Methods Of Making A Niobium Metal Oxide and Oxygen Reduced Niobium Oxides

Abstract

Methods to at least partially reduce a niobium oxide are described wherein the process includes mixing the niobium oxide and niobium powder to form a powder mixture that is then heat treated to form heat treated particles which then undergo reacting in an atmosphere which permits the transfer of oxygen atoms from the niobium oxide to the niobium powder, and at a temperature and for a time sufficient to form an oxygen reduced niobium oxide. Oxygen reduced niobium oxides having high porosity are also described as well as capacitors containing anodes made from the oxygen reduced niobium oxides.

1 - 66 . (canceled) 
     
     
         67 . A method to control porosity in pressed and sintered valve metal sub-oxide powders comprising adjusting the granule size and/or pre-heat treatment temperature of said valve metal sub-oxide to obtain a pre-determined porosity. 
     
     
         68 . A method of making valve metal oxide particles, comprising:
 heat treating a starting valve metal oxide under vacuum or inert conditions to form agglomerated particles; and optionally   deagglomerating said agglomerated particles.   
     
     
         69 - 91 . (canceled) 
     
     
         92 . The valve metal oxide particles formed by the method of  claim 68 . 
     
     
         93 . A capacitor comprising the valve metal oxide particles of  claim 92 . 
     
     
         94 . The capacitor of  claim 93 , wherein said capacitor has a capacitance of from about 40,000 to about 300,000 CV/g. 
     
     
         95 . The capacitor of  claim 94 , wherein said capacitor has a DC leakage of from about 0.05 to about 5 nA/CV. 
     
     
         96 . The method of  claim 68 , further comprising at least partially reducing said valve metal oxide particles to form an oxygen reduced valve metal oxide. 
     
     
         97 . The oxygen reduced valve metal formed by the method of  claim 96 . 
     
     
         98 . A capacitor comprising the oxygen reduced valve metal of  claim 97 . 
     
     
         99 . The capacitor of  claim 98 , wherein said capacitor has a capacitance of from about 40,000 to about 300,000 CV/g. 
     
     
         100 . The capacitor of  claim 98 , wherein said capacitor has a DC leakage of from about 0.05 to about 5 nA/CV. 
     
     
         101 . (canceled) 
     
     
         102 . A method of making agglomerated particles, comprising heat treating a starting valve metal oxide to form agglomerated particles, wherein said agglomerated particles have a pore size distribution that is at least 10% greater than a pore size distribution of said starting valve metal oxide, and wherein said agglomerated particles have a BET surface area that is at least 90% of a BET surface area of said starting valve metal oxide. 
     
     
         103 - 116 . (canceled) 
     
     
         117 . The agglomerated particles formed by the method of  claim 102 . 
     
     
         118 . A capacitor comprising the agglomerated particles of  claim 117 . 
     
     
         119 . The capacitor of  claim 118 , wherein said capacitor has a capacitance of from about 40,000 to about 300,000 CV/g. 
     
     
         120 . The capacitor of  claim 118 , wherein said capacitor has a DC leakage of from about 0.05 to about 5 nA/CV. 
     
     
         121 . The method of  claim 102 , further comprising at least partially reducing said agglomerated particles to form an oxygen reduced valve metal oxide. 
     
     
         122 . The oxygen reduced valve metal formed by the method of  claim 121 . 
     
     
         123 . A capacitor comprising the oxygen reduced valve metal of  claim 122 . 
     
     
         124 . The capacitor of  claim 123 , wherein said capacitor has a capacitance of from about 40,000 to about 300,000 CV/g. 
     
     
         125 . The capacitor of  claim 123 , wherein said capacitor has a DC leakage of from about 0.05 to about 5 nA/CV. 
     
     
         126 - 226 . (canceled) 
     
     
         227 . Oxygen reduced niobium oxide granules, wherein the oxygen reduced niobium oxide granules have a multi-modal pore size distribution of from about 0.1 to about 20 microns, after being pressed and sintered, and are formed from oxygen reduced niobium oxide having a BET surface area of from about 0.5 to about 8 m 2 /g, wherein said granules after being pressed and sintered have a bimodal pore size distribution of from about 0.1 to about 10 microns.