# US 7,745,352 B2 · Curing methods for silicon dioxide thin films deposited from alkoxysilane precursor with harp II process

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- Number: US 7,745,352 B2
- Document ID: US7745352B2
- Status: Granted
- Kind: B2
- Application number: 11/845,445
- Filed: 2007-08-27
- Published: 2009-03-05
- Granted: 2010-06-29
- Earliest claimed: 2007-08-27
- Assignees: Applied Materials, Inc.
- Inventors: Abhijit Basu Mallick; Srinivas D. Nemani; Timothy W. Weidman
- Web page: https://patentgrep.com/patent/US7745352B2

## CPC

- H10P 14/6529: {by exposure to a gas or vapour}
- H10P 95/00: Generic processes or apparatus for manufacture or treatments not covered by the other groups of this subclass
- H10P 14/6336: {in the presence of a plasma [PECVD]}
- H10P 14/6339: {deposition by cyclic CVD, e.g. ALD, ALE or pulsed CVD}
- H10P 14/6686: {the compound being a molecule comprising at least one silicon-oxygen bond and the compound having hydrogen or an organic group attached to the silicon or oxygen, e.g. a siloxane}
- H10P 14/69215: {the material being a silicon oxide, e.g. SiO2}
- H10P 14/6922: {the material containing Si, O and at least one of H, N, C, F or other non-metal elements, e.g. SiOC, SiOC:H or SiONC}
- H10P 14/6939: {characterised by the metal}
- H10P 14/69392: {the material containing hafnium, e.g. HfO2}
- H10P 14/69395: {the material containing zirconium, e.g. ZrO2}
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10

## Abstract

Methods of curing a silicon oxide layer on a substrate are provided. The methods may include the processes of providing a semiconductor processing chamber and a substrate and forming an silicon oxide layer overlying at least a portion of the substrate, the silicon oxide layer including carbon species as a byproduct of formation. The methods may also include introducing an acidic vapor into the semiconductor processing chamber, the acidic vapor reacting with the silicon oxide layer to remove the carbon species from the silicon oxide layer. The methods may also include removing the acidic vapor from the semiconductor processing chamber. Systems to deposit a silicon oxide layer on a substrate are also described.

## Claims

### Claim 1

A method of curing a silicon oxide layer on a substrate, the method comprising:
providing a semiconductor processing chamber and a substrate;
forming a silicon oxide layer overlying at least a portion of the substrate the silicon oxide layer including carbon species as a byproduct of formation;
introducing an acidic vapor into the semiconductor processing chamber after forming the silicon oxide layer, the acidic vapor reacting with the silicon oxide layer, wherein the reaction between the acidic vapor and the silicon oxide layer removes the carbon species from the silicon oxide layer; and
removing the acidic vapor from the semiconductor processing chamber.

### Claim 2 (depends on 1)

The method of claim 1 wherein the silicon oxide layer is deposited using an alkoxysilane process.

### Claim 3 (depends on 1)

The method of claim 1 wherein the silicon oxide layer is deposited using a plasma CVD process.

### Claim 4 (depends on 1)

The method of claim 1 wherein introducing an acidic vapor further comprises flowing HCl gas into the semiconductor processing chamber.

### Claim 5 (depends on 4)

The method of claim 4 wherein the HCl gas is flowed with a siloxane precursor.

### Claim 6 (depends on 1)

The method of claim 1 wherein introducing an acidic vapor further comprises in situ generation of HCl or CH3COOH.

### Claim 7 (depends on 6)

The method of claim 6 wherein the in situ generation of HCl or CH3COOH is performed using chloro-silaxane or acetoxy-siloxane.

### Claim 8 (depends on 7)

The method of claim 7 wherein the chloro-siloxane is selected from the group comprising dichlorodiethoxysiloxane or chlorotriethoxysiloxane.

### Claim 9 (depends on 7)

The method of claim 7 wherein the acetoxy-siloxane is diacetoxydi-tert-butylsilane.

### Claim 10 (depends on 1)

The method of claim 1 wherein the acidic vapor catalyzes the removal of an alkoxyl group from an organo-silicon compound in the silicon oxide layer to leave a silanol moiety.

### Claim 11 (depends on 1)

The method of claim 1 wherein the vapor is a mixture of acid and water having a water to acid ratio.

### Claim 12 (depends on 1)

The method of claim 1 wherein the water to acid ratio is about 100:1 to about 1:100.

### Claim 13 (depends on 1)

The method of claim 1 wherein the reaction between the acidic vapor and silicon oxide layer is performed between 10 mTorr to atmospheric pressure.

### Claim 14 (depends on 1)

The method of claim 1 wherein the reaction between the acidic vapor and silicon oxide layer is performed between 60 degrees C. to 600 degrees C.

### Claim 15 (depends on 1)

The method of claim 1 wherein the silicon oxide layer is exposed to the acidic vapor for a period between 1 second and 24 hours.

### Claim 16 (depends on 1)

The method of claim 1 wherein a plurality of structures are formed on a surface of the substrate wherein the structures include gaps and trenches having height to width aspect rations of 7:1 or more.

### Claim 17 (depends on 1)

The method of claim 1 wherein the initially formed silicon oxide layer that includes the carbon species is a flowable silicon oxide layer.

### Claim 18 (depends on 1)

The method of claim 1 further comprising annealing the silicon oxide layer subsequent to the introduction of the acidic vapor into the semiconductor processing chamber in order to increase density of the silicon oxide layer.

### Claim 19 (depends on 10)

The method of claim 10, wherein the silanol moiety reacts with other silanol moieties present in the silicon oxide layer to form a silicon oxide network.