JP6568922B2 - 複合材料 - Google Patents
複合材料 Download PDFInfo
- Publication number
- JP6568922B2 JP6568922B2 JP2017233117A JP2017233117A JP6568922B2 JP 6568922 B2 JP6568922 B2 JP 6568922B2 JP 2017233117 A JP2017233117 A JP 2017233117A JP 2017233117 A JP2017233117 A JP 2017233117A JP 6568922 B2 JP6568922 B2 JP 6568922B2
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- Prior art keywords
- conductive
- fibers
- conductive polymer
- resin
- composite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- CMLFRMDBDNHMRA-UHFFFAOYSA-N 2h-1,2-benzoxazine Chemical compound C1=CC=C2C=CNOC2=C1 CMLFRMDBDNHMRA-UHFFFAOYSA-N 0.000 description 2
- XMTQQYYKAHVGBJ-UHFFFAOYSA-N 3-(3,4-DICHLOROPHENYL)-1,1-DIMETHYLUREA Chemical compound CN(C)C(=O)NC1=CC=C(Cl)C(Cl)=C1 XMTQQYYKAHVGBJ-UHFFFAOYSA-N 0.000 description 2
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Description
i)硬化性樹脂マトリックスを含浸させた強化繊維の少なくとも1つの構造層と、
ii)強化繊維に隣接したまたは近接した少なくとも1つの導電性の複合粒子と、を含む。
導電性ブリッジを生成する。この材料の解決策は、多層複合構造の耐衝撃性および積層剥離強度を同時に改善させ得る一方、電流、例えば落雷によって生じたものなどを、複合構造の広域範囲にわたって、拡散させるか放散させ、それによって、局所部分に対する突発的な損害の可能性を減らす。その上、導電性複合粒子は、潜在的に、落雷の直接的な影響、また、特に、第3世代複合構造におけるエッジグロー(edge glow)現象を軽減するか排除するための効率的な解決策であり得る。最終的に、導電性の複合粒子は、複合材の電磁性能の面で更なる利益をもたらすことができる。高導電性および/または磁性充填材に基づく複合粒子は、複合構造の電磁干渉(EMI)遮蔽効率、誘電率および透磁率特性に適応させるための柔軟なツールとして使用され得る。
図1は、本開示の一実施形態に係る導電性複合粒子を概略的に描写する。図1は、球形状粒子を示すが、本開示の導電性の複合粒子は、限定するものではないが、球状、回転楕円、楕円、立方体、多面体、棒状、円盤形状、および同様のものを含む任意の適切な形状のものであり得る、別個の、3次元構造であることが理解されるべきである。その上、粒子は、明確に定義された幾何形状を有してもよいし、あるいは、不規則な形状であってもよい。
材料、非金属の導電性材料、およびそれらの組み合わせを含み得る。適切な金属材料は、限定されるものではないが、銀、金、白金、パラジウム、ニッケル、銅、鉛、錫、アルミニウム、チタン、それらの合金および混合物を含む任意の既知の金属を含む。好適には、金属材料は、1×107S/mよりも大きく、より好適には3×107S/mよりも大きい導電率を有する。適切な非金属の導電性材料は、限定されるものではないが、炭素またはグラファイトをベースとした材料を含む。
線照射、マイクロ波照射、電子ビーム、ガンマ線照射または他の適切な熱もしくは非熱照射によってもたらされる、ポリマー鎖の架橋によって樹脂マトリックスを硬くすることを言う。
Scientific Publishing、Amsterdam、1990、Chapter7、pp189〜224を参照)によって説明されたグループ寄与法に基づく計算によって決定され得る。
、熱可塑性ポリマーから選択される。一般に、少なくとも150℃のTg、好適には20
0℃を超えるTgを有する、熱可塑性ポリマーが適切である。
−A−Y
ここで、Aは、二価の炭化水素基、好適には芳香族であり、Yは、活性水素をもたらす基、特に、OH、NH2、NHR’またはSHであり、ここで、R’は、8までの炭素原
子を含有する炭化水素基であるか、あるいは他の架橋反応性をもたらすもの、特に、エポキシ、(メタ)クリレート、シアネート、イソシアネート、アセチレン、エチレンビニル、アリル、ベンゾキサジン、無水物、オキサゾリン、マレイミドおよび飽和状態を含有するモノマーである。
本開示の導電性複合粒子は、単一または多数ステップ工程に従って製造され得る。一実施形態では、粒子は、2つのステップ工程によって製造され、そのステップ工程は、ポリマー材料の中に導電性成分を分散させるための最初の高せん断配合ステップを含み、粒子サイズ削減ステップが後に続く。導電性複合粒子を製造するための例示的な方法は、図2に例示される。導電性材料31およびポリマー材料32は、ペレットを形成するために押出機33において配合される。「導電性材料」は1つ以上の導電性材料を含み得、「ポリマー材料」は1つ以上のポリマーを含み得ることが理解されるべきである。そのような実施形態では、ポリマー材料および導電性材料は、好適には、導電性材料およびポリマーの同種の物理的混合物を形成するために、同時にまたは連続的に、押出機の中に供給され得る。押出機の中に導入される出発ポリマー材料32は、非晶相にあり得、または融けた形態にあり得る。
、比表面積(SSA)は、好適には、0.1m2/gよりも高い。適切な金属材料の例は
、低密度の525ニッケル薄片(AD=0.65g/cm3、米国、Novamet S
pecialty Products Corp.から利用可能)、CAP9銀粉末(SSA=3.0m2/g、英国、Johnson Mattheyから利用可能)、FS3
4銀薄片(SSA=1.2m2/g、英国、Johnson Mattheyから利用可
能)およびCH‐L7粒状銅(AD=0.6〜0.7g/cm3、SSA=0.23m2/g、ドイツ、GGP Metalpowder AGから利用可能)である。
用可能)、マイクロメートルの4012合成グラファイト薄片(SSA=1.5m2/g
、米国、Asbury Graphite Mills,Inc.から利用可能)である。被膜生成物の例は、米国、Novamet Specialty Products Corp.からのニッケル被膜グラファイト薄片(AD=1.7g/cm3〜1.9g/
cm3)である。
る。他の方法が、当業者に既知の従来の技法、例えば、機械的混合、音波処理、高せん断混合、ロータ・ステータ混合およびゾルゲル技法などを使用して、ポリマー材料の中に導電性材料を分散させるために使用され得ることが理解されるべきである。
本開示の導電性複合粒子は、繊維強化ポリマー層、例えば、プリプレグプライ間の積層間粒子として使用され得る。そのように、この文脈におけるホスト樹脂系は、繊維強化ポリマー層またはプリプレグプライの樹脂マトリックスである。
ールなどを伴う)ホルムアルデヒド縮合物樹脂、ポリエステル、アクリル、およびそれらの組み合わせを含む。一実施形態では、ホスト樹脂マトリックスは、熱硬化性組成物であり、その組成物において、導電性複合粒子のポリマー成分の少なくとも50%は、樹脂マトリックスの硬化の間に可溶性である。
好適であり、好適には、分子毎に少なくとも2つのアミノ基を有する芳香族アミンであり、また、特に好適には、ジアミノジフェニルスルホンであり、例えば、ここで、アミノ基は、スルホン基に関してメタの位置またはパラの位置にある。特定の例は、3,3’−および4−,4’−ジアミノジフェニルスルホン(DDS)、メチレンジアニリン、ビス(4−アミノ−3,5−ジメチルフェニル)−1,4−ジイソプロピルベンゼン、ビス(4−アミノフェニル)−1,4−ジイソプロピルベンゼン、4,4’メチレンビス−(2,6−ジエチル)−アニリン(LonzaからのMDEA)、4,4’メチレンビス−(3−クロロ、2,6−ジエチル)−アニリン(LonzaからのMCDEA)、4,4’メチレンビス−(2,6−ジイソプロピル)−アニリン(LonzaからのM‐DIPA)、3,5−ジエチルトルエン−2,4/2,6−ジアミン(LonzaからのD‐ETDA80)、4,4’メチレンビス−(2‐イソプロピル−6−メチル)−アニリン(LonzaからのM‐MIPA)、4−クロロフェニル−N,N−ジメチル−尿素(例えば、Monuron)、3,4−ジクロロフェニル−N,N−ジメチル−尿素(例えば、DiuronTM)およびジシアノジアミド(例えば、Pacific Anchor ChemicalからのAmicure TM CG1200)である。
本開示の複合材料は、異なる工程を使用して製造され得る。一般に、導電性複合粒子を複合材料の製造に組み込むための方法は、
(a)複合混合物を形成するためにポリマー材料内に少なくとも1つの導電性材料を分散させることと、
(b)任意選択的に複合混合物を熱処理することと、
(c)複合混合物からマイクロンサイズの導電性複合粒子を形成することと、
(d)任意選択的にマイクロンサイズの導電性複合粒子を熱処理することと、
(e)強化繊維の隣接した層間の少なくとも1つの積層間領域に導電性複合粒子を組み込む複合材料の積み重ねを形成することであって、各複合材料は、少なくとも1つの繊維強化ポリマー層を含み、繊維強化ポリマー層は、硬化性樹脂マトリックスを含浸させた強化繊維から成る、当該形成することと、を含み得る。
断された長さを有するテープ、トウプレグ、またはウェブの形態にあり得る。
本開示の別の態様によれば、上述したような、導電性複合粒子を形成するために使用されるポリマー材料と導電性材料の導電性混合物は、導電性ポリマー繊維、織られていない材料および構造(例えば、スクリム、マット、ウェブ、ベール、フリース、織物、繊維プリフォーム、および同様のもの)を製造するために使用され得る。
て細かいフィラメントを形成するために押し出されたポリマーの流れを急速に弱める。フィラメントは、次いで、高速度の空気によって収集スクリーンの上に吹き飛ばされ、それ故、自己結合された不織ウェブを形成する。あるいは、押し出された、連続的なフィラメントは、断片に細断され得、次いで、不織ウェブを形成するために加熱されたマンドレルの上に散乱させられ、冷却が後に続く。
率および強靭化などの特性を局所的に与えるように強化繊維に対して不均一に存在し得る。そのような非けん縮織物は、樹脂注入に適合した構造繊維プリフォームの中に組み込まれ得る。
本発明の複合材料は、任意の分野における有用性であって、その分野において、それが複合材料/構造に改善された導電率を与えることを要求される、有用性を見い出している。本開示の一実施形態によれば、本開示の複合材料のz方向の導電率は、従来の第三世代の炭素繊維強化材料について測定された値よりも少なくとも1桁大きい。
以下の例では、以下の測定方法を使用した。
硬化された複合材料の導電率は、ブリッジ法において印加した電圧と電流との間の比率として抵抗値を記録するBurster‐Resistomat2316ミリオームメータによって測定した。Kelvinテストプローブは、2つのサンプル表面間に接触をもたらすために使用した。全ての測定は、標準の湿度条件において室温(RT)で4線式測定方法に従って実行した。
粒子サイズ分布は、0.02μmから2000μmまでの範囲で動作するMalvern Mastersizer2000を使用して測定した。
70重量%の最終濃度を達成するために十分な量のフィラメント状ニッケル(Ni)薄片(Novametから利用可能な525ニッケル粉末)は、ツインスクリュー押出機(SumitomoからのSumikaexel5003P)における溶融混合工程によって機能性ポリエーテルスルホン(PES)ポリマー内に分散した。同じPESポリマーの純サンプルは、対照標準として使用した。分散レベルを最適化するための高せん断スクリュープロファイルを使用した。プロファイルは、押出機の胴部においてせん断と圧力による力との間の最適なバランスを作り出すためにカオス的混合部と結合された従来の混合区分を含む。使用した温度プロファイルおよび工程条件は表1に報告される。
実施例1の複合ニッケル/PES微粒子は、英国、Cytec Engineered
Materials Ltdによって供給されたCYCOM(登録商標)977−2−34%−194‐IMS24K一方向テープ(エポキシをベースとしたマトリックスを含浸させた一方向炭素繊維)の表面上への散布工程によって分散させた。粒子荷重は、テープにおける総樹脂体積に基づいて10体積%であった。複数のそのようなテープは、微粒子を隣接したテープ間に位置付けて、一方を別の頂部上にレイアップし、1.5mmの厚さの擬似等方性テストパネルを形成した。パネルは、次いで、オートクレーブにおいて180℃で2時間の硬化周期に従って硬化した。このテストパネルは、「2A」としてラベル付けた。
スとしたマトリックスに溶解され、多層パネルの積層間領域に(導電性粒子として)金属成分を解放する。そのような手法で、局所的な導電性棚部またはブリッジは、隣接した炭素繊維層間に生成した。
実施例2において使用した同じ複合Ni/PES微粒子の2つの異なる荷重(10体積%および20体積%)は、英国、Cytec Engineered MaterialsからのCYCOM(登録商標)977−2−34%−194−IMS24K一方向テープの表面上に別個に分散した。異なる粒子荷重を有する2つのテストパネルは、微粒子がその上に分散されたテープをレイアップすることによって形成した。結果として生じるテストパネルは、熱機械特性上の複合微粒子の効果を決定するために評価した。10%微粒子を含有するテストパネルは「3B」としてラベル付け、20%微粒子を含有するテストパネルは「3C」としてラベル付けた。比較目的のために、複合Ni/PES微粒子を含有しなかった類似のテストパネルを製造し、「参照2」としてラベル付けた。
テストパネルの機械的性能は、表3に示される。
導入は、それぞれ、参照2のパネルと比較してモードIにおける積層剥離成長抵抗において、それぞれ、60%および73%の改善を生み出すように決定した。また、モードII値における積層剥離成長抵抗の同時の10%〜15%の増加を観測した。加えて、複合Ni/PES微粒子の10%の導入は、30J衝撃後の圧縮強度における25%の増加を結果としてもたらした一方、損害範囲を大幅に削減した。
(英国、Johnson Mattheyからの)十分な量の銀(Ag)粉末CAP9は、複合混合物(ポリマー成分+導電性成分)の70重量%の最終Ag濃度を達成するためにツインスクリュー押出機(SumitomoからのSUMIKAEXEL5003P)における溶融混合工程によって、商業的に利用可能な機能性ポリエーテルスルホンポリマー内に分散した。高せん断スクリュープロファイルを使用した。使用した温度プロファイルおよび工程条件は、表1に示される。
代替の導電性複合混合物「5A」は、実施例1に記載したようなツインスクリュー押出機(英国、SumitomoからのSUMIKAEXEL5003P)において、商業的に利用可能な機能性ポリエーテルスルホン(PES)ポリマーの中に商業的に利用可能な粒状銅(Cu)(GGP Metalpowder AGからのCH‐L7)を分散させることによって生成した。複合混合物の全体の重量に基づいて65重量%の銅濃度を得た。
4つの異なるパネル(7A〜7D)は、例5に記載した導電性複合Cu/PES粒子と表7に示される異なる導電性粒子:非導電性粒子の比率における非導電性の熱可塑性(TP)粒子を使用して例2に記載したように製作し硬化した。硬化したパネルのz方向の導電率を測定し、結果を表7に示す。実施例2に開示したような「参照1」パネルは、本明細書において比較のために使用する。
Claims (7)
- 硬化性複合材料であって、
硬化性樹脂マトリックスを含浸させた強化繊維の少なくとも1つの構造層と、
該構造層に隣接し、不規則に配列された導電性ポリマー繊維を含む、不織ベールと、
を含み、
前記導電性ポリマー繊維は導電性の材料およびポリマー材料の混合物から形成され、各導電性ポリマー繊維の前記ポリマー材料は1つ以上のポリマーを含み、該1つ以上のポリマーは、最初に固相であるとともに、前記硬化性樹脂マトリックスの硬化の前に前記硬化性樹脂マトリックスに実質的に不溶性であるが、前記樹脂マトリックスの硬化に際して液相への少なくとも部分的な相転移を経ることができる、硬化性複合材料。 - 樹脂注入に適合した構造プリフォームであって、
樹脂の無い強化繊維の1つ以上の層と、
不規則に配列された導電性ポリマー繊維を含む少なくとも1つの不織ベールと、
を含み、
前記導電性ポリマー繊維は導電性の材料およびポリマー材料の混合物から形成され、各導電性ポリマー繊維の前記ポリマー材料は1つ以上のポリマーを含み、該1つ以上のポリマーは、最初に固相であるとともに、樹脂注入によって前記プリフォームの中に導入されることになる硬化性樹脂組成物に実質的に不溶性であるが、前記樹脂を注入されたプリフォームの硬化周期の間に液相への少なくとも部分的な相転移を経ることができる、構造プリフォーム。 - 複合構造を製作する方法であって、
(a)レイアップを形成するために、硬化性樹脂マトリックスを含浸させた強化繊維の2つ以上の構造層を積み重ねた配列でレイアップすることと、
(b)不規則に配列された導電性ポリマー繊維を含む、少なくとも1つの不織ベールを2つの隣接した構造層間に置くことと、
(c)前記レイアップを硬化することと、
を含み、
前記導電性ポリマー繊維は導電性の材料およびポリマー材料の混合物から形成され、各導電性ポリマー繊維の前記ポリマー材料は1つ以上のポリマーを含み、該1つ以上のポリマーは、最初に固相であるとともに、前記レイアップの硬化前に前記硬化性樹脂マトリックスに実質的に不溶性であり、次いで、硬化の間に、前記ポリマー材料は、前記樹脂マトリックスに溶解することによって液相への少なくとも部分的な相転移を経る、方法。 - 複合構造を製作する方法であって、
(a)(i)乾燥繊維の複数層と、(ii)2つの隣接した繊維層間に置かれた、導電性ポリマー繊維を含む少なくとも1つの不織ベールと、を含む、乾燥繊維プリフォームを形成することと、
(b)硬化性の液体の樹脂組成物を前記乾燥繊維プリフォームに注入することと、
(c)前記樹脂を注入した繊維プリフォームを硬化することと、を含み、
前記導電性ポリマー繊維は導電性の材料およびポリマー材料の混合物から形成され、各導電性ポリマー繊維の前記ポリマー材料は1つ以上のポリマーを含み、該1つ以上のポリマーは、最初に固相であるとともに、注入の間と、前記樹脂を注入した繊維プリフォームの硬化の前とにおいては、前記硬化性の樹脂組成物に実質的に不溶性であり、次いで、硬化の間に前記ポリマー成分は、前記樹脂組成物に溶解することによって液相への少なくとも部分的な相転移を経る、方法。 - 樹脂注入に適合した構造繊維プリフォームであって、
該構造繊維プリフォームは、導電性ポリマー繊維と物理的に結合した強化繊維を含み、
前記導電性ポリマー繊維は導電性の材料およびポリマー材料の混合物から形成され、各導電性ポリマー繊維の前記ポリマー成分は1つ以上のポリマーを含み、該1つ以上のポリマーは、最初に固相であるとともに、樹脂注入の間に前記プリフォームに導入されることになる硬化性樹脂組成物に実質的に不溶性であるが、前記樹脂を注入されたプリフォームの硬化周期の間に液相への少なくとも部分的な相転移を経ることができる、構造繊維プリフォーム。 - 前記繊維の前記物理的結合は、混合させること、繊維の同じ層において整列させること、繊維の異なる層であるが隣接した層に位置決めすることから選択される、請求項5に記載の構造プリフォーム。
- 樹脂注入に適合した構造プリフォームであって、
該構造プリフォームは、複数の織物プライを含み、該複数の織物プライの少なくとも1つは、強化繊維および導電性ポリマー繊維を含み、
前記導電性ポリマー繊維は導電性の材料およびポリマー材料の混合物から形成され、各導電性ポリマー繊維の前記ポリマー成分は1つ以上のポリマーを含み、該1つ以上のポリマーは、最初に固相であるとともに、樹脂注入の間に当該プリフォームに導入されることになる硬化性樹脂組成物に実質的に不溶性であるが、前記樹脂を注入されたプリフォームの硬化周期の間に液相への少なくとも部分的な相転移を経ることができる、構造プリフォーム。
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US10370079B2 (en) | 2019-08-06 |
US20180029686A1 (en) | 2018-02-01 |
KR20200101468A (ko) | 2020-08-27 |
US10507900B2 (en) | 2019-12-17 |
RU2014146307A (ru) | 2016-06-10 |
TW201343735A (zh) | 2013-11-01 |
WO2014011293A2 (en) | 2014-01-16 |
KR102251006B1 (ko) | 2021-05-13 |
EP2838702B1 (en) | 2020-06-10 |
TWI567118B (zh) | 2017-01-21 |
CN104334327B (zh) | 2016-10-12 |
CA2870921A1 (en) | 2014-01-16 |
GB201206885D0 (en) | 2012-06-06 |
BR112014025708B1 (pt) | 2021-07-20 |
MX2014012265A (es) | 2015-03-09 |
US20160107739A1 (en) | 2016-04-21 |
JP2015518436A (ja) | 2015-07-02 |
CA2870921C (en) | 2021-05-18 |
EP2838702A2 (en) | 2015-02-25 |
RU2631299C2 (ru) | 2017-09-20 |
KR102146500B1 (ko) | 2020-08-21 |
AU2017204658B2 (en) | 2018-11-08 |
JP2018039273A (ja) | 2018-03-15 |
JP6259446B2 (ja) | 2018-01-10 |
AU2013289104B2 (en) | 2017-07-06 |
AU2013289104A1 (en) | 2014-10-02 |
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