JP6046739B2 - 複合構造用表面フィルムおよびその作成方法 - Google Patents
複合構造用表面フィルムおよびその作成方法 Download PDFInfo
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- JP6046739B2 JP6046739B2 JP2014546043A JP2014546043A JP6046739B2 JP 6046739 B2 JP6046739 B2 JP 6046739B2 JP 2014546043 A JP2014546043 A JP 2014546043A JP 2014546043 A JP2014546043 A JP 2014546043A JP 6046739 B2 JP6046739 B2 JP 6046739B2
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- surface film
- epoxy
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- resin
- epoxy resin
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Description
表面フィルム組成物は少なくとも2つの多官能性エポキシ樹脂を含み、その一方は、1より多いエポキシ官能基を有するエポキシノボラック樹脂である。第2のエポキシ樹脂は、非ノボラック多官能性エポキシ樹脂、好ましくは4官能性または3官能性エポキシ樹脂(すなわち、1分子あたり3または4個のエポキシ官能基を有するエポキシ樹脂)である。
前述の多官能性樹脂の混合物に基づく樹脂マトリックスを強化するために、1以上のポリマー強化剤を表面フィルム組成物に添加する。ポリマー強化剤は、(i)エポキシ樹脂、ビスフェノール、エラストマーポリマーの反応によって形成される予備反応付加物;(ii)ポリエーテルスルホン(PES)とポリエーテルエーテルスルホン(PEES)とのコポリマー;および(iii)コア−シェルゴム粒子;ならびにそれらの組み合わせからなる群から選択される。好ましい実施形態において、この群からの2つの強化剤の組み合わせを使用する。強化剤(複数可)の量は、合計して、表面フィルム組成物の総重量基準で約10%〜約20重量%である。
Thermoset Specialtiesから入手可能なEPALLOY(登録商標)5000(ビスフェノールAジグリシジルエーテルを水素化することによって調製される脂環式エポキシ)である。予備反応付加物での使用に好適な他の脂環式エポキシドとしては、Momentive Specialty Chemicalsによって提供されるEPONEX脂環式エポキシ樹脂、例えばEPONEX Resin 1510を挙げることができる;
oration (Houston, Tex.)から商標名Kane Ace MXで市販されている。コア−シェルゴム粒子を粒子の好適な液体エポキシ樹脂中懸濁液として表面フィルム組成物に添加することが好ましいが、必須ではない。Kane Ace MX411は、25重量%のコア−シェルゴム粒子のMY721エポキシ樹脂中懸濁液であり、好適なコア−シェルゴム粒子源である。DER331樹脂中に分散された25〜37重量%の同じコア−シェルゴム粒子を含有するKane Ace MX120、MX125、またはMX156も、好適なコア−シェルゴム粒子源である。MX257、MX215およびMX451などの他の好適なコア−シェルゴム粒子源も使用することができる。別の市販のコア−シェルゴム粒子源は、Dow Chemical Co.から得られるParaloid(商標)EXL−2691(約200nmの平均粒子サイズを有するメタクリレート−ブタジエン−スチレンCSR粒子)である。
セラミック微小球を表面フィルム組成物に添加して、フィルムの表面平滑性を改善する。1つの実施形態では、不活性シリカ−アルミナセラミック材料で作られた中空セラミック微小球を使用する。セラミック微小球は、60,000psiを超える破砕強度、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得る。セラミック微小球はその高い軟化点のために溶媒に対して非吸収性となり、不燃性となり、そして化学薬品に対して高度に耐性となり得る。約0.1〜約20ミクロン、好ましくは約1〜約15ミクロンの直径を有する微小球が特に好適であることが判明している。本発明の表面フィルム組成物での使用に特に好適な市販のセラミック微小球の一例は、Zeelan Industries, Inc.によって商標Zeeospheres(登録商標)、たとえば、G−200、G210およびW−200で販売されている。これらは、厚肉で無臭の淡灰白色中空シリカ−アルミナ球である。好ましい実施形態では、多官能性樹脂とセラミック微小球との組み合わせは、表面フィルム組成物の50重量%超、好ましくは60重量%超を構成する。ある実施形態において、セラミック微小球の量は、表面フィルム組成物の総重量基準で、少なくとも20重量%、好ましくは少なくとも25%または少なくとも30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、20%〜40重量%、または25%〜35重量%の範囲内であり得る。
多官能性エポキシド樹脂は、高温(たとえば、150°F(65℃)より高い温度で活性化されるさまざまな潜在性アミン系硬化剤によって硬化させることができる。好適な硬化剤の例としては、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挙げられる。イミダゾールおよびアミン複合体のクラスの化合物も使用することができる。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、表面フィルム組成物の総重量基準で1〜5重量%の範囲内の量で存在する。
微粒子形態(たとえば、粉末)の無機フィラーを表面フィルム組成物にレオロジー修飾成分として添加して、樹脂性組成物の流動を制御し、樹脂性組成物中での凝集を防止する。表面フィルム組成物で使用することができる好適な無機フィラーとしては、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挙げられる。1つの実施形態では、疎水性ヒュームドシリカ(たとえば、Cab−O−Sil TS−720)を無機フィラーとして使用する。無機フィラーの量は、表面フィルム組成物の総重量基準で1〜5重量%の範囲内であり得る。
表面フィルム組成物は、硬化または未硬化表面フィルムの機械的、電気的、光学的、難燃性、および/または熱的特性の1以上に影響を及ぼす1以上の任意の添加剤をさらに含み得る。添加剤は、表面フィルムがその上に形成される複合基体のエポキシ樹脂と化学的に反応するか、またはそれらと非反応であり得る材料を含んでもよい。そのような添加剤としては、紫外線(UV)安定剤、顔料/染料、および伝導性材料が挙げられるが、これらに限定されるものではない。そのような添加剤を使用する場合、それらの総量は表面フィルム組成物の総重量基準で5重量%未満である。
ルの長さ、および約1000のアスペクト比(L/D)を有し得る。
表面フィルム組成物の成分を、成分の混合、加熱、および/または冷却の機能を備えた
合容器に添加することができる。さらに、成分の混合を促進するために、1以上の有機溶媒も必要に応じて混合物に添加することができる。そのような溶媒の例としては、メチルエチルケトン(MEK)、アセトン、ジメチルアセトアミド、およびN−メチルピロリドンを挙げることができるが、これらに限定されるものではない。表面フィルムを続いて、通常のフィルム形成過程を使用して表面フィルム組成物から形成する。そのように形成された表面フィルムは、意図される用途に応じて、約0.01〜0.45psf(1平方フィートあたりのポンド)のフィルム重量を有し得る。
硬化表面フィルムのガラス転移温度(Tg)は、変調DSC(TA 2910)または熱的機械的分析器(TMA2940、TA Instruments)のいずれかを使用し、窒素下、10℃/分の傾斜にて30℃〜230℃の温度範囲内で測定した。
塗料除去剤流体取り込みおよび表面鉛筆硬度変化を、航空宇宙用複合構造塗料除去過程のために使用したベンジルアルコール系塗料除去剤溶液(McGeanから入手可能なCee Bee 2012AまたはHenkelから入手可能なTurco 1270−6)の浸漬時間(室温で168時間まで)にわたって測定することによって、未塗装の表面仕上げされた複合パネル(2”×2”試料サイズ、厚さ0.15mm)の塗料除去剤耐性を測定した。各試験パネルの重量を24時間、48時間および168時間(7日)までの期間で塗料除去剤に浸漬した前後で測定した。試験パネルの塗料除去剤流体取り込み(浸漬時間にわたる重量変化、重量%で表す)を同じ試験間隔で168時間(7日)までの浸漬で測定した。
塗装前のUV暴露の有り無しの両方で、表面フィルムで表面処理された塗装された複合パネル(3”×6”の試料サイズ、厚さ0.15mmの形態)の乾燥および湿潤スクライブ塗膜密着性をASTM D3359にしたがって測定した。ASTM D3359は、
フィルムに作られた切れ目上に粘着テープを施用し、除去することによって、基体に対するコーティングフィルムの表面接着を評価するための標準的試験方法(クロスハッチスクライブテープ試験)である。硬化した試験パネルをゼロ(UVなし)、200kJ/m2または1000kJ/m2の紫外線(UV−A)放射にAATCC試験法16、オプション3にしたがって暴露した。UV試験のために使用する装置は、Xeno耐候性試験機、例えばAtlas CI3000 FadeoMeterである。各試験パネル表面を調製し(清浄化、サンディングの有り無しの両方)、航空宇宙用塗装で使用される外部装飾用塗料コーティング(エポキシ塗料プライマー、続いてポリウレタン系トップコート)を施用した。その後、乾燥塗膜密着性試験をASTM D3359にしたがって実施した。湿潤塗膜密着性を実施するために、UV暴露した試験パネルを塗装し、次いで75°Fで7日間脱イオン水中に浸漬した。湿潤塗膜密着性試験を次いでASTM D3359にしたがって実施した。
硬化した表面フィルムを有する試験パネルを切断して、約6×5インチの試験クーポンを形成し、それらの導電性または表面抵抗率(オーム/平方、またはミリオーム/平方)を、四探針AVO(登録商標)Ducter(登録商標)DLRO10X Digital Low Resistivity Ohmmeterを使用して測定した。
塗装され、表面仕上げされた複合試験パネル(4”×6”の試料サイズ、厚さ0.15mmの形態)のミクロ亀裂発生に対する耐性も測定した。塗装された試験パネルを−55℃〜71℃で最大2000×サイクルまでの熱サイクルに供した。熱サイクル後の各試験パネルの表面を顕微鏡下で400×、800×、1200×、1600×および2000×熱サイクルにさらされた後のミクロ亀裂発生率について調べた。亀裂密度(試験パネルサイズの面積で示される表面塗装亀裂の数)を使用して、表面仕上げされた複合試験パネルのミクロ亀裂耐性を測定する。亀裂の最大長さは0.1インチ未満でなければならない。2000×熱サイクル後のミクロ亀裂試験結果を表4で示す。
%、3%などを含む。
Claims (14)
- 塗料除去剤に対して高い耐性を有する表面フィルムであって、前記表面フィルムは≧180℃のガラス転移温度(Tg)およびASTM D−3363によると7Hまたはそれ以上の鉛筆硬度を有し、
ベンジルアルコール系塗料除去溶液と7日間、20℃〜25℃の範囲内の温度で接触させた後、前記表面フィルムは0.5%未満の流体吸収を示し、鉛筆硬度は2H鉛筆等級を超えて減少せず、そして
前記表面フィルムは:
1より多いエポキシ官能基を有するエポキシノボラック樹脂;
3官能性または4官能性エポキシ樹脂;
セラミック微小球;
潜在性アミン系硬化剤;
微粒子無機フィラー;ならびに
(a)エポキシ樹脂、ビスフェノール、およびエラストマーの反応によって形成される予備反応付加物;(b)ポリエーテルスルホン(PES)およびポリエーテルエーテルスルホン(PEES)のコポリマー;(c)コア−シェルゴム(CSR)粒子;ならびにそれらの組み合わせからなる群から選択される少なくとも1つの強化剤
を含む硬化性樹脂組成物から形成される、表面フィルム。 - −55℃〜71℃で2000×熱サイクル試験に付した後に、0.3亀裂/インチ2未満のミクロ亀裂密度を示す、請求項1記載の表面フィルム。
- 少なくとも1つの強化剤が、テトラブロモビスフェノールA、ビスフェノールA、およびATBNまたはCTBNエラストマーのジグリシジルエーテルの反応によって形成される予備反応付加物を含む、請求項1〜3のいずれか1項に記載の表面フィルム。
- 少なくとも1つの強化剤が予備反応付加物およびPES−PEESコポリマーを含む、請求項1〜4のいずれか1項に記載の表面フィルム。
- セラミック微小球がシリカ−アルミナセラミック材料から作られた、1〜50ミクロンの範囲内の粒子サイズを有する中空微小球である、請求項1〜5のいずれか1項に記載の表面フィルム。
- エポキシ樹脂およびセラミック微小球が表面フィルム組成物の総重量の60重量%超を構成する、請求項1〜6のいずれか1項に記載の表面フィルム。
- 微粒子形態の伝導性材料をさらに含み、前記表面フィルムが落雷保護(LSP)または電磁干渉(EMI)シールドを提供することができる、請求項1〜7のいずれか1項に記載の表面フィルム。
- 請求項1〜8のいずれか1項に記載の表面フィルムは、ポリエステルマット、ガラスマットまたは伝導性担体から選択される不織担体によって担持されている。
- 硬化性樹脂組成物が硬化促進剤としてビス尿素をさらに含む、請求項1〜9のいずれか1項に記載の表面フィルム。
- その上に形成された表面フィルムを有する複合基体を含む複合構造であって、複合基体がマトリックス樹脂および強化繊維を含み、表面フィルムが、≧180℃のガラス転移温度(Tg)およびASTM D−3363によると7H以上の鉛筆硬度を有し、
ベンジルアルコール系塗料除去溶液と7日間、20〜25℃の範囲内の温度で接触した後、前記表面フィルムが0.50%未満の流体吸収を示し、鉛筆硬度が2H鉛筆等級を超えて減少せず、そして
表面フィルムが:
1より多いエポキシ官能基を有するエポキシのボラック樹脂;
3官能性または4官能性エポキシ樹脂;
セラミック微小球;
アミン系硬化剤;
微粒子無機フィラー;および
(a)エポキシ樹脂、ビスフェノール、およびエラストマーの反応によって形成される予備反応付加物;(b)ポリエーテルスルホン(PES)およびポリエーテルエーテルスルホン(PEES)のコポリマー;(c)コア−シェルゴム(CSR)粒子;ならびにそれらの組み合わせから選択される少なくとも1つの強化剤
を含む硬化性樹脂組成物から形成される、複合構造。 - 前記複合基体がプリプレグレイアップを含み、プリプレグレイアップが互いに積み重ねられた複数のプリプレグ層から構成され、各層がマトリックス樹脂を含浸させた強化繊維を含み、そして表面フィルムがプリプレグレイアップの外表面上に形成される、請求項11記載の複合構造。
- 表面フィルム上に施用された塗料コーティングをさらに含む、請求項11または12記載の複合構造。
- 複合構造を作成する方法であって:
(a)積み重ね配列で配置された複数のプリプレグ層であって、各プリプレグ層が未硬化または部分的に硬化した樹脂マトリックス樹脂および強化繊維を含むプリプレグ層から構成される、成形可能なプリプレグレイアップを提供し;
(b)1より多いエポキシ官能基を有するエポキシノボラック樹脂;
3官能性または4官能性エポキシ樹脂;
セラミック微小球;
潜在性アミン系硬化剤;
微粒子無機フィラー;ならびに
(a)エポキシ樹脂、ビスフェノール、およびエラストマーの反応によって形成される予備反応付加物;(b)ポリエーテルスルホン(PES)およびポリエーテルエーテルスルホン(PEES)のコポリマー;(c)コア−シェルゴム(CSR)粒子;およびそれらの組み合わせ
からなる群から選択される少なくとも1つの強化剤
を含む硬化性樹脂組成物から表面フィルムを形成し;
(c)表面フィルムをプリプレグレイアップと接触させ;そして
(d)表面フィルムおよびプリプレグレイアップを250°F〜350°F(120℃〜175℃)の範囲内の温度で同時硬化させることを含み、
それによって、硬化した表面フィルムが、≧180℃のガラス転移温度(T g )およびASTM D−3363により7H以上の鉛筆硬度を有し、
ベンジルアルコール系塗料除去溶液と7日間20℃〜25℃の範囲内の温度で接触させた後、硬化した表面フィルムが0.5%未満の流体吸収を示し、鉛筆硬度が2H鉛筆等級を超えて減少しない、方法。
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CN103987751B (zh) | 2017-09-12 |
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CA2858549C (en) | 2019-03-26 |
BR112014007044A2 (pt) | 2017-04-11 |
MX358605B (es) | 2018-08-28 |
TW201329154A (zh) | 2013-07-16 |
US20130149934A1 (en) | 2013-06-13 |
US9925729B2 (en) | 2018-03-27 |
EP2825579B1 (en) | 2017-03-15 |
RU2014127858A (ru) | 2016-01-27 |
KR101984198B1 (ko) | 2019-05-30 |
AU2012347889A1 (en) | 2014-02-06 |
CA2858549A1 (en) | 2013-06-13 |
CN103987751A (zh) | 2014-08-13 |
BR112014007044B1 (pt) | 2020-09-24 |
RU2608400C2 (ru) | 2017-01-18 |
MX2014006534A (es) | 2014-07-10 |
ES2626499T3 (es) | 2017-07-25 |
AU2012347889B2 (en) | 2016-04-07 |
EP2825579A2 (en) | 2015-01-21 |
WO2013086063A2 (en) | 2013-06-13 |
IN2014CN04162A (ja) | 2015-07-17 |
KR20140109855A (ko) | 2014-09-16 |
TWI558759B (zh) | 2016-11-21 |
US9676961B2 (en) | 2017-06-13 |
WO2013086063A3 (en) | 2014-01-16 |
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