Preparation method of formamidinium lead halide perovskite quantum dots

Patent metadata

Field	Value
Publication number	US-11208592-B2
Application number	US-201916420351-A
Country	US
Kind code	B2
Filing date	May 23, 2019
Priority date	Jun 6, 2018
Publication date	Dec 28, 2021
Grant date	Dec 28, 2021

Abstract

There is provided a method of preparing formamidinium lead halide perovskite quantum dots having a photoluminescence quantum yield higher than before. The disclosed method comprises steps of: preparing a lead halide solution by dissolving lead halide (II), oleic acid and oleylamine in a nonpolar solvent; preparing a formamidinium solution by dissolving formamidine acetate salt and oleic acid in a nonpolar solvent; mixing the formamidinium solution and the lead halide solution to form quantum dots; and centrifuging the mixed solution to obtain sediment; dispersing the sediment in a nonpolar solvent to prepare a crude quantum dot solution; mixing the crude quantum dot solution with methyl acetate; and centrifuging the crude quantum dot solution mixed with the methyl acetate to obtain sediment as purified quantum dots. The durable quantum dots are stably formed by injecting the lead halide solution into the formamidinium solution heated at 60° C.-90° C.

First claim

The invention claimed is:

1. A method of preparing formamidinium lead halide perovskite quantum dots, comprising steps of:
(a) preparing a lead halide solution by dissolving lead halide (II), oleic acid and oleylamine in a nonpolar solvent;
(b) preparing a formamidinium solution by dissolving formamidine acetate salt and oleic acid in a nonpolar solvent;
(c) mixing the formamidinium solution and the lead halide solution under hot conditions to form formamidinium lead halide perovskite quantum dots;
(d) purifying the quantum dots by centrifuging the mixed solution of the formamidinium solution and the lead halide solution in which the quantum dots have been formed to obtain sediment; dispersing the sediment in a nonpolar solvent to prepare a crude quantum dot solution; mixing the crude quantum dot solution with methyl acetate; and centrifuging the crude quantum dot solution mixed with the methyl acetate to obtain sediment as purified quantum dots.

2. The method of claim 1 , wherein a volume ratio of the methyl acetate and the crude quantum dot solution in the mixing is substantially 1:1 in the step (d).

3. The method of claim 1 , wherein the formamidinium solution and the lead halide solution are mixed under a temperature condition at 60° C.-90° C. in the step (c).

4. The method of claim 1 , wherein the formamidinium solution and the lead halide solution are mixed by injecting the lead halide solution into the formamidinium solution in the step (c).

5. The method of claim 1 , wherein the formamidinium solution and the lead halide solution are mixed such that a molar ratio of lead ions and formamidinium ions becomes from 1:3.75 to 1:15 in the step (c).

6. The method of claim 5 , wherein the formamidinium solution and the lead halide solution are mixed such that a molar ratio of lead ions and formamidinium ions becomes substantially 1:11.25.

7. A method of preparing formamidinium lead halide perovskite quantum dots, comprising steps of:
(e) preparing a lead halide solution by dissolving lead halide (II), oleic acid and oleylamine in a nonpolar solvent;
(f) preparing a formamidinium solution by dissolving formamidine acetate salt and oleic acid in a nonpolar solvent;
(g) mixing the formamidinium solution and the lead halide solution by injecting the lead halide solution into the formamidinium solution heated at 60° C.-90° C. to form formamidinium lead halide perovskite quantum dots.

8. The method of claim 7 , wherein the formamidinium solution and the lead halide solution are mixed such that a molar ratio of lead ions and formamidinium ions becomes from 1:3.75 to 1:15 in the step (c).

9. The method of claim 7 , wherein the formamidinium solution and the lead halide solution are mixed such that a molar ratio of lead ions and formamidinium ions becomes substantially 1:11.25.

Assignees

• Toyota Motor Co Ltd
• Univ Electro Communications

Inventors

• Masuda Taizo
• Sasaki Kiyoto
• Qing Shen
• Liu Feng
• Zhang Yaohong
• Ding Chao

Classifications

• C09K11/664

  Halogenides (C09K11/661 takes precedence) · CPC title

• C09K11/06 Primary

  containing organic luminescent materials · CPC title

• C01G21/16

  Halides · CPC title

• C07C257/12

  having carbon atoms of amidino groups bound to hydrogen atoms · CPC title

• C01P2002/34

  perovskite-type (ABO3) · CPC title