IP Library Granted Patent US 12,302,681
Granted Patent B2
US 12,302,681 · App. 18/469,253 · Granted May 13, 2025

Method of formulating perovskite solar cell materials

Inventors: Michael D. Irwin (Heath, TX); Jerred A. Chute (Dallas, TX); Vivek V. Dhas (Dallas, TX)
Assignee: CubicPV Inc.
H10K30/451B05D1/38B05D3/107H01G9/2045H01L31/0304H03K5/19H03K5/2472H03K17/223H10K30/15H10K30/151H10K71/12H10K71/40H10K85/30H01L2031/0344Y02E10/542Y02E10/549
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Quick Facts
Patent No.
US 12,302,681
App. No.
18/469,253
Granted
May 13, 2025
Kind
B2
Abstract

A method for preparing photoactive perovskite materials. The method comprises the steps of preparing a lead and tin halide precursor ink. Preparing a lead and tin halide precursor ink comprises the steps of introducing a lead halide and a tin halide into a vessel; introducing a first solvent to the vessel; and contacting the lead halide and the halide with the first solvent to dissolve the lead halide and the tin halide to form the lead and tin halide precursor ink; depositing the lead and tin halide precursor ink onto a substrate; drying the lead and tin halide precursor ink to form a thin film; annealing the thin film; and rinsing the thin film with a solvent comprising: a second solvent; a first salt selected from the group consisting of methylammonium halide, formamidinimum halide, guanidinium halide, 1,2,2-triaminovinylammonium halide, and 5-aminovaleric acid hydrohalide; and a second salt selected from the group consisting of methylammonium halide, formamidinimum halide, guanidinium halide, 1,2,2-triaminovinylammonium halide, and 5-aminovaleric acid hydrohalide.

Claims (42)

1. A method comprising the steps of:

preparing a precursor ink, wherein preparing the precursor ink comprises the steps of:

introducing lead halide and tin halide into a vessel, wherein the lead halide comprises a mixture of lead (II) chloride and lead (II) iodide;

introducing a first solvent to the vessel; and

contacting the lead halide and the tin halide with the first solvent to dissolve the lead halide and the tin halide to form the precursor ink;

depositing the precursor ink onto a substrate;

drying the precursor ink to form a thin film;

annealing the thin film; and

rinsing the thin film with a solution comprising:

a second solvent;

a first salt selected from the group consisting of methylammonium iodide, formamidinimum halide, guanidinium halide, 1,2,2-triaminovinylammonium halide, and 5-aminovaleric acid hydrohalide.

2. 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.

3. The method of claim 1 , wherein annealing the thin film occurs for about ten minutes at a temperature of about 50° C.

4. The method of claim 1 , wherein contacting the lead halide and the tin halide with the first solvent to dissolve the lead halide and the tin halide occurs between about 20° C. to about 150° C.

5. The method of claim 1 , wherein contacting the lead halide and the tin halide with the first solvent to dissolve the lead halide and the tin halide occurs at about 85° C.

6. The method of claim 1 , wherein the first solvent is selected from the group consisting of dry dimethylformamide, dimethylsulfoxide (DMSO), methanol, ethanol, propanol, butanol, tetrahydrofuran, formamide, pyridine, pyrrolidine, chlorobenzene, dichlorobenzene, dichloromethane, chloroform, and combinations thereof.

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

8. The method of claim 1 , wherein the solution further comprises:

a second salt selected from the group consisting of methylammonium halide, formamidinium halide, guanidinium halide, 1,2,2-triaminovinylammonium halide, and 5-aminovaleric acid hydrohalide.

9. The method of claim 8 , wherein the first salt comprises formamidinium iodide and the second salt comprises guanidium iodide, or wherein the first salt comprises methylammonium iodide and the second salt comprises guanidium iodide.

10. The method of claim 1 , wherein the mixture of lead (II) chloride and lead (II) iodide is mixed in a ratio of 10 mol of lead (II) chloride to 90 mol of lead (II) iodide.

11. A perovskite material prepared by a process comprising the steps of:

preparing a precursor ink, wherein preparing the precursor ink comprises the steps of:

introducing a lead halide and tin halide into a vessel, wherein the lead halide comprises a mixture of lead (II) chloride and lead (II) iodide;

introducing a first solvent to the vessel; and

contacting the lead halide and the tin halide with the first solvent to dissolve the lead halide and the tin halide to form the precursor ink;

depositing the precursor ink onto a substrate;

drying the precursor ink to form a thin film;

annealing the thin film; and

rinsing the thin film, to form the perovskite material, with a solution comprising:

a second solvent; and

a first salt selected from the group consisting of methylammonium iodide, formamidinimum halide, guanidinium halide, 1,2,2-triaminovinylammonium halide, and 5-aminovaleric acid hydrohalide.

12. The perovskite material of claim 11 , 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.

13. The perovskite material of claim 11 , wherein contacting the lead halide and tin halide with the first solvent to dissolve the lead halide and the tin halide occurs between about 20° C. to about 150° C.

14. The perovskite material of claim 11 , wherein the first solvent is selected from the group consisting of dry dimethylformamide, dimethylsulfoxide (DMSO), methanol, ethanol, propanol, butanol, tetrahydrofuran, formamide, pyridine, pyrrolidine, chlorobenzene, dichlorobenzene, dichloromethane, chloroform, and combinations thereof.

15. The perovskite material of claim 11 , wherein the second solvent selected from the group consisting of dimethylformamide, isopropanol, methanol, ethanol, butanol, chloroform, chlorobenzene, dimethylsulfoxide, water, and combinations thereof.

16. The perovskite material of claim 11 , wherein the solution further comprises:

a second salt selected from the group consisting of methylammonium halide, formamidinium halide, guanidinium halide, 1,2,2-triaminovinylammonium halide, and 5-aminovaleric acid hydrohalide.

17. The perovskite material of claim 16 , wherein the first salt comprises formamidinium iodide and the second salt comprises guanidium iodide, or wherein the first salt comprises methylammonium iodide and the second salt comprises guanidium iodide.

18. The perovskite material of claim 11 , wherein contacting the lead halide and the tin halide with the first solvent to dissolve the lead halide and the tin halide occurs at about 85° C.

19. The perovskite material of claim 11 , wherein annealing the thin film occurs for ten minutes at a temperature of about 50° C.

20. The perovskite material of claim 11 , wherein the mixture of lead (II) chloride and lead (II) iodide is mixed in a ratio of 10 mol of lead (II) chloride to 90 mol of lead (II) iodide.

Assignments (5)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 18, 2023
From: IRWIN, MICHAEL D.; CHUTE, JERRED A.; DHAS, VIVEK V.
To: HUNT ENERGY ENTERPRISES, L.L.C.
Reel/Frame 064939/0551 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 18, 2023
From: HUNT CONSOLIDATED, INC.; HUNT ENERGY ENTERPRISES, L.L.C.
To: HEE SOLAR, L.L.C.
Reel/Frame 064939/0846 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 18, 2023
From: CUBIC PEROVSKITE LLC
To: CUBICPV INC.
Reel/Frame 064942/0898 →
CHANGE OF NAME Recorded Sep 18, 2023
From: HEE SOLAR, L.L.C.
To: HUNT PEROVSKITE TECHNOLOGIES, L.L.C.
Reel/Frame 064943/0635 →
CHANGE OF NAME Recorded Sep 18, 2023
From: HUNT PEROVSKITE TECHNOLOGIES, L.L.C.
To: CUBIC PEROVSKITE LLC
Reel/Frame 064943/0638 →
Continuity (7)
Continuation 17970465 · Oct 20, 2022
Continuation 16939907 · Jul 27, 2020
Continuation 15996944 · Jun 4, 2018
Continuation 15068187 · Mar 11, 2016
Continuation 14711330 · May 13, 2015
Provisional Application 62032137 · Aug 1, 2014
Related Publication 20240008295A1 · Jan 4, 2024
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