Fine particle recovery methods for valve metal powders
View Patent ↗A process and system for producing tantalum or other valve metal particles is provided comprising forming tantalum particles in a reduction process carried out in a reactor vessel, and using a siphon to transfer fine tantalum particles out of the reaction mixture to a recovery vessel. This particle transfer can occur while the reaction mixture is agitated. The tantalum particles can be automatically withdrawn when the reaction mixture has a depth level greater than the fluid level of the tantalum fine particle recovery vessel, and outflow automatically stops when the fluid levels of the reactor and particle recovery vessel equilibrate. Tantalum or other valve metal powders made by the processes, and capacitors made with valve metal powders are also provided.
1. Process for producing and recovery of tantalum particles, comprising:
forming tantalum particles by adding at least one reducing agent into a reaction mixture comprising a reducible tantalum halide and molten diluent salt in a reactor vessel to form fine tantalum particles;
transferring fine tantalum particles from said reaction mixture to outside the reactor vessel through a siphon comprising a tubular member having an inlet end positioned within the mixture for fine particle extraction from the reaction mixture and a discharge end located outside the vessel for fine particle recovery; and
further comprising positioning the inlet end of said siphon at a location within the reaction mixture where the transferred tantalum particles predominantly have a particle size less than about 2,000 nm, wherein the reaction mixture is at rest during said transferring of said fine tantalum particles.
2. The process of claim 1 , further comprising positioning the inlet end of said siphon at a depth within the reaction mixture where the transferred tantalum particles are predominantly primary particles.
3. Process for producing and recovery of tantalum particles, comprising:
forming tantalum particles by adding at least one reducing agent into a reaction mixture comprising a reducible tantalum halide and molten diluent salt in a reactor vessel while agitating the reaction mixture to form fine tantalum particles;
transferring fine tantalum particles from said reaction mixture to a recovery vessel separate from the reactor vessel through a siphon comprising a tubular member having an inlet end positioned within the reaction mixture and a discharge end located outside the vessel, wherein said transferring of said fine tantalum particles comprising outflowing of fluid containing fine tantalum particles from the reactor vessel to a separate recovery vessel via the siphon when the fluid level of the reaction mixture in the reactor vessel is higher than the fluid level in the recovery vessel and said outflowing discontinuing when the liquid level equals that of the recovery vessel; and
further comprising positioning the inlet end of said siphon at a location within the reaction mixture where the transferred tantalum particles predominantly have a particle size less than about 2,000 nm; and
further comprising positioning the recovery vessel within an overflow collector container, wherein outflow of said fluid from the reactor vessel to the recovery vessel when the fluid surface level in the reactor vessel exceeds the fluid level in the recovery vessel continues until fluid level of the recovery vessel reaches an upper open end thereof and overflows into the collector container and the fluid level in the reactor vessel falls to the level of said upper open end of the recovery vessel.
4. The process of claim 3 , further comprising positioning the inlet end of said siphon at a location within the reaction mixture where the transferred tantalum particles predominantly are primary particles.
5. The process of claim 3 , further comprising positioning the inlet end of said siphon at a location within the reaction mixture where at least 75 weight % of the transferred tantalum particles are primary particles.
6. The process of claim 3 , further comprising positioning the inlet end of said siphon at a location within the reaction mixture where the transferred tantalum particles predominantly have a particle size from about 1 nm to about 2,000 nm.
7. The process of claim 3 , wherein said adding of a reducible tantalum halide comprises adding potassium fluorotantalate.
8. The process of claim 3 , wherein said forming comprising dissolving K 2 TaF 7 in molten alkali halide diluent salt, and adding sodium to reduce K 2 TaF 7 to Ta particles.
9. The process of claim 3 , wherein the diluent salt is potassium chloride, potassium fluoride, sodium chloride, sodium fluoride, or combinations thereof.
10. The process of claim 3 , further comprising maintaining the reaction mixture at a temperature of about 770° C. to about 880° C.
11. The process of claim 3 , further comprising washing and heat treating said transferred fine particles to form a tantalum powder.