JP2017082215A - 繊維強化熱可塑性樹脂成形品および繊維強化熱可塑性樹脂成形材料 - Google Patents
繊維強化熱可塑性樹脂成形品および繊維強化熱可塑性樹脂成形材料 Download PDFInfo
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- JP2017082215A JP2017082215A JP2016211418A JP2016211418A JP2017082215A JP 2017082215 A JP2017082215 A JP 2017082215A JP 2016211418 A JP2016211418 A JP 2016211418A JP 2016211418 A JP2016211418 A JP 2016211418A JP 2017082215 A JP2017082215 A JP 2017082215A
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- fiber
- thermoplastic resin
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- boron nitride
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Landscapes
- Reinforced Plastic Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
熱可塑性樹脂(A)、炭素繊維(B)、有機繊維(C)、ならびに、窒化ホウ素および/または黒鉛(D)を含む繊維強化熱可塑性樹脂成形品であって、熱可塑性樹脂(A)、炭素繊維(B)、有機繊維(C)、ならびに、窒化ホウ素および/または黒鉛(D)の合計100重量部に対して、熱可塑性樹脂(A)を20〜93重量部、炭素繊維(B)を5〜40重量部、有機繊維(C)を1〜30重量部、ならびに、窒化ホウ素および/または黒鉛(D)を1〜30重量部含み、前記炭素繊維(B)の重量平均繊維長(LWb)が0.7〜2mmであり、かつ、前記有機繊維(C)の重量平均繊維長(Lwc)が2.5〜5mmである、繊維強化熱可塑性樹脂成形品。
熱可塑性樹脂(A)、炭素繊維(B)、有機繊維(C)、窒化ホウ素および/または黒鉛(D)、ならびに、200℃における溶融粘度が熱可塑性樹脂(A)より低い化合物(E)を含む繊維強化熱可塑性樹脂成形材料であって、熱可塑性樹脂(A)、炭素繊維(B)、有機繊維(C)、ならびに、窒化ホウ素および/または黒鉛(D)の合計100重量部に対して、熱可塑性樹脂(A)を20〜93重量部、炭素繊維(B)を5〜40重量部、有機繊維(C)を1〜30重量部窒化ホウ素および/または黒鉛(D)を1〜30重量部、ならびに、200℃における溶融粘度が熱可塑性樹脂(A)より低い化合物(E)を1〜20重量部含む、繊維強化熱可塑性樹脂成形材料。
ηsp/c=[η]+0.45×[η]2(但し[η]は極限粘度)
[η]=1.23×10−4M0.83
c=0.7 。
引張破断伸度(%)=[(切断時の長さ(mm)−250)/250]×100 。
(加熱減量)[重量%]={(加熱前重量−加熱後重量)/加熱前重量}×100 。
(溶融粘度変化率[%])={|(200℃にて2時間加熱前の200℃における溶融粘度−200℃にて2時間加熱後の200℃における溶融粘度)|/(200℃にて2時間加熱前の200℃における溶融粘度)}×100 。
重量平均繊維長=Σ(Mi2×Ni)/Σ(Mi×Ni)
Mi:繊維長(mm)
Ni:繊維長Miの強化繊維の個数。
各実施例および比較例に用いた熱可塑性樹脂(A)、化合物(E)について、40mmのパラレルプレートを用いて、0.5Hzにて、粘弾性測定器により200℃における溶融粘度を測定した。また、化合物(E)を200℃の熱風乾燥機に2時間静置した後、同様に200℃における溶融粘度を測定し、乾燥前後の溶融粘度変化率を測定した。
成形品を200〜300℃に設定したホットステージの上にガラス板間に挟んだ状態で加熱し、フィルム状にして均一分散させた。炭素繊維(B)および有機繊維(C)が均一分散したフィルムを、光学顕微鏡(50〜200倍)にて観察した。無作為に選んだ1000本の炭素繊維(B)と、同様に無作為に選んだ1000本の有機繊維(C)について、それぞれ繊維長を計測して、下記式から重量平均繊維長を算出した。
平均繊維長=Σ(Mi2×Ni)/Σ(Mi×Ni)
Mi:繊維長(mm)
Ni:繊維長Miの繊維の個数
各実施例および比較例により得られたISO型ダンベル試験片について、ISO 178に準拠し、3点曲げ試験冶具(圧子半径5mm)を用いて支点距離を64mmに設定し、試験速度2mm/分の試験条件にて曲げ強度を測定した。試験機として、“インストロン(登録商標)”万能試験機5566型(インストロン社製)を用いた。
各実施例および比較例により得られたISO型ダンベル試験片の平行部を切り出し、株式会社東京試験機製C1−4−01型試験機を用い、ISO179に準拠してVノッチ付きシャルピー衝撃試験を実施し、衝撃強度(kJ/cm2)を算出した。
各実施例および比較例により得られたISO型ダンベル試験片から、20mm×20mm×4mm厚の試験片を切り出し、アルバック理工製GH−1Sを用いて、80℃における厚み方向の熱伝導率を測定した。また、前記ISO型ダンベル試験片から20mm×4mm×4mm厚の試験片を5枚切り出し、流れ方向を垂直にして、試験片5枚を横に並べ、アルバック理工製GH−1Sを用いて、80℃における流れ方向の熱伝導率を測定した。
各実施例および比較例により得られた、80mm×80mm×3mm厚の試験片表裏それぞれの面に存在する未分散CF束の個数を目視でカウントした。評価は50枚の成形品について行い、その合計個数について繊維分散性の判定を以下の基準で行い、Aを合格とした。
A:未分散CF束が1個未満
B:未分散CF束が1個以上。
各実施例および比較例により得られた80mm×10mm×4mm厚の試験片の中央部、または成形材料の断面を、倍率を200〜2000倍として写真撮影し、写真上に観察される(D)黒鉛のうち、粒径の大きいものから50個選択し、50個の粒径を測定してその平均値を求めた。なお、写真上に観察される黒鉛円形でない場合には、最大径を粒径として測定した。
成形材料を倍率10〜100倍で写真撮影し、写真上に観察される成形材料のうち、成形材料の繊維束配向方向の長さを測定した。成形材料を無作為に100個選択し、100個の長さを測定して、その平均値を求めることで算出した。
ポリアクリロニトリルを主成分とする共重合体から紡糸、焼成処理、表面酸化処理を行い、総単糸数24,000本、単繊維径7μm、単位長さ当たりの質量1.6g/m、比重1.8g/cm3、表面酸素濃度比[O/C]0.2の連続炭素繊維を得た。この連続炭素繊維のストランド引張強度は4,880MPa、ストランド引張弾性率は225GPaであった。続いて、多官能性化合物としてグリセロールポリグリシジルエーテルを2重量%になるように水に溶解させたサイジング剤母液を調製し、浸漬法により炭素繊維にサイジング剤を付与し、230℃で乾燥を行った。こうして得られた炭素繊維のサイジング剤付着量は1.0重量%であった。
(A−1)
ポリプロピレン樹脂(プライムポリマー(株)製“プライムポリプロ”(登録商標)J137)とマレイン酸変性ポリプロピレン樹脂(三井化学(株)製“アドマー”(登録商標)QE840)を重量比85/15でペレットブレンドしたものを用いた。200℃における溶融粘度を上記(1)に記載の方法により測定した結果、50Pa・sであった。
ポリカーボネート樹脂(帝人化成(株)製、“パンライト”(登録商標)L−1225L)を用いた。200℃における溶融粘度を上記(1)に記載の方法により測定した結果、14000Pa・sであった。
ポリフェニレンサルファイド樹脂(東レ(株)製“トレリナ(登録商標)”M2888)を用いた。測定温度を310℃とした以外は、上記(1)に記載の方法により溶融粘度を測定した結果、50Pa・sであった。
(C−1)
ポリエステル繊維(東レ(株)製、“テトロン(登録商標)”2200T−480−705M、単繊維繊度:4.6dtex、融点:260℃)を用いた。熱伝導率は、0.15W/m・Kであった。
ポリフェニレンサルファイド繊維(東レ(株)製“トルコン”(登録商標)400T−100−190、単繊維繊度4.0dtex、融点285℃)を用いた。熱伝導率は、0.29W/m・Kであった。
ポリテトラフルオロエチレン繊維(東レ(株)製“トヨフロン”(登録商標)440T−60F−S290−M190、単繊維繊度7.3dtex、融点327℃)を用いた。熱伝導率は、0.25W/m/Kであった。
液晶ポリエステル繊維(KBセーレン(株)製“ゼクシオン”(登録商標)220T−48f、単繊維繊度4.0dtex、融点330℃)を用いた。熱伝導率は、0.60W/m・Kであった。
(D−1)
黒鉛:鱗片状黒鉛CFW−50A((株)中越黒鉛工業所製)を用いた。
窒化ホウ素:鱗片状窒化ホウ素SGP(デンカ株式会社製)を用いた。
(E−1)
固体の水添テルペン樹脂(ヤスハラケミカル(株)製“クリアロン”(登録商標)P125、軟化点125℃)を用いた。これを含浸助剤塗布装置内のタンク内に投入し、タンク内の温度を200℃に設定し、1時間加熱して溶融状態にした。この時の、200℃における溶融粘度を上記(1)に記載の方法により測定した結果、1Pa・sであり、また、溶融粘度変化率を算出した結果、1.2%であった
(E−2)
固体のビスフェノールA型エポキシ樹脂(三菱化学(株)製 jER1004AF(E−2)、軟化点97℃)を、熱可塑性樹脂(A)にポリカーボネート樹脂を用いた際の化合物(E)に用いた。これを、前述したP125と同様にして、溶融粘度を上記(1)に記載の方法により測定した結果、1Pa・sであり、また、溶融粘度変化率を算出した結果、1.1%であった。
(株)日本製鋼所製TEX−30α型2軸押出機(スクリュー直径30mm、L/D=32)の先端に設置された電線被覆法用のコーティングダイを設置した長繊維強化樹脂ペレット製造装置を使用し、押出機シリンダー温度を220℃に設定し、上記に示した熱可塑性樹脂(A−1)と黒鉛(D−1)をメインホッパーから供給し、スクリュー回転数200rpmで溶融混練した。黒鉛(D−1)は、(A)〜(D)の合計100重量部に対し、20重量部とした。200℃にて加熱溶融させた化合物(E)を、(A)〜(D)の合計100重量部に対し、8.7重量部となるように吐出量を調整し、炭素繊維(B)および有機繊維(C−1)からなる繊維束に付与して複合繊維束(F)とした後、溶融した熱可塑性樹脂(A−1)と黒鉛(D−1)を含む組成物を吐出するダイス口(直径3mm)へ供給して、炭素繊維(B)および有機繊維(C−1)の周囲を被覆するように連続的に配置した。この時の複合繊維束(F)内部断面は、炭素繊維(B)および有機繊維(C−1)が偏在していた。偏在状態は、炭素繊維(B)、有機繊維(C−1)のそれぞれ少なくとも一部が、熱可塑性樹脂(A−1)と黒鉛(D−1)とを含む組成物に接していた。得られたストランドを冷却後、カッターでペレット長7mmに切断し、長繊維ペレットとした。この時、(A)〜(D)の合計100重量部に対し、炭素繊維(B)が20重量部、有機繊維(C−1)が10重量部となるように、引取速度を調整した。得られた長繊維ペレットの炭素繊維(B)および有機繊維(C)の長さと、ペレット長さは実質的に同じであった。なお、偏在状態は、得られた長繊維ペレットの繊維長手方向に対して垂直な断面を倍率300倍に設定した光学顕微鏡にて観察し、得られた顕微鏡像の画像処理を行い解析した。
(A)〜(D)の合計100重量部に対し、黒鉛(D−1)が10重量部、熱可塑性樹脂(A−1)が60重量部となるようにした以外は、実施例1と同様にして成形品を作製し、評価を行った。評価結果はまとめて表1に示した。
有機繊維(C)を(C−2)に変更した以外は、実施例1と同様にして成形品を作製し、評価を行った。評価結果はまとめて表1に示した。
熱可塑性樹脂(A)を(A−2)に、有機繊維(C)を(C−3)に、化合物(E)を(E−2)に変更し、さらに、シリンダー温度を300℃、金型温度を80℃に変更した以外は、実施例1と同様にして成形品を作製し、評価を行った。評価結果はまとめて表1に示した。
熱可塑性樹脂(A)を(A−2)に、有機繊維(C)を(C−4)に、化合物(E)を(E−2)に変更し、さらに、シリンダー温度を300℃、金型温度を80℃に変更した以外は、実施例1と同様にして成形品を作製し、評価を行った。評価結果はまとめて表1に示した。
(A)〜(D)の合計100重量部に対し、有機繊維(C−4)を20重量部、黒鉛(D−1)を10重量部となるように変更した以外は、実施例5と同様にして成形品を作製し、評価を行った。評価結果はまとめて表1に示した。
熱可塑性樹脂(A)を(A−3)に、有機繊維(C)を(C−3)に、化合物(E)を(E−2)に変更し、さらに、シリンダー温度を330℃、金型温度を130℃に変更した以外は、実施例1と同様にして成形品を作製し、評価を行った。評価結果はまとめて表1に示した。
黒鉛(D)を窒化ホウ素(D−2)に変更した以外は、実施例1と同様にして成形品を作製し、評価を行った。評価結果はまとめて表1に示した。
(A)〜(D)の合計100重量部に対し、熱可塑性樹脂(A−1)が60重量部、有機繊維(C)が0重量部、化合物(E)が6.4重量部となるようにした以外は、実施例1と同様にして成形品を作製し、評価を行った。評価結果はまとめて表2に示した。
(A)〜(D)の合計100重量部に対し、熱可塑性樹脂(A−1)が35重量部、炭素繊維(B)が45重量部、有機繊維(C−1)が0重量部、化合物(E)が12.4重量部となるようにした以外は、実施例1と同様にして成形品を作製し、評価を行った。評価結果はまとめて表2に示した。
(A)〜(D)の合計100重量部に対し、熱可塑性樹脂(A−1)が70重量部、炭素繊維(B)が0重量部、化合物(E)が4.3重量部となるようにした以外は、実施例1と同様にして成形品を作製し、評価を行った。評価結果はまとめて表2に示した。
(A)〜(D)の合計100重量部に対し、熱可塑性樹脂(A)が70重量部、黒鉛(D−1)が0重量部となるようにした以外は、実施例1と同様にして成形品を作製し、評価を行った。評価結果はまとめて表2に示した。
2 有機繊維(C)
3 熱可塑性樹脂(A)と、窒化ホウ素および/または黒鉛(D)を含む組成物
Claims (14)
- 熱可塑性樹脂(A)、炭素繊維(B)、有機繊維(C)、ならびに、窒化ホウ素および/または黒鉛(D)を含む繊維強化熱可塑性樹脂成形品であって、熱可塑性樹脂(A)、炭素繊維(B)、有機繊維(C)、ならびに、窒化ホウ素および/または黒鉛(D)の合計100重量部に対して、熱可塑性樹脂(A)を20〜93重量部、炭素繊維(B)を5〜40重量部、有機繊維(C)を1〜30重量部、ならびに、窒化ホウ素および/または黒鉛(D)を1〜30重量部含み、前記炭素繊維(B)の重量平均繊維長(LWb)が0.7〜2mmであり、かつ、前記有機繊維(C)の重量平均繊維長(Lwc)が2.5〜5mmである、繊維強化熱可塑性樹脂成形品。
- 厚み方向における熱伝導率が0.5〜4W/m・Kである、請求項1に記載の繊維強化熱可塑性樹脂成形品。
- 曲げ強度が150〜300MPaである、請求項1または2に記載の繊維強化熱可塑性樹脂成形品。
- 前記窒化ホウ素および/または黒鉛(D)が鱗片状黒鉛を含む、請求項1〜3のいずれかに記載の繊維強化熱可塑性樹脂成形品。
- 前記窒化ホウ素および/または黒鉛(D)の最大粒径が10〜100μmである、請求項1〜4のいずれかに記載の繊維強化熱可塑性樹脂成形品。
- 前記有機繊維(C)が、ポリエチレンテレフタレート繊維、ポリアミド繊維、ポリフェニレンサルファイド繊維およびフッ素樹脂繊維からなる群より選ばれる少なくとも1種である、請求項1〜5のいずれかに記載の繊維強化熱可塑性樹脂成形品。
- 前記熱可塑性樹脂(A)が、ポリプロピレン樹脂、ポリアミド樹脂、ポリカーボネート樹脂およびポリフェニレンサルファイド樹脂からなる群より選ばれる少なくとも1種である、請求項1〜6のいずれかに記載の繊維強化熱可塑性樹脂成形品。
- 前記熱可塑性樹脂(A)、炭素繊維(B)、有機繊維(C)、ならびに、窒化ホウ素および/または黒鉛(D)の合計100重量部に対して、さらに200℃における溶融粘度が熱可塑性樹脂(A)より低い化合物(E)を1〜20重量部含む、請求項1〜7のいずれかに記載の繊維強化熱可塑性樹脂成形品。
- 熱可塑性樹脂(A)、炭素繊維(B)、有機繊維(C)、窒化ホウ素および/または黒鉛(D)、ならびに、200℃における溶融粘度が熱可塑性樹脂(A)より低い化合物(E)を含む繊維強化熱可塑性樹脂成形材料であって、熱可塑性樹脂(A)、炭素繊維(B)、有機繊維(C)、ならびに、窒化ホウ素および/または黒鉛(D)の合計100重量部に対して、熱可塑性樹脂(A)を20〜93重量部、炭素繊維(B)を5〜40重量部、有機繊維(C)を1〜30重量部ならびに窒化ホウ素および/または黒鉛(D)を1〜30重量部、ならびに、200℃における溶融粘度が熱可塑性樹脂(A)より低い化合物(E)を1〜20重量部含む、繊維強化熱可塑性樹脂成形材料。
- 前記炭素繊維(B)および有機繊維(C)に化合物(E)が含浸されてなる複合繊維束(F)が、前記熱可塑性樹脂(A)ならびに窒化ホウ素および/または黒鉛(D)を含む組成物により被覆されてなり、かつ、炭素繊維(B)および有機繊維(C)の長さと繊維強化熱可塑性樹脂成形材料の長さが実質的に同じである、請求項9に記載の繊維強化熱可塑性樹脂成形材料。
- 前記窒化ホウ素および/または黒鉛(D)が鱗片状黒鉛を含む、請求項9または10に記載の繊維強化熱可塑性樹脂成形材料。
- 前記窒化ホウ素および/または黒鉛(D)の最大粒径が50〜500μmである、請求項9〜11のいずれかに記載の繊維強化熱可塑性樹脂成形材料。
- 前記有機繊維(C)が、ポリエチレンテレフタレート繊維、ポリアミド繊維およびポリフェニレンサルファイド繊維からなる群より選ばれる少なくとも1種である、請求項9〜12のいずれかに記載の繊維強化熱可塑性樹脂成形材料。
- 前記熱可塑性樹脂(A)が、ポリプロピレン樹脂、ポリアミド樹脂、ポリカーボネート樹脂およびポリフェニレンサルファイド樹脂からなる群より選ばれる少なくとも1種である、請求項9〜13のいずれかに記載の繊維強化熱可塑性樹脂成形材料。
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