IP Library › Granted Patent US 10,557,214
Granted Patent B2
US 10,557,214 · App. 15/560,412 · Granted Feb 11, 2020

Methods of preparation of organometallic halide structures

Inventors: Osman Bakr (Thuwal, SA); Makhsud I. Saidaminov (Thuwal, SA); Ahmed L. Abdelhady (Thuwal, SA); Kristian Rahbek Knudsen (Thuwal, SA)
Assignee: KING ABDULLAH UNIVERSITY OF SCIENCE AND TECHNOLOGY
C30B29/12C01G1/06C30B7/14C30B31/12C30B35/007C01P2002/34
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Quick Facts
Patent No.
US 10,557,214
App. No.
15/560,412
Granted
Feb 11, 2020
Kind
B2
Abstract

Methods of growing organometallic halide structures such as AMX3 single crystal organometallic halide perovskites, using the inverse temperature solubility.

Claims (20)

1. A method of making an AMX3 structure, comprising:

dissolving MX2 and AX in a solvent to form dissolved AMX3 in a container, wherein A is an organic cation or Cesium (Cs), M is a divalent cation selected from the group consisting of: Pb, Sn, Cu, Ni, Co, Fe, Mn, Pd, Cd, Ge, Cs, or Eu, and X is selected from a halide; and

heating the mixture in the solvent to a temperature to form the AMX3 structure, wherein the temperature corresponds to the inverse temperature solubility for dissolved AMX3.

2. The method of claim 1 wherein A is selected from alkyl-ammonium, formamidinum (FA), 5-ammoniumvaleric acid, or Cs.

3. The method of claim 1 , wherein the AMX 3 structure is selected from the group consisting of: MAPbI 3 , MAPbBr 3 , FAPbBr 3 , FAPbI 3 , MAPbCl 3 , FAPbCl 3 , CsPbI 3 , CsPbCl 3 , CsPbBr 3 , FASnI 3 , FASnBr 3 , FASnCl 3 , MASnI 3 , MASnBr 3 , and MASnCl 3 , wherein MA is methylammonium and FA is formamidinum.

4. The method of claim 1 , wherein the solvent is selected from the group consisting of: N,N-dimethylformamide (DMF), dimethylsulfoxide (DMSO), gamma-butyrolactone (GBL), dichlorobenzene (DCB), toluene, and a combination thereof.

5. The method of claim 1 , wherein the AMX3 structure is a single crystal.

6. The method of claim 1 , wherein when the AMX3 structure is a MAPbBr3 perovskite structure and the solvent is N,N-dimethylformamide (DMF).

7. The method of claim 1 , wherein when the AMX3 structure is MAPbI3 perovskite structure and the solvent is γ-butyrolactone (GBL).

8. The method of claim 1 , further comprising: controlling the size of the AMX3 structure by adjusting one or more of the following: bottom surface dimensions of the container, the temperature, the concentration of MX2, the concentration of AX, and the concentration of the solvent.

9. The method of claim 1 , further comprising: forming the AMX3 structure as a part of a nanoparticle, wherein the nanoparticle is a quantum dot or a core-shell nanoparticle.

10. The method of claim 1 , further comprising: doping the AMX3 structure with a dopant.

11. The method of claim 10 , wherein the AMX 3 structure is selected from the group consisting of: doped MAPbI 3 , doped MAPbBr 3 , doped FAPbBr 3 , doped FAPbI 3 , doped MAPbCl 3 , doped FAPbCl 3 , doped CsPbI 3 , doped CsPbCl 3 , doped CsPbBr 3 , doped FASnI 3 , doped FASnBr 3 , doped FASnCl 3 , doped MASnI 3 , doped MASnBr 3 , and doped MASnCl 3 , wherein MA is methylammonium and FA is formamidinum.

12. The method of claim 1 , wherein the structure is selected from a nanowire or a wafer crystal.

13. The method of claim 1 , further comprising: after the AMX3 structure is formed, replenishing the dissolved AMX3; and growing the APbX3 structure further.

14. The method of claim 1 , wherein the container includes a template to form the AMX3 structure according to the template.

15. The method of claim 1 , wherein the AMX3 structure is formed in about 1 to about 6 hours.

16. The method of claim 1 , wherein one or more dimensions of the AMX3 structure is about 1 mm to about 10 mm and a thickness is about 0.05 mm to about 3 mm.

17. The method of claim 1 , wherein one or more of MX2 and AX do not exhibit inverse temperature solubility.

18. The method of claim 10 , wherein the dopant includes one or more of bismuth, gold, indium tin germanium, phosphine, copper, strontium, cadmium, calcium, and nickel ions.

Continuity (2)
Provisional Application 62137506 · Mar 24, 2015
Related Publication 20180066383A1 · Mar 8, 2018