IP Library Granted Patent US 11,300,870
Granted Patent B2
US 11,300,870 · App. 16/859,545 · Granted Apr 12, 2022

Hybrid perovskite material processing

Inventors: Michael D. Irwin (Heath, TX); Kamil Mielczarek (Rowlett, TX); Vivek V. Dhas (Dallas, TX)
Assignee: CUBICPV INC.
G03C8/365B05D1/38B05D3/107C01D3/12C01G21/16C07C19/00C09D11/52H01G9/2059H01L51/0003H01L51/4206H01L51/4226C07C233/03C07C317/04G03C2001/03558H01G9/2009H01G9/2031H01L51/0007H01L51/0026H01L2251/306
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Quick Facts
Patent No.
US 11,300,870
App. No.
16/859,545
Granted
Apr 12, 2022
Kind
B2
Abstract

A method for preparing photoactive perovskite materials. The method comprises the steps of: introducing a lead halide and a first solvent to a first vessel and contacting the lead halide with the first solvent to dissolve the lead halide to form a lead halide solution, introducing a Group 1 metal halide a second solvent into a second vessel and contacting the Group 1 metal halide with the second solvent to dissolve the Group 1 metal halide to form a Group 1 metal halide solution, and contacting the lead halide solution with the Group 1 metal halide solution to form a thin-film precursor ink. The method further comprises depositing the thin-film precursor ink onto a substrate, drying the thin-film precursor ink to form a thin film, annealing the thin film; and rinsing the thin film with a salt solution.

Claims (30)

1. A method comprising the steps of:

preparing a thin-film precursor ink, wherein preparing the thin-film precursor ink comprises the steps of:

contacting a lead halide with a first solvent to dissolve the lead halide to form a lead halide solution;

contacting a Group 1 metal halide with a second solvent to dissolve the group 1 metal halide to form a Group 1 metal halide solution;

contacting the lead halide solution with the Group 1 metal halide solution to form the thin-film precursor ink;

depositing the thin-film precursor ink onto a substrate; drying the thin-film precursor ink to form a thin film; annealing the thin film; and

rinsing the thin film with a salt solution comprising a third solvent and a salt selected from the group consisting of methylammonium halide, formamidinium halide, guanidinium halide, ethene tetramine halide, imidazolium halide, 1,2,2-triaminovinylammonium halide, and 5-aminovaleric acid hydrohalide,

wherein the thin-film precursor ink has a molar concentration of the Group 1 metal halide that is between 1% and 25% of the molar concentration of the lead halide.

2. The method of claim 1 , wherein the lead halide comprises lead (II) iodide.

3. The method of claim 1 , wherein the Group 1 metal halide comprises cesium iodide.

4. The method of claim 1 , wherein the Group 1 metal halide comprises rubidium iodide.

5. The method of claim 1 , wherein the Group 1 metal halide comprises sodium iodide.

6. The method of claim 1 , wherein the Group 1 metal halide comprises potassium iodide.

7. The method of claim 1 , wherein the first solvent and the second solvent are selected from the group consisting of dry N-cyclohexyl-2-pyrrolidone, alkyl-2-pyrrolidone, dimethylformamide (DMF), dialkylformamide, dimethylsulfoxide (DMSO), methanol, ethanol, propanol, butanol, tetrahydrofuran, formamide, tert-butylpyridine, pyridine, alkylpyridine, pyrrolidine, chlorobenzene, dichlorobenzene, dichloromethane, chloroform, and combinations thereof.

8. The method of claim 1 , wherein the first solvent comprises dry dimethylformamide (DMF).

9. The method of claim 1 , wherein the second solvent comprises dimethylsulfoxide (DMSO).

10. The method of claim 1 , wherein the third solvent is selected from the group consisting of dimethylformamide, isopropanol, methanol, ethanol, butanol, chloroform, chlorobenzene, dimethylsulfoxide, water, and combinations thereof.

11. The method of claim 1 , wherein annealing the thin film occurs for between about 5 to about 30 minutes at a temperature between about 40 C to about 60 C.

12. The method of claim 1 , wherein the salt comprises formamidinium iodide.

13. The method of claim 1 , wherein the salt comprises methylammonium iodide.

14. The method of claim 1 , wherein rinsing the thin film comprises at least partial submersion in the salt solution.

15. A method comprising the steps of:

preparing a thin-film precursor ink, wherein preparing the thin-film precursor ink comprises the steps of:

contacting a lead halide and a Group 1 metal halide with a first solvent to form a thin-film precursor solution;

depositing the thin-film precursor ink onto a substrate; drying the thin-film precursor ink to form a thin film; annealing the thin film; and

rinsing the thin film with a salt solution comprising a second solvent and a salt selected from the group consisting of methylammonium halide, formamidinium halide, guanidinium halide, ethene tetramine halide, imidazolium halide, 1,2,2-triaminovinylammonium halide, and 5-aminovaleric acid hydrohalide,

wherein the thin-film precursor ink has a molar concentration of the Group 1 metal halide that is between 1% and 25% of the molar concentration of the lead halide.

16. The method of claim 15 , further comprising contacting a third solvent with the first solvent or the thin-film precursor solution.

17. The method of claim 15 , wherein the lead halide comprises lead (II) iodide and the Group 1 metal halide comprises cesium iodide.

18. The method of claim 15 , wherein the lead halide comprises lead (II) iodide and the Group 1 metal halide comprises rubidium iodide.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 15, 2021
From: CUBIC PEROVSKITE LLC
To: CUBICPV INC.
Reel/Frame 058517/0919 →
CHANGE OF NAME Recorded Aug 1, 2021
From: HUNT PEROVSKITE TECHNOLOGIES, L.L.C.
To: CUBIC PEROVSKITE LLC
Reel/Frame 057047/0232 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 27, 2020
From: IRWIN, MICHAEL D.; MIELCZAREK, KAMIL; DHAS, VIVEK V.
To: HUNT PEROVSKITE TECHNOLOGIES, L.L.C.
Reel/Frame 052504/0675 →
Continuity (3)
Continuation 15882307 · Jan 29, 2018
Division 15489431 · Apr 17, 2017
Related Publication 20200257190A1 · Aug 13, 2020
Cited By (5)
US 12,231,080 US 12,355,395 US 12,408,469 US 12,414,402 US 12,525,916