# US 11,898,072 B2 · Fluorescent semiconductor nanocrystal material, preparation and application thereof

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- Number: US 11,898,072 B2
- Document ID: US11898072B2
- Status: Granted
- Kind: B2
- Application number: 17/338,306
- Filed: 2021-06-03
- Published: 2021-09-23
- Granted: 2024-02-13
- Earliest claimed: 2019-10-31
- Assignees: Shanghai Jiao Tong University
- Applicants: Shanghai Jiao Tong University
- Inventors: Liang Li; Qinggang Zhang
- Web page: https://patentgrep.com/patent/US11898072B2

## CPC

- C09K 11/02: Use of particular materials as binders, particle coatings or suspension media therefor
- C09K 11/565: {with zinc cadmium}
- C09K 11/621: {Chalcogenides}
- C09K 11/665: {with alkali or alkaline earth metals}
- C09K 11/883: {with zinc or cadmium}
- G01N 21/6428: {Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" (in vivo A61B5/00; immunoassay G01N33/53)}
- G01N 21/6489: {Photoluminescence of semiconductors}
- G01T 1/2023: {Selection of materials}
- H10F 39/1898: {Indirect radiation image sensors, e.g. using luminescent members}
- H10H 20/8512: {Wavelength conversion materials}
- C09K: MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)
- G01T: MEASUREMENT OF NUCLEAR OR X-RADIATION (radiation analysis of materials, mass spectrometry G01N23/00; tubes for determining the presence, intensity, density or energy of radiation or particles H01J47/00)
- H10F: INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
- H10H: INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS

## Abstract

A method for preparing a fluorescent semiconductor nanocrystal material. At least one semiconductor nanocrystal precursor is uniformly mixed with a micro/mesoporous material to form a mixture. The mixture is calcined under a temperature higher than or equal to a collapse temperature of the micro/mesoporous material to obtain the fluorescent semiconductor nanocrystal material. This application also provides a fluorescent semiconductor nanocrystal material prepared through the method, and applications thereof in the manufacture of a light-emitting diode device and a color conversion display panel.

## Claims

### Claim 1

A method for preparing a fluorescent semiconductor nanocrystal material, comprising:
(1) uniformly mixing at least one semiconductor nanocrystal precursor with a micro/mesoporous material to form a mixture; and
(2) calcining the mixture under a temperature higher than or equal to a collapse temperature of the micro/mesoporous material to make pores of the micro/mesoporous material collapse, encapsulating the at least one semiconductor nanocrystal precursor in the pores of the micro/mesoporous material to produce the fluorescent semiconductor nanocrystal material;
wherein the at least one fluorescent semiconductor nanocrystal material is in a form of powder.

### Claim 2 (depends on 1)

The method of claim 1, wherein a ratio of a total weight of the at least one semiconductor nanocrystal precursor to a weight of the micro/mesoporous material is 1:(0.05-20); and the at least one semiconductor nanocrystal precursor and the micro/mesoporous material are mixed uniformly through liquid phase mixing or solid phase mixing.

### Claim 3 (depends on 1)

The method of claim 1, wherein a pore size of the micro/mesoporous material is 0.5-50 nm.

### Claim 4 (depends on 1)

The method of claim 1, wherein in step (2), the calcination of the mixture is performed at 300-2000° C. for 10-600 min.

### Claim 5 (depends on 1)

The method of claim 1, wherein in step (2), the calcination of the mixture is performed at a pressure of 0.1-20 MPa.

### Claim 6 (depends on 1)

The method of claim 1, wherein the at least one semiconductor nanocrystal precursor consists of an AX precursor and a BX2 precursor; a molar ratio of the AX precursor to the BX2 precursor is 1:1; wherein A is Cs, Rb or K; B is Pb, Sn, Ge, In, Ag, Bi, Sb, Zn, Ca or Ba; and X is Cl, Br or I.

### Claim 7 (depends on 1)

The method of claim 1, wherein the at least one semiconductor nanocrystal precursor consists of an AX precursor, a B′X2 precursor and a BX2 precursor; a molar ratio of the AX precursor to the sum of the B′X2 precursor and the BX2 precursor is 1:1; wherein A is Cs, Rb or K; B′ and B are different, and are each independently selected from the group consisting of Pb, Sn, Ge, In, Ag, Bi, Sb, Zn, Ca and Ba; and X is Cl, Br or I.

### Claim 8 (depends on 1)

The method of claim 1, wherein the at least one semiconductor nanocrystal precursors consists of a cationic precursor and an anionic precursor; a molar ratio of the cationic precursor to the anionic precursor is 1:1; the cationic precursor is used to provide a cation Dn+, wherein n is an integer selected from 1-10; the cationic precursor is selected from the group consisting of hydrochlorides and nitrates of Zn, Cd and Hg, and hydrate thereof; the anionic precursor is used to provide an anion Yn−, wherein n is an integer selected from 1-10; and the anionic precursor is selected from the group consisting of simple substances and inorganic salts of S, Se, Te.

### Claim 9 (depends on 1)

The method of claim 1, wherein the at least one semiconductor nanocrystal precursor consists of a first precursor for providing a monovalent cation, a second precursor for providing a trivalent cation and a third precursor for providing a divalent anion;
wherein the first precursor is a compound of a IB group metal, and is selected from the group consisting of CuCl, CuBr, CuI, AgCl, AgBr, AgI and a combination thereof;
the second precursor is an organic acid salt of a IIIA group metal, and is selected from the group consisting of formate, acetate and propionate of In, Ga and Al;
the third precursor is an inorganic salt consisting of a VIA group element and a metal element, wherein the VIA group element is S and Se; and
a molar ratio of the first precursor to the second precursor to the third precursor is 0.5:0.5:1.

### Claim 10 (depends on 1)

The method of claim 1, wherein the micro/mesoporous material is a microporous material, a mesoporous material or a combination thereof, the microporous material is selected from the group consisting of microporous molecular sieve, microporous silica, microporous titania, microporous alumina, microporous transition metal oxide, microporous sulfide, silicate, aluminate and transition metal nitride and a combination thereof; and the mesoporous material is selected from the group consisting of mesoporous molecular sieve, mesoporous silica, mesoporous titania, mesoporous alumina, mesoporous carbon, mesoporous transition metal oxide, mesoporous sulfide, silicate, aluminate and transition metal nitride and a combination thereof.

### Claim 11 (depends on 6)

A fluorescent semiconductor nanocrystal material prepared by the method of claim 6, wherein the fluorescent semiconductor nanocrystal material has a nanocrystal structure of perovskite ABX3; a molar ratio of A to B to X in ABX3 is 1:1:3; A is Cs, Rb or K; B is Pb, Sn, Ge, In, Ag, Bi, Sb, Zn, Ca or Ba; and X is Cl, Br or I.

### Claim 12 (depends on 7)

A fluorescent semiconductor nanocrystal material prepared by the method of claim 7, wherein the fluorescent semiconductor nanocrystal material has a nanocrystal structure of halide B′X2-modified perovskite ABX3, and a molar ratio of A to (B′+B) to X is 1:1:3; A is Cs, Rb or K; B′ and B are different, and are independently selected from the group consisting of Pb, Sn, Ge, In, Ag, Bi, Sb, Zn, Ca and Ba; and X is Cl, Br or I.

### Claim 13 (depends on 8)

A fluorescent semiconductor nanocrystal material prepared by the method of claim 8, wherein the fluorescent semiconductor nanocrystal material has a binary Dn+Yn− nanocrystal structure; n is an integer selected from 1-10; a molar ratio of D to Y in Dn+Yn− is 1:1; and D is Zn, Cd or Hg, and Y is S, Se or Te.

### Claim 14 (depends on 9)

A fluorescent semiconductor nanocrystal material prepared by the method of claim 9, wherein the fluorescent semiconductor nanocrystal material has a ternary IB-IIIA-VIA nanocrystal structure with a general formula of G+ M3+(N2−)2, wherein G+ is Cu+ or Ag+; M3+ is In3+, Ga3+ or Al3+; N2− is S2− or Se2−; and a molar ratio of G+ to M3+ to N2− is 0.5:0.5:1.

### Claim 15 (depends on 11)

A light-emitting diode (LED) device, wherein the LED device comprises the fluorescent semiconductor nanocrystal material of claim 11.

### Claim 16 (depends on 11)

A color conversion display panel, wherein the color conversion display panel comprises the fluorescent semiconductor nanocrystal material of claim 11.

### Claim 17 (depends on 11)

A fluorescent scintillator, wherein the fluorescent scintillator is made of the fluorescent semiconductor nanocrystal material of claim 11.

### Claim 18 (depends on 11)

A biological detection device, wherein the biological detection device comprises the fluorescent semiconductor nanocrystal material of claim 11.