Zirconia particles

• US 7,429,422 B2
• Filed: 06/07/2007
• Issued: 09/30/2008
• Est. Priority Date: 12/30/2004
• Status: Active Grant

• Current Assignee: 3M Innovative Properties Company (3M Company)
• Original Assignee: 3M Innovative Properties Company (3M Company)
• Inventors: Kolb, Brant U., Brady, John T., Davidson, Robert S., Hendrickson, Mark J., Higgins, James A., Anderson, Danny B.
• Primary Examiner(s): Vanoy; Timothy C
• Application Number:
  US11/759,520
• Publication Number:
  US 20070232705A1
• Time in Patent Office: 481 Days
• Field of Search: 428/411.1, 428/418, 428/423.1, 428/425.9, 428/458, 428/480, 428/500
• US Class Current: 428/411.1
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01G 25/02 Oxides
• CPC Class Codes: C01P 2002/70 defined by measured X-ray, neutron or electron diffraction data
• CPC Class Codes: C01P 2002/88 by thermal analysis data, e.g. TGA, DTA, DSC
• CPC Class Codes: C01P 2004/64 Nanometer sized, i.e. from 1-100 nanometer
• CPC Class Codes: C09C 1/00 Treatment of specific inorganic materials other than fibrous fillers tenebrescent materials C09K9/00; luminescent materials C09K11/00; Preparation of carbon black
• CPC Class Codes: Y10T 428/25 Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
• CPC Class Codes: Y10T 428/31504 Composite [nonstructural laminate]
• CPC Class Codes: Y10T 428/31529 Next to metal
• CPC Class Codes: Y10T 428/31551 Of polyamidoester [polyurethane, polyisocyanate, polycarbamate, etc.]
• CPC Class Codes: Y10T 428/31609 Particulate metal or metal compound-containing
• CPC Class Codes: Y10T 428/31681 Next to polyester, polyamide or polyimide [e.g., alkyd, glue, or nylon, etc.]
• CPC Class Codes: Y10T 428/31786 Of polyester [e.g., alkyd, etc.]
• CPC Class Codes: Y10T 428/31855 Of addition polymer from unsaturated monomers

Abstract

Zirconia particles, methods of making zirconia particles, composite materials that contain the zirconia particles, methods of making the composite materials, and zirconia sols that contain the zirconia particles are described. The zirconia particles are substantially non-associated and have an average size no greater than 50 nanometers and may contain yttrium. The zirconia particles are prepared by a method that includes two separate hydrothermal treatments.

Claims

1. A method of making a composite material, said method comprising:

forming a zirconia sol comprising;

preparing a first feedstock comprising a zirconium salt;

subjecting the first feedstock to a first hydrothermal treatment to form a zirconium-containing intermediate and a byproduct;

forming a second feedstock by removing at least a portion of the byproduct of the first hydrothermal treatment; and

subjecting the second feedstock to a second hydrothermal treatment to form a zirconia sol comprising zirconia particles;

adding an organic matrix material; and

removing at least a portion of a liquid phase from the zirconia sol.

2. The method of claim 1, wherein the first feedstock further comprises an yttrium salt.

3. The method of claim 1, wherein the zirconium-containing intermediate has a percent conversion of 40 to 75 percent.

4. The method of claim 1, wherein forming the second feedstock comprises removing an acidic byproduct formed during the first hydrothermal treatment.

5. The method of claim 1, wherein the zirconia sol is substantially free of a polyether carboxylic acid.

6. The method of claim 1, wherein the zirconia particles comprise 0.1 to 8 weight percent yttrium based on a weight of inorganic oxides in the zirconia particles, have an average primary particle size no greater than 50 nanometers, have a dispersion index of 1 to 3, and have a crystal structure that is at least 70 percent cubic, tetragonal, or combination thereof.

7. The method of claim 1, further comprising reacting the surface of the zirconia particles with a surface modifying agent.

8. The method of claim 7, wherein the surface modifying agent is reactive with the organic matrix.

9. The method of claim 8, wherein the surface modifying agent comprises beta-carboxyethyl acrylate, mono-2-(methacryloxyethyl)succinate, mono(methacryloxypolyethylene glycol)succinate, or combinations thereof.

10. The method of claim 1, wherein removing at least a portion of the liquid phase from the zirconia sol occurs prior to adding the organic matrix.

11. The method of claim 1, further comprising modifying the surface of the zirconia particles with a surface modifying agent having a non-polar group and extracting the surface modified zirconia particles into a water immiscible solvent or monomer.

12. The method of claim 1, wherein the organic matrix comprises polymerizable monomers or reactive oligomers.

13. The method of claim 12, further comprising reacting the organic matrix is reacted to form a polymeric material.

14. A method of making a composite material, the method comprising:

forming a zirconia sol using a hydrothermal method wherein the zirconia sol product of the hydrothermal method prior to any additional treatment comprises zirconia particles dispersed in an aqueous medium comprising a carboxylic acid, wherein the carboxylic acid has no greater than four carbon atoms and is substantially free of a polyether carboxylic acid and wherein the zirconia particles have an average primary particle size no greater than 30 nanometers, a dispersion index of 1 to 5, and a crystal structure that is at least 50 percent cubic, tetragonal, or a combination thereof;

adding an organic matrix material to the zirconia sol; and

removing at least a portion of the aqueous medium from the zirconia sol.

15. The method of claim 14, wherein the zirconia particles comprise 0.1 to 8 weight percent yttrium based on a weight of inorganic oxides in the zirconia particles.

16. The method of claim 14, further comprising reacting the surface of the zirconia particles with a surface modifying agent.

17. The method of claim 16, wherein the surface modifying agent is reactive with the organic matrix.

18. The method of claim 17, wherein the surface modifying agent comprises beta-carboxyethyl acrylate, mono-2-(methacryloxyethyl)succinate, mono(methacryloxypolyethylene glycol)succinate, or combinations thereof.

19. The method of claim 14, wherein removing at least a portion of the liquid phase from the zirconia sol occurs prior to adding the organic matrix.

20. The method of claim 14, further comprising modifying the surface of the zirconia particles with a surface modifying agent having a non-polar group and extracting the surface modified zirconia particles into a water immiscible solvent or monomer.