High purity niobium and products containing the same, and methods of making the same

Abstract

High purity niobium metals and alloys containing the same are described. The niobium metal preferably has a purity of at least 99.99% and more preferably at least 99.999%. In addition, niobium metal and alloys thereof are described, which either have a grain size of about 150 microns or less, or a texture in which a (100) intensity within any 5% increment of thickness is less than about 30 random, or an incremental log ratio of (111):(100) intensity of greater than about −4.0, or any combination of these properties. Also described are articles and components made from the niobium metal which include, but are not limited to, sputtering targets, capacitor cans, resistive film layers, wire, and the like. Also disclosed is a process for making the high purity niobium metal which includes the step of reacting a salt-containing niobium and a metal salt along with at least one compound capable of reducing the salt-containing niobium to niobium and in a reaction container. The reaction container or liner in the reaction container and the agitator or liner on the agitator are made from a metal material having the same or higher vapor pressure of melted niobium. The high purity niobium product preferably has a fine and uniform microstructure.

1 - 27 . (canceled)  
   
   
       28 . Niobium metal having a) an average grain size of about 150 microns or less, or b) a texture in which a (100) pole figure has a center peak intensity equal to or less than about 30 random or c) a log ratio of (111):(100) center peak intensities of greater than about −4.0, or combinations thereof.  
   
   
       29 - 41 . (canceled)  
   
   
       42 . A sputtering target comprising the niobium metal of  claim 28 .  
   
   
       43 . (canceled)  
   
   
       44 . A process for making niobium metal, comprising reacting a salt containing niobium and a metal salt with at least one agent capable of reducing the salt containing niobium to niobium in a reaction container having an agitator, wherein the reaction container or a liner in the reaction container and the agitator or a liner on the agitator are made from a metal material having the same or higher vapor pressure of niobium at the melting point of the niobium.  
   
   
       45 . The process of  claim 44 , wherein the salt containing niobium comprises niobium oxide and the metal salt comprises potassium-tantalum fluoride and the agent comprises sodium.  
   
   
       46 . The process of  claim 45 , further comprising adding at least one diluent salt comprising sodium fluoride and/or sodium chloride to said agitator.  
   
   
       47 . The process of  claim 44 , wherein the reaction container or liner and the agitator or liner on the agitator are metal-based, wherein said metal is nickel, chromium, iron, manganese, titanium, zirconium, hafnium, vanadium, technetium, ruthenium, cobalt, rhodium, palladium, platinum, or any combination thereof.  
   
   
       48 . The process of  claim 47 , wherein the metal is nickel or a nickel-based alloy.  
   
   
       49 . The process of  claim 47 , wherein the metal is chromium or a chromium-based alloy.  
   
   
       50 . The process of  claim 47 , wherein the metal is iron or an iron-based alloy.  
   
   
       51 . The process of  claim 44 , further comprising recovering niobium by dissolving the second salt in an aqueous solution.  
   
   
       52 . The process of  claim 51 , further comprising melting said recovered niobium and optionally said metal from said metal salt in a sufficient vacuum to remove substantially any existing impurities in said recovered niobium and obtain high purity niobium and optionally said metal.  
   
   
       53 . The process of  claim 52 , wherein the vacuum is 10 −4  torr or more.  
   
   
       54 . The process of  claim 52 , wherein the pressure above the melted recovered niobium is lower than the vapor pressures of substantially all of the impurities.  
   
   
       55 . The process of  claim 52 , wherein the impurities are removed by vaporization of the impurities.  
   
   
       56 . The process of  claim 52 , wherein said melting is accomplished by electron beam melting.  
   
   
       57 . The process of  claim 52 , wherein said melting is accomplished by vacuum arc remelt processing.  
   
   
       58 . The process of  claim 52 , wherein the high purity niobium is allowed to form a solid and subjected to a rolling process, a forging process, or both.  
   
   
       59 - 73 . (canceled)  
   
   
       74 . A niobium sputtering component comprising an average grain size of about 150 microns or less and a uniform texture of primary (111) throughout a thickness of the component.