Method for preparing perovskite crystal

Patent metadata

Field	Value
Publication number	US-10883193-B2
Application number	US-201815866629-A
Country	US
Kind code	B2
Filing date	Jan 10, 2018
Priority date	May 19, 2017
Publication date	Jan 5, 2021
Grant date	Jan 5, 2021

Abstract

The instant disclosure provides a method for preparing a perovskite crystal, including a mixing step, a crystallization step, a diluting step and a recrystallization step. The mixing step includes adding a first precursor and a second precursor into a solvent for forming a supersaturated solution. The crystallization step includes stirring the supersaturated solution for initiating a reaction between the first and second precursors in the supersaturated solution to form a perovskite powder in a solution. The diluting step includes adding the solvent to the solution and stirring the solution for dissociating the perovskite powder in the solution to form a clear solution. The recrystallization step includes adding a crystal seed into the clear solution for initiating a crystallization process on the crystal seed and forming the perovskite crystal.

First claim

What is claimed is:

1. A method for preparing a perovskite crystal, including:
a crystallization step including stirring a supersaturated solution to form a resulting solution containing a perovskite powder, wherein the supersaturated solution is formed by adding a first precursor and a second precursor into a solvent, and the perovskite powder is formed from a reaction between the first precursor and the second precursor;
a diluting step including adding the solvent to the resulting solution and stirring the resulting solution for dissolving the perovskite powder in the resulting solution to directly form a clear solution, the clear solution is an unsaturated solution; and
a recrystallization step including adding a crystal seed into the clear solution for initiating a crystallization process on the crystal seed and forming the perovskite crystal.

2. The method according to claim 1 , wherein the first precursor includes a halide having a general formula AX, and the second precursor includes a metal halide having a general formula MX 2 , A being selected from the group consisting of CH(NH 2 ) 2 , CH 3 CH 2 NH 3 , CH 3 NH 3 and Cs, M being selected from the group consisting of Pb and Sn, and X being selected from the group consisting of Cl, Br and I.

3. The method according to claim 2 , wherein the first precursor includes at least two halides having a general formula AX, and A includes at least two selected from the group consisting of CH(NH 2 ) 2 , CH 3 CH 2 NH 3 , CH 3 NH 3 and Cs.

4. The method according to claim 1 , wherein the solvent is γ-butyrolactone, dimethylformamide or a mixture thereof.

5. The method according to claim 1 , wherein the crystallization step are carried out with a temperature ranging from 57 to 204° C.

6. The method according to claim 1 , wherein the diluting step is carried out with a temperature ranging from 100 to 204° C.

7. The method according to claim 1 , wherein the recrystallization step is carried out with a temperature ranging from 80 to 204° C.

8. The method according to claim 1 , wherein the first precursor is CH 3 NH 3 I and the second precursor is PbI 2 , wherein a molar ratio between the first precursor and the second precursor ranges from 1:1 to 3:1.

9. The method according to claim 8 , wherein the solvent is γ-butyrolactone, and the recrystallization step is carried out with a temperature ranging from 80 to 204° C.

10. A method for preparing a perovskite crystal, including:
stirring a supersaturated solution to form a resulting solution containing to form a perovskite powder; wherein the supersaturated solution is formed by adding a first precursor and a second precursor into a solvent;
adding more of the solvent to the resulting solution for dissolving the perovskite powder and directly forming a clear solution, the clear solution is an unsaturated solution; and
adding a crystal seed into the clear solution for forming the perovskite crystal.

11. The method according to claim 10 , wherein the first precursor includes a halide, and the second precursor includes a metal halide.

12. The method according to claim 10 , wherein the solvent includes γ-butyrolactone, dimethylformamide or a mixture thereof.

13. The method according to claim 10 , wherein the supersaturated solution is stirred at a temperature ranging from 57 to 204° C.

14. The method according to claim 10 , wherein the solvent is added to the solution at a temperature ranging from 100 to 204° C. for forming the clear solution.

15. A method for preparing a perovskite crystal, including:
stirring a supersaturated solution to form a resulting solution containing a perovskite powder; wherein the supersaturated solution is formed by adding enough amount of a first precursor and a second precursor into a solvent;
adding more of the solvent to the resulting solution for dissolving the perovskite powder until the resulting solution directly becomes clear and unsaturated; and
adding a crystal seed into the resulting solution which is clear for forming the perovskite crystal.

16. The method according to claim 15 , wherein the first precursor includes a halide, and the second precursor includes a metal halide, and the solvent includes γ-butyrolactone, dimethylformamide or a mixture thereof.

17. The method according to claim 16 , wherein the first precursor having a general formula AX, and the second precursor having a general formula MX 2 , A being selected from a group consisting of CH(NH 2 ) 2 , CH 3 CH 2 NH 3 , CH 3 NH 3 and Cs, M being selected from a group consisting of Pb and Sn, and X being selected from a group consisting of Cl, Br and I.

18. The method according to claim 15 , wherein the first precursor is CH 3 NH 3 I and the second precursor is PbI 2 , and a molar ratio between the first precursor and the second precursor ranges from 1:1 to 3:1.

Assignees

• Univ Nat Tsing Hua

Inventors

• Wei Tzu-Chien
• Teng Ko-Chi

Classifications

• B01D9/0036 Primary

  Crystallisation on to a bed of product crystals; Seeding · CPC title

• C30B29/12

  Halides · CPC title

• C30B33/02

  Heat treatment (C30B33/04, C30B33/06 take precedence) · CPC title

• C30B7/14

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

• C30B29/32 Primary

  Titanates; Germanates; Molybdates; Tungstates · CPC title