Method for manufacturing nanophase TiC-based composite powders by metallothermic reduction

Abstract

Disclosed herein is a method for economically manufacturing high quality TiC powder, TiCN powder or ultrafine nanophase TiC+Ni (Co, Al) and TiCN+Ni (Co, Al) composite powders by means of metallothermic reduction. The method comprises the steps of preparing a starting solution of titanium tetrachloride (TiCl 4 ) in a carbon chloride, feeding the starting solution into a closed container containing molten magnesium (Mg) under inert atmosphere, vacuum-separating unreacted liquid-phase Mg and magnesium chloride (MgCl 2 ) remaining after reduction of magnesium from the closed container, and collecting a TiC compound from the closed container. TiC powder, TiCN powder or ultrafine nanophase TiC+Ni (Co, Al) and TiCN+Ni (Co, Al) composite powders having a particle size of a few tens nm can be manufactured in a simpler manner using economically advantageous starting materials such as titanium tetrachloride and carbon chlorides.

1 . A method for manufacturing nanophase TiC-based composite powders by means of metallothermic reduction, comprising the steps of: 
 preparing a starting solution of titanium tetrachloride (TiCl 4 ) in a carbon chloride;    feeding the starting solution into a closed container containing molten magnesium (Mg) under inert atmosphere;    vacuum-separating unreacted liquid-phase Mg and magnesium chloride (MgCl 2 ) remaining after reduction of magnesium from the closed container; and    collecting a TiC compound from the closed container.    
     
     
         2 . The method for manufacturing nanophase TiC-based composite powders by means of metallothermic reduction according to  claim 1 , wherein in the step of preparing a starting solution of titanium tetrachloride (TiCl 4 ) in a carbon chloride, the carbon chloride is carbon tetrachloride (CCl 4 ) or tetrachloroethylene (C 2 Cl 4 ).  
     
     
         3 . The method for manufacturing nanophase TiC-based composite powders by means of metallothermic reduction according to  claim 1 , wherein in the step of preparing a starting solution of titanium tetrachloride (TiCl 4 ) in a carbon chloride, the carbon chloride (CCl 4  or C 2 Cl 4 ) is used in an amount of 1.05˜1.15 moles, relative to one mole of titanium tetrachloride (TiCl 4 ).  
     
     
         4 . The method for manufacturing nanophase TiC-based composite powders by means of metallothermic reduction according to  claim 1 , wherein in the step of feeding the starting solution into a closed container containing molten magnesium (Mg) under inert atmosphere, the feeding of the starting solution is controlled at a rate of 10˜20 g/min.  
     
     
         5 . The method for manufacturing nanophase TiC-based composite powders by means of metallothermic reduction according to  claim 1 , wherein the inert atmosphere of the closed container containing molten magnesium (Mg) is created by heating at 200° C. under vacuum for 1 hour, feeding argon gas at 1.1 atm, and heating to a temperature of above 1000° C.  
     
     
         6 . The method for manufacturing nanophase TiC-based composite powders by means of metallothermic reduction according to  claim 1 , wherein the molten magnesium (Mg) contained in the closed container under inert atmosphere is used in an amount of 8˜14 moles, relative to one mole of the starting solution.  
     
     
         7 . The method for manufacturing nanophase TiC-based composite powders by means of metallothermic reduction according to  claim 1 , wherein the molten magnesium (Mg) contained in the closed container under inert atmosphere further includes at least one metal selected from nickel (Ni), cobalt (Co) and aluminum (Al).