US2018043437A1PendingUtilityA1

Methods For Producing Metal Powders And Metal Masterbatches

39
Assignee: Nanoscale Powders LLCPriority: Aug 12, 2016Filed: Aug 7, 2017Published: Feb 15, 2018
Est. expiryAug 12, 2036(~10.1 yrs left)· nominal 20-yr term from priority
C22B 34/14B22F 9/24C22B 34/1277B22F 2301/205B22F 2304/10C22C 14/00B22F 9/28C22B 5/04B22F 9/20
39
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Claims

Abstract

A method for producing a metal powder that combines molten reducing metal and metal halide in a space that is substantially free of oxygen and water, wherein the molten reducing metal is sodium and/or potassium, or aluminum (or magnesium or titanium) and is present in a stoichiometric excess to the metal halide which is a solid or liquid, thereby producing metal particles and salt, removing unreacted reducing metal, optionally removing the salt, and recovering the metal powder, is described. A method for producing a metal masterbatch wherein the molten reducing metal is aluminum, magnesium, and/or titanium and after combining molten aluminum (or magnesium or titanium) and metal halide in the reaction space, substantially removing the produced metal salt to obtain the metal masterbatch which comprises at least a portion of the molten aluminum (or magnesium or titanium) and at least one metal also is described.

Claims

exact text as granted — not AI-modified
What is claimed is: 
     
         1 . A method for producing a metal powder, the method comprising:
 a) combining at least one metal halide and at least one molten reducing metal in a space that is substantially free of oxygen and water, wherein said molten reducing metal is present in a stoichiometric excess to the metal halide, to obtain a reaction product that comprises at least one metal salt and metal, and wherein the molten reducing metal comprises i) at least 90 wt % sodium or potassium or a mixture of potassium and sodium or ii) at least 90 wt % aluminum, magnesium, or titanium based on total weight of said molten reducing metal, and the at least one metal halide is a solid or liquid, with the proviso that the molten reducing metal is different from the metal of the at least one metal halide;   b) substantially removing unreacted said molten reducing metal in said reaction product;   c) recovering at least said metal, wherein the metal of the metal salt is the molten reducing metal, and the ‘metal’ recovered from the reaction product is from the metal of the metal halide.   
     
     
         2 . The method of  claim 1 , wherein in step c), the at least one metal salt is recovered with said metal. 
     
     
         3 . The method of  claim 2 , wherein said method further comprises d) separating said metal from said metal salt. 
     
     
         4 . The method of  claim 1 , wherein two or more metal halides are used and wherein said metal recovered comprises a metal alloy or intermetallic compound from each metal of the two or more metal halides. 
     
     
         5 . The method of  claim 1 , wherein said at least one metal halide is at least one metal chloride. 
     
     
         6 . A method for producing a metal masterbatch, the method comprising:
 a) combining at least one metal halide and at least one molten reducing metal in a space that is substantially free of oxygen and water, wherein said molten reducing metal is present in a stoichiometric excess to the metal halide, to obtain a reaction product that comprises at least one metal salt and metal, and wherein the molten reducing metal comprises at least 90 wt % aluminum, magnesium, or titanium based on total weight of said molten reducing metal, and the at least one metal halide is a solid or liquid, with the proviso that the molten reducing metal is different from the metal of the at least one metal halide;   b) substantially removing said at least one metal salt to obtain said metal masterbatch comprising at least a portion of said molten reducing metal and the metal, wherein the metal of the metal salt is the molten reducing metal, and the ‘metal’ recovered from the reaction product is from the metal of the metal halide, wherein the removing of at least one metal salt occurs during or after formation of said reaction product.   
     
     
         7 . The method of  claim 1 , wherein said at least one metal halide comprises Ti halide, V halide, Cr halide, Mn halide, Fe halide, Co halide, Ni halide, Cu halide, Zn halide, Ga halide, Ge halide, As halide, Se halide, Zr halide, Nb halide, Mo halide, Ru halide, Rh halide, Pd halide, Ag halide, Cd halide, In halide, Sn halide, Sb halide, C halide, Si halide, Te halide, Hf halide, Ta halide, W halide, Hg halide, Tl halide, Pb halide, or Bi halide or any combination thereof. 
     
     
         8 . The method of  claim 6 , wherein said at least one metal halide is at least one metal chloride. 
     
     
         9 . The method of  claim 6 , wherein two or more metal halides are used and wherein said metal recovered comprises a metal alloy, intermetallic compound, or ceramic from each metal of the two or more metal halides. 
     
     
         10 . The method of  claim 1 , wherein said at least one metal halide is at least one metal chloride. 
     
     
         11 . The method of  claim 6 , wherein said metal masterbatch comprises aluminum, hafnium, and zirconium. 
     
     
         12 . The method of  claim 6 , further comprising adding a carbide, nitride, or boride forming component to said metal halide or to said molten reducing metal or both, and wherein said metal of the reaction product comprises a metal carbide, a metal nitride, or a metal boride or any combination thereof. 
     
     
         13 . The method of  claim 12 , wherein said carbide forming component comprises carbon containing gas, carbon tetrachloride or solid carbon. 
     
     
         14 . The method of  claim 12 , wherein said boride forming component comprises boron trichloride or a boron hydride. 
     
     
         15 . The method of  claim 6 , wherein said substantially removing said at least one metal salt comprises vaporization of said at least one metal salt and removal thereof from said metal masterbatch. 
     
     
         16 . The method of  claim 1 , wherein said at least one metal halide is combined as a solid with said molten reducing metal. 
     
     
         17 . The method of  claim 16 , wherein said at least one metal halide is combined as a solid with a portion of said molten reducing metal to form a mixture, and said portion of said molten reducing metal is at a temperature that avoids reaction with said metal halide. 
     
     
         18 . The method of  claim 17 , said method further comprising combining said mixture with part or all of the remaining portion of said molten reducing metal that is at a temperature that permits reaction with said metal halide. 
     
     
         19 . The method of  claim 1 , wherein said combined at least one metal halide and at least one molten reducing metal passes through a reaction zone that comprises at least one closed pipe that causes turbulence in combined at least one metal halide and at least one molten reducing metal and that optionally empties into a tank or filter. 
     
     
         20 . The method of  claim 1 , wherein said molten reducing metal comprises said at least 90 wt % sodium or potassium or a mixture of potassium and sodium, and wherein combined at least one metal halide and at least one molten reducing metal passes through a reaction zone that empties into a settling tank that includes at least one outlet that is located at a height in the settling tank that permits said molten reducing metal from step b) to at least partly be removed by said outlet but not said molten salt or said metal, and wherein said combined at least one metal halide, at least one molten reducing metal, and at least one metal salt together are at a temperature that results in phase separation of the molten reducing metal from said metal salt and said metal. 
     
     
         21 . The method of  claim 18 , wherein said combining said mixture with part or all of the remaining portion of said molten reducing metal that is at a temperature that permits reaction with said metal halide comprises utilizing an eductor. 
     
     
         22 . The method of  claim 1 , prior to at least step b), wherein said molten reducing metal comprises at least 90 wt % sodium or potassium or a mixture of potassium and sodium, and wherein at least one metal halide, at least one molten reducing metal and at least one metal salt together are at a temperature that causes phase separation of the molten reducing metal from said metal salt and said metal. 
     
     
         23 . The method of  claim 1 , wherein said substantially removing said at least one metal salt comprises permitting the vaporization of at least a portion of said at least one metal salt and removal thereof from said metal masterbatch. 
     
     
         24 . The method of  claim 1 , wherein the at least one metal halide comprises at least a first metal halide and a second metal halide, with the first metal halide reactive with the metal salt and the second metal halide non-reactive with the metal salt, wherein the metal of the second metal halide is the same or different from the molten reducing metal. 
     
     
         25 . The method of  claim 6 , wherein the at least one metal halide comprises at least a first metal halide and a second metal halide, with the first metal halide reactive with the metal salt and the second metal halide non-reactive with the metal salt, wherein the metal of the second metal halide is the same or different from the molten reducing metal. 
     
     
         26 . The method of  claim 24 , wherein the second metal halide is NaCl and the molten reducing metal is said at least 90 wt % sodium, and the first metal halide is AlCl 3 . 
     
     
         27 . The method of  claim 25 , wherein the second metal halide is NaCl and the molten reducing metal is said at least 90 wt % sodium, and the first metal halide is AlCl 3 . 
     
     
         28 . The method of  claim 6 , wherein said at least one metal halide comprises Ti halide, V halide, Cr halide, Mn halide, Fe halide, Co halide, Ni halide, Cu halide, Zn halide, Ga halide, Ge halide, As halide, Se halide, Zr halide, Nb halide, Mo halide, Ru halide, Rh halide, Pd halide, Ag halide, Cd halide, In halide, C halide, Si halide, Sn halide, Sb halide, Te halide, Hf halide, Ta halide, W halide, Hg halide, Tl halide, Pb halide, or Bi halide or any combination thereof. 
     
     
         29 . The method of  claim 24 , wherein said first metal halide and said second metal halide form a eutectic mixture. 
     
     
         30 . The method of  claim 1 , wherein said at least one metal halide is two or more metal halides, and one metal halide is a solid or liquid and the other metal halide is a vapor, solid, or liquid. 
     
     
         31 . The method of  claim 6 , wherein said at one least metal halide is two or more metal halides, and one metal halide is a solid or liquid and the other metal halide is a vapor, solid, or liquid. 
     
     
         32 . The method of  claim 1 , wherein said metal salt at least partially coats or encapsulates said metal. 
     
     
         33 . The method of  claim 1 , wherein said molten reducing metal is aluminum alloy. 
     
     
         34 . The method of  claim 1 , wherein said molten reducing metal is magnesium alloy. 
     
     
         35 . The method of  claim 1 , wherein said molten reducing metal is titanium alloy. 
     
     
         36 . The method of  claim 6 , wherein said molten reducing metal is aluminum alloy. 
     
     
         37 . The method of  claim 6 , wherein said molten reducing metal is magnesium alloy. 
     
     
         38 . The method of  claim 6 , wherein said molten reducing metal is titanium alloy.

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