# US 11,306,245 B2 · Method for preparing CsPbX3 perovskite quantum dot film by one-step crystallization

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- Number: US 11,306,245 B2
- Document ID: US11306245B2
- Status: Granted
- Kind: B2
- Application number: 16/747,733
- Filed: 2020-01-21
- Published: 2021-04-15
- Granted: 2022-04-19
- Earliest claimed: 2019-10-09
- Assignees: North China Electric Power University
- Applicants: North China Electric Power University
- Inventors: Yong Ding; Cheng Liu; Songyuan Dai; Yi Yang; Xuepeng Liu; Molang Cai
- Web page: https://patentgrep.com/patent/US11306245B2

## CPC

- C09K 11/665: {with alkali or alkaline earth metals}
- B05D 1/005: {Spin coating}
- C01G 21/006: {Compounds containing lead, with or without oxygen or hydrogen, and containing two or more other elements}
- C01G 21/16: Halides
- C23C 18/02: by thermal decomposition
- C23C 18/1204: {inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds}
- B82Y 20/00: Nanooptics, e.g. quantum optics or photonic crystals
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- B82Y 40/00: Manufacture or treatment of nanostructures
- C01P 2002/34: perovskite-type (ABO3)
- C01P 2002/82: by IR- or Raman-data
- C01P 2002/84: by UV- or VIS- data
- C01P 2004/03: obtained by SEM
- C01P 2004/04: obtained by TEM, STEM, STM or AFM
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C09K: MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- B05D: PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL (conveying articles or workpieces through baths of liquid B65G, e.g. B65G49/02)
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04)
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

The present disclosure provides a method for preparing a perovskite quantum dot film by one-step crystallization, and belongs to the field of perovskite quantum dot material technology. The present disclosure uses adamantanemethylamine and hydrohalic acid as ligands, first mixes a cesium halide, a lead halide, and the ligands with a solvent to obtain a precursor solution, then deposits the precursor solution on a substrate, and then heats the substrate to obtain the CsPbX3 perovskite quantum dot film. The present disclosure uses adamantanemethylamine and hydrohalic acid as the ligands, which can quickly coat the perovskite, complex with the CsPbX3 perovskite, and directly form the perovskite quantum dot via a strong steric effect. Further, the present disclosure is simple and inexpensive, can directly obtain a high-quality perovskite quantum dot film with a thickness of more than 500 nm by one-step crystallization.

## Claims

### Claim 1

A method for preparing a CsPbX3 perovskite quantum dot film by one-step crystallization, comprising:
(1) mixing a cesium halide, a lead halide, and a ligand with a solvent to obtain a precursor solution;
(2) depositing the precursor solution on a substrate, and then heating the substrate to obtain the CsPbX3 perovskite quantum dot film;
X in the CsPbX3 being one or more of Cl, Br, or I; and
the ligand being adamantanemethylamine and hydrohalic acid.

### Claim 2 (depends on 1)

The method according to claim 1, wherein a molar ratio of adamantanemethylamine to hydrohalic acid in the ligand is 1:2-2:1.

### Claim 3 (depends on 1)

The method according to claim 1, wherein the solvent in step (1) is one or more of N, N-dimethyl formamide, dimethyl sulfoxide, γ-butyrolactone, or N, N-dimethyl acetamide.

### Claim 4 (depends on 1)

The method according to claim 1, wherein a molar ratio of the cesium halide to the lead halide to the ligand to the solvent in step (1) is (0.1-2) mol:(0.1-2) mol:(0.1-2) mol:1 mL.

### Claim 5 (depends on 1)

The method according to claim 1, wherein the depositing approach in step (2) is spin coating, drop coating, scrape coating, spray coating, or printing.

### Claim 6 (depends on 5)

The method according to claim 5, wherein when the depositing approach is the spin coating, the spin coating comprises a first stage and a second stage in sequence, the spin coating in the first stage is at a rate of 1000 rpm for a duration of 10 s, and at an acceleration of 500 rpm·s−1 from rest to reaching the spin coating rate; and the spin coating in the second stage is at a rate of 2000 rpm for a duration of 20 s, and at an acceleration of 1000 rpm·s−1 from the spin coating rate in the first stage to reaching the spin coating rate in the second stage.

### Claim 7 (depends on 1)

The method according to claim 1, wherein the heating in step (2) is at a temperature of 60° C.-180° C. for a duration of 1-30 min.