# US 11,897,766 B2 · Method for producing copper-selenide nanoparticles, aggregated bodies of copper-selenide nanoparticles, copper-selenide nanoparticles, and film-coated structure

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- Number: US 11,897,766 B2
- Document ID: US11897766B2
- Status: Granted
- Kind: B2
- Application number: 17/980,209
- Filed: 2022-11-03
- Published: 2023-03-02
- Granted: 2024-02-13
- Earliest claimed: 2019-09-30
- Assignees: Shoei Chemical Inc.
- Applicants: Shoei Chemical Inc.
- Inventors: Patrick Haben
- Web page: https://patentgrep.com/patent/US11897766B2

## CPC

- C01B 19/007: {Tellurides or selenides of metals (C01B19/002 takes precedence)}
- B22F 1/054: Nanosized particles
- B22F 1/16: Metallic particles coated with a non-metal (coated with lubricating or binding agents or with organic material B22F1/10)
- B22F 9/24: starting from liquid metal compounds, e.g. solutions
- B22F 2301/10: Copper
- B22F 2301/20: Refractory metals
- B22F 2304/05: Submicron size particles
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- B82Y 40/00: Manufacture or treatment of nanostructures
- C01P 2002/84: by UV- or VIS- data
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- B22F: WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER (making alloys by powder metallurgy C22C); APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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

In a method for producing nanoparticles of copper selenide, a flowable copper precursor is formed by combining a copper starting material and a ligand, and a flowable selenium precursor is formed by suspending a selenium starting material in a liquid. Then a flowable copper-selenium mixture including a lower-polarity solvent is formed by combining the flowable copper precursor and the flowable selenium precursor. The flowable copper-selenium mixture is conducted through at least one heating unit, and the nanoparticles of copper selenide are isolated in an oxygen-depleted environment. The isolation includes combining a solution containing the nanoparticles of copper selenide and a deoxygenated, higher-polarity solvent to precipitate the nanoparticles.

## Claims

### Claim 1

A method for producing copper-selenide nanoparticles by flow process, the method comprising:
forming a flowable copper precursor by combining a copper starting material and a ligand;
forming a flowable selenium precursor by suspending a selenium starting material in a liquid;
forming a flowable copper-selenium mixture by combining the flowable copper precursor and the flowable selenium precursor, the flowable copper-selenium mixture including a lower-polarity solvent;
forming a segmented flow of the flowable copper-selenium mixture by appending a segment of an immiscible, non-reacting fluid to each of a series of fixed-length segments of the flowable copper-selenium mixture;
forming a solution containing copper-selenide nanoparticles by conducting the segmented flow of the flowable copper-selenium mixture through at least one heating unit; and
isolating the nanoparticles of copper selenide in an oxygen-depleted environment, including combining the solution containing copper-selenide nanoparticles and a deoxygenated, higher-polarity solvent to precipitate the nanoparticles of copper selenide, the higher-polarity solvent being more polar than the lower-polarity solvent.

### Claim 2 (depends on 1)

The method of claim 1 wherein combining the copper starting material and the ligand includes combining with the lower-polarity solvent.

### Claim 3 (depends on 1)

The method of claim 1 wherein the liquid includes the lower-polarity solvent.

### Claim 4 (depends on 1)

The method of claim 1 wherein the at least one heating unit includes a conduit arranged in a controlled-temperature medium.

### Claim 5 (depends on 1)

The method of claim 1 wherein the ligand comprises an amine ligand.

### Claim 6 (depends on 5)

The method of claim 5 wherein in the flowable copper-selenium mixture, 0.5 mol or more of the amine ligand is contained in 1 mol equivalent of copper.

### Claim 7 (depends on 1)

The method of claim 1 wherein the deoxygenated higher-polarity solvent is sparged with a non-reacting gas to remove dissolved oxygen.

### Claim 8 (depends on 1)

The method of claim 1 wherein each of the copper precursor and the selenium precursor are sparged with a non-reacting gas to remove dissolved oxygen.