# US 10,246,637 B2 · One-pot method for preparing core-shell nanocrystals

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- Number: US 10,246,637 B2
- Document ID: US10246637B2
- Status: Granted
- Kind: B2
- Application number: 15/149,131
- Filed: 2016-05-07
- Published: 2016-11-10
- Granted: 2019-04-02
- Earliest claimed: 2015-05-08
- Assignees: Massachusetts Institute of Technology
- Applicants: Massachusetts Institute of Technology
- Inventors: Zhengtao Deng; Tian Ming; He Dong; Aishuang Xiang; Jing Kong
- Web page: https://patentgrep.com/patent/US10246637B2

## CPC

- C09K 11/883: {with zinc or cadmium}
- B01J 13/02: Making microcapsules or microballoons {(for medical preparations A61K9/50)}
- C09B 67/0097: {Dye preparations of special physical nature; Tablets, films, extrusion, microcapsules, sheets, pads, bags with dyes}
- B82Y 15/00: Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
- B82Y 40/00: Manufacture or treatment of nanostructures
- Y10S 977/882: Assembling of separate components, e.g. by attaching
- C09K: MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C09B: ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES {, e.g. PIGMENTS}; MORDANTS; LAKES (fermentation or enzyme using processes to synthesise a desired chemical compound C12P)
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- Y10S: TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS

## Abstract

A method for preparing a core-shell nanocrystal can include mixing an M-containing precursor solution, an X-containing precursor solution, and an acid or alcohol in an inert atmosphere at a first temperature to form a reaction mixture; maintaining the reaction mixture at the first temperature to grow the MX core of the nanocrystal; raising the temperature of the reaction mixture to a second temperature; and maintaining the reaction mixture at the second temperature to grow a shell of the nanocrystal.

## Claims

### Claim 1

A method for preparing a core-shell nanocrystal comprising:
mixing an M-containing precursor solution, an X-containing precursor solution, and an acid or alcohol in an inert atmosphere at a first temperature to form a reaction mixture;
maintaining the reaction mixture at the first temperature to grow an MX semiconductor crystalline core of the nanocrystal;
raising the temperature of the reaction mixture to a second temperature; and
maintaining the reaction mixture at the second temperature to grow a semiconductor crystalline shell of the nanocrystal for a period of between 5 to 120 minutes.

### Claim 2 (depends on 1)

The method of claim 1, wherein the M-containing precursor solution includes zinc, cadmium, or mercury.

### Claim 3 (depends on 1)

The method of claim 1, wherein the first temperature is between 40° C. and 140° C.

### Claim 4 (depends on 1)

The method of claim 1, wherein the X-containing precursor solution includes sulfur, selenium, or tellurium.

### Claim 5 (depends on 1)

The method of claim 1, wherein the acid includes a thioglycolic acid.

### Claim 6 (depends on 1)

The method of claim 1, wherein the acid or alcohol includes a mercaptopropionic acid or alcohol.

### Claim 7 (depends on 1)

The method of claim 1, wherein the nanocrystal is polyhedral.

### Claim 8 (depends on 1)

The method of claim 1, wherein the acid or alcohol includes a thiol group.

### Claim 9 (depends on 1)

The method of claim 1, wherein the acid or alcohol includes a selenol group.

### Claim 10 (depends on 1)

The method of claim 1, wherein the shell includes MS or MSe.

### Claim 11 (depends on 1)

The method of claim 1, wherein the reaction mixture is aqueous.

### Claim 12 (depends on 1)

The method of claim 1, further comprising maintaining the reaction mixture at the first temperature for a period of between 5 minutes and 2 hours.

### Claim 13 (depends on 1)

The method of claim 1, wherein the inert atmosphere includes argon or nitrogen.

### Claim 14

A method of preparing a core-shell nanocrystal comprising:
forming a reaction mixture containing a first group II (M1) precursor, a second group II precursor (M2), a first group VI precursor (X1), and an acid or alcohol including a second group VI material (X2);
maintaining the reaction mixture at a first temperature to grow the M1X1 core of the nanocrystal;
raising the temperature of the reaction mixture to a second temperature; and
maintaining the reaction mixture at the second temperature to grow a M2X2 shell of the nanocrystal for a period of between 5 to 120 minutes.

### Claim 15 (depends on 14)

The method of claim 14, wherein M1 includes zinc, cadmium, or mercury.

### Claim 16 (depends on 14)

The method of claim 14, wherein M2 includes zinc, cadmium, or mercury.

### Claim 17 (depends on 14)

The method of claim 14, wherein the first temperature is between 40° C. and 140° C.

### Claim 18 (depends on 14)

The method of claim 14, wherein X1 includes sulfur, selenium, or tellurium.

### Claim 19 (depends on 14)

The method of claim 14, wherein X2 includes sulfur, selenium, or tellurium.

### Claim 20 (depends on 14)

The method of claim 14, wherein the acid or alcohol includes a thiol group.

### Claim 21 (depends on 14)

The method of claim 14, wherein the acid or alcohol includes a selenol group.

### Claim 22 (depends on 14)

The method of claim 14, wherein the acid includes a thioglycolic acid.

### Claim 23 (depends on 14)

The method of claim 14, wherein the acid includes a mercaptopropionic acid.

### Claim 24 (depends on 14)

The method of claim 14, wherein the nanocrystal is polyhedral.

### Claim 25 (depends on 14)

The method of claim 14, wherein the reaction mixture is aqueous.

### Claim 26 (depends on 14)

The method of claim 14, further comprising maintaining the reaction mixture at the first temperature for a period of between 5 minutes and 2 hours.

### Claim 27 (depends on 14)

The method of claim 14, wherein the inert atmosphere includes argon or nitrogen.
