WO2014157101A1 - 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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- 0 C(CC1)CCC1[C@@]1COC(CCC(C2)SC(CC3)CC(C*4)=C3OC[C@]4C3C=CCCC3)C2CC1 Chemical compound C(CC1)CCC1[C@@]1COC(CCC(C2)SC(CC3)CC(C*4)=C3OC[C@]4C3C=CCCC3)C2CC1 0.000 description 2
- FMZPVXIKKGVLLV-UHFFFAOYSA-N C(c(cccc1)c1OC1)N1c1ccccc1 Chemical compound C(c(cccc1)c1OC1)N1c1ccccc1 FMZPVXIKKGVLLV-UHFFFAOYSA-N 0.000 description 1
- KIPQGPQFYOUSOR-UHFFFAOYSA-N Cc1cc(-c2cc(C)ccc2C2(c(cc3)ccc3O)c(cc3)ccc3O)c2cc1 Chemical compound Cc1cc(-c2cc(C)ccc2C2(c(cc3)ccc3O)c(cc3)ccc3O)c2cc1 KIPQGPQFYOUSOR-UHFFFAOYSA-N 0.000 description 1
- XMDNWBPAAUNLNH-UHFFFAOYSA-N Cc1cc(CCC2(c(cc3)ccc3O)c(cc3)ccc3O)c2cc1 Chemical compound Cc1cc(CCC2(c(cc3)ccc3O)c(cc3)ccc3O)c2cc1 XMDNWBPAAUNLNH-UHFFFAOYSA-N 0.000 description 1
- AOICJFSTAFNZLL-UHFFFAOYSA-N OC1C=CC(C2(c(cc3)ccc3O)c3ccccc3Cc3ccccc23)=CC1 Chemical compound OC1C=CC(C2(c(cc3)ccc3O)c3ccccc3Cc3ccccc23)=CC1 AOICJFSTAFNZLL-UHFFFAOYSA-N 0.000 description 1
- DJJLVZCWOGYYQE-UHFFFAOYSA-N Oc1ccc(C(CC2)(C3C2CCCC3)c(cc2)ccc2O)cc1 Chemical compound Oc1ccc(C(CC2)(C3C2CCCC3)c(cc2)ccc2O)cc1 DJJLVZCWOGYYQE-UHFFFAOYSA-N 0.000 description 1
- OVVCSFQRAXVPGT-UHFFFAOYSA-N Oc1ccc(C2(CCCC2)c(cc2)ccc2O)cc1 Chemical compound Oc1ccc(C2(CCCC2)c(cc2)ccc2O)cc1 OVVCSFQRAXVPGT-UHFFFAOYSA-N 0.000 description 1
- SDDLEVPIDBLVHC-UHFFFAOYSA-N Oc1ccc(C2(CCCCC2)c(cc2)ccc2O)cc1 Chemical compound Oc1ccc(C2(CCCCC2)c(cc2)ccc2O)cc1 SDDLEVPIDBLVHC-UHFFFAOYSA-N 0.000 description 1
- OUSNRDRORMYDPE-UHFFFAOYSA-N Oc1ccc(C2(c(cc3)ccc3O)c3ccccc3CCC2)cc1 Chemical compound Oc1ccc(C2(c(cc3)ccc3O)c3ccccc3CCC2)cc1 OUSNRDRORMYDPE-UHFFFAOYSA-N 0.000 description 1
- YWFPGFJLYRKYJZ-UHFFFAOYSA-N Oc1ccc(C2(c(cccc3)c3-c3ccccc23)c(cc2)ccc2O)cc1 Chemical compound Oc1ccc(C2(c(cccc3)c3-c3ccccc23)c(cc2)ccc2O)cc1 YWFPGFJLYRKYJZ-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
[式(C-1)中、R1、R2、R3及びR4は水素原子又は炭化水素基を示し、R1、R2、R3又はR4が炭化水素基である場合、それらは炭素数1~4の直鎖若しくは分岐のアルキル基である、又は、隣り合うR1及びR2若しくは隣り合うR3及びR4が結合して炭素数6~10の置換若しくは無置換の芳香環又は炭素数6~10の置換若しくは無置換の脂環構造を形成しており、xは、0又は1を示す。]
[式(C-1)中、R1、R2、R3及びR4は水素原子又は炭化水素基を示し、R1、R2、R3又はR4が炭化水素基である場合、それらは炭素数1~4の直鎖若しくは分岐のアルキル基である、又は、隣り合うR1及びR2若しくは隣り合うR3及びR4が結合して炭素数6~10の置換若しくは無置換の芳香環又は炭素数6~10の置換若しくは無置換の脂環構造を形成しており、xは、0又は1を示す。]
[式(C-1)中、R1、R2、R3及びR4は水素原子又は炭化水素基を示し、R1、R2、R3又はR4が炭化水素基である場合、それらは炭素数1~4の直鎖若しくは分岐のアルキル基である、又は、隣り合うR1及びR2若しくは隣り合うR3及びR4が結合して炭素数6~10の置換若しくは無置換の芳香環又は炭素数6~10の置換若しくは無置換の脂環構造を形成しており、xは、0又は1を示す。]
[式(A-1)中、R5は、炭素数1~12の鎖状アルキル基、炭素数3~8の環状アルキル基、炭素数6~14のアリール基、又は炭素数1~12の鎖状アルキル基若しくはハロゲンで置換されたアリール基を示す。結合手には水素原子が結合されていてもよい。]
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)
(C’)成分:他の硬化剤
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
PA1010(1)(ポリアミド1010、平均粒子径10μm、ダイセル・エボニック製)
PA1010(2)(ポリアミド1010、平均粒子径20μm、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:靱性向上剤
YP-70(フェノキシ樹脂、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をポリアミド樹脂粒子の融点とした。結果を表2に示す。また、例として、PA12及びPA1010(2)のDSCチャートを図5に示す。図5中、(a)がPA12のDSCチャートであり、(b)がPA1010(2)のDSCチャートである。
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、実施例1及び比較例1の各第2の樹脂組成物のDSCチャートを図6に示す。図6中、(a)が実施例1の第2の樹脂組成物のDSCチャートであり、(b)が比較例1の第2の樹脂組成物のDSCチャートである。
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。この樹脂硬化物を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)下記一般式(C-1)で表され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)下記一般式(C-1)で表される硬化剤、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、ポリアミド12樹脂粒子又はポリアミド1010樹脂粒子を含む、プリプレグ。
[式(C-1)中、R1、R2、R3及びR4は水素原子又は炭化水素基を示し、R1、R2、R3又はR4が炭化水素基である場合、それらは炭素数1~4の直鎖若しくは分岐のアルキル基である、又は、隣り合うR1及びR2若しくは隣り合うR3及びR4が結合して炭素数6~10の置換若しくは無置換の芳香環又は炭素数6~10の置換若しくは無置換の脂環構造を形成しており、xは、0又は1を示す。] - 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、及び前記(D)成分を15~45質量部含有する、請求項1に記載のプリプレグ。
- 請求項1又は2に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)下記一般式(C-1)で表される硬化剤と、
(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、ポリアミド12樹脂粒子又はポリアミド1010樹脂粒子を含む、粒子含有樹脂組成物。
[式(C-1)中、R1、R2、R3及びR4は水素原子又は炭化水素基を示し、R1、R2、R3又はR4が炭化水素基である場合、それらは炭素数1~4の直鎖若しくは分岐のアルキル基である、又は、隣り合うR1及びR2若しくは隣り合うR3及びR4が結合して炭素数6~10の置換若しくは無置換の芳香環又は炭素数6~10の置換若しくは無置換の脂環構造を形成しており、xは、0又は1を示す。]
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