# US 10,319,589 B2 · High performance thin films from solution processible two-dimensional nanoplates

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- Number: US 10,319,589 B2
- Document ID: US10319589B2
- Status: Granted
- Kind: B2
- Application number: 15/510,618
- Filed: 2015-09-10
- Published: 2017-07-06
- Granted: 2019-06-11
- Earliest claimed: 2014-09-12
- Assignees: The Regents of the University of California
- Applicants: The Regents of the University of California
- Inventors: Xiangfeng Duan; Yu Huang
- Web page: https://patentgrep.com/patent/US10319589B2

## CPC

- H10P 14/265: {using solutions}
- B05D 1/005: {Spin coating}
- B05D 1/18: performed by dipping
- H10D 30/6741: {Group IV materials, e.g. germanium or silicon carbide (TFTs having oxide semiconductors H10D30/6755)}
- H10D 30/675: {Group III-V materials, Group II-VI materials, Group IV-VI materials, selenium or tellurium}
- H10P 14/2905: {Silicon, silicon germanium or germanium}
- H10P 14/3238: {being insulating materials}
- H10P 14/3436: {being chalcogenide semiconductor materials not being oxides, e.g. ternary compounds}
- H10P 14/3461: {Nanoparticles}
- H10P 34/42: with electromagnetic radiation, e.g. laser annealing (laser cutting H10P54/20)
- H10P 95/90: Thermal treatments, e.g. annealing or sintering
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
- B05D: PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL (conveying articles or workpieces through baths of liquid B65G, e.g. B65G49/02)
- H10D: INORGANIC ELECTRIC SEMICONDUCTOR DEVICES

## Abstract

A method of forming a thin film includes: (1) providing an ink composition including nanoplates of a layered material disposed in a liquid dispersion medium; (2) applying the ink composition over a substrate to form a coating; and (3) annealing the coating to form a thin film of the layered material over the substrate.

## Claims

### Claim 1

A method of forming a thin film, comprising:
providing an ink composition including nanoplates of a layered material disposed in a liquid dispersion medium;
applying the ink composition over a substrate to form a coating; and
annealing the coating to form a thin film of the layered material over the substrate.

### Claim 2 (depends on 1)

The method of claim 1, wherein the layered material is a transition metal chalcogenide or a post-transition metal chalcogenide.

### Claim 3 (depends on 1)

The method of claim 1, wherein the layered material is selected from Bi2Se3, Bi2Te3, MoS2, MoSe2, WS2, WSe2, TaS2, TiS2, SnS2, and NbSe2.

### Claim 4 (depends on 1)

The method of claim 1, wherein the nanoplates have a lateral dimension of at least 100 nm, at least 200 nm, at least 300 nm, at least 400 nm, at least 500 nm, at least 600 nm, at least 700 nm, at least 800 nm, at least 900 nm, at least 1 μm, at least 2 μm, or at least 3 μm.

### Claim 5 (depends on 1)

The method of claim 1, wherein the nanoplates have a thickness of up to 39 nm, up to 36 nm, up to 33 nm, up to 30 nm, up to 27 nm, up to 24 nm, up to 21 nm, up to 18 nm, up to 15 nm, up to 12 nm, up to 9 nm, or up to 6 nm.

### Claim 6 (depends on 1)

The method of claim 1, wherein a surface coverage of the substrate by the nanoplates is at least 70%, at least 80%, at least 90%, at least 95%, at least 98%, at least 99%, or at least 99.5%.

### Claim 7 (depends on 1)

The method of claim 1, wherein neighboring ones of the nanoplates in the thin film form plane-to-plane contacts.

### Claim 8 (depends on 1)

The method of claim 1, wherein applying the ink composition is via spin-coating, dip-coating, screen printing, or inkjet printing.

### Claim 9 (depends on 1)

The method of claim 1, wherein annealing the coating is via thermal annealing at a temperature in the range of 150° C. to 400° C., 150° C. to 300° C., 300° C. to 400° C., or 240° C. to 350° C.

### Claim 10 (depends on 1)

The method of claim 1, wherein annealing the coating is via laser annealing.

### Claim 11 (depends on 1)

The method of claim 1, wherein a carrier mobility of the thin film at 300 K is at least 20 cm2·V−1·s−1, at least 30 cm2·V−1·s−1, at least 40 cm2·V−1·s−1, at least 50 cm2V−1·s−1, at least 60 cm2V−1·s−1, at least 70 cm2V−1·s−1, at least 80 cm2·V−1·s−1, at least 90 cm2·V−1·s−1, at least 100 cm2·V−1·s−1, or at least 110 cm2·V−1·s−1.

### Claim 12 (depends on 1)

The method of claim 1, wherein a conductivity of the thin film at 300 K is at least 100 S·cm−1, at least 200 S·cm−1, at least 300 S·cm−1, at least 400 S·cm−1, at least 500 S·cm−1, at least 600 S·cm−1, or at least 700 S·cm−1.

### Claim 13

A method of forming nanoplates, comprising:
combining a metal-containing precursor, a chalcogenide-containing precursor, a capping agent, and a reducing solvent to form a reaction mixture; and
heating the reaction mixture to form nanoplates of a metal chalcogenide,
wherein the nanoplates have a lateral dimension of at least 500 nm, and have a thickness of up to 9 nm.

### Claim 14 (depends on 13)

The method of claim 13, wherein the capping agent is poly(vinylpyrrolidone).

### Claim 15 (depends on 13)

The method of claim 13, wherein the reducing solvent is a polyol.

### Claim 16 (depends on 13)

The method of claim 13, wherein heating the reaction mixture is carried out at a temperature in the range of 100° C. to 300° C. or 150° C. to 200° C., and for a duration in the range of 0.4 hr to 5 hr or 1 hr to 4 hr.

### Claim 17 (depends on 13)

The method of claim 13, wherein the metal is a transition metal or a post-transition metal.

### Claim 18 (depends on 13)

The method of claim 13, wherein the metal is selected from Bi, Mo, W, Ta, Ti, Sn, and Nb, and the chalcogenide is selected from Se, Te, and S.

### Claim 19 (depends on 13)

The method of claim 13, wherein the lateral dimension of the nanoplates is at least 2 μm or at least 3 μm, and the thickness of the nanoplates is up to 6 nm.

### Claim 20 (depends on 13)

The method of claim 13, wherein the metal chalcogenide is a first metal chalcogenide, and the method further comprises performing epitaxial growth of a second metal chalcogenide over the nanoplates, and the second metal chalcogenide is different from the first metal chalcogenide.

### Claim 21 (depends on 1)

The method of claim 1, wherein the nanoplates have a hexagonal geometry.

### Claim 22 (depends on 1)

The method of claim 1, wherein the thin film has a homogeneous composition of the layered material.