IP Library Granted Patent US 8,961,828
Granted Patent B2
US 8,961,828 · App. 13/989,306 · Granted Feb 24, 2015

Colloidal infrared reflective and transparent conductive aluminum-doped zinc oxide nanocrystals

Inventors: Raffaella Buonsanti (Berkeley, CA); Delia J. Milliron (Oakland, CA)
Assignee: The Regents of the University of California
C30B7/14C30B29/16H01L31/022483C01G9/02C30B29/22H01B1/02C01P2002/54C01P2002/72C01P2002/77C01P2002/82C01P2002/84C01P2002/85C01P2004/04C01P2004/64B82Y30/00
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Quick Facts
Patent No.
US 8,961,828
App. No.
13/989,306
Granted
Feb 24, 2015
Kind
B2
Abstract

The present invention provides a method of preparing aluminum-doped zinc oxide (AZO) nanocrystals. In an exemplary embodiment, the method includes (1) injecting a precursor mixture of a zinc precursor, an aluminum precursor, an amine, and a fatty acid in a solution of a vicinal diol in a non-coordinating solvent, thereby resulting in a reaction mixture, (2) precipitating the nanocrystals from the reaction mixture, thereby resulting in a final precipitate, and (3) dissolving the final precipitate in an apolar solvent. The present invention also provides a dispersion. In an exemplary embodiment, the dispersion includes (1) nanocrystals that are well separated from each other, where the nanocrystals are coated with surfactants and (2) an apolar solvent where the nanocrystals are suspended in the apolar solvent. The present invention also provides a film. In an exemplary embodiment, the film includes (1) a substrate and (2) nanocrystals that are evenly distributed on the substrate.

Claims (31)

1. A method comprising:

injecting a precursor mixture comprising a zinc precursor, an aluminum precursor, an amine, and a fatty acid into a solution of a vicinal diol and a non-coordinating solvent to produce a reaction mixture, wherein the non-coordinating solvent is selected from a group consisting of octadecene, benzylether, and phenylether;

precipitating aluminum-doped zinc oxide nanocrystals from the reaction mixture to form a final precipitate; and

dissolving the final precipitate in an apolar solvent.

2. The method of claim 1 , wherein the zinc precursor is selected from a group consisting of zinc stearate, zinc acetylacetonate, and zinc acetate.

3. The method of claim 1 , wherein the aluminum precursor is selected from a group consisting of aluminum acetylacetonate, aluminum stearate, and aluminum oleate.

4. The method of claim 1 , wherein the amine comprises oleylamine.

5. The method of claim 1 , wherein the fatty acid is selected from a group consisting of oleic acid and stearic acid.

6. The method of claim 1 , wherein the vicinal diol is selected from a group consisting of 1,2-dodecanediol, 1,2-hexadecanediol, and 1-2 octanediol.

7. A method comprising:

injecting a precursor mixture comprising a zinc precursor, an aluminum precursor, an amine, and a fatty acid into a solution of a vicinal diol and a non-coordinating solvent to produce a reaction mixture, wherein the aluminum precursor is selected from a group consisting of aluminum stearate and aluminum oleate;

precipitating aluminum-doped zinc oxide nanocrystals from the reaction mixture to form a final precipitate; and

dissolving the final precipitate in an apolar solvent.

8. The method of claim 1 , wherein precipitating the aluminum-doped zinc oxide nanocrystals comprises:

washing the aluminum-doped zinc oxide nanocrystals in the reaction mixture with a second apolar solvent;

dissolving the washed nanocrystals in a third apolar solvent; and

rinsing the dissolved nanocrystals in the second apolar solvent.

9. The method of claim 8 , wherein the second apolar solvent comprises ethanol and the third apolar solvent is selected from a group consisting of hexane and toluene.

10. The method of claim 1 , wherein the apolar solvent is selected from a group consisting of hexane, toluene, and chloroform.

11. The method of claim 1 , wherein a temperature of the solution is between 230° C. and 280° C. during the injecting.

12. The method of claim 1 , wherein a temperature of the solution between 210° C. and 260° C. during the precipitating.

13. The method of claim 1 , wherein precipitating the aluminum-doped zinc oxide nanocrystals comprises reacting the mixture with the solution to incorporate aluminum in the aluminum precursor into a crystal lattice of a zinc oxide reaction product.

14. The method of claim 1 , further comprising:

depositing the aluminum-doped zinc oxide nanocrystals on a substrate.

15. The method of claim 14 , wherein the substrate is selected from a group consisting of glass, silicon, quartz, indium tin oxide, and fluorine-doped SnO 2 .

16. The method of claim 14 , further comprising:

removing organic ligands from surfaces of the aluminum-doped zinc oxide nanoparticles.

17. A method comprising:

injecting a precursor mixture comprising a zinc precursor, an aluminum precursor, an amine, and a fatty acid into a solution of a vicinal diol and a non-coordinating solvent to produce a reaction mixture;

precipitating aluminum-doped zinc oxide nanocrystals from the reaction mixture to form a final precipitate; and

dissolving the final precipitate in an apolar solvent, wherein the apolar solvent comprises toluene.

Assignments (2)
CONFIRMATORY LICENSE Recorded Nov 1, 2013
From: REGENTS OF THE UNIVERSITY OF CALIFORNIA, THE
To: ENERGY, UNITED STATES DEPARTMENT OF
Reel/Frame 031611/0281 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 19, 2013
From: BUONSANTI, RAFFAELLA; MILLIRON, DELIA
To: THE REGENTS OF THE UNIVERSITY OF CALIFORNIA
Reel/Frame 030645/0544 →
Continuity (2)
Provisional Application 61417160 · Nov 24, 2010
Related Publication 20130266800A1 · Oct 10, 2013