Method of making quantum dots

Patent metadata

Field	Value
Publication number	US-9850593-B2
Application number	US-201414284292-A
Country	US
Kind code	B2
Filing date	May 21, 2014
Priority date	Nov 22, 2011
Publication date	Dec 26, 2017
Grant date	Dec 26, 2017

Abstract

Quantum dots and methods of making quantum dots are provided.

First claim

What is claimed is:

1. A method for making quantum dots comprising:
combining one or more highly reactive chalcogenide precursors comprising a secondary phosphine chalcogenide, one or more highly reactive metal precursors comprising a metal carboxylate, a solvent, and a seed stabilizing agent comprising a phosphonic acid at a reaction temperature above about 200° C. to form a reaction mixture where the ratio of metal to chalcogenide is in a range from about 1:1 to about 1:0.5, wherein the solvent and the seed stabilizing agent are not the same, and
quenching the reaction mixture after nucleation by cooling the reaction mixture to a quenching temperature that is lower than the reaction temperature, resulting in seed quantum dots, and
adding additional stoichiometric amounts of the highly reactive secondary phosphine chalcogenide precursor comprising a secondary phosphine chalcogenide and the highly reactive metal precursor comprising a metal carboxylate to the quenched reaction mixture including the seed quantum dots under conditions suitable to increase the size of the seed quantum dots to a desired size.

2. A method in accordance with claim 1 wherein a metal precursor comprises cadmium oleate (Cd(Oleate) 2 ).

3. A method m accordance with claim 1 wherein the seed stabilizing agent is octadecylphosphonic acid.

4. A method in accordance with claim 1 wherein the reaction temperature is sufficient to form the quantum dots.

5. A method in accordance with claim 1 wherein quenching comprises dropping the temperature to a temperature sufficiently low to prevent nucleation and Ostwald ripening.

6. A method in accordance with claim 1 wherein quenching comprises dropping the temperature to a temperature sufficiently low to prevent nucleation and Ostwald ripening, but is sufficiently high for a subsequent growth of the quantum dot.

7. A method in accordance with claim 1 wherein the seed quantum dots comprise CdSe and the reaction temperature is about 270° C.

8. A method in accordance with claim 1 wherein the step of quenching the reaction mixture is accomplished by rapid addition of a non-coordinating solvent to the reaction mixture sufficient to lower the reaction mixture temperature to the quenching temperature.

9. A method in accordance with claim 8 wherein the non-coordinating solvent is 1-octadecene.

10. A method in accordance with claim 7 wherein the quenching temperature is in a range from about 200 to about 240° C.

11. A method in accordance with claim 1 wherein the quantum dots are increased to a desired size at which the reaction mixture lacks unreacted metal precursor and unreacted secondary phosphine chalcogenide precursor.

12. A method according to claim 11 wherein the quantum dots of desired size are removed from the reaction mixture without purification and are then overcoated with a coating.

13. A method in accordance with claim 12 wherein the coating comprises one or more semiconductor materials, at least one of which is different from the composition of the quantum dot being coated.

14. A method in accordance with claim 12 wherein the quantum dots of desired size are overcoated without purification in the reaction mixture with a coating comprising one or more semiconductor materials.

15. A method in accordance with claim 12 wherein the coating comprises two or more layers.

16. A method in accordance with claim 1 wherein the additional amounts of the metal precursor and the secondary phosphine chalcogenide precursor are provided to a reaction vessel including the quantum dots as a substantially steady or substantially constant infusion such that as metal and chalcogenide precursors are consumed or otherwise used to grow the quantum dots, additional supply of metal and chalcogenide precursors are provided to the reaction vessel to continue growth of the quantum dots until a desired quantum dot size is reached.

Assignees

• Samsung Electronics Co Ltd
• Samsung Electronics Co Ltd

Inventors

• Liu Wenhao
• Breen Craig

Classifications

• H10P14/3461

  Nanoparticles · CPC title

• H10P14/3431

  Selenides · CPC title

• H10P14/265

  using solutions · CPC title

• H10P14/3428 Primary

  Sulfides · CPC title

• B22F1/17

  Metallic particles coated with metal · CPC title