# US 10,483,116 B2 · Methods of depositing metal films using metal oxyhalide precursors

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- Number: US 10,483,116 B2
- Document ID: US10483116B2
- Status: Granted
- Kind: B2
- Application number: 16/180,817
- Filed: 2018-11-05
- Published: 2019-03-21
- Granted: 2019-11-19
- Earliest claimed: 2015-08-28
- Assignees: Applied Materials, Inc.
- Applicants: Applied Materials, Inc.
- Inventors: Xinyu Fu; David Knapp; David Thompson; Jeffrey W. Anthis; Mei Chang
- Web page: https://patentgrep.com/patent/US10483116B2

## CPC

- H10P 14/432: {using selective deposition}
- C23C 16/06: characterised by the deposition of metallic material
- C23C 16/08: from metal halides
- C23C 16/45527: {characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations}
- C23C 16/45553: {characterized by the use of precursors specially adapted for ALD}
- H10D 30/6755: {Oxide semiconductors, e.g. zinc oxide, copper aluminium oxide or cadmium stannate}
- H10P 14/43: Chemical deposition, e.g. chemical vapour deposition [CVD]
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
- 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)
- H10D: INORGANIC ELECTRIC SEMICONDUCTOR DEVICES

## Abstract

Processing methods comprising exposing a substrate to an optional nucleation promoter followed by sequential exposure of a first reactive gas comprising a metal oxyhalide compound and a second reactive gas to form a metal film on the substrate.

## Claims

### Claim 1

A processing method comprising exposing a substrate to a first reactive gas and a second reactive gas to deposit a metal film on the substrate, the first reactive gas having an initial composition and a final composition, the initial composition comprising a metal oxyhalide, the final composition comprising a metal halide, the metal film having a resistivity less than 200 μΩ-cm and a metal content greater than 50 atomic percent.

### Claim 2 (depends on 1)

The method of claim 1, wherein the metal oxyhalide comprises one or more of a tungsten, molybdenum, niobium, vanadium and/or chromium.

### Claim 3 (depends on 1)

The method of claim 1, wherein the metal oxyhalide comprises substantially no fluorine.

### Claim 4 (depends on 1)

The method of claim 1, wherein the metal oxyhalide comprises a metal oxychloride.

### Claim 5 (depends on 4)

The method of claim 4, wherein the metal oxychloride comprises tungsten oxychloride.

### Claim 6 (depends on 5)

The method of claim 5, wherein the metal halide comprises tungsten pentachloride.

### Claim 7 (depends on 1)

The method of claim 1, wherein second reactive gas comprises a hydrogen-containing compound and the metal film is a metal film.

### Claim 8 (depends on 1)

The method of claim 1, wherein the second reactive gas comprises a nitrogen-containing compound and the metal film comprises a metal nitride.

### Claim 9 (depends on 1)

The method of claim 1, further comprising exposing a substrate to a nucleation promoter.

### Claim 10 (depends on 9)

The method of claim 9, wherein the nucleation promoter is selected from the group consisting of trialkylaluminum, trialkylgallium, trialkylindium, disilane, trisilane, tetrasilane, diethylsilane, derivatives thereof and combinations thereof.

### Claim 11 (depends on 10)

The method of claim 10, wherein the substrate comprises a dielectric.

### Claim 12 (depends on 10)

The method of claim 10, wherein exposure to the nucleation promoter occurs substantially simultaneously with a first exposure to the metal oxyhalide.

### Claim 13 (depends on 1)

The method of claim 1, wherein the final composition comprises a mixture of metal oxyhalide and metal halide.

### Claim 14 (depends on 13)

The method of claim 13, wherein the composition of the first reactive gas transitions gradually from the initial composition to the final composition.

### Claim 15 (depends on 13)

The method of claim 13, wherein the composition of the first reactive gas changes abruptly from the initial composition to the final composition.

### Claim 16 (depends on 1)

The method of claim 1, wherein the final composition comprises no metal oxyhalide.

### Claim 17

A processing method comprising
positioning a substrate having a dielectric surface in a processing chamber;
treating the dielectric surface with a nucleation promoter selected from the group consisting of trialkylaluminum, trialkylgallium, trialkylindium, disilane, trisilane, tetrasilane, diethylsilane, derivatives thereof and combinations thereof; and
sequentially exposing at least a portion of the treated dielectric surface to a first reactive gas and a second reactive gas to form a tungsten film, the first reactive gas having substantially no fluorine, an initial composition and a final composition, the initial composition comprising tungsten oxychloride and the final composition comprising tungsten halide and the second reactive gas comprises hydrogen.