Method for fabrication of halide perovskite single crystal comprising low-temperature solvation process

Patent metadata

Field	Value
Publication number	US-12385156-B2
Application number	US-202318176505-A
Country	US
Kind code	B2
Filing date	Mar 1, 2023
Priority date	Sep 2, 2020
Publication date	Aug 12, 2025
Grant date	Aug 12, 2025

Abstract

The present disclosure relates to a method of preparing a halide perovskite single crystal, including a process of enhancing a solubility of a precursor by using a low-temperature solvent.

First claim

We claim:

1. A method of preparing a halide perovskite single crystal, comprising:
preparing a perovskite precursor solution by dissolving a perovskite raw material compound in a solvent;
increasing a solubility of the perovskite precursor solution by controlling a temperature of the perovskite precursor solution; and
growing the halide perovskite single crystal while gradually changing the temperature of the perovskite precursor solution with increased solubility,
wherein the increasing the solubility of the perovskite precursor solution includes lowering the temperature of the perovskite precursor solution by cooling the perovskite precursor solution.

2. The method of claim 1 ,
wherein the perovskite raw material compound includes MX 2 and R 1 NH 3 X, and
wherein the halide perovskite single crystal is represented by the following Chemical Formula 1:
R 1 NH 3 MX 3 ; and   [Chemical Formula 1]

in the Chemical Formula 1:
R 1 includes a linear or branched alkyl group comprising 1 to 10 carbon atoms,
M includes a metal cation selected from the group consisting of Pb 2+ , Cu 2+ , Ni 2+ , Co 2+ , Fe 2+ , Mn 2+ , Cr 2+ , Pd 2+ , Cd 2+ , Cs 2+ , Yb 2+ , Sn 2+ , Ge 2+ , Eu 2+ and combinations thereof, and
X includes a halogen anion.

3. The method of claim 2 ,
wherein the halogen is Cl or Br, and
wherein the growing the halide perovskite single crystal includes gradually increasing the temperature of the perovskite precursor solution with increased solubility.

4. The method of claim 1 ,
wherein, in the increasing of the solubility of the perovskite precursor solution, a temperature range of the cooled perovskite precursor solution is −60° C. to 0° C.

5. The method of claim 1 ,
wherein the degree of gradually changing the temperature of the perovskite precursor solution in the growing the halide perovskite single crystal is set differently for each temperature section of the perovskite precursor solution with increased solubility.

6. The method of claim 5 ,
wherein when the temperature of the perovskite precursor solution with increased solubility is gradually increased in the growing the halide perovskite single crystal, a temperature increase rate decreases for each temperature section as the temperature increases.

7. The method of claim 5 ,
wherein when the temperature of the perovskite precursor solution with increased solubility is gradually increased in the growing the halide perovskite single crystal, the temperature of the perovskite precursor solution increases at a temperature increase rate of 0.5° C./min to 0.7° C./min in a temperature range of 25° C. to 60° C., at a temperature increase rate of 0.3° C./min to 0.4° C./min in a temperature range of 60° C. to 100 20 C. and at a temperature increase rate of 0.2° C./min to 0.28° C. in a temperature range of 100° C. or more.

8. The method of claim 1 , further comprising:
placing the perovskite precursor solution with increased solubility on a substrate and putting a cover thereon before the growing the halide perovskite single crystal; and
removing the cover after the growing the halide perovskite single crystal.

Assignees

• Univ Ewha Ind Collaboration

Inventors

• Jo William
• Cho Yun Ae
• Jung Hye Ri

Classifications

• C30B29/54

  Organic compounds · CPC title

• C30B7/14

  the crystallising materials being formed by chemical reactions in the solution · CPC title

• C30B7/08

  by cooling of the solution · CPC title

• C30B7/04 Primary

  using aqueous solvents · CPC title

• C30B29/12 Primary

  Halides · CPC title