JPWO2014157097A1 - プリプレグ、繊維強化複合材料及び粒子含有樹脂組成物 - Google Patents
プリプレグ、繊維強化複合材料及び粒子含有樹脂組成物 Download PDFInfo
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Abstract
Description
各実施例、比較例について、表1に示す割合で原料を加熱混合し、粒子を含有しない第1の樹脂組成物(表中の「第1」の組成)と、粒子を含有する第2の樹脂組成物(表中の「第2」の組成)を得た。なお、ここで用いた原料は以下に示す通りである。
F−a(ビスフェノールF−アニリン型、四国化成工業(株)製)
P−a(フェノール−アニリン型、四国化成工業(株)製)
(B)成分:エポキシ樹脂
「セロキサイド」(登録商標)2021P((株)ダイセル製)
(C)成分:硬化剤
BPF(9,9−ビス(4−ヒドロキシフェニル)フルオレン、大阪ガスケミカル製)
BPC(1,1−ビス(4−ヒドロキシフェニル)シクロヘキサン、シグマ・アルドリッチ社製)TDP(ビス(4−ヒドロキシフェニル)スルフィド、東京化成工業(株)製)
(D)成分:ポリアミド樹脂粒子
PA6/12(75/25)(カプロラクタムとラウロラクタムとを75:25のモル比で共重合させたポリアミド6/12共重合体(ランダム共重合体)からなる微粒子、平均粒子径20μm)
PA6/12(80/20)(カプロラクタムとラウロラクタムとを80:20のモル比で共重合させたポリアミド6/12共重合体(ランダム共重合体)からなる微粒子、平均粒子径20μm)
PA6/12(90/10)(カプロラクタムとラウロラクタムとを90:10のモル比で共重合させたポリアミド6/12共重合体(ランダム共重合体)からなる微粒子、平均粒子径20μm)
(D’)成分: ポリアミド樹脂粒子
PA6(ポリアミド6、平均粒子径10μm、ダイセル・エボニック製)
PA12(ポリアミド12、平均粒子径10μm、ダイセル・エボニック製)
(E)成分:靭性向上剤
フェノキシ樹脂(YP−70、新日鉄住金化学(株)製)
得られた第1及び第2の樹脂組成物をそれぞれ離型紙上に70〜100℃で塗布し、18g/m2の第1の樹脂フィルム及び25g/m2の第2の樹脂フィルムを得た。得られた第1の樹脂フィルムを、一方向に引き揃えた炭素繊維の上下から供給して繊維間に含浸し、炭素繊維層を形成した。続いて、第2の樹脂フィルムを炭素繊維層の上下からラミネートして表面層を形成し、プリプレグを作製した。このプリプレグの単位面積当たりの炭素繊維量は150g/m2であり、炭素繊維層及び表面層中の合計の樹脂組成物量(マトリックス樹脂量)は86g/m2であった。
上記(D)成分及び(D’)成分であるポリアミド樹脂粒子を、示差熱量計(DSC)を用いて、25℃から10℃/分の速度で昇温し、得られた吸熱ピークのトップの温度をポリアミド樹脂粒子の融点とした。吸熱ピークが複数ある場合は、最も吸熱の大きいピークのトップの温度を融点とした。結果を表2に示す。また、一例として、PA6/12(80/20)のDSCチャートを図5に示す。
得られた第2の樹脂組成物を、示差熱量計(DSC)を用いて、25℃から10℃/分の速度で昇温し、得られた吸熱ピークのトップの温度を第2の樹脂組成物中でのポリアミド樹脂粒子の融解温度とした。結果を表1に示す。また、一例として、PA6/12(80/20)を用いた実施例3の第2の樹脂組成物のDSCチャートを図6に示す。
得られた第2の樹脂組成物を、180℃のオーブン中で2時間硬化して樹脂硬化物を得た。得られた硬化物を、示差熱量計(DSC)を用いて、JIS K7121(1987)に基づいて求めた中間点温度をガラス転移温度として測定した。結果を表1に示す。
得られた第2の樹脂組成物を、180℃の温度で2時間硬化させ、厚さ2mmの樹脂硬化物を得た。この樹脂硬化物について、JIS J 7171に従い曲げ弾性率測定を行った。結果を表1に示す。
得られたプリプレグを、[+45°/0°/−45°/90°]4s構成で、擬似等方的に32プライ積層し、オートクレーブにて、圧力0.6MPa、室温から2℃/分で180℃まで昇温した後、同温で2時間加熱硬化し、CFRPを得た。このCFRPについて、SACMA SRM 2R−94に従い、縦150mm×横100mmのサンプルを切り出し、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。結果を表1に示す。
繊維強化複合材料中の任意の炭素繊維が伸びる方向に直交する面で繊維強化複合材料を切断したときの切断面を顕微鏡観察(500倍)により分析し、500μm×100μmの範囲について画像解析を行うことでポリアミド粒子の分布を観察することにより、炭素繊維層間の1つの樹脂硬化物に含まれるポリアミド樹脂の含有量C1と、1つの炭素繊維層内に含まれるポリアミド樹脂の含有量C2とを算出した。この測定を、異なる炭素繊維層及び樹脂硬化物の組み合わせとなる任意の5箇所について行い、C1及びC2の5箇所の平均値を用いて、1プリプレグ当たりのC1の容量割合{C1/(C1+C2)}×100を求めた。結果を表1に示す。
Claims (4)
- 強化繊維と、前記強化繊維の繊維間に含浸された、(A)ベンゾオキサジン樹脂、(B)エポキシ樹脂、及び、(C)分子中に2個以上のフェノール性水酸基を有する硬化剤を含有する樹脂組成物と、を含む強化繊維層と、
前記強化繊維層の少なくとも一方の表面上に設けられた、(A)ベンゾオキサジン樹脂、(B)エポキシ樹脂、(C)分子中に2以上のフェノール性水酸基を有する硬化剤、及び、(D)平均粒子径が5〜50μmのポリアミド樹脂粒子を含有する表面層と、
を備え、
前記ポリアミド樹脂粒子は、カプロラクタムとラウロラクタムとを9:1〜7:3のモル比で共重合させた共重合体からなる、180℃以上の融点を有する粒子を含む、プリプレグ。 - 前記表面層は、前記(A)成分と前記(B)成分との合計を100質量部としたときに、前記(A)成分を65〜80質量部、前記(B)成分を20〜35質量部、前記(C)成分を5〜20質量部、前記(D)成分を15〜45質量部含有する、請求項1記載のプリプレグ。
- 請求項1又は2記載のプリプレグを複数積層し、加圧下で加熱して得られる繊維強化複合材料。
- (A)ベンゾオキサジン樹脂と、
(B)エポキシ樹脂と、
(C)分子中に2以上のフェノール性水酸基を有する硬化剤と、
(D)平均粒子径が5〜50μmのポリアミド樹脂粒子と、
を含有し、
前記ポリアミド樹脂粒子は、カプロラクタムとラウロラクタムとを9:1〜7:3のモル比で共重合させた共重合体からなる、180℃以上の融点を有する粒子を含む、粒子含有樹脂組成物。
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JP2013072005 | 2013-03-29 | ||
JP2013072005 | 2013-03-29 | ||
PCT/JP2014/058098 WO2014157097A1 (ja) | 2013-03-29 | 2014-03-24 | プリプレグ、繊維強化複合材料及び粒子含有樹脂組成物 |
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US (1) | US20160032065A1 (ja) |
EP (1) | EP2980137A4 (ja) |
JP (1) | JP6422857B2 (ja) |
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DE102015213537A1 (de) * | 2015-07-17 | 2017-01-19 | Siemens Aktiengesellschaft | Fester, insbesondere bandförmiger, Isolationswerkstoff, Formulierung für ein Imprägniermittel zur Herstellung eines Isolationssystems in einem Vakuumimprägnierverfahren damit und Maschinen mit derartigem Isolationssystem |
JP7198454B2 (ja) * | 2018-02-27 | 2023-01-04 | 国立大学法人東海国立大学機構 | 繊維強化熱可塑性樹脂の成形物の製造方法 |
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- 2014-03-24 WO PCT/JP2014/058098 patent/WO2014157097A1/ja active Application Filing
- 2014-03-24 CN CN201480019411.3A patent/CN105189624A/zh active Pending
- 2014-03-24 US US14/780,336 patent/US20160032065A1/en not_active Abandoned
- 2014-03-24 JP JP2015508493A patent/JP6422857B2/ja active Active
- 2014-03-24 KR KR1020157025538A patent/KR20150137059A/ko not_active Application Discontinuation
- 2014-03-24 EP EP14776022.7A patent/EP2980137A4/en not_active Withdrawn
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JP2008255309A (ja) * | 2007-03-13 | 2008-10-23 | Osaka Gas Co Ltd | エポキシ樹脂組成物およびその硬化物 |
JP2010525101A (ja) * | 2007-04-17 | 2010-07-22 | ヘクセル コーポレイション | 熱可塑性粒子のブレンドを含む複合材料 |
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WO2012051045A2 (en) * | 2010-10-12 | 2012-04-19 | Hexcel Corporation | Improving solvent resistance of epoxy resins toughened with polyethersulfone |
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JP6422857B2 (ja) | 2018-11-14 |
KR20150137059A (ko) | 2015-12-08 |
WO2014157097A1 (ja) | 2014-10-02 |
EP2980137A1 (en) | 2016-02-03 |
CN105189624A (zh) | 2015-12-23 |
EP2980137A4 (en) | 2016-11-09 |
US20160032065A1 (en) | 2016-02-04 |
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