Passivated metal nanoparticles having an epoxide-based oligomer coating

Patent metadata

Field	Value
Publication number	US-9745190-B2
Application number	US-201113178398-A
Country	US
Kind code	B2
Filing date	Jul 7, 2011
Priority date	Jul 7, 2010
Publication date	Aug 29, 2017
Grant date	Aug 29, 2017

Abstract

This invention provides metal nanoparticles (e.g., aluminum, chromium, iron and magnesium) having an epoxide-based oligomer coating, compositions thereof, method of making the same, and methods of use thereof, including for energy related applications.

First claim

What is claimed is:

1. A non-pyrophoric nanoparticle comprising:
a) a core comprising metallic aluminum, wherein the core is greater than 70% by weight metallic aluminum, and less than 10% aluminum oxide; and
b) a coating surrounding the core, wherein the coating comprises an epoxide-based oligomer comprising a repeat unit having the following structure prior to any cross-polymerization:

wherein:
n is 2 to 20;

R 1 is H, alkyl (C≦18) , alkenyl (C≦18) , alkynyl (C≦18) , acyl (C≦18) , aryl (C≦18) , aralkyl (C≦18) , heteroaryl (C≦18) , alkoxy (C≦18) , acyloxy (C≦18) , alkylamino (C≦18) , dialkylamino (C≦18) , amido (C≦18) or a substituted version thereof; and
R 2 is alkenyl (C≦18) ,

and wherein the molar ratio of the aluminum to a monomer of the epoxide-based oligomer is from about 0.5:1 to about 10:1.

2. The non-pyrophoric nanoparticle of claim 1 , wherein R 1 is H.

3. The non-pyrophoric nanoparticle of claim 1 , wherein R 2 is octa-7-en-1-yl.

4. The non-pyrophoric nanoparticle according to claim 1 , wherein the R 2 groups of one or more of the oligomers have been cross-polymerized to one another.

5. The non-pyrophoric nanoparticle of claim 4 , wherein the cross-polymerization comprises an olefin polymerization reaction of the carbon-carbon double bonds of the R 2 groups.

6. The non-pyrophoric nanoparticle of 4 , wherein the cross polymerization further comprises a co-polymerization of the double bonds of the R 2 groups with the double bonds of an alkadiene (C4-30) .

7. The non-pyrophoric nanoparticle of claim 6 , wherein the alkadiene (C4-30) is 1,13 tetradecadiene.

8. The non-pyrophoric nanoparticle of claim 1 , wherein the molar ratio of the aluminum to the monomer of the epoxide-based oligomer is from about 1:1 to about 5:1.

9. The non-pyrophoric nanoparticle of claim 8 , wherein the molar ratio of the aluminum to the monomer of the epoxide-based oligomer is about 1:1.

10. The non-pyrophoric nanoparticle of claim 8 , wherein the molar ratio of the aluminum to the monomer of the epoxide-based oligomer is about 2:1.

11. The non-pyrophoric nanoparticle of claim 8 , wherein the molar ratio of the aluminum to the monomer of the epoxide-based oligomer is about 5:1.

12. The non-pyrophoric nanoparticle of claim 1 , wherein the core is greater than 80% by weight aluminum.

13. The non-pyrophoric nanoparticle of claim 12 , wherein the core is greater than 90% by weight aluminum.

14. The non-pyrophoric nanoparticle of claim 13 , wherein the core is greater than 95% by weight aluminum.

15. The non-pyrophoric nanoparticle of claim 1 , wherein the core is less than 5% by weight aluminum oxide.

16. The non-pyrophoric nanoparticle according to claim 1 , wherein the nanoparticle has an average diameter from about 10 nm to about 500 nm.

17. The non-pyrophoric nanoparticle of claim 16 , wherein the nanoparticle has an average diameter from about 10 nm to about 300 nm.

18. The non-pyrophoric nanoparticle of claim 17 , wherein the nanoparticle has an average diameter from about 10 to about 150 nm.

19. The non-pyrophoric nanoparticle of claim 17 , wherein the nanoparticle has an average diameter from about 10 to about 40 nm.

20. The non-pyrophoric nanoparticle of claim 19 , wherein the nanoparticle has an average diameter of about 19 nm.

21. The non-pyrophoric nanoparticle of claim 19 , wherein the nanoparticle has an average diameter of about 25 nm.

22. The non-pyrophoric nanoparticle of claim 17 , wherein the nanoparticle has a diameter of about 100 nm.

23. A method for the preparation of a non-pyrophoric nanoparticle, comprising reacting an alane-amine complex with titanium isopropoxide and an epoxide monomer to form the non-pyrophoric nanoparticle.

24. The method of claim 23 , wherein the alane amine complex is N,N-dimethylethylamine alane.

25. The method of claim 23 , wherein the alane amine complex is dissolved in a first solvent prior to the reacting of the alane-amine complex with titanium isopropoxide and the epoxide monomer.

26. The method of claim 25 , wherein the first solvent comprises toluene.

27. The method of claim 25 , wherein the first solvent comprises diethyl ether.

28. The method of claim 23 , wherein the titanium isopropoxide is dissolved in a second solvent prior to the reacting of the alane-amine complex with titanium isopropoxide and the epoxide monomer.

29. The method of claim 28 , wherein the second solvent comprises toluene.

30. The method of claim 23 , wherein the reacting of the alane-amine complex with titanium isopropoxide and the epoxide monomer occurs at approximately 300K and over approximately from about 10 to about 60 minutes.

31. The method of claim 23 , wherein the reacting of the alane-amine complex with titanium isopropoxide and the epoxide monomer occurs at from about 300K to about 450K.

32. The method of claim 23 , further comprising removing the solvent after the reacting of the alane-amine complex with titanium isopropoxide and the epoxide monomer.

33. The method of claim 23 , further comprising cross-polymerizing two or more R 1 or R 2 groups so that one oligomer chain is covalently attached with R 1 or R 2 of another oligomer chain's R 1 or R 2 group.

Assignees

• Jelliss Paul
• Buckner Steven
• Chung Stephen W
• Thomas Brandon J
• Univ Saint Louis

Inventors

• Jelliss Paul
• Buckner Steven
• Chung Stephen W
• Thomas Brandon J

Classifications

• B22F1/054

  Nanosized particles · CPC title

• B22F1/102

  Metallic powder coated with organic material · CPC title

• B22F1/0018

  Operations & Transport · mapped topic

• Y10T428/2991

  Coated · CPC title

• B22F2999/00

  Aspects linked to processes or compositions used in powder metallurgy · CPC title