# US 12,110,584 B2 · Low temperature growth of transition metal chalcogenides

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- Number: US 12,110,584 B2
- Document ID: US12110584B2
- Status: Granted
- Kind: B2
- Application number: 17/361,231
- Filed: 2021-06-28
- Published: 2022-12-29
- Granted: 2024-10-08
- Earliest claimed: 2021-06-28
- Assignees: Applied Materials, Inc.
- Applicants: Applied Materials, Inc.
- Inventors: Chandan Das; Susmit Singha Roy; Bhaskar Jyoti Bhuyan; John Sudijono; Abhijit Basu Mallick; Mark Saly
- Web page: https://patentgrep.com/patent/US12110584B2

## CPC

- C23C 16/305: {Sulfides, selenides, or tellurides}
- H10P 14/69394: {the material containing titanium, e.g. TiO2}
- C23C 16/04: Coating on selected surface areas, e.g. using masks
- C23C 16/06: characterised by the deposition of metallic material
- C23C 16/40: Oxides
- C23C 16/4485: {by evaporation without using carrier gas in contact with the source material (C23C16/4486 takes precedence)}
- C23C 16/45523: {Pulsed gas flow or change of composition over time}
- C23C 16/45525: {Atomic layer deposition [ALD]}
- C23C 16/56: After-treatment
- H10P 14/20: of semiconductor materials
- H10P 14/3436: {being chalcogenide semiconductor materials not being oxides, e.g. ternary compounds}
- H10P 14/6336: {in the presence of a plasma [PECVD]}
- H10P 14/6544: {to change the morphology of the insulating materials, e.g. transformation of an amorphous layer into a crystalline layer}
- H10P 14/668: {the materials being characterised by the deposition precursor materials}
- H10P 14/6939: {characterised by the metal}
- H10P 14/203: {using transformation of metal, e.g. oxidation or nitridation}
- H10P 14/3434: {being oxide semiconductor materials (Group IIB-VIA semiconductor materials H10P14/3424)}
- H10P 14/6339: {deposition by cyclic CVD, e.g. ALD, ALE or pulsed CVD}
- C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04)
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10

## Abstract

Transition metal dichalcogenide films and methods for depositing transition metal dichalcogenide films on a substrate are described. Methods for converting transition metal oxide films to transition metal dichalcogenide films are also described. The substrate is exposed to a precursor and a chalcogenide reactant to form the transition metal dichalcogenide film. The exposures can be sequential or simultaneous.

## Claims

### Claim 1

A method of depositing a film, the method comprising:
forming a transition metal oxide film on a substrate surface, forming the transition metal oxide film comprises forming a transition metal film followed by oxidizing the transition metal film by exposing the transition metal film to a plasma treatment of one or more of O2 or O3 to form the transition metal oxide film; and
converting the transition metal oxide film to a transition metal dichalcogenide film.

### Claim 2 (depends on 1)

The method of claim 1, wherein the transition metal oxide film is converted to the transition metal dichalcogenide film after forming the transition metal oxide film having a thickness in a range of from 15 Å to 25 Å.

### Claim 3 (depends on 2)

The method of claim 2, further comprising repeating forming the transition metal oxide film and converting the transition metal oxide film to form a transition metal dichalcogenide film with a final thickness up to 200 Å.

### Claim 4 (depends on 1)

The method of claim 1, wherein the substrate surface comprises a dielectric material and a conductive material.

### Claim 5 (depends on 4)

The method of claim 4, wherein the transition metal oxide film forms selectively on the dielectric material.

### Claim 6 (depends on 1)

The method of claim 1, wherein converting the transition metal oxide film to the transition metal dichalcogenide film is conducted at a temperature in a range of from 350° C. to 500° C. and at a pressure in a range of from 1 Torr to 10 Torr.

### Claim 7 (depends on 1)

The method of claim 1, wherein converting the transition metal oxide film to the transition metal dichalcogenide film is conducted for a time period in a range of from 30 minutes to 60 minutes.

### Claim 8 (depends on 1)

The method of claim 1, wherein converting the transition metal oxide film to the transition metal dichalcogenide film comprises pulsing the transition metal oxide film with one or more of sulfur (S), selenium (Se) and tellurium (Te).

### Claim 9

A method of depositing a film, the method comprising:
forming a transition metal dichalcogenide film in a process cycle consisting essentially of sequential exposure of a substrate to a transition metal oxide precursor, a purge gas, a chalcogenide reactant, and purge gas.

### Claim 10 (depends on 9)

The method of claim 9, wherein the transition metal dichalcogenide film has a transition metal comprising one or more of tungsten (W), molybdenum (Mo), tantalum (Ta), titanium (Ti), or ruthenium (Ru).

### Claim 11 (depends on 9)

The method of claim 9, wherein the transition metal oxide precursor comprises one or more of WOF4, WO2F2, WOCl4, WO2Cl2, WOBr4, WO2Br2, WOI4, WO2I2, MoOF4, MoO2F2, MoOCl4, MoO2Cl2, MoOBr4, MoO2Br2, MoOI4, MoO2I2, TaOF4, TaO2F2, TaOCl4, TaO2Cl2, TaOBr4, TaO2Br2, TaOI4, TaO2I2, TiOF4, TiO2F2, TiOCl4, TiO2Cl2, TiOBr4, TiO2Br2, TiOI4, TiO2I2, RuOF4, RuO2F2, RuOCl4, RuO2Cl2, RuOBr4, RuO2Br2, RuOI4, and RuO2I2.

### Claim 12 (depends on 9)

The method of claim 9, wherein the transition metal dichalcogenide film is substantially free of oxygen.

### Claim 13 (depends on 9)

The method of claim 9, further comprising purging the substrate of the transition metal oxide precursor prior to exposing the substrate to the chalcogenide reactant.

### Claim 14 (depends on 13)

The method of claim 13, wherein purging comprises one or more of applying a vacuum or flowing a purge gas over the substrate, the purge gas comprising one or more of nitrogen (N2), helium (He), and argon (Ar).

### Claim 15 (depends on 9)

The method of claim 9, wherein the chalcogenide reactant is selected from the group consisting of sulfur (S), selenium (Se), and tellurium (Te).

### Claim 16

A method of depositing a film, the method comprising:
forming a transition metal oxide film in a transition metal oxide process cycle comprising sequential exposure of a substrate to a transition metal precursor, a purge gas, an oxide reactant comprising a plasma of one or more of O2 or O3, and a purge gas; and
converting the transition metal oxide film to a transition metal dichalcogenide film in a chalcogen process cycle comprising sequential exposure of the transition metal oxide film to a chalcogenide reactant and a purge gas.

### Claim 17 (depends on 16)

The method of claim 16, wherein the chalcogen process cycle is performed after each metal oxide process cycle.

### Claim 18 (depends on 16)

The method of claim 16, wherein the transition metal oxide process cycle is repeated a number of times to form a transition metal oxide film of a predetermined thickness prior to performing the chalcogen process cycle.