JP2011219766A - プリプレグおよび炭素繊維強化複合材料 - Google Patents
プリプレグおよび炭素繊維強化複合材料 Download PDFInfo
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- JP2011219766A JP2011219766A JP2011142641A JP2011142641A JP2011219766A JP 2011219766 A JP2011219766 A JP 2011219766A JP 2011142641 A JP2011142641 A JP 2011142641A JP 2011142641 A JP2011142641 A JP 2011142641A JP 2011219766 A JP2011219766 A JP 2011219766A
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- Prior art keywords
- fibers
- particles
- conductive
- core
- prepreg
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- Y10T442/2426—Elemental carbon containing
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- Y10T442/60—Nonwoven fabric [i.e., nonwoven strand or fiber material]
- Y10T442/643—Including parallel strand or fiber material within the nonwoven fabric
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Abstract
【解決手段】[A]炭素繊維と[B]熱硬化性樹脂を含み、かつ下記(1)、(2)の少なくともいずれか一方を満たすプリプレグ。(1)[C]熱可塑性樹脂の粒子または繊維、および[D]導電性の粒子または繊維を含み、[[C]の配合量(重量部)]/[[D]の配合量(重量部)]で表される重量比が1〜1000である。(2)[E]熱可塑性樹脂の核または芯が導電性物質で被覆された導電性の粒子または繊維を含む。
【選択図】なし
Description
(1)[C]熱可塑性樹脂の粒子または繊維、および[D]導電性の粒子または繊維を含み、[[C]の配合量(重量部)]/[[D]の配合量(重量部)]で表される重量比が1〜1000である。
(2)[E]熱可塑性樹脂の核または芯が導電性物質で被覆された導電性の粒子または繊維を含む。
(1)[C]熱可塑性樹脂の粒子または繊維、および[D]導電性の粒子または繊維を含み、[[C]の配合量(重量部)]/[[D]の配合量(重量部)]で表される重量比が1〜1000である。
(2)[E]熱可塑性樹脂の核または芯が導電性物質で被覆された導電性の粒子または繊維を含む。
(1)[C]熱可塑性樹脂の粒子または繊維、および[D]導電性の粒子または繊維を含み、[[C]の配合量(重量部)]/[[D]の配合量(重量部)]で表される重量比が1〜1000である。
(2)[E]熱可塑性樹脂の核または芯が導電性物質で被覆された導電性の粒子または繊維を含む。
(1)[C]熱可塑性樹脂の粒子または繊維、および[D]導電性の粒子または繊維
(2)[E]熱可塑性樹脂の核または芯が導電性物質で被覆された導電性の粒子または繊維。
・“トレカ(登録商標)”T800S−24K−10E(繊維数24,000本、引張強度5.9GPa、引張弾性率290GPa、引張伸度2.0%の炭素繊維、東レ(株)製)
・“トレカ(登録商標)”T700S−24K−50C(繊維数24,000本、引張強度4.9GPa、引張弾性率230GPa、引張伸度2.1%の炭素繊維、東レ(株)製)。
・ビスフェノールA型エポキシ樹脂、“エピコート(登録商標)”825(ジャパンエポキシレジン(株)製)
・テトラグリシジルジアミノジフェニルメタン、ELM434(住友化学(株)製)
・末端に水酸基を有するポリエーテルスルホン“スミカエクセル(登録商標)”PES5003P(住友化学(株)製)
・4,4’−ジアミノジフェニルスルホン(三井化学ファイン(株)製)。
・ナイロン12粒子SP−10(東レ(株)製、形状:真球)
・下記の製造方法で得られたエポキシ変性ナイロン粒子A
透明ポリアミド(商品名“グリルアミド(登録商標)”−TR55、エムザベルケ社製)90重量部、エポキシ樹脂(商品名“エピコート(登録商標)”828、油化シェル(株)社製)7.5重量部および硬化剤(商品名“トーマイド(登録商標)”#296、富士化成工業(株)社製)2.5重量部を、クロロホルム300重量部とメタノール100重量部の混合溶媒中に添加して均一溶液を得た。次に、得られた均一溶液を塗装用のスプレーガンを用いて霧状にして、良く撹拌して3000重量部のn−ヘキサンの液面に向かって吹き付けて溶質を析出させた。析出した固体を濾別し、n−ヘキサンで良く洗浄した後に、100℃の温度で24時間の真空乾燥を行い、真球状のエポキシ変性ナイロン粒子Aを得た。
・下記の製造方法で得られたTR−55短繊維
オリフィスを1個もうけた口金から吐出した透明ポリアミド(商品名“グリルアミド(登録商標)”−TR55、エムザベルケ社製)の繊維をカットし、断面形状が真円のTR−55短繊維(繊維長1mm)を得た。
・ジビニルベンゼンポリマー粒子にニッケルをメッキし、さらにその上に金をメッキした粒子“ミクロパール(登録商標)”AU215(積水化学(株)製、形状:真球、比重:1.8g/cm3、導電性層の厚さ:110nm、[核の体積]/[導電性層の体積]:22.8)。
粒子“ミクロパール(登録商標)”AU225(積水化学(株)製、形状:真球、比重:2.4g/cm3、導電性層の厚さ:200nm、[核の体積]/[導電性層の体積]:20.2)。
酢酸第1鉄(アルドリッチ社製)0.01gと酢酸コバルト4水和物(ナカライテスク社製)0.21gとをエタノール(ナカライテスク社製)40mLに加え、超音波洗浄機で10分間懸濁した。この懸濁液に、結晶性チタノシリケート粉末(エヌイーケムキャット社製“チタノシリケート(登録商標)”)(TS−1)2.0gを加え、超音波洗浄機で10分間処理し、60℃の恒温下でメタノールを除去することにより、TS−1の結晶表面に上記酢酸金属塩を担持した固体触媒を得た。
スパッタリング装置CFS−4ES−231(芝浦メカトロニクス(株)製)にエポキシ変成ナイロン粒子Aを10g基板に乗せ、ターゲットが銅、ガス成分がアルゴン、ガス圧が2.0×10−1Pa、基板の温度が80℃、電力が500Wの条件にて行い、導電性層の厚さが、110nmの導電性粒子Cを作製した。導電性粒子の形状は真球、比重は、1.4g/cm3、[核の体積]/[導電性層の体積]は18.6であった。
スパッタリング装置CFS−4ES−231(芝浦メカトロニクス(株)製)にエポキシ変成ナイロン粒子Aを10g基板に乗せ、ターゲットがチタン、ガス成分がアルゴン、ガス圧が3.0×10−1Pa、基板の温度が80℃、電力が500Wの条件にて行い、導電性層の厚さが、130nmの導電性粒子Dを作製した。導電性粒子の形状は真球、比重は、1.3g/cm3、[核の体積]/[導電性層の体積]は15.7であった。
1000mlの無電解銅メッキ液MK−430(室町ケミカル(株)製)にエポキシ変性ナイロン粒子Aを100g添加し、次いで50℃で45分間メッキ処理を行い、導電性粒子Eを作製した。導電性粒子Eの形状は真球、比重は1.4g/cm3、導電性層の厚さは120nm、[核の体積]/[導電性層の体積]は17.0であった。
1000mlの無電解ニッケルメッキ液NLT−PLA(日鉱メタルプレーティング(株)製)にエポキシ変性ナイロン粒子Aを100g添加し、次いで50℃で60分間メッキ処理を行い、導電性粒子Fを作製した。導電性粒子Fの形状は真球、比重は1.4g/cm3、導電性層の厚さは180nm、[核の体積]/[導電性層の体積]は11.2であった。
透明ポリアミド(商品名“グリルアミド(登録商標)”−TR55、エムザベルケ社製)60重量部、エポキシ樹脂(商品名“エピコート(登録商標)”828、油化シェル(株)社製)30重量部および硬化剤(商品名“トーマイド(登録商標)”#296、富士化成工業(株)社製)10重量部を、クロロホルム300重量部とメタノール100重量部の混合溶媒中に添加して均一溶液を得た。次に、得られた均一溶液を塗装用のスプレーガンを用いて霧状にして、良く撹拌して3000重量部のn−ヘキサンの液面に向かって吹き付けて溶質を析出させた。析出した固体を濾別し、n−ヘキサンで良く洗浄した後に、100℃の温度で24時間の真空乾燥を行い、真球状のエポキシ変性ナイロン粒子Hを得た。
“ミクロパール(登録商標)”AU215 100重量部に、3−(フェニルアミノ)プロピルトリメトキシシラン 2重量部をミキサーで攪拌しながら噴霧し、次いで100℃で12時間熱処理し、“ミクロパール(登録商標)”AU215の表面処理品Iを得た。
150mlの98重量%硫酸溶液および50mlの60重量%硝酸溶液に“ベルパール(登録商標)”C−2000 100g添加し、次いで120℃で20分間攪拌し、フィルターで分離した後、水で充分洗浄し、“ベルパール(登録商標)”C−2000の表面処理品Jを得た。
・“トレカ(登録商標)”ミルドファイバーMLD−30(東レ(株)製、断面形状:真円、比重:1.8g/cm3、繊維長30μm)
・“トレカ(登録商標)”チョップドファイバーT008−3(東レ(株)製、断面形状:真円、比重:1.8g/cm3、繊維長3mm)。
1000mlの無電解銅メッキ液MK−430(室町ケミカル(株)製)にTR−55短繊維(繊維長1mm)を100g添加し、次いで50℃で45分間メッキ処理を行い、導電性繊維Aを作製した。導電性繊維Aの断面形状は真円、比重は1.6g/cm3、導電性層の厚さは100nm、[芯の体積]/[導電性層の体積]は13.3であった。
粒子の平均粒径については、例えば、走査型電子顕微鏡などの顕微鏡にて粒子を1000倍以上に拡大し写真撮影し、無作為に粒子を選び、その粒子の外接する円の直径を粒径とし、その粒径の平均値(n=50)として求めた。また、導電性物質で被覆されてなる導電性粒子の[核の体積]/[導電性層の体積]で表される体積比を求める際は、まず導電性粒子の核の平均径(平均粒径)を前記手法にて測定し、その後、導電性物質で被覆されてなる導電性粒子の断面を走査型顕微鏡にて1万倍に拡大し写真撮影し、導電性層の厚さを測定(n=10)し、その平均値を計算した。かかる測定は、上記無作為に選んだ導電性粒子(n=50)について実施した。導電性粒子の核の平均粒径と導電性層の厚さの平均値の2倍を足し合わせることで導電性粒子の平均径(平均粒径)とした。そして、導電性粒子の核の平均径(平均粒径)と導電性粒子の平均径(平均粒径)を用いて、[核の体積]/[導電性層の体積]で表される体積比を計算した。なお、粒子が非球状の場合は、核の外接球を仮定し、その上に上記方法にて測定した導電性層が被覆された球を仮定して計算した計算値を体積比に用いた。
・ナイロン12粒子SP−10(東レ(株)製)・・・10.2μm
・エポキシ変性ナイロン粒子A・・・12.5μm。
・“ミクロパール”AU215・・・15.5μm
・“ミクロパール”AU225・・・25.0μm
・“ベルパール”C−2000・・・15.3μm
・導電性粒子B・・・13.8μm
・導電性粒子C・・・12.7μm
・導電性粒子D・・・12.9μm
・導電性粒子E・・・12.7μm
・導電性粒子F・・・13.0μm
・導電性粒子G・・・13.1μm
・“ミクロパール”AU215の表面処理品I・・・15.5μm
・“ベルパール”C−2000の表面処理品J・・・15.3μm。
繊維の平均径(平均繊維径)については、例えば、走査型電子顕微鏡などの顕微鏡にて繊維断面を1000倍以上に拡大し写真撮影し、無作為に繊維断面を選び、その繊維断面の外接する円の直径を繊維径とし、その繊維径の平均値(n=50)として求めた。また、導電性物質で被覆されてなる導電性繊維の[芯の体積]/[導電性層の体積]で表される体積比を求める際は、まず導電性繊維の芯の平均繊維径を前記手法にて測定した。その後、導電性物質で被覆されてなる導電性繊維の断面を走査型顕微鏡にて1万倍に拡大し写真撮影し、導電性層の厚さを測定(n=10)し、その平均値を計算した。かかる測定は、上記無作為に選んだ導電性繊維(n=50)について実施した。導電性繊維の芯の平均繊維径と導電性層の厚さの平均値の2倍を足し合わせることで導電性繊維の平均繊維径とする。そして、導電性繊維の芯の平均繊維径と導電性繊維の平均繊維径を用いて、[芯の体積]/[導電性層の体積]で表される体積比を計算した。なお、熱可塑性樹脂繊維と導電性繊維の各繊維の平均繊維径測定結果は、下記のとおりであった。
・TR−55短繊維・・・5.4μm。
・“トレカ”ミルドファイバーMLD−30・・・7.2μm
・“トレカ”チョップドファイバーT008−3・・・6.9μm
・導電性繊維A・・・5.6μm。
プリプレグを、2枚の表面の平滑なポリ四フッ化エチレン樹脂板間に挟持して密着させ、7日間かけて徐々に150℃迄温度を上昇させてゲル化、硬化させて板状の樹脂硬化物を作製した。硬化後、密着面と垂直な方向から切断し、その断面を研磨後、光学顕微鏡で200倍以上に拡大しプリプレグの上下面が視野内に納まるようにして写真撮影した。同様な操作により、断面写真の横方向の5ヵ所でポリ四フッ化エチレン樹脂板間の間隔を測定し、その平均値(n=10)をプリプレグの厚さとした。
ダイアインスツルメンツ(株)製MCP−PD51型粉体抵抗測定システムを用いて、4探針電極を有する円筒型セルにサンプルをセットし、試料に60MPaの圧力を加えた状態で試料の厚さと抵抗値を測定し、その値から体積固有抵抗を計算した。
・“ミクロパール”AU215・・・1.4×10−3Ωcm
・“ミクロパール”AU225・・・1.6×10−3Ωcm
・“ベルパール”C−2000・・・2.0×10−2Ωcm
・導電性粒子B・・・5.0×10−2Ωcm
・導電性粒子C・・・3.5×10−2Ωcm
・導電性粒子D・・・5.2×10−2Ωcm
・導電性粒子E・・・4.5×10−4Ωcm
・導電性粒子F・・・4.0×10−2Ωcm
・導電性粒子G・・・6.1×10−4Ωcm
・“ミクロパール”AU215表面処理品I・・・1.4×10−3Ωcm
・“ベルパール”C−2000表面処理品J・・・2.0×10−2Ωcm。
・“トレカ”ミルドファイバーMLD−30・・・6.6×10−2Ωcm
・“トレカ”チョップドファイバーT008−3・・・9.3×10−2Ωcm
・導電性繊維A・・・7.1×10−3Ωcm。
一方向プリプレグを、[+45°/0°/−45°/90°]3s構成で、擬似等方的に24プライ積層し、オートクレーブにて、180℃の温度で2時間、0.59MPaの圧力下、昇温速度1.5℃/分で成形して25個の積層体を作製した。これらの各積層体から、縦150mm×横100mmのサンプルを切り出し、SACMA SRM 2R−94に従い、サンプルの中心部に6.7J/mmの落錘衝撃を与え、衝撃後圧縮強度を求めた。
一方向プリプレグを、それぞれ[+45°/0°/−45°/90°]3s構成で、擬似等方的に24プライ積層し、オートクレーブにて、180℃の温度で2時間、0.59MPaの圧力下、昇温速度1.5℃/分で成形して25個の積層体を作製した。これらの各積層体から、縦50mm×横50mmのサンプルを切り出し、両面に導電性ペースト“ドータイト”(登録商標)D−550(藤倉化成(株)製)を塗布したサンプルを作製した。これらのサンプルを、アドバンテスト(株)製R6581デジタルマルチメーターを用いて、四端子法で積層方向の抵抗を測定し、体積固有抵抗を求めた。
混練装置で、50重量部の“エピコート(登録商標)”825と50重量部のELM434に、10重量部のPES5003Pを配合して溶解した後、19.98重量部のエポキシ変性ナイロン粒子Aと0.02重量部の“ミクロパール(登録商標)”AU215を混練し、さらに硬化剤である4,4’−ジアミノジフェニルスルホンを40重量部混練して、熱硬化性樹脂組成物を調製した。
炭素繊維、熱可塑性樹脂粒子または導電性粒子の種類や配合量を表1〜4に示すように変更した以外は、実施例1と同様にしてプリプレグを作製した。作製した一方向プリプレグを用いて、プリプレグの厚み20%の深さの範囲に存在する粒子の存在率、繊維強化複合材料の衝撃後圧縮強度および導電性を測定した。
混練装置で、50重量部の“エピコート(登録商標)”825と50重量部のELM434に、10重量部のPES5003Pを配合して溶解した後、さらに硬化剤である4,4’−ジアミノジフェニルスルホンを40重量部混練して、熱硬化性樹脂組成物を調製した。このマトリックス樹脂を一次樹脂とした。
混練装置で、50重量部の“エピコート(登録商標)”825と50重量部のELM434に、10重量部のPES5003Pを配合して溶解した後、硬化剤である4,4’−ジアミノジフェニルスルホンを40重量部混練して、熱硬化性樹脂組成物を作製した。
熱可塑性樹脂の繊維または粒子、導電性の粒子または繊維の種類を表5に示すように変更し、熱可塑性樹脂の粒子または繊維の散布量が6.5g/m2、および導電性の粒子または繊維の散布量が0.5g/m2とした以外は、実施例25と同様にしてプリプレグを作製した。作製した一方向プリプレグを用いて、プリプレグの厚み20%の深さの範囲に存在する前記粒子または繊維の存在率、繊維強化複合材料の衝撃後圧縮強度および導電性を測定した。
熱可塑性樹脂の繊維または導電性の繊維の種類を表5に示すように変更し、それらの散布量を7.0g/m2とした以外は、実施例25と同様にしてプリプレグを作製した。作製した一方向プリプレグを用いて、プリプレグの厚み20%の深さの範囲に存在する前記粒子または繊維の存在率、繊維強化複合材料の衝撃後圧縮強度および導電性を測定した。
2:層間形成層(層間)
3:熱可塑性樹脂の粒子
4:導電性の粒子
5:炭素繊維
6:熱硬化性樹脂
Claims (18)
- [A]炭素繊維と[B]熱硬化性樹脂を含み、かつ下記(1)、(2)の少なくともいずれか一方を満たすプリプレグ。
(1)[C]熱可塑性樹脂の粒子または繊維、および[D]導電性の粒子または繊維を含み、[[C]の配合量(重量部)]/[[D]の配合量(重量部)]で表される重量比が1〜1000である。
(2)[E]熱可塑性樹脂の核または芯が導電性物質で被覆された導電性の粒子または繊維を含む。 - 前記(1)を満たす請求項1のプリプレグ。
- 前記(2)を満たす請求項1のプリプレグ。
- 前記[D]導電性の粒子または繊維の粒径または繊維径は、その平均径が、前記[C]熱可塑性樹脂の粒子または繊維の粒径または繊維径の平均径と同じかもしくはそれより大きく、その平均径は大きくとも150μmである請求項2に記載のプリプレグ。
- 前記[D]導電性の粒子または繊維は、カーボン粒子、無機材料の核が導電性物質で被覆された粒子、有機材料の核が導電性物質で被覆された粒子、炭素繊維、無機材料の芯が導電性物質で被覆された繊維および有機材料の芯が導電性物質で被覆された繊維からなる群から選ばれた少なくとも一種である、請求項2または3に記載のプリプレグ。
- 前記熱可塑性樹脂が、G1cが1500〜50000J/m2である、請求項3に記載のプリプレグ。
- 前記[C]熱可塑性樹脂の粒子または繊維、前記[D]導電性の粒子または繊維、および、前記[E]熱可塑性樹脂の核または芯が導電性物質で被覆された導電性の粒子または繊維はいずれも、その平均径が、1〜150μmである、請求項1〜6のいずれかに記載のプリプレグ。
- 前記[D]導電性の粒子または繊維が、体積固有抵抗が10〜10−9Ωcmである、請求項2、4、および、5のいずれかに記載のプリプレグ。
- 前記導電性物質が、体積固有抵抗が10〜10−9Ωcmである、請求項3または6に記載のプリプレグ。
- 前記[C]熱可塑性樹脂の粒子または繊維、前記[D]導電性の粒子または繊維、および、前記[E]熱可塑性樹脂の核または芯が導電性物質で被覆された導電性の粒子または繊維はいずれも、その90〜100重量%が、両表面から厚さ方向の20%の深さの範囲内に局在している、請求項1〜9のいずれかに記載のプリプレグ。
- 前記[C]熱可塑性樹脂の粒子または繊維、前記[D]導電性の粒子または繊維、および、前記[E]熱可塑性樹脂の核または芯が導電性物質で被覆された導電性の粒子または繊維の総重量が、プリプレグに対して1〜20重量%である、請求項1〜10のいずれかに記載のプリプレグ。
- 前記[D]導電性の粒子または繊維、および、前記[E]熱可塑性樹脂の核または芯が導電性物質で被覆された導電性の粒子または繊維は、その比重が、0.8〜3.2である、請求項1〜11のいずれかに記載のプリプレグ。
- 前記[D]導電性の粒子または繊維、および、前記[E]熱可塑性樹脂の核または芯が導電性物質で被覆された導電性の粒子または繊維が、表面処理を施されたものである、請求項1〜12のいずれかに記載のプリプレグ。
- 前記表面処理が、カップリング処理、酸化処理、オゾン処理、プラズマ処理、コロナ処理、およびブラスト処理からなる群から選ばれた少なくとも一種の処理である、請求項13に記載のプリプレグ。
- カップリング処理がシランカップリング処理である、請求項14に記載のプリプレグ。
- 酸化処理が、薬液酸化処理である、請求項14に記載のプリプレグ。
- 炭素繊維が、260〜400GPaの引張弾性率を有する、請求項1〜16のいずれかに記載のプリプレグ。
- [A]炭素繊維と[B]熱硬化性樹脂を含み、かつ下記(1)、(2)の少なくともいずれか一方を満たす炭素繊維強化複合材料。
(1)[C]熱可塑性樹脂の粒子または繊維、および[D]導電性の粒子または繊維を含み、[[C]の配合量(重量部)]/[[D]の配合量(重量部)]で表される重量比が1〜1000である。
(2)[E]熱可塑性樹脂の核または芯が導電性物質で被覆された導電性の粒子または繊維を含む。
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