Composite of metal oxide nanoparticles and carbon, method of production thereof, electrode and electrochemical element employing said composite

Patent metadata

Field	Value
Publication number	US-9287553-B2
Application number	US-201113638542-A
Country	US
Kind code	B2
Filing date	Mar 31, 2011
Priority date	Mar 31, 2010
Publication date	Mar 15, 2016
Grant date	Mar 15, 2016

Abstract

A composite powder in which highly dispersed metal oxide nanoparticle precursors are supported on carbon is rapidly heated under nitrogen atmosphere, crystallization of metal oxide is allowed to progress, and highly dispersed metal oxide nanoparticles are supported by carbon. The metal oxide nanoparticle precursors and carbon nanoparticles supporting said precursors are prepared by a mechanochemical reaction that applies sheer stress and centrifugal force to a reactant in a rotating reactor. The rapid heating treatment in said nitrogen atmosphere is desirably heating to 400° C.-1000° C. By further crushing the heated composite, its aggregation is eliminated and the dispersity of metal oxide nanoparticles is made more uniform. Examples of a metal oxide that can be used are manganese oxide, lithium iron phosphate, and lithium titanate. Carbons that can be used are carbon nanofiber and Ketjen Black.

First claim

The invention claimed is:

1. A method for producing a composite of metal oxide nanoparticles and carbon having an ultra thin film structure in which crystalized metal oxide nanoparticles are contained inside the carbon, the method comprising:
applying a shear stress and centrifugal force to a solution including a starting material of metal oxide nanoparticles and carbon powder in a rotating reactor to allow reaction and obtain a composite powder of carbon and metal oxide nanoparticle precursors supported and dispersed thereon; and
heating the composite powder under a nitrogen atmosphere from room temperature to no less than 700° C. within a 3 to 5 minute time period to obtain the composite of metal oxide nanoparticles and carbon having an ultra thin film structure in which crystalized metal oxide nanoparticles are contained inside the carbon.

2. The method for producing a composite of metal oxide nanoparticles and carbon according to claim 1 , wherein the composite powder is heated under nitrogen atmosphere to 700° C.-1000° C.

3. The method for producing a composite of metal oxide nanoparticles and carbon according to claim 2 , wherein shear stress and centrifugal force is applied to the solution including a reaction suppressor along with a reactant in said reactor to allow reaction.

4. The method for producing a composite of metal oxide nanoparticles and carbon according to claim 1 , wherein the metal oxide is represented by MxOz, AxMyOz, Mx(DO 4 )y, and AxMy(DO 4 )z (wherein M: metal element and A: alkali metal or lanthanoids).

5. The method for producing a composite of metal oxide nanoparticles and carbon according to claim 4 , wherein said metal oxide is any one of manganese oxide MnO, lithium iron phosphate LiFePO 4 , and lithium titanate Li 4 Ti 5 O 12 .

6. The method for producing a composite of metal oxide nanoparticles and carbon according to claim 2 , wherein the metal oxide is represented by MxOz, AxMyOz, Mx(DO 4 )y, and AxMy(DO 4 )z (wherein M: metal element and A: alkali metal or lanthanoids).

7. The method for producing a composite of metal oxide nanoparticles and carbon according to claim 3 , wherein the metal oxide is represented by MxOz, AxMyOz, Mx(DO 4 )y, and AxMy(DO 4 )z (wherein M: metal element and A: alkali metal or lanthanoids).

8. The method for producing a composite of metal oxide nanoparticles and carbon according to claim 6 , wherein said metal oxide is any one of manganese oxide MnO, lithium iron phosphate LiFePO 4 , and lithium titanate Li 4 Ti 5 O 12 .

9. The method for producing a composite of metal oxide nanoparticles and carbon according to claim 7 , wherein said metal oxide is any one of manganese oxide MnO, lithium iron phosphate LiFePO 4 , and lithium titanate Li 4 Ti 5 O 12 .

10. The method for producing a composite of metal oxide nanoparticles and carbon according to claim 1 , wherein the composite powder is dried under a vacuum before being heated under the nitrogen atmosphere.

11. The method for producing a composite of metal oxide nanoparticles and carbon according to claim 3 , wherein the reaction suppressor is selected from one of levulinic acid and an aminoalcohol in the amount of 1 to 3 moles relative to 1 mole of the metal oxide nanoparticles.

12. A method for producing a composite of metal oxide nanoparticles and carbon having an ultra thin film structure in which crystalized metal oxide nanoparticles are contained inside the carbon, the method consisting of:
applying a shear stress and centrifugal force to a solution including a starting material of metal oxide nanoparticles, carbon powder and a reaction suppressor in a rotating reactor to allow a controlled reaction to obtain a composite powder of carbon with metal oxide nanoparticle precursors supported and dispersed thereon; and
heating the composite powder under a nitrogen atmosphere from room temperature to no less than 700° C. for a time period within 3 to 5 minutes to obtain a composite of metal oxide nanoparticles and carbon having a thin film structure wherein crystalized metal oxide nanoparticles are supported by the carbon.

13. The method for producing a composite of metal oxide nanoparticles and carbon according to claim 12 , wherein the metal oxide is represented by MxOz, AxMyOz, Mx(DO 4 )y, and AxMy(DO 4 )z (wherein M: metal element and A: alkali metal or lanthanoids).

14. The method for producing a composite of metal oxide nanoparticles and carbon according to claim 13 , wherein said metal oxide is any one of manganese oxide MnO, lithium iron phosphate LiFePO 4 , and lithium titanate Li 4 Ti 5 O 12 .

15. The method for producing a composite of metal oxide nanoparticles and carbon according to claim 12 , wherein the reaction suppressor is selected from one of levulinic acid and an aminoalcohol in the amount of 1 to 3 moles relative to 1 mole of the metal oxide nanoparticles.

16. The method for producing a composite of metal oxide nanoparticles and carbon according to claim 12 where the metal oxide nanoparticles have a thickness of 1 nm or less at 2-5 atomic layers level on a plate of 5-100 nm in diameter.

17. The method of producing a composite of metal oxide nanoparticles and carbon according to claim 16 wherein the nanoparticles are manganese oxide.

Assignees

• Naoi Katsuhiko
• Naoi Wako
• Ishimoto Shuichi
• Tamamitsu Kenji
• Nippon Chemicon

Inventors

• Naoi Katsuhiko
• Naoi Wako
• Ishimoto Shuichi
• Tamamitsu Kenji

Classifications

• C01B25/45 Primary

  containing plural metal, or metal and ammonium · CPC title

• C01G45/02

  Oxides · CPC title

• Y02E60/13

  Energy storage using capacitors · CPC title

• Y10S977/811

  Of specified metal oxide composition, e.g. conducting or semiconducting compositions such as ITO, ZnOx · CPC title

• H01G4/008

  Selection of materials · CPC title