IP Library Granted Patent US 11,508,924
Granted Patent B2
US 11,508,924 · App. 16/939,907 · Granted Nov 22, 2022

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.
H01L51/4206B05D1/38B05D3/107H01G9/2045H01L31/0304H01L51/0003H01L51/0026H01L51/0077H01L51/422H01L51/4226H03K5/19H03K5/2472H03K17/223H01L2031/0344Y02E10/542Y02E10/549
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Quick Facts
Patent No.
US 11,508,924
App. No.
16/939,907
Granted
Nov 22, 2022
Kind
B2
Abstract

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

Claims (42)

1. A method comprising the steps of:

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

introducing a germanium halide into a vessel;

introducing a first solvent to the vessel; and

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

depositing the germanium halide precursor ink onto a substrate;

drying the germanium halide precursor ink to form a thin film;

annealing the thin film; and

rinsing the thin film with a solution comprising:

a second solvent; and

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

2. 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.

3. The method of claim 1 , wherein contacting the germanium halide with the first solvent to dissolve the germanium halide occurs between about 20° C. to about 150° C.

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

5. 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.

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

7. The method of claim 1 , wherein the second solvent is 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 rinsing the thin film with a 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.

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

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

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

introducing a germanium halide into a vessel;

introducing a first solvent to the vessel; and

contacting the germanium halide with the first solvent to dissolve the germanium halide;

depositing the germanium halide precursor ink onto a substrate;

drying the germanium halide 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, formamidinium halide, guanidinium halide, 1,2,2-triaminovinylammonium halide, and 5-aminovaleric acid hydrohalide.

12. 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.

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

14. The perovskite material of claim 11 , wherein contacting the germanium halide with the first solvent to dissolve the germanium halide occurs at about 85° C.

15. 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.

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

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

18. 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.

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 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 Jul 27, 2021
From: HUNT CONSOLIDATED, INC.; HUNT ENERGY ENTERPRISES, L.L.C.
To: HEE SOLAR, L.L.C.
Reel/Frame 056994/0957 →
CHANGE OF NAME Recorded Jul 27, 2021
From: HEE SOLAR, L.L.C.
To: HUNT PEROVSKITE TECHNOLOGIES, L.L.C.
Reel/Frame 056998/0548 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 27, 2020
From: IRWIN, MICHAEL D.; CHUTE, JERRED A.; DHAS, VIVEK V.
To: HUNT ENERGY ENTERPRISES, L.L.C.
Reel/Frame 053320/0912 →
Continuity (5)
Continuation 15996944 · Jun 4, 2018
Continuation 15068178 · Mar 11, 2016
Continuation 14711330 · May 13, 2015
Provisional Application 62032137 · Aug 1, 2014
Related Publication 20200358436A1 · Nov 12, 2020
Cited By (5)
US 12,231,080 US 12,355,395 US 12,408,469 US 12,414,402 US 12,525,916