Method for Manufacturing Conductive Inorganic Oxide Particles and Conductive Inorganic Oxide Particles Obtained by the Method

Abstract

A method for manufacturing conductive inorganic oxide particles in which conductivity is furnished by doping a dopant metal component into the inorganic oxide particle including preparing an inorganic oxide particles-containing slurry which contains the inorganic oxide particles, the inorganic oxide particles-containing slurry which is made to contain a dopant metal component and an electrolysis method is carried out for electrolytic doping to dope a dopant metal component into the inorganic oxide particles by using a electrolytic doping unit, filtering and drying the slurry after finishing the electrolytic doping and collecting particles by filter, and firing the particles collected by filter to obtain conductive inorganic oxide particles.

1 . A method for manufacturing conductive inorganic oxide particles in which conductivity is furnished by doping a dopant metal component into the inorganic oxide particle;
 wherein the doping is electrolytic doping where the dopant metal component and a constituent component of the inorganic oxide particles are made to be a composite by carrying out electrolysis of inorganic oxide particles-containing slurry which includes a dopant metal component, wherein the doping is followed by filtering and drying the slurry and collection of the particles by filter.   
     
     
         2 . The method for manufacturing conductive inorganic oxide particles according to  claim 1  in which conductivity is furnished by doping a dopant metal component into the inorganic oxide particle, wherein the method comprises:
 a step for preparing the inorganic oxide particles-containing slurry which is made to contain the inorganic oxide particles; 
 a step for doping a dopant metal component into the inorganic oxide particles, wherein the inorganic oxide particles-containing slurry includes a dopant metal component, by carrying out an electrolysis method for electrolytic doping; 
 a step for filtrating and drying the slurry after finishing the electrolytic doping and collecting particles by filter; and 
 a step for firing the particles collected by filter to obtain conductive inorganic oxide particles. 
 
     
     
         3 . The method for manufacturing conductive inorganic oxide particles according to  claim 2 , wherein the inorganic oxide particles are particles made of zinc oxide, titanium oxide, silica, alumina, zirconia, magnesia, cerium oxide, nickel oxide, tin oxide, tellurium oxide or vanadium oxide. 
     
     
         4 . The method for manufacturing conductive inorganic oxide particles according to  claim 2 , wherein the inorganic oxide particles have an average primary particle diameter of 1 nm to 30 nm. 
     
     
         5 . The method for manufacturing conductive inorganic oxide particles according to  claim 2 , wherein the inorganic oxide particles-containing slurry contains 5% by weight to 30% by weight of the inorganic oxide particles. 
     
     
         6 . The method for manufacturing conductive inorganic oxide particles according to  claim 2 , wherein the inorganic oxide particles-containing slurry contains an electrolyte at a concentration of 0.001 mol/l to 0.05 mol/l. 
     
     
         7 . The method for manufacturing conductive inorganic oxide particles according to  claim 2 , wherein a dopant metal component made to be contained in the inorganic oxide particles-containing slurry is contained at a concentration of 0.1% by weight to 20.0% by weight in terms of an oxide of the dopant metal component. 
     
     
         8 . The method for manufacturing conductive inorganic oxide particles according to  claim 2 , wherein a dissolvable anode electrode made of a dopant metal is used in the electrolysis method to supply dopant metal ions to the inorganic oxide particles-containing slurry by electrolysis to maintain a concentration of the dopant metal ions at a constant level. 
     
     
         9 . The method for manufacturing conductive inorganic oxide particles according to  claim 2 , wherein a cathode electrode made of the dopant metal is used in the electrolysis method. 
     
     
         10 . The method for manufacturing conductive inorganic oxide particles according to  claim 2 , wherein electrolysis in the electrolysis method is carried out while stirring the slurry. 
     
     
         11 . The method for manufacturing conductive inorganic oxide particles according to  claim 2 , wherein electrolysis in the electrolysis method is carried out at a current density of 0.3 mA/cm 2  to 100 mA/cm 2 . 
     
     
         12 . The method for manufacturing conductive inorganic oxide particles according to  claim 2 , wherein electrolysis in the electrolysis method is carried out by setting a slurry temperature in the range of 30° C. to 85° C. 
     
     
         13 . The method for manufacturing conductive inorganic oxide particles according to  claim 2 , wherein, stirring of the slurry after finishing the electrolysis to improve particle dispersion is carried out for 1 hr or more. 
     
     
         14 . The method for manufacturing conductive inorganic oxide particles according to  claim 2 , wherein an atmosphere of the firing is a hydrogen-containing atmosphere, an inert gas atmosphere, an ammonia gas atmosphere or a vacuum atmosphere. 
     
     
         15 . The method for manufacturing conductive inorganic oxide particles according to  claim 2 , wherein a firing temperature of the firing is from 250° C. to 800° C. 
     
     
         16 . The method for manufacturing conductive inorganic oxide particles according to  claim 2 , wherein a carbon dioxide gas is bubbled during the electrolysis in the electrolysis method. 
     
     
         17 . The method for manufacturing conductive inorganic oxide particles according to  claim 2 , wherein, a pyrolysis treatment step for pyrolyzing basic metal carbonate generated by the carbon dioxide gas bubbling is performed after the article collection step and before the particle firing step. 
     
     
         18 . The method for manufacturing conductive inorganic oxide particles according to  claim 2 , wherein the dopant metal component is one kind or two or more kinds of components selected from gallium, indium, copper, antimony, arsenic, boron, thallium, bismuth, vanadium, niobium, tantalum and iron. 
     
     
         19 . A conductive inorganic oxide powder composed of the conductive inorganic oxide particles obtained by doping a dopant metal component into the inorganic oxide particle according to the method for manufacturing conductive inorganic oxide particles according to  claim 2 , wherein the conductive inorganic oxide powder is composed of conductive inorganic oxide particles having an average primary particle diameter of 3 nm to 40 nm. 
     
     
         20 . The conductive inorganic oxide powder according to  claim 19 , wherein 0.1% by weight to 20.0% by weight of the dopant metal component is contained in terms of the oxide of the dopant metal component. 
     
     
         21 . The conductive inorganic oxide powder according to  claim 19 , wherein any of zinc oxide particles, titanium oxide particles, silica particles, alumina particles, zirconia particles, magnesia particles, cerium oxide particles, nickel oxide particles, tin oxide particles, tellurium oxide particles and vanadium oxide particles are used as the inorganic oxide particles. 
     
     
         22 . The conductive inorganic oxide powder according to  claim 19 , wherein the dopant metal component is one kind or two or more kinds of components selected from gallium, indium, copper, antimony, arsenic, boron, thallium, bismuth, vanadium, niobium, tantalum and iron. 
     
     
         23 . The conductive inorganic oxide powder according to  claim 19 , wherein a sum component amount of the respective components, an amount of metal components constituting the inorganic oxide particles, an amount of a dopant metal component and an amount of an oxygen component is preferable to be 99.9% by weight or more against 100% by weight of an amount of the conductive inorganic oxide powder. 
     
     
         24 . The conductive inorganic oxide powder according to  claim 19 , wherein powder resistivity measured in the state that 1.0 g of the conductive inorganic oxide powder in a cylindrical vessel (inner diameter: 18 mm) is pressed with a pressure of 100 kg/cm 2  and resistance is measured between both pressed edges of a specimen is 500 Ω·cm or less.