IP Library Granted Patent US 10,910,569
Granted Patent B2
US 10,910,569 · App. 15/574,611 · Granted Feb 2, 2021

Organo-metal halide perovskites films and methods of making the same

Inventors: Kai Zhu (Littleton, CO); Mengjin Yang (Dallas, TX); Yuanyuan Zhou (Providence, RI); Nitin Prabhakar Padture (Providence, RI)
Assignee: Alliance for Sustainable Energy, LLC
H01L51/0077H01L51/0007H01L51/0026H01L51/4226Y02E10/549Y02P70/50
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Quick Facts
Patent No.
US 10,910,569
App. No.
15/574,611
Granted
Feb 2, 2021
Kind
B2
Abstract

An aspect of the present disclosure is a method that includes applying a solution that includes a first solvent, a halogen-containing precursor, and a metal halide to a substrate to form a coating of the solution on the substrate, contacting the coating with a second solvent to form a first plurality of organo-metal halide perovskite crystals on the substrate, and thermally treating the first plurality of organo-metal halide perovskite crystals, such that at least a portion of the first plurality of organo-metal halide perovskite crystals is converted to a second plurality of organo-metal halide perovskite crystals on the substrate. The halogen-containing precursor and the metal halide are present in the solution at a molar ratio of the halogen-containing precursor to the metal halide between about 1.01:1.0 and about 2.0:1.0, and a property of the second plurality of organo-metal halide perovskite crystals is improved relative to a property of the first plurality of organo-metal halide perovskite crystals.

Claims (31)

1. A method comprising:

applying a solution comprising a first solvent, a halogen-containing precursor, and a metal halide to a substrate to form a coating of the solution on the substrate;

contacting the coating with a second solvent to form a first plurality of organo- metal halide perovskite crystals on the substrate; and

thermally treating the first plurality of organo-metal halide perovskite crystals, such that at least a portion of the first plurality of organo-metal halide perovskite crystals is converted to a second plurality of organo-metal halide perovskite crystals on the substrate, wherein:

the halogen-containing precursor consists of a cation and a halide,

the metal halide consists of a metal and the halide,

the halogen-containing precursor is provided in the solution in stoichiometric excess,

the first plurality of organo-metal halide perovskite crystals have an average crystal size between 30 nm and 200 nm,

the second plurality of organo-metal halide perovskite crystals have an average crystal size between 1 μm and 2 μm, and

the second plurality of organo-metal halide perovskite crystals consists essentially of the cation, the metal, and the halide.

2. The method of claim 1 , wherein the first plurality of organo-metal halide perovskite crystals form as a film on the substrate.

3. The method of claim 1 , wherein the first solvent has a boiling point temperature greater than about 150° C.

4. The method of claim 1 , wherein the first solvent comprises at least one of 1-methyl-2-pyrrolidinone, γ-butyrolactone, or dimethyl sulfoxide.

5. The method of claim 1 , wherein the halogen-containing precursor comprises at least one of a methylammonium halide, a formamidinium halide, or a cesium iodide.

6. The method of claim 5 , wherein the methylammonium halide consists of methylammonium iodide (MAI).

7. The method of claim 6 , wherein:

the stoichiometric excess corresponds to a molar ratio of the MAI to the metal halide between greater than about 1.01:1.0 and equal to 2.0:1.0.

8. The method of claim 7 , wherein the molar ratio is between 1.2:1.0 and 2.0:1.0.

9. The method of claim 1 , wherein the metal halide comprises at least one of PbI 2 , SnI 2 , BiI 3 , or InI 3 .

10. The method of claim 1 , wherein the second solvent has a boiling point temperature below about 150° C.

11. The method of claim 1 , wherein the second solvent comprises at least one of diethyl ether, toluene, chlorobenzene, or hexane.

12. The method of claim 1 , wherein the applying comprises at least one of spin-coating, curtain-coating, dip-coating, or spraying the solution onto a surface of the substrate.

13. The method of claim 1 , wherein the applying is performed at a temperature between about 0° C. and about 35° C.

14. The method of claim 1 , wherein the applying is performed over a period of time between about 1 second and about 1 hour.

15. The method of claim 1 , wherein the contacting comprises immersing the coating and the substrate in the second solvent.

16. The method of claim 15 , wherein the immersing is performed for a period of time between about 30 seconds and about 1 hour.

17. The method of claim 1 , wherein the thermally treating comprises heating the first plurality of organo-metal halide perovskite crystals to a temperature between about 35° C. and about 200° C.

18. The method of claim 17 , wherein the thermally treating is performed for a period of time between about 5 seconds and about 1 hour.

19. The method of claim 1 , wherein the thermally treating is performed in an oxygen-containing environment.

20. The method of claim 1 , wherein the second plurality of organo-metal halide perovskite crystals comprises an alkylammonium metal halide crystal.

21. The method of claim 20 , wherein the alkylammonium metal halide crystal comprises a methylammonium lead iodide crystal.

Assignments (3)
CHANGE OF NAME Recorded Dec 16, 2025
From: ALLIANCE FOR SUSTAINABLE ENERGY, LLC
To: ALLIANCE FOR ENERGY INNOVATION, LLC
Reel/Frame 073993/0276 →
CONFIRMATORY LICENSE Recorded Jun 12, 2018
From: NATIONAL RENEWABLE ENERGY LABORATORY
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 046339/0708 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 16, 2017
From: ZHU, KAI; YANG, MENGJIN
To: ALLIANCE FOR SUSTAINABLE ENERGY, LLC
Reel/Frame 044151/0851 →
Continuity (2)
Provisional Application 62163451 · May 19, 2015
Related Publication 20180151813A1 · May 31, 2018