METHOD OF FORMULATING PEROVSKITE SOLAR CELL MATERIALS

• US 20160035496A1
• Filed: 05/13/2015
• Published: 02/04/2016
• Est. Priority Date: 08/01/2014
• Status: Active Grant

• Current Assignee: Cubicpv Incorporated
• Original Assignee: Hunt Energy Enterprises LLC (Hunt Family)
• Inventors: Irwin, Michael D., Chute, Jerred A., Dhas, Vivek V.
• Granted Patent: US 9,305,715 B2
• Time in Patent Office: Days
• US Class Current: 1/1
• CPC Class Codes: B05D 1/38 with intermediate treatment intermediate treatment per se B05D3/00
• CPC Class Codes: B05D 3/107 Post-treatment of applied coatings
• CPC Class Codes: H01G 9/2045 comprising a semiconductor electrode comprising elements of the fourth group of the Periodic System (C, Si, Ge, Sn, Pb) with or without impurities, e.g. doping materials
• CPC Class Codes: H01L 2031/0344 Organic materials
• CPC Class Codes: H01L 31/0304 including, apart from doping materials or other impurities, only AIIIBV compounds
• CPC Class Codes: H03K 17/223 in field-effect transistor switches
• CPC Class Codes: H03K 5/19 Monitoring patterns of pulse trains indicating amplitude G01R19/00; indicating frequency G01R23/00; measuring characteristics of individual pulses G01R29/02
• CPC Class Codes: H03K 5/2472 using field effect transistors H03K5/2436 takes precedence
• CPC Class Codes: H10K 30/15 Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2 photo-electrochemical devices comprising a liquid electrolyte or a solid electrolyte H01G9/20
• CPC Class Codes: H10K 30/151 the wide bandgap semiconductor comprising titanium oxide, e.g. TiO2
• CPC Class Codes: H10K 30/451 comprising a metal-semiconductor-metal [m-s-m] structure
• CPC Class Codes: H10K 71/12 using liquid deposition, e.g. spin coating
• CPC Class Codes: H10K 71/40 Thermal treatment, e.g. annealing in the presence of a solvent vapour
• CPC Class Codes: H10K 85/30 Coordination compounds
• CPC Class Codes: H10K 85/50 Organic perovskites; Hybrid organic-inorganic perovskites [HOIP], e.g. CH3NH3PbI3
• CPC Class Codes: Y02E 10/542 Dye sensitized solar cells
• CPC Class Codes: Y02E 10/544 Solar cells from Group III-V materials
• CPC Class Codes: Y02E 10/549 Organic PV cells

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

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 solution;

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 selected from the group consisting of methylammonium iodide, formamidinium iodide, guanidinium iodide, 1,2,2-triaminovinylammonium iodide, and 5-aminovaleric acid hydroiodide.

3. 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.

4. 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.

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

C. to about 150°

C.

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

C.

7. The method of claim 1, wherein the lead halide precursor ink has a concentration of the lead halide between about 0.001M and about 10M.

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

9. The method of claim 1, wherein annealing the thin film occurs for up to 24 hours at a temperature between about 20°

C. to about 300°

C.

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

C.

11. 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.

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

13. The method of claim 11, wherein the salt is dissolved in the second solvent in a concentration of between about 0.001M and about 10M.

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

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

31. 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.

2. (canceled)

16. 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 with a second solvent and a salt selected from the group consisting of methylammonium iodide, formamidinium iodide, guanidinium iodide, 1,2,2-triaminovinylammonium iodide, and 5-aminovaleric acid hydroiodide to form the perovskite material.

18. The perovskite material of claim 16, 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.

19. The perovskite material of claim 16, 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.

20. The perovskite material of claim 16, wherein contacting the lead halide with the solvent to dissolve the lead halide occurs between about 20°

C. to about 150°

C.

21. The perovskite material of claim 16, wherein contacting the lead halide with the solvent to dissolve the lead halide occurs at about 85°

C.

22. The perovskite material of claim 16, wherein the lead halide precursor ink has a concentration of the lead halide between about 0.001M and about 10M.

23. The perovskite material of claim 16, wherein depositing the lead halide precursor ink onto the substrate occurs by drop casting, spin casting, slot-die printing, screen printing, or ink-jet printing.

24. The perovskite material of claim 16, wherein annealing the thin film occurs for up to 24 hours at a temperature between about 20°

C. to about 300°

C.

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

C.

26. The perovskite material of claim 16, wherein the second solvent selected from the group consisting of dimethylformamide, isopropanol, methanol, ethanol, butanol, chloroform chlorobenzene, dimethylsulfoxide, water, and combinations thereof.

27. The perovskite material of claim 16, wherein the salt comprises formamidinium iodide.

28. The perovskite material of claim 27, wherein the salt is dissolved in the second solvent in a concentration of between about 0.001M and about 10M.

29. The perovskite material of claim 16, wherein the salt comprises methylammonium iodide.

30. The perovskite material of claim 16, wherein rinsing the thin film comprises at least partial submersion in the second solvent.

32. The perovskite material of claim 16, 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. (canceled)