US4543295A — High temperature polyimide film laminates and pro…

Claim 1

Independent Claim 95 words

A process for laminating high temperature resistant polyimide film comprising the steps of: providing at least two layers of a thin polyimide film; providing at least one layer of polyimide adhesive on one of said at least two layers of polyimide film; assembling said two layers of polyimide film to form a sandwich; said polyimide adhesive layer being a polyamic acid that is imidized to the polyimide state prior to assembling of the polyimide film sandwich; and subjecting the film-adhesive sandwich to heat and pressure to thermoplastically bond the sandwich into a void-free laminate structure.

Claim 2

Dependent Claim 95 words

A process for laminating high temperature resistant polyimide film comprising the steps of: providing at least two layers of a thin polyimide film; providing at least one layer of polyimide adhesive on one of said at least two layers of polyimide film; assembling said two layers of polyimide film to form a sandwich; said polyimide adhesive layer being a polyamic acid that is imidized to the polyimide state prior to assembling of the polyimide film sandwich; and subjecting the film-adhesive sandwich to heat and pressure to thermoplastically bond the sandwich into a void-free laminate structure.

Claim 3

Dependent Claim 44 words

The process of claim 1 wherein the polyimide adhesive is in liquid form and is coated on only one layer of polyimide film and this coated layer is heated to an elevated temperature to imidize the adhesive layer prior to assembly of the sandwich.

Claim 4

Dependent Claim 79 words

The process of claim 2 wherein the coating adhesive and polyimide film layers are subjected to low humidity environment for fifteen minutes and thereafter heated in a forced air oven for one-half hour at 373 K.; heated to and maintained for one hour at 493 K.; cooled to 373 K. prior to being removed from the oven and permitted to cool to room temperature to yield an imidized adhesive film on the polyimide film of approximately 0.5 mil thickness.

Claim 5

Dependent Claim 28 words

The process of claim 1 wherein a film of polyimide adhesive is prepared and imidized prior to being positioned on one of the layers of the polyimide film.

Claim 6

Dependent Claim 99 words

The process of claim 3 including: providing a steel pressure mold; spraying a thin layer of a release agent on the mold surface; preheating the steel press platens to 505 K.; inserting the polyimide film-adhesive sandwich between the press platens and applying a pressure in the range of 50-300 psi thereto; heating the press platens to 616 K. and maintaining this temperature and pressure for five minutes; cease heating and permit cooling to 373 K.; removing the imidized sandwich from the pressure mold and permitting it to cool to room temperature to recover a clear flexible void-free laminate structure.

Claim 7

Dependent Claim 99 words

The process of claim 4 including: providing a steel pressure mold; spraying a thin layer of a release agent on the mold surface; preheating the steel press platens to 505 K.; inserting the polyimide film-adhesive sandwich between the press platens and applying a pressure in the range of 50-300 psi thereto; heating the press platens to 616 K. and maintaining this temperature and pressure for five minutes; cease heating and permit cooling to 373 K.; removing the imidized sandwich from the pressure mold and permitting it to cool to room temperature to recover a clear flexible void-free laminate structure.

Claim 8

Dependent Claim 37 words

The method of claim 1 wherein the polyimide film layers are selected from the group consisting of polyimides formed as the reaction product of (a) pyromellitic dianhydride and 4,4'-oxydianiline and (b) 3,3', 4,4'-benzophenone tetracarboxylic dianhydride and 4,4'-oxydianiline.

Claim 9

Dependent Claim 85 words

The method of claim 1 wherein the polyimide adhesives are selected from the adhesive group consisting of the reaction product of (a) 3,3', 4,4'-benzophenone tetracarboxylic dianhydride and 3,3' dianimohenzophenone, (b) two parts 3,3', 4,4'-benzophenone tetracarboxylic dianhydride plus one part pyromellitic dianhydride and 3,3'-diaminohenzophenone, and (c) three parts 3,3', 4,4'-benzophenone tetracarboxylic dianhydride plus one part pryomellitic dianhydride and 4,4'-diaminohenzophenone, with the members of each group being employed in a concentration of approximately 15% solids in one member of the solvent group consisting of N,N'-dimethylacetamide and bis(2-methoxyethyl)ether.

Claim 10

Dependent Claim 38 words

The process of claim 1 wherein a layer of conductive metal film is also provided between each two layers of polyimide film and a layer of polyimide adhesive is provided adjacent each surface of the metal film layer.

Claim 11

Dependent Claim 44 words

The process of claim 9 wherein the metal film layer is selected from the group consisting of aluminum, brass, copper, chromium, titanium, stainless steel and alloys thereof, and each member of the group being in the thickness range of 1 mil to 30 mil.

Claim 12

Dependent Claim 118 words

A process for laminating high-temperature polyimide film and metal foil comprising the steps of: providing at least two layers of thin polyimide film; providing a metal foil layer between two layers of the polyimide film; providing a thermoplastic polyimide adhesive layer between each surface of the metal foil layer and the adjacent polyimide film layer; assembling the polyimide film, metal foil and adhesive so as to give film-adhesive-metal-adhesive-film sandwich; said polyimide adhesive layer being a polyamic acid that is imidized to remove its solvent and converted to the polyimide state prior to the step of assembling the sandwich; and subjecting the sandwich assembly to heat and pressure to thermally bond the sandwiched assembly into a void-free laminate structure.

Claim 13

Dependent Claim 118 words

A process for laminating high-temperature polyimide film and metal foil comprising the steps of: providing at least two layers of thin polyimide film; providing a metal foil layer between two layers of the polyimide film; providing a thermoplastic polyimide adhesive layer between each surface of the metal foil layer and the adjacent polyimide film layer; assembling the polyimide film, metal foil and adhesive so as to give film-adhesive-metal-adhesive-film sandwich; said polyimide adhesive layer being a polyamic acid that is imidized to remove its solvent and converted to the polyimide state prior to the step of assembling the sandwich; and subjecting the sandwich assembly to heat and pressure to thermally bond the sandwiched assembly into a void-free laminate structure.

Claim 14

Dependent Claim 31 words

The process as in claim 11 wherein the metal foil layer is selected from the group of metal foils consisting of copper, stainless steel, chromium, titanium, aluminum, brass and alloys thereof.

Claim 15

Dependent Claim 28 words

The process of claim 11 wherein the polyimide adhesive is applied to the laminate surfaces in liquid form and consists of a polyamic acid dissolved in a solvent.

Claim 16

Dependent Claim 21 words

The process of claim 11 wherein the polyimide adhesive is a thin film of a polyimide that has been previously imidized.

Claim 17

Dependent Claim 67 words

The process of claim 11 wherein the polyimide adhesive is a linear polyamic acid adhesive solution selected from the group consisting of: (a) 3,3', 4,4'-benzophenone tetracarboxylic dianhydride and 3,3' diaminohenzophenone; (b) two parts 3,3', 4,4'-benzophenone tetracarboxylic dianhydride to one part pyromellitic dianhydride and 3,3'-diaminohenzophenone; and (c) three parts 3,3', 4,4'-benzophenone tetracarboxylic dianhydride to one part pyromellitic dianhydride and 4,4'-diaminohenzophenone, each group member being dissolved in a solvent.

Claim 18

Dependent Claim 33 words

The process of claim 15 wherein the adhesive solid concentration is approximately 15% and the solvent is selected from the group consisting of N,N'-dimethylacetamide, bis(2-methoxyethyl)ether, N,N-dimethylformamide, N-methyl-2-pyrrolidone, dimethylsulfoxide, tetrahydrofuran, m-dioxane, p-dioxane and 1,2-bis(2-methoxyethoxy)ethane.

Claim 19

Dependent Claim 55 words

The process of claim 15 wherein the solvent is N,N'-dimethylacetamide and the adhesive is imidized prior to lamination by applying a thin layer of the liquid adhesive to a smooth surface and heating to approximately 493° F. in air and maintaining this temperature for approximately one hour to recover a thin film of polyimide adhesive.

Claim 20

Dependent Claim 78 words

The process of claim 15 wherein the solvent is bis(2-methoxyethyl)ether and the adhesive is imidized by applying a thin coat of the liquid adhesive onto a smooth surface and heating in air to approximately 373° F. and maintaining this temperature for approximately one-half hour, increasing and maintaining the temperature to 453° F. for approximately one hour and further increasing and maintaining the temperature to 493° F. for an additional hour to recover a thin film of polyimide adhesive.

Claim 21

Dependent Claim 93 words

A process for forming a laminate structure including the steps of: providing at least one layer of a thin polyimide film; providing at least one layer of a thin metal film; forming a layer of polyimide adhesive by forming a layer of polyamic acid and imidizing said layer of polyamic acid to form said layer of polyimide adhesive; positioning said layers of polyimide film and metal with said layer of polyimide adhesive therebetween; and bonding said layers of polyimide film and metal together under heat and pressure to form a substantially void-free laminate.

Claim 22

Dependent Claim 93 words

A process for forming a laminate structure including the steps of: providing at least one layer of a thin polyimide film; providing at least one layer of a thin metal film; forming a layer of polyimide adhesive by forming a layer of polyamic acid and imidizing said layer of polyamic acid to form said layer of polyimide adhesive; positioning said layers of polyimide film and metal with said layer of polyimide adhesive therebetween; and bonding said layers of polyimide film and metal together under heat and pressure to form a substantially void-free laminate.

Claim 23

Dependent Claim 53 words

The process of claim 19 wherein said step of forming a layer of polyimide adhesive includes: applying a layer of polyamic acid dissolved in a solvent to one surface of a layer to be laminated; and heating said layer of polyamic acid to imidize said layer to form said layer of polyimide adhesive.

Claim 24

Dependent Claim 19 words

The process of claim 20 wherein: said layer of polyamic acid is applied to said layer of polyimide film.

Claim 25

Dependent Claim 46 words

The process of claim 19 wherein said step of forming a layer of polyimide adhesive includes: forming a layer of polyamic acid on a support surface, heating said polyamic acid layer to form a layer of polyimide film, and removing said polyimide film from said support.

Claim 26

Dependent Claim 32 words

The process of claim 19 wherein said step of bonding includes: placing said layers of polyimide film, polyimide adhesive and metal in a press and subjecting said layers to heat and pressure.

Claim 27

Dependent Claim 66 words

The process of claim 23 wherein the polyimide adhesive is a linear polyamic acid adhesive solution selected from the group consisting of: (a) 3,3', 4,4'-benzophenone tetracarboxylic dianhydride and 3,3'-diaminohenzophenone; (b) two parts 3,3', 4,4'-benzophenone tetracarboxylic dianhydride to one part pyromellitic dianhydride and 3,3'-dianimohenzophenone; and (c) three parts 3,3', 4,4'-benzophenone tetracarboxylic dianhydride to one part pyromellitic dianhydride and 4,4'-diaminohenzophenone, each group member being dissolved in a solvent.

Claim 28

Dependent Claim 92 words

A laminate of high temperature resistant polyimide film comprising of: at least two layers of a thin polyimide film; and at least one layer of polyimide adhesive between said at least two layers of polyimide film; said two layers of polyimide film and said layer of adhesive forming a sandwich; said polyimide adhesive layer being a polyamic acid imidized to the polyimide state prior to assembling of the polyimide film sandwich; and said film-adhesive sandwich having been formed by heat and pressure to thermoplastically bond the sandwich into a void-free laminate structure.

Claim 29

Dependent Claim 92 words

A laminate of high temperature resistant polyimide film comprising of: at least two layers of a thin polyimide film; and at least one layer of polyimide adhesive between said at least two layers of polyimide film; said two layers of polyimide film and said layer of adhesive forming a sandwich; said polyimide adhesive layer being a polyamic acid imidized to the polyimide state prior to assembling of the polyimide film sandwich; and said film-adhesive sandwich having been formed by heat and pressure to thermoplastically bond the sandwich into a void-free laminate structure.

Claim 30

Dependent Claim 44 words

The laminate process of claim 25 wherein: said polyimide adhesive is coated on only one layer of polyimide film as a polyamic acid and this coated layer is heated to an elevated temperature to imidize the adhesive layer prior to assembly of the sandwich.

Claim 31

Dependent Claim 33 words

The laminate of claim 25 wherein: said layer of polyimide adhesive is prepared and imidized to form a free film prior to being positioned on one of the layers of the polyimide film.

Claim 32

Dependent Claim 37 words

The laminate of claim 25 wherein: the polyimide film layers are selected from the group consisting of polyimides formed as the reaction product of (a) pyromellitic dianhydride and 4,4'-oxydianiline and (b) 3,3', 4,4'-benzophenone tetracarboxylic dianhydride and 4,4'-oxydianiline.

Claim 33

Dependent Claim 57 words

The laminate of claim 25 wherein the polyimide adhesives are selected from the adhesive group consisting of the reaction product of (a) 3,3', 4,4'-benzophenone tetracarboxylic dianhydride and 3,3'-diaminohenzophenone, (b) two parts 3,3', 4,4'-benzophenone tetracarboxylic dianhydride plus one part pyromellitic dianhydride and 3,3'-diaminohenzophenone, and (c) three parts 3,3', 4,4'-benzophenone tetracarboxylic dianhydride plus one part pyromellitic dianhydride and 4,4'-diaminohenzophenone.

Claim 34

Dependent Claim 33 words

The laminate of claim 25 including: a layer of conductive metal film between each two layers of polyimide film and a layer of polyimide adhesive adjacent each surface of the metal film layer.

Claim 35

Dependent Claim 43 words

The laminate of claim 30 wherein the metal film layer is selected from the group consisting of aluminum, brass, chromium, titanium, copper, stainless steel and alloys thereof, each member of the group being in the thickness range of 1 mil to 30 mil.

Claim 36

Dependent Claim 108 words

A laminate of high-temperature polyimide film and metal foil comprising of: at least two layers of thin polyimide film; a metal foil layer between said two layers of polyimide film; a thermoplastic polyimide adhesive layer between each surface of the metal foil layer and the adjacent polyimide film layer; the polyimide film, metal foil and adhesive being assembled to form a film-adhesive-metal-adhesive-film sandwich; said polyimide adhesive layer being formed from a polyamic acid imidized to remove its solvent and converted to the polyimide state prior to being assembled in the sandwich; and said sandwich assembly being bonded together under heat and pressure to form a void-free laminate structure.

Claim 37

Dependent Claim 108 words

A laminate of high-temperature polyimide film and metal foil comprising of: at least two layers of thin polyimide film; a metal foil layer between said two layers of polyimide film; a thermoplastic polyimide adhesive layer between each surface of the metal foil layer and the adjacent polyimide film layer; the polyimide film, metal foil and adhesive being assembled to form a film-adhesive-metal-adhesive-film sandwich; said polyimide adhesive layer being formed from a polyamic acid imidized to remove its solvent and converted to the polyimide state prior to being assembled in the sandwich; and said sandwich assembly being bonded together under heat and pressure to form a void-free laminate structure.

Claim 38

Dependent Claim 30 words

The laminate of claim 32 wherein the metal foil layer is selected from the group of metal foils consisting of copper, stainless steel, chromium, titanium, aluminum, brass, and alloys thereof.

Claim 39

Dependent Claim 28 words

The laminate of claim 32 wherein the polyimide adhesive is applied to the laminate surfaces in liquid form and consists of a polyamic acid dissolved in a solvent.

Claim 40

Dependent Claim 26 words

The laminate of claim 34 wherein the polyimide adhesive is a thin film of a polyimide that has been imidized prior to inclusion in the sandwich.

Claim 41

Dependent Claim 70 words

The laminate of claim 32 wherein the polyimide adhesive is a linear polyamic acid adhesive solution selected from the group consisting of the reaction products of: (a) 3,3', 4,4'-benzophenone tetracarboxylic dianhydride and 3,3'-diaminohenzophenone; (b) two parts 3,3', 4,4'-benzophenone tetracarboxylic dianhydride to one part pyromellitic dianhydride and 3,3'-diaminohenzophenone; and (c) three parts 3,3', 4,4'-benzophenone tetracarboxylic dianhydride to one part pyromellitic dianhydride and 4,4'-diaminohenzophenone, each group member being dissolved in a solvent.

Claim 42

Dependent Claim 33 words

The laminate of claim 36 wherein the adhesive solid concentration is approximately 15% and the solvent is selected from the group consisting of N,N'-dimethylacetamide, bis(2-methoxyethyl)ether, N,N-dimethylformamide, N-methyl-2-pyrrolidone, dimethylsulfoxide, tetrahydrofuran, m-dioxane, p-dioxane and 1,2-bis(2-methoxyethoxy)ethane.

Claim 43

Dependent Claim 82 words

A laminate of polyimide film and metal including: at least one layer of a thin polyimide film; at least on layer of a thin metallic film; and a layer of polyimide adhesive between said layer of polyimide film and said layer of metallic film; said layers having been bonded together by heat and pressure to form a substantially void-free laminate, and said layer of polyimide adhesive having been formed by imidizing a layer of polyamic acid prior to bonding said layers together.

Claim 44

Dependent Claim 82 words

A laminate of polyimide film and metal including: at least one layer of a thin polyimide film; at least on layer of a thin metallic film; and a layer of polyimide adhesive between said layer of polyimide film and said layer of metallic film; said layers having been bonded together by heat and pressure to form a substantially void-free laminate, and said layer of polyimide adhesive having been formed by imidizing a layer of polyamic acid prior to bonding said layers together.

Claim 45

Dependent Claim 48 words

A laminate as in claim 38 wherein: said layer of polyimide adhesive was formed by applying a layer of polyamic acid to one of said polyimide film or said metallic film and heating said layer of polyamic acid to imidize said layer to form said layer of polyimide.

Claim 46

Dependent Claim 20 words

A laminate as in claim 39 wherein: said layer of polyamic acid was applied to said layer of polyimide film.

Claim 47

Dependent Claim 38 words

A laminate as in claim 38 wherein: said layer of polyimide adhesive was formed as a free film by forming a layer of polyamic acid and heating said layer of polyamic acid to form said layer of polyimide.

Claim 48

Dependent Claim 65 words

A laminate as in claim 38 wherein: said polyimide adhesive is selected from the group consisting of the reaction products of: (a) 3,3', 4,4'-benzophenone tetracarboxylic dianhydride and 3,3'-diaminohenzophenone; (b) two parts 3,3', 4,4'-benzophenone tetracarboxylic dianhydride to one part pyromellitic dianhydride and 3,3'-diaminohenzophenone; and (c) three parts 3,3', 4,4'-benzophenone tetracarboxylic dianydride to one part pyromellitic dianhydride and 4,4'-dianimohenzophenone, each group member being dissolved in a solvent.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1988-09-23	1989-03-25	1989-09-24	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1992-09-23	1993-03-25	1993-09-24	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1996-09-23	1997-03-25	1997-09-24	$7700.00	Window Closed / Lapsed

High temperature polyimide film laminates and process for preparation thereof

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