JPH0247364A - Treatment of fiber substrate - Google Patents

Abstract

PURPOSE:To perform uniform application of a coupling agent to a fiber substrate without causing migration of the agent by immersing a fiber substrate in a coupling agent, squeezing the substrate and drying the impregnated agent with an infrared drier. CONSTITUTION:A fiber substrate composed of an inorganic fiber and/or organic fiber is immersed in a coupling agent (usually a silane coupling agent such as aminosilanes and vinylsilanes) and squeezed. The impregnated coupling agent is dried with an infrared drier (the wavelength range of the infrared radiation is preferably 0.76mum to 1mm) to achieve uniform application of the coupling agent. The obtained fiber substrate has a uniform coating layer of the coupling agent and exhibits excellent adhesivity to a matrix resin. Accordingly, a printed circuit board produced by the use of the substrate has excellent heat-resistance and can be used as a circuit of an electronic apparatus having improved performance and reduced size.

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention relates to a method for processing fiber #a substrate suitable for use in printed wiring boards and the like.

(Conventional technology and its problems) Generally, ma-filled composite materials include an impregnated mat of fiber base material,
Laminated prepreg material consisting of fiber base material and resin, made by filament winding method, short m#! There are injection molded products that have dispersed These are all tensile strength,
This was done with the expectation that it would improve impact strength, Young's modulus, etc., improve dimensional stability, and improve heat resistance, and it has also had practical effects. However, its properties are affected by the properties of the resin and the structure, shape, and organization of the filler;
Among these, the interface between the filled jAIU1 base material and the matrix resin has a large influence, and it is customary to treat the surface of the Ml fiber base material with a coupling agent. Glass, an inorganic fiber, is an important fiber base material used in fiber-filled composite materials! There are carbon fibers, carbon fibers, etc., and organic fibers such as aromatic boric acid fibers, aromatic polyester fibers, etc., and the above-mentioned treatments have been applied to improve the adhesion of both types. In particular, the above-mentioned fiber base material has excellent electrical properties and heat resistance, and also has i?
! Taking advantage of its low % expansion rate, it can be combined with an appropriate matrix resin to form a fiber-filled composite material, which is then laminated, hardened, printed, and used as a substrate in industrial equipment.

However, in recent years, as electronic devices have become more sophisticated and more compact, the characteristics required of the printed layout i7 board have become even more advanced, and even the slightest amount of snow can interfere with the adhesion between the Ryouzetsu 75 material and the matrix resin. In some cases, the characteristics at high temperatures are insufficient, making it difficult to manufacture high-precision circuits.

The purpose of the present invention is to improve these drawbacks and to produce a composite material with excellent heat resistance that fully utilizes the heat resistance of the fiber base material and matrix resin. The present invention provides a treatment method for uniformly applying a coupling agent to a material.

(Means for Solving the Problems) The above object is to solve the problem when applying a coupling agent treatment to a fiber base material made of inorganic fibers and/or organic fibers.
This is achieved by a method for treating a fiber base material, which is characterized by impregnating the M base material with a coupling agent, squeezing the liquid, and then drying it with an infrared dryer.

The inorganic fibers used in the method of the present invention are not particularly limited, but glass fibers or carbon fibers are usually used. Further, the organic a-fiber is not particularly limited as long as it is of a rigid polymer type, and aromatic l-aryamide fiber or aromatic polyester fiber is usually used. More specifically, as the aromatic boria fiber, poly-p-phenylene terephthalamide and poly-m-phenylene terephthalamide are preferably mentioned, and as the aromatic polyester fiber, preferably polyalkylene terephthalate and polyester fiber are used. Examples include alkylene isophthalates and polyalkylene naphthalates, and particularly preferred are polymers obtained from terephthalic acid, isophthalic acid, or ester-forming derivatives thereof, and ethylene glycol, 1,4-butanediol, or ester-forming derivatives thereof. Examples include polymers and copolymers.

The fiber base material used in the method of the present invention includes the above-mentioned inorganic fibers, the above-mentioned organic fibers alone, or woven and knitted fabrics made by blending or interweaving them. Textiles are preferred.

Normally, when producing fiber optic fiber composite materials, the fiber base material is treated with a coupling agent etc. before impregnation with the matrix resin, but in the method of the present invention, after the Jam base material is impregnated with the coupling agent. , squeezed, and then dried in an infrared dryer.

As the coupling agent, silane-based ones can be used, such as r-aminopropyltriethoxysilane, r-aminopropyltrimethoxysilane, imidacillinsilane, N-aminoethylaminopropyltrimethoxysilane, etc. Silane, N-phenyl-r-aminopropyltrimethoxysilane, aminosilanes such as N-β-(N-vinylbenzylaminoethyl)-r-aminopropyltrimethoxysilane hydrochloride, γ-glycidoxypropyltrimethoxysilane Epoxysilanes such as r
Examples include chlorosilanes such as -chloropropyltrimethoxysilane, methacrylretins such as r-methacryloxypropyltrimethoxysilane, and vinylsilanes such as vinyltrimethoxysilane and vinyltriethoxysilane. The amount of the coupling agent attached to the fiber base material is also the commonly used 0.01 to 2 double ring%, preferably 0.1 to 1% by weight.

The infrared wavelength range of the infrared dryer used in the method of the present invention is not particularly limited, but is preferably in the range of 0.76 μm or more and 1 mm or less, which is the usual infrared range that heats water effectively and in a short time. However, the present invention is not limited to this wavelength range, and the point is that the infrared rays have a frequency that is approximately at the same level as the natural frequency of water molecules, so that the energy of the infrared rays is absorbed by water tζ without waste. Infrared rays with wavelengths within a certain range are sufficient. Therefore, as an infrared heat source, it is possible to use a tungsten light bulb, a glober made of sintered silicon carbide into a rod shape, a Nernst Gloer made of zinc oxide and yttrium oxide baked at high temperature, a mercury lamp, etc. However, it is not limited to heat sources within this range.

The step of preparing a fiber optic composite material by impregnating a fiber base material treated with a coupling agent with a matrix resin can be carried out according to a conventional method. These matrix resins may be conventional ones, such as epoxy resins, unsaturated polyester resins, and polyimide resins.

(Function) When performing a coupling treatment on a fiber base material, if the fiber base material is impregnated with a coupling agent and then dried with an infrared dryer, heat can be instantaneously distributed to the center of MAm. The coupling agent adheres uniformly without migration.

Therefore, when the fibers treated with the coupling agent obtained above are impregnated with an appropriate matrix resin to form a composite material, the coupling agent enhances the adhesion between the two. This improves the heat resistance of the composite material.

(Actual example) Example 1 Glass fiber yarn with EOG75 110 and twist number 1z was used for both the warp and weft, and the density was 44 warp/'l 5 mm.

A glass fiber plain woven fabric was woven with a weft of 55 threads/25 mm.

Next, the fabric was heat cleaned at 370°C to remove the raw wire binder and warp sizing agent.

After heat cleaning, the fabric was impregnated with 1ζ treatment solution prepared by adjusting epoxy silane (manufactured by Toshi Silicone Co., Ltd. 81 (6040) 1" 1J 11% to pH 5 to 4 with an acetic acid aqueous solution so that the impregnation rate was 25% xi%. After squeezing the liquid!
, an infrared dryer with a wavelength of 11μ I trowel dryer 2 1. I did it.

On the other hand, 100ij 1 part of bisphenol A type epoxy dark fat (manufactured by Ciba Geigy, GZ801A75), 1 part of dicyandiamide triplex, 0.2 parts by weight of penzyldimethylamine, 15 parts by weight of acetone, 20 parts by weight of methyl cellosolve,
An epoxy resin solution was prepared using 1 part by weight of dimethylformamide.

The silane-treated glass fiber fabric was impregnated with the epoxy resin solution and dried at 160° C. for 4 minutes to obtain a prepreg to which 50% by weight of epoxy resin was added. Stack 8 sheets of this prepreg, place 18μ thick copper foil on both outermost surfaces,
This was heated at 170° C. for 2 hours under pressure at 50 kf/cm to obtain a printed wiring board of an example of the present invention having a thickness of 1.6 squares.

Comparative Example 1 The same glass fiber plain weave as in Example 1 was used, and instead of the infrared dryer having a wavelength of 2.9μ as in Example 1, steam! It was dried in a spring dryer, and a printed wiring board of a comparative example was obtained in the same manner as in Example 1. Next, the results of comparing #4 thermal properties of the printed wiring board obtained in the example of the present invention with a comparative example will be described.

Regarding heat resistance, using the printed wiring boards obtained in Example 1 and Comparative Example 1, the boiling retention time, that is, the time until the interface of the printed wiring boards started peeling in a 260°C solder bath was measured. . The measurement results are shown in Table 1.

Table 1 This is a significant improvement compared to the previous version.

Furthermore, poly-p-phenylene terephthalamide fiber cloth (Kevlar 48, manufactured by Depont Co., Ltd., plain weave, thread = (warp/weft) 188D
/195D, dense variation = 34 lines/34 lines (per fi5mm)
, thickness: Q, l mm, basis weight = 62 f/m, and the same treatment as in Example 1 and Comparative Example 1 was performed, and the same effect was obtained.

(Effects of the invention) As detailed above, the fiber base material obtained by the method of the present invention has a coupling agent uniformly adhered to it and has good adhesion with the matrix resin, so both of them can be used to form a fiber optic composite. A printed wiring board made by laminating and curing these materials has excellent heat resistance, and can therefore be used for circuits of high-performance, miniaturized electronic devices.

Claims (1)

[Claims] (1) When applying a coupling agent treatment to a fiber base material made of inorganic fibers and/or organic fibers, the fiber base material is impregnated with the coupling agent, squeezed, and then dried with an infrared dryer. A method for treating a fiber base material.