IP Library Granted Patent US 10,741,779
Granted Patent B2
US 10,741,779 · App. 15/996,944 · Granted Aug 11, 2020

Method of formulating perovskite solar cell materials

Inventors: Michael D. Irwin (Dallas, TX); Jerred A. Chute (Dallas, TX); Vivek V. Dhas (Dallas, TX)
Assignee: Hunt Perovskite Technologies, L.L.C.
H01L51/4206B05D1/38B05D3/107H01G9/2045H01L31/0304H01L51/0003H01L51/0026H01L51/0077H01L51/422Y02E10/542Y02E10/549
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Quick Facts
Patent No.
US 10,741,779
App. No.
15/996,944
Granted
Aug 11, 2020
Kind
B2
Abstract

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

introducing a lead 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 with the first solvent to dissolve the lead halide to form the lead halide precursor ink;

depositing the lead halide precursor ink onto a substrate;

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

2. 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.

3. 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.

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

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

6. 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.

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

8. 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.

9. The method of claim 1 , wherein the first salt comprises formamidinium iodide and the second salt comprises guanidium iodide.

10. The method of claim 1 , 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 lead halide precursor ink, wherein preparing a lead halide precursor ink comprises the steps of:

introducing a lead 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 with the first solvent to dissolve the lead halide;

depositing the lead halide precursor ink onto a substrate;

drying the lead 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;

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; and

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.

12. 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.

13. 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.

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

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

16. 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.

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

18. 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.

19. The perovskite material of claim 11 , wherein the first salt comprises formamidinium iodide and the second salt comprises guanidium iodide.

20. The perovskite material of claim 11 , 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 →
CHANGE OF NAME Recorded Apr 13, 2020
From: HEE SOLAR, L.L.C.
To: HUNT PEROVSKITE TECHNOLOGIES, L.L.C.
Reel/Frame 052385/0490 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 7, 2018
From: IRWIN, MICHAEL D.; CHUTE, JERRED A.; DHAS, VIVEK V.
To: HUNT ENERGY ENTERPRISES, L.L.C.
Reel/Frame 046012/0149 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 4, 2018
From: HUNT CONSOLIDATED, INC.; HUNT ENERGY ENTERPRISES, L.L.C.
To: HEE SOLAR, L.LC.
Reel/Frame 045978/0818 →
Continuity (4)
Continuation 15068187 · Mar 11, 2016
Continuation 14711330 · May 13, 2015
Provisional Application 62032137 · Aug 1, 2014
Related Publication 20180287082A1 · Oct 4, 2018
Cited By (6)
US 12,231,080 US 12,302,681 US 12,355,395 US 12,408,469 US 12,414,402 US 12,525,916