# US 8,541,053 B2 · Enhanced densification of silicon oxide layers

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- Number: US 8,541,053 B2
- Document ID: US8541053B2
- Status: Granted
- Kind: B2
- Application number: 13/178,057
- Filed: 2011-07-07
- Published: 2012-01-12
- Granted: 2013-09-24
- Earliest claimed: 2010-07-08
- Assignees: Molecular Imprints, Inc.
- Applicants: Marlon Menezes; Frank Y. Xu; Fen Wan
- Inventors: Marlon Menezes; Frank Y. Xu; Fen Wan
- Web page: https://patentgrep.com/patent/US8541053B2

## CPC

- G03F 7/0002: {Lithographic processes using patterning methods other than those involving the exposure to radiation, e.g. by stamping}
- B82Y 10/00: Nanotechnology for information processing, storage or transmission, e.g. quantum computing or single electron logic
- B82Y 40/00: Manufacture or treatment of nanostructures
- H10P 95/00: Generic processes or apparatus for manufacture or treatments not covered by the other groups of this subclass
- Y10T 428/249953: Composite having voids in a component [e.g., porous, cellular, etc.]
- G03F: PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR; (phototypographic composing devices B41B; photosensitive materials or processes for photographic purposes G03C; electrophotography, sensitive layers or processes therefor G03G)
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
- Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION

## Abstract

Densifying a multi-layer substrate includes providing a substrate with a first dielectric layer on a surface of the substrate. The first dielectric layer includes a multiplicity of pores. Water is introduced into the pores of the first dielectric layer to form a water-containing dielectric layer. A second dielectric layer is provided on the surface of the water-containing first dielectric layer. The first and second dielectric layers are annealed at temperature of 600° C. or less. In an example, the multi-layer substrate is a nanoimprint lithography template. The second dielectric layer may have a density and therefore an etch rate similar to that of thermal oxide, yet may still be porous enough to allow more rapid diffusion of helium than a thermal oxide layer.

## Claims

### Claim 1

A method comprising:
providing a substrate with a first dielectric layer, wherein the first dielectric layer defines a multiplicity of water-containing pores and wherein providing the substrate with the first dielectric layer further comprises forming the first dielectric layer on the substrate and contacting the first dielectric layer with a fluid comprising water;
providing a second dielectric layer on the water-containing first dielectric layer; and
steam annealing the first and second dielectric layers at a temperature of 600° C. or less.

### Claim 2 (depends on 1)

The method of claim 1, wherein the substrate is impermeable to water.

### Claim 3 (depends on 1)

The method of claim 1, wherein steam annealing the first and second dielectric layers at a temperature of 600° C. or less increases the density of the first dielectric layer and the second dielectric layer.

### Claim 4 (depends on 1)

The method of claim 1, wherein before steam annealing, the first dielectric layer comprises SiOx, wherein x≠2.

### Claim 5 (depends on 1)

The method of claim 1, wherein the first dielectric layer comprises a silicon-containing polymer.

### Claim 6 (depends on 1)

The method of claim 1, wherein providing the second dielectric layer on the first dielectric layer comprises a chemical vapor deposition process or a spin coating process.

### Claim 7 (depends on 6)

The method of claim 6, wherein providing the second dielectric layer on the first dielectric layer comprises a spin coating process, and the spin coating process comprises spin coating a polysilazane film or a spin-on-glass film on the water-containing first dielectric layer.

### Claim 8 (depends on 1)

The method of claim 1, wherein a ratio of an etch rate of the second dielectric layer after annealing to an etch rate of thermal oxide is between 1:1 and 1.25:1.

### Claim 9 (depends on 1)

The method of claim 1, wherein forming the first dielectric layer on the substrate comprises a spin coating process or a chemical vapor deposition process.

### Claim 10 (depends on 1)

The method of claim 1, wherein the fluid is a vapor or a liquid.

### Claim 11 (depends on 1)

The method of claim 1, wherein contacting the first dielectric layer with a fluid comprising water comprises chemical mechanical planarization of the first dielectric layer.

### Claim 12 (depends on 1)

The method of claim 1, wherein contacting the first dielectric layer with a fluid comprising water comprises contacting the first dielectric layer with an aqueous solution or water.

### Claim 13 (depends on 1)

A device fabricated by the method of claim 1.

### Claim 14

A method of fabricating an imprint lithography template, the method comprising:
providing a fused silica substrate with a porous layer, wherein the porous layer defines a multiplicity of water-containing pores and wherein providing the fused silica substrate with the porous layer further comprises forming the porous layer on the fused silica substrate and contacting the porous layer with a fluid comprising water;
providing a cap layer on the water-containing porous layer; and
steam annealing the porous layer and the cap layer at a temperature of 600° C. or less to increase a density of the cap layer.

### Claim 15 (depends on 14)

The method of claim 14, wherein providing the cap layer on the water-containing porous layer comprises spin-coating a polymerizable material on the water-containing porous layer.

### Claim 16 (depends on 15)

The method of claim 15, further comprising patterning the polymerizable material to form a patterned cap layer on the water-containing porous layer.

### Claim 17 (depends on 15)

The method of claim 15, further comprising pre-baking the polymerizable material before steam annealing the porous layer and the cap layer.

### Claim 18 (depends on 14)

An imprint lithography template fabricated by the method of claim 14.