TWI597166B - 剝離層、使用其之表面製備及結合複合結構之方法 - Google Patents

剝離層、使用其之表面製備及結合複合結構之方法 Download PDF

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Publication number
TWI597166B
TWI597166B TW101144822A TW101144822A TWI597166B TW I597166 B TWI597166 B TW I597166B TW 101144822 A TW101144822 A TW 101144822A TW 101144822 A TW101144822 A TW 101144822A TW I597166 B TWI597166 B TW I597166B
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Taiwan
Prior art keywords
resin
release layer
composite substrate
epoxy
range
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TW101144822A
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English (en)
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TW201345716A (zh
Inventor
趙藝強
達利夫 庫瑪 柯里
庫納 高朗 夏
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氰特科技股份有限公司
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/28—Shaping operations therefor
    • B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C37/00—Component parts, details, accessories or auxiliary operations, not covered by group B29C33/00 or B29C35/00
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    • B29C37/0075—Using separating agents during or after moulding; Applying separating agents on preforms or articles, e.g. to prevent sticking to each other using release sheets
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Description

剝離層、使用其之表面製備及結合複合結構之方法
本發明概言之係關於用於在結合之前複合基材、更具體而言基於樹脂之複合基材之表面製備的剝離層。
手動磨砂、粗砂噴射及剝離層移除係製備在航天工業中用於黏著劑結合之基於樹脂之複合基材之表面的習用方法。藉由剝離層移除之黏著劑結合係該三種技術中之最常見者，此乃因其節省大量人力且產生更加均勻處理之表面。剝離層移除通常涉及將乾燥之有紋理織物材料施加至基於樹脂之複合基材之結合表面上，之後固化。固化後，移除(即剝離)剝離層以顯露粗糙化或有紋理結合表面。然而，乾燥剝離層在剝離後往往在結合表面上留下殘餘斷裂纖維。此導致差的黏著劑結合性質，此乃因殘餘纖維可存在以下缺陷：防止黏著劑完全潤濕複合基材之結合表面，藉此導致黏著失效。一般工業經驗係剝離層方法關於結合性能無可靠性及預測性。
本發明提供在剝離後不留下殘餘纖維且可與不同基於樹脂之複合基材良好地運作之富樹脂剝離層。富樹脂剝離層包括經不同於複合基材之樹脂基質的樹脂基質浸漬之編織織物。該剝離層經設計以使在自複合基材表面人工移除剝離層時，剝離層樹脂之薄膜保留在複合基材表面上以產生可結合表面，但在同一表面上未保留編織織物之纖維材 料。此富樹脂剝離層能夠修飾不同複合物之表面用於與多種黏著劑可靠結合。因此，可將其視為「通用」剝離層。
本發明亦提供使用上文論述之剝離層製備用於複合物結合之表面的方法。亦揭示形成結合複合結構之方法，其包括：將剝離層施加至包括纖維強化樹脂之第一複合基材表面上；共固化剝離層及第一複合基材；自第一複合基材移除剝離層，在複合基材表面上留下剝離層樹脂之薄層；將黏著劑膜施加至第一複合基材之經修飾表面及第二複合基材表面中之至少一者上；使第一複合基材之經修飾表面與第二複合基材表面接觸，其間具有黏著劑膜；及固化以結合基材。
已發現可在以下方面實現優勢：用富樹脂剝離層處理纖維強化樹脂複合基材以修飾經處理複合基材表面，以便有利於並促進表面處理之複合結構與第二複合基材之間更強且更長持續時間結合。在剝離富樹脂剝離層(11)後，複合基材(10)表面由其上剩餘之薄樹脂膜(12)修飾。圖1圖解說明剝離層之運作機制。移除剝離層後剩餘樹脂之厚度係剝離前之剝離層初始厚度之約2%-15%。此剩餘剝離層樹脂層為黏著劑結合(包括共結合及二級結合)提供一致表面層。複合結合工業中之共結合宜指使用黏著劑結合固化預浸材與未固化預浸材。二級結合宜指使用黏著劑結合固化預浸材與另一固化預浸材。控制剝離層樹脂之流變性及固化動力學以使固化期間剝離層樹脂與複合基材之樹脂之間 之摻和最小化，藉此剝離層樹脂調配物具有實質上比複合基材之樹脂調配物快之固化動力學。由於富樹脂剝離層可與各種纖維強化樹脂複合基材一起使用，故可將其視為「通用」剝離層。
本文論述之纖維強化樹脂複合基材包括通常用於製造航天結構零件之預浸材或預浸材疊層。本文所用術語「預浸材」係指經基質樹脂浸漬之纖維之片或薄板。基質樹脂可以未固化或部分固化狀態存在。本文所用術語「預浸材疊層」係指複數個彼此堆疊放置之預浸材層。疊層內之預浸材層可相對於彼此以所選定向定位。舉例而言，預浸材疊層可包含具有單向纖維架構之預浸材層，其中纖維相對於疊層之最大尺寸(例如長度)以0°、90°、所選角度θ及其組合定向。應進一步理解，在某些實施例中，預浸材可具有纖維架構之任一組合，例如單向及多維。
在圖1中，本發明之富樹脂剝離層包括由樹脂基質(11b)浸漬之編織織物(11a)，且端視所浸漬編織織物之特定類型，以剝離層之總重量計具有至少20重量%之樹脂含量。在某些實施例中，樹脂含量在20%-50%範圍內。樹脂調配物及織物構築經選擇以使在移除剝離層後複合基材表面上未留下斷裂纖維。剝離期間之斷裂線(13)係在樹脂基質(11b)內或纖維-樹脂界面處，但不在織物內，如由圖2所圖解說明。固化後易於自複合基材表面移除富樹脂剝離層。為此，其呈現根據滾筒剝離測試ASTM D1781不大於10 in-lb/英吋寬度之剝離強度。
富樹脂剝離層之織物包括複數根以編織圖案編織之紗線。每一紗線包括複數個加撚在一起之連續纖維絲線(單一纖維)。編織織物之織物重量在50-250 gsm(克/m2)、較佳70-220 gsm範圍內，且厚度在50-250 μm、較佳100-200 μm範圍內。厚度主要隨重量及纖維類型變化，但亦取決於編織。編織織物之纖維類型可選自各種合成材料，包括聚酯(聚對苯二甲酸乙二酯、聚對苯二甲酸丁二酯、聚對苯二甲酸三亞甲基酯、聚乳酸及其共聚物)、聚乙烯、聚丙烯耐綸、彈性材料，例如LYCRA®；及高性能纖維，例如聚芳醯胺(例如Kevlar)、聚醯亞胺、聚乙烯亞胺(PEI)、聚噁唑(例如Zylon)、聚苯并咪唑(PBI)、聚醚醚酮(PEEK)及玻璃。纖維材料之主要要求係：材料不易碎且具有所需抗張強度。此外，織物可具有熱定型整理或其他習用整理。
紗線支數可以線性質量密度單位丹尼爾(denier)表示。丹尼爾等於以克表示之9000米紗線之重量。數目愈低，則紗線愈精細。對於一捲織物，在輥方向上運行且對於輥之全長連續之紗線係經向紗線。橫跨輥方向運行之短紗線稱為緯向紗線。對於富樹脂剝離層，基於以下特徵選擇織物：經向紗線之線性質量密度在50-250丹尼爾、較佳70-230丹尼爾範圍內，且緯向紗線之線性質量密度在50-250丹尼爾、較佳70-230丹尼爾範圍內，經向抗張強度為至少70 lbf/in，較佳80 lbf/in；緯向抗張強度為至少40 lbf/in，較佳50 lbf/in。編織圖案不受限且可為平紋編織、斜紋編織、方平編織、錦緞編織及諸如此類。對於基 於聚合物之織物，編織密度不應過高(即，緊密編織)，以便可產生紗線之低樹脂浸漬及不完全浸漬。
圖3係可用於富樹脂剝離層之例示性聚酯織物的掃描電子顯微鏡(SEM)影像。此特定織物之重量為110 gsm且紗線之線性質量密度為125丹尼爾。如自圖3可見，此類型之聚酯織物並不緊密織造且在編織中含有微小開口。在自複合表面剝離含有此類型之聚酯織物之剝離層時，產生具有粗糙化表面且無斷裂纖維之樹脂膜。該粗糙化表面對於結合係合宜的。緊密編織織物(例如玻璃織物)亦可用於形成富樹脂剝離層以產生對於複合結合合宜之表面粗糙度。圖4顯示可用於富樹脂剝離層之例示性玻璃織物。此玻璃織物比圖3中所示聚酯織物更緊密織造且更厚；其重量為205 gsm且厚度為175 μm。
剝離層之樹脂基質係自包括以下之可固化樹脂組合物形成：至少一種具有至少2之環氧官能度之環氧酚醛樹脂；選自多元酚之二縮水甘油醚之二官能基環氧樹脂；選自胺基苯酚之三縮水甘油醚之三官能基環氧樹脂；無機填料粒子(例如發煙二氧化矽)；及固化劑。以組合物之總重量計，環氧酚醛樹脂佔至少40重量%、較佳50-70重量%。以樹脂組合物之總重量計，二官能基環氧樹脂係以10-35重量%、較佳15-25重量%之量存在，三官能基環氧樹脂係以10-30重量%、較佳10-20重量%之量存在。
環氧酚醛樹脂之實例包括彼等藉由使酚(例如苯酚、鄰甲酚、間甲酚、對甲酚、對第三丁基苯酚、對壬基苯酚、 2,6-二甲苯酚、間苯二酚、雙酚-A、α及β-萘酚及萘二醇)與醛(例如乙醛、甲醛、糠醛、乙二醛及對羥基苯甲醛)在酸觸媒存在下反應獲得者。
適宜環氧酚醛樹脂包括由以下結構I代表之酚環氧酚醛樹脂及甲酚環氧酚醛樹脂：
其中n係0至8之整數，R=H或CH3。在R=H時，樹脂係苯酚酚醛樹脂。在R=CH3時，樹脂係甲酚酚醛樹脂。酚環氧酚醛樹脂係以DEN 428、DEN 431、DEN 438、DEN 439及DEN 485自Dow Chemical公司購得。甲酚環氧酚醛樹脂係以ECN 1235、ECN 1273及ECN 1299自Ciba-Geigy公司購得。
另一適宜環氧酚醛樹脂係具有由以下結構II代表之二環戊二烯主鏈之烴環氧酚醛樹脂：
其中n係0至7之整數。該等烴環氧酚醛樹脂之市售實例包括來自Vantico公司之Tactix® 71756、Tactix® 556及Tactix® 756。在一個實施例中，結構I之酚醛樹脂與結構II之含有二環戊二烯之酚醛樹脂結合使用。
適宜二官能基環氧樹脂包括雙酚A或雙酚F之二縮水甘油醚，例如由Dow Chemical公司供應之EponTM 828(液體環氧樹脂)、D.E.R.331、D.E.R.661(固體環氧樹脂)。
胺基苯酚之三縮水甘油醚係以Araldite® MY 0510、MY 0500、MY 0600、MY 0610自Huntsman Advanced Materials購得。
適於剝離層樹脂組合物中之環氧樹脂之固化劑包括一類稱作路易士酸(Lewis Acid)之固化劑：三氟化硼(BF3)、三氯化硼(BCl3)及其複合物，例如BF3-胺複合物及BCl3-胺複合物。BF3-胺複合物之實例包括來自Ato-Tech之BF3-MEA、來自Air Products之Anchor 1040(與苄胺及異丙胺複合之BF3)、來自Air Products之Anchor 1115(與異丙胺加合物複合之BF3)及亦來自Air Products之Anchor 1170(與氯苄胺複合之BF3)。BCl3-胺複合物之實例包括OmincureTM BC-120。製備複合物以在正常使用情況下提供液體或固體形式。許多市售基於環氧之預浸材包括基於胺之固化劑，例如3,3'-二胺基二苯基碸(DDS)及二氰基二醯胺(DICY)，其顯示其固化動力學實質上比含有上述固化劑(例如BF3液體)之剝離層樹脂調配物慢。因此，剝離層樹脂調配物可足夠快速固化以使共固化過程期間與預浸材 樹脂之摻和最小化。
將呈顆粒形式(例如粉末)之無機填料作為流變性改良組份添加至剝離層樹脂組合物中以控制樹脂性組合物之流量並防止於其中聚集。可用於表面膜組合物中之適宜無機填料包括發煙二氧化矽、滑石粉、雲母、碳酸鈣、氧化鋁。以表面膜組合物之總重量計，無機填料之量可在1-10重量%、較佳1-5重量%範圍內。
在一實施例中，以樹脂組合物之總重量計，剝離層之樹脂組合物可包括：約45-55%苯酚酚醛環氧樹脂；約5-15%含有二環戊二烯之酚醛環氧樹脂、約20-30%雙酚A之二縮水甘油醚；約15-25%胺基苯酚之三縮水甘油醚；約5-15%BF3固化劑及約1-5%無機填料。
此外，若需要，亦可向上述樹脂組合物中添加一或多種有機溶劑以有利於組份之混合。該等溶劑之實例可包括(但不限於)甲基乙基酮(MEK)、丙酮、二甲基乙醯胺及N-甲基吡咯啶酮。
富樹脂剝離層可藉由以下方式形成：使用習用溶劑或熱熔融塗佈方法將上述樹脂組合物塗佈於編織織物上，以便完全浸漬織物中之紗線。若需要，隨後使濕剝離層乾燥以將揮發物含量減少至較佳小於2重量%。乾燥可藉由於室溫下風乾隔夜之後於140℉-170℉下乾燥、或(若需要)於高溫下爐乾燥以減少乾燥時間來完成。隨後，可藉由將可移除脫模紙或合成膜(例如聚酯膜)施加於相對側上保護乾燥富樹脂剝離層。該等脫模紙或合成膜係在使用剝離層進 行表面結合之前移除。將乾燥剝離層施加至未固化(或部分固化)之基於樹脂之複合基材(例如基於環氧之預浸材)之表面上。其後，使剝離層與複合基材一起進行共固化。隨後移除剝離層以在複合基材上留下薄樹脂膜，藉此形成準備用於與另一複合基材黏著劑結合之經修飾表面。
對於兩個複合基材之共結合及二級結合，將可固化黏著劑膜施加至已經固化之第一複合基材之經修飾表面與第二複合基材表面中之至少一者上。使第一固化複合基材之經修飾表面與第二複合基材表面接觸，以使黏著劑介於基材之間。隨後實施固化以形成結合複合結構。本文所用術語「固化」(「curing」及「cure」)係指可藉由加熱、暴露於紫外光或輻射實施之聚合及/或交聯製程。
富樹脂剝離層及基於樹脂之複合基材(例如基於環氧之預浸材)之共固化可於高於230℉(110℃)、更特定而言在250℉-375℉(121℃-190℃)範圍內之溫度下實施。已發現本文所述富樹脂剝離層之優勢在於剝離層可在上述固化範圍內與大多數市售預浸材共固化。該預浸材包括以CYCOM 997、CYCOM 977-2、CYCOM 934、CYCOM 970、CYCOM 5317-3、CYCOM 5320-1及CYCOM 851自Cytec Industries公司購得之樹脂預浸漬織物及/或膠帶；來自Hexcel公司之Hexply 8552；及來自Toray Industries公司之Toray 3900-2。在共固化後，固化富樹脂剝離層呈現如由調節差示掃描量熱(DSC)方法所量測之140℃、在一些實施例中為140℃-200℃之玻璃化轉變溫度(Tg)。
實例
以下實例闡釋本文揭示之富樹脂剝離層及其應用之一些實施例，且不應理解為限制本發明之範疇。
實例1
富樹脂剝離層係藉由用樹脂調配物浸漬聚酯織物製得，該樹脂調配物包含(以重量%表示)：45%苯酚-甲醛酚醛環氧樹脂；11%含有二環戊二烯之酚醛環氧樹脂；23%雙酚A之二縮水甘油醚；14%胺基苯酚之三縮水甘油醚；5%液體BF3及2%發煙二氧化矽。聚酯織物具有以下性質：
先後使用熱熔融方法及溶劑添加方法混合樹脂調配物。在進行熱熔融混合後，向樹脂組合物中添加甲基乙基酮(MEK)溶劑以形成82%固體懸浮液。使用溶劑塗佈方法將濕樹脂組合物塗佈於織物上且於室溫下乾燥過夜，之後進行爐乾燥過程，以將揮發物含量減少至小於2%。乾燥剝離層之樹脂含量為約43重量%且厚度為約140 μm。
或者，亦可於室溫下在溶劑輔助之過程中混合樹脂調配物與MEK。以與上述相同之方式將82%固體含量下之所得濕樹脂混合物塗佈至織物上。
如上文所論述乾燥剝離層用於製備纖維強化之基於環氧之預浸材CYCOM 997膠帶(來自Cytec Industries公司)之表面。於177℃下共固化後，剝離剝離層，留下經修飾表面準備用於結合。實施滾筒剝離測試(ASTM D1781)以評價剝離層之剝離強度。測試結果指示11.1牛頓(2.5 in-lb/英吋寬度)。此顯示易於剝離剝離層。實施藉由ATR-FTIR(衰減全反射)之表面分析以研究固化及移除剝離層後預浸材之經處理表面。發現在預浸材頂部上留下約3-10 μm之剝離層樹脂薄層。圖5係移除富樹脂剝離層後經處理表面之掃描電子顯微鏡(SEM)影像，其顯示未保留織物之斷裂纖維。
實例2
富樹脂剝離層係藉由用以下樹脂調配物浸漬聚酯織物製作：以重量%表示，45%苯酚-甲醛酚醛環氧樹脂；11%含有二環戊二烯之酚醛環氧樹脂；22.5%雙酚A之二縮水甘油醚；13.5%胺基苯酚之三縮水甘油醚；6% BF3-MEA；及2%發煙二氧化矽。織物具有以下性質：
以與實例1相同之方式將樹脂調配物混合，塗佈於織物 上，乾燥並測試。觀察到類似結果-在移除富樹脂剝離層後在預浸材頂部上留下約3-10 μm之剝離層樹脂薄層，但未保留織物之斷裂纖維。
實例3
富樹脂剝離層係藉由用樹脂調配物浸漬聚酯織物製得，該樹脂調配物包含(以重量%表示)：44.5%苯酚-甲醛酚醛環氧樹脂；9%含有二環戊二烯之酚醛環氧樹脂；22%雙酚A之二縮水甘油醚；18%胺基苯酚之三縮水甘油醚；4.7%液體BF3及1.8%發煙二氧化矽。聚酯織物具有以下性質：
以與實例1相同之方式將樹脂調配物混合，塗佈於織物上，乾燥並測試。觀察到類似結果-在移除富樹脂剝離層後在預浸材頂部上留下約3-10 μm之剝離層樹脂薄層，但未保留織物之斷裂纖維。
實例4
富樹脂剝離層係藉由用樹脂調配物浸漬聚酯織物製得，該樹脂調配物包含(以重量%表示)：44%苯酚-甲醛酚醛環氧樹脂；9%含有二環戊二烯之酚醛環氧樹脂；22%雙酚A之二縮水甘油醚；17%胺基苯酚之三縮水甘油醚；6%BF3- MEA及2%發煙二氧化矽。聚酯織物具有以下性質：
以與實例1相同之方式將樹脂調配物混合，塗佈於織物上，乾燥並測試。觀察到類似結果-在移除富樹脂剝離層後在預浸材頂部上留下約3-10 μm之剝離層樹脂薄層，但未保留織物之斷裂纖維。
實例5
富樹脂剝離層係藉由用樹脂調配物浸漬聚酯織物製得，該樹脂調配物包含(以重量%表示)：45.5%苯酚-甲醛酚醛環氧樹脂；11.4%含有二環戊二烯之酚醛環氧樹脂；22.8%雙酚A之二縮水甘油醚；13.7%胺基苯酚之三縮水甘油醚；4.8%液體BF3及1.8%發煙二氧化矽。聚酯織物具有以下性質：
以與實例1相同之方式將樹脂調配物混合，塗佈於織物 上，乾燥並測試。觀察到類似結果-在移除富樹脂剝離層後在預浸材頂部上留下約3-10 μm之剝離層樹脂薄層，但未保留織物之斷裂纖維。
實例6
富樹脂剝離層係藉由用樹脂調配物浸漬玻璃織物製得，該樹脂調配物包含(以重量%表示)：44.5%苯酚-甲醛酚醛環氧樹脂；8.9%含有二環戊二烯之酚醛環氧樹脂；22.3%雙酚A之二縮水甘油醚；17.8%胺基苯酚之三縮水甘油醚；4.7%液體BF3及1.8%發煙二氧化矽。玻璃織物具有以下性質：
以與實例1相同之方式混合樹脂調配物，塗佈至織物上。乾燥後，乾燥剝離層之樹脂含量為約28重量%且厚度為約195 μm。隨後以與實例1相同之方式測試富樹脂剝離層。觀察到類似結果-在移除富樹脂剝離層後在預浸材頂部上留下約3-10 μm之剝離層樹脂薄層，但未保留織物之斷裂纖維。
實例7
富樹脂剝離層係藉由用實例6中揭示之樹脂調配物浸漬聚酯織物製得。聚酯織物具有以下性質：
以與實例1相同之方式將樹脂調配物混合，塗佈於織物上，乾燥並測試。觀察到類似結果-在移除富樹脂剝離層後在預浸材頂部上留下約3-10 μm之剝離層樹脂薄層，但未保留織物之斷裂纖維。
實例8 雙重疊剪切測試
使用市售黏著劑FM 318 M.05 psf(來自Cytec Industries公司)將CYCOM 970預浸材(來自Cytec Industries公司)彼此結合。於每一測試溫度下測試3至4個結合預浸材試樣。在結合之前，使用如實例1中論述之富樹脂剝離層製備預浸材之結合表面。表2顯示基於雙重疊剪切測試(ASTM D3528)之23℃、-55℃及72℃測試溫度下之平均剪切數據。如表2中可見，剝離層促進各種測試溫度下之黏結失效。
實例9 雙懸臂樑測試
結合預浸材試樣係使用各種市售預浸材材料及市售黏著劑FM 309-1(來自Cytec Industries公司)形成。在結合之前，使用如實例1中論述之富樹脂剝離層製備預浸材之結合表面。於23℃及-55℃下實施雙懸臂樑測試(ASTM D5528)以量測結合預浸材之板間斷裂韌性(G1c)且結果示於圖6中。
使用結構黏著劑FM 309-1 M.05 psf使CYCOM 5317-6預浸材(來自Cytec Industries公司)共結合。在共結合之前，使用利用圖4中所示玻璃織物形成之富樹脂剝離層以在一個預浸材上製備結合表面。圖7A及7B顯示共結合預浸材之G1c測試後之黏結失效條件。
術語「第一」、「第二」及諸如此類在本文中並不表示任何次序、量或重要性，而是用於將元素彼此區分，且術語「一」(「a」及「an」)在本文中並不表示限制量，而是表示存在所提及項目中之至少一者。與量連用之修飾詞「約」(「approximately」或「about」)涵蓋所述值且具有由上下文指定之含義(例如，包括與特定量量測相關之誤差度)。如本文所用後綴「(s)」意欲包括單數及複數個其修飾之項，藉此包括該項中之一或多種(例如，金屬包括一或多種金屬)。本文中揭示之範圍具涵蓋性且可獨立組合(例如，「高達約25 wt%、或更特定而言約5 wt%至約20 wt%」之範圍包括「約5 wt%至約25 wt%」範圍之終點及 所有中間值等)。
儘管本文闡述各種實施例，但自說明書應瞭解，可由彼等熟習此項技術者作出要素之各種組合、其中之改變或改良，且此在本發明範疇內。另外，為適應特定情況或材料亦可對本發明之教示實施多項改良，此並不背離本發明之基本範疇。因此，本文並非意欲將本發明限制於所揭示之作為實施本發明最佳設想模式之特定實施例，而係意欲使本發明包括所有屬於隨附申請專利範圍範疇內之實施例。
10‧‧‧基材
11‧‧‧剝離層
11a‧‧‧編織織物
11b‧‧‧樹脂基質
12‧‧‧樹脂膜
13‧‧‧斷裂線
圖1示意性顯示本發明之富樹脂剝離層之運作機制。
圖2顯示在自複合基材移除剝離層時出現之斷裂線。
圖3係可用於富樹脂剝離層之例示性聚酯織物的掃描電子顯微鏡(SEM)影像。
圖4係可用於富樹脂剝離層之例示性玻璃織物的掃描電子顯微鏡(SEM)影像。
圖5係移除富樹脂剝離層後經處理表面之掃描電子顯微鏡(SEM)影像。
圖6顯示實例中用於各種黏著性結合預浸材之斷裂韌性(G1c)數據。
圖7A及7B係顯示一個實例之斷裂韌性(G1c)測試後共結合預浸材之黏結失效條件的光學顯微鏡影像。
10‧‧‧基材
11‧‧‧剝離層
11a‧‧‧編織織物
11b‧‧‧樹脂基質
12‧‧‧樹脂膜

Claims (21)

  1. 一種剝離層系統，其用於各種複合基材之表面製備，該系統包含：(a)複合基材，其包含經固化之第一樹脂基質浸漬之強化纖維；及(b)黏附至該複合基材表面之可移除之富樹脂剝離層，該剝離層包含經不同於該第一樹脂基質之經固化之第二樹脂基質浸漬的編織織物，藉此在自該複合基材表面人工移除該剝離層時，在該複合基材表面上保留該第二樹脂基質之薄膜，以提供能夠與另一複合基材共結合及二級結合之可結合表面，其中該第二樹脂基質係自包含以下之樹脂組合物形成：至少一種具有至少2之環氧官能度之環氧酚醛樹脂；選自多元酚之二縮水甘油醚的二官能基環氧樹脂；選自胺基苯酚之三縮水甘油醚的三官能基環氧樹脂；固化劑；及無機填料粒子；其中該剝離層具有以該剝離層之總重量計至少20重量%之樹脂含量，且其中該編織織物包含複數根以編織圖案編織之紗線，該等紗線具有70lbf/in之經向抗張強度、40lbf/in之緯向抗張強度、在50至250丹尼爾(denier)範圍內之經向線性質量密度及在50至250丹尼爾範圍內之緯向線性質量 密度。
  2. 如請求項1之系統，其中該等紗線具有80lbf/in之經向抗張強度、50lbf/in之緯向抗張強度、在70至230丹尼爾範圍內之經向線性質量密度及在70至230丹尼爾範圍內之緯向線性質量密度。
  3. 如請求項1之系統，其中該第二樹脂基質之剩餘薄膜具有為移除前之該剝離層初始厚度之2%至15%的厚度。
  4. 如請求項1之系統，其中該樹脂組合物包含至少一種選自由以下結構代表之酚環氧酚醛樹脂及甲酚環氧酚醛樹脂的環氧酚醛樹脂： 其中n係0至8之整數，R=H或CH3。
  5. 如請求項4之系統，其中該樹脂組合物另外包含由以下結構代表之含有二環戊二烯之酚醛環氧樹脂： 其中n=0至7之整數。
  6. 如請求項1之系統，其中該編織織物具有在50gsm至250 gsm範圍內之織物重量。
  7. 如請求項6之系統，其中該編織織物具有在70gsm至220gsm範圍內之織物重量。
  8. 如請求項1之系統，其中該編織織物具有在50μm至250μm範圍內之織物厚度。
  9. 如請求項8之系統，其中該編織織物具有在100μm至200μm範圍內之織物厚度。
  10. 如請求項1之系統，其中該編織織物之該等紗線係由選自由以下組成之群之材料製造：聚醛、聚乙烯、聚丙烯、耐綸(nylon)、彈性材料、聚芳醯胺、聚醯亞胺、聚乙烯亞胺(PEI)、聚噁唑、聚苯并咪唑(PBI)、聚醚醚酮(PEEK)及玻璃。
  11. 如請求項1之系統，其中該剝離層具有以該剝離層之總重量計至少20重量%之樹脂含量。
  12. 如請求項11之系統，其中該剝離層具有以該剝離層之總重量計在20重量%至50重量%範圍內之樹脂含量。
  13. 如請求項1之系統，其中該剝離層具有140℃之玻璃化轉變溫度(Tg)。
  14. 如請求項13之系統，其中該剝離層具有在140℃至200℃範圍內之玻璃化轉變溫度(Tg)。
  15. 如請求項1之系統，其中該固化劑選自由BF3、BCl3及其複合物組成之群。
  16. 如請求項1之系統，其中該第二樹脂基質係自包含以下之樹脂組合物形成： 具有至少2之環氧官能度之酚環氧酚醛樹脂；具有至少2之環氧官能度之含有二環戊二烯之環氧酚醛樹脂；雙酚A之二縮水甘油醚；胺基苯酚之三縮水甘油醚；選自由BF3、BCl3及其複合物組成之群之固化劑；及發煙二氧化矽。
  17. 如請求項1之系統，其中以該組合物之總重量計，該等酚醛樹脂佔至少20重量%。
  18. 一種用於各種複合基材之表面製備之方法，其包含：(a)提供包含經第一樹脂基質浸漬之強化纖維的複合基材；(b)使富樹脂剝離層與該複合基材之表面接觸，該剝離層係藉由用包含以下之可固化樹脂組合物浸漬編織織物而形成：至少一種具有至少2之環氧官能度之環氧酚醛樹脂；選自多元酚之二縮水甘油醚的二官能基環氧樹脂；選自胺基苯酚之三縮水甘油醚的三官能基環氧樹脂；固化劑；及無機填料粒子，其中該編織織物包含複數根以編織圖案編織之紗線，該等紗線具有70lbf/in之經向抗張強度、40lbf/in之緯向抗張強度、在50至250丹尼爾範圍內之經向線性質量密度及在50至250丹尼爾範圍內之緯向線性質量密度； (c)共固化該剝離層及該複合基材；及(d)自該複合基材之該表面移除該剝離層，以便在該複合基材表面上保留來自該剝離層之樹脂之薄膜，以提供能夠與另一複合基材共結合及二級結合之可結合表面。
  19. 如請求項18之方法，其中該共固化係於高於230℉(110℃)之溫度下實施。
  20. 如請求項19之方法，其中該共固化係於250℉至375℉(121℃至190℃)之溫度範圍內實施。
  21. 一種形成結合複合結構之方法，其包含：(a)提供包含經第一樹脂基質浸漬之強化纖維的第一複合基材；(b)提供包含經第二樹脂基質浸漬之強化纖維的第二複合基材；(c)使富樹脂剝離層與該第一複合基材之表面接觸，該剝離層係藉由用包含以下之可固化樹脂組合物浸漬編織織物而形成：至少一種具有至少2之環氧官能度之環氧酚醛樹脂；選自多元酚之二縮水甘油醚的二官能基環氧樹脂；選自胺基苯酚之三縮水甘油醚的三官能基環氧樹脂；固化劑；及無機填料粒子，其中該編織織物包含複數根以編織圖案編織之紗線，該等紗線具有70lbf/in之經向抗張強度、40lbf/in之緯 向抗張強度、在50至250丹尼爾範圍內之經向線性質量密度及在50至250丹尼爾範圍內之緯向線性質量密度；(d)於高於230℉(110℃)之溫度下共固化該剝離層及該第一複合基材；(e)自該複合基材之該表面移除該剝離層，以便在該複合基材表面上保留來自該剝離層之樹脂之薄膜以提供可結合表面，但該同一表面上未保留來自該編織織物之纖維材料；(f)將黏著劑膜施加於該第一複合基材之該可結合表面或該第二複合基材之表面上；(g)使該第一複合基材之該可結合表面與該第二複合基材之表面接觸，其間具有黏著劑膜；及(h)固化以結合該第一及第二複合基材。
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