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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

Inactive Publication Date: 2010-04-29
KEMET BLUE POWDER CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0006]Disclosed and claimed herein are methods for producing tantalum powder. In one embodiment, a method includes loading an unheated reactor vessel with a layer of solid K2TaF7, loading the unheated reactor vessel with a layer of solid sodium metal over the layer of solid K2TaF7, and then loading the unheated reactor vessel with a layer of solid diluent salt over the layer of solid K2TaF7 and the layer of sol

Problems solved by technology

Moreover, the demands on purity and surface area for use in electrolytic capacitors are very high.
However, one of the problems with producing tantalum powder having a uniform particle size is that a sodium reduction reaction of K2TaF7 is highly exothermic, with the reaction rate increasing as temperature increases.
This is significant since both temperature and reaction rate tend to have a negative effect on the uniformity of tantalum crystal growth, which in turn directly affects the uniformity of the resulting tantalum particles produced.
However, none of the prior art techniques are able to adequately control crystal growth such that the particle size distribution for the tantalum powder is optimized.

Method used

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  • Method for Combination Solid State and Molten Salt Tantalum Reduction
  • Method for Combination Solid State and Molten Salt Tantalum Reduction

Examples

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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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Abstract

A two-phase reduction method for producing tantalum powder includes loading an unheated reaction vessel with a layer of K2TaF7, then a layer of solid sodium metal, and then followed by a layer of solid diluent salt. A first heating phase is used to promote the solid state reduction of the layer of K2TaF7, which results in the production of very fine tantalum particles while minimizing tantalum crystal growth. A second heating phase is then used to melt the contents of the reactor vessel and react primary quantities of sodium metal and K2TaF7 to produce tantalum powder. In certain embodiments, the fine tantalum particles produced during the first heating phase serve as the nucleation sites needed for tantalum crystal growth in the second heating phase.

Description

FIELD OF THE INVENTION[0001]The present disclosure relates generally to tantalum reduction products and, more particularly, to a method for the reduction of tantalum using a combination solid state and molten salt tantalum reduction so as to control undesirable crystal growth in order to optimize the particle size distribution of tantalum powder.BACKGROUND OF THE INVENTION[0002]With evolution and microminiaturization of microprocessors and other electronics, the need for high-capacitance tantalum capacitors has rapidly increased. Moreover, the demands on purity and surface area for use in electrolytic capacitors are very high.[0003]In order to satisfy the need in the art for high-purity tantalum powder, potassium tantalum fluoride (K2TaF7) is generally reduced using sodium metal so as to form tantalum powder. One of the key qualities of tantalum powder is that it should have a very narrow particle size distribution. The optimum median particle size is a function of the intended form...

Claims

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Application Information

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IPC IPC(8): C22C27/02B22F9/20
CPCH01G9/0525B22F9/20
Inventor CRAWLEY, JOHN
Owner KEMET BLUE POWDER CORP
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