Method for Combination Solid State and Molten Salt Tantalum Reduction
a technology of solid state and molten salt, applied in the field of tantalum reduction products, can solve the problems of high demand for purity and surface area for use in electrolytic capacitors, affecting the uniformity of the resulting tantalum particles, and increasing reaction ra
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example 1
[0023]At ambient temperature, an empty reactor vessel with approximately 100 gallons capacity is pre-loaded with 1.0 Kgs of K2TaF7 powder as a single pile in the center-bottom of the vessel. On top of this layer of K2TaF7 is placed a solid 1.0 Kg ingot of sodium metal also at room temperature. This composite is then buried under 300 Kg of KCl. For the first heating phase, the reactor is closed and the air replaced with argon per typical reduction procedures and heated to 300° C. degrees at a rate of 1 degree Celsius per minute, and then held at 300° C. for 60 minutes. This arrangement results in a solid state reduction reaction between the metallic sodium and K2TaF7. The amount of sodium metal used in this phase is in excess of the stoicheometric amount needed to completely reduce the 1.0 Kg of K2TaF7, thereby minimizing the rate of crystal growth of the submicron tantalum particles formed during this first phase.
[0024]For the second heating phase, the sealed reactor is then further...
example 2
[0025]A reduction is performed in a similar fashion as in Example 1, except that in this Example 2 the 1.0 Kg of solid K2TaF7 and 1.0 Kg ingot of sodium metal are combined in a 5-inch diameter by 12-inch long steel reactor vessel fitted with a funnel-shaped lid topped with a 2-inch ball valve. This vessel is placed into a hot wall tube furnace and heated to 300° C. following a similar procedure as the first heating phase of Example 1. After holding at 300° C. for 60 minutes, the vessel is removed from the tube furnace, up-ended and attached by a pipe union to a 2-inch pipe nipple penetrating the lid of an empty, cold conventional sodium reduction reactor. The ball valve built into the lid of the small reactor is opened allowing the product of the solid state reduction to fall from the small vessel through the pipe nipple into the conventional reactor. Thereafter, 300 Kgs of KCl are poured into the conventional reactor and the reactor is heated under argon until the KCl is melted at ...
example 3
[0026]At ambient temperature, an empty reactor vessel with approximately 100 gallons capacity is pre-loaded with 100 Kgs of K2TaF7 powder as a single pile in the center-bottom of the vessel. On top of this layer of K2TaF7 is placed a solid 30 Kg ingot of sodium metal also at room temperature. As with Example 1, this composite is then buried under 300 Kg of KCl. For the first heating phase, the reactor is closed and the air replaced with argon per typical reduction procedures and heated to 300° C. degrees at a rate of 1 degree Celsius per minute, and then held at 300° C. for 60 minutes. This arrangement results in a solid state reduction reaction between the metallic sodium and K2TaF7. The amount of sodium metal used in this phase is in slightly excess of the stoicheometric amount needed to completely reduce the 100 Kg of K2TaF7, thereby minimizing the rate of crystal growth of the submicron tantalum particles formed during this first phase.
[0027]For the second heating phase, the sea...
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