# US 2019/0169498 A1 · Compositions and methods relating to luminescent structures

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- Number: US 2019/0169498 A1
- Document ID: US20190169498A1
- Status: Published application
- Kind: A1
- Application number: 16/323,824
- Filed: 2017-08-25
- Published: 2019-06-06
- Earliest claimed: 2016-08-26
- Assignees: King Abdullah University of Science and Technology
- Applicants: King Abdullah University of Science and Technology
- Inventors: Makhsud I. SAIDAMINOV; Osman M. BAKR
- Web page: https://patentgrep.com/patent/US20190169498A1

## CPC

- C09K 11/665: {with alkali or alkaline earth metals}
- C01G 21/006: {Compounds containing lead, with or without oxygen or hydrogen, and containing two or more other elements}
- C09K 11/0833: {with alkali or alkaline earth metals}
- C01P 2002/34: perovskite-type (ABO3)
- C01P 2006/80: Compositional purity
- C09K: MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

Described herein are compositions and methods relating to luminescent structures.

## Claims

### Claim 1

A method for synthesizing a zero-dimensional perovskite, comprising:
mixing at least one of CsR or Cs(R)2 with at least one of PbR or Pb(R)2 in a solvent to create a mixture, wherein R is at least one of a halogen, a halogen anion, a monovalent anion, or the conjugate base of an acid;
heating the mixture to a temperature in a range of about 40° C. to about 180° C. and holding the mixture at the temperature for a period of time to form a precipitate, or
mixing the mixture with an antisolvent vapor and exposing the mixture to the antisolvent vapor for a period of time to form a precipitate;
isolating the precipitate;
washing the precipitate with a wash solvent to produce a washed precipitate; and
drying the washed precipitate by a drying method to produce the zero-dimensional perovskite.

### Claim 2 (depends on 1)

The method of claim 1, wherein R is at least one of Br, Cl, I, or CH3COO.

### Claim 3 (depends on 1)

The method of claim 1, wherein the mixing is done with a ratio of about 1 to about 1.

### Claim 4 (depends on 1)

The method of claim 1, wherein the temperature is about 120° C.

### Claim 5 (depends on 1)

The method of claim 1, wherein CsBr and PbBr2 are mixed.

### Claim 6 (depends on 1)

The method of claim 1, wherein the solvent is selected from the group consisting of DMSO, DMSO-DMF, DMF, and GBL.

### Claim 7 (depends on 1)

The method of claim 1, wherein the antisolvent is one or more of hydrocarbons, halocarbons, ethers, and ketones.

### Claim 8 (depends on 1)

The method of claim 1, wherein the holding period of time is about one hour or more.

### Claim 9 (depends on 1)

The method of claim 1, wherein the isolation method comprises:
filtering the precipitate with a filtering apparatus to obtain the isolated precipitate; and
storing at room temperature or heating the isolated precipitate to about 120° C. and holding the isolated precipitate at said temperature for about three hours.

### Claim 10 (depends on 1)

The method of claim 1, wherein the wash solvent is selected from the group consisting of DMSO, DMSO-DMF, DMF, and GBL.

### Claim 11 (depends on 1)

The method of claim 1, wherein the drying method comprises storing the washed precipitate at room temperature or heating the washed precipitate at about 100° C. for a period of time.

### Claim 12 (depends on 11)

The method of claim 11, wherein the period of time for the drying step is about 6 hours to about 16 hours.

### Claim 13 (depends on 1)

The method of claim 1, wherein the zero-dimensional perovskite is a zero-dimensional luminescent perovskite.

### Claim 14 (depends on 1)

The method of claim 1, wherein the zero-dimensional perovskite has a purity of at least about 95%.

### Claim 15 (depends on 1)

The method of claim 1, wherein the zero-dimensional perovskite is a purified Cs4PbBr6, Cs4PbCl6, Cs4PbI6, Cs4Pb(CH3COO)6 composition and has a purity of at least 95%.

### Claim 16 (depends on 1)

The method of claim 1, wherein the zero-dimensional perovskite is a purified Cs4PbBr6 composition, comprising at least 95% pure solid Cs4PbBr6 with a photoluminescence quantum yield of at least about 38% and an emission peak at about 515-525 nm following excitation at 365 nm.

### Claim 17

A zero-dimensional perovskite composition, comprising at least 95% pure solid zero-dimensional perovskite, wherein the zero-dimensional perovskite has a formula of Cs4Pb(R1)6 and a photoluminescence quantum yield of about 38% or greater, wherein R1 is a halogen, a halogen anion, a monovalent anion, or the conjugate base of an acid.

### Claim 18 (depends on 17)

The zero-dimensional perovskite composition of claim 17 wherein the zero-dimensional composition is at least one of purified Cs4PbBr6, Cs4PbCl6, Cs4PbI6, or Cs4Pb(CH3COO)6.

### Claim 19 (depends on 17)

The zero-dimensional perovskite composition of claim 17, wherein the zero-dimensional perovskite composition is a purified Cs4PbBr6 composition, comprising at least 95% pure solid Cs4PbBr6 with a photoluminescence quantum yield of at least about 38% and an emission peak at about 515-525 nm following excitation at 365 nm.