# US 10,121,658 B2 · Method of fabricating black phosphorus ultrathin film and black phosphorus ultrathin film thereof

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- Number: US 10,121,658 B2
- Document ID: US10121658B2
- Status: Granted
- Kind: B2
- Application number: 15/576,664
- Filed: 2016-03-24
- Published: 2018-05-17
- Granted: 2018-11-06
- Earliest claimed: 2015-05-28
- Assignees: Korea Research Institute of Standards and Science
- Applicants: Korea Research Institute of Standards and Science
- Inventors: Hyuksang Kwon; Jeong Won Kim; Eun Seong Lee
- Web page: https://patentgrep.com/patent/US10121658B2

## CPC

- H10P 14/38: {characterised by treatments done after the formation of the materials}
- H10F 77/45: Wavelength conversion means, e.g. by using luminescent material, fluorescent concentrators or up-conversion arrangements
- H10F 77/496: {Luminescent members, e.g. fluorescent sheets (wavelength conversion means for photovoltaic cells H10F77/45)}
- H10P 14/22: using physical deposition, e.g. vacuum deposition or sputtering
- H10P 14/24: using chemical vapour deposition [CVD]
- H10P 14/3402: {characterised by the chemical composition}
- H10P 34/42: with electromagnetic radiation, e.g. laser annealing (laser cutting H10P54/20)
- H10P 95/00: Generic processes or apparatus for manufacture or treatments not covered by the other groups of this subclass
- H10D 30/6757: {characterised by the structure of the channel, e.g. transverse or longitudinal shape or doping profile (TFTs having channel structures for preventing kink or snapback effects H10D30/6708; TFTs having lightly-doped source or drain extensions H10D30/6715)}
- H10D 62/57: the imperfections being on the surface of the semiconductor body, e.g. the body having a roughened surface
- H10D 62/80: characterised by the materials
- H10F 77/12: Active materials
- H10H 20/822: Materials of the light-emitting regions
- Y02E 10/52: PV systems with concentrators
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
- H10F: INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
- H10D: INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
- H10H: INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

The present invention relates to a method of fabricating a black phosphorus thin film and a black phosphorus thin film thereof and, more particularly, to a method of fabricating a black phosphorus ultrathin film by forming the black phosphorous ultrathin film in a chamber by active oxygen and removing accompanying black phosphorus oxide film water. The black phosphorus ultrathin film has a surface that does not substantially have defects and is uniform in a large area, and has a surface roughness property of 1 nm or less, to represent a high application property to an optoelectronic device and a field effect transistor.

## Claims

### Claim 1

A method of fabricating a black phosphorous ultrathin film, comprising:
forming a black phosphorous thin film; and
forming the black phosphorous ultrathin film by irradiating an ultraviolet ray into a chamber and
etching the black phosphorous thin film using active oxygen generated by a reaction between the irradiated ultraviolet ray and oxygen.

### Claim 2 (depends on 1)

The method of fabricating a black phosphorous ultrathin film of claim 1, wherein the black phosphorous thin film is a black phosphorous thin film formed from pristine black phosphorous by a mechanical exfoliation method or a chemical vapor deposition method.

### Claim 3 (depends on 1)

The method of fabricating a black phosphorous ultrathin film of claim 1, further comprising confirming etching of the black phosphorous ultrathin film using any one or more of an optical image and a Raman spectroscopy.

### Claim 4 (depends on 3)

The method of fabricating a black phosphorous ultrathin film of claim 3, further comprising removing a black phosphorous oxide film by treating the black phosphorous ultrathin film of which the etching is confirmed using water.

### Claim 5 (depends on 4)

The method of fabricating a black phosphorous ultrathin film of claim 4, further comprising confirming a thickness of the black phosphorous ultrathin film from which the black phosphorous oxide film is removed using any one or more of an optical image, a Raman spectroscopy, an atomic force microscope, and a scanning tunneling microscope.

### Claim 6 (depends on 1)

The method of fabricating a black phosphorous ultrathin film of claim 1, wherein the chamber is formed so that oxygen is continuously introduced thereinto and exhausted therefrom.

### Claim 7 (depends on 6)

The method of fabricating a black phosphorous ultrathin film of claim 6, wherein the oxygen is introduced into the chamber in 100 to 600 sccm.

### Claim 8 (depends on 1)

The black phosphorous ultrathin film fabricated by the method of fabricating a black phosphorous ultrathin film of claim 1 and having a surface roughness in a range of 1 nm or less in an area of 10 μm×10 μm.

### Claim 9 (depends on 8)

The black phosphorous ultrathin film of claim 8, wherein the black phosphorous ultrathin film has a thickness of 3 nm or less.

### Claim 10 (depends on 9)

The black phosphorus ultrathin film of claim 9, wherein the black phosphorus ultrathin film has one or two photoluminescence (PL) peaks at a wavelength of 700 to 1000 nm, the PL peaks comprising any one or two or more of a single PL peak by a black phosphorus single-atomic layer at a wavelength of 750 to 810 nm and a single PL peak by a black phosphorus two-atomic layer at a wavelength of 870 to 930 nm.

### Claim 11 (depends on 9)

The optoelectronic device comprising the black phosphorous ultrathin film of claim 9.

### Claim 12 (depends on 1)

A black phosphorous ultrathin film fabricated by the method of fabricating a black phosphorous ultrathin film of claim 1 and having a surface roughness in a range of 1 nm or less in an area of 10 μm×10 μm and a thickness of 8 nm or more.

### Claim 13 (depends on 12)

A field effect transistor comprising the black phosphorous ultrathin film of claim 12.
