Methods of making titanium diboride powders

Abstract

The present disclosure is directed towards methods of making titanium diboride products in various sizes. An aspect of the method provides (a) selecting a target average particle size for a target titanium diboride product; (b) selecting at least one processing variable from the group consisting of: an amount of sulfur, an inert gas flow rate, a soak time, and a reaction temperature; (c) selecting a condition of the processing variable based upon the target average particle size; and (d) producing an actual titanium diboride product having an actual average particle size using the at least one processing variable, wherein due to the at least one processing variable, the actual average particle size corresponds to the target average particle size.

1 . A method comprising:
 (a) selecting a target average particle size for a target titanium diboride product;   (b) selecting at least one processing variable from the group consisting of: an amount of sulfur, an inert gas flow rate, a soak time, and a reaction temperature;   (c) selecting a condition of the processing variable based upon the target average particle size; and   (d) producing an actual titanium diboride product having an actual average particle size using the at least one processing variable,   wherein due to the at least one processing variable, the actual average particle size corresponds to the target average particle size.   
     
     
         2 . The method of  claim 1 , further wherein the at least one processing variable is the amount of sulfur;
 wherein the condition of the amount of sulfur is not greater than about 1.0 wt. %;   further wherein the actual average titanium diboride particle size is not greater than about 7 microns.   
     
     
         3 . The method of  claim 1 , further wherein the at least one processing variable is the reaction temperature;
 wherein the condition of the reaction temperature is in the range of at least about 1450 C to 1500 C; further wherein the actual average titanium diboride particle size is in the range from about 4 microns to about 7 microns.   
     
     
         4 . The method of  claim 1 , further wherein the at least one processing variable is the soak time;
 wherein the condition of the soak time is in the range of about 0.5 hrs to about 1 hour;   further wherein the actual average titanium diboride particle size is in the range of about 4.5 microns to about 8 microns.   
     
     
         5 . The method of  claim 1 , further wherein the at least one processing variable is the inert gas flow rate and the amount of sulfur;
 wherein the condition of the amount of sulfur is in the amount of not greater than about 1 wt. %;   wherein the condition of the inert gas flow rate is in the range of at least about 0.5 liters per minute;   further wherein the actual average titanium diboride particle size not greater than about 6.5 microns.   
     
     
         6 . The method of  claim 1 , wherein the producing step further comprises carbothermically reacting. 
     
     
         7 . The method of  claim 1 , wherein the producing step further comprises:
 preparing a precursor mixture; and   reacting the precursor mixture in a reactor to produce the actual titanium diboride product.   
     
     
         8 . The method of  claim 7 , further wherein the preparing step comprises:
 mixing into a liquid to form a suspension:
 a boron source; 
 a carbon source; 
 a titanium source; and 
   drying the suspension to produce the precursor mixture having a plurality of agglomerations.   
     
     
         9 . A method comprising:
 (a) selecting a target average particle size for a target titanium diboride product;   (b) selecting an amount of sulfur based upon the target average particle size;   (c) producing an actual titanium diboride product having an actual average particle size,   wherein, due to the amount of sulfur, the actual average particle size corresponds to the target average particle size.   
     
     
         10 . The method of  claim 9 , wherein the amount of sulfur is not greater than about 1.0 wt. %;
 further wherein the actual average titanium diboride particle size is not greater than about 7 microns.   
     
     
         11 . The method of  claim 9 , further comprising:
 selecting at least one processing variable from the group consisting of: an inert gas flow rate, a soak time, and a reaction temperature; and   selecting a condition of the processing variable based upon at least one of:
 the target average particle size; and 
 the amount of sulfur. 
   
     
     
         12 . The method of  claim 9 , further comprising:
 deagglomerating the actual titanium diboride product to remove a plurality of agglomerations in the titanium diboride product.   
     
     
         13 . The method of  claim 9 , wherein deagglomerating further comprises:
 milling the titanium diboride product for a length of time based upon the amount of sulfur in the precursor mixture.   
     
     
         14 . The method of  claim 9 , wherein the producing step further comprises:
 preparing an agglomerated mixture including:
 mixing into a liquid the boron source; the carbon source; the titanium source, and optional additives to form a suspension; and 
 drying the suspension to produce the agglomerated mixture. 
   
     
     
         15 . The method of  claim 9 , wherein the drying step further comprises spray drying. 
     
     
         16 . The method of  claim 9 , wherein the producing step comprises carbothermically reacting. 
     
     
         17 . A method comprising:
 (a) selecting a target average particle size for a target titanium diboride product;   (b) selecting an amount of sulfur based upon the target average particle size;   (c) producing an actual titanium diboride product having an actual average particle size,   wherein, due to the amount of sulfur, the actual average particle size corresponds to the target average particle size;
 wherein the producing comprises:
 reacting a precursor mixture in a reactor, the precursor mixture including: 
 a titanium source; 
 a boron source; 
 a carbon source; and 
 the amount of sulfur. 
 
   
     
     
         18 . The method of  claim 17 , further comprising the step of:
 processing the actual titanium diboride product into a product selected from: a cathode; and a structure of an aluminum electrolysis cell.