JPWO2011064994A1 - 炭素繊維強化複合材料 - Google Patents
炭素繊維強化複合材料 Download PDFInfo
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- JPWO2011064994A1 JPWO2011064994A1 JP2011543104A JP2011543104A JPWO2011064994A1 JP WO2011064994 A1 JPWO2011064994 A1 JP WO2011064994A1 JP 2011543104 A JP2011543104 A JP 2011543104A JP 2011543104 A JP2011543104 A JP 2011543104A JP WO2011064994 A1 JPWO2011064994 A1 JP WO2011064994A1
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- Prior art keywords
- carbon fiber
- composite material
- reinforced composite
- fiber reinforced
- resin
- Prior art date
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- 239000004917 carbon fiber Substances 0.000 title claims abstract description 108
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- 239000011208 reinforced composite material Substances 0.000 title claims abstract description 36
- 229920005989 resin Polymers 0.000 claims abstract description 62
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- 239000010410 layer Substances 0.000 claims description 17
- 229920002554 vinyl polymer Polymers 0.000 claims description 13
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/042—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with carbon fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/40—Shaping or impregnating by compression not applied
- B29C70/42—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles
- B29C70/46—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles using matched moulds, e.g. for deforming sheet moulding compounds [SMC] or prepregs
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2351/06—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
- Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
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- Y10T442/2984—Coated or impregnated carbon or carbonaceous fiber fabric
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- Composite Materials (AREA)
- Mechanical Engineering (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Reinforced Plastic Materials (AREA)
- Laminated Bodies (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
- Moulding By Coating Moulds (AREA)
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Abstract
Description
(1)連続した炭素繊維と、変性ポリオレフィン系樹脂を含有するマトリックス樹脂からなる炭素繊維強化複合材料。
(2)前記マトリックス樹脂が、海島構造からなる多相構造を形成し、海島構造の島部分(独立した相)の径が平均0.01μm以上であり、0.5μm以下であることを特徴とする(1)に記載の炭素繊維強化複合材料。
(3)前記変性ポリオレフィン系樹脂が、ポリオレフィン系樹脂を、エチレン性二重結合および極性基を同一分子内に含む単量体によりグラフト変性することにより得られる樹脂であることを特徴とする(1)または(2)に記載の炭素繊維強化複合材料。
(4)前記変性ポリオレフィン系樹脂が、エチレン性二重結合および極性基を同一分子内に含む単量体に加え、さらに芳香族ビニル化合物または、共役ジエン系化合物を用いてグラフト変性し得られる樹脂であることを特徴とする(1)〜(3)のいずれかに記載の炭素繊維強化複合材料。
(5)エチレン性二重結合および極性基を同一分子内に含む単量体が、(メタ)アクリル酸、無水マレイン酸、(メタ)アクリル酸グリシジルから選ばれる少なくとも1種である(3)または(4)に記載の炭素繊維強化複合材料。
(6)芳香族ビニル化合物または共役ジエン系化合物が、スチレン、イソプレンから選ばれる少なくとも1種である(4)または(5)に記載の炭素繊維強化複合材料。
(7)前記変性ポリオレフィン系樹脂のグラフト率が0.25以上であることを特徴とする(3)〜(6)のいずれかに記載の炭素繊維強化複合材料。
(8)前記変性ポリオレフィン系樹脂のグラフト部分の長さが、数平均分子量で1000以上であること特徴とする(3)〜(7)のいずれかに記載の炭素繊維強化複合材料。
(9)マトリックス樹脂の重量含有率が20%〜70%である(1)〜(8)のいずれか一項に記載の炭素繊維強化複合材料。
(10)前記連続した炭素繊維の形状がUD(一方向配列材)、織物または編物である(1)〜(9)のいずれか一項に記載の炭素繊維強化複合材料。
(11)あらかじめマトリックス樹脂と炭素繊維を1層ずつあるいは複数層で交互に積層したうえで、マトリックス樹脂の融点以上の温度条件下で溶融状態のマトリックス樹脂を加圧下で炭素繊維に含浸せしめた後、冷却、硬化させることにより作製される(1)〜(10)のいずれか一項に記載の炭素繊維強化複合材料。
(12)あらかじめマトリックス樹脂と炭素繊維を1層ずつあるいは複数層で交互に積層したうえで、マトリックス樹脂の融点以上の温度条件下において加圧下で作製した炭素繊維複合材料を、重ねて積層し、マトリックス樹脂の融点以上の温度条件下において加圧下で作製される(1)〜(11)のいずれか一項に記載の炭素繊維複合材料
(13)前記海島構造の島部分(独立した相)の数が、10μm2あたり4000個以上であることを特徴とする(2)〜(12)いづれか一項に記載の炭素繊維強化複合材料。
(14)前記海島構造において、ポリオレフィン系樹脂からなる海部分(連続した相)に、エチレン性二重結合および極性基を同一分子内に含む単量体及び、芳香族ビニル化合物または共役ジエン系化合物からなる島部分(独立した相)を有することを特徴とする(2)〜(13)いづれか一項に記載の炭素繊維強化複合材料。
(15)ASTM−D2344に基づく見かけの層間せん断強度が25℃で25MPa以上である(1)〜(14)のいずれか一項に記載の炭素繊維強化複合材料。
<変性ポリオレフィン樹脂の製造>
(製造例1)メタクリル酸グリシジル/スチレン(GMA/St)変性ポリプロピレンの製造:(a)ホモポリプロピレン((株)プライムポリマー製J105G、MFR=9)100重量部、(b)1,3−ジ(t−ブチルパーオキシイソプロピル)ベンゼン(日本油脂(株)製;パーブチルP、1分間半減期温度;175℃)0.5重量部を、200℃に設定した二軸押出機(TEX44;L/D=40、日本製鋼所製)のホッパーに供給して溶融混練した後、シリンダー途中より(c)スチレン5重量部、(d)メタクリル酸グリシジル5重量部の混合液を圧入し、溶融混練して、変性ポリプロピレン樹脂のペレットを得た。樹脂のメルトフローレート(MFR)は、JIS K7210に準拠して230℃で測定した結果100(g/10min)であった。得られたペレットをTダイ製膜機に供給し、厚さ100μmのフィルムを得た。また、これとは別にペレットを凍結粉砕し、変性ポリプロピレンのパウダーを得た。また、得られたペレットを熱キシレン中に溶解させ、晶析して得られたグラフトポリマーを滴定し、グラフト率が1.2であることがわかった。グラフトポリマーを晶析したあとの母液(キシレン溶液)を濃縮し、GPCにより分子量を求めた。この分子量は4400であり、この値をグラフト鎖の分子量とした。
東邦テナックス社製PAN系炭素繊維(商品名:IM60S平織材、繊維目付:195g/m2、密度:1.80g/cm3、商品名:W3101平織材、繊維目付:200g/m2、密度:1.76g/cm3))
<炭素繊維複合材料の層間せん断強度測定>
ASTM−D2344に準拠して行った。
マトリックス樹脂中の島部分(独立した相)の数の測定は、以下のような方法により行った。
2値化の方法:自動
固定しきい値:無
外縁補正:四辺
穴埋め:有
小図形除去面積:10nm2
補正方法:収縮
収縮分離:回数10、小図形5、接触度100
雑音除去フィルター:無
シェーディング:無
<炭素繊維複合材料の作製方法>
(実施例1)
凸型(厚さ2mm、6.5cm角)形状を有するステンレス板(厚さ1cm、10cm角)に、中心部に孔(厚さ1cm、6.5cm角)があいたステンレス製スペーサー(厚さ1cm、10cm角)を噛み合わせた。孔の中に剥離フィルムとしてテフロン(登録商標)シートを置き、その上から製造例1にて作製した変性ポリプロピレンフィルムと炭素繊維平織材を交互に重ね、ポリプロピレン層は合計13層、炭素繊維層は12層となるように積層した。積層したポリプロピレンは、複合材料の全重量に対して、50重量%となるようにし、炭素繊維平織材は、アセトン溶剤にてサイジング剤を除去したものを用いた。
25cm角の正方形状のステンレス板状に20cm角のテフロン(登録商標)シートを置き、その上に製造例1にて作製した変性ポリプロピレンフィルムと15cm角の炭素繊維平織材を順に重ねた。さらに上部に製造例1にて作製した変性ポリプロピレンフィルムと20cm角のテフロン(登録商標)シートを積層した。積層したポリプロピレンは、複合材料の全重量に対して、50重量%となるようにし、炭素繊維平織材は、アセトン溶剤にてサイジング剤を除去したものを用いた。
(実施例7)
サイジング剤の除去を行っていない炭素繊維平織材を用いた以外は、上記実施例1と全く同じ方法にて行った。結果を表1に示す。
(実施例8)
製造例2にて作製した変性ポリプロピレンを用いた以外は、上記実施例1と全く同じ方法にて行った。結果を表1に示す。
(比較例5)
未変性のポリプロピレンフィルムを用いた以外は、上記実施例6と全く同じ方法にて行った。結果を表1に示す。
(比較例6)
未変性のポリプロピレンフィルムおよびサイジング剤の除去を行っていない炭素繊維平織剤を用いた以外は、上記実施例6と全く同じ方法にて行った。結果を表1に示す。
(比較例7)
QE−060Eフィルムを用い、加圧条件を20MPaとした以外は、上記実施例1と全く同じ方法にて行った。結果を表1に示す。
Claims (15)
- 連続した炭素繊維と、変性ポリオレフィン系樹脂を含有するマトリックス樹脂からなる炭素繊維強化複合材料。
- 前記マトリックス樹脂が、海島構造からなる多相構造を形成し、海島構造の島部分(独立した相)の径が平均0.01μm以上であり、0.5μm以下であることを特徴とする請求項1に記載の炭素繊維強化複合材料。
- 前記変性ポリオレフィン系樹脂が、ポリオレフィン系樹脂を、エチレン性二重結合および極性基を同一分子内に含む単量体によりグラフト変性することにより得られる樹脂であることを特徴とする請求項1または2に記載の炭素繊維強化複合材料。
- 前記変性ポリオレフィン系樹脂が、エチレン性二重結合および極性基を同一分子内に含む単量体に加え、さらに芳香族ビニル化合物または、共役ジエン系化合物を用いてグラフト変性し得られる樹脂であることを特徴とする請求項1〜3のいずれかに記載の炭素繊維強化複合材料。
- エチレン性二重結合および極性基を同一分子内に含む単量体が、(メタ)アクリル酸、無水マレイン酸、(メタ)アクリル酸グリシジルから選ばれる少なくとも1種である請求項3または4に記載の炭素繊維強化複合材料。
- 芳香族ビニル化合物または共役ジエン系化合物が、スチレン、イソプレンから選ばれる少なくとも1種である請求項4または5に記載の炭素繊維強化複合材料。
- 前記変性ポリオレフィン系樹脂のグラフト率が0.25以上であることを特徴とする請求項3〜6のいずれかに記載の炭素繊維強化複合材料。
- 前記変性ポリオレフィン系樹脂のグラフト部分の長さが、数平均分子量で1000以上であること特徴とする請求項3〜7のいずれかに記載の炭素繊維強化複合材料。
- マトリックス樹脂の重量含有率が20%〜70%である請求項1〜8のいずれか一項に記載の炭素繊維強化複合材料。
- 前記連続した炭素繊維の形状がUD(一方向配列材)、織物または編物である請求項1〜9のいずれか一項に記載の炭素繊維強化複合材料。
- あらかじめマトリックス樹脂と炭素繊維を1層ずつあるいは複数層で交互に積層したうえで、マトリックス樹脂の融点以上の温度条件下で溶融状態のマトリックス樹脂を加圧下で炭素繊維に含浸せしめた後、冷却、硬化させることにより作製される請求項1〜10のいずれか一項に記載の炭素繊維強化複合材料。
- あらかじめマトリックス樹脂と炭素繊維を1層ずつあるいは複数層で交互に積層したうえで、マトリックス樹脂の融点以上の温度条件下において加圧下で作製した炭素繊維複合材料を、重ねて積層し、マトリックス樹脂の融点以上の温度条件下において加圧下で作製される請求項1〜11のいずれか一項に記載の炭素繊維複合材料
- 前記海島構造の島部分(独立した相)の数が、10μm2あたり4000個以上であることを特徴とする請求項2〜12のいづれか一項に記載の炭素繊維強化複合材料。
- 前記海島構造において、ポリオレフィン系樹脂からなる海部分(連続した相)に、エチレン性二重結合および極性基を同一分子内に含む単量体及び、芳香族ビニル化合物または共役ジエン系化合物からなる島部分(独立した相)を有することを特徴とする請求項2〜13のいづれか一項に記載の炭素繊維強化複合材料。
- ASTM−D2344に基づく見かけの層間せん断強度が25℃で25MPa以上である請求項1〜14のいずれか一項に記載の炭素繊維強化複合材料。
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JP2005213679A (ja) | 2004-01-29 | 2005-08-11 | Sanyo Chem Ind Ltd | 無機繊維用集束剤 |
JP2005213478A (ja) | 2004-02-02 | 2005-08-11 | Idemitsu Kosan Co Ltd | ポリオレフィン系炭素繊維強化樹脂組成物及びそれからなる成形品 |
JP2006167982A (ja) * | 2004-12-13 | 2006-06-29 | Daicel Chem Ind Ltd | 長繊維強化熱可塑性樹脂構造体の製造方法 |
US7935760B2 (en) * | 2005-06-22 | 2011-05-03 | Exxonmobil Chemical Patents Inc. | Process of making a heterogeneous polymer blend |
JP2010235774A (ja) * | 2009-03-31 | 2010-10-21 | Toyobo Co Ltd | 炭素長繊維強化ポリプロピレン複合材料 |
-
2010
- 2010-11-25 EP EP20100832844 patent/EP2508552A1/en not_active Withdrawn
- 2010-11-25 US US13/512,716 patent/US20120295504A1/en not_active Abandoned
- 2010-11-25 WO PCT/JP2010/006864 patent/WO2011064994A1/ja active Application Filing
- 2010-11-25 JP JP2011543104A patent/JP5740313B2/ja active Active
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JP5947421B2 (ja) | 2016-07-06 |
US20120295504A1 (en) | 2012-11-22 |
WO2011064994A1 (ja) | 2011-06-03 |
JP5740313B2 (ja) | 2015-06-24 |
EP2508552A1 (en) | 2012-10-10 |
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