# US 8,541,107 B2 · Pigmented polyimide films and methods relating thereto

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- Number: US 8,541,107 B2
- Document ID: US8541107B2
- Status: Granted
- Kind: B2
- Application number: 12/850,739
- Filed: 2010-08-05
- Published: 2011-02-17
- Granted: 2013-09-24
- Earliest claimed: 2009-08-13
- Assignees: E. I. Du Pont de Nemours and Company
- Applicants: Thomas Edward Carney; Jeffrey Michael Bartolin; Meredith L Dunbar; Scott John Herrmann
- Inventors: Thomas Edward Carney; Jeffrey Michael Bartolin; Meredith L Dunbar; Scott John Herrmann
- Web page: https://patentgrep.com/patent/US8541107B2

## CPC

- C09D 179/08: Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08J 5/18: Manufacture of films or sheets
- C09J 7/20: characterised by their carriers
- C09J 7/22: Plastics; Metallised plastics
- C09J 7/35: Heat-activated
- C09J 163/00: Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
- C08J 2379/08: Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08K 3/013: Fillers, pigments or reinforcing additives
- C08K 3/36: Silica
- C09J 2463/00: Presence of epoxy resin
- C09J 2479/086: in the substrate
- Y10T 428/259: Silicic material
- Y10T 428/26: Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
- Y10T 428/28: Web or sheet containing structurally defined element or component and having an adhesive outermost layer
- Y10T 428/287: including epoxy group or epoxy polymer
- Y10T 428/2982: Particulate matter [e.g., sphere, flake, etc.]
- Y10T 428/31511: Of epoxy ether
- Y10T 428/31721: Of polyimide
- C09D: COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D)
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)
- C09J: ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES (preparation of glue or gelatine C09H)
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION

## Abstract

The present disclosure is directed to a base film having a thickness from 8 to 152 microns, a 60 degree gloss value from 2 to 35, an optical density greater than or equal to 2 and a dielectric strength greater than 1400 V/mil. The base film comprises a chemically converted (partially or wholly aromatic) polyimide in an amount from 63 to 96 weight percent of the base film. The base film further comprises a pigment and a matting agent. The matting agent is present in an amount from 1.6 to 10 weight percent of the base film, has a median particle size from 1.3 to 10 microns, and has a density from 2 to 4.5 g/cc. The pigment is present in an amount from 2 to 35 weight percent of the base film. The present disclosure is also directed to coverlay films comprising the base film in combination with an adhesive layer.

## Claims

### Claim 1

A base film comprising:
A. a chemically converted polyimide in an amount from 63 to 96 weight percent of the base film, the chemically converted polyimide being derived from:
a. at least 50 mole percent of an aromatic dianhydride, based upon a total dianhydride content of the polyimide, and
b. at least 50 mole percent of an aromatic diamine based upon a total diamine content of the polyimide;
B. a pigment, other than carbon black, present in an amount from 2 to 35 weight percent of the base film; and
C. a particulate matting agent that:
a. is silica and is present in an amount from 1.6 to 10 weight percent of the base film,
b. has a median particle size from 1.3 to 10 microns,
c. has a density from 2 to 4.5 g/cc,
and the base film has a 60 degree gloss from 2 to 35.

### Claim 2 (depends on 1)

The base film in accordance with claim 1 wherein:
a. the aromatic dianhydride is selected from the group consisting of:
pyromellitic dianhydride,
3,3′,4,4′-biphenyl tetracarboxylic dianhydride,
3,3′,4,4′-benzophenone tetracarboxylic dianhydride,
4,4′-oxydiphthalic anhydride,
3,3′,4,4′-diphenyl sulfone tetracarboxylic dianhydride,
2,2-bis(3,4-dicarboxyphenyl) hexafluoropropane,
bisphenol A dianhydride, and mixtures thereof; and
b. the aromatic diamine is selected from the group consisting of:
3,4′-oxydianiline,
1,3-bis-(4-aminophenoxy) benzene,
4,4′-oxydianiline,
1,4-diaminobenzene,
1,3-diaminobenzene,
2,2′-bis(trifluoromethyl) benzidene,
4,4′-diaminobiphenyl,
4,4′-diaminodiphenyl sulfide,
9,9′-bis(4-amino)fluorine and mixtures thereof.

### Claim 3 (depends on 1)

The base film in accordance with claim 1 wherein the chemically converted polyimide is derived from pyromellitic dianhydride and 4,4′-oxydianiline.

### Claim 4 (depends on 1)

A multilayer film comprising the base film of claim 1 and an adhesive layer.

### Claim 5 (depends on 4)

The multilayer film in accordance with claim 4, wherein the adhesive layer is an epoxy resin selected from the group consisting of:
bisphenol A epoxy resin, cresol novolac epoxy resin, phosphorus containing epoxy resin, and mixtures thereof.

### Claim 6 (depends on 4)

The multilayer film in accordance with claim 4, wherein the multilayer film is a coverlay film.

### Claim 7 (depends on 1)

The base film in accordance with claim 1, wherein the base film has a thickness from 8 to 152 microns.

### Claim 8 (depends on 1)

The base film in accordance with claim 1, wherein the chemically converted polyimide is created by a chemical conversion process that includes the use of a tertiary amine.

### Claim 9 (depends on 8)

The base film in accordance with claim 8, wherein the tertiary amine used in the chemical conversion process is pyridine.

### Claim 10 (depends on 8)

The base film in accordance with claim 8, wherein the tertiary amine used in the chemical conversion process is beta-picoline.

### Claim 11 (depends on 1)

The base film in accordance with claim 1, wherein the chemically converted polyimide is created by a chemical conversion process that includes the use of an anhydride dehydrating material.

### Claim 12 (depends on 11)

The base film in accordance with claim 11, wherein the anhydride dehydrating material used in the chemical conversion process is acetic anhydride.

### Claim 13 (depends on 1)

The base film in accordance with claim 1, wherein the base film has a 60 degree gloss from 10 to 35.

### Claim 14 (depends on 1)

The base film in accordance with claim 1, wherein the base film has an optical density greater than or equal to 2.

### Claim 15 (depends on 1)

The base film in accordance with claim 1, wherein the base film has a dielectric strength greater than 1400 V/mil.

### Claim 16 (depends on 1)

The base film in accordance with claim 1, wherein the pigment is present in an amount from 15 to 35 weight percent of the polyimide film.

### Claim 17

A base film comprising:
A. a chemically converted polyimide in an amount from 63 to 96 weight percent of the base film, the chemically converted polyimide being derived from:
a. at least 50 mole percent of an aromatic dianhydride, based upon a total dianhydride content of the polyimide, and
b. at least 50 mole percent of an aromatic diamine based upon a total diamine content of the polyimide;
B. a dye present in an amount from 2 to 35 weight percent of the base film; and
C. a particulate matting agent, providing the base film with a 60 degree gloss from 2 to 35, that:
a. is silica and is present in an amount from 1.6 to 10 weight percent of the base film,
b. has a median particle size from 1.3 to 10 microns, and
c. has a density from 2 to 4.5 g/cc.

### Claim 18 (depends on 17)

The base film in accordance with claim 17, wherein the dye is present in an amount from 15 to 35 weight percent of the polyimide film.