JP6987761B2 - 複合構造物のための表面材 - Google Patents
複合構造物のための表面材 Download PDFInfo
- Publication number
- JP6987761B2 JP6987761B2 JP2018527872A JP2018527872A JP6987761B2 JP 6987761 B2 JP6987761 B2 JP 6987761B2 JP 2018527872 A JP2018527872 A JP 2018527872A JP 2018527872 A JP2018527872 A JP 2018527872A JP 6987761 B2 JP6987761 B2 JP 6987761B2
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- Prior art keywords
- layer
- electrically conductive
- surface material
- fibers
- conductive surface
- 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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- 239000010949 copper Substances 0.000 claims description 18
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Landscapes
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- Glass Compositions (AREA)
Description
一実施形態において、補剛層は、流体バリアとして役立つこともできる連続した非多孔質熱可塑性層であり、複合構造物の損傷許容性を改良することができる。熱可塑性層は、特に、自動配置のために表面材が連続したまたは細長いテープの形態であるとき、約50μm〜約153μm(または約2〜約6ミル)の厚さを有してもよい。しかし、表面材の用途に応じて、より大きな厚さが可能である。この実施形態において、熱可塑性層は一切の強化繊維を含有せず、統合表面材はまた、炭素繊維などの強化繊維の一切の付加的な層を含有しない。
別の実施形態において、表面材は、図1に示される構成要素を含み、そこで補剛層12は、ガラス熱硬化樹脂を含有する硬化性組成物で被覆または注入されている織布または不織布ベールから構成される。
[式中、
n=1〜3]。
商業的に入手可能なDPCD系エポキシノボラックの例には、Huntsman製のTactix(登録商標)556、およびTactix(登録商標)756が含まれる。
図2によって表されるさらに別の実施形態において、統合表面材は、硬化性樹脂層22に埋め込まれた多孔質導電層21と、外側の織布または不織布ベール23(以下、「繊維層」)と、外側の不織布層24とを含む表面材である。繊維層23および不織布層24の外面は、実質的にまたは完全に不粘着性である。そして硬化性樹脂22は、繊維層23も不織布層24もどちらの厚さにわたっても浸透しない。この表面材が複合基材上に置かれるとき、繊維層23は剛性を提供するために複合基材と接触しており、不織布層24は複合部品の最も外側の層になる。多孔質導電層21は、図1を参照して前述した通りである。一実施形態において、多孔質導電層は金属スクリーンである。織布または不織布ベール23は、他の実施形態について前述した通りである。不織布層24は、図1において不織布層14を参照して前述した通りである。一実施形態において、層23および24は、同一であるかまたは異なった面積重量を有する不織布ベールである。層23および24が異なった面積重量を有する不織布ベールであるとき、大きいほうの面積重量を有する不織布ベールは、複合基材と接触しており、小さいほうの面積重量を有する不織布ベールは、表面材が適用された後に最終複合部品内の最も外側の層である。この表面材は、前述した通りATLまたはAFPなどの自動配置のための細い幅のテープの形態であってもよい。
本開示の別の態様は、複合構造物内の外側の流体バリアとして機能する表面材に関する。このような流体バリアは、多孔質コアを含有する複合サンドイッチパネルのために特に有用である。複合サンドイッチパネルは典型的に、オートクレーブ処理によって接着剤でコアに同時硬化された複合表皮を有する。コア材料は、軽量ハニカム、硬質フォーム、紙または木材などの様々な形態をとってもよい。好ましくは、コアはハニカム材料であるが、これは材料の非常に低い重量のためにすぐれた構造特性を提供するからである。複合サンドイッチパネルは、高い剛性対重量および強度対重量比のために、航空宇宙用構造部材において広範囲にわたる用途がある。
本明細書中で用いられるとき用語「硬化する(cure)」および「硬化(curing)」は、高温での加熱、紫外線および放射線暴露、または化学添加剤によって引き起こされるプレポリマー物質または樹脂先駆物質の不可逆的な固化を意味する。用語「硬化性(curable)」は、固化材料に硬化され得ることを意味する。本明細書中で用いられるとき「部分的に硬化された」は、100%未満の硬化度を意味する。
[式中、n=0〜5、およびR=HまたはCH3]を有するフェノールホルムアルデヒドノボラックまたはクレゾール−ホルムアルデヒドノボラックのポリグリシジル誘導体であるエポキシノボラック樹脂である。R=Hであるとき、樹脂はフェノールノボラック樹脂である。R=CH3であるとき、樹脂はクレゾールノボラック樹脂である。前者は、Dow Chemical Co製のDEN428、DEN431、DEN438、DEN439、およびDEN485として商業的に入手可能である。後者は、Ciba−Geigy Corp製のECN1235、ECN1273、およびECN1299として商業的に入手可能である。使用されてもよい他の適したノボラックには、Celanese Polymer Specialty Co製のSU−8が含まれる。好ましい実施形態において、エポキシノボラック樹脂は、25℃において4000〜10,000mPa・sの粘度およびASTM D−1652によって測定される時に約190g/eq〜約235g/eqのエポキシド当量(EEW)を有する。
を有するメチレンジアニリンのテトラグリシジルエーテルである。構造物中のアミン基は、芳香環構造のパラ−または4,4’位置に示されるが、しかしながら、2,1’、2,3’、2,4’、3,3’、3,4’などの他の異性体が可能な代替形であることは理解されるはずである。商業的に入手可能な四官能性エポキシ樹脂の例は、Huntsman Advanced Materialsによって供給されるAraldite(登録商標)MY9663、MY9634、MY9655、MY−721、MY−720、MY−725である。
熱硬化性組成物は、1つまたは複数のポリマー強化剤をさらに含有してもよい。ポリマー強化剤は、熱可塑性ポリマー、エラストマー、コア−シェルゴム粒子の他、エポキシ樹脂と、ビスフェノールと、弾性ポリマーとの反応生成物である予備反応付加物、およびそれらの組合せからなる群から選択されてもよい。いくつかの実施形態において、この群からの2つの異なった強化剤の組合せが使用される。強化剤の量は、合計で、組成物の全重量に基づいて約1%〜約30%、いくつかの場合、約10重量%〜約20重量%であってもよい。予備反応付加物に関して、適したエポキシ樹脂には、ビスフェノールAのジグリシジルエーテル、テトラブロモビスフェノールAのジグリシジルエーテル、ビスフェノールAの水素化ジグリシジルエーテル、またはビスフェノールFの水素化ジグリシジルエーテルが含まれる。脂環式エポキシもまた適しており、それらには、1分子中に少なくとも1つの脂環式基および少なくとも2つのオキシラン環を含有する化合物が含まれる。特定の例には、脂環式アルコールのジエポキシド、以下の構造によって表される水素化ビスフェノールAが含まれる:
多官能性エポキシド樹脂は様々なアミン系潜硬化剤によって硬化されてもよく、それらは高温(例えば150°F(65℃)を超える温度)で活性化される。適した硬化剤の例には、ジシアンジアミド(DICY)、グアナミン、グアニジン、アミノグアニジン、およびそれらの誘導体が含まれる。イミダゾールおよびアミン錯体のクラスの化合物もまた、使用されてもよい。実施形態において、硬化剤はジシアンジアミドである。アミン系硬化剤は、樹脂フィルム組成物の全重量に基づいて約1重量%〜約5重量%の範囲内の量において存在している。
セラミック微小球を熱硬化性組成物に添加して、それから形成された樹脂フィルムの表面平滑性を改良してもよい。それらは中空または固体セラミック微小球であってもよい。一実施形態において、不活性シリカ−アルミナセラミック材料から製造された中空セラミック微小球が使用される。セラミック微小球は、60,000psi超の圧砕強さ、約3.7〜4.6の誘電率、1000〜1100℃(または1832〜2012°F)の範囲の軟化点、および0.1ミクロン〜50ミクロン、または1〜50ミクロンの範囲の粒径を有してもよい。セラミック微小球の高い軟化点は、それらを溶媒に対して非吸収性、難燃性、および高度に耐薬品性であるようにできる。約0.1μm〜約20μm、好ましくは約1μm〜約15μmの範囲の直径を有する微小球は、特に適していることがわかった。本樹脂フィルム組成物において使用するために特に適している商業的に入手可能なセラミック微小球の例は、商品名Zeeospheres(登録商標)の、例えば、G−200、G210およびW−200としてZeelan Industries,Inc.によって販売されている。これらは、厚壁を有し、無臭、および明るい灰色の中空シリカ−アルミナ球である。好ましい実施形態において、多官能性樹脂とセラミック微小球との組合せは、樹脂フィルム組成物の50重量%超、好ましくは60重量%超を構成する。特定の実施形態において、セラミック微小球の量は、樹脂フィルム組成物の全重量に基づいて少なくとも20重量%である。いくつかの実施形態において、セラミック微小球の量は、熱硬化性組成物の全重量に基づいて約20重量%〜約40重量%、または約25重量%〜約35重量%の範囲内であってもよい。他の実施形態において、セラミック微小球の量は、約3重量%〜約15重量%、または約5重量%〜約10重量%の範囲内であってもよい。
粒状形態(例えば粉末)の無機充填剤をレオロジー改質成分として熱硬化性組成物に添加して樹脂組成物の流れを制御し、そこでの凝集を防ぐ。樹脂フィルム組成物において使用されてもよい適した無機充填剤には、タルク、マイカ、炭酸カルシウム、アルミナ、およびヒュームドシリカが含まれる。一実施形態において、疎水性ヒュームドシリカ(例えばCab−O−Sil TS−720)が無機充填剤として使用される。無機充填剤の量は、熱硬化性組成物の全重量に基づいて約1重量%〜約5重量%の範囲内であってもよい。
熱硬化性組成物は、硬化または未硬化樹脂フィルムの機械的、電気的、光学的、および熱的性質の1つまたは複数に影響を与える1つまたは複数の任意選択の添加剤をさらに含有してもよい。このような添加剤には、限定されないが、紫外線(UV)安定剤、顔料/染料、および導電材料が含まれる。このような添加剤が使用されるとき、それらの全量は、熱硬化性組成物の全重量に基づいて約5重量%未満である。
本明細書に開示される表面材を繊維強化ポリマー複合基材上に適用し、150°F(65℃)を超える温度、より詳しくは、200°F〜365°F(または93℃〜185℃)の範囲内の温度でそれと同時硬化することができる。繊維強化ポリマー複合基材は、硬化性母材樹脂で含浸または注入された強化繊維から構成される。いくつかの実施形態において、複合基材は、プリプレグプライまたはプリプレグレイアップであってもよい。プリプレグレイアップは、積み重ね順序において配列された複数のプリプレグプライから構成される。各々のプリプレグプライは、母材樹脂、例えばエポキシ樹脂で含浸/注入された布または方向性をもって整列された連続した繊維の形態の強化繊維から構成される。方向性をもって整列された繊維は、一方向または複数方向繊維であってもよい。一般的には、硬化性導電性表面材を繊維強化ポリマー複合基材上に適用して、それは未硬化または部分的に硬化した状態であり、その後に同時硬化して、最も外側の層としてそれに接着された固化表面フィルムを有する完全に硬化した複合構造物を形成してもよい。
ペレット化された形態のPEKKをシングルクルー押出機に供給し、それは、PEKKペレットが押出機バレルを通って移動する時にそれらを溶融するために必要とされる温度に加熱された。押出機を出る溶融材料はダイに入ってPEKKフィルムを形成し、それをその後冷却した。
被覆樹脂溶液は以下の調合に従って調製された:
固体エポキシ付加物(DER 661)、ジェットミル粉砕された:100g
MEK溶媒:50g
DICY:15g
ヒュームドシリカ(Cabosil TS 720):5g
熱および圧力を適用することによって銅スクリーン(175gsm)が硬化性SM905表面フィルム(90gsm)中に埋め込まれた。17gsmの面積重量を有する不織布ガラスベール(Technical Fibre Products製のOptiveil(登録商標))を熱および圧力の適用によってスクリーン含有樹脂層の一方の面に積層して、ガラスベールを樹脂層に接着したが、表面層の樹脂はガラスベールの厚さにわたって浸透せず、そして次に、10gsmのガラスベール(Technical Fibre Products製のOptiveil(登録商標))を樹脂層の反対側の面に同様に接着した。得られた積層体を6.35mm(または0.25インチ)の幅を有する細いストリップにスリットした。表面テープが複合基材上に適用された後に10gsmのガラスベールは最も外側の表面層であり、17gsmのガラスベールは複合基材と接触している。
熱および圧力を適用することによって銅スクリーン(175gsm)が硬化性SM905表面フィルム(90gsm)中に埋め込まれた。8gsmの面積重量を有する不織布ガラスベール(Technical Fibre Products製のOptiveil(登録商標))を熱および圧力の適用によってスクリーン含有樹脂層の一方の面に積層して、ベールを樹脂層に接着したが、表面層の樹脂はベールの厚さにわたって浸透せず、そして次に、別の8gsmの炭素ベール(Technical Fibre Products製のOptiveil(登録商標))を樹脂層の反対側の面に同様に接着した。得られた積層体を6.35mm(または0.25インチ)の幅を有する細いストリップにスリットした。表面テープが複合基材上に適用された後に炭素ベールの1つが最も外側の表面層であり、他方は複合基材と接触している。
熱および圧力を適用することによって銅スクリーン(175gsm)が硬化性SM905表面フィルム(90gsm)中に埋め込まれた。12gsmの面積重量を有する銅被覆炭素ベール(すなわち、不織布銅被覆炭素繊維)(Technical Fibre Products製のOptiveil(登録商標))を熱および圧力の適用によってスクリーン含有樹脂層の一方の面に積層して、ベールを樹脂層に接着したが、表面層の樹脂はベールの厚さにわたって浸透せず、そして次に、12gsmの面積重量を有する別の銅被覆炭素ベール(Technical Fibre Products製のOptiveil(登録商標))を樹脂層の反対側の面に同様に接着した。得られた積層体を6.35mm(または0.25インチ)の幅を有する細いストリップにスリットした。表面テープが複合基材上に適用された後に銅被覆炭素ベールの1つが最も外側の表面層であり、他方は複合基材と接触している。
本開示において、量に関連して使用される修飾語「およそ」および「約」は、表記値を含めており、文脈によって要求される意味を有する(例えば、特定の量の測定に伴なう誤差の程度を含める)。例えば、「約」の後の数は、その記載数のプラスマイナス0.1%〜1%の記載数を意味することができる。本明細書中で用いられるとき接尾語「(s)」は、それが修飾する語の単数形と複数形の両方を包含することを意図し、それによってその用語の1つまたは複数を包含する(例えば、金属(metal(s))は、1つまたは複数の金属を包含する)。本明細書に開示された範囲は端点およびその範囲の全ての中間値を含めており、例えば、「1%〜10%」は、1%、1.5%、2%、2.5%、3%、3.5%等を包含する。
Claims (20)
- (a)補剛層と、
(b)1つまたは複数の熱硬化樹脂と硬化剤とを含む硬化性樹脂層と、
(c)前記補剛層と前記硬化性樹脂層との間の導電層と、
(d)前記硬化性樹脂層に積層された不織布層
とを含む、統合電気導電性表面材であって、
前記補剛層(a)および前記不織布層(d)が最も外側の層であり、前記最も外側の層の露出面が室温(20℃〜25℃)において実質的に不粘着性であり、
前記補剛層が非多孔質熱可塑性層であり、前記非多孔質熱可塑性層が、1つまたは複数のポリアリールエーテルケトン(PAEK)ポリマーを含む、統合電気導電性表面材。 - 前記PAEKポリマーが、ポリ(エーテルケトン)(「PEK」)、ポリ(エーテルエーテルケトン)(「PEEK」)、ポリ(エーテルケトンケトン)(「PEKK」)、ポリ(エーテルケトンエーテルケトンケトン)(「PEKEKK」)、ポリ(エーテルエーテルケトンエーテルエーテルケトン)(「PEEKEEK」)、ポリ(エーテルジフェニルケトン)(「PEDK」)、ポリ(エーテルジフェニルエーテルケトン)(「PEDEK」)、ポリ(エーテルジフェニルエーテルケトンケトン)(「PEDEKK」)、およびポリ(エーテルケトンエーテルナフタレン)(「PEKEN」)からなる群から選択される、請求項1に記載の電気導電性表面材。
- 前記非多孔質熱可塑性層が、以下の性質:
ASTM D−882によって測定された時に640MPa(または93ksi)〜2.1GPa(または305ksi)の引張弾性率、ASTM D−882によって測定された時に27MPa(または4ksi)〜76MPa(または11ksi)の降伏点引張強さ、ASTM D−882によって測定された時に41MPa(または5.9ksi)〜110MPa(または16ksi)の破断点引張強さ、およびASTM D−882によって測定された時に4%〜10%の降伏点または破断点伸び(全ての性質が23℃において決定される)
を有する、請求項1に記載の電気導電性表面材。 - 前記導電層が、銅、アルミニウム、青銅、チタン、またはそれらの合金の多孔質または非多孔質金属層である、請求項1に記載の電気導電性表面材。
- 前記導電層が、76μm未満の厚さを有する非多孔質層である、請求項1に記載の電気導電性表面材。
- 前記導電層が、60gsm〜350gsmの範囲内の面積重量を有する多孔質層である、請求項1に記載の電気導電性表面材。
- 前記導電層が金属スクリーンまたはエキスパンデッドメタル箔である、請求項1に記載の電気導電性表面材。
- 前記導電層が非多孔質金属箔である、請求項1に記載の電気導電性表面材。
- 前記不織布層(d)が、ポリマー繊維、無機繊維、金属被覆繊維、およびそれらの組合せからなる群から選択される不規則に配向された繊維を含む、請求項1に記載の電気導電性表面材。
- 前記不織布層(d)の前記繊維が、炭素繊維、金属被覆炭素繊維、金属被覆ガラス繊維、金属被覆ポリエステル繊維、金属被覆ポリアミド繊維、およびそれらの組合せからなる群から選択される、請求項9に記載の電気導電性表面材。
- 前記不織布層(d)の繊維が、ポリアミド繊維、ポリエステル繊維、ガラス繊維、およびそれらの組合せからなる群から選択される、請求項10に記載の電気導電性表面材。
- 前記不織布層(d)が10gsm〜50gsmの範囲内の面積重量を有する、請求項1に記載の電気導電性表面材。
- 前記不織布層(d)が金属被覆をさらに含み、それが硬化性樹脂層(b)と接触していない、請求項1に記載の電気導電性表面材。
- 自動配置のために適している連続したまたは細長いテープの形態である、請求項1に記載の電気導電性表面材。
- 前記テープが、0.125インチ〜12インチ(または3.17mm〜305mm)の範囲の幅およびその幅の少なくとも十(10)倍である長さを有する、請求項14に記載の電気導電性表面材。
- 前記テープの全厚さが76μm〜229μmの範囲内である、請求項14に記載の電気導電性表面材。
- 硬化性母材樹脂で含浸された強化繊維を含む複合基材と、
前記補剛層が前記複合基材と接触しているように前記複合基材の表面に積層される請求項1に記載の電気導電性表面材と、を含む、複合構造物。 - 前記複合基材が、積み重ね配列において配列された複数のプリプレグプライを含むプリプレグレイアップであり、各々のプリプレグプライが、硬化性母材樹脂で含浸されるかまたはその中に埋め込まれる一方向強化用繊維を含む、請求項17に記載の複合構造物。
- 硬化性母材樹脂で含浸された強化繊維を含む、複合基材を形成する工程と、
複数の請求項14に記載の電気導電性表面材を自動配置方法によって複合基材上に直接に、並列に分配して、保護表面層を前記複合基材上に形成する工程であって、自動配置する間に前記表面材中の前記補剛層が前記複合基材に面している工程と、
前記保護表面層と前記複合基材とを同時硬化する工程と、を含む、複合構造物を形成するための方法。 - 前記複合基材が、プリプレグテープを直接に成形面上に分配して圧縮する工程を包含する自動配置方法においてプリプレグテープをレイアップすることによって形成される、請求項19に記載の方法。
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EP3383640B1 (en) | 2023-06-07 |
EP3383640A1 (en) | 2018-10-10 |
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US11027856B2 (en) | 2021-06-08 |
US11565825B2 (en) | 2023-01-31 |
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ES2954423T3 (es) | 2023-11-22 |
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AU2020233766B2 (en) | 2022-04-07 |
US20210253270A1 (en) | 2021-08-19 |
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