JPH05138808A - Copper clad laminated sheet - Google Patents
Copper clad laminated sheetInfo
- Publication number
- JPH05138808A JPH05138808A JP32801391A JP32801391A JPH05138808A JP H05138808 A JPH05138808 A JP H05138808A JP 32801391 A JP32801391 A JP 32801391A JP 32801391 A JP32801391 A JP 32801391A JP H05138808 A JPH05138808 A JP H05138808A
- Authority
- JP
- Japan
- Prior art keywords
- epoxy resin
- inorganic filler
- copper
- copper clad
- coupling agent
- 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.)
- Pending
Links
Landscapes
- Epoxy Resins (AREA)
- Laminated Bodies (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、熱的特性やスルーホー
ル信頼性に優れ、またボイドの発生が少なく、製造面で
も作業性のよい銅張積層板に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a copper clad laminate having excellent thermal characteristics and through hole reliability, little void generation, and good workability in manufacturing.
【０００２】[0002]
【従来の技術】近年、ＩＣ、ＬＳＩ等の集積回路を使用
した電子・電気機器の発達はめざましく、それらに使用
される銅張積層板も多種多様となり、かつ一段と優れた
特性が要求されるようになってきた。ガラス不織布を基
材とする銅張積層板では、ガラス織布を基材する銅張積
層板と電気特性が同等であり、寸法安定性、スルーホー
ル信頼性も優れ、かつ打抜加工に優れていることから、
その需要が急速に伸びてきた。2. Description of the Related Art In recent years, the development of electronic / electrical devices using integrated circuits such as ICs and LSIs has been remarkable, and the copper clad laminates used for them have been diversified, and further excellent characteristics are required. Has become. The copper-clad laminate based on non-woven glass has the same electrical characteristics as the copper-clad laminate based on woven glass, and has excellent dimensional stability and through-hole reliability, as well as excellent punching processing. Because
The demand has increased rapidly.
【０００３】また、ガラス不織布を基材とする銅張積層
板に使用されるエポキシ樹脂は、厳しい要求特性に対応
すべく種々改良が加えられてまた。すなわち、半田耐熱
性や耐熱衝撃性、硬化収縮や熱膨張係数、耐トラッキン
グ性など、熱的・電気的・機械的特性を向上するため、
無機充填剤を配合することがおこなわれているが、未だ
十分満足すべきものが得られていない。Further, the epoxy resin used for the copper clad laminate having a glass non-woven fabric as a base material has been subjected to various improvements in order to meet strict requirements. That is, in order to improve the thermal / electrical / mechanical properties such as solder heat resistance, thermal shock resistance, curing shrinkage, thermal expansion coefficient, and tracking resistance,
Inorganic fillers have been added, but satisfactory results have not been obtained yet.
【０００４】銅張積層板に無機充填剤を大量に配合する
と、基材に含浸するエポキシ樹脂ワニスの粘度が上昇
し、これを塗布含浸するとき基材に塗布むらが生じ、ボ
イドや板厚不良の原因となる欠点がある。粘度を下げる
ため無機充填剤を減少させると特に半田耐熱性、耐熱衝
撃性などの特性が低下する欠点がある。これらを改良す
るため、無機充填剤を大量に配合する一方、これにシラ
ンカップリング剤を添加するということが試みられてい
るが、なお十分な効果が得られていない。When a large amount of an inorganic filler is added to a copper-clad laminate, the viscosity of the epoxy resin varnish impregnated into the base material increases, and when this is applied and impregnated, coating unevenness occurs on the base material, resulting in voids and defective plate thickness. There is a drawback that causes If the amount of the inorganic filler is reduced to reduce the viscosity, there is a drawback that properties such as solder heat resistance and thermal shock resistance are deteriorated. In order to improve these, it has been attempted to add a silane coupling agent to a large amount of an inorganic filler, but the sufficient effect has not been obtained yet.
【０００５】[0005]
【発明が解決しようとする課題】本発明は、上記の事情
に鑑みてなされたもので、耐熱性、耐熱衝撃性、スルー
ホール信頼性に優れ、かつボイドの発生が少なく、作業
性のよい、ガラス不織布主基材の銅張積層板を提供しよ
うとするものである。SUMMARY OF THE INVENTION The present invention has been made in view of the above circumstances, and is excellent in heat resistance, thermal shock resistance, through hole reliability, and has less voids and good workability. It is intended to provide a copper clad laminate having a glass non-woven fabric main substrate.
【０００６】[0006]
【課題を解決するための手段】本発明者は、上記の目的
を達成しようと鋭意研究を重ねた結果、無機充填剤の一
定量とチタネートカップリング剤を配合することによっ
て、上記の目的を達成できることを見いだし、本発明を
完成させたものである。Means for Solving the Problems As a result of intensive research aimed at achieving the above object, the present inventor achieved the above object by blending a fixed amount of an inorganic filler and a titanate coupling agent. The inventors have found what can be done and completed the present invention.
【０００７】即ち、本発明は、ガラス不織布にエポキシ
樹脂を含浸乾燥させたプリプレグ（I ）の両面に、ガラ
ス織布にエポキシ樹脂を含浸乾燥させたプリプレグ（I
I）を重ね合わせ、その少なくとも片面に銅箔を配置し
加熱加圧一体に成形する銅張積層板において、前記プリ
プレグ（I ）に含浸する樹脂として、エポキシ樹脂、硬
化剤、無機充填剤およびチタネートカップリング剤を必
須成分とし、かつエポキシ樹脂 100重量部に対し無機充
填剤を35〜90重量部を配合してなるエポキシ樹脂組成物
を用いることを特徴とする銅張積層板である。That is, according to the present invention, a glass woven fabric is impregnated with an epoxy resin and dried on both sides of a prepreg (I) obtained by impregnating and drying a glass nonwoven fabric with an epoxy resin.
In a copper-clad laminate in which I) are superposed and a copper foil is placed on at least one surface of the prepreg (I) to be integrally molded under heat and pressure, epoxy resin, curing agent, inorganic filler and titanate are used as the resin with which the prepreg (I) is impregnated. A copper-clad laminate characterized by using an epoxy resin composition comprising a coupling agent as an essential component and an inorganic filler in an amount of 35 to 90 parts by weight with respect to 100 parts by weight of an epoxy resin.
【０００８】以下、本発明を詳細に説明する。The present invention will be described in detail below.
【０００９】本発明に用いるエポキシ樹脂組成物は、エ
ポキシ樹脂、硬化剤、無機充填剤およびチタネートカッ
プリング剤を必須成分とするものである。通常積層板用
として使用されている全てのエポキシ樹脂が、ここで用
いるエポキシ樹脂として使用することができる。例え
ば、ビスフェノールＡ型エポキシ樹脂、ビスフェノール
Ｆ型エポキシ樹脂、ノボラック型エポキシ樹脂、臭素化
エポキシ樹脂等が挙げられ、これらは単独もしくは 2種
以上混合して使用することができる。The epoxy resin composition used in the present invention contains an epoxy resin, a curing agent, an inorganic filler and a titanate coupling agent as essential components. All epoxy resins commonly used for laminates can be used as the epoxy resin used here. Examples thereof include bisphenol A type epoxy resin, bisphenol F type epoxy resin, novolac type epoxy resin and brominated epoxy resin, and these can be used alone or in combination of two or more.
【００１０】エポキシ樹脂組成物に用いる硬化剤として
は、ジシアンジアミド、ジアミノジフェニルスルホン、
第三アミン塩、三フッ化ホウ素塩等が挙げられ、これら
は単独もしくは 2種以上混合して使用することができ
る。As the curing agent used in the epoxy resin composition, dicyandiamide, diaminodiphenyl sulfone,
Examples thereof include tertiary amine salts and boron trifluoride salts, which can be used alone or in admixture of two or more.
【００１１】エポキシ樹脂組成物に用いる無機充填剤と
しては、タルク、シリカ、アルミナ、水酸化アルミニウ
ム、三酸化アンチモン等が挙げられ、これらは単独もし
くは2種以上混合して使用することができる。無機充填
剤の配合割合は、エポキシ樹脂 100重量部に対して35〜
90重量部配合することが望ましい、配合割合が35重量部
未満であると、耐熱性、耐熱衝撃性の向上が期待できな
い。また、90重量部を超えると粘度が増大して、塗布含
浸した基材に塗布むらが生じ、ボイドや板厚不良とな
り、また、耐熱衝撃性も低下し好ましくない。これは樹
脂中の無機充填剤が、応力集中源となって材料を脆弱化
させ、無機充填剤の補強効果を上回るためと推測され
る。Examples of the inorganic filler used in the epoxy resin composition include talc, silica, alumina, aluminum hydroxide, antimony trioxide and the like, and these can be used alone or in admixture of two or more. The blending ratio of the inorganic filler is 35 to 100 parts by weight of the epoxy resin.
It is desirable to add 90 parts by weight, and if the mixing ratio is less than 35 parts by weight, improvement in heat resistance and thermal shock resistance cannot be expected. On the other hand, if it exceeds 90 parts by weight, the viscosity is increased, resulting in coating unevenness on the substrate impregnated with the coating, resulting in voids and poor plate thickness, and also reduced thermal shock resistance, which is not preferable. It is speculated that this is because the inorganic filler in the resin serves as a stress concentration source to weaken the material and exceeds the reinforcing effect of the inorganic filler.
【００１２】また、エポキシ樹脂組成物に用いるチタネ
ートカップリング剤としては、イソプロピルトリデシル
ベンゼンスルホニルチタネート、テトライソプロピルビ
ス（ジオクチルホスファイト）チタネート、テトラオク
チルビス（ジトリデシルホスファイト）チタネート、テ
トラ（2,2-ジアリルオキシメチル−1-ブチル）ビス（ジ
トリデシル）ホスファイトチタネート等が挙げられ、こ
れらは単独もしくは 2種以上混合して使用することがで
きる。チタネートカップリング剤の配合方法としては、
これを他の成分と一緒に配合してもよいし、また、予め
無機充填剤に施したものを使用することもできる。The titanate coupling agent used in the epoxy resin composition includes isopropyltridecylbenzenesulfonyl titanate, tetraisopropylbis (dioctylphosphite) titanate, tetraoctylbis (ditridecylphosphite) titanate, tetra (2,2, Examples thereof include 2-diallyloxymethyl-1-butyl) bis (ditridecyl) phosphite titanate, which can be used alone or in combination of two or more kinds. As a method of blending the titanate coupling agent,
This may be blended with other components, or the one previously applied to the inorganic filler may be used.
【００１３】エポキシ樹脂組成物は、エポキシ樹脂、硬
化剤、無機充填剤およびチタネートカップリング剤を必
須成分とするが、本発明の目的に反しない範囲におい
て、硬化促進剤その他の成分を添加配合することができ
る。The epoxy resin composition contains an epoxy resin, a curing agent, an inorganic filler and a titanate coupling agent as essential components, but a curing accelerator and other components are added and blended within the range not deviating from the object of the present invention. be able to.
【００１４】エポキシ樹脂組成物をワニスとして調製す
るには、エポキシ樹脂を溶剤に溶解し、硬化剤及び硬化
促進剤を加えて攪拌し、次に無機充填剤およびチタネー
トカップリング剤を配合し、均一に混合してワニスとす
る。こうして得られたワニスは、ガラス不織布に含浸乾
燥させてプリプレグ（Ｉ）をつくる。別に、無機充填剤
およびチタネートカップリング剤を含まないワニス（エ
ポキシ樹脂溶液）は、それをガラス織布に含浸乾燥させ
てプリプレグ（II）をつくる。プリプレグ（Ｉ）の複数
枚を重ね合わせ、その両側にプリプレグ（II）を重ね、
更にその少なくとも片側に銅箔を配置して、加熱加圧一
体に成形して銅張積層板を製造することができる。こう
して製造された銅張積層板は、電子・電気機器の配線板
に使用される。To prepare an epoxy resin composition as a varnish, the epoxy resin is dissolved in a solvent, a curing agent and a curing accelerator are added, and the mixture is stirred, then an inorganic filler and a titanate coupling agent are added, and the mixture is homogenized. Mix with to make a varnish. The varnish thus obtained is impregnated into a glass nonwoven fabric and dried to prepare a prepreg (I). Separately, a varnish (epoxy resin solution) containing no inorganic filler and titanate coupling agent is impregnated into a woven glass cloth and dried to form a prepreg (II). Multiple pieces of prepreg (I) are piled up, and prepreg (II) is piled up on both sides,
Further, a copper foil may be disposed on at least one side of the copper foil, and the copper foil and the copper clad laminate may be manufactured by heat and pressure integral molding. The copper clad laminate thus manufactured is used for a wiring board of electronic / electrical equipment.
【００１５】[0015]
【作用】本発明は、比較的大量の無機充填剤とともにチ
タネートカップリング剤を併用することによって、耐熱
性、耐熱衝撃性に優れ、しかもボイドの発生が少なく、
作業性のよいガラス不織布主基材の銅張積層板を得るこ
とができたものである。即ち、無機充填剤を35〜90重量
部配合することによって、耐熱性、耐熱衝撃性を向上さ
せ、また、チタネートカップリング剤の使用により、作
業性を良くしかつボイドの発生を抑えることができた。
さらにチタネートカップリング剤を用いることによっ
て、ある種の可撓性が付与され一段と耐熱衝撃性などが
向上するものと考えられる。The present invention is excellent in heat resistance and thermal shock resistance by using a titanate coupling agent together with a relatively large amount of an inorganic filler, and further, the generation of voids is small.
It was possible to obtain a copper clad laminate having a glass non-woven fabric main substrate with good workability. That is, by adding 35 to 90 parts by weight of an inorganic filler, heat resistance and thermal shock resistance can be improved, and by using a titanate coupling agent, workability can be improved and generation of voids can be suppressed. It was
Further, it is considered that the use of the titanate coupling agent imparts a certain degree of flexibility and further improves the thermal shock resistance.
【００１６】[0016]
【実施例】次に本発明を実施例によって説明するが、本
発明はこれらの実施例によって限定されるものではな
い。以下の実施例及び比較例において、「部」とは「重
量部」を意味する。EXAMPLES The present invention will now be described with reference to examples, but the present invention is not limited to these examples. In the following Examples and Comparative Examples, "part" means "part by weight".
【００１７】実施例１ ビスフェノールＡ型エポキシ樹脂（エポキシ当量 480）
100部をメチルエチルケトン35部に溶解し、ジシアンジ
アミド 3部と2-エチル-4−メチルイミダゾール0.1部を
加えて攪拌し、無機充填剤として水酸化アルミニウム50
部、チタネートカップリング剤としてテトラオクチルビ
ス（ジトリデシルホスファイト）チタネート 0.5部配合
し、均一に攪拌混合してワニスを調製した。Example 1 Bisphenol A type epoxy resin (epoxy equivalent 480)
Dissolve 100 parts in 35 parts of methyl ethyl ketone, add 3 parts of dicyandiamide and 0.1 part of 2-ethyl-4-methylimidazole, stir, and mix with 50% aluminum hydroxide as an inorganic filler.
Parts, and 0.5 parts of tetraoctyl bis (ditridecyl phosphite) titanate as a titanate coupling agent were mixed and uniformly mixed with stirring to prepare a varnish.
【００１８】このワニスを用いて、ガラス不織布に連続
的に含浸させ、 165℃に保持したオーブンで 6分間乾燥
させてプリプレグ（Ｉ）を作った。プリプレグ（Ｉ）を
6枚重ね合わせ、その両面に別に準備した無機充填剤、
チタネートカップリング剤を含まないエポキシ樹脂ワニ
スをガラス織布に含浸乾燥させたプリプレグ（II）を重
ね合わせ、さらにその両面に厚さ16μm の銅箔を配置し
て、 170℃に加熱した熱盤に挟み、50kg／cm2 の圧力で
90分間加熱加圧一体に成形して銅張積層板を製造した。A glass non-woven fabric was continuously impregnated with this varnish and dried in an oven maintained at 165 ° C. for 6 minutes to prepare a prepreg (I). Prepreg (I)
6 sheets stacked, inorganic fillers prepared separately on both sides,
Epoxy resin varnish containing no titanate coupling agent was impregnated into glass woven fabric, and dried prepreg (II) was placed on top of each other, and 16 μm thick copper foil was placed on both sides of the prepreg (II) and placed on a heating plate heated to 170 ° C. With a pressure of 50 kg / cm 2
A copper clad laminate was manufactured by integrally molding for 90 minutes under heat and pressure.
【００１９】実施例２ 実施例１のワニスの配合において、水酸化アルミニウム
を80部、テトラオクチルビス（ジトリデシルホスファイ
ト）チタネートを 0.8部に、配合量をそれぞれ増加した
以外は、すべて実施例１と同一にしてワニスを調製し
た。このワニスを用いて実施例１と同一条件で銅張積層
板を製造した。Example 2 In the formulation of the varnish of Example 1, except that aluminum hydroxide was 80 parts, tetraoctylbis (ditridecylphosphite) titanate was 0.8 parts, and the compounding amounts were respectively increased, Example 1 A varnish was prepared in the same manner as above. Using this varnish, a copper clad laminate was manufactured under the same conditions as in Example 1.
【００２０】比較例１ 実施例１のワニスの配合において、チタネートカップリ
ング剤の替わりにシランカップリング剤として3-グリシ
ドキシプロピルトリメトキシシラン 0.5部を配合した以
外は、実施例１と同様にしてワニス、銅張積層板を製造
した。Comparative Example 1 The same procedure as in Example 1 was repeated except that 0.5 part of 3-glycidoxypropyltrimethoxysilane was added as a silane coupling agent in place of the titanate coupling agent in the formulation of the varnish of Example 1. To produce a varnish and a copper clad laminate.
【００２１】比較例２ 実施例１のワニスの配合において、水酸化アルミニウ
ム、テトラオクチルビス（ジトリデシルホスファイト）
チタネートを配合しないで、実施例１と同様にしてワニ
ス、銅張積層板を製造した。Comparative Example 2 In the formulation of the varnish of Example 1, aluminum hydroxide and tetraoctylbis (ditridecyl phosphite) were used.
A varnish and a copper clad laminate were produced in the same manner as in Example 1 without adding titanate.
【００２２】実施例１〜２及び比較例１〜２で製造した
銅張積層板について、半田耐熱性、耐熱衝撃性、スルー
ホール信頼性、ボイドの発生状況を試験したので、その
結果を表１に示した。本発明は、いずれの特性において
も優れており、本発明の効果が確認された。The copper clad laminates produced in Examples 1 and 2 and Comparative Examples 1 and 2 were tested for solder heat resistance, thermal shock resistance, through hole reliability, and void generation. The results are shown in Table 1. It was shown to. The present invention is excellent in all characteristics, and the effect of the present invention was confirmed.
【００２３】[0023]
【表１】 ＊1 ：銅張積層板25mm×25mmの試験片を 260℃及び 280
℃の半田浴に浮かべ、フクレの発生するまでの時間を試
験した、 ＊2 ：銅箔をエッチングした50mm×50mmの試験片10個
を、 122℃，1atm， 7時間の条件で前処理をした後、 2
60℃の半田浴に30秒間ディップし、フクレの発生の有無
を調べた、 ＊3 ： 200穴の導通したスルーホール基板をつくり、 2
60℃のオイルに10秒間浸漬した後に20℃のオイルに10秒
間浸漬することを 1サイクルとし、各サイクル毎に導通
抵抗を測定し、断線するまでのサイクル数を試験した、 ＊4 ：成形した銅張積層板30枚中にボイドが発生した銅
張積層板の枚数を調べた。[Table 1] * 1: A copper-clad laminate 25 mm × 25 mm test piece is used at 260 ° C and 280
Floating in a solder bath at ℃ was tested for blistering time. * 2: 10 50mm x 50mm test pieces with copper foil etched were pretreated under the conditions of 122 ℃, 1atm, and 7 hours. After 2
It was dipped in a solder bath at 60 ° C for 30 seconds and checked for blister formation. * 3: A 200-hole conductive through-hole board was made.
Soaking in oil at 60 ℃ for 10 seconds and then in oil at 20 ℃ for 10 seconds was set as one cycle, the conduction resistance was measured for each cycle, and the number of cycles until disconnection was tested. * 4: Molded The number of copper-clad laminates in which a void occurred in 30 copper-clad laminates was examined.
【００２４】[0024]
【発明の効果】以上の説明及び表１から明らかなよう
に、本発明のガラス不織布主基材の銅張積層板は、耐熱
性、耐熱衝撃性、スルーホール信頼性に優れ、塗布含浸
等の作業性がよく、また、ボイドの発生が少なく、電子
・電気機器用として好適なものである。As is apparent from the above description and Table 1, the copper-clad laminate of the glass non-woven fabric main substrate of the present invention has excellent heat resistance, thermal shock resistance and through-hole reliability, and is excellent in coating impregnation. The workability is good, and the generation of voids is small, and it is suitable for electronic and electric devices.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.5 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｂ３２Ｂ 27/20 Ｚ 6122−4Ｆ 27/38 Ｃ０８Ｋ 3/00 7167−4Ｊ Ｃ０８Ｌ 63/00 ＮＫＹ 8830−4Ｊ Ｈ０５Ｋ 1/03 Ｋ 7011−4Ｅ ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 5 Identification code Office reference number FI Technical display location B32B 27/20 Z 6122-4F 27/38 C08K 3/00 7167-4J C08L 63/00 NKY 8830- 4J H05K 1/03 K 7011-4E
Claims (1)
させたプリプレグ（Ｉ）の両面に、ガラス織布にエポキ
シ樹脂を含浸乾燥させたプリプレグ（II）を重ね合わ
せ、その少なくとも片面に銅箔を配置し加熱加圧一体に
成形する銅張積層板において、前記プリプレグ（Ｉ）に
含浸する樹脂として、エポキシ樹脂、硬化剤、無機充填
剤およびチタネートカップリング剤を必須成分とし、か
つエポキシ樹脂 100重量部に対し前記無機充填剤を35〜
90重量部を配合してなるエポキシ樹脂組成物を用いるこ
とを特徴とする銅張積層板。1. A prepreg (I) obtained by impregnating and drying a glass woven fabric with an epoxy resin is laminated on both sides of a prepreg (I) obtained by impregnating and drying a glass nonwoven fabric with an epoxy resin, and a copper foil is arranged on at least one side thereof. In the copper-clad laminate which is integrally molded by heating and pressurizing, the epoxy resin, the curing agent, the inorganic filler and the titanate coupling agent are essential components as the resin to be impregnated in the prepreg (I), and the epoxy resin is 100 parts by weight. Against the above-mentioned inorganic filler 35 ~
A copper-clad laminate characterized by using an epoxy resin composition containing 90 parts by weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32801391A JPH05138808A (en) | 1991-11-16 | 1991-11-16 | Copper clad laminated sheet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32801391A JPH05138808A (en) | 1991-11-16 | 1991-11-16 | Copper clad laminated sheet |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05138808A true JPH05138808A (en) | 1993-06-08 |
Family
ID=18205543
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP32801391A Pending JPH05138808A (en) | 1991-11-16 | 1991-11-16 | Copper clad laminated sheet |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05138808A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997035457A1 (en) * | 1996-03-22 | 1997-09-25 | Alliedsignal Inc. | Fillers for improved epoxy laminates |
-
1991
- 1991-11-16 JP JP32801391A patent/JPH05138808A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997035457A1 (en) * | 1996-03-22 | 1997-09-25 | Alliedsignal Inc. | Fillers for improved epoxy laminates |
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