High density, low oxygen re and re-based consolidated powder materials for use as deposition sources & methods of making same

Abstract

A method of making Re and Re-based materials comprises steps of: providing a Re powder starting material or a Re powder starting material and at least one additional powder material; subjecting at least the Re powder to a first degassing treatment for reducing the oxygen content thereof; increasing the density of the degassed Re powder or a mixture of the degassed Re powder and the at least one additional powder material to form a green billet; subjecting the billet to a second degassing treatment to further reduce the oxygen content; and consolidating the billet to form a consolidated material with greater than about 95% of theoretical density and low oxygen content below about 200 ppm for Re and below about 500 ppm for Re-based materials formed from the mixture, excluding oxygen from non-metallic compounds and ceramics. Materials so produced are useful in the manufacture of deposition sources such as sputtering targets.

1 . A method comprising steps of:
 (a) providing a Re powder starting material or a Re powder starting material and at least one additional powder material;   (b) subjecting at least said Re powder to a first degassing treatment for reducing the oxygen content thereof;   (c) increasing the density of said degassed Re powder or a mixture of said degassed Re powder and said at least one additional powder material to form a green billet;   (d) subjecting said green billet to a second degassing treatment to further reduce the oxygen content thereof; and   (e) consolidating said green billet to form a consolidated material with greater than about 95% of theoretical density and low oxygen content below about 200 ppm for Re and below about 500 ppm for Re-based materials formed from said mixture, excluding oxygen from non-metallic compounds and/or ceramics.   
     
     
         2 . The method according to  claim 1 , wherein:
 step (e) comprises consolidating said green billet and forming a consolidated material with greater than about 99% of theoretical density and low oxygen content below about 100 ppm for Re and below about 200 ppm for Re-based materials formed from said mixture, excluding oxygen from non-metallic compounds and/or ceramics.   
     
     
         3 . The method according to  claim 1 , further comprising a step of:
 (f) forming at least one deposition source from said consolidated material.   
     
     
         4 . The method according to  claim 3 , wherein:
 step (f) comprises forming at least one sputtering target.   
     
     
         5 . The method according to  claim 1 , wherein:
 step (c) comprises forming said green billet by cold isostatic pressing (CIP) or mechanical pressing; and   step (d) comprises maintaining said billet at an elevated temperature while contacting said billet with H 2  gas.   
     
     
         6 . The method according to  claim 1 , wherein step (e) comprises steps of:
 (e 1 ) encapsulating said billet of degassed green material in a container; and   (e 2 ) subjecting said encapsulated billet to hot isostatic pressing (HIP) to form said consolidated material.   
     
     
         7 . The method according to  claim 1 , wherein step (e) comprises steps of:
 (e 1 ) subjecting said billet of degassed green material to vacuum hot pressing (VHP) or spark plasma sintering (SPS) to achieve <˜97% of theoretical density; and   (e 2 ) subjecting the thus-treated billet to hot isostatic pressing (HIP) to form said consolidated material with >˜97% of theoretical density.   
     
     
         8 . The method according to  claim 1 , wherein:
 step (a) comprises providing a Re powder starting material; and   step (e) comprises forming a consolidated Re material having 100% of theoretical density and oxygen content below about 100 ppm.   
     
     
         9 . The method according to  claim 1 , wherein:
 step (a) comprises providing a Re powder starting material and a predetermined amount of at least one additional powder material comprising at least one transition metal element X; and   step (e) comprises forming a consolidated material of formula Re—X, comprising predetermined proportions of Re and said at least one transition metal.   
     
     
         10 . The method according to  claim 9 , wherein:
 step (a) comprises providing a predetermined amount at least one additional powder material comprising at least one transition metal selected from the group consisting of Mo, Co, Ru, W, and Cr; and   step (e) comprises forming a consolidated Re—X material having greater than about 99.0% of theoretical density, oxygen content below about 200 ppm, a Re phase, an X phase, and a Re—X phase.   
     
     
         11 . The method according to  claim 1 , wherein:
 step (a) comprises providing a Re powder starting material and a predetermined amount of at least one additional powder material comprising at least one material Y selected from the group consisting of non-metallic elements, non-metallic compounds, and ceramic materials; and   step (e) comprises forming a consolidated material of formula Re—Y, comprising predetermined proportions of Re and said at least one non-metallic element, non-metallic compound, or ceramic material.   
     
     
         12 . The method according to  claim 11 , wherein:
 Y is at least one carbide or nitride or an oxide of Ti, Si, or Mg.   
     
     
         13 . The method according to  claim 1 , wherein:
 step (a) comprises providing a predetermined amount of Re powder starting material, a predetermined amount of at least one additional powder material comprising at least one transition metal element X, and a predetermined amount of at least one additional powder material comprising at least one material Y selected from the group consisting of non-metallic elements, non-metallic compounds, and ceramic materials; and   step (e) comprises forming a consolidated material of formula Re—X—Y, comprising predetermined proportions of Re, said at least one transition metal element X, and said at least one non-metallic element, non-metallic compound, or ceramic material Y.   
     
     
         14 . The method according to  claim 13 , wherein:
 X is at least one transition metal selected from the group consisting of Mo, Co, Ru, W, and Cr; and Y is at least one carbide or nitride or an oxide of Ti, Si, or Mg.   
     
     
         15 . The method according to  claim 1 , wherein:
 steps (c)-(e) are replaced by a single step process.   
     
     
         16 . The method according to  claim 15 , wherein steps (c)-(e) are replaced by a process selected from the group consisting of: vacuum hot pressing (VHP), spark plasma sintering (SPS), microwave sintering, atmospheric pressure H 2  sintering, and vacuum H 2  sintering. 
     
     
         17 . A deposition source comprising consolidated Re powder material having greater than about 95% of theoretical density and oxygen content below about 200 ppm. 
     
     
         18 . The deposition source as in  claim 17 , wherein said consolidated Re powder material has greater than about 99% of theoretical density and oxygen content below about 100 ppm. 
     
     
         19 . The deposition source as in  claim 18 , wherein said consolidated Re powder material has 100% of theoretical density. 
     
     
         20 . A deposition source comprising consolidated Re—X powder material, where X is at least one transition metal element, said consolidated Re—X powder material having greater than about 95% of theoretical density, oxygen content below about 500 ppm, a Re phase, an X phase, and a Re—X phase. 
     
     
         21 . The deposition source as in  claim 20 , wherein said consolidated Re—X powder material has greater than about 99% of theoretical density and oxygen content below about 200 ppm. 
     
     
         22 . The deposition source as in  claim 20 , wherein said at least one transition metal element X is selected from the group consisting of Mo, Co, Ru, W, and Cr. 
     
     
         23 . A deposition source comprising consolidated Re—Y powder material, where Y is at least one non-metallic element, non-metallic compound, or ceramic material, said consolidated Re—Y powder material having greater than about 95% of theoretical density and oxygen content below about 500 ppm, excluding oxygen from non-metallic compounds and/or ceramics. 
     
     
         24 . The deposition source as in  claim 23 , wherein said consolidated Re—Y powder material has greater than about 99% of theoretical density and oxygen content below about 200 ppm, excluding oxygen from non-metallic compounds and/or ceramics. 
     
     
         25 . The deposition source as in  claim 23 , wherein Y is at least one carbide or nitride or oxide of Ti, Si, and Mg. 
     
     
         26 . A deposition source comprising consolidated Re—X—Y powder material, where X is at least one transition metal element and Y is at least one non-metallic element, non-metallic compound, or ceramic material, said consolidated Re—X—Y powder material having greater than about 95% of theoretical density and oxygen content below about 500 ppm, excluding oxygen from non-metallic compounds and/or ceramics. 
     
     
         27 . The deposition source as in  claim 26 , wherein said consolidated Re—X—Y powder material has greater than about 99% of theoretical density and oxygen content below about 200 ppm, excluding oxygen from non-metallic compounds and/or ceramics. 
     
     
         28 . The deposition source as in  claim 26 , wherein said at least one transition metal element X is selected from the group consisting of Mo, Co, Ru, W, and Cr; and Y is at least one carbide or nitride or an oxide of Ti, Si, or Mg.