# US 2015/0147482 A1 · Chamber undercoat preparation method for low temperature ald films

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- Number: US 2015/0147482 A1
- Document ID: US20150147482A1
- Status: Published application
- Kind: A1
- Application number: 14/089,653
- Filed: 2013-11-25
- Published: 2015-05-28
- Earliest claimed: 2013-11-25
- Assignees: Lam Research Corporation
- Applicants: Lam Research Corporation
- Inventors: Hu Kang; Jun Qian; Adrien LaVoie
- Web page: https://patentgrep.com/patent/US20150147482A1

## CPC

- C23C 16/45525: {Atomic layer deposition [ALD]}
- C23C 16/4404: {Coatings or surface treatment on the inside of the reaction chamber or on parts thereof}
- 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)

## Abstract

Methods and apparatus disclosed herein relate to the formation and use of undercoats on the interior surfaces of reaction chambers used to deposit films on substrates. The undercoats are deposited through atomic layer deposition methods. The disclosed undercoats help prevent metal contamination, provide improved resistance to flaking, and are relatively thin. Because of the superior resistance to flaking, the disclosed undercoats allow more substrates to be processed between subsequent cleaning operations, thereby increasing throughput.

## Claims

### Claim 1

A method of forming an undercoat on interior surfaces of a reaction chamber for processing substrates, comprising:
(a) introducing a flow of a first reactant in vapor phase into the reaction chamber and allowing the first reactant to adsorb onto the interior surfaces of the reaction chamber;
(b) introducing a flow of a second reactant in vapor phase into the reaction chamber while the first reactant is adsorbed on the interior surfaces of the reaction chamber; and
(c) exposing the reaction chamber to plasma when the flow of at least one of the first and second reactants has ceased, in order to drive a reaction between the first and second reactants on the interior surfaces of the reaction chamber to form the undercoat, wherein the undercoat conformally coats the interior surfaces of the reaction chamber;
wherein operations (a)-(c) occur when there is no substrate present in the reaction chamber, and
wherein operations (a)-(c) are repeated until the undercoat is at least about 0.1 μm thick.

### Claim 2 (depends on 1)

The method of claim 1, wherein the temperature in the reaction chamber does not vary by more than about 2° C. during operations (a)-(c).

### Claim 3 (depends on 2)

The method of claim 2, wherein the undercoat is an oxide, nitride, a carbide, or a carbonitride.

### Claim 4 (depends on 3)

The method of claim 3, wherein the second reactant comprises O2 and N2O.

### Claim 5 (depends on 2)

The method of claim 2, wherein the undercoat is a noble metal, a lanthanide oxide, a group 4 metal oxide, or a group 5 metal oxide.

### Claim 6 (depends on 1)

The method of claim 1, wherein the undercoat conformally coats a substrate carrier.

### Claim 7 (depends on 1)

The method of claim 1, wherein the undercoat is no more than about 0.5 μm thick.

### Claim 8 (depends on 6)

The method of claim 6, wherein the undercoat is no more than about 0.2 μm thick.

### Claim 9 (depends on 1)

The method of claim 1, further comprising:
(d) receiving a substrate in the reaction chamber;
(e) introducing a flow of a third reactant in vapor phase into the reaction chamber and allowing the third reactant to adsorb onto the surface of the substrate;
(f) introducing a flow of a fourth reactant in vapor phase into the reaction chamber while the third reactant is adsorbed on the surface of the substrate; and
(g) exposing the reaction chamber to plasma when the flow of at least one of the third and fourth reactants has ceased, in order to drive a reaction between the third and fourth reactants to form a second film on the surface of the substrate.

### Claim 10 (depends on 9)

The method of claim 9, wherein the first reactant and second reactant are the same as the third reactant and fourth reactant, respectively.

### Claim 11 (depends on 10)

The method of claim 10, wherein the second and fourth reactants each comprise O2 and N2O.

### Claim 12 (depends on 10)

The method of claim 10, wherein reaction chamber pressure, reaction chamber temperature, dosing durations, plasma exposure durations, and RF power values remain substantially constant between operations (a)-(c) and operations (e)-(g).

### Claim 13 (depends on 9)

The method of claim 9, wherein the temperature in the reaction chamber does not vary by more than about 2° C. during operations (a)-(g).

### Claim 14 (depends on 13)

The method of claim 13, wherein operation (e) begins within about 5 minutes after a last iteration of operation (c).

### Claim 15 (depends on 9)

The method of claim 9, wherein the reaction chamber is not purged between a last iteration of operation (c) and a first iteration of operation (e).

### Claim 16 (depends on 9)

The method of claim 9, wherein operations (d)-(g) are repeated with a plurality of substrates, and wherein film deposited on the interior surfaces of the reaction chamber during operations (a)-(g) does not begin to flake or peel off until a total of at least about 7.5 μm of the second film has been deposited on the substrates.

### Claim 17 (depends on 9)

The method of claim 9, wherein operations (d)-(g) are repeated with a plurality of substrates, and wherein film deposited in operations (a)-(g) does not begin to flake or peel off until at least about 300 substrates have been processed through the reaction chamber using operations (d)-(g).

### Claim 18 (depends on 1)

The method of claim 1, wherein a first iteration of operations (a)-(c) are performed at a first level of RF flux and a second iteration of operations (a)-(c) are performed at a second level of RF flux, where the first and second levels of RF flux are different.

### Claim 19

A method of treating a reaction chamber for depositing films on substrates, comprising:
(a) removing previously deposited film from interior surfaces of the reaction chamber to clean the reaction chamber; and
(b) depositing an undercoat on the cleaned interior surfaces of the reaction chamber by an atomic layer deposition process;
wherein operation (b) occurs when there is no substrate present in the reaction chamber.

### Claim 20 (depends on 19)

The method of claim 19, wherein the undercoat is deposited to a thickness between about 0.1-0.5 μm.

### Claim 21 (depends on 19)

The method of claim 19, wherein operations (b) is performed isothermally.

### Claim 22

A reaction chamber ready for depositing films on substrates, comprising:
one or more inlets for introducing vapor phase reactants to the reaction chamber;
one or more outlets for removing vapor phase material from the reaction chamber;
a plasma generator for generating a plasma that is exposed to the reaction chamber; and
an undercoat on the interior surfaces of the reaction chamber, wherein the undercoat is about 0.5 μm thick or less, and wherein the undercoat conformally covers interior surfaces of the reaction chamber.