys. It reacts violentiy with sodium and potassium to produce nitrogen. Most metals are converted iato nitrates arsenic, antimony, and tin form oxides. Chrome, iron, and aluminum readily dissolve ia dilute nitric acid but with concentrated acid form a metal oxide layer that passivates the metal, ie, prevents further reaction. 

The reaction temperature of 500—600°C is much lower than that required for the reductive chlorination. The volatile chlorides evolve from the molten salt bath. The boiling points of NbCl, TaCl, and WOCl He between 228 and 248°C. These compounds must therefore be separated by means of a distillation column. The chlorination of ferroalloys produces very pure tantalum pentachloride in toimage quantities. The TaCl contains less than 5 )J.g Nb/g Ta, and other metallic impurities are only amount to 1—2 lg/g Ta. 

Tantalum Compounds. Potassium heptafluorotantalate [16924-00-8] K TaF, is the most important tantalum compound produced at plant scale. This compound is used in large quantities for tantalum metal production. The fluorotantalate is prepared by adding potassium salts such as KCl and KF to the hot aqueous tantalum solution produced by the solvent extraction process. The mixture is then allowed to cool under strictiy controlled conditions to get a crystalline mass having a reproducible particle size distribution. To prevent the formation of oxyfluorides, it is necessary to start with reaction mixtures having an excess of about 5% HF on a wt/wt basis. The acid is added directiy to the reaction mixture or together with the aqueous solution of the potassium compound. Potassium heptafluorotantalate is produced either in a batch process where the quantity of output is about 300—500 kg K TaFy, or by a continuously operated process (28). 

Fig. 3. Schematic of a reactor used to produce tantalum powder by the sodium reduction process.

The dramatic improvements in the physical and chemical properties of tantalum powder produced by the sodium reduction process are evident in the lessening of chemical impurities (see Table 5). The much-improved chemistry reflects the many modifications to the process put in place after 1990. 

Post-Reduction Processing. The primary tantalum powder produced by the sodium reduction process is treated to convert the metal to a form suitable for use as capacitor-grade powder and feedstock for wire and sheet. 

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