Continuous synthesis of upconverting nanoparticles

Patent metadata

Field	Value
Publication number	US-11649173-B2
Application number	US-202117237836-A
Country	US
Kind code	B2
Filing date	Apr 22, 2021
Priority date	Apr 22, 2020
Publication date	May 16, 2023
Grant date	May 16, 2023

Abstract

Synthesizing upconverting nanoparticles includes heating a precursor solution comprising one or more rare earth salts, an alkali metal salt or alkaline earth salt, and a solvent comprising a plasticizer in a microwave reactor to yield a product mixture, and cooling the product mixture to yield the upconverting nanoparticles. Core-shell upconverting nanoparticles are synthesized by combining the upconverting nanoparticles with a precursor solution comprising one or more rare earth salts, an alkali metal salt or alkaline earth salt, and a solvent comprising a plasticizer to yield a nanoparticle mixture, heating the nanoparticle mixture in a microwave reactor to yield a product mixture, and cooling the product mixture to yield the core-shell upconverting nanoparticles.

First claim

What is claimed is:

1. A method of synthesizing upconverting nanoparticles, the method comprising:
heating a precursor solution comprising one or more rare earth salts, an alkali metal salt or an alkaline earth salt, and a solvent in a microwave reactor to yield a product mixture; and
cooling the product mixture to yield the upconverting nanoparticles, wherein at least one of the one or more rare earth salts comprises trifluoroacetate, and the solvent comprises oleic acid and a plasticizer including one or both of dioctyl terephthalate and bis(2-ethylhexyl) adipate.

2. The method of claim 1 , wherein the one or more rare earth salts comprise one or more of yttrium, ytterbium, and erbium.

3. The method of claim 1 , wherein a boiling point of the plasticizer at atmospheric pressure is at least 320° C.

4. The method of claim 1 , wherein a dielectric permittivity of the plasticizer is at least 4 or at least 5.

5. The method of claim 1 , wherein the plasticizer further comprises dibutyl phthalate.

6. The method of claim 1 , comprising heating the precursor solution to a temperature of at least 280° C.

7. The method of claim 6 , comprising heating the precursor solution to a temperature of at least 305° C.

8. The method of claim 1 , wherein heating the product mixture comprises heating for a length of time between 5 minutes and 45 minutes.

9. The method of claim 1 , further comprising flowing the precursor solution through the microwave reactor.

10. A method of synthesizing core-shell upconverting nanoparticles, the method comprising:
heating a precursor solution comprising one or more rare earth metal salts, an alkali metal salt or an alkaline earth metal salt, and a solvent in a microwave reactor;
combining the upconverting nanoparticles of claim 1 with the precursor solution to yield a nanoparticle mixture;
heating the nanoparticle mixture in the microwave reactor to yield a product mixture; and
cooling the product mixture to yield the core-shell upconverting nanoparticles, wherein at least one of the one or more rare earth salts comprises trifluoroacetate, and the solvent comprises oleic acid and a plasticizer including one or both of dioctyl terephthalate and bis(2-ethylhexyl) adipate.

11. The method of claim 10 , wherein the upconverting nanoparticles comprise cubic nanoparticles.

12. The method of claim 10 , wherein the upconverting nanoparticles comprise hexagonal nanoparticles.

13. The method of claim 10 , wherein a boiling point of the plasticizer at atmospheric pressure is at least 320° C.

14. The method of claim 10 , wherein a dielectric permittivity of the plasticizer is at least 4 or at least 5.

15. The method of claim 10 , wherein the plasticizer further comprises dibutyl phthalate.

16. The method of claim 10 , comprising heating the precursor solution to a temperature of at least 280° C.

17. The method of claim 16 , comprising heating the precursor solution to a temperature of at least 305° C.

18. The method of claim 10 , further comprising flowing the precursor solution through the microwave reactor.

Assignees

• Egatz Gomez Ana
• Ros Alexandra
• Univ Arizona State

Inventors

• Egatz-Gomez Ana
• Ros Alexandra

Classifications

• B01J2219/00162

  controlling the pressure · CPC title

• B01J2219/00141

  Microwaves · CPC title

• C01F17/265

  Fluorides · CPC title

• B82Y30/00

  Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title

• C01F17/36 Primary

  halogen being the only anion, e.g. NaYF4 · CPC title