JP6889332B2 - 強化繊維束、強化繊維開繊織物、および繊維強化複合体、並びにそれらの製造方法 - Google Patents
強化繊維束、強化繊維開繊織物、および繊維強化複合体、並びにそれらの製造方法 Download PDFInfo
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- JP6889332B2 JP6889332B2 JP2020524416A JP2020524416A JP6889332B2 JP 6889332 B2 JP6889332 B2 JP 6889332B2 JP 2020524416 A JP2020524416 A JP 2020524416A JP 2020524416 A JP2020524416 A JP 2020524416A JP 6889332 B2 JP6889332 B2 JP 6889332B2
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Description
繊維強化複合材料に用いられる炭素繊維は、マトリックス樹脂と化学組成および分子構造が異なり、マトリックス樹脂との相溶性が低いため、炭素繊維に対するマトリックス樹脂の接着性が低く、マトリックス樹脂の含浸性が低くなる。
これらの成形法では、強化繊維が繊維束の形態で使用される場合が多い。強化繊維が繊維束の形態で使用される場合、繊維束の開繊状態が繊維強化複合材料の機械的強度に大きく影響を与える。
前記被覆粒子が、コア粒子と、前記コア粒子表面の少なくとも一部を被覆する合成樹脂被覆とからなり、
前記コア粒子が、前記合成樹脂被覆を介して前記炭素繊維表面に一体的に接合されている、開繊炭素繊維束。
[2]前記コア粒子が、カーボン粒子、シリカ粒子、アルミナ粒子、酸化チタン粒子、炭酸カルシウム粒子、タルク粒子、ジビニルベンゼン樹脂粒子からなる群より選択される少なくとも1種を含む、[1]に記載の開繊炭素繊維束。
[3]前記合成樹脂が、エポキシ樹脂、ウレタン樹脂、シリコーン樹脂、フェノール樹脂、ビニルエステル樹脂からなる群より選択される硬化性樹脂を少なくとも1種を含む、[1]または[2]に記載の開繊炭素繊維束。
[4]少なくとも1つの前記被覆粒子が、2本以上の炭素繊維と接合されている、[1]〜[3]のいずれかに記載の開繊炭素繊維束。
[5]前記コア粒子の平均粒子径が、1〜25μmである、[1]〜[4]のいずれかに記載の開繊炭素繊維束。
[6][1]〜[5]のいずれかに記載の開繊繊維束と、前記開繊炭素繊維束に含浸されたマトリックス樹脂とを含む、繊維強化複合材料。
[7]前記マトリックス樹脂が熱可塑性樹脂である、[6]に記載の繊維強化複合材料。
[8]コア粒子に未硬化の硬化性樹脂を付着させて、コア粒子表面の少なくとも一部を未硬化の硬化性樹脂により被覆する工程と、
複数の炭素繊維からなる炭素繊維束に、前記未硬化の硬化性樹脂により被覆したコア粒子を接触させて、前記炭素繊維表面に未硬化の硬化性樹脂を介してコア粒子を付着させる工程と、
前記未硬化の硬化性樹脂を硬化させて、前記コア粒子が硬化性樹脂を介して前記炭素繊維表面に一体的に接合するように被覆粒子を形成する工程と、
を含む、開繊炭素繊維束の製造方法。
[9]前記硬化性樹脂の硬化が、常温硬化、加熱硬化、活性エネルギー線硬化から選択される少なくとも1種により行われる、[8]に記載の方法。
[10]前記硬化性樹脂が、主剤および硬化剤からなる二液型硬化性樹脂である、[8]または[9]に記載の方法。
本発明の開繊炭素繊維束は、複数の炭素繊維からなる炭素繊維束と、前記炭素繊維間に配置された被覆粒子とを備えるものである。本発明の一実施形態による開繊炭素繊維束を図1の模式図を参照しながら説明する。本発明による開繊炭素繊維束1は、炭素繊維11Aの表面にコア粒子12Aが、合成樹脂13Aを介して一体的に接合されたものである。図1に示すように、被覆粒子14Aは、コア粒子12Aの表面が合成樹脂13Aにより被覆された構成を有している。コア粒子12Aを被覆する合成樹脂13Aは、炭素繊維11Aの表面に濡れ広がることでコア粒子12Aと炭素繊維11Aとを接合し、それによりコア粒子12Aは合成樹脂13Aを介して炭素繊維11Aの表面に一体的に接合している。このような構造とすることにより、コア粒子12Aは炭素繊維11Aの表面と強固に接合しているため、炭素繊維束と熱可塑性樹脂製シートとを加熱しながら加圧して炭素繊維間に熱可塑性樹脂を含浸させた場合であっても、炭素繊維表面に結合したコア粒子が繊維束の外に排出されることがなく、開繊状態を保ちながら熱可塑性樹脂を炭素繊維間に含浸させることができる。
各炭素繊維は、一般的に単繊維であり、また、炭素繊維は複数集まって炭素繊維束を構成する。各炭素繊維束を構成している炭素繊維の本数は、1000〜50000本が好ましく、2000〜30000本が好ましい。
被覆粒子は、コア粒子と、コア粒子表面を被覆する合成樹脂被覆とからなる。コア粒子は、その表面全体が合成樹脂により被覆されてもよいし、表面の一部が合成樹脂により被覆されてもよい。
硬化性樹脂は硬化前の状態が液状、ペースト状ないし半固形状であり、硬化により固化するものであれば特に制限なく使用することができ、例えば、樹脂を溶剤にした樹脂溶液を加熱乾燥等により溶剤を除去して固体の樹脂としたもの、モノマーないしオリゴマー溶液を重合し固体状のポリマーとしたもの、あるいは二種以上のモノマーないしオリゴマーを反応させて固体状のポリマーとしたものなども、本発明の硬化性樹脂に含まれるものとする。
上記した開繊炭素繊維束は、例えば、以下の方法により製造することができる。即ち、(1)コア粒子に未硬化の硬化性樹脂を付着させて、コア粒子の少なくとも一部を未硬化の硬化性樹脂により被覆し、(2)複数の炭素繊維からなる炭素繊維束に、前記未硬化の硬化性樹脂により被覆したコア粒子を接触させて、前記炭素繊維表面に未硬化の硬化性樹脂を介してコア粒子を付着させ、(3)前記未硬化の硬化性樹脂を硬化させて、前記コア粒子が硬化性樹脂を介して前記炭素繊維表面に一体的に接合するように被覆粒子を形成する、ことにより上記した開繊炭素繊維束を製造することができる。以下、各工程について説明する。
先ず、コア粒子に未硬化の硬化性樹脂を付着させる。コア粒子としては、上記したような無機粒子または有機粒子を使用することができる。また、未硬化の硬化性樹脂とは、硬化前の状態が液状、ペースト状ないし半固形状であり、硬化により固化するものを意味し、好適には上記したような樹脂を使用することができる。コア粒子に未硬化の硬化性樹脂を付着させるは、未硬化の硬化性樹脂にコア粒子を浸漬したり、コア粒子に未硬化の硬化性樹脂を塗布することにより行うことができる。コア粒子に未硬化の硬化性樹脂を付着させることで、コア粒子表面の少なくとも一部を未硬化の硬化性樹脂により被覆することができる。コア粒子表面の全体が未硬化の硬化性樹脂により被覆されるようにするためには、未硬化の硬化性樹脂にコア粒子を浸漬することにより、コア粒子に未硬化の硬化性樹脂を付着させることが好ましい。
次に、未硬化の硬化性樹脂により被覆したコア粒子を、複数の炭素繊維からなる炭素繊維束に接触させることにより、炭素繊維表面に未硬化の硬化性樹脂を介してコア粒子を付着させる。未硬化の硬化性樹脂により被覆したコア粒子を炭素繊維束に接触させる手段としては、特に制限させるものではなく、例えば、コア粒子を添加した炭素繊維束を、回転、振動させるなどの方法が挙げられる。未硬化の硬化性樹脂で被覆されたコア粒子が炭素繊維表面に付着すると、未硬化の硬化性樹脂は炭素繊維表面にも濡れ広がり、コア粒子と炭素繊維との間が未硬化の熱硬化性樹脂により埋まり、図1〜図3に示したような状態となる。
次いで、未硬化の硬化性樹脂を硬化させる。コア粒子が上記したような状態で炭素繊維表面に付着した状態で未硬化の硬化性樹脂を硬化させることで、コア粒子が硬化性樹脂を介して炭素繊維表面に一体的に接合するように被覆粒子が形成される。被覆粒子は、硬化性樹脂を介して炭素繊維表面に強固に結合するため、炭素繊維どうしが密着せずに一定の間隔を保つことができる。その結果、炭素繊維束を開繊した状態で保持することができる。
本発明の繊維強化複合材料は、上記した開繊炭素繊維束と、開繊炭素繊維束に含浸されたマトリックス樹脂と含む。マトリックス樹脂としては、熱硬化性樹脂または熱可塑性樹脂のいずれであってもよいが、繊維強化複合材料に優れた曲げ弾性率および曲げ強度を付与できる観点から、熱可塑性樹脂が好ましい。
<開繊炭素繊維束の作製>
主剤のエポキシ化合物1質量%、硬化剤のアミン化合物1質量%、および溶媒のアセトン98質量%を混合した溶液を作製した。
次に、この溶液にシリカ粒子(日揮触媒化成製、商品名「ESPHERIQUE 150N」、平均粒径6μm、比表面積190m2/g)を、数秒間接触させた後、該シリカ粒子を炭素繊維束(台湾プラスチック社製、商品名TC−35 12K,フィラメント数12000本)の表面に添加した。
次いで、該シリカ粒子を添加した炭素繊維束を、素手で約5分間回転および振動させ、該シリカ粒子を炭素繊維束内部に侵入させた。該シリカ粒子を侵入させた炭素繊維束を室温にて24時間静置し、開繊炭素繊維束を得た。
開繊炭素繊維束におけるシリカ粒子および二液型エポキシ樹脂の合計付着量は、1質量%であった。
マトリックス樹脂としてポリプロピレン(PP)樹脂(プライムポリマー社製 商品名「J108M」)を用いた。ポリプロピレン樹脂をフィルム状に押出し、溶融状態のポリプロピレン樹脂フィルムを、上記で得られた開繊炭素繊維束からなる織物上に積層し、その後、250℃に加熱しながら1MPaの圧力で3分間に亘って圧縮することにより、ポリプロピレン樹脂を開繊炭素繊維束中に含浸させて、厚みが250μmの炭素繊維強化複合体を得た。なお、炭素繊維強化複合体中において、炭素繊維の含有量は、50質量%であった。
開繊処理を行っていない炭素繊維束(台湾プラスチック社製、商品名TC−35 12K,フィラメント数12000本)を用いたこと以外は、実施例1Aと同様の手法で炭素繊維強化複合体を作製し、同様に曲げ強度の評価を行った。測定結果は、下記表1に示される通りであった。
原料として、以下の材料を使用した。
[炭素繊維織物]
3K織物:台湾プラスチックス社製 商品名「EC3C」(PAN系炭素繊維束、サイジング材:エポキシ系樹脂、フィラメント数:3000本、目付量:200g/m2、厚み:0.19mm、平織)
[シリカ粒子]
シリカ粒子1:日揮触媒化成株式会社製、商品名「ESPHERIQUE N15」(平均粒径6μm、比表面積5m2/g)
[樹脂フィルム]
PP1:プライムポリマー社製、商品名「J108M」(ホモポリプロピレン樹脂)100重量部と、三洋化成工業株式会社製、商品名「ユーメックス1010」(酸変性ポリプロピレン)10重量部とを押出機にて、溶融混練した後、成膜化したPPフィルム
PVC1:徳山積水工業株式会社製 塩化ビニル系樹脂(重合度400)を成膜化したPVCフィルム
PPS1:東レ株式会社製、ポリフェニレンサルファイド樹脂製フィルム、商品名「トレリナ」(厚み50μm)
PEEK1:信越ポリマー株式会社製 ポリエーテルエーテルケトン樹脂製フィルム、商品名「Shin−Etsu Sepla Film」(厚み50μm)
次に上記エタノール水にシリカ粒子1を5質量部添加し、開繊含浸液1を製造した。
その後、3K織物を用意し、炭素繊維束重量に対して0.75倍の開繊含浸液を塗布した。その後、得られた炭素繊維束を、300℃で2分間加熱し、乾燥させた。
上記した炭素繊維強化複合材料を、複数枚数重ねて、熱融着によって一体化させて試験片を作製した。得られた試験片の曲げ強度をJIS K7074に準拠して測定した。結果を表2に示す。
実施例1Bの開繊含浸液を水100質量部にシリカ粒子1を混合した開繊含浸液に変更した以外は同様に開繊処理及びマトリクス樹脂との含浸を行い、得られた炭素繊維強化複合材料の曲げ強度を評価した。結果を表2に示す。
実施例1Bのマトリクス樹脂をPP1からPVC1に変更した以外は同様に炭素繊維強化複合材料を製造し、曲げ強度を評価した。結果を表2に示す。
比較例1Bのマトリクス樹脂をPP1からPVC1に変更した以外は同様に炭素繊維強化複合材料を製造し、曲げ強度を評価した。結果を表2に示す。
実施例1Bのマトリクス樹脂をPP1からPPS1に変更した以外は同様に炭素繊維強化複合材料を製造し、曲げ強度を評価した。結果を表2に示す。
実施例1Bのマトリクス樹脂をPP1からPPS1に変更し、エタノールをアセトンに変更した以外は同様に炭素繊維強化複合材料を製造し、曲げ強度を評価した。結果を表2に示す。
実施例1Bのマトリクス樹脂をPP1からPPS1に変更し、開繊含浸液を水100質量部のみとした以外は同様に炭素繊維強化複合材料を製造し、曲げ強度を評価した。結果を表2に示す。
実施例1Bのマトリクス樹脂をPP1からPEEK1に変更した以外は同様に炭素繊維強化複合材料を製造し、曲げ強度を評価した。結果を表2に示す。
実施例1Bのマトリクス樹脂をPP1からPEEK1に変更し、エタノールをアセトンに変更した以外は同様に炭素繊維強化複合材料を製造し、曲げ強度を評価した。結果を表2に示す。
実施例1Bのマトリクス樹脂をPP1からPEEK1に変更し、開繊含浸液を水100質量部のみとした以外は同様に炭素繊維強化複合材料を製造し、曲げ強度を評価した。結果を表2に示す。
実施例1B〜実施例5B、比較例1B〜比較例4Bの評価結果から、コア粒子と、コア粒子の表面の少なくとも一部を被覆するように硬化性樹脂被膜とからなる被覆粒子が、炭素繊維表面に一体的に接合されるようにするためには、炭素繊維に付着したサイジング剤を軟化又は溶解せしめる有機溶剤に接触させることも重要であることがわかる。この実験結果をより詳細に検証するために、代表的なサイジング剤であるエポキシ樹脂を各種溶媒に浸漬し、溶解試験を実施した。
<開繊含浸液の作製>
1,5−ジヒドロキシナフタレン(和光純薬社製商品名「048−02342」)10質量部、メチルアミン(和光純薬社製商品名「132−01857」)4質量部、およびホルマリン(ホルムアルデヒドの含有量:37質量%、和光純薬社製商品名「064−00406」)8質量部を含むモノマーと、溶媒としてエタノール水(エタノールの含有量:50質量%、和光純薬社製商品名「057−00456」)600質量部とを均一に混合して、ナフトキサジン樹脂溶液を作製した。
次に上記ナフトキサジン樹脂溶液にシリカ粒子1を5質量部添加し、開繊含浸液1を製造した。
その後、3K織物を用意し、炭素繊維束重量に対して0.75倍の開繊含浸液を塗布した。その後、得られた炭素繊維束を、130℃で2分間加熱し、ナフトキサジン樹脂の重合を生じさせた開繊繊維束を経た。
上記した炭素繊維強化複合材料を、複数枚数重ねて、熱融着によって一体化させて試験片を作製した。得られた試験片の曲げ強度をJIS K7074に準拠して測定した。結果を表3に示す。
実施例7Bのマトリクス樹脂をPPS1からPEEK1に変更した以外は同様に炭素繊維強化複合材料を製造し、曲げ強度を評価した。結果を表3に示す。
Claims (10)
- マトリックス樹脂を含浸させて繊維強化複合材料として使用される開繊炭素繊維束であって、
複数の炭素繊維からなる炭素繊維束と、前記炭素繊維間に配置された被覆粒子とを備え、
前記被覆粒子が、コア粒子と、前記コア粒子表面の少なくとも一部を被覆する合成樹脂被覆とからなり、
前記コア粒子が、前記合成樹脂被覆を介して前記炭素繊維表面に一体的に接合されており、
前記コア粒子の平均粒子径が、1〜25μmであり、
前記マトリックス樹脂が熱可塑性樹脂(但し、最低粘度が1000cPs以下の熱可塑性樹脂を除く)である、開繊炭素繊維束。 - 前記コア粒子が、カーボン粒子、シリカ粒子、アルミナ粒子、酸化チタン粒子、炭酸カルシウム粒子、タルク粒子、ジビニルベンゼン樹脂粒子からなる群より選択される少なくとも1種を含む、請求項1に記載の開繊炭素繊維束。
- 前記合成樹脂が、エポキシ樹脂、ウレタン樹脂、シリコーン樹脂、フェノール樹脂、ビニルエステル樹脂からなる群より選択される硬化性樹脂を少なくとも1種を含む、請求項1または2に記載の開繊炭素繊維束。
- 少なくとも1つの前記被覆粒子が、2本以上の炭素繊維と接合されている、請求項1〜3のいずれか一項に記載の開繊炭素繊維束。
- 請求項1〜4のいずれか一項に記載の開繊繊維束と、前記開繊炭素繊維束に含浸されたマトリックス樹脂とを含む、繊維強化複合材料。
- 前記マトリックス樹脂が、ポリオレフィン系樹脂、ポリアミド樹脂、アクリル樹脂、ポリアミド樹脂、ポリカーボネート樹脂、ポリフェニレンサルファイド樹脂、及びポリエーテルエーテルケトン樹脂からなる群より選択される熱可塑性樹脂である、請求項5に記載の繊維強化複合材料。
- マトリックス樹脂を含浸させて繊維強化複合材料として使用される開繊炭素繊維束を製造する方法であって、
コア粒子に未硬化の硬化性樹脂を付着させて、コア粒子表面の少なくとも一部を未硬化の硬化性樹脂により被覆する工程と、
複数の炭素繊維からなる炭素繊維束に、前記未硬化の硬化性樹脂により被覆したコア粒子を接触させて、前記炭素繊維表面に未硬化の硬化性樹脂を介してコア粒子を付着させる工程と、
前記未硬化の硬化性樹脂を硬化させて、前記コア粒子が硬化性樹脂を介して前記炭素繊維表面に一体的に接合するように被覆粒子を形成する工程と、
を含み、
前記コア粒子に未硬化の硬化性樹脂を付着させる工程が、前記硬化性樹脂が溶解し得る有機溶剤と水との混合溶媒に前記コア粒子を分散させた溶液を、前記炭素繊維に接触させることにより実施され、
前記コア粒子の平均粒子径が、1〜25μmであり、
前記マトリックス樹脂が熱可塑性樹脂(但し、最低粘度が1000cPs以下の熱可塑性樹脂を除く)である、
る、開繊炭素繊維束の製造方法。 - 前記硬化性樹脂の硬化が、常温硬化、加熱硬化、活性エネルギー線硬化から選択される少なくとも1種により行われる、請求項7に記載の方法。
- 前記硬化性樹脂が、主剤および硬化剤からなる二液型硬化性樹脂である、請求項7または8に記載の方法。
- 前記硬化性樹脂がエポキシ樹脂であり、
前記有機溶剤が、酢酸エチル、アセトニトリル、ジメチルスルホキシド、酢酸、トルエン、1−プロパノール、およびエタノールからなる群より選択される、請求項7〜9のいずれか一項に記載の方法。
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