# US 5,707,681 A · Method of producing coatings on electronic substrates

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- Number: US 5,707,681 A
- Document ID: US5707681A
- Status: Granted
- Kind: A
- Application number: 08/798,405
- Filed: 1997-02-07
- Granted: 1998-01-13
- Earliest claimed: 1997-02-07
- Assignees: Dow Corning Corporation
- Inventors: Jeffrey Nicholas Bremmer; Youfan Liu
- Web page: https://patentgrep.com/patent/US5707681A

## CPC

- H10P 14/6925: {the material comprising hydrogen silsesquioxane, e.g. HSQ}
- B05D 3/0254: {After-treatment}
- H10P 14/6342: {Liquid deposition, e.g. spin-coating, sol-gel techniques or spray coating}
- 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 14/6922: {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}
- Y02P 20/10: Process efficiency
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
- B05D: PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL (conveying articles or workpieces through baths of liquid B65G, e.g. B65G49/02)
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

This invention pertains to a method for producing an insoluble coating on a substrate by curing a composition comprising hydrogen silsesquioxane at a temperature of 375.degree. C. or less for a time sufficient to produce a coating having >80% SiH. It has been found that when the hydrogen silsesquioxane resin is cured at a temperature of 375.degree. C. or less that that the insoluble SiH containing coating shows improved film stress.

## Claims

### Claim 1

A method of forming an insoluble coating on a substrate wherein said method comprises
(A) coating the substrate with a coating composition comprising a soluble hydrogen silsesquioxane resin having silicon-bonded hydrogen to form a soluble hydrogen silsesquioxane resin coating on the substrate;
(B) heating the soluble hydrogen silsesquioxane resin coating to a temperature of 375.degree. C. or less for a period of time sufficient to convert the hydrogen silsesquioxane resin coating into an insoluble final coating retaining in the insoluble final coating >80% of the silicon-bonded hydrogen from the soluble hydrogen silsesquioxane resin.

### Claim 2 (depends on 1)

The method as claimed in claim 1 wherein the coating composition additionally comprises a solvent and the solvent is evaporated to form the hydrogen silsesquioxane resin coating on the substrate.

### Claim 3 (depends on 2)

The method as claimed in claim 2 wherein the coating composition contains from 20 to 99.9 weight % solvent based on the weight of the coating composition.

### Claim 4 (depends on 2)

The method as claimed in claim 2 wherein the solvent is selected from the group consisting of alcohols, aromatic hydrocarbons, alkanes, ketones, esters, glycol ethers, and dimethylpolysiloxanes.

### Claim 5 (depends on 1)

The method as claimed in claim 1 wherein the hydrogen silsesquioxane resin is a resin having units of the formula HSi(OH).sub.x (OR).sub.y O.sub.z/2, in which each R is independently an organic group or a substituted organic group which, when bonded to silicon through the oxygen atom, forms a hydrolyzable substituent, wherein x=0 to 2, y=0 to 2, z=1 to 3, and x+y+z=3.

### Claim 6 (depends on 1)

The method as claimed in claim 1 wherein the hydrogen silsesquioxane resin is a resin having the formula (HSiO.sub.3/2).sub.n wherein n is an integer having a value of at least 8.

### Claim 7 (depends on 1)

The method as claimed in claim 1 wherein the coating composition further comprises a catalyst containing an element selected from the group consisting of platinum, rhodium and copper.

### Claim 8

The method as claimed in 7 wherein the catalyst is present in an amount sufficient to provide 5 to 1000 ppm platinum, rhodium or copper based on the weight of the hydrogen silsesquioxane resin.

### Claim 9 (depends on 1)

The method as claimed in claim 1 wherein the coating composition further contains a ceramic oxide precursor comprising a compound containing an element selected from the group consisting of aluminum, titanium, zirconium, tantalum, niobium, vanadium, boron and phosphorous and wherein the compound contains at least one hydrolyzable substituent selected from the group consisting of alkoxy and acyloxy and the compound is present in an amount such that the coating composition contains from 0.1 to 30 weight % of the ceramic oxide precursor based on the weight of hydrogen silsesquioxane resin.

### Claim 10 (depends on 1)

The method as claimed in claim 1 wherein the substrate is coated by spin coating.

### Claim 11 (depends on 1)

The method as claimed in claim 1 wherein the substrate is an electronic substrate.

### Claim 12 (depends on 1)

The method as claimed in claim 1 wherein the hydrogen silsesquioxane resin coating is heated to a temperature of 350.degree. C.

### Claim 13 (depends on 1)

The method as claimed in claim 1 wherein the coating produce in (B) contains .gtoreq.8% silicon-bonded hydrogen.