JP6833679B2 - 高いz方向電気伝導率をもつ複合材料 - Google Patents
高いz方向電気伝導率をもつ複合材料 Download PDFInfo
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- JP6833679B2 JP6833679B2 JP2017515720A JP2017515720A JP6833679B2 JP 6833679 B2 JP6833679 B2 JP 6833679B2 JP 2017515720 A JP2017515720 A JP 2017515720A JP 2017515720 A JP2017515720 A JP 2017515720A JP 6833679 B2 JP6833679 B2 JP 6833679B2
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Description
本明細書では、用語「ナノ粒子」は、少なくとも1つの寸法が約0.1マイクロメートルよりも小さく(<100ナノメートル)、アスペクト比が約50:1から約5000:1である材料を意味する。ナノ粒子の寸法は、動的光散乱(DSL)技術によって決定することができる。例えば、Horiba製のSZ−100などのナノ粒子アナライザーを使用してもよい。
炭素ベールは、約2gsmから約10gsm、いくつかの実施態様では約2gsmから約6gsmを含む、約1gsm(g/m2)から約30gsmの面積重量を有する、ランダムに配置された繊維の軽量な不織ベールである。
本明細書の目的に適したポリマー強化粒子には、熱可塑性又はエラストマー粒子が含まれる。これらのポリマー強化粒子は、金属などの伝導性被覆がされていない。
強化繊維を含浸/注入するための硬化性マトリックス樹脂(又は樹脂組成物)は、1種又は複数種の未硬化の熱硬化性樹脂を含有する硬化可能又は熱硬化可能な樹脂であり、これには、エポキシ樹脂、イミド(ポリイミド及びビスマレイミドなど)、ビニルエステル樹脂、シアン酸エステル樹脂、イソシアネート変性エポキシ樹脂、フェノール樹脂、ベンゾオキサジン、ホルムアルデヒド縮合樹脂(尿素、メラミン及びフェノールなど)、不飽和ポリエステル、そのハイブリッド、ブレンド及び組合せが含まれるが、それだけには限定されない。
本明細書の目的のための強化繊維には、高い引張り強さ、例えば、500ksi(又は3447MPa)超を有する炭素又はグラファイト繊維が含まれる。強化繊維は、連続一方向又は多方向繊維として、織布又は多軸織物として、複数のフィラメントからできている連続トウの形態であってよい。一方向繊維は、一方向のみに延びる(又は伸びる)繊維を意味する。多軸織物には、非捲縮織物が含まれる。いくつかの実施態様では、強化繊維は、不織層ではなく、一方向繊維又は織布の形態である。さらに、炭素繊維は、寸法を整えても整えなくてもよい。
用語「プリプレグ」は、本明細書では、繊維の体積の少なくとも一部分内に硬化性樹脂組成物を含浸させた繊維のシート又は層を意味する。航空宇宙構造体を製造するのに使用するプリプレグは通常、一方向強化用繊維、例えば炭素繊維の樹脂含浸シートであり、しばしば「テープ」又は「一方向テープ」と呼ばれる。プリプレグは、完全含浸プリプレグ又は部分含浸プリプレグであってよい。強化繊維に含浸しているマトリックス樹脂は、部分硬化又は未硬化状態であってよい。用語「含浸(impregnated)」は、本明細書では、含浸プロセスを受け、それによって繊維が少なくとも部分的にマトリックス樹脂によって囲まれる、又はマトリックス樹脂に包埋される繊維を意味する。
本明細書に記載された樹脂組成物は、鋳造又は成形された構造材料を製造するために使用でき、改善された体積電気伝導率を有する繊維強化耐力又は耐衝撃複合材構造体の製作に特に適している。
以下の実施例で製造した複合材試料を、z方向電気伝導率及び機械的性質を測定するための以下の手順に従って試験した。
抵抗率(ρ) [ohm−m]=(V/I)/t・A
伝導率(σ) (S/m)=1/ρ
ここで:
V=潜在的な電圧(ボルト)
I=強制電流(アンペア)
T=z寸法である試料の厚さ(m)
A=X×Y寸法である断面積(m2)
表3に開示した配合に基づいて4種の異なる樹脂組成物を調製した。コントロール1.1及びコントロール2.1は、層間粒子を含む及び含まない2つのベースライン樹脂系であり、樹脂1.0及び樹脂2.0は、その2つのMWCNT修飾バージョンである。組成物は、重量百分比(w/w)で報告されている。
アラルダイト(登録商標)MY0510は、Huntsmanから入手可能なp−アミノフェノール樹脂のトリグリシジルエーテルであり、
SUMIKAEXCEL 5003Pは、Sumitomo Chemical Co.から入手可能なポリエーテルスルホンポリマーであり、
MWCNTは、15nmの平均直径及び約1mmの平均長さを有する多層カーボンナノチューブを意味し、
TGP3551は、硬化の際に不溶性であるEvonik製のポリアミド粉末Vestasint(登録商標)TGP3551を意味し、
P84粒子は、硬化の際に樹脂に膨潤及び可溶化する、平均粒径分布d50が44ミクロンであるEvonik製の芳香族ポリイミド粒子であり、
架橋TP粒子は、25ミクロンの平均粒径を有するCytec Industries Inc.製の架橋PES−PEESの粒子であり、また
4,4’DDSは、4,4’−ジアミノジフェニルスルホンを意味する。
表6に開示した配合に従って3種の異なる樹脂組成物を調製した。組成物は、重量百分比(w/w)で報告されている。コントロール7.0は、ベースライン粒子強化樹脂系であり、樹脂7.1及び樹脂7.2は、その炭素修飾バージョンである。標準的なプリプレグ製造プロセスに適した流動学的プロファイルをもつ配合をもたらすために、比較的低い濃度の炭素充填剤が選択された。
Claims (22)
- 少なくとも二層の、第1の硬化性マトリックス樹脂を含浸させた強化用炭素繊維と
強化用炭素繊維の隣接する層の間に形成された層間領域であって、(i)強化用炭素繊維を含浸している第1の硬化性マトリックス樹脂と同じであるか、又は異なる第2の硬化性マトリックス樹脂、(ii)層間領域で第2の硬化性マトリックス樹脂の中に分散された伝導性ナノサイズ粒子、及び(iii)ランダムに配置された炭素繊維を含み、層間領域で第2の硬化性マトリックス樹脂に包埋された不織炭素ベール、を含む層間領域と
を含み、
それぞれの伝導性ナノサイズ粒子の動的光散乱(DLS)技術によって測定された寸法は100nmよりも小さい
硬化性複合材料。 - 層間領域が、ポリマー粒子をさらに含む、請求項1に記載の硬化性複合材料。
- 不織炭素ベールが、1gsmから30gsm、又は2gsmから10gsmの面積重量を有する、請求項1又は2に記載の硬化性複合材料。
- 伝導性ナノサイズ粒子が、カーボンナノチューブ(CNT)、カーボンナノ繊維、カーボンナノロープ、カーボンナノリボン、カーボンナノフィブリル、カーボンナノニードル、カーボンナノシート、カーボンナノロッド、カーボンナノコーン、スクロール様形状を有するカーボンナノスクロール、カーボンナノオーム、カーボンブラック粒子、グラファイトナノ小板、グラファイトナノドット、グラフェン、及びそれらの組合せからなる群から選択される、炭素系ナノサイズ構造体である、請求項1から3の何れか一項に記載の硬化性複合材料。
- 炭素系ナノサイズ構造体が、カーボンナノチューブ(CNT)である、請求項4に記載の硬化性複合材料。
- 伝導性ナノサイズ粒子が、複合材料中の全ての硬化性マトリックス樹脂の全重量に対して0.1重量%から10重量%の範囲内の量で存在する、請求項1から5の何れか一項に記載の硬化性複合材料。
- 少なくともいくつかのポリマー粒子が、不織炭素ベールを貫通している、請求項2に記載の硬化性複合材料。
- ポリマー粒子が、複合材料中の全ての硬化性マトリックス樹脂の全重量に対して2重量%から20重量%の含有量で存在する、請求項2又は7に記載の硬化性複合材料。
- ポリマー粒子が、第2の硬化性マトリックス樹脂内で不溶性の熱可塑性粒子又は不溶性エラストマー粒子であり、且つ複合材料の硬化の際に層間領域で離散粒子として残存する、請求項2に記載の硬化性複合材料。
- ポリマー粒子が、
ポリイミド、ポリアミドイミド、ポリアミド、ポリフタルアミド、ポリエーテルケトン、ポリエーテルエーテルケトン、ポリエーテルケトンケトン、ポリアリールエーテルケトン、ポリ硫化フェニレン、液晶ポリマー、及びそれらの共重合体からなる群から選択される少なくとも1種の熱可塑性材料を含む、第2の硬化性マトリックス樹脂内で不溶性の熱可塑性粒子であるか、
架橋ポリブタジエン、ポリアクリル、ポリアクリロニトリル、及びポリスチレンからなる群から選択される少なくとも1種のポリマー材料を含む不溶性エラストマー粒子であるか、又は
不溶性架橋熱可塑性粒子であり、各粒子が、
(a)反応性基に対して化学的に反応性である架橋結合剤を用いて1種又は複数種の反応性基を有する架橋性の熱可塑性ポリマーを架橋させることによって作成される架橋ネットワークと、
(b)1種又は複数種の反応性基を有する少なくとも1種の化合物、反応性基に対して化学的に反応性である架橋剤、及び熱可塑性ポリマーを反応させることによって作成される、独立した架橋ネットワークと絡み合った熱可塑性ポリマー鎖を含む相互侵入ポリマーネットワーク(IPN)
のうちの1つを含む、請求項9に記載の硬化性複合材料。 - 強化用炭素繊維を含浸している第1の硬化性マトリックス樹脂が、全体にわたって分散されている伝導性ナノサイズ粒子をさらに含む、請求項1に記載の硬化性複合材料。
- 強化用炭素繊維を含浸している第1の硬化性マトリックス樹脂が、1種又は複数種の熱硬化性樹脂を含む、請求項1に記載の硬化性複合材料。
- 熱硬化性樹脂が、エポキシ樹脂、イミド、ビニルエステル樹脂、シアン酸エステル樹脂、フェノール樹脂、ベンゾオキサジン、ホルムアルデヒド縮合樹脂、不飽和ポリエステル、及びそれらの組合せから選択される、請求項12に記載の硬化性複合材料。
- 強化用炭素繊維の少なくとも1つの層が、連続一方向繊維又は織布の形態である、請求
項1に記載の硬化性複合材料。 - 複合材構造体を製作する方法であって:
(a)各プリプレグプライが、硬化性マトリックス樹脂中に包埋されている強化用炭素繊維の繊維層、及びマトリックス樹脂全体にわたって分散された伝導性ナノサイズ粒子を含む、複数のプリプレグプライを形成すること;
(b)少なくとも1つの不織炭素ベールが2本の隣接するプリプレグプライの間に配置されるように、少なくとも1つの不織炭素ベールと一緒にプリプレグプライを積み重ね配置にレイアップし、ラミネートを形成すること;
(c)圧力を加えてラミネートを一体化すること;並びに
(d)ラミネートを硬化すること;
を含み、
少なくとも1つの不織炭素ベールが、ランダムに配置された炭素繊維を含み、それぞれの伝導性ナノサイズ粒子の動的光散乱(DLS)技術によって測定された寸法は100nmよりも小さい、
方法。 - (a)の各プリプレグプライが、強化用炭素繊維の層の少なくとも一面に隣接して配置されたポリマー粒子をさらに含み、且つ
(c)の一体化の後、少なくともいくつかのポリマー粒子が、不織炭素ベールを貫通する、
請求項15に記載の方法。 - 複合材料を製作する方法であって:
(a)その中に分散された伝導性ナノサイズ粒子を含む少なくとも1つの硬化性樹脂フィルムを形成すること;
(b)不織炭素ベールが樹脂フィルムと繊維層の間に配置されるように、少なくとも1つの硬化性樹脂フィルムを少なくとも1つの不織炭素ベール及び強化用炭素繊維の繊維層に配置すること;
(c)硬化性樹脂フィルム、不織炭素ベール及び繊維層に熱及び圧力を加えて、樹脂含浸炭素繊維及び樹脂含浸炭素ベールを含むプリプレグプライを形成すること
を含み、
少なくとも1つの不織炭素ベールが、ランダムに配置された炭素繊維を含み、それぞれの伝導性ナノサイズ粒子の動的光散乱(DLS)技術によって測定された寸法は100nmよりも小さい、
方法。 - (a)の少なくとも1つの硬化性樹脂フィルムが、ポリマー粒子をさらに含み、且つ
(e)で熱及び圧力を加えた後、少なくともいくつかのポリマー粒子が不織炭素ベールを貫通する、
請求項17に記載の方法。 - 繊維層が2つの不織炭素ベールの間に配置され、各樹脂フィルムが不織炭素ベールの1つと接触するように、2つの硬化性樹脂フィルムが(a)で形成され、且つ2つの不織炭素ベールが2つの樹脂フィルム及び繊維層と(c)で混合される、請求項17又は18に記載の方法。
- 不織炭素ベールが、1gsmから30gsm、又は2gsmから10gsmの面積重量を有する、請求項15又は17に記載の方法。
- 伝導性ナノサイズ粒子が、カーボンナノチューブである、請求項15又は17に記載の方法。
- 強化用炭素繊維の繊維層が、連続一方向繊維又は織布の形態である、請求項15又は17に記載の方法。
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BR112017005619B1 (pt) | 2021-12-14 |
EP3197674B1 (en) | 2021-11-10 |
BR112017005619A2 (pt) | 2018-01-23 |
TWI677424B (zh) | 2019-11-21 |
EP3197674A1 (en) | 2017-08-02 |
US10213984B2 (en) | 2019-02-26 |
CA2961910A1 (en) | 2016-03-31 |
CN107107537A (zh) | 2017-08-29 |
WO2016048885A1 (en) | 2016-03-31 |
CA2961910C (en) | 2022-08-16 |
ES2905454T3 (es) | 2022-04-08 |
JP2021020462A (ja) | 2021-02-18 |
AU2015321585A1 (en) | 2017-03-16 |
RU2017113772A3 (ja) | 2019-02-21 |
CN107107537B (zh) | 2020-03-10 |
US10549499B2 (en) | 2020-02-04 |
US20160082691A1 (en) | 2016-03-24 |
RU2017113772A (ru) | 2018-10-24 |
US20190143633A1 (en) | 2019-05-16 |
RU2702556C2 (ru) | 2019-10-08 |
TW201615390A (zh) | 2016-05-01 |
JP2017535447A (ja) | 2017-11-30 |
AU2015321585B2 (en) | 2019-07-11 |
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