# US 10,373,864 B2 · Systems and methods for wetting substrates

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- Number: US 10,373,864 B2
- Document ID: US10373864B2
- Status: Granted
- Kind: B2
- Application number: 15/852,961
- Filed: 2017-12-22
- Published: 2018-06-28
- Granted: 2019-08-06
- Earliest claimed: 2016-12-27
- Assignees: Applied Materials, Inc.
- Applicants: Applied Materials, Inc.
- Inventors: Paul McHugh; Bridger Hoerner; Marvin Bernt; Thomas H. Oberlitner; Brian Aegerter; Richard W. Plavidal; Andrew Anten; Adam McClure; Randy Harris
- Web page: https://patentgrep.com/patent/US10373864B2

## CPC

- H10W 20/096: {by contacting with gases, liquids or plasmas}
- C25D 7/12: Semiconductors
- H10P 14/47: Electrolytic deposition, i.e. electroplating; Electroless plating
- H10W 20/056: {by filling conductive material into holes, grooves or trenches}
- H10W 20/081: {by forming openings in the dielectric parts}
- C25D 5/34: Pretreatment of metallic surfaces to be electroplated
- H10W 20/023: {the interconnections being through-semiconductor vias}
- H10W: GENERIC PACKAGES, INTERCONNECTIONS, CONNECTORS OR OTHER CONSTRUCTIONAL DETAILS OF DEVICES COVERED BY CLASS H10
- C25D: PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10

## Abstract

Methods of wetting a semiconductor substrate may include forming a controlled atmosphere in a processing chamber housing the semiconductor substrate. The semiconductor substrate may define a plurality of features, which may include vias. The methods may include flowing a wetting agent into the processing chamber. A chamber pressure may be maintained below about 100 kPa. The methods may also include wetting the plurality of features defined in the substrate.

## Claims

### Claim 1

A method of wetting a semiconductor substrate, the method comprising:
forming a carbon dioxide atmosphere in a processing chamber housing the semiconductor substrate, wherein the semiconductor substrate defines a plurality of features;
flowing a wetting agent into the processing chamber while maintaining the carbon dioxide atmosphere, wherein a chamber pressure is maintained below about 100 kPa during the flowing; and
wetting the plurality of features defined in the substrate.

### Claim 2 (depends on 1)

The method of wetting a semiconductor substrate of claim 1, further comprising:
pressurizing the processing chamber to about atmospheric conditions; and
maintaining the wetting agent in contact with the plurality of features for a period of time subsequent pressurizing the processing chamber.

### Claim 3 (depends on 2)

The method of wetting a semiconductor substrate of claim 2, wherein the period of time is less than about one minute.

### Claim 4 (depends on 1)

The method of wetting a semiconductor substrate of claim 1, wherein the substrate defines at least 1,000 features, and wherein less than 5% of the features contain a bubble defect in the wetting agent.

### Claim 5 (depends on 1)

The method of wetting a semiconductor substrate of claim 1, wherein the carbon dioxide atmosphere is formed by a continuous purge of carbon dioxide, a pump down and backfill of carbon dioxide, a carbon dioxide replacement operation, or by a load lock transfer process into a carbon dioxide environment.

### Claim 6 (depends on 1)

The method of wetting a semiconductor substrate of claim 1, wherein the carbon dioxide atmosphere comprises greater than 50% carbon dioxide.

### Claim 7 (depends on 1)

The method of wetting a semiconductor substrate of claim 1, wherein the plurality of features comprise vias formed in the semiconductor substrate, and wherein at least one via is characterized by a diameter of at least about 20 μm.

### Claim 8 (depends on 1)

The method of wetting a semiconductor substrate of claim 1, wherein the wetting agent comprises degassed deionized water.

### Claim 9 (depends on 8)

The method of wetting a semiconductor substrate of claim 8, wherein the degassed deionized water is degassed below about 20 ppm.

### Claim 10 (depends on 1)

The method of wetting a semiconductor substrate of claim 1, wherein the wetting agent is flowed into the processing chamber by a gravity-induced flow, a forced flow, or a spray.

### Claim 11 (depends on 1)

The method of wetting a semiconductor substrate of claim 1, wherein the chamber pressure is maintained below about 20 kPa during delivery of the wetting agent into the chamber.

### Claim 12 (depends on 1)

The method of wetting a semiconductor substrate of claim 1, wherein the wetting agent absorbs over 98% of carbon dioxide residing in the plurality of features defined by the substrate.

### Claim 13

A method of wetting a semiconductor substrate, the method comprising:
forming a controlled atmosphere in a processing chamber housing the semiconductor substrate, wherein the semiconductor substrate defines a plurality of vias including at least one via characterized by a diameter greater than about 50 μm, and wherein the controlled atmosphere comprises one or more fluids selected from the group consisting of carbon dioxide, carbon monoxide, oxygen, nitrogen, argon, ammonia, bromine, diazene, acetylene, krypton, xenon, radon, nitrous oxide, hydrogen selenide, and hydrocarbons;
reducing a pressure within the processing chamber to below about 10 kPa;
flowing a wetting agent into the processing chamber while maintaining the controlled atmosphere;
pressurizing the processing chamber above about 50 kPa; and
wetting the plurality of vias defined on the semiconductor substrate, wherein less than 1% of the vias contain a defect in the wetting.

### Claim 14 (depends on 13)

The method of wetting a semiconductor substrate of claim 13, wherein the wetting agent comprises water.

### Claim 15 (depends on 13)

The method of wetting a semiconductor substrate of claim 13, wherein, subsequent the pressurizing, the chamber is maintained at a pressure above about 50 kPa for a period of time.

### Claim 16 (depends on 15)

The method of wetting a semiconductor substrate of claim 15, wherein the period of time is between about 1 second and about 20 seconds.

### Claim 17

A method of wetting a substrate, the method comprising:
providing a substrate to a processing chamber, wherein the substrate defines a plurality of features;
displacing air from the plurality of features defined in the substrate, wherein the air is displaced with carbon dioxide;
spraying deionized water into the processing chamber, wherein the deionized water is degassed below about 5 ppm, and wherein the spraying occurs while maintaining a pressure within the processing chamber below about 100 kPa with the carbon dioxide;
pressurizing the processing chamber above about 50 kPa for a period of time; and
wetting the plurality of features defined on the substrate, wherein greater than 99% of the carbon dioxide is removed from the features.

### Claim 18 (depends on 17)

The method of wetting a substrate of claim 17, wherein pressurizing the processing chamber raises the pressure above about 90 kPa.

### Claim 19 (depends on 17)

The method of wetting a substrate of claim 17, wherein the substrate defines over one million features, and wherein less than 0.01% of features of the plurality of features are characterized by a defect comprising a bubble within the deionized water.