High voltage tantalum anode and method of manufacture

Abstract

Tantalum powders produced using a tantalum fiber precursor are described. The tantalum fiber precursor is chopped or cut into short lengths having a uniform fiber thickness and favorable aspect ratio. The chopped fibers are formed into a primary powder having a controlled size and shape, narrow/tight particle size distribution, and low impurity level. The primary powder is then agglomerated into an agglomerated powder displaying suitable flowability and pressability such that pellets with good structural integrity and uniform pellet porosity are manufacturable. The pellet is sintered and anodized to a desired formation voltage. The thusly created capacitor anode has a dual morphology or dual porosity provided by a primary porosity of the individual tantalum fibers making up the primary powder and a larger secondary porosity formed between the primary powders agglomerated into the agglomerated powder.

What is claimed is: 
     
       1. A capacitorassembly, comprising:
 a) a casing comprising first and second inner wall surfaces; 
 b) at least a first tantalum anode housed inside the casing, wherein:
 i) the first tantalum anode is characterized as having been fabricated from tantalum fibers having a diameter ranging from 0.5 μm to 2.5 μm and a length ranging from 5 μm to 50 μm so that the tantalum fibers have a length: diameter (L/D) aspect ratio ranging from 2 to 100, the tantalum fibers forming a tantalum powder as a loosely packed mass of the tantalum fibers, and 
 ii) wherein the tantalum powder is characterized as having been agglomerated into a randomly oriented, substantially non-aligned, porous agglomerated tantalum powder having a primary porosity density ranging from 1.5 g/cc to 4.5 g/cc, which agglomerated tantalum powder is characterized as having been pressed into a tantalum pellet having a secondary porosity density ranging from 4 g/cc to 6.5 g/cc, and 
 iii) wherein the tantalum pellet is characterized as having been sintered so that the sintered tantalum pellet has:
 A) an inter-granule pore size distribution attributed to the primary porosity of a sintered density at:
 d10 of ranging from 0.5 μm to 2 μm; and 
 d90 of ranging from 3 μm to 10 μm; and 
 
 B) an intra-granule pore size distribution attributed to the secondary porosity of sintered density at:
 d10 of ranging from 20 μm to 40 μm; and 
 d90 of ranging from 60 μm to 100 μm; and 
 
 
 iv) the sintered pellet is characterized as having then been anodized to a formation voltage greater than zero up to 550 V to form a dielectric oxide on the tantalum fibers and thereby provide the tantalum anode; 
 
 c) an insulative seal comprising a feedthrough wire electrically connected to the first tantalum anode, wherein the feedthrough wire extends outside the casing and is electrically isolated from the casing; 
 d) a cathode comprising cathode active material supported by and in electrical contact with the first inner wall surface and with the second inner wall surface of the casing; 
 e) a separator preventing direct physical contact between the first tantalum anode and the cathode active material supported on the first and second inner wall surfaces of the casing while allowing for ion flow therethrough; and 
 f) an electrolyte contacting the cathode and the first anode. 
 
     
     
       2. The capacitor of  claim 1 , including a second tantalum anode housed inside the casing, wherein the second tantalum anode is electrically connected in parallel with the first tantalum anode, and wherein a cathode current collector comprising opposed major current collector faces supporting the cathode active material is disposed intermediate the first and second tantalum anodes. 
     
     
       3. The capacitor of  claim 1 , wherein there are “n” tantalum anodes electrically connected in parallel with each other and housed inside the casing, and wherein there are n−1 cathode current collectors supporting the cathode active material on opposed major current collector faces thereof and disposed intermediate side-by-side adjacent ones of the n tantalum anodes. 
     
     
       4. The capacitor of  claim 1 , wherein the casing comprises a first casing member having a first face wall joined to a surrounding side wall and a second casing member having a second face wall secured to the surrounding side wall of the first casing member. 
     
     
       5. The capacitor of  claim 1 , wherein the feedthrough wire is connected to the first tantalum anode and a wire extends from the first tantalum anode to the second tantalum anode to electrically connect the first and second tantalum anodes in parallel. 
     
     
       6. The capacitor of  claim 1  wherein the tantalum fibers comprising the tantalum powder have a length-to-diameter (L/D) aspect ratio ranging from 2 to 100. 
     
     
       7. The capacitor of  claim 1 , wherein the tantalum fibers comprising the tantalum powder have a L/D aspect ratio ranging from 10 to 40. 
     
     
       8. The capacitor of  claim 1 , wherein the agglomerated tantalum powder has substantially no fines less than 200 mesh. 
     
     
       9. The capacitor of  claim 1  wherein, prior to being sintered and anodized to form the first tantalum anode, the tantalum pellet has a pressed density of 3 g/cc to 8 g/cc. 
     
     
       10. The capacitor of  claim 1  wherein, prior to being sintered and anodized to form the first tantalum anode, the tantalum pellet has a pressed density of 4 g/cc to 6.5 g/cc. 
     
     
       11. The capacitor of  claim 1 , wherein the tantalum pellet is characterized as having been sintered at a temperature ranging from 1,200° C. to 2,200° C., for a time ranging from 0.1 to 120 minutes, and at a vacuum of <1×10 −4  Torr (Argon). 
     
     
       12. The capacitor of  claim 1 , wherein the tantalum pellet is characterized as having been sintered at a temperature ranging from 1,500° C. to 1,850° C., for a time ranging from 1 to 10 minutes, and at a vacuum of <1×10 −5  Torr (Argon). 
     
     
       13. The capacitor of  claim 1 , wherein, prior to being anodized to form the first tantalum anode, the sintered tantalum pellet has a the sintered density ranging from 4 g/cc to 9 g/cc. 
     
     
       14. The capacitor of  claim 1 , wherein, prior to being anodized to form the first tantalum anode, the sintered tantalum pellet has a the sintered density ranging from 5 g/cc to 8 g/cc. 
     
     
       15. The capacitor of  claim 1 , wherein, prior to being anodized to form the first tantalum anode, the sintered tantalum pellet has a d50 an inter-granule pore size distribution attributed to the primary porosity of sintered density at d50 ranging from 1 μm to 5 μm, and a d50 an intra-granule pore size distribution attributed to the secondary porosity of sintered density at d50 ranging from 30 μm to 80 μm. 
     
     
       16. The capacitor of  claim 1  wherein, prior to being pressed into the tantalum pellet, the agglomerated tantalum powder has an agglomerate density ranging from 1.5 g/cc to 4.5 g/cc. 
     
     
       17. The capacitor of  claim 1 , wherein, prior to being pressed into the tantalum pellet, the agglomerated tantalum powder is has an agglomerate a primary density ranging from 2.5 g/cc to 3.5 g/cc. 
     
     
       18. The capacitor of  claim 1 , wherein, prior to being pressed into the tantalum pellet, the agglomerated tantalum powder has an agglomerate diameter of distribution at:
 i) d10 of 74 μm; 
 ii) d50 ranging from 200 μm to 500 μm; and 
 iii) d90 of 1,000 μm. 
 
     
     
       19. The capacitor of  claim 1 , wherein, prior to being pressed into the tantalum pellet, the agglomerated tantalum powder has a d50 inter-granular pore size attributed to the primary porosity of agglomerate pore size ranging from 1 μm to 5 μm. 
     
     
       20. The capacitor of  claim 1 , wherein, prior to being pressed into the tantalum pellet, the agglomerated tantalum powder has a d50 inter-granular pore size attributed to the primary porosity of agglomerate pore size ranging from 2 μm to 3 μm. 
     
     
       21. The capacitor of  claim 1 , wherein, prior to being pressed into the tantalum pellet, the agglomerated tantalum powder has an inter-granular pore size attributed to the primary porosity of agglomerate pore size distribution at d10 of 0.5 μm and at d90 of 20 μm. 
     
     
       22. The capacitor of  claim 1 , wherein the sintered tantalum pellet is characterized as having been anodized in an electrolyte comprising H 3 PO 4  and having a conductivity up to about 20,000 μS at 40° C. 
     
     
       23. A capacitorassembly, comprising:
 a) a casing comprising first and second inner wall surfaces; 
 b) at least a first tantalum anode and a second tantalum anode electrically connected in parallel and housed inside the casing, wherein:
 i) the parallel connected first and second tantalum anodes are characterized as each having been fabricated from tantalum fibers having a diameter ranging from 0.5 μm to 2.5 μm and a length ranging from 5 μm to 50 μm so that the tantalum fibers have a length: diameter aspect ratio ranging from 2 to 100, the tantalum fibers forming a tantalum powder as a loosely packed mass of the tantalum fibers, and 
 ii) wherein the tantalum powder is characterized as having been agglomerated into a randomly oriented, substantially non-aligned, porous agglomerated tantalum powder having a primary porosity density ranging from 1.5 g/cc to 4.5 g/cc, which agglomerated tantalum powder is characterized as having been pressed into a first tantalum pellet and into a second tantalum pellet, both pellets having a secondary porosity density ranging from 4 g/cc to 6.5 g/cc, and 
 iii) wherein the first and second tantalum pellets are characterized as having been sintered so that the sintered first and second tantalum pellets each have:
 A) an inter-granule pore size distribution attributed to the primary porosity of a sintered density at:
 d10 of ranging from 0.5 μm to 2 μm; and 
 d50 ranging from 1 μm to 5 μm; and 
 d90 of ranging from 3 μm to 10 μm; and 
 
 B) an intra-granule pore size distribution attributed to the secondary porosity of sintered density at:
 d10 of ranging from 20 μm to 40 μm; and 
 d50 ranging from 30 μm to 80 μm; and  
 d90 of ranging from 60 μm to 100 μm; and 
 
 
 iv) the sintered first and second tantalum pellets are characterized as having then been anodized to a formation voltage greater than zero up to 550 V to form a dielectric oxide on the tantalum fibers and thereby provide the first and second tantalum anodes; 
 
 c) an insulative seal comprising a feedthrough wire electrically connected to at least the first tantalum anode, wherein the feedthrough wire extends outside the casing and is electrically isolated from the casing; 
 d) a cathode comprising cathode active material supported by and in electrical contact with the first inner wall surface and with the second inner wall surface of the casing; 
 e) a cathode current collector comprising opposed major current collector faces supporting the cathode active material and being disposed intermediate the first and second tantalum anodes; 
 f) a separator material preventing direct physical contact between the first and second tantalum anodes and the cathode active material supported on the first and second inner wall surfaces of the casing, and between the first and second tantalum anodes and the cathode active material supported on the cathode current collector, the separator material allowing for ion flow through; and 
 g) an electrolyte contacting the cathode and the first and second anodes. 
 
     
     
       24. A capacitorassembly, comprising:
 a) a casing comprising first and second inner wall surfaces; 
 b) “n” tantalum anodes electrically connected in parallel and housed inside the casing, wherein:
 i) the parallel connected n tantalum anodes are each characterized as having been fabricated from tantalum fibers having a diameter ranging from 0.5 μm to 2.5 μm and a length ranging from 5 μm to 50 μm so that the tantalum fibers have a length: diameter aspect ratio ranging from 2 to 100, the tantalum fibers forming a tantalum powder as a loosely packed mass of the tantalum fibers, 
 ii) wherein the tantalum powder is characterized as having been agglomerated into a randomly oriented, substantially non-aligned, porous agglomerated tantalum powder having a primary porosity density ranging from 1.5 g/cc to 4.5 g/cc, which agglomerated tantalum powder is characterized as having been pressed into “n” tantalum pellets, each of the n pellets having a secondary porosity density ranging from 4 g/cc to 6.5 g/cc, and 
 iii) wherein the n tantalum pellets are characterized as having been sintered so that the sintered tantalum pellets have:
 A) an inter-granule pore size distribution attributed to the primary porosity of a sintered density at:
 d10 of ranging from 0.5 μm to 2 μm; and 
 d50 ranging from 1 μm to 5 μm; and  
 d90 of ranging from 3 μm to 10 μm; and 
 
 B) an intra-granule pore size distribution attributed to the secondary porosity of sintered density at:
 d10 of ranging from 20 μm to 40 μm; and 
 d50 ranging from 10 μm to 80 μm; and 
 d90 of ranging from 60 μm to 100 μm; and 
 
 
 iv) the sintered pellets are characterized as having then been anodized to a formation voltage greater than zero of at least 300 V up to 550 V to form a dielectric oxide on the tantalum fibers and thereby provide the n tantalum anodes; 
 
 c) an insulative seal comprising a feedthrough wire electrically connected to at least a first one of the n tantalum anodes, wherein the feedthrough wire extends outside the casing and is electrically isolated from the casing; 
 d) a cathode comprising cathode active material supported by and in electrical contact with the first inner wall surface and with the second inner wall surface of the casing; 
 e) n−1 cathode current collectors housed inside the casing, each cathode current collector comprising opposed major current collector faces supporting cathode active material and being disposed intermediate side-by-side adjacent ones of the n tantalum anodes; 
 f) a separator material preventing direct physical contact between the tantalum anodes and the cathode active material supported on the first and second inner wall surfaces of the casing, and between the tantalum anodes and the cathode active material supported on the n−1 cathode current collectors, the separator material allowing for ion flow through; and 
 g) an electrolyte contacting the cathodes and the anodes. 
 
     
     
       25. A tantalum anode for incorporation into a capacitor, the tantalum anode comprising:
 a) tantalum fibers having a diameter ranging from 0.5 μm to 2.5 μm and a length ranging from 5 μm to 50 μm so that the tantalum fibers have a length: diameter aspect ratio ranging from 2 to 100, wherein the tantalum fibers form a tantalum powder as a loosely packed mass of the tantalum fibers, and 
 b) wherein the tantalum powder is characterized as having been agglomerated into a randomly oriented, substantially non-aligned, porous agglomerated tantalum powder having a primary porosity density ranging from 1.5 g/cc to 4.5 g/cc, which agglomerated tantalum powder is characterized as having been pressed into a tantalum pellet having a secondary porosity density ranging from 4 g/cc to 6.5 g/cc, and 
 c) wherein the tantalum pellet is characterized as having been sintered so that the sintered tantalum pellet has:
 i) an inter-granule pore size distribution attributed to the primary porosity of a sintered density at:
 d10 of ranging from 0.5 μm to 2 μm; and 
 d50 ranging from 1 μm to 5 μm; and 
 d90 of ranging from 3 μm to 10 μm; and 
 
 ii) an intra-granule pore size distribution attributed to the secondary porosity of sintered density at:
 d10 of ranging from 20 μm to 40 μm; and 
 d50 ranging from 30 μm to 80 μm; and 
 d90 of 60 μm to 100 μm; and 
 
 
 d) the sintered pellet is characterized as having then been anodized to a formation voltage greater than zero of at least 300 V up to 550 V to form a dielectric oxide on the tantalum fibers and thereby provide the tantalum anode. 
 
     
     
       26. A method for providing a tantalum anode for an electrolytic capacitor, the method comprising the steps of:
 a) providing tantalum fibers having a diameter ranging from 0.5 μm to 2.5 μm and a length ranging from 5 μm to 50 μm so that the tantalum fibers have a length: diameter aspect ratio ranging from 2 to 100; 
 b) providing a tantalum powder as a loosely packed mass of the tantalum fibers; 
 c) agglomerating the tantalum powder into a randomly oriented, substantially non-aligned, porous agglomerated tantalum powder having a primary porosity density ranging from 1.5 g/cc to 4.5 g/cc; 
 d) pressing the agglomerated tantalum powder into a tantalum pellet of a desired shape, the tantalum pellet having a secondary porosity density ranging from 4 g/cc to 6.5 g/cc; 
 e) sintering the tantalum pellet into a coalesced body of the tantalum fibers to thereby provide a sintered tantalum pellet having:
 i) an inter-granule pore size distribution attributed to the primary porosity of a sintered density at:
 d10 of ranging from 0.5 μm to 2 μm; and 
 d50 ranging from 1 μm to 5 μm; and 
 d90 of ranging from 3 μm to 10 μm; and 
 
 ii) an intra-granule pore size distribution attributed to the secondary porosity of sintered density at:
 d10 of ranging from 20 μm to 40 μm; and 
 d50 ranging from 30 μm to 80 μm; and 
 d90 of ranging from 60 μm to 100 μm; and 
 
 
 f) anodizing the sintered tantalum pellet to a formation voltage greater than zero up to 550 V to form a dielectric oxide on the tantalum fibers and thereby provide the tantalum anode. 
 
     
     
       27. The method of  claim 26 , including providing the tantalum fibers comprising the tantalum powder having a L/D aspect ratio ranging from 10 to 40. 
     
     
       28. The method of  claim 26 , including providing the agglomerated tantalum powder having substantially no fines less than 200 mesh. 
     
     
       29. The capacitor of claim 1, wherein the sintered tantalum pellet is characterized as having been anodized to a formation voltage that is at least 300 V up to 550 V. 
     
     
       30. The capacitor of claim 23, wherein the first and second sintered tantalum pellets are characterized as having been anodized to a formation voltage that is at least 300 V up to 550 V. 
     
     
       31. The method of claim 26, including anodizing the sintered tantalum pellet to a formation voltage that is at least 300 V up to 550 V.