JP2020514128A - 構造能力及び難燃性能を有する複合材料 - Google Patents
構造能力及び難燃性能を有する複合材料 Download PDFInfo
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- JP2020514128A JP2020514128A JP2019548640A JP2019548640A JP2020514128A JP 2020514128 A JP2020514128 A JP 2020514128A JP 2019548640 A JP2019548640 A JP 2019548640A JP 2019548640 A JP2019548640 A JP 2019548640A JP 2020514128 A JP2020514128 A JP 2020514128A
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Abstract
Description
a)硬化性樹脂を含浸させた又は硬化性樹脂中に埋め込まれた強化繊維の少なくとも2つの層と;
b)強化繊維の隣接層間の層間領域と;
c)層間領域におけるポリマー強靱化粒子(P1)と不溶性の難燃性粒子(P2)との組み合わせと
を含む複合材料を指向する。
強化繊維に含浸させる/注入するための硬化性樹脂(又は樹脂組成物)は好ましくは、1つ若しくは複数の未硬化の熱硬化性樹脂を含有する硬化性又は熱硬化性樹脂であり、それらには、エポキシ樹脂、(例えばポリイミド又はビスマレイミドなどの)イミド、ビニルエステル樹脂、シアネートエステル樹脂、イソシアネート変性エポキシ樹脂、フェノール樹脂、フラン樹脂、ベンゾオキサジン、(例えば尿素、メラミン又はフェノールなどの)ホルムアルデヒド縮合物樹脂、ポリエステル、アクリル系樹脂、それらのハイブリッド、ブレンド及び組み合わせが含まれるが、それらに限定されない。
高性能複合材料及びプリプレグを製造するために、好適な強化繊維は、高い引張強さ、好ましくはASTM C1557−14に従って測定されるときに500ksi(すなわち3447MPa)超の引張強さを有する。この目的のために有用である繊維には、炭素繊維又は黒鉛繊維、ガラス繊維及び炭化ケイ素、アルミナ、ホウ素、石英等で形成された繊維、並びに例えばポリオレフィン、ポリ(ベンゾチアゾール)、ポリ(ベンズイミダゾール)、ポリアリレート、ポリ(ベンゾオキサゾール)、芳香族ポリアミド、ポリアリールエーテル等の有機ポリマーから形成された繊維が含まれ、2つ若しくはそれ以上のそのような繊維を有する混合物が含まれてもよい。好ましくは、繊維は、ガラス繊維、炭素繊維、及び商品名KEVLARでDuPont Companyによって販売される繊維などの、芳香族ポリアミド繊維から選択される。強化繊維は、複数のフィラメントでできた不連続又は連続トウの形態で、連続一方向若しくは多方向テープとして、又は織布、不捲縮布、若しくは不織布として使用されてもよい。織形態は、平織、繻子織、又は綾織スタイルから選択されてもよい。不捲縮布は、多数の層及び繊維配向を有してもよい。
一実施形態によれば、特定量のポリマー強靱化粒子及び燃性粒子が、強化繊維の含浸の前に(すなわち、プリプレグ製造の前に)樹脂組成物と混合される。プリプレグ層を製造するために、樹脂フィルムが、先ず粒子含有樹脂組成物を剥離紙上へコートすることによって製造される。次に、そのような樹脂フィルムの1つ若しくは2つが、繊維に含浸させるために熱及び圧力の助けの下で強化繊維の層の一面若しくは両面上へ積層され、それによって単位面積当たりの繊維の特定の重量の繊維強化ポリマー層(又はプリプレグ層)を形成する。積層プロセス中に、粒子のサイズが繊維フィラメント間の間隔よりも大きいという事実のために、粒子は濾去され、繊維層の外側にとどまる。結果として生じるプリプレグ層は、粒子がその中に埋め込まれている母材樹脂の1つ若しくは2つの層に隣接した構造的繊維強化層を含有する。その後、その中に強靱化粒子を含有する2つ若しくはそれ以上のプリプレグ層がレイアッププロセスによって他の層のトップ上に積層されたものである場合、粒子は、2つの隣接層間の層間領域に配置される。この実施形態において、(粒子なしの)層間領域での母材樹脂は、強化繊維に含浸させる樹脂と同じものである。
本明細書に開示される複合材料は、隠れエリアで良好な溶け落ち防護能力及び低い火炎伝播を有する航空機構造物を製造するのに好適であるプリプレグの形態にあってもよい。例えば、複合プリプレグは、一次及び二次航空機構造物、立体及び弾道構造物を製造するために使用されてもよい。そのような構造部材には、複合胴体及び翼構造物が含まれる。とりわけ、複合プリプレグは、燃焼性要件を満たす必要があろう耐荷重性又は耐衝撃性構造物の製造に特に好適である。本明細書に開示されるプリプレグはまた、航空、船舶、自動車、及び鉄道などの、他の輸送機関用途向けの構成部品の製造にも適用できる。
燃焼性は、あるものがどの程度容易に燃えて又は着火して、火災又は燃焼を引き起こすかである。燃焼性試験FAR 25.853又はCS25 App.F Part−I(a)(1)(i)は、火炎の作用に供された材料が燃えるかどうかを評価するために用いられる簡単な試験である。
エポキシ樹脂/炭素繊維クーポンについて、aにおいて発生した煙の毒性は、BSS 7239に従って測定した。
試験は、火炎温度を用いて較正された熱源としてプロパンバーナーを使用して40cm×40cmフラットパネルに関して実施した。衝突後火災をシミュレートするために、パネル表面での熱フラックスを、約1160℃の火炎温度で182kW/m2に固定した。層状熱電対(タイプN)を、試験中に火炎温度をモニタするために「高温面」でパネルの近くに配置した。3つの熱電対タイプKを使用してパネルと直接に接触している「低温面」の温度分布をモニタした。追加の熱電対及び熱フラックス(HF)検出器をまた、パネルから30.48cmすなわち12インチの距離にそれぞれ配置して試験中にパネル上方の高温ガスの温度及び熱フラックスをモニタした。2つのビデオカメラを使用してパネルを通しての火侵入を検出し、試験中のパネル反応を評価した。「高温面」(火暴露面)及び「低温面」での温度をモニタしながら、溶け落ち試験を5分間行った。図2は、この試験のためのセットアップを例示する。
5=パネルは激しく損傷を受けた:目に見える乾燥繊維の60%超のパネルの低温面
4=パネルはひどく損傷を受けた:目に見える乾燥繊維の40〜60%の低温面
3=パネルは損傷を受けた:目に見える乾燥繊維の20〜40%の低温面側
2=パネルはわずかに損傷を受けた:目に見える乾燥繊維の10〜20%の低温面
1=パネルはほとんど損傷を受けなかった:目に見える乾燥繊維のゼロ又は10%未満の低温面
30ジュール衝撃後の衝撃後圧縮(CAI)を、24層準等方性ラミネートを使用して測定した。測定は、EN 2565方法Bに従って調製され、180℃で2時間硬化させられた、欠陥を含まないパネルから摘出されたクーポンに関して室温で行った。検体を機械加工し、衝撃を与え、ASTM D7136/37に従って試験した。
プリプレグ製造
5つの樹脂組成物を表1に示される処方に従って調製した。樹脂組成物対照1.0は、いかなる粒子も含有しない。他の樹脂組成物のそれぞれは、ポリマー強靱化粒子と難燃性粒子との異なる組み合わせで変性した。成分の量は、重量比(w/w)百分率で報告する。
Araldite PY 306は、Huntsmanから入手可能なビスフェノールFジグリシジルエーテル樹脂である。
Araldite MY 0510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る。
SUMIKAEXCEL 5003Pは、住友化学から入手可能なポリエーテルスルホンポリマーである。
Exolit(登録商標)AP 462(粒子a)は、Clariantによって商業化された20ミクロンの平均粒径のメラミン系コーティング付きのアンモニウムポリホスフェート粒子である。
Vestosint(登録商標)Z2649(粒子b)は、Evonikから入手可能な脂肪族ナイロン粒子である。
16層、[+,0,−,90]2sに等しいレイアップ及び約3.2mmの厚さの対照パネル2.0を製造するために、粒子を有しない対照プリプレグ1.0を使用した。複数のプリプレグ1.1、1.3及び1.4を使用して、それぞれ、表3の複合パネル2.1、2.2及び2.3を調製した。これらのパネルは、プリプレグをレイアップして準等方性形態[+,0,−,90]2sのレイアップ(各レイアップは約3.2mm厚さである)を形成すること、引き続く177℃で及び6バール圧力で2時間のオートクレーブ中での圧密及び硬化によって製造した。粒子含有プリプレグを、前記粒子がレイアップの間紙領域にとどまるようにレイアップした。全ての硬化パネルを60秒垂直燃焼及び毒性試験に供した。燃焼性試験及び毒性試験結果を表3に報告する。
40cm×40cmの寸法を有する対照パネル2.4を製造するために、複数の対照プリプレグ1.0を使用した。パネル2.5及び2.6を、それぞれ、複数のプリプレグ1.2及びプリプレグ1.4から製造した。これらのパネルは、プリプレグをレイアップして準等方性形態[+,−,0,90]sのレイアップ(各レイアップは約1.6mm厚さである)を形成すること、引き続く177℃で及び6バール圧力で2時間のオートクレーブ中での圧密及び硬化によって製造した。全ての硬化パネルを溶け落ち試験に供し、結果を表4に報告する。
[+,0,−,90]3s形態に従った、24層の対照パネルをレイアップすること、引き続く177℃で及び6バール圧力で2時間のオートクレーブ中での圧密及び硬化によって、対照パネル2.7を製造した。パネル2.8及び2.9を、それぞれ、複数のプリプレグ1.2及びプリプレグ1.4から製造した。欠陥を含まないクーポンを、パネルから摘出し、CAI試験に供した。パネルの詳細及び機械的試験結果を表5に報告する。
プリプレグ製造
表6に示される処方に従って樹脂組成物を調製した。いかなる粒子も含有しなかった、樹脂組成物対照1.0は、対照と見なされる。様々な樹脂組成物は、ポリマー強靱化粒子と難燃性粒子との異なる組み合わせを含有した。量は、重量比(w/w)百分率で報告する。
複数のプリプレグ3.1、3.2及び3.3を使用して、表8に開示される複合パネル4.1、4,2及び4.3をそれぞれ調製した。パネル製造及びクーポン試験は、実施例1に記載された手順と同様であった。試験結果を表8に報告する。比較のために、層間粒子を有していなかった対照パネル2.0に関して生じた結果を表8にまた報告する。
複数のプリプレグ3.1及び3.3を使用して、表9に開示される複合パネル4.4及び4.5をそれぞれ調製した。パネル製造及び試験は、実施例1に記載された手順と同様であった。試験結果を表9に報告する。比較のために、AP462粒子のみを有する比較パネル2.5に関して生じた結果を表9にまた報告する。
複数のプリプレグ3.3を使用して、それぞれ、CAI及びGIc試験用の複合パネル4.6及び4.7を調製した。パネルの詳細及び機械的試験結果を表10に報告する。比較のために、層間粒子を有しない対照パネル2.7についての結果をまた報告する。
プリプレグ製造
表12に示される処方に従って2つの樹脂組成物を調製した。いかなる粒子も含有しない、樹脂組成物対照1.0は、対照と見なされる。様々な樹脂組成物は、ポリマー強靱化粒子と難燃性粒子との異なる組み合わせを含有した。量は、重量比(w/w)百分率で報告する。
複数のプリプレグ5.1及び5.2を使用して、表14に開示される複合パネル6.1及び6.2を、それぞれ、調製した。パネル製造及びクーポン試験は、実施例1に記載された手順と同様であった。試験結果を表14に報告する。比較のために、層間粒子を有しない、対照パネル2.0に関して生じた結果を表14にまた報告する。
複数のプリプレグ5.1及び5.2を使用して、表15に開示される複合パネル6.3及び6.4を、それぞれ、調製した。パネル製造及び試験は、実施例1に記載された手順と同様であった。試験結果を表15に報告する。比較のために、AP462粒子のみを有する比較パネル2.5に関して生じた結果を表15にまた報告する。
パネル6.5及び6.6を、実施例1及び2に記載された手順と同様のCAI及びGIc試験用にプリプレグ5.2を使用して製造した。層間粒子を有しない対照パネル2.7及び2.11に関する結果と比較して機械的結果を表16に報告する。
プリプレグ製造
表18に示される処方に従って樹脂組成物7.1を調製した。いかなる粒子も含有しなかった、樹脂組成物対照1.0は、対照と見なされる。量は、重量比(w/w)百分率で報告する。NT1−15G(粒子e)は、15%w/wの合成黒鉛を含有するEvonik製の導電性ポリイミド粒子である。
前の実施例についてのように一方向炭素繊維IMS65 E23 24Kに含浸させるために樹脂7.1を使用し、約190gsmの単位面積当たりの繊維の重量及び約36重量%の樹脂含有量のプリプレグ7.1をもたらした。
パネル8.2及び8.3を、前に記載された手順と同様のCAI及びGIc試験用にプリプレグ7.1を使用して製造した。層間粒子を有しない対照パネル2.7及び2.11に関する結果と比較して機械的結果を表20に報告する。
プリプレグ製造
表22に示される処方に従って、樹脂組成物9.1及び9.2を調製した。量は、重量比(w/w)百分率で報告する。Amgard PA1(Solvay製)を、窒素及びリン含有難燃性粒子として使用した。SEN6065は、255〜285g/eqのエポキシ当量及び7.3%のリン含有量の、Shin−Aから商業的に入手可能なリン変性エポキシである。リン変性エポキシの使用は、改善された難燃性特性を付与することを意図した。
複数のプリプレグ9.1及び9.2を使用して、表24に開示される複合パネル10.1及び10.2を、それぞれ、調製した。パネル製造及びクーポン試験は、実施例1に記載された手順と同様であった。試験結果を表24に報告する。比較のために、層間粒子を全く持たなかった、対照パネル2.0に関して生じた結果を表24にまた報告する。
パネル10.3〜10.6を、前に記載された手順と同様のCAI及びGIc試験のためにプリプレグ9.1及び9.2を使用して製造した。いかなる層間粒子も持たなかった、対照パネル2.7及び2.11についての結果と比較して機械的結果を表25に報告する。
本開示において、量に関連して用いられる修飾語「およそ」及び「約」は、表記の値を含み、文脈によって決められる意味を有する(例えば、特定の量の測定に関連した誤差の程度を包含する)。例えば、「約」に続く数は、その列挙される数のプラスマイナス0.1%〜1%の列挙される数を意味することができる。接尾語「(s)」は、本明細書で用いるところでは、それが修飾する用語の単数形及び複数形の両方を包含し、それによってその用語の1つ若しくは複数を包含する(例えば、金属(metal(s))は、1つ若しくは複数の金属を包含する)ことを意図する。本明細書に開示される範囲は、端点及びその範囲の全ての中間値を含み、例えば、「1%〜10%」は、1%、1.5%、2%、2.5%、3%、3.5%等を包含する。
Claims (20)
- 複合材料であって、
硬化性樹脂を含浸させた強化繊維の少なくとも2つの層と;
強化繊維の隣接層の間に形成された層間領域と;
前記層間領域におけるポリマー強靱化粒子(P1)と難燃性粒子(P2)との組み合わせと
を含む複合材料。 - ポリマー強靱化粒子対難燃性粒子の重量比(P1:P2)が1:3〜2:1の範囲にある、請求項1に記載の複合材料。
- 強化繊維の隣接層の間に形成された前記層間領域が全樹脂含有量の5%〜40%の範囲の総重量を有する、請求項1又は2に記載の複合材料。
- 前記難燃性粒子が、前記粒子が火又は200℃よりも上の温度に曝されたときに膨張するという点において熱膨張性である、請求項1〜3のいずれか一項に記載の複合材料。
- 前記ポリマー強靱化粒子が、熱可塑性ポリマー又は架橋熱可塑性ポリマーの粒子である、請求項1〜4のいずれか一項に記載の複合材料。
- 前記ポリマー強靱化粒子が、ポリアミド、芳香族ポリイミド、及び架橋PES−PEES、ポリイミドと黒鉛とのブレンドの少なくとも1つを含む、請求項1〜5のいずれか一項に記載の複合材料。
- 前記難燃性粒子が少なくとも1つのリン化合物を含む、請求項1〜6のいずれか一項に記載の複合材料。
- 前記難燃性粒子が窒素及びリン化合物を含む、請求項7に記載の複合材料。
- 前記難燃性粒子がメラミンをさらに含む、請求項7又は8に記載の複合材料。
- 前記難燃性粒子が、アンモニウムポリホスフェート、メラミンシアヌレート、メラミンホスフェート、メラミンポリホスフェート、及びメラミンポリ(金属ホスフェート)の少なくとも1つを含む、請求項1〜6のいずれか一項に記載の複合材料。
- 前記難燃性粒子が、メラミン又はメラミン含有樹脂内に封入されたアンモニウムポリホスフェートを含む、請求項1〜10のいずれか一項に記載の複合材料。
- 前記層間領域が硬化性樹脂を含み、前記ポリマー強靱化粒子が、前記複合材料の硬化中に前記層間領域で前記硬化性樹脂に不溶性であり、硬化後にばらばらの粒子としてとどまる、請求項1〜11のいずれか一項に記載の複合材料。
- 前記層間領域が硬化性樹脂を含み、前記ポリマー強靱化粒子が、前記複合材料の硬化中に前記層間領域で前記硬化性樹脂に可溶性である、請求項1〜10のいずれか一項に記載の複合材料。
- 前記ポリマー強靱化粒子が、5〜50ミクロン(μm)の範囲の平均粒径(d50)を有する、請求項1〜13のいずれか一項に記載の複合材料。
- 前記層間領域における前記硬化性樹脂が、前記強化繊維に含浸させる前記硬化性樹脂の組成と同じ組成を有する、請求項1〜14のいずれか一項に記載の複合材料。
- 前記硬化性樹脂が1つ若しくは複数のエポキシ樹脂を含む、請求項1〜15のいずれか一項に記載の複合材料。
- 前記硬化性樹脂が、二官能性、三官能性及び四官能性エポキシ樹脂から選択される少なくとも2つの多官能性エポキシ樹脂と、前記エポキシ樹脂と均質の混合物を形成することができる熱可塑性ポリマーとの組み合わせを含む、請求項1〜16のいずれか一項に記載の複合材料。
- 前記熱可塑性ポリマーが、PES、PEES、PES−PEESコポリマー、及びフェノキシから選択される、請求項17に記載の複合材料。
- 前記硬化性樹脂が、多官能性エポキシ樹脂又はフェノール樹脂を有機ホスフィン酸又はそれの酸無水物と反応させることによって得られるリン変性エポキシ樹脂又はフェノール樹脂を含む、請求項1〜18のいずれか一項に記載の複合材料。
- 前記硬化性樹脂が、多官能性エポキシ樹脂をDOPOと反応させることによって調製されるDOPO(すなわち9,10−ジヒドロ−9−オキサ−10−ホスファフェナントレン10−オキシド)の誘導体を含む、請求項1〜18のいずれか一項に記載の複合材料。
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