Metal oxide nanoparticles, methods of making, and methods of use

• US 20050063898A1
• Filed: 08/29/2003
• Published: 03/24/2005
• Est. Priority Date: 08/29/2003
• Status: Active Grant

• Current Assignee: Sabic Innovative Plastics IP BV (Government of Saudi Arabia)
• Original Assignee: General Electric Company
• Inventors: Ja Chisholm, Bret
• Granted Patent: US 7,169,375 B2
• Time in Patent Office: Days
• US Class Current: 423/608
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01G 1/00 Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general electrolytic production of inorganic compounds C25B1/00
• CPC Class Codes: C01G 19/02 Oxides
• CPC Class Codes: C01G 23/053 Producing by wet processes, e.g. hydrolysing titanium salts
• CPC Class Codes: C01G 25/02 Oxides
• CPC Class Codes: C01P 2004/64 Nanometer sized, i.e. from 1-100 nanometer
• CPC Class Codes: C09C 1/3684 Treatment with organo-silicon compounds
• CPC Class Codes: C09C 3/12 Treatment with organosilicon compounds C09C3/006 takes precedence
• CPC Class Codes: Y10S 977/773 Nanoparticle, i.e. structure having three dimensions of 100 nm or less
• CPC Class Codes: Y10S 977/775 Nanosized powder or flake, e.g. nanosized catalyst
• CPC Class Codes: Y10S 977/777 Metallic powder or flake
• CPC Class Codes: Y10S 977/811 Of specified metal oxide composition, e.g. conducting or semiconducting compositions such as ITO, ZnOx

Abstract

Disclosed is a method of preparing treated metal oxide nanoparticles from sols prepared from metal alkoxides and organosilanes. The treated nanoparticles are useful high refractive index additives in the manufacture of optical articles.

Claims

1. A method of making metal oxide nanoparticles, comprising:

hydrolyzing metal alkoxide with an acidic alcohol solution, wherein the acidic alcohol solution comprises an alkyl alcohol, water, and an acid to form a first sol comprising metal oxide nanoparticles;

treating the first sol with an organosilane to form a second sol comprising treated metal oxide nanoparticles; and

treating the second sol with an organic base in an amount of about 0.1;

1 to about 0.9;

1 molar ratio of organic base to acid to form a third sol comprising treated metal oxide nanoparticles.

2. The method of claim 1, wherein the metal is titanium, cerium, zirconium, or tin;

and the alkoxide is a linear or branched C₁-C₁₂ alkoxide.

3. The method of claim 1, wherein the acid is present in an amount of about 0.1:

1 to about 2;

1 molar ratio of acid to metal alkoxide.

4. The method of claim 1, wherein the water is present in an amount of about 0.1:

1 to about 5;

1 molar ratio of water to metal alkoxide.

5. The method of claim 1, wherein the organosilane is an alkoxyorganosilane, an aryloxyorganosilane, an arylalkoxyorganosilane, an arlyalkylalkoxyorganosilane, an alkylaminoorganosilane, or a combination comprising at least one of the foregoing organosilanes.

6. The method of claim 1, wherein the organosilane lacks groups reactive with a polymerizable compound.

7. The method of claim 1, wherein the organosilane is in an amount of about 1:

1 to about 1;

10 molar ratio of metal alkoxide to organosilane.

8. The method of claim 1, wherein the organic base is a linear or branched chain C₁-C₁₂ alkylamine.

9. The method of claim 1, wherein the second sol is formed at a temperature of about 25°

C. to about 100°

C. for about 8 hours.

10. The method of claim 1, further comprising combining a polymerizable compound with the third sol to form a mixture;

and removing solvent from the mixture to form a polymerizable composition.

11. The method of claim 10, wherein the polymerizable composition exhibits a yellowness index of less than about 30 as measured by ASTM D1925 using a path length of 1 mm.

12. The method of claim 10, further comprising combining an initiator with the third sol.

13. An article prepared from curing the polymerizable composition of claim 10.

14. An optical article or light management film prepared from curing the polymerizable composition of claim 10.

15. A method of making titanium oxide nanoparticles, comprising:

hydrolyzing titanium tetraalkoxide with an acidic alcohol solution to form a first sol comprising titanium oxide nanoparticles, wherein the acidic alcohol solution comprises

an alkyl alcohol,

water in an amount of about 0.1;

1 to about 5;

1 molar ratio of water to titanium tetraalkoxide, and

an acid in an amount of about 0.1;

1 to about 2;

1 molar ratio of acid to titanium tetraalkoxide;

treating the first sol with an organosilane to form a second sol comprising treated titanium oxide nanoparticles; and

treating the second sol with an organic base in an amount of about 0.1;

1 to about 0.9;

1 molar ratio of organic base to acid to form a third sol comprising treated titanium oxide nanoparticles.

16. The method of claim 15, further comprising combining a polymerizable compound with the third sol to form a mixture;

and removing solvent from the mixture to form a polymerizable composition.

17. The method of claim 16, wherein the polymerizable composition exhibits a yellowness index of less than about 30 as measured by ASTM D1925 using a path length of 1 mm.

18. An article prepared from curing the polymerizable composition of claim 16.

19. A composition, comprising:

a polymerizable compound; and

treated titanium oxide nanoparticles, wherein the treated titanium oxide nanoparticles are prepared by hydrolyzing titanium tetraalkoxide with an acidic alcohol solution to form a first sol, wherein the acidic alcohol solution comprises

an alkyl alcohol,

water in an amount of about 0.1;

1 to about 5;

1 molar ratio of water to titanium tetraalkoxide, and

an acid in an amount of about 0.1;

1 to about 2;

1 molar ratio of acid to titanium tetraalkoxide;

treating the first sol with an organosilane to form a second sol; and

treating the second sol with an organic base in an amount of about 0.1;

1 to about 0.9;

1 molar ratio of organic base to acid to form a third sol comprising treated titanium oxide nanoparticles.