# US 2019/0355576 A1 · Thin film formation method

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- Number: US 2019/0355576 A1
- Document ID: US20190355576A1
- Status: Published application
- Kind: A1
- Application number: 16/347,904
- Filed: 2018-05-11
- Published: 2019-11-21
- Earliest claimed: 2017-06-12
- Assignees: Ulvac, Inc.; International Business Machines Corporation
- Applicants: Ulvac, Inc.; International Business Machines Corporation
- Inventors: Masanobu HATANAKA; Yohei OGAWA; Keon-chang LEE; Nobuyuki KATO; Takakazu YAMADA; John ROZEN
- Web page: https://patentgrep.com/patent/US20190355576A1

## CPC

- C23C 16/0272: {Deposition of sub-layers, e.g. to promote the adhesion of the main coating}
- H10P 14/69391: {the material containing aluminium, e.g. Al2O3}
- C23C 16/32: Carbides
- C23C 16/34: Nitrides {(C23C16/303 takes precedence)}
- 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 16/45536: {Use of plasma, radiation or electromagnetic fields}
- C23C 16/45553: {characterized by the use of precursors specially adapted for ALD}
- H10D 64/011: {of electrodes ohmically coupled to a semiconductor}
- H10P 14/6339: {deposition by cyclic CVD, e.g. ALD, ALE or pulsed CVD}
- H10P 14/69394: {the material containing titanium, e.g. TiO2}
- H10P 14/69397: {the material containing two or more metal elements}
- 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
- H10D: INORGANIC ELECTRIC SEMICONDUCTOR DEVICES

## Abstract

This method comprises: a first step for raising the temperature of an object on which a film is being formed to at least 200° C. and changing from a first state in which a film-forming material and a carrier gas are supplied to the object on which the film is being formed to deposit the film-forming material on the object on which the film is being formed to a second state in which the supply of the film-forming material is eliminated from the first state; and a second step for raising the temperature of the object on which the film is being formed to at least 200° C. and changing from a third state in which hydrogen gas and a carrier gas are supplied to the object on which the film is being formed to reduce the film-forming material to a fourth state in which the supply of the hydrogen gas is eliminated from the third state. The film-forming material is any one material selected from the group consisting of Al(CxH2x+1)3, Al(CxH2x+1)2H, and Al(CxH2x+1)2Cl. An aluminum carbide film with an aluminum atom content of at least 20 atom % is formed on the surface of the object on which the film is formed by alternately repeating the first step and the second step.

## Claims

### Claim 1

A thin film formation method comprising:
a first step of setting a temperature of a film formation subject to 200° C. or higher and changing a first state, in which a film formation material containing aluminum and carbon and a carrier gas of the film formation material are supplied to the film formation subject so that the film formation material collects on the film formation subject, to a second state, in which supplying of the film formation material is omitted from the first state, wherein
the film formation material is any one selected from a group consisting of Al(CxH2x+1)3, Al(CxH2x+1)2H, and Al(CxH2x+1)2Cl, where x is an integer of one or greater in each general formula, and
the thin film formation method further comprises a state that repeats the first step, thereby forming an aluminum carbide film on a surface of the film formation subject such that the aluminum carbide film has a content rate of aluminum atoms that is 20 atomic percent or greater.

### Claim 2 (depends on 1)

The thin film formation method according to claim 1, further comprising:
a second step of changing a third state, in which an active species, which includes hydrogen produced by exciting a reduction gas containing hydrogen, and a carrier gas of the reduction gas are supplied to the film formation subject to reduce the film formation material, to a fourth state, in which supplying of the reduction gas is omitted from the third state; and
a state that alternately repeats the first step and the second step.

### Claim 3 (depends on 1)

The thin film formation method according to claim 1, wherein the film formation material is any one selected from a group consisting of dimethylaluminum hydride and diethylaluminum hydride.

### Claim 4 (depends on 1)

The thin film formation method according to claim 1, wherein in a method for forming the aluminum carbide film, the film formation subject is placed in a vacuum chamber, the pressure of which is set within a range of 50 Pa to 1000 Pa, and the temperature of the film formation subject is set within a range of 200° C. to 500° C. so that the aluminum carbide film is formed to have a content rate of aluminum atoms that is 50 atomic percent or greater.

### Claim 5 (depends on 1)

The thin film formation method according to claim 1, wherein the surface of the film formation subject includes irregularities.

### Claim 6 (depends on 1)

The thin film formation method according to claim 1, further comprising:
a formation step of forming the surface of the film formation subject so that the surface is conductive prior to the first step.

### Claim 7 (depends on 1)

The thin film formation method according to claim 1, wherein the film formation material includes a first film formation material, the thin film formation method further comprising:
a third step of setting the temperature of the film formation subject to 200° C. or higher and changing a fifth state, in which a second film formation material containing aluminum and a carrier gas of the second film formation material are supplied to the film formation subject so that the second film formation material collects on the film formation subject, to a sixth state, in which supplying of the second film formation material is omitted from the fifth state,
wherein the second film formation material is any one selected from a group consisting of 1-methylpyrrolidine alane, trimethylamine borane hydride alane, and dimethylaluminum i-propoxide.

### Claim 8 (depends on 7)

The thin film formation method according to claim 7, further comprising:
a state that repeats the third step.

### Claim 9 (depends on 1)

The thin film formation method according to claim 1, wherein
the film formation material includes a first film formation material,
in the first state, a second film formation material containing aluminum is further supplied to the film formation subject so that the second film formation material collects on the film formation subject,
in the second state, supplying of the first film formation material and the second film formation material is omitted from the first state, and
the second film formation material is any one selected from a group consisting of 1-methylpyrrolidine alane, trimethylamine borane hydride alane, and dimethylaluminum i-propoxide.

### Claim 10 (depends on 2)

The thin film formation method according to claim 2, wherein the reduction gas includes at least one of hydrogen gas, hydrazine, and organic hydrazine.

### Claim 11 (depends on 2)

The thin film formation method according to claim 2, wherein the third state supplies the reduction gas and the carrier gas to the film formation subject that is heated or supplies a plasma generated by the reduction gas and the carrier gas to the film formation subject, thereby supplying an active species including the hydrogen to the film formation subject.