Method for the production of valve metal powders
View Patent ↗The present invention relates to a process for the deoxidation of valve metal primary powders by means of reducing metals and/or metal hydrides, and a process for the production of tantalum powders that are suitable as anode material for electrolytic capacitors.
1. A process for producing a deoxidized valve metal powder which comprises subjecting a valve metal powder to a deoxidation to remove residual oxygen which comprises a reducing metal and/or its hydride, wherein the deoxidation is carried out without contact between the valve metal powder to be deoxidized and a liquid reducing metal and/or metal hydride and wherein the deoxidation is carried out under an inert carrier gas at a pressure of 100 to 450 hPa and at a temperature between 690° C. to 800° C. wherein the oxygen content of the valve metal to be deoxidized is 2500 μg/m 2 to 3600 μg/m 2 and wherein the reducing metal and/or metal hydride and the valve metal powder to be deoxidized are placed at separate points in a reactor so that the reducing metal /metal hydride comes into contact with the valve metal powder only via the gaseous phase, and wherein the valve metal powder has a specific surface and the specific surface is reduced by less than a factor of 2 during deoxidation.
2. The process as claimed in claim 1 , wherein said metal is aluminum, magnesium, calcium, barium and/or lanthanum and/or its hydride.
3. The process according to claim 1 , wherein the deoxidation is carried out at a partial vapor pressure of the reducing metal/metal hydride of 5 to 110 hPa.
4. The process according to claim 3 , wherein the vapor pressure of the reducing metal/metal hydride is less than 100 hPa.
5. The process according to claim 3 , wherein the vapor pressure of the reducing metal is between 30 and 80 hPa.
6. The process according to claim 1 , wherein said valve metal powder is titanium, zirconium, hafnium, vanadium, niobium, tantalum, molybdenum and/or tungsten powder.
7. The process according to claim 6 , wherein said valve powder is niobium powder.
8. The process according to claim 6 , wherein said valve powder is tantalum.
9. The process according to claim 1 , wherein said reducing metal or said metal hydride is magnesium and/or magnesium hydride.
10. The process according to claim 1 , wherein the deoxidation is carried out under an inert carrier gas at a pressure of 100 to 450 hPa.
11. The process according to claim 1 , wherein the deoxidation is carried out under an inert carrier gas at a pressure of 200 to 400 hPa.
12. The process according to claim 1 , which comprises reducing the metal hydride under an inert carrier gas, wherein the deoxidation is carried without contact between the valve metal powder to be deoxidized and liquid reducing metal hydride and wherein the deoxidation is carried out under an inert carrier gas at a pressure of 50 to 500 hPa and wherein the oxygen content of the valve metal to be deoxidized is 2400 μg/m 2 to 4500 μg/m 2 .
13. The process according to claim 12 , wherein said metal hydride is magnesium and/or magnesium hydride.
14. The process according to claim 1 , wherein said valve metal powder is a tantalum powder with a specific surface of 4 to 8 m 2 /g, which after pressing at a pressing density of 5 g/cm 3 and sintering at 1210° C. over 10 minutes has, after forming up to a forming voltage of 10V, a capacity of 220,000 to 350,000 μFV/g.
15. The process according to claim 1 , wherein said valve metal powder is a tantalum powder with a specific surface of 3.5 to 6 m 2 /g, which after pressing at a pressing density of 5 g/cm 3 and sintering at 1210° C. over 10 minutes has, after forming up to a forming voltage of 10V, a capacity of 180,000 to 250,000 μFV/g.
16. The process according to claim 1 , wherein the deoxidation is carried without contact between the valve metal powder to be deoxidized and liquid reducing metal hydride and wherein the deoxidation is carried out under an inert carrier gas at a pressure of 100 to 450 hPa and a temperature from 690 to 800 ° C. wherein the oxygen content of the valve metal to be deoxidized is 2500 μg/m 2 to 3600 μg/m 2 .
17. The process according to claim 1 , wherein the deoxidation is carried without contact between the valve metal powder to be deoxidized and liquid reducing metal hydride and wherein the deoxidation is carried out under an inert carrier gas at a pressure of 200 to 400 hPa and a temperature from 690 to below 760 ° C. wherein the oxygen content of the valve metal to be deoxidized is 2600 μg/m 2 to 3100 μg/m 2 .
18. The process according to claim 1 , wherein the oxygen content of the valve metal to be deoxidized is less than 3000 μg/m 2 .