JP2000239420A - Production of laminated sheet - Google Patents
Production of laminated sheetInfo
- Publication number
- JP2000239420A JP2000239420A JP11047842A JP4784299A JP2000239420A JP 2000239420 A JP2000239420 A JP 2000239420A JP 11047842 A JP11047842 A JP 11047842A JP 4784299 A JP4784299 A JP 4784299A JP 2000239420 A JP2000239420 A JP 2000239420A
- Authority
- JP
- Japan
- Prior art keywords
- glass cloth
- epoxy resin
- resin
- glass
- inorganic filler
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
Description
【0001】[0001]
【発明の属する技術分野】本発明は、ガラスクロスの上
に中間層樹脂を塗布し、さらに、その上にガラス不織布
を載置し、得られたプリプレグ2枚をガラス不織布を内
側にして重ね合わせ加熱加圧するコンポジット積層板の
製造方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method of applying an intermediate layer resin on a glass cloth, further placing a glass nonwoven fabric thereon, and laminating two obtained prepregs with the glass nonwoven fabric inside. The present invention relates to a method for producing a composite laminate to be heated and pressed.
【0002】[0002]
【従来の技術】ガラスクロスの上に中間層樹脂を塗布
し、さらに、その上にガラス不織布を載置し、得られた
プリプレグ2枚をガラス不織布を内側にして重ね合わせ
加熱加圧するコンポジット積層板の製造方法では、プリ
プレグ製造設備に樹脂が固着し、これがガラスクロスを
破り、安定してプリプレグを製造することができず、生
産性が低下するという問題がある。この中間層樹脂のし
み出しを防止するための方法として、ガラスクロスにエ
ポキシ樹脂を含浸乾燥させることが知られている。ガラ
スクロスにエポキシ樹脂のみを含浸させた場合は、ガラ
スクロス反対面から中間層樹脂がしみ出さないようにす
るためには含浸後十分に乾燥させなければならない。こ
のため、得られたコンポジット積層板は、銅箔とプリプ
レグの密着性が低下する傾向があった。一方、無機充填
材等を添加したエポキシ樹脂をガラスクロスに含浸させ
た場合では、無機充填材等の添加量や粒径が適切でない
と中間層樹脂のしみ出しを十分に防止できなかったり、
逆にしみ出しを防止できても、積層板の打抜き性が低下
するなどの問題があった。2. Description of the Related Art A composite laminate is prepared by coating an intermediate resin layer on a glass cloth, placing a glass nonwoven fabric thereon, stacking two obtained prepregs with the glass nonwoven fabric inside, and applying heat and pressure. In the production method of (1), there is a problem that the resin adheres to the prepreg production facility, which breaks the glass cloth, making it impossible to produce the prepreg stably, thereby lowering the productivity. As a method for preventing the exudation of the intermediate layer resin, it is known that a glass cloth is impregnated with an epoxy resin and dried. When the glass cloth is impregnated only with the epoxy resin, it must be sufficiently dried after the impregnation in order to prevent the intermediate layer resin from seeping out from the opposite side of the glass cloth. For this reason, in the obtained composite laminate, the adhesion between the copper foil and the prepreg tends to decrease. On the other hand, in the case where the glass cloth is impregnated with an epoxy resin to which an inorganic filler or the like has been added, if the amount and the particle size of the inorganic filler and the like are not appropriate, the bleeding of the interlayer resin cannot be sufficiently prevented,
On the contrary, even if the bleeding can be prevented, there is a problem that the punching property of the laminate is reduced.
【0003】[0003]
【発明が解決しようとする課題】本発明は、ガラスクロ
スの上に中間層樹脂を塗布する工程を有するコンポジッ
ト積層板の製造方法において、打抜き性等を低下させる
ことなく中間層樹脂がガラスクロス反対面からしみ出さ
ないようにすることを目的とする。SUMMARY OF THE INVENTION The present invention relates to a method for producing a composite laminate having a step of applying an intermediate layer resin on a glass cloth. The purpose is to prevent seepage from the surface.
【0004】[0004]
【課題を解決するための手段】本発明は、ガラスクロス
の上に中間層樹脂を塗布し、さらに、その上にガラス不
織布を載置し、得られたプリプレグ2枚をガラス不織布
を内側にして重ね合わせ加熱加圧するコンポジット積層
板の製造方法において、前記ガラスクロスとして、微粒
子状無機充填材を全樹脂量に対し1〜5重量%添加した
エポキシ樹脂を予め含浸させたガラスクロスを使用する
ことを特徴とする積層板の製造方法に関するものであ
る。According to the present invention, an intermediate layer resin is applied on a glass cloth, and a glass non-woven fabric is further placed thereon, and the obtained two prepregs are placed with the glass non-woven fabric inside. In the method for manufacturing a composite laminate in which heating and pressurization are performed by superposition, as the glass cloth, a glass cloth pre-impregnated with an epoxy resin to which 1 to 5% by weight of a particulate inorganic filler is added based on the total resin amount is used. The present invention relates to a method for manufacturing a laminated board, which is a feature of the present invention.
【0005】[0005]
【発明の実施の形態】本発明では、微粒子状無機充填材
を1〜5重量%添加したエポキシ樹脂をガラスクロスに
含浸することにより、積層板の打抜き性を低下させるこ
となく、プリプレグ製造時中間層樹脂がガラスクロス反
対面からしみ出さないようにするものである。従来から
ガラスクロスの上に中間層樹脂を塗布する工程を有する
コンポジット積層板の製造方法の場合、中間層樹脂がガ
ラスクロスからしみ出さないようにする方法として、ガ
ラスクロスに、エポキシ樹脂を含浸させる方法では、ガ
ラスクロスの織り目空隙に対しエポキシ樹脂の引掛かり
が弱く、中間層樹脂が、予めガラスクロスに含浸させた
エポキシ樹脂と共に、ガラスクロスの織り目の空隙から
抜け落ちる。本発明では、ガラスクロスに含浸させるエ
ポキシ樹脂に微粒子状無機充填材を1〜5重量%添加し
ておくことにより、ガラスクロスの織り目空隙に微粒子
状無機充填材が引掛かり、この空隙を埋め、中間層樹脂
が抜け落ちることを防止する。DESCRIPTION OF THE PREFERRED EMBODIMENTS According to the present invention, an epoxy resin containing 1 to 5% by weight of a particulate inorganic filler is impregnated into a glass cloth so that the punching property of a laminate is not reduced, and an intermediate time during the production of a prepreg is reduced. This is to prevent the layer resin from exuding from the opposite side of the glass cloth. Conventionally, in the case of a method for producing a composite laminate having a step of applying an intermediate layer resin on a glass cloth, as a method of preventing the intermediate layer resin from exuding from the glass cloth, the glass cloth is impregnated with an epoxy resin. In the method, the epoxy resin is weakly caught by the textured voids of the glass cloth, and the interlayer resin falls out of the textured voids of the glass cloth together with the epoxy resin previously impregnated into the glass cloth. In the present invention, by adding 1 to 5% by weight of the particulate inorganic filler to the epoxy resin impregnated into the glass cloth, the particulate inorganic filler is caught in the textured voids of the glass cloth and fills the voids. Prevents the interlayer resin from falling off.
【0006】ガラスクロスに含浸させるエポキシ樹脂に
微粒子状無機充填材を5重量%を越えて添加すると、微
粒子状無機充填材が中間層樹脂とガラスクロスに含浸さ
れたエポキシ樹脂との界面での架橋構造の妨げとなり、
中間層樹脂とエポキシ樹脂含浸ガラスクロスとの密着性
が弱まり打抜き性が低下する。また、1重量%未満で
は、中間層樹脂がガラスクロス反対面からしみ出さない
ためには十分な効果が得られない。本発明の目的を達成
するために、微粒子状無機充填材の粒径は、平均粒径で
100nm〜100μmのものが好ましい。100nm
より小さいと含浸するワニス粘度が高くなり取扱いが難
しくガラスクロスへの含浸性も低下する。100μmよ
り大きいとガラスクロスからしみ出し防止効果が小さく
なる。特に好ましい範囲は200〜700nmである。When more than 5% by weight of a particulate inorganic filler is added to an epoxy resin impregnated in a glass cloth, the particulate inorganic filler is crosslinked at the interface between the interlayer resin and the epoxy resin impregnated in the glass cloth. Hinder the structure,
The adhesiveness between the intermediate layer resin and the glass cloth impregnated with the epoxy resin is weakened, and the punching property is reduced. If the content is less than 1% by weight, a sufficient effect cannot be obtained because the interlayer resin does not exude from the opposite surface of the glass cloth. In order to achieve the object of the present invention, the fine particle inorganic filler preferably has an average particle diameter of 100 nm to 100 μm. 100nm
If it is smaller, the viscosity of the varnish to be impregnated becomes high, handling becomes difficult, and the impregnating property to the glass cloth also decreases. If it is larger than 100 μm, the effect of preventing seepage from the glass cloth is reduced. A particularly preferred range is from 200 to 700 nm.
【0007】本発明において、ガラスクロスに含浸させ
るエポキシ樹脂に添加する微粒子状無機充填材は、微粒
子シリカ、微粒子アルミニウム化合物、微粒子マグネシ
ウム化合物、微粒子カルシウム化合物等があり、特に限
定されないが、粒径が上記200〜700nmの範囲に
入る微粒子微粒子シリカが好ましい。In the present invention, the particulate inorganic filler to be added to the epoxy resin impregnated in the glass cloth includes particulate silica, particulate aluminum compound, particulate magnesium compound, particulate calcium compound and the like, and is not particularly limited. The fine particle silica in the range of 200 to 700 nm is preferable.
【0008】本発明において、中間層樹脂としてエポキ
シ樹脂が使用されるが、通常、ビスフェノ−ルA型エポ
キシ樹脂及び又はハロゲン化ビスフェノールA型エポキ
シ樹脂を主成分とし、さらに必要に応じてノボラック型
エポキシ樹脂を配合した樹脂組成物が使用される。中間
層樹脂には、通常、耐燃性、耐熱性等の向上のために無
機充填材を樹脂分100重量部に対して50〜150重
量部配合する。無機充填材は特に限定されるものではな
く、コンポジット積層板に使用されるものであればいか
なるものでも使用可能である。本発明において、ガラス
不織布は、通常目付け量20〜150g/m2 のものが
使用される。In the present invention, an epoxy resin is used as a resin for the intermediate layer. Usually, a bisphenol A type epoxy resin and / or a halogenated bisphenol A type epoxy resin are used as a main component, and if necessary, a novolak type epoxy resin is used. A resin composition containing a resin is used. In general, the intermediate layer resin is blended with 50 to 150 parts by weight of an inorganic filler for 100 parts by weight of the resin in order to improve the flame resistance, heat resistance and the like. The inorganic filler is not particularly limited, and any inorganic filler can be used as long as it is used for a composite laminate. In the present invention, a glass nonwoven fabric having a basis weight of 20 to 150 g / m 2 is used.
【0009】本発明において、ガラスクロスに微粒子状
無機充填材、好ましくはその一部又は全部として微粒子
シリカを添加したエポキシ樹脂を含浸し加熱乾燥後、中
間層樹脂を塗布し、その上にガラス不織布を載置しさら
に加熱乾燥してプリプレグを得る。このプリプレグは2
枚ガラス不織布面を内側にして重ね合わせ、必要により
その片面又は両面に銅箔を重ね、加熱加圧して目的とす
るコンポジット積層板を得ることができる。In the present invention, a glass cloth is impregnated with a particulate inorganic filler, preferably an epoxy resin to which a particulate silica is added as a part or all thereof, dried by heating, coated with an intermediate layer resin, and a glass non-woven fabric is placed thereon. Is placed and further dried by heating to obtain a prepreg. This prepreg is 2
The sheets are laminated with the glass nonwoven fabric surface inside, and copper foil is laminated on one side or both sides as necessary, and the resulting composite laminate can be obtained by heating and pressing.
【0009】[0009]
【実施例】実施例1〜2及び比較例1〜2 ガラスクロスに含浸させるエポキシ樹脂ワニスとして、
ビスフェノ−ルA型エポキシ樹脂、臭素化ビスフェノー
ルA型エポキシ樹脂、ノボラック型エポキシ樹脂、テト
ラブロムビスフェノ−ルA、ノボラック型フェノール樹
脂、及び硬化促進剤として2−エチル−4−メチルイミ
ダゾ−ルを使用した。実施例1と比較例2においては、
微粒子シリカを添加し、実施例2においては水酸化アル
ミニウムを添加した。各成分は表1に示す割合にて配合
した。Examples Examples 1-2 and Comparative Examples 1-2 As epoxy resin varnish impregnated in glass cloth,
Bisphenol A type epoxy resin, brominated bisphenol A type epoxy resin, novolak type epoxy resin, tetrabromobisphenol A, novolak type phenol resin, and 2-ethyl-4-methylimidazole as a curing accelerator. used. In Example 1 and Comparative Example 2,
Fine particle silica was added, and in Example 2, aluminum hydroxide was added. Each component was blended in the ratio shown in Table 1.
【0010】[0010]
【表1】 [Table 1]
【0011】また、中間層樹脂として、ビスフェノ−ル
A型エポキシ樹脂、臭素化ビスフェノールA型エポキシ
樹脂、ジシアンジアミド、及び硬化促進剤として2−エ
チル−4−メチルイミダゾ−ルを用い、水酸化アルミニ
ウムを主成分とする無機充填材を配合した。各成分の配
合割合を表2に示した。Also, bisphenol A type epoxy resin, brominated bisphenol A type epoxy resin, dicyandiamide as the intermediate layer resin, and 2-ethyl-4-methylimidazole as a curing accelerator are used, and aluminum hydroxide is used. An inorganic filler as a main component was blended. Table 2 shows the mixing ratio of each component.
【0012】[0012]
【表2】 [Table 2]
【0013】(注1)ビスA型エポキシ樹脂:エピクロ
ン850(エポキシ当量190、大日本インキ化学
(株)製) (注2)臭素化ビスA型エポキシ樹脂:GX153(エ
ポキシ当量400、大日本インキ化学(株)製) (注3)クレゾ−ルノボラック型エポキシ樹脂:エピコ
−ト180S75(エポキシ当量210、油化シェルエ
ポキシ(株)製) (注4)ノボラック型フェノール樹脂:PR−5147
0(住友デュレズ(株)製) (注5)微粒子シリカ:カ−プレックス#67(シオノ
ギ製薬(株)製) (注6)水酸化アルミニウム:CL−310(住友化学
(株)製)(Note 1) Bis A type epoxy resin: Epicron 850 (epoxy equivalent 190, manufactured by Dainippon Ink and Chemicals, Inc.) (Note 2) Brominated bis A type epoxy resin: GX153 (epoxy equivalent 400, Dainippon Ink (Chemical Co., Ltd.) (Note 3) Cresol-novolak type epoxy resin: Epicoat 180S75 (Epoxy equivalent 210, manufactured by Yuka Shell Epoxy Co., Ltd.) (Note 4) Novolak type phenol resin: PR-5147
0 (manufactured by Sumitomo Durez Co., Ltd.) (Note 5) Fine particle silica: Carplex # 67 (manufactured by Shionogi Pharmaceutical Co., Ltd.) (Note 6) Aluminum hydroxide: CL-310 (manufactured by Sumitomo Chemical Co., Ltd.)
【0014】前記エポキシ樹脂ワニスをガラスクロス
(200g/cm2 )に含浸し、次いで、中間層樹脂を
塗布し加熱乾燥しつつ、その上にガラス不織布(100
g/cm2 )を載置し、加熱乾燥してプリプレグを得
た。このプリプレグ2枚をガラス不織布面を内側にして
重ね合わせ、この両表面に銅箔を重ね、加熱加圧してコ
ンポジット積層板を得た。プリプレグ製造課程におい
て、中間層樹脂塗布後、中間層樹脂のガラスクロス反対
面からのしみ出しを観察した。そして、得られたコンポ
ジット積層板の打抜き性を測定した。結果を表3に示
す。A glass cloth (200 g / cm 2 ) is impregnated with the epoxy resin varnish, and then an intermediate layer resin is applied and dried by heating.
g / cm 2 ) and heated and dried to obtain a prepreg. The two prepregs were overlapped with the glass nonwoven fabric surface inside, copper foils were overlapped on both surfaces, and heated and pressed to obtain a composite laminate. In the prepreg manufacturing process, after the application of the intermediate layer resin, seepage of the intermediate layer resin from the opposite surface of the glass cloth was observed. And the punching property of the obtained composite laminate was measured. Table 3 shows the results.
【0015】[0015]
【表3】 [Table 3]
【0016】(評価方法) 1. 中間層樹脂のしみ出し(プリプレグ製造時) ○:中間層樹脂がガラスクロスの反対面側にしみ出な
い。 ×:中間層樹脂がガラスクロスの反対面側にしみ出る。 2.打抜き性:エッチングにより銅箔を除去した140
×140mmの積層板を、0.7mmφ、2.0mmピッ
チの連続穴、及び1.0mmφ、2.5mmピッチの連続
穴の開けられる金型を用いて100トン打抜きプレス
(遠藤プレス(株)製)で打ち抜いた。 ○:クラック、穴周りに剥離が生じない。 △:クラックなし、穴間を直結しない剥離が生じる。 ×:クラック、または、穴間を直結する剥離が生じる。(Evaluation method) Exudation of intermediate layer resin (at the time of prepreg production) ○: Intermediate layer resin does not exude to the opposite side of glass cloth. X: The intermediate layer resin exudes on the opposite side of the glass cloth. 2. Punching property: 140 from which copper foil was removed by etching
A 100-ton punching press (manufactured by Endo Press Co., Ltd.) is used to mold a laminated plate of × 140 mm using a mold capable of forming continuous holes of 0.7 mmφ, 2.0 mm pitch, and continuous holes of 1.0 mmφ, 2.5 mm pitch. ). :: No cracking or peeling around holes. Δ: No crack, peeling not directly connecting between holes occurs. ×: Cracking or peeling directly connecting the holes occurs.
【0017】[0017]
【発明の効果】本発明は、ガラスクロスの上に中間層樹
脂を塗布し、さらに、その上にガラス不織布を載置し、
得られたプリプレグ2枚をガラス不織布を内側にして重
ね合わせ加熱加圧するコンポジット積層板の製造方法に
おいて、ガラスクロスに微粒子状無機充填材を添加した
エポキシ樹脂をガラスクロスに含浸させることにより、
打抜き性等の特性を低下させること無く、プリプレグ製
造時に中間層樹脂がガラスクロス反対面からしみ出さな
いようにすることができる。従って、本発明の方法は、
コンポジット積層板の特性を低下させることなく、生産
効率を向上させることが出来るのでその工業的価値は極
めて大なるものである。According to the present invention, an intermediate layer resin is applied on a glass cloth, and further, a glass nonwoven fabric is placed thereon.
In a method for producing a composite laminate in which two obtained prepregs are laminated and heated and pressed with the glass nonwoven fabric inside, the glass cloth is impregnated with an epoxy resin added with a particulate inorganic filler,
The intermediate layer resin can be prevented from exuding from the opposite surface of the glass cloth at the time of prepreg production without deteriorating properties such as punching properties. Thus, the method of the present invention
Since the production efficiency can be improved without deteriorating the properties of the composite laminate, its industrial value is extremely large.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 FI テーマコート゛(参考) C08L 63/00 C08L 63/00 C Fターム(参考) 4F072 AB09 AB29 AD24 AD28 AD29 AF03 AF06 AG03 4F100 AA19H AA20A AB17 AB33 AG00A AG00C AK01B AK53A BA05 BA06 BA10A BA13 CA23 CA23A DE01A DG12A DG15C DH01A EH012 EH461 EJ202 EJ421 EJ422 EJ82A EJ861 GB43 JK20 JL02 JL06 YY00A 4J002 CD051 CD061 CD121 DE076 DE146 DJ016 FD016 GF00──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) C08L 63/00 C08L 63/00 C FF term (Reference) 4F072 AB09 AB29 AD24 AD28 AD29 AF03 AF06 AG03 4F100 AA19H AA20A AB17 AB33 AG00A AG00C AK01B AK53A BA05 BA06 BA10A BA13 CA23 CA23A DE01A DG12A DG15C DH01A EH012 EH461 EJ202 EJ421 EJ422 EJ82A EJ861 GB43 JK20 JL02 JL06 YY00A 4J002 CD051 CD061 CD121 DE076 DE076
Claims (3)
し、さらに、その上にガラス不織布を載置し、得られた
プリプレグ2枚をガラス不織布を内側にして重ね合わせ
加熱加圧するコンポジット積層板の製造方法において、
前記ガラスクロスとして、微粒子状無機充填材微粒子シ
リカを全樹脂量に対し1〜5重量%添加したエポキシ樹
脂を予め含浸させたガラスクロスを使用することを特徴
とする積層板の製造方法。1. A composite laminate in which an intermediate layer resin is applied on a glass cloth, a glass nonwoven fabric is further placed thereon, and two obtained prepregs are overlapped with the glass nonwoven fabric inside and heated and pressed. In the manufacturing method of
A method for producing a laminated board, wherein a glass cloth pre-impregnated with an epoxy resin containing 1 to 5% by weight of a particulate inorganic filler fine particle silica based on the total resin amount is used as the glass cloth.
粒子シリカである請求項1記載の積層板の製造方法。2. The method for producing a laminate according to claim 1, wherein a part or all of the particulate inorganic filler is particulate silica.
が、ノボラック型エポキシ樹脂、とビスフェノ−ルA型
エポキシ樹脂及び又はハロゲン化ビスフェノールA型エ
ポキシ樹脂を主成分とするエポキシ樹脂である請求項1
又は2記載の積層板の製造方法。3. The epoxy resin impregnated in the glass cloth is a novolak type epoxy resin, an epoxy resin containing a bisphenol A type epoxy resin and / or a halogenated bisphenol A type epoxy resin as a main component.
Or the manufacturing method of the laminated plate of 2.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP04784299A JP4206548B2 (en) | 1999-02-25 | 1999-02-25 | Laminate production method |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP04784299A JP4206548B2 (en) | 1999-02-25 | 1999-02-25 | Laminate production method |
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JP4206548B2 JP4206548B2 (en) | 2009-01-14 |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2003012893A (en) * | 2001-07-02 | 2003-01-15 | Toray Ind Inc | Epoxy resin composition and method for repairing/ reinforcing concrete structure using the composition |
JP2007161979A (en) * | 2005-11-16 | 2007-06-28 | Hitachi Chem Co Ltd | Resin composition for lamianted board, prepreg for laminated board using the same, the resultant laminated board, and metal-clad laminated board |
-
1999
- 1999-02-25 JP JP04784299A patent/JP4206548B2/en not_active Expired - Fee Related
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2003012893A (en) * | 2001-07-02 | 2003-01-15 | Toray Ind Inc | Epoxy resin composition and method for repairing/ reinforcing concrete structure using the composition |
JP2007161979A (en) * | 2005-11-16 | 2007-06-28 | Hitachi Chem Co Ltd | Resin composition for lamianted board, prepreg for laminated board using the same, the resultant laminated board, and metal-clad laminated board |
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JP4206548B2 (en) | 2009-01-14 |
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