Production of high-purity niobium monoxide and capacitor production therefrom

Abstract

The present invention relates to high-purity niobium monoxide powder (NbO) produced by a process of combining a mixture of higher niobium oxides and niobium metal powder or granules; heating and reacting the compacted mixture under controlled atmosphere to achieve temperature greater than about 1945° C., at which temperature the NbO is liquid; solidifying the liquid NbO to form a body of material; and fragmenting the body to form NbO particles suitable for application as capacitor anodes. The NbO product is unusually pure in composition and crystallography, and can be used for capacitors and for other electronic applications. The method of production of the NbO is robust, does not require high-purity feedstock, and can reclaim value from waste streams associated with the processing of NbO electronic components. The method of production also can be used to make high-purity NbO 2 and mixtures of niobium metal/niobium monoxide and niobium monoxide/niobium dioxide. The method further is ideal for doping of the product oxides to enhance particular characteristics of the materials. The method further allows the production of single crystal or directionally-solidified ingots. In contrast to the spongy, highly porous agglomerates produced by other techniques, the present invention produces solid, non-porous ingots that can be fragmented to fine, non-porous angular particles suitable for electronic applications.

1 . A high-purity niobium monoxide (NbO) powder, produced by a process comprising: 
 a) combining a mixture of (1) a niobium oxide selected from the group consisting of Nb 2 O 5 , NbO 2 , and/Nb 2 O 3 , and (2) metallic niobium;    b) forming a compact of said mixture;    c) reacting the mixture with a heat source such that a temperature greater than 1945° C. is achieved;    d) solidifying the reacted mixture to form a body of material; and    e) fragmenting the body to form niobium monoxide powder.    
     
     
         2 . The niobium monoxide powder as recited in  claim 1 , wherein the mass ratio of Nb 2 O 5  to niobium metal powder or granules in the mixture is about 1:1.  
     
     
         3 . The niobium monoxide powder as recited in  claim 1 , wherein the mass ratio of NbO 2  to niobium metal powder or granules in the mixture is about 1.3:1.  
     
     
         4 . The niobium monoxide powder as recited in  claim 1 , wherein the mass ratio of Nb 2 O 3  to niobium metal or granules in the mixture is about 2.5:1.  
     
     
         5 . The niobium monoxide powder as recited in  claim 1 , wherein the niobium oxide is Nb 2 O 5 .  
     
     
         6 . The niobium monoxide powder as recited in  claim 1 , wherein the heat source is an electron beam furnace.  
     
     
         7 . The niobium monoxide powder as recited in  claim 1 , wherein the heat source is a plasma-arc furnace.  
     
     
         8 . The niobium monoxide powder as recited in  claim 1 , wherein the heat source is an induction furnace.  
     
     
         9 . The niobium monoxide powder as recited in  claim 1 , wherein the heat source is an electric resistance furnace.  
     
     
         10 . The niobium monoxide powder as recited in  claim 1 , wherein the heat source is a vacuum arc remelting furnace.  
     
     
         11 . The niobium monoxide powder as recited in  claim 1 , wherein the reaction process achieves a temperature greater than or equal to 1945° C.  
     
     
         12 . The niobium monoxide powders as recited in  claim 1 , wherein the mixture further comprises niobium monoxide revert, niobium metal lead wire, or other niobium-containing waste products.  
     
     
         13 . The niobium monoxide powders as recited in  claim 1 , wherein the niobium oxide and metallic niobium are present in substantially powder or granular form.  
     
     
         14 . A method of producing niobium monoxide ingots or powder which comprises: 
 a) combining a mixture of (1) a niobium oxide selected from the group consisting of Nb 2 O 5 , NbO 2 , and/Nb 2 O 3 , and (2) metallic niobium, wherein the niobium oxide and metallic niobium are present in powder or granular form;    b) forming a compact of said mixture;    c) reacting the mixture with a heat source such that a temperature greater than 1945° C. is achieved;    d) solidifying the reacted mixture to form a body of material; and    e) fragmenting the body of material to form the NbO powder.    
     
     
         15 . The method as recited in  claim 14 , wherein the mass ratio of Nb 2 O 5  to niobium metal powder or granules in the mixture is about 1:1.  
     
     
         16 . The method as recited in  claim 14 , wherein the mass ratio of NbO 2  to niobium metal powder or granules in the mixture is about 1.3:1.  
     
     
         17 . The method as recited in  claim 14 , wherein the mass ratio of Nb 2 O 3  to niobium metal or granules in the mixture is about 2.5:1.  
     
     
         18 . The method as recited in  claim 14 , wherein the niobium oxide is Nb 2 O 5 .  
     
     
         19 . The method as recited in  claim 14 , wherein the reaction achieves a temperature of 1945° C. or greater.  
     
     
         20 . The method as recited in  claim 14 , wherein the heat source is an electron beam furnace.  
     
     
         21 . The method as recited in  claim 14 , wherein the heat source is a plasma-arc furnace.  
     
     
         22 . The method as recited in  claim 14 , wherein the heat source is an induction furnace.  
     
     
         23 . The method as recited in  claim 14 , wherein the heat source is a vacuum arc remelting furnace.  
     
     
         24 . The method as recited in  claim 14 , wherein the mixture further comprises niobium monoxide revert, niobium metal lead wire, or other niobium-containing waste products.  
     
     
         25 . A high-purity niobium monoxide (NbO) ingot, produced by a process comprising: 
 a) combining a mixture of (1) a niobium oxide selected from the group consisting of Nb 2 O 5 , NbO 2 , and/Nb 2 O 3 , and (2) metallic niobium;    b) forming a compact of said mixture;    c) reacting the mixture with a heat source such that a temperature greater than 1945° C. is achieved; and    d) solidifying the reacted mixture to form a body of material.    
     
     
         26 . The niobium monoxide ingot as recited in  claim 25 , wherein the weight ratio of Nb 2 O 5  to metallic niobium in the mixture is about 1:1.  
     
     
         27 . The niobium monoxide ingot as recited in  claim 25 , wherein the weight ratio of NbO 2  to metallic niobium in the mixture is about 1.3:1.  
     
     
         28 . The niobium monoxide ingot as recited in  claim 25 , wherein the weight ratio of Nb 2 O 3  to metallic niobium in the mixture is about 1.25:1.  
     
     
         29 . The niobium monoxide ingot as recited in  claim 25 , wherein the niobium oxide is Nb 2 O 5 .  
     
     
         30 . The niobium monoxide ingot as recited in  claim 25 , wherein the heat source is an electron beam furnace.  
     
     
         31 . The niobium monoxide ingot as recited in  claim 25 , wherein the heat source is a plasma-arc furnace.  
     
     
         32 . The niobium monoxide ingot as recited in  claim 25 , wherein the heat source is an induction furnace.  
     
     
         33 . The niobium monoxide ingot as recited in  claim 25 , wherein the heat source is an electric resistance furnace.  
     
     
         34 . The niobium monoxide ingot as recited in  claim 25 , wherein the heat source is a vacuum arc remelting furnace.  
     
     
         35 . The niobium monoxide ingot as recited in  claim 25 , wherein electronic valves are produced from the niobium monoxide ingots.  
     
     
         36 . The niobium monoxide ingot as recited in  claim 25 , wherein slices cut from ingots or parts of ingots are used as mounting surfaces for electronic devices.  
     
     
         37 . The niobium monoxide ingot as recited in  claim 25 , wherein the mixture is adjusted to yield NbO 2 .  
     
     
         38 . The niobium monoxide ingot as recited in  claim 25 , wherein the niobium oxide and metallic niobium are present in powder or granular form.