IP Library Granted Patent US 7,235,190
Granted Patent B1
US 7,235,190 · App. 10/933,069 · Granted Jun 26, 2007

Nanocluster-based white-light-emitting material employing surface tuning

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Quick Facts
Patent No.
US 7,235,190
App. No.
10/933,069
Granted
Jun 26, 2007
Kind
B1
Abstract

A method for making a nanocrystal-based material capable of emitting light over a sufficiently broad spectral range to appear white. Surface-modifying ligands are used to shift and broaden the emission of semiconductor nanocrystals to produce nanoparticle-based materials that emit white light.

Claims (49)

1. A method for making a white-light-emitting material, comprising:

forming a solution of CdS nanocrystals;

reacting a surface of said CdS nanocrystals with a surface-modifying compound to form a solution of surface-dominated light-emitting nanoparticles; aging said surface-dominated light-emitting nanoparticles to broaden a light-emission spectrum of said surface-dominated light-emitting nanoparticles to produce a white-light-emitting material, wherein said solution of CdS nanocrystals is formed by an inverse micelle method.

2. The method of claim 1 , wherein a Cd salt used to form said solution of CdS nanocrystals by said inverse micelle method is selected from the group consisting of cadmium nitrate, cadmium chloride, cadmium iodide, and cadmium perchlorate.

3. The method of claim 1 , wherein a sulfide source used to form said solution of CdS nanocrystals by said inverse micelle method is selected from the group consisting of ammonium sulfide, hydrogen sulfide, lithium sulfide, and sodium sulfide.

4. The method of claim 1 , wherein a first solvent used to form said solution of CdS nanocrystals by said inverse micelle method is selected from the group consisting of alkanes, aromatic hydrocarbons, ethers, cyclic ethers, tetrahydrofuran, and alcohols containing at least 8 carbon atoms.

5. The method of claim 1 , wherein a first surfactant used to form said solution of CdS nanocrystals by said inverse micelle method comprises an anionic surfactant.

6. The method of claim 1 , wherein a first surfactant used to form said solution of CdS nanocrystals by said inverse micelle method is selected from the group consisting of AOT, quaternary ammonium salts comprising alkyl chains containing 16 or more carbon atoms, and alkylated polyethers of the formula CH 3 (CH 2 ) m (CH 2 CH 2 O) n OH where m is at least 8 and n is at least 4.

7. A method for making a white-light-emitting material, comprising:

forming a solution of CdS nanocrystals;

reacting a surface of said CdS nanocrystals with a surface-modifying compound to form a solution of surface-dominated light-emitting nanoparticles; and

aging said surface-dominated light-emitting nanoparticles to broaden a light-emission spectrum of said surface-dominated light-emitting nanoparticles to produce a white-light-emitting material, wherein the step of forming said solution of CdS nanocrystals comprises dissolving a plurality of preformed CdS nanocrystals in a solvent solution.

8. The method of claim 7 , wherein said solvent solution comprises a second solvent and a second surfactant.

9. The method of claim 8 , wherein said second surfactant is selected from the group consisting of AOT, quaternary ammonium salts comprising alkyl chains containing at least 16 carbon atoms, and alkylated polyethers of the formula CH 3 (CH 2 ) m (CH 2 CH 2 O) n OH where m is at least 8 and n is at least 4.

10. The method of claim 8 , wherein said second solvent is selected from the group consisting of alkyl hydrocarbons, aromatic hydrocarbons, and alcohols containing 8 or more carbon atoms.

11. A method for making a white-light-emitting material, comprising:

forming a solution of CdS nanocrystals;

reacting a surface of said CdS nanocrystals with a surface-modifying compound to form a solution of surface-dominated light-emitting nanoparticles; a aging said surface-dominated light-emitting nanoparticles to broaden a light-emission spectrum of said surface-dominated light-emitting nanoparticles to produce a white-light-emitting material, and encapsulating said aged surface-dominated light-emitting nanoparticles with an encapsulant to produce a white-light-emitting material.

12. The method of claim 11 , wherein said solution of CdS nanocrystals is formed by an inverse micelle method.

13. The method of claim 12 , wherein a Cd salt used to form said solution of CdS nanocrystals by said inverse micelle method is selected from the group consisting of cadmium nitrate, cadmium chloride, cadmium iodide, and cadmium perchlorate.

14. The method of claim 12 , wherein a sulfide source used to form said solution of CdS nanocrystals by said inverse micelle method is selected from the group consisting of ammonium sulfide, hydrogen sulfide, lithium sulfide, and sodium sulfide.

15. The method of claim 12 , wherein a fourth solvent used to form said solution of CdS nanocrystals by said inverse micelle method is selected from the group consisting of alkanes, tetrahydrofuran, alcohols containing at least 8 carbon atoms, octyl ether, and benzyl ether.

16. The method of claim 12 , wherein a third surfactant used to form said solution of CdS nanocrystals by said inverse micelle method comprises an anionic surfactant.

17. The method of claim 12 , wherein a third surfactant used to form said solution of CdS nanocrystals by said inverse micelle method is selected from the group consisting of AOT, quaternary ammonium salts comprising alkyl chains containing at least 16 carbon atoms, and alkylated polyethers of the formula CH 3 (CH 2 ) m (CH 2 CH 2 O) n OH where m is at least 8 and n is at least 4.

18. The method of claim 11 , wherein a method for forming said solution of CdS nanocrystals comprises dissolving a plurality of preformed CdS nanocrystals in a solvent solution.

19. The method of claim 18 , wherein said solvent solution comprises a fifth solvent and a fourth surfactant.

20. The method of claim 19 , wherein said fourth surfactant is selected from the group consisting AOT, quaternary ammonium salts comprising alkyl chains containing at least 10 carbon atoms, and alkylated polyethers of the formula CH 3 (CH 2 ) m (CH 2 CH 2 O) n OH where m is at least 8 and n is at least 4.

21. The method of claim 19 , wherein said fifth solvent is selected from the group consisting of alkyl hydrocarbons containing between 5 and 16 carbon atoms, ethers, cyclic ethers, tetrahydrofuran, and alcohols containing at least 6 carbon atoms.

22. The method of claim 11 , wherein said surface-modifying compound comprises an electron-donating ligand.

23. The method of claim 11 , wherein said surface-modifying compound is selected from a group consisting of thiols, amines, and phosphines.

24. The method of claim 11 , wherein said encapsulant is selected from the group consisting of AOT, tri-octyl phosphine, an ormosil, a silica glass, a silicone, and an epoxy.

25. A method for making a white-light-emitting material, comprising:

forming a solution of CdS nanocrystals in a solvent solution;

reacting a surface of said CdS nanocrystals with a surface-modifying compound to form a solution of surface-dominated light-emitting nanoparticles;

aging said solution of said surface-dominated light-emitting nanoparticles to broaden a light-emission spectrum of said surface-dominated light-emitting nanoparticles to form a solution of aged surface-dominated light-emitting nanoparticles:

applying said solution to a surface;

and

evaporating said solvent from said solution of aged surface-dominated light-emitting nanoparticles to form a film containing said aged surface-dominated light-emitting nanoparticles to produce a white-light-emitting material.

26. The method of claim 25 , wherein said surface-modifying compound is selected from a group consisting of thiols, amines, and phosphines.

27. The method of claim 25 , wherein said solvent solution comprises a solvent and a surfactant.

28. The method of claim 27 , wherein said surfactant is selected from the group consisting of AOT, quaternary ammonium salts comprising alkyl chains containing 16 or more carbon atoms, and alkylated polyethers of the formula CH 3 (CH 2 ) m (CH 2 CH 2 O) n OH where m is at least 8 and n is at least 4.

29. The method of claim 27 , wherein said solvent is selected from the group consisting of alkanes, aromatic hydrocarbons, ethers, cyclic ethers, tetrahydrofuran, and alcohols containing at least 8 carbon atoms.

30. A method for making a white-light-emitting material comprising:

combining approximately 2 wt % Li 4 [S 4 Cd 10 (SC 6 H 5 ) 16 ] with approximately 98 wt % (aminopropyl)methylsiloxane-dimethylsiloxane copolymer to form a mixture;

deaerating the mixture;

heating the mixture to an elevated temperature to form a plurality of CdS nanocrystals; and

combining the mixture with an encapsulant precursor solution to form a nanoparticle-containing precursor solution.

31. The method of claim 30 , wherein said elevated temperature is between 100° C. and 250° C.

32. The method of claim 30 , further comprising curing the nanoparticle-containing precursor solution to form a white-light-emitting material.

Assignments (3)
CHANGE OF NAME Recorded Sep 6, 2017
From: SANDIA CORPORATION
To: NATIONAL TECHNOLOGY & ENGINEERING SOLUTIONS OF SANDIA, LLC
Reel/Frame 043767/0054 →
CONFIRMATORY LICENSE Recorded Dec 20, 2004
From: SANDIA CORPORATION
To: ENERGY, U.S. DEPARTMENT OF
Reel/Frame 015474/0672 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 6, 2004
From: WILCOXON, JESS P.; ABRAMS, BILLIE L.; THOMA, STEVEN G.
To: SANDIA CORPORATION, OPERATOR OF SANDIA NATIONAL LABORATORIES
Reel/Frame 015427/0775 →