JPH03182583A - High performance cover lay and bond-ply adhesive agent having thermal activation type hardening mechanism based on epoxy - Google Patents

Abstract

PURPOSE: To obtain an improved material that can be used for bonding electronic circuit materials by subjecting an aziridine component and a polyester component to a first reaction between them and then subjecting the obtained aziridine/polyester component and an epoxy component to a second reaction between them.

CONSTITUTION: An aziridine component is reacted with one or more polyester compounds (first reaction step). The aziridine/polyester component obtained in the first reaction step is reacted with one or more trismethanenovolac-epoxy components (second reaction step). One of the above epoxy components is an electronic grade resin, such as a trismethanenovolac-epoxy component, the temperature in the above second reaction is required to be as high as 250 to 400 °F, and thus an improved adhesive that can be used for bonding electronic circuit materials can be obtained. Further, the intermediate bonding material obtained in the first reaction step can be stored for a long period of time without deteriorating the properties.

COPYRIGHT: (C)1991,JPO

Description

DETAILED DESCRIPTION OF THE INVENTION The rapid development of the electronic circuit industry over the past 25 years has also facilitated the development of high performance construction materials. however,
The development of high performance construction materials has not led to the development of high performance adhesive materials and systems that can bond these construction materials together in the harsh environmental conditions found in the automotive and military industries in particular. Currently available adhesive materials and systems have, for example, peel strength, chemical resistance, moisture resistance, high temperature stability, dimensional stability especially in the Z-axis direction, adequate flowability, room temperature storage stability before processing and processability. etc., but typically fails to meet one or more requirements regarding one or more of the aforementioned characteristics.

Therefore, there was a need for an adhesive material that satisfies all the requirements for properties suitable for harsh environmental conditions while retaining ease of use.

and 1 and 211 One of the objects of the present invention is to provide an improved adhesive material (aclhe
sive material).

One of the features of the invention is to provide an improved material that can be used for bonding electronic circuit construction materials.

Another feature of the invention is the use of a two-step reaction sequence to provide the adhesive material.

Another feature of the invention is to provide an adhesive material using a two-stage reaction sequence in which the intermediate adhesive material obtained in the first reaction stage can be stored for long periods of time without deterioration of the properties of the adhesive material. .

Yet another feature of the present invention is that the first reaction occurs between the aziridine component and the polyester component, and the aziridine/polyester component
The object of the present invention is to provide an improved adhesive material by causing a second reaction between a polyester component and at least one epoxy component. Note that at least one type of epoxy component is electronic grade (electronic grade).
grade) li [l fat.

The above and other features of the present invention are characterized in that a hydroxyl-terminated polyester component and an aziridine curing component are reacted at room temperature, and the resulting polyester/aziridine component is combined with at least one, preferably two or more, epoxy resins. This is accomplished by reacting with the ingredients. One of the epoxy components is an electronic grade resin such as trismethane novolac epoxy. Additionally, the second reaction requires a temperature of 250°F to 400°F. Setting the reaction temperature to such a high temperature will shorten the shelf life of the unreacted intermediate mixture of the polyester/aziridine component and the epoxy component.
That is, carrying out the second reaction stage increases the period during which great adhesion performance can be provided. This intermediate mixture is used as a release substrate until needed.
or between two release materials.

The features of the present invention will become clearer from the following description.

The material composition of the present invention contains at least one type, preferably two or more types of epoxy components. One of the epoxy components must be selected from electronic grade resins such as, for example, trismethane epoxy novolac sold by Dow under the trade name Quatrex 5010. The remaining optional epoxy components include those of the visible "bis-epi" type, such as Ce1anes.
e Epi-Rez 5132, as well as hard "novolak" types, such as Dow D, E, 8.438
The material compositions of the present invention further include a high molecular weight polyester component that is hydroxyl terminated and has minimal carboxylic acid functionality, such as DuPont's 49002, and an aziridine curing component, such as Cordova Che
+*1cal Co, including Xama 2 or 7.

In the two-step curing (reaction) sequence as described above, the aziridine is first reacted with the carboxylic acid of the polyester as described below.

(2) In the above formula, R represents a high molecular weight polyester component, and X represents a repeating unit of the aziridine component. This reaction proceeds at room temperature.

The second reaction is unique to the present invention and consists of reacting the (1) group with the -C-C group of the epoxy component as described below.

In the above formula, Y represents trismethane epoxy alone or in combination with bis-epiepoxy and/or novolac epoxy having the structure below.

Prepare a mixture of the following ingredients.

Polyester resin consisting of DuPont 49002 base resin with a solids content of 17-20? An epoxy novolac known under the trade name Dow DEN 438 was dissolved in methyl ethyl ketone at a solids content of 85% by weight. an electronic grade epoxy resin known under the trade name Dow Quatrex 5010 dissolved in methyl ethyl ketone at a solids content of 75%; a polyfunctional aziridine known under the trade name Xama 7;

This mixture has a polyester component with a solids content of 80% by weight and a solids content of 10wt. E% epoxy novolak and 10% by weight solids content electronic grade epoxy;
It is formed by mixing 0.25 parts by weight of aziridine with 100 parts by weight of the mixture containing the solvent. This component mixture can be prepared in one of two ways:

Method 1) Mix the polyester and aziridine together thoroughly and let the aziridine/carboxylic acid reaction take place in a vacuum at room temperature for more than 30 minutes, then add the epoxy.

Method 2) Put the polyester, epoxy and aziridine separately into a container without mixing them, mix thoroughly after introducing all the ingredients, and let stand for at least 30 minutes before use to allow the aziridine/carboxylic acid reaction to occur. cause to occur

The homogeneous solution is applied to a 2s+il thick polyimide (eg Kapton) film using a reverse roll coating method to form a 1ml thick dry coating on the polyimide film. This polyimide film was heated to 25 fpm (fee 1
7 minutes), dry at 212°F, combine with a 1 ml thick release material in a combined coater and laminator operating station, roll up and store at room temperature until use (or Depending on the application, the homogeneous solution is stored between two release materials so that the adhesive material can be used on any surface to be bonded.

The roll was cut into pieces, the release material was removed, and the coated film was 1 oz.

placed on a sheet of copper. The composite structure was placed between two caul plates with high temperature release material on both sides and pressurized with a hydraulic press at a temperature of 375° F. and a pressure of 250 psi for one day. The resulting composite product NI structure is 8N511
As a result of being destroyed by the methods of PC-FC-232B and 241B, the properties shown in Table I were exhibited.

Up to - L LI Poundser inea inch MEK = Methyl ethyl ketone TOL = Toluene IP^ = Isopropyl alcohol T111 = ) Lichlorethylene MC - Methylene chloride Rainbow specific pressure 1, adhesive mixture to polyimide (laminated) The film is applied and foiled in a straight line at a temperature of 300"F and a pressure of 90-100 psi. The resulting structure is cured for 2 hours at 150F, 2 hours at 275F, and 2 hours at 350F. do.

2. Apply to a release material and bond with another release material to form a backless film.

The adhesive composition of the present invention is suitable for coverlay and bond ply comprising 50-90% by weight polyester and 90-50% by weight epoxy.
ly) constitute an adhesive coating material. This material is
It has a unique latent heat-responsive curing mechanism consisting of one, preferably two, epoxy components, where one of the epoxy components is selected from electronic grade resins such as trismethane epoxy novolac, and the remaining epoxy The ingredients are selected from novolac or bis-shrimp epoxies. In addition, the polyester is a high molecular weight polyester terminated with hydroxyl groups and has a carboxylic acid functionality determined by an acid number of 0.2 to 4.0.

The present invention cures through a two-step reaction sequence to form a fully cross-linked network structure without producing volatile by-products for film-to-film, foil-to-film, foil-to-foil and hardboard-to-hardboard bonding. The present invention provides high-performance lamination coverlays and bondbly adhesives that can be used for. The adhesive material of the present invention has excellent flexibility, high adhesive strength, solder resistance, moisture resistance, chemical resistance and Z-axis stability, and can be processed continuously and/or over time. You can also.

Additionally, since the second stage curing process is performed at high temperatures, the coating material can be stored for a long period of time before this curing process is performed. This epoxy-based adhesive material can be coated onto an insulating film or release material in a continuous operation and stored indefinitely at room temperature before further processing;
or in-l on various foils or films.
Since it can be laminated onto a substrate and cured without generating volatile by-products, it has overall superior properties compared to conventional systems, and also has the advantage of high Z-axis stability. A flexible bondbrid is obtained.

The present invention is not limited to the preferred embodiments described above, and various modifications can be made within the scope thereof.

Claims (20)

[Claims] (1) a step of reacting the aziridine component with at least one type of polyester compound;
The aziridine/polyester component obtained in the polyester reaction step is
A method of providing an adhesive material comprising reacting with a trismethane novolac epoxy component of a type. 2. The method of claim 1, wherein the epoxy component comprises a component selected from bis-epoxy compounds and novolak epoxy compounds. (3) Before reacting the aziridine/polyester component with at least one epoxy component, the aziridine/polyester component is
3. The method of claim 2, further comprising the step of mixing the polyester component and the epoxy compound and applying the resulting mixture to the required location of the adhesive material. 4. The method of claim 3, further comprising the step of: (4) applying the mixture between and bonding a plurality of supports selected from film, foil, and hardboard. (5) The method according to claim 1, wherein the polyester component is used in an amount of 50% to 90% by weight, and the epoxy component is used in an amount of 90% to 50% by weight. (6) The polyester compound is selected from high molecular weight polyesters having hydroxyl end groups and a carboxylic acid functionality determined by an acid number of 0.2 to 4.0.
The provision method described in . 7. The method of claim 1, wherein the epoxy component and the aziridine/polyester component are reacted by heating the mixture of the epoxy component and the aziridine/polyester component at a temperature of 250<0>F to 400<0>F. (8) A product having two surfaces adhered to each other according to the method of providing an adhesive material according to claim 1. (9) A composite product of film-to-film bonding, foil-to-foil bonding, or foil-to-film bonding having surfaces bonded according to the method of claim 3. (10) The method according to claim 1, wherein the aziridine component, the polyester component, and the epoxy component are mixed and then reacted. (11) A mixture produced by the method according to claim 3 for application to surfaces to be bonded to each other. (12) Storage means for an adhesive coating for use on a surface to be subjected to a second stage reaction to adhere to a second surface, the adhesive coating being prepared by the method of claim 1; Storage means for an adhesive coating comprising at least one applied release material. (13) A composite structure including a first structure, a second structure, and an adhesive material for bonding a first surface of the first structure and a first surface of the second structure to each other, A composite structure in which the adhesive material includes: an aziridine component, a polyester component, and an epoxy component selected from an electronic grade resin epoxy component group. (14) The composite structure according to claim 13, wherein the electronic grade resin component is a trismethane novolac epoxy component. (15) The epoxy component is at least one selected from the bis-epoxy component and the novolak epoxy component.
14. The composite structure of claim 13, also comprising another epoxy component of the type. 16. The composite structure of claim 13, wherein the first structure and the second structure are selected from polyimide film, metal foil, and hardboard. (17) The aziridine component and the polyester component are combined in the first reaction, and the -N- group of the resulting aziridine/polyester component reacts with the ▲mathematical formula, chemical formula, table, etc.▼ group of the epoxy component in the second reaction. Claim 13
Composite structure described in. (18) The composite structure according to claim 13, wherein the first structure and the second structure are release materials, and the combination of the aziridine component, the polyester component, and the epoxy component is not heated. (19) A claim that includes a third structure and a fourth structure, and a combination of the components is disposed between the third structure and the fourth structure after removing the release material. 19. The composite structure according to 18. (20) Claim 19 Heated at a temperature of 300°F or more
Composite structure described in.