IP Library Granted Patent US 11,800,726
Granted Patent B1
US 11,800,726 · App. 17/970,465 · Granted Oct 24, 2023

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 11,800,726
App. No.
17/970,465
Granted
Oct 24, 2023
Kind
B1
Abstract

A method for preparing photoactive perovskite materials. The method comprises the steps of preparing a bismuth halide precursor ink. Preparing a bismuth halide precursor ink comprises the steps of introducing a bismuth halide into a vessel; introducing a first solvent to the vessel; and contacting the bismuth halide with the first solvent to dissolve the bismuth halide to form the bismuth halide precursor ink; depositing the bismuth halide precursor ink onto a substrate; drying the bismuth 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 bismuth halide precursor ink, wherein preparing a bismuth halide precursor ink comprises the steps of:

introducing a bismuth halide into a vessel;

introducing a first solvent to the vessel; and

contacting the bismuth halide with the first solvent to dissolve the bismuth halide to form the bismuth halide precursor ink;

depositing the bismuth halide precursor ink onto a substrate;

drying the bismuth 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.

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 bismuth halide with the first solvent to dissolve the bismuth halide occurs between about 20° C. to about 150° C.

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

6. The method of claim 1 , wherein depositing the bismuth halide precursor ink onto the substrate occurs by drop casting, spin casting, slot-die printing, screen printing, or ink-jet printing.

7. 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.

8. 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.

9. The method of claim 1 , wherein the first salt is selected from the group consisting of methylammonium iodide, formamidinium iodide, guanidinium iodide, 1,2,2-triaminovinylammonium iodide, and 5-aminovaleric acid hydroiodide.

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

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

12. The method of claim 1 , wherein rinsing the thin film comprises at least partial submersion in the second solvent.

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

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

introducing a bismuth halide into a vessel;

introducing a first solvent to the vessel; and

contacting the bismuth halide with the first solvent to dissolve the bismuth halide to form the bismuth halide precursor ink;

depositing the bismuth halide precursor ink onto a substrate;

drying the bismuth 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.

14. The perovskite material of claim 13 , 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.

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

16. The perovskite material of claim 13 , 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.

17. The perovskite material of claim 13 , wherein the second solvent selected from the group consisting of dimethylformamide, isopropanol, methanol, ethanol, butanol, chloroform, chlorobenzene, dimethylsulfoxide, water, and combinations thereof.

18. The perovskite material of claim 13 , wherein the first salt is selected from the group consisting of methylammonium iodide, formamidinium iodide, guanidinium iodide, 1,2,2-triaminovinylammonium iodide, and 5-aminovaleric acid hydroiodide.

19. The perovskite material of claim 18 , wherein the first salt comprises formamidinium iodide and the second salt comprises guanidium iodide.

20. The perovskite material of claim 18 , wherein the first salt comprises methylammonium iodide and the second salt comprises guanidium iodide.

Assignments (5)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 27, 2022
From: IRWIN, MICHAEL D.; CHUTE, JERRED A.; DHAS, VIVEK V.
To: HUNT ENERGY ENTERPRISES, L.L.C.
Reel/Frame 061560/0501 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 27, 2022
From: HUNT CONSOLIDATED, INC.; HUNT ENERGY ENTERPRISES, L.L.C.
To: HEE SOLAR, L.L.C.
Reel/Frame 061560/0655 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 27, 2022
From: CUBIC PEROVSKITE LLC
To: CUBICPV INC.
Reel/Frame 061788/0657 →
CHANGE OF NAME Recorded Oct 27, 2022
From: HEE SOLAR, L.L.C.
To: HUNT PEROVSKITE TECHNOLOGIES, L.L.C.
Reel/Frame 061790/0112 →
CHANGE OF NAME Recorded Oct 27, 2022
From: HUNT PEROVSKITE TECHNOLOGIES, L.L.C.
To: CUBIC PEROVSKITE LLC
Reel/Frame 061790/0202 →
Continuity (5)
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