DK164092B - Method for the manufacture of metal-laminated substrate material for printed circuit boards, accelerated epoxy resin-hardener-catalyst system for use in the method and double band press for performing the method - Google Patents

Description

DK 164092 B

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a process for the preparation of metal cached base material for conductors - plates of the kind set forth in the preamble of claim 1, to an accelerated epoxide resin-hardener catalyst system for use in the process, and a double-band press of the preamble of claim 12 specified species for carrying out the method.

Metal-cached base materials for conductor plates have heretofore been made exclusively discontinuously by compression of cut, heat-cured resin-provided laminates and metal foils in floor presses. Such a process is costly and provides basic materials whose quality varies within the individual plate. Therefore, a continuous process has long been desired.

A step towards continuity exhibits the method of GB-A-2,108,427, whereby glass fiber webs provided with a heat curable resin which is cooled to avoid an undesirable pre-reaction of the resin prior to compression and the metal foil to be cached are compressed with 20 in a pressing device, under pressure and heat, and the resulting base material is cut into lengths. The pressing, however, occurs intermittently in such a way that the fiberglass web and the copper foil introduced into the press are at a standstill each time during the pressing process, and the pressing product is ejected tactically. The product of this method therefore consists of single sections, the dimensions of which are limited by the dimensions of the hot plates and which are interconnected via non-compressed, ie. useless paragraphs. Here, too, the quality varies greatly within the individual plate, which, when the consumer wants high, homogeneous quality of the conductor plates, leads to large quantities of debris.

From EP-B1-0,036,635 there is known an apparatus for joining several strip-shaped layers of material to a composite film comprising a double-band press with revolving heating steel strips. On the inlet side of the double-band press, each steel band is assigned a protective shield that serves 2

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for thermal insulation. With the help of the two protective shields, heating of the layers of material above room temperature is avoided. Double-band presses of the kind mentioned are known from the manufacture of decorative laminates.

DE-C-1,216,522 discloses a method for producing sheet-shaped plastic material, in particular for treating the surfaces of wood sheets, plywood, chipboard and the like, whereby resin impregnated, particularly melamine resin impregnated, is used as preferred starting materials for the coating layers. paper. According to a previously mentioned variant, as a top and bottom layer, a plate, e.g. of copper, be applicable. This plate is already punched out in the required manner to form a particular pattern for a printed circuit. Instead of the above-mentioned sheets of wood and the like, phenolic resin-impregnated paper or epoxide-resin-impregnated fiberglass tissue can also be used for the inner layer. In this process, the preheating occurs under pressure as it takes place in a space in a preheating block that is less than the layer thickness of the material to be processed.

It is an object of the invention to provide a process for producing metal-cached base material of the kind specified in the preamble which can be carried out continuously and furthermore results in a material of high, homogeneous quality which, in particular, largely holds the objectives.

This object is fulfilled according to the invention with the special features specified in the characterizing part of claim 1.

Suitable embodiments are defined in claims 2-9.

According to another aspect, it is an object of the invention to provide an accelerated resin system for use in the method of the invention.

This object is achieved with an accelerated epoxide-resin curing system, which is characterized by the characterizing part of claim 35 10. An advantageous embodiment of this system is defined in claim 11.

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3

According to a third aspect, the object of the invention is to provide a double-band press for carrying out the method according to the invention, which takes up the starting materials, namely the fiberglass webs on one side and the metal foil to be cached, on the other hand and processes them into a metal-cached base material. for high-homogeneous quality conductor boards that meet the targets to a great extent. This object is fulfilled with the double-band press defined in claim 12, and suitable embodiments of this press are defined in claims 13 to 18.

The advantages of the invention are based on a targeted combination of measures that together lead to optimal products.

According to a particular feature, an accelerated resin system is used in the method 15 of the invention. This is one of the prerequisites before achieving optimal results.

Thus, accelerated epoxide resin systems, that is, accelerated heat-curable epoxide-curing catalyst systems, are preferred.

Suitable accelerators include the following pyridine compounds: 25 30 35 4 0

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2-benzoylpyridine 3-benzoylpyridine 4-benzoylpyridine 2-benzylpyridine 3-benzylpyridine 4-benzylpyridine 2-benzylaminopyridine 4-dimethylaminopyridine 2-methoxypyridine 4-tert-butylpyridine-3-cyanopyridine-3-cyanopyridine 3-Ethylpyridine-3-ethyl-4-methylpyridine-2-phenylpyridine-2,6-diaminopyridine-3-methylpyridine 2- (aminomethyl) -pyridine 2-amino-4-methylpyridine 2,4-dimethylpyridine

Another advantageous group of accelerators are the substituted imidazole compounds known per se, including imidazole itself, namely: N-methylimidazole 2-methylimidazole 2-phenylimidazole 4-phenylimidazole 4-methylimidazole 2-methylbenzimidazole 5,6-dimethylbenzimidazole 1- -phenylbenzimidazole 1,2-dimethylimidazole 4,5-diphenylimidazole 2- ethyl-4-methylimidazole carbonyl diimidazole 5

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imidazole 2-undecylimidazole 1-cyanoethyl-2-phenylimidazole 2-phenylbenzimidazole 5 Particularly good results are obtained with a combination of dicyandiamide, respectively. benzyldimethylamine with the aforementioned pyridines, respectively. imidazoles. In this way, according to the invention, a stronger acceleration is generally sought than with known resin systems, above all in order to achieve an economical flow rate in the press.

A further special feature consists in the use of a pre-cured resin. Resin impregnated webs in which the resin is pre-cured to B state have been found to be particularly suitable. Thus, a more advanced B-state, i.e. with less resin flow than by pre-curing for floor presses.

A particularly important feature is the pressureless preheating of the woven webs impregnated with the accelerated resin.

It is extremely surprising that the pressure-free preheating of the heat-curing resin system provides for the use of a suitable double-band press and thus continuous production of impeccable quality metal-cached base material webs, 25 especially when considering a hardened , ie ready-reacted resin is inert and no longer involved in bonding, and that the curing reaction of the accelerated, pre-cured resin system is further promoted by the preheating of the laminate webs. What is surprising to a person skilled in the art is particularly evident in the light of the aforementioned GB and EP writings and the prejudice set forth therein. One skilled in the art would be of the opinion that the resin to avoid an undesirable pre-reaction should be cooled after application and before the press, i.e. the full reaction capacity of the resin 35 was to be reserved for the formation of a bond between the individual layers during the pressing process. When you stick around

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6 that this recommendation is given for a normal curing, ie. not accelerated and non-cured resin, the present preheating occurs of a resin which, upon curing, has already lost part of its reaction capacity, and whose reaction capacity due to the acceleration of heating decreases further rapidly, to be pure reason. However, this preheating measure, which is diametrically opposed to the prior art recommendation, allows for continuous production of metal-cached base material for conductor plates. Obviously, due to the pre-reaction induced by the preheating of the accelerated and hardened resin, the resin is activated for the subsequent reaction under pressure, so that in the press itself a bonding takes place which starts quickly.

For carrying out the method, the impregnated fiberglass webs are brought together prior to entry into the double-band press and pre-pressurized to reduce the viscosity of the resin system independently of the metal foils, while the 20 metal foils in this region are not yet connected to the fiberglass webs and are spatially separated and physically transported. Seen in the transport direction, only after this pressure-free preheating zone is the joining and bonding of the preheated glass fiber webs and the metal foils.

Then these are compressed with each other at elevated temperature and under pressure.

The pressureless preheating of the impregnated fiberglass webs leads to a viscosity reduction of the heat-curable resin, thereby bringing the resin into the contacting glass fiberglass webs that touch each other intimately, so that no application of the interfacial pressure is overcome. between the fiberglass tissue webs, respectively. their resin layers. In addition, the pre-reaction caused by the preheating of the accelerated and pre-cured resin leads to an activation of the resin to the subsequent pressure reaction, such that the metal foils of the

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one side and the fiberglass webs on the other hand are quickly connected to each other in the double band press itself.

The above-mentioned viscosity reduction of the resin in the pressure-less preheating zone also allows for the withdrawal of entrapped air vesicles in the resin layers, which otherwise assemble into larger vesicles and may hinder the desired homogeneous quality of the base material.

In the present process, the differences between lower quality and mid-range high-quality regions in the individual plates observed by a discontinuous or by the above-described rate method are eliminated so that the base material produced exhibits a uniformly high quality and can be cut into sheets of homogeneous quality.

Double-band presses which can be used in connection with the pressureless preheating zone are e.g. disclosed in EP-A-0.026.396 and 0.026.401 as well as in US-A-4,336,096.

As already mentioned, the resin system of the fiberglass webs, when joined together before the preheating zone of the double-band press 20, is already pre-cured, namely in general to the B state. An advanced B-state, i.e. with a lower resin flow than by pre-curing by floor pressing. The multilayer laminate product is generally uniformly heated in the pressureless preheating zone prior to the pressurized zone. Due to the lowering of the viscosity, whereby the resin becomes soft and plastic, there is already a smoothing of any irregularities present and an intimate contact between the layers. The preheating temperature is dependent on the resin system, and preferably it is approx. 80 to 100 ° C. From the pressureless preheating zone, the multilayer laminate product comes with e.g. a temperature of 100 ° C into the pressure-acting zone, being immediately preceded by one or two, preferably separately preheated metal foils, and advantageously compressed by increasing temperature, for example at 150 to δ

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210 ° C at 25-80 bar. The multi-layered base material now formed is then cooled, preferably under pressure, especially while maintaining the compression pressure, advantageously below the glass resin point of the resin, optionally further tempered and further processed. The cooling under pressure, i.e. in the press, serves to stabilize the high quality of the base material obtained by the continuous process, especially to avoid deformation.

Other significant advantages of the present process are the following: - the optimum utilization in cutting completion, as the continuous web can be cut to any length, - the material saving, since only a two-sided edging 15 is needed, - the energy saving, since the cooling process and thus - the qualitative improvement of the laminate, especially with respect to dimensional stability, 20 - a reduction of the extension, keeping the metal foil surface cleaner.

Compared to the discontinuous manufacturing methods in so-called floor presses, a significant saving of workflows is obtained, namely cutting across prepegs to the format length, cutting across the metal foil to the format length, the pre-laying of prepeg packages, the construction of laminate packages, the separation of the laminate packages, the lapses of the costly press plates and the lapses of the lining paper that can only be used once.

The invention will be explained in more detail below with the aid of the exemplary embodiment of an apparatus suitable for carrying out the method of the present invention.

35 0 9

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The apparatus shown in the drawing comprises a double-band press 1 with a pressurized zone 2 and a pressure-free preheating zone 3 in front thereof. The pressurized zone 2 is divided into a longer irrigation area 4 following the preheating zone 3 and a shorter cooling area following the heating zone 5. The heating zone, in turn, has three temperature ranges 41, 42 and 43 that can be independently controlled from eachother. The double-band press 1 has, before the pressure-acting zone 2, a more spaced-apart heated inlet-10 control drum pair 6, 6 ', after the pressure-effective zone 2 a correspondingly shaped, less spaced-out outlet-control drum pair 7, 7' and in connection to the inlet guide drum pair support rollers 11, 11 'for the pressure bands 8, 8' of the double belt press 1. In order to keep the temperature constant, the preheating zone 3 is delimited by the pressure band 8 heated by the inlet control drum 6 by the double belt press 1. a pair of heat shields 9, 9 '. The latter consists of a chilled plate. For the cooling, cooling hoses, here of copper, are used in which the flow rate of the refrigerant can be controlled so that accurate temperature control is possible. Instead of cooling hoses, cooling pockets with a forced line can also be used. The heat shields 9, 9 'are arranged displaceable in a horizontal direction so that the temperature controlled preheating zone can be approached to 25 or removed from the pressure-acting zone 2, ie. also controlled with respect to their spatial device.

The principle of operation of the double-band press used in accordance with the invention is based on the fact that on the goods web which is continuously moved through the press, a uniform and also constant pressure is applied over the width of the goods web.

This is done here by transferring the pressure from pressure cushions (not shown) in the press to the endless steel - pressure bands 8 which run through the press synchronously with the goods web and at the same time serve as finishing sensors. Preferably, relatively high-mass printing tapes are used, e.g. steel strip with a thickness of approx. 2 mm, which ensures a good heat transfer.

10

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The heating area 4 in the press 1 exhibits e.g. a length of 3 m, which allows for a maximum construction length of the total double band press 1, ie. the pre-heating zone 3 preferably has a length of 40-100 cm. The cooling region 5 exhibits a length of 1 m in the illustrative embodiment shown.

Prior to the double-band press, coil rollers 12, 13 with 2 coils 14-17 are provided for prepegs, i.e.

10 fiberglass fabrics, fiberglass or paper webs with the resin system, and an additional coil coil 18 with two coils 19, 21 for metal foils. There are guide rollers 22, 22 'for the metal foils between the coil coil 18 and the double belt press 1.

15 After the double belt press in the production direction, an edge pruning device 23 and then a longitudinal cutter device 24 are found.

For heating the preheating zone, in turn, the heat-inlet control drum pair 6, 6 ', 20 can be used, as shown, for example, in the drawing. Temperature control means such as plates 9, 9 'may be provided.

In a preferred embodiment, the double belt press may have support rollers 11, 11 'for the printing bands.

Advantageously, the pressurized heating region is divided into different, independently controllable temperature ranges.

In the pressure-free preheating zone, according to a preferred embodiment, spatially controlled guiding means are provided to support the separate supply of the fiberglass web and the metal foil.

During operation, four prepeg trajectories, i.e. laminates provided with a resin-hardener-accelerator system and pre-cured until an advanced B state is combined and fed to the preheating zone 3, where the four-layered product, depending on the resin system, is pressurized to a temperature of approx.

11 to 80 to 100 ° C. At the same time, metal sheets are supplied from the two coils 19, 21 by the coil roller 18, which are separated from the above prepegs between the corresponding heat shield 9 or 9 'and the corresponding pressure band 8 or 8' and immediately before the pressurized zone 2 is combined with the said prepegs. While the temperature in the preheating zone as stated is up to 100 ° C, the temperature of the inlet drums is higher so that the metal foil is heated stronger than the said prepegs. In the three temperature ranges 41, 42 and 43 10 of the heating region 4 in the pressure-acting zone 2, the assembled single layers are compressed at a pressure exceeding 25 bar and at a temperature rising from 150 to approx. 190 ° C, to a base material web and bonded by curing the still reactive resin. The temperature of the first temperature range 41 is lower than the temperature of the second temperature range 42, which may be equal to the temperature of the third temperature range 43 and is 190-200 ° C. In the subsequent cooling region 5, the base material web is cooled under pressure. At this critical stage, the application of pressure 20 prevents a deterioration in quality, especially a deformation of the product. The base material web now leaves, cooled to approx. 100 ° C, the cooling region 5. In the subsequent edge pruning device 23, the pressing edges at both sides of the base material web are removed, whereupon it is cut to a desired length in the trunking device 24.

Between the cooling zone and the edge pruning device, a post-tempering zone may be provided for mold stabilization of the base material.

Advantageously, the illustrated apparatus 30 operates with a dwell time in the heating region 4, which corresponds to a feed rate in the double-band press of approx. 3 m / min. The residence time and the feed rate are dependent on the cure temperature and the reaction rate of the resin-hardener-accelerator system used.

35 If only base material cached on one side is made, a heat-resistant separator 12 0

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laminating film should be wound on the corresponding coil and run into the double-band press instead of the metal foil. As a separating foil, e.g. an aluminum foil / silicone treated or cached with polythetrafluoroethylene is used. After separation from the double-band press, the separating foil can be peeled off from the finished base material web and reused.

Of course, although the process of the present invention is illustrated by means of a six-layer base material, base materials having a different number of layers can also be made.

The operating conditions described are primarily dependent on the resin system used and can be varied accordingly.

The present process and apparatus herein may be used for caching with copper or with other metal foils. They are particularly suitable for caching with so-called combination foils, e.g. Cu / Al used to produce the finest conductor boards (the so-called 20 "etchible / stripable" boards).

The invention is further illustrated by the following examples.

Example 1.

A glass-finish fabric of finish-finish, commonly used in copper-cached fiberglass epoxide 2 resin laminates for conductive sheets, weighed 200 g / m, is wetted with a resin solution consisting of 100 parts of a polymer, partially brominated bisphenol-A -glycidyl ether 30 with a proportion of epoxidized novolac of 1-15%, preferably 5-12%, 3.2 parts of dicyandiamide, 0.28 parts of 3-methylpyridine and 80 parts of methylglycol. The prepeg thus impregnated and dried at 165 ° C has a resin content of 42% and one

resin flux of 10%. Seven of these prepegs are post-35 O

heating to 80 ° C in continuous flow on the apparatus referred to herein with the double-sided 35 'on thick copper

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coating foil to a 1.5-Iran thick laminate at a temperature rising from 150 to 195 ° C and at a pressure of 45 bar. The test of the laminate gives surprisingly positive results that are above the average in terms of 5 dimensional stability, and also show properties that are equivalent to the properties of commercially available laminates.

The laminate produced exhibits a thickness tolerance of 3/100 mm. In comparison, the standards for rigid laminates indicate a tolerance of ± 13/100 mm, which is also fully utilized by products from a floor press.

Example 2.

A glass tissue as set forth in Example 1 is soaked with a resin solution consisting of 100 parts of a polymer, 15 partially brominated bisphenol A-glycidyl ether with a proportion of epoxidized novolak of 1-15%, preferably 5-12%, 3.4 parts of dicyandiamide. , 0.33 parts of 4-dimethylaminopyridine and 80 parts of methylglycol. The thus-soaked and dried prepeg at 170 ° C has a resin content of 44% and a resin flux of 8%.

20 After preheating, several of these prepegs turn to 85 ° C

pressed continuously through the double-sided 35 µm copper foil coating apparatus of this invention into a 1.5 mm thick laminate at a temperature rising from 155 to 200 ° C under a pressure of 50 bar. In this embodiment, a test of the laminate also provides values with respect to dimensional stability above the norm and, moreover, laminate properties comparable to the characteristics of commercially available products.

Example 3.

With a resin blend of 100 parts of a polymer, partially brominated bisphenol-A-glycidyl ether having a proportion of epoxidized novolak of 1-15%, preferably 5-12%, and having an epoxy equivalent weight of between 350 and 520, 3.0 parts 35 dicyandiamide, 0.40 parts of 2-amino-4-methylpyridine and 80 parts of methylglycol impregnate a 100 g / m heavy glass tissue with co 14

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for use as set forth in Example 1 and dried at 165 ° C. The resin content is 44% and the resin flux 10%. Two of these prepegs, after preheating to 80 ° C, are pressed continuously into the present apparatus 5 with one-sided 35 µm thick copper foil coating using a separation foil at a temperature rising from 150 to 190 ° C; and at a pressure of 50 bar to form a 0.2 mm thick laminate. The test gives the same good results as in Example 2.

10

Examples 4-13.

The compositions and operating conditions of Examples 4-13 are summarized in the following table.

15 20 25 30 35

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Claims (18)

A method of making metal cached base material for conductor sheets, a) wherein the glass fiber webs provided with a heat-curable resin and the metal foil (12) to be cached are pressed together with each other under pressure and heat, and b) thereby cutting the base material thus obtained. lengths, characterized by the following special features: (c) fiberglass webs are used; (c) impregnated with an accelerated resin system; and (c) resin is pre-cured; (d) fiberglass webs are assembled and pre-pressurized to reduce the viscosity of the resin system. e) the pressurally preheated glass fiber webs are brought together with the metal foil or metal foils and compressed in the pressure zone by a double band press (1) to the base material web at temperatures of 150 to 210 ° C. Process according to claim 1, characterized in that the fiberglass web and the metal foils are compressed under a pressure of 25-80 bar. Method according to claim 1 or 2, characterized in that the base material web produced by compression is cooled in a pressure zone (5) under pressure, preferably arranged within the double-band press (1). Process according to one of claims 1-3, characterized in that the base material produced is post-tempered. Process according to one of claims 1-4, characterized in that, in the manufacture of base material cached on one side with metal foil, a separating foil is fed and pressed on the other side, and that after the expiry of the double-band press (1) is pulled from the base material web. Method according to one of claims 1 to 5, characterized in that the fiberglass webs and the metal foil or each metal foil are preheated separately. Process according to claim 6, characterized in that the metal foil or each metal foil is preheated to a higher temperature than the glass fiber webs. A method according to any one of claims 1-7, characterized in that the glass fiber webs are first combined with the metal foil or each metal foil immediately before the pressure zone of the double-band press (1). Process according to one of claims 1-8, characterized in that glass fiber webs impregnated with an accelerated epoxide hardener catalyst system are used and pre-cured. An accelerated epoxide resin hardener catalyst system for use in the process of any one of claims 1-9, characterized in that it contains as an accelerator substituted pyridine compounds, imidazole or substituted imidazole, especially in combination with dicyandiamide or benzyldimethylamine. Accelerated epoxide hardener catalyst system 20 according to claim 10, characterized in that it contains 0.2-0.8% by weight of the accelerator or accelerator mixture, based on solid epoxy resin. Heatable double-band press (1) for carrying out the method according to one of claims 1-9, 25 a) with a pressure-acting heat area (4) for compressing the glass fiber webs and metal foils, characterized by b) a pressure-free preheating arranged in front of the heating area (4) and (c) in the region of the pressureless preheating zone (3), spatially spaced guide means (12, 13; 18) for the fiberglass webs and the metal foil or each metal foil. Double-band press (1) according to claim 12, characterized in that the preheating zone (3) has a heat shield pair (9, 9 ·) with adjustable cooling. Double-band press (1) according to claim 13, characterized in that the heat shields (9, 9 ') are arranged slidably in a horizontal direction. Double-band press (1) according to one of claims 12-14 with an inlet drum pair (6, 6 ') and an outlet drum pair (7, 5 7'), characterized in that adjacent to the inlet drum pair (6, 6 ') support rollers (11, 11. for the pressure bands (8, 81) of the double belt press (1). Double-band press (1) according to one of claims 12 to 15, characterized in that, in addition to 10, the pressure-acting heating area (4) has a pressure-acting cooling area (5) as well. Double-band press (1) according to one of claims 12 to 16, characterized in that the pressure-acting heating area (4) is divided into independently adjustable temperature ranges (41, 42, 43). Double-band press (1) according to one of claims 15 to 17, characterized in that the distance between the two inlet drums (6, 6 ') is greater than the distance between the two outlet drums (7, 7'). 20 25 30 35