TW201634291A - 複合材料之結合 - Google Patents
複合材料之結合 Download PDFInfo
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- TW201634291A TW201634291A TW104136075A TW104136075A TW201634291A TW 201634291 A TW201634291 A TW 201634291A TW 104136075 A TW104136075 A TW 104136075A TW 104136075 A TW104136075 A TW 104136075A TW 201634291 A TW201634291 A TW 201634291A
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- Prior art keywords
- matrix resin
- composite substrate
- curing
- cured
- curable
- Prior art date
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- 239000002131 composite material Substances 0.000 title claims abstract description 128
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- 239000011347 resin Substances 0.000 claims abstract description 163
- 239000000758 substrate Substances 0.000 claims abstract description 108
- 238000000034 method Methods 0.000 claims abstract description 57
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- 238000004026 adhesive bonding Methods 0.000 claims abstract description 11
- 239000011159 matrix material Substances 0.000 claims description 71
- 239000010410 layer Substances 0.000 claims description 68
- -1 tertiary amine boron trifluoride complexes Chemical class 0.000 claims description 33
- 239000000835 fiber Substances 0.000 claims description 31
- 239000003795 chemical substances by application Substances 0.000 claims description 30
- 125000000524 functional group Chemical group 0.000 claims description 29
- 229920000647 polyepoxide Polymers 0.000 claims description 28
- 239000003822 epoxy resin Substances 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 22
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- 238000006243 chemical reaction Methods 0.000 claims description 11
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- 239000002759 woven fabric Substances 0.000 claims description 10
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- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 8
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 150000004703 alkoxides Chemical class 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052785 arsenic Inorganic materials 0.000 claims description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 2
- 229910000085 borane Inorganic materials 0.000 claims description 2
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- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
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Abstract
本發明係關於一種在黏著性結合前進行複合基材之表面預處理的方法。將可固化表面處理層施覆於基於樹脂之可固化複合基材上,接著共固化。共固化後,該複合基材完全固化而該表面處理層保持部分固化。該表面處理層可係樹脂薄膜或由經樹脂浸漬之織物構成之可移除剝離層。表面預處理後,該複合基材具有化學活性可結合表面,其可黏著性結合至另一複合基材以形成共價結合之結構。
Description
本申請案主張2014年11月3日申請之美國臨時專利申請案第62/074,266號之權利,該案以全文引用的方式併入本文中。
10‧‧‧剝離層
10a‧‧‧編織織物
10b‧‧‧可固化基質樹脂
11‧‧‧複合基材
11a‧‧‧強化纖維
11b‧‧‧未固化/可固化基質樹脂
12‧‧‧裂線
13‧‧‧經部分固化之樹脂
13a‧‧‧具有化學活性官能基之粗糙可結合表面
20‧‧‧可固化樹脂薄膜
21‧‧‧複合基材/第一複合基材
21a‧‧‧強化纖維
21b‧‧‧未固化或可固化基質樹脂
30‧‧‧第二複合基材
31‧‧‧黏著性薄膜
32‧‧‧可結合表面
圖1A-1B繪示根據本發明之一實施例之使用剝離層於複合基材上製造可結合表面之方法。
圖2示意性繪示根據本發明之另一實施例之複合基材,其具有表面樹脂薄膜形成於其上。
圖3繪示表面處理後之兩種複合基材之黏著性結合。
圖4係根據一個實施例之表面處理樹脂相對於標準預浸材樹脂之DSC測量值的記錄曲線。
黏著性結合已習知地用作連接複合結構(諸如彼等用於航太工業中者)之方法。目前,主要藉由以下三種方法中之一者進行複合結構之黏著性結合:(1)共固化;(2)共結合及(3)二級結合。
「共固化」涉及藉由同時固化及結合來連接未固化之複合部件,其中該等複合部件係與黏著劑一起固化,從而導致化學結合。然而,難以將此項技術應用於未固化之預浸材之結合以製造具有複雜形狀之大結構部件。未固化之複合材料(例如,預浸材)係黏性的(即,觸感黏性)且缺乏自我支撐必需之剛性。因此,未固化之複合材料難以
處理。例如,難以在具有複雜三維形狀之工具上裝配並結合未固化之複合材料。
「共結合」涉及藉由黏著性結合將經預固化之複合部件連接至未固化之複合部件,其中該黏著劑及該未固化之複合部件係在結合期間固化。該經預固化之複合部件通常在黏著性結合前需要額外之表面預處理步驟。
「二級結合」係藉由黏著性結合將經預固化之複合部件連接在一起,其中僅該黏著劑固化。此結合方法通常需要表面預處理各經預先固化之複合部件之結合表面。
用於共結合及二級結合之適當表面處理係達成黏性結合之結構中之結合線完整性之最高水準的首要條件。結合線完整性通常係指結合之表面之整體品質及穩固性。習知共結合及二級結合方法通常包括在黏著性結合前根據製造商之說明書表面處理複合結構。表面處理包括(但不限於)噴砂處理、砂磨打光、剝離層、刷底漆等。此等表面處理方法主要藉由表面之機械粗糙化來改良黏著性。經粗糙化之表面因結合界面處之機械連鎖而令黏著更佳。經預固化之複合結構之此種共結合或二級結合之局限性在於在共固化結合中結合機制僅透過機械連鎖發生而無化學鍵形成。若操作不當,則此類表面處理可在使用最終結合之結構時變為結合失敗之原因。此外,在複合物結合之裝配件之界面缺乏化學鍵形成之情況下,結合線品質之評定對確保發生適當結合係至關重要的。可惜,結合線品質之評定通常係困難的且此項技術中已知之用以量測結合線品質的當前技術非很好地適用於量測並評估弱鍵之所有可能原因。
在航太工業中,黏著劑通常與機械扣件(例如,鉚釘、螺釘及螺栓)組合使用以安全並可靠地固定結構性材料。很少使用結構性黏著劑作為連接航空器中之結構性部分之唯一機制。由經黏著性結合之部
件所提供之一些優點包括較輕重量、較少應力集中、耐久性、較低零件計數等。儘管具有此等優點,但黏著性結合之用途有限,部分係因評定結合線完整性之難度。目前,未知存在用於量測經連接之部件之結合強度之非破壞性方法。用以量測經黏著性結合之連接處之強度之唯一方法係找出最終強度,其藉由破壞該鍵來獲得。出於顯而易見之原因,此類型之破壞性測試在工業製造環境(諸如航空器之裝配)中不實用。此外,測試大量試樣以測定黏著劑之平均負載容量之驗證測試不保證各種及每種經結合之結構將具有預期之結合強度。
為滿足國家(諸如美國)之某些航空認證要求,目前要求一級結構之結構性冗餘。目前最新技術結合方法無法滿足彼等要求。目前,僅經共固化之結構才被美國聯邦航空管理局(FAA)認證為一級結構且廣泛用於航太工業中。因此,仍需要可在製造環境中用作產生可靠性及高強度化學鍵且同時提供結合線品質之極佳再現性之方法之黏著性結合方法或技術。此外,仍需要可滿足結構性冗餘要求(例如,彼等由美國FAA設定者)而不添加額外製造步驟之結合方法。
本文揭示一種表面預處理方法,其能夠產生化學活性複合表面,該表面可經由使用基於樹脂之黏著劑來化學結合至另一基材。此結合方法在複合表面與黏著劑之間產生化學鍵,導致在基材間形成更強鍵。此外,此結合方法最小化污染物對複合基材之結合表面之影響。此外,此結合方法可以工業規模實踐且對目前用於工業中之基礎結構無需作出大量改變。
本文揭示之結合方法容許藉由在待結合之表面產生化學反應性官能基,形成經共固化之結構而達成可認證之結合方法之方式。因此,本文揭示之新穎結合方法提供滿足結構性冗餘要求(例如,彼等由美國FAA設定者)而不添加額外製造步驟之方式。
前述化學活性複合表面係使用可放置於經纖維強化之樹脂基材
(或「複合基材」)上之可固化表面處理層來產生。在一個實施例中,該可固化表面處理層係富含樹脂之剝離層。圖1A-1B繪示如何使用富含樹脂之剝離層來產生具有化學活性官能基之可結合表面。參照圖1A,使可固化剝離層10首先積層於未固化或可固化複合基材11之最外表面上。該未固化/可固化複合基材由經未固化或可固化基質樹脂11b(其含有一或多種熱固性樹脂)灌注或浸漬之強化纖維11a構成。舉例而言,該等強化纖維11a可係連續單向性碳纖維。該可固化剝離層10由經不同於複合基材11之未固化/可固化基質樹脂11b之可固化基質樹脂10b灌注或浸漬之編織織物10a構成。剝離層10之基質樹脂亦含有一或多種熱固性樹脂;然而,其係經調配使得剝離層之樹脂比複合基材11之樹脂固化更慢。因此,在相同固化條件下,當複合基材11完全固化時,剝離層之樹脂僅部分固化。接著,藉由高溫加熱預定時間直至複合基材11完全固化而剝離層10僅部分固化以進行剝離層10及複合基材11之共固化。由於共固化,剝離層之基質樹脂在界面區域上與複合基質樹脂交纏或反應。控制剝離層樹脂及基材基質樹脂之固化動力學以在剝離層樹脂基材間獲得所需量之交纏物。共固化後,沿圖1A中所示之裂線12剝離該剝離層(包括其中之織物),複合基材11上留下經部分固化之樹脂13之剩餘薄膜,如圖1B中所示。在剝離期間,裂線12係處在纖維-樹脂界面,但非於織物內。因此,形成具有化學活性官能基之粗糙可結合表面13a(圖1B)。
在另一實施例中,該可固化表面處理層係如圖2中所示之可固化樹脂薄膜20(無任何織物嵌埋於其中)。在此實施例中,該可固化樹脂薄膜20係於包括經未固化或可固化基質樹脂21b灌注或浸漬之強化纖維21a的複合基材21上形成及所得結構係共固化。舉例而言,強化纖維11a可係連續單向性碳纖維。如在剝離層之情況下,該樹脂薄膜係經調配使得其比複合基材之樹脂固化更慢。因此,當複合基材完全固
化時,該表面樹脂薄膜係僅部分固化及經固化之複合基材配備具有化學活性官能基之可結合表面。
在上文實施例中,該表面處理層(剝離層/樹脂薄膜)及複合基材之共固化可在自約室溫(20℃-25℃)至約375℉(191℃)之範圍內之溫度下在自約0psi至約80psi(或約0MPa至約0.55MPa)之壓力下進行約1h至約12h。此外,共固化可在高壓釜中或藉由其中未施加外部壓力之非高壓釜(out-of-autoclave)達成。
具有上述可結合表面之第一經固化之複合基材11或21可用夾於基材之間且與該可結合表面32接觸之基於樹脂之可固化黏著性薄膜31而連接至第二複合基材30,如圖3中所示。基於樹脂之黏著性薄膜31係處於未固化或經部分固化之狀態且具有可與第一基材(11或21)之可結合表面32上之化學活性官能基反應之化學官能基。在影響結合之後續加熱處理期間,此等官能基彼此反應以形成化學鍵或共價鍵。
第二複合基材30可係經固化之複合基材,該複合基材已經受針對第一複合基材(11或21)描述之相同剝離層表面預處理以便於形成具有化學活性官能基之對應可結合表面。然後經連接之複合基材經受高溫加熱處理以使黏著劑固化,產生共價結合之結構-此稱為二級結合。黏著性薄膜31可施覆於第一及第二複合基材之任一或兩個可結合表面上。
或者,該第二複合基材30之可結合表面可由其他已知表面處理(諸如吹砂法、噴砂處理、乾剝離層表面預處理等)來製造。「乾剝離層」係通常由尼龍、玻璃或聚酯製得之乾燥編織織物(無樹脂),將其施覆至複合基材之結合表面,接著固化。固化後,移除該乾剝離層以顯示具有紋理之結合表面。
在一替代實施例中,第二複合基材30在其連接至第一經固化之複合基材(11或21)時係處於未固化狀態。在此種情況下,未固化之複
合基材30及可固化黏著性薄膜31係在後續加熱步驟中同時固化-此稱為共結合。
在根據本文揭示之方法之複合基材之共結合或二級結合期間,化學鍵或共價鍵係在存在於基於樹脂之黏著劑中之反應性部分與複合基材之可結合表面上之化學反應性官能基(其衍生自表面處理層(富含樹脂之剝離層/表面樹脂薄膜))之間形成。因此,共價結合之結構基本上無黏著劑-複合基材界面。本文描述之可結合表面上之化學活性官能基之存在藉由增加經結合之基材間之結合強度並改良結合可靠性來最佳化後續結合步驟。此外,相較於由習知共結合或二級結合方法製得之經結合之結構,共價結合之結構對污染物更具抗性。
如本文使用之術語「固化」包含由基礎成分之混合;高溫加熱;曝露於紫外光及輻射所引起之聚合材料之聚合及/或交聯。如本文使用之「完全固化」係指100%之固化度。如本文使用之「部分固化」係指小於100%之固化度。
與複合基材共固化後,經部分固化之表面處理層之固化度可在完全固化之10%-75%之範圍內,例如,25%-75%或25%-50%。經部分固化之表面處理層(剝離層/樹脂薄膜)含有未反應/非交聯之官能基,該表面係可結合表面之化學活性官能基之來源。熱固性樹脂系統之固化度可藉由微差掃描熱量法(DSC)測定。熱固性樹脂系統在固化期間經歷不可逆之化學反應。隨樹脂系統中之成分固化,樹脂釋出熱量,其藉由DSC儀器監測。可使用固化熱以測定樹脂材料之固化百分率。舉例而言,下列簡單計算可提供此資訊:固化%=[△H未固化-△H固化]/[△H未固化]X 100%
在涉及剝離層之實施例中,該剝離層基於該剝離層之總重量之至少20重量%之樹脂含量,此取決於浸漬之織物之特定類型。在某些實施例中,該樹脂含量係在約20重量%至約80重量%,或約20重量%
至約50重量%之範圍內。織物可包括玻璃、尼龍或聚酯纖維,然而本文涵蓋其他類型之織物。在一個實施例中,本發明之富含樹脂之剝離層含有(基於該剝離層之總重量之重量百分率計):約20%至約80%之熱固性基質樹脂;約2%至約20%之固化劑;及約5%至約40%之額外改性劑或填充劑添加劑。
在本文描述之實施例中,該表面處理層及該複合基材之樹脂成分係自可固化樹脂組合物形成,該組合物包括:一或多種熱固性樹脂;至少一種固化劑;及(視需要)添加劑、改性劑及填充劑。該複合基材之基質樹脂亦可包括少量熱塑性材料(諸如作為增韌劑之聚醯胺及聚醚碸)。
合適之熱固性樹脂之實例包括(但不限於)環氧樹脂、酚醛樹脂、氰酸酯、聚醯亞胺、雙馬來醯亞胺、聚酯、聚胺基甲酸酯、苯并噁嗪(包括聚苯并噁嗪)、其組合及其前驅物。
特別適合係每個分子具有複數個環氧官能基之多官能性環氧樹脂(或聚環氧化物)。該等聚環氧化物可係飽和、不飽和、環狀或非環狀、脂族、芳族或雜環聚環氧化合物。合適之聚環氧化物之實例包括藉由表氯醇或表溴醇與多酚在鹼之存在下之反應製得之聚縮水甘油醚。因此,合適之多酚係(例如)間苯二酚、鄰苯二酚、對苯二酚、雙酚A(雙(4-羥基苯基)-2,2-丙烷)、雙酚F(雙(4-羥基苯基)-甲烷)、氟4,4’-二羥基苯甲酮、雙酚Z(4,4’-環亞己基-雙酚)及1,5-羥基萘。作為聚縮水甘油醚之基礎之其他合適之多酚係苯酚與甲醛或乙醛之酚醛樹脂型已知縮合產物。
合適之環氧樹脂之實例包括雙酚A或雙酚F之二縮水甘油醚,例如,購買自Dow Chemical Co.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,例如,來自Huntsman Corp.之ARALDITE® MY 0510、MY 0500、MY 0600、
MY 0610。額外實例包括基於苯酚之酚醛環氧樹脂,購買自Dow Chemical Co.之DEN 428、DEN 431、DEN 438、DEN 439及DEN 485;基於甲酚之酚醛環氧樹脂,購買自Ciba-Geigy Corp.之ECN 1235、ECN 1273及ECN 1299;烴酚醛環氧樹脂,購買自Huntsman Corp.之TACTIX ® 71756、TACTIX ®556及TACTIX ®756。
根據一個實施例,該表面處理層之固化劑(或硬化劑)係經優先選擇以容許比複合基材之基質樹脂之固化速率更慢之固化速率。該等硬化劑可選自具有充分確定之反應性之熟知硬化劑。例如,用於環氧樹脂之按遞增固化速率之順序排列之硬化劑通常歸類為:聚硫醇<聚醯胺<脂族多胺<芳族多胺衍生物<三級胺三氟化硼錯合物<酸酐<咪唑<芳族多胺<氰基胍<酚醛樹脂。此列表僅係導引及分類內存在重疊。該表面處理層之硬化劑通常選自朝向反應順序之高端所列出之群,然而複合基材之硬化劑可通常選自朝向反應順序之開始之群。
可用於表面處理層及複合基材之硬化劑之特定實例包括(但不限於)三聚氰胺及經取代之三聚氰胺衍生物、脂族及芳族一級胺、脂族及芳族三級胺、三氟化硼錯合物、胍、二氰二胺、雙縮脲(包括2,4-甲苯雙-(二甲基脲),以CA 150購買自CVC Thermoset Specialties)、4,4’-亞甲基雙-(苯基二甲基脲),例如,購自CVC Thermoset Specialties之CA 152)及4,4’-二胺基二苯基碸(4,4-DDS)。可組合一或多種固化劑。
表1提供基於環氧之複合基材(例如,預浸材)及基於環氧之表面處理層之硬化劑配對之一些實例以達成不同固化速率。
根據另一實施例,該表面處理層之熱固性樹脂組合物含有一或多種可減慢熱固性樹脂與硬化劑間之反應速率之固化抑制劑。因此,該表面處理層可含有與彼等複合基材中者相同但因抑制劑之存在而將以較慢速率固化之熱固性樹脂及硬化劑。出於本發明之目的,可使用減慢熱固性樹脂與硬化劑間之反應速率之任何抑制劑。
就基於環氧之組合物而言,合適之固化抑制劑之實例包括(但不限於)硼酸、三氟硼烷及其衍生物(諸如硼酸烷基酯、烷基硼烷、三甲氧基硼氧烴三聚物)及具有1至3之pKa之有機酸(諸如馬來酸、水楊酸、草酸及其混合物)。其他抑制劑包括金屬氧化物、金屬氫氧化物及金屬之烷氧化物,其中該金屬係鋅、錫、鈦、鈷、錳、鐵、矽、硼或鋁。當使用此種抑制劑時,抑制劑之量在樹脂組合物中可多達約15
份/一百份樹脂或PHR,例如,約1至約5PHR。「PHR」係基於樹脂組合物中之所有樹脂之總重量。
在另一實施例中,該複合基材之基質樹脂可含有一或多種添加劑、催速劑或觸媒,其等作用係增大熱固性樹脂與其中之硬化劑間之反應速率。
可用於本文揭示之目的之觸媒係彼等催化熱固性樹脂與固化劑之反應之觸媒者。就環氧樹脂而言,合適之觸媒之實例係含有胺、膦、雜環氮、銨、鏻、砷或鋶部分之化合物。合適之觸媒係雜環含氮及含胺化合物。本文中可使用之合適之雜環含氮及含胺化合物包括(例如)咪唑、咪唑啶、咪唑啉、苯并咪唑、噁唑、吡咯、噻唑、吡啶、吡嗪、嗎啉、噠嗪、嘧啶、吡咯啶、吡唑、喹噁啉、喹唑啉、酞嗪(phthalozine)、喹啉、嘌呤、吲唑、吲哚、吲哚嗪(indolazine)、酚嗪、酚吡嗪、酚噻嗪、吡咯啉、吲哚啉、哌啶、哌嗪、其組合物及類似物。當使用此類觸媒時,觸媒量在樹脂組合物中可多達15份/一百份樹脂或PHR,例如,約1至約5PHR。
亦可向表面處理層/複合基材之樹脂組合物中添加微粒形式(例如,粉末)之無機填充劑作為流變學改性成分以控制該樹脂組合物之流動並阻止於其中聚集。合適之無機填充劑包括(但不限於)、氧化鋁、碳酸鈣、雲母、滑石、發煙二氧化矽經研磨或沉澱之白堊、石英粉、氧化鋅、氧化鈣及二氧化鈦。若存在,則樹脂組合物中之填充劑之量可基於該樹脂組合物之總重量約0.5重量%至約40重量%,或約1至約10重量%,或約1至約5重量%。
在使用富含樹脂之剝離層以進行表面處理之實施例中,該剝離層可藉由將樹脂組合物塗覆於編織織物上以便於使用習知溶劑或熱熔塗覆方法完全浸漬織物中之紡線來形成。然後容許乾燥濕剝離層以使揮發物含量(較佳)減少至小於2重量%。乾燥可藉由在室溫下空氣乾燥整
夜,接著在約140℉至約170℉下烘箱乾燥,或在必要時藉由高溫烘箱乾燥以減少乾燥時間來完成。隨後,可藉由在兩對立面上施覆可移除之剝離紙或合成薄膜(例如,聚酯薄膜)來保護經乾燥之剝離層。使用剝離層以進行表面處理前移除此類剝離紙或合成薄膜。
在使用表面樹脂薄膜以進行表面處理之實施例中,該樹脂薄膜可藉由使用習知膜塗覆方法將樹脂組合物塗覆至可移除之載劑(例如,剝離紙)上來形成。然後容許乾燥濕樹脂薄膜。隨後,將該樹脂薄膜放置於複合基材之表面上,並移除該載劑。
複合基材
本內文中之複合基材係指經纖維強化之樹脂複合基材,包括預浸材或預浸材積層(諸如彼等用於製造航太複合結構者)。如本文使用之術語「預浸材」係指已經可固化基質樹脂浸漬之纖維材料層(例如,單向性纖維束或纖維帶、非編織氈或織物層)。複合基材中之基質樹脂可處於未固化或部分固化之狀態。纖維強化材料可係編織或非編織織物層之形式或連續單向性纖維。如本文使用之「單向性纖維」係指在相同方向上對齊之強化纖維層。如本文使用之術語「預浸材疊層」係指複數個已疊合於堆疊配置中之預浸材層。例如,預浸材層之數量可係2至100層,或10至50層。
可手動或藉由自動化方法(諸如自動鋪帶(ATL))完成預浸材層之疊層。疊層中之預浸材層可以彼此相對之選定方向放置。例如,預浸材疊層可包含具有單向性纖維構築之預浸材層,其中纖維係以相對於疊層之最大維度(諸如長度)之選定角度θ(例如,0°、45°或90°)定向。應進一步瞭解,在某些實施例中,該等預浸材可具有纖維構築(諸如單向對齊之纖維、多向性纖維及編織織物)之任何組合。
預浸材可藉由用基質樹脂系統灌注或浸漬連續纖維或編織織物,產生柔韌及黏性之材料片來製造。此通常被稱為預浸過程。在該
等纖維、其定向及樹脂基材之調配之精確規格可經指定以達成預浸材之預期用途之最佳性能。亦可根據要求指定每平方米纖維體積。
術語「浸漬」係指將可固化基質樹脂材料引入強化纖維中以便於用該樹脂部分或完全囊封該等纖維。用於製造預浸材之基質樹脂可採取樹脂薄膜或液體之形式。此外,該基質樹脂在結合前係處於可固化或未固化狀態。浸漬可藉由施加熱及/或壓力來促進。
舉例而言,該浸漬方法可包括:(1)連續移動纖維層(例如,呈單向性纖維或織物網之形式)通過(加熱)之熔融浸漬基質樹脂組合物浴以完全或大體上完全浸濕該等纖維;或(2)相對於纖維層(例如,呈平行配置之連續單向性纖維或織物層之形式)按壓頂部及底部樹脂薄膜。
複合基材(例如,預浸材)中之強化纖維可採取以下形式:短切纖維、連續纖維、長絲、纖維束、纖維捆束、纖維片、纖維層及其組合。連續纖維可進一步採用以下中之任何一種:單向性(以一種方向對齊)、多向性(以不同方向對齊)、非編織、編織、針織物、縫紉物、繞絲及編結組態及渦流氈、毛氈墊及短切氈結構。編織纖維結構可包含複數個編織纖維束,每個纖維束包括複數個長絲(例如,成千上萬根長絲)。在其他實施例中,纖維束可藉由交叉牽引針、引緯編織針或少量樹脂黏合劑(諸如熱塑性樹脂)而固定。
纖維材料包括(但不限於)玻璃(包括電或E型玻璃)、碳(包括石墨)、聚芳醯胺、聚醯胺、高模數聚乙烯(PE)、聚酯、聚對伸苯基苯并噁唑(PBO)、硼、石英、玄武岩、陶瓷及其組合。
就高強度複合材料(諸如彼等用於航太及汽車應用中者)之製造而言,強化纖維較佳具有大於3500MPa之抗張強度。
通常,複合基材/預浸材之基質樹脂類似於上述表面處理層之基
質樹脂。
黏著劑
用於結合複合基材之黏著劑係適用於與未固化或可固化複合基材共固化之可固化組合物。該可固化黏著劑組合物可包含一或多種熱固性樹脂、固化劑及/或觸媒及(視需要)增韌劑、填充劑、流動控制試劑、染料等。該等熱固性樹脂包括(但不限於)環氧樹脂、不飽和聚酯樹脂、雙馬來醯亞胺、聚醯亞胺、氰酸酯、酚醛樹脂等。
可用於該可固化黏著劑組合物中之環氧樹脂可包括每個分子具有複數個環氧基團之多官能環氧樹脂,諸如彼等針對剝離層及複合基材之基質樹脂揭示者。
該等固化劑可包括(例如)胍(包括經取代之胍)、脲(包括經取代之脲)、三聚氰胺樹脂、胍胺、胺(包括一級及二級胺、脂族及芳族胺)、醯胺、酐及其混合物。特別合適係可在大於160℉(71℃)或大於200℉之溫度(例如,350℉)下活化之基於胺之潛伏性固化劑。合適之基於胺之潛伏性固化劑之實例包括二氰二胺(DICY)、胍胺、胍、胺胍及其衍生物。特別合適之基於胺之潛伏性固化劑係二氰二胺(DICY)
固化催速劑可結合基於胺之潛伏性固化劑使用以促進環氧樹脂與基於胺之固化劑間之固化反應。合適之固化催速劑可包括經烷基及芳基取代之脲(包括芳族或脂環族二甲基脲);基於甲苯二胺或亞甲基二苯胺之雙縮脲。雙縮脲之實例係2,4-甲苯雙(二甲基脲)。舉例而言,二氰二胺可與作為催速劑之經取代之雙縮脲組合使用。
增韌劑可包括熱塑性或彈性聚合物及聚合微粒(諸如核殼橡膠(CSR)微粒)。合適之熱塑性聚合物包括具有或不具有反應性官能基之聚芳碸。具有官能基之聚芳碸之實例包括(例如)具有末端胺基官能基之聚醚碸-聚醚醚碸(PES-PEES)共聚物。合適之彈性聚合物包括羧基封端之丁二烯腈聚合物(CTBN)及胺基封端之丁二烯丙烯腈(ATBN)彈
性物。CSR微粒之實例包括彼等以商標Kane Ace®購買獲得者,諸如MX 120、MX 125及MX 156(全部含有25重量%CSR微粒分散於液體雙酚A環氧樹脂中)。
無機填充劑可係呈微粒形式(例如,粉末、薄片)及可選自發煙二氧化矽石英粉、氧化鋁、雲母、滑石及黏土(例如,高嶺土)。
實例
提供下列實例以闡述本發明之某些態樣。
實例1
此實例證實基於受控固化動力學之概念之表面處理的效應。
藉由製造含有以下各物(以重量份計)之樹脂調配物來形成表面處理薄膜:50份含有二環戊二烯之酚醛環氧樹脂;80份雙酚A之二縮水甘油醚;10份對胺基苯酚環氧樹脂;10份聚(醚)碸;39份4,4’-二胺基二苯基碸;及2份發煙二氧化矽。
使用熱熔法混合樹脂混合物,接著以0.054psf(磅每平方英尺)將該樹脂混合物塗覆成無支撐薄膜。手動疊合該樹脂薄膜與10層預浸材材料,使得該樹脂薄膜為最頂層。該預浸材材料包括經含有以下各物之基於環氧之基質樹脂浸漬的玻璃纖維:經彈性物改性之雙A環氧樹脂、經酚醛改性之環氧樹脂、二氰基胍及1,1’-4(甲基間伸苯基)雙(3,3’-二甲基脲)。然後在250℉下在80psi下加熱3小時以使具有樹脂薄膜之未固化之積層固化。固化後,經固化之複合體具有可結合表面。自工具上移除經固化之複合積層並與另一以類似方法製得之已經受相同表面處理之經固化之複合積層連接。結合步驟不使用黏著劑且僅表面處理官能基可用於結合。然後在350℉下在80psi下將經連接之物件加熱90min。
實例2
下列實例比較顯示不含有緩慢固化表面處理薄膜之表面處理之
效應。
藉由製造含有以下各物(以重量份計)之樹脂調配物來形成表面處理薄膜:50份含有二環戊二烯之酚醛環氧樹脂;80份雙酚A之二縮水甘油醚;10份對胺基苯酚環氧樹脂;10份聚(醚)碸;29份4,4’-二胺基二苯基碸;2份二氰二胺;及2份發煙二氧化矽。
使用熱熔法混合樹脂混合物,接著以0.054psf將該樹脂混合物塗覆成無支撐薄膜。手動疊合該樹脂薄膜與10層預浸材材料,使得該樹脂薄膜為最頂層。該預浸材材料與描述於實例1中之預浸材材料相同。然後藉由在250℉下在80psi下加熱3小時使該未固化之積層固化。固化後,經固化之複合體具有可結合表面。自工具上移除經固化之複合體並與另一以類似方法製得之含有相同可結合表面之經固化之複合積層連接。結合步驟不使用黏著劑且僅表面處理官能基可用於結合。然後在350℉下在80psi下將經連接之物件加熱90min。
實例3
下列實例證實涉及使用可移除剝離層以改良表面粗糙度並促進結合之表面處理。
藉由製造含有以下各物(以重量份計)之樹脂調配物來形成表面處理層:50份含有二環戊二烯之酚醛環氧樹脂;80份雙酚A之二縮水甘油醚;10份對胺基苯酚環氧樹脂;10份聚(醚)碸;19份4,4’-二胺基二苯基碸;及2份發煙二氧化矽。
使用熱熔法混合樹脂混合物,接著將該樹脂混合物塗覆於來自Porcher Industries之基於聚酯之織物(Porcher 8115)上以浸漬該織物,及容許乾燥經樹脂浸漬之織物,從而形成剝離層。手動疊合該剝離層與10層預浸材材料,使得該剝離層為最頂層。該預浸材材料包括經含有以下各物之基於環氧之基質樹脂浸漬之碳纖維:基於亞甲基二苯胺之四官能環氧樹脂;基於間胺基苯酚之三官能環氧樹脂;聚醚碸;
3,3’-二胺基-二苯基碸及間苯二甲酸二醯肼(催速劑)。然後藉由在350℉下在80psi下加熱3小時使未固化之複合積層固化。固化後,自工具上移除經固化之複合體,移除剝離層,並與另一以類似方法製得之已經受與剝離層相同之表面處理之經固化之複合積層連接。使用之黏著劑係FM 309-1(購買自Cytec Engineered Materials)。然後在350℉下在40psi下將經連接之物件加熱90min以達成固化。
經結合之結構之機械性質及表徵
藉由根據ASTM D5528完成之G1c破裂韌性測試確定實例1至3中製得之經結合之結構之機械性能。該等G1c結果顯示於表2中。
相較於其中硬化劑引起表面處理樹脂之完全固化之表面處理,表2藉由證實達成經改良之結合強度顯示本發明之表面處理之優點。
熱表徵
表面處理層之固化速率與基礎預浸材材料之固化速率之比較可藉由微差掃描熱量法(DSC)容易評定。圖4顯示揭示於實例3中之預浸材材料及表面處理層之DSC曲線。如可自圖4中看出,表面處理樹脂之開始固化溫度高於預浸樹脂之開始固化溫度。在此特定實施例中,該預浸材材料開始經歷固化並以高於表面處理層之速率之速率消耗反應性環氧樹脂官能基。因此,預浸材材料完全固化後,表面處理樹脂處於部分固化狀態且含有未反應之官能基。
11‧‧‧第一複合基材
21‧‧‧第一複合基材
30‧‧‧第二複合基材
31‧‧‧黏著性薄膜
32‧‧‧可結合表面
Claims (28)
- 一種在黏著性結合前進行表面預處理之方法,其包括:(a)提供包含經第一可固化基質樹脂浸漬之強化纖維之複合基材;(b)將表面處理層施覆於該複合基材之表面上,該表面處理層包含不同於該第一基質樹脂之第二可固化基質樹脂;(c)使該複合基材及該表面處理層共固化,直至該複合基材完全固化而該表面處理層保持部分固化,其中該第二基質樹脂係經調配以比該第一基質樹脂更慢之速率固化,及共固化(c)後,該表面處理層提供具有化學活性之官能基之可結合表面。
- 如請求項1之方法,其中該表面處理層係樹脂薄膜,其不包含織物或強化纖維嵌埋於其中。
- 如請求項1之方法,其中該表面處理層包含經該第二可固化基質樹脂灌注之編織織物,及共固化(c)後,自該複合基材之表面移除該表面處理層,在該複合基材之表面上留下部分固化之基質樹脂之薄膜,該薄膜提供具有化學活性官能基之粗糙可結合表面。
- 如請求項1之方法,其中該等第一及第二可固化基質樹脂包含一或多種多官能環氧樹脂。
- 如請求項1之方法,其中該等第一及第二基質樹脂包含經選擇以不同速率影響固化之不同固化劑。
- 如請求項5之方法,其中該等第一及第二基質樹脂包含一或多種環氧樹脂,用於該等第一及第二基質樹脂之固化劑係選自由以下各物組 成之群:三聚氰胺及經取代之三聚氰胺衍生物、聚硫醇、聚醯胺、脂族多胺、芳族多胺衍生物、三級胺三氟化硼錯合物、酸酐、咪唑、芳族多胺、氰基胍、酚醛樹脂,及用於該第一及第二可固化基質樹脂之固化劑係經選擇以能夠使該第一基質樹脂相對於該第二基質樹脂以更快速率固化。
- 如請求項6之方法,其中該第一基質樹脂包含1,3-雙(4-胺基苯氧基)苯,且該第二基質樹脂包含4,4’-二胺基二苯基碸或(3-(4-胺基苯甲醯基)氧基苯基)-4-胺基苯甲酸酯,作為固化劑。
- 如請求項6之方法,其中該第一基質樹脂包含4,4’-二胺基二苯基碸或3,3’-二胺基二苯基碸,且該第二基質樹脂包含三聚氰胺,作為固化劑。
- 如請求項6之方法,其中該第一基質樹脂包含4,4’-二胺基二苯基碸與二氰基胍之組合,且該第二基質樹脂包含4,4’-二胺基二苯基碸或三聚氰胺,作為固化劑。
- 如請求項6之方法,其中該第一基質樹脂包含3,3’-二胺基二苯基碸,且該第二基質樹脂包含4,4’-二胺基二苯基碸,作為固化劑。
- 如請求項6之方法,其中該第一基質樹脂包含雙苯胺M,且該第二基質樹脂包含4,4’-二胺基二苯基碸,作為固化劑。
- 如請求項6之方法,其中該第一基質樹脂包含4,4’-二胺基二苯基碸,且該第二基質樹脂包含(3-(4-胺基苯甲醯基)氧基苯基)-4-胺基苯甲酸酯,作為固化劑。
- 如請求項6之方法,其中該第一基質樹脂包含雙苯胺P,且該第二基質樹脂包含3,3’-二胺基二苯基碸,作為固化劑。
- 如請求項6之方法,其中該第一基質樹脂包含3,3’-二胺基二苯基碸與間苯二甲酸二醯肼之組合,且該第二基質樹脂包含三聚氰胺,作為固化劑。
- 如請求項1之方法,其中該第二可固化基質樹脂包含一或多種熱固性樹脂、固化劑及可減慢該第二基質樹脂中該等一或多種熱固性樹脂與該固化劑間之反應速率之抑制劑。
- 如請求項15之方法,其中該抑制劑係選自由以下各物組成之群:硼酸;三氟硼烷;硼酸烷基酯;烷基硼烷;三甲氧基硼氧烴三聚物;具有1至3之pKa之有機酸,包括馬來酸、水楊酸、草酸;金屬氧化物;金屬氫氧化物及金屬之烷氧化物,其中該金屬係選自:鋅、錫、鈦、鈷、錳、鐵、矽、硼或鋁;及其組合。
- 如請求項1之方法,其中該第一可固化基質樹脂包含一或多種熱固性樹脂、固化劑及可提高該等一或多種熱固性樹脂與該固化劑間之反應速率之催速劑。
- 如請求項17之方法,其中該第一基質樹脂包含一或多種環氧樹脂且該催速劑係選自含有以下各物之化合物:胺、膦、雜環氮、銨、鏻、砷或鋶部分。
- 如請求項17之方法,其中該第一基質樹脂包含一或多種環氧樹脂且該催速劑係選自由以下各物組成之群:苯并咪唑、咪唑、咪唑啶、咪唑啉、噁唑、吡咯、噻唑、吡啶、吡嗪、嗎啉、噠嗪、嘧啶、吡咯啶、吡唑、喹噁啉、喹唑啉、酞嗪(phthalozine)、喹啉、嘌呤、吲唑、吲哚、吲哚嗪(indolazine)、酚嗪、酚吡嗪、酚噻嗪、吡咯啉、吲哚啉、哌啶、哌嗪及其組合。
- 一種固化之複合基材,其具有藉由如請求項1之方法製得之具有化學活性官能基之可結合表面。
- 一種結合方法,其包括:(a)提供包含經第一可固化基質樹脂浸漬之強化纖維之第一複 合基材;(b)將富含樹脂之可移除剝離層施覆於該第一複合基材之表面上,該剝離層包含經第二可固化基質樹脂灌注或浸漬之編織織物,該第二可固化基質樹脂係經調配以比該第一可固化基質樹脂更慢之速率固化;(c)使該第一複合基材及該剝離層共固化,直至該第一複合基材完全固化而該剝離層中之該第二基質樹脂保持部分固化;(d)自該第一複合基材之表面移除該剝離層,在該第一複合基材之表面上留下部分固化之第二基質樹脂之薄膜,該薄膜提供具有化學活性官能基之粗糙可結合表面;(e)用該等複合基材間之可固化黏著性薄膜使該固化之第一複合基材連接至第二複合基材,其中該可固化黏著性薄膜包含可與該第一複合基材之可結合表面上之化學活性官能基反應之化學活性官能基;及(f)使該黏著性薄膜固化以形成共價結合之結構。
- 如請求項21之結合方法,其中該第二複合基材在連接至該固化之第一複合基材前係固化。
- 如請求項21之結合方法,其中該第二複合基材在連接至該第一複合基材前係未固化或部分固化,及在(f)之固化期間,該黏著性薄膜及該第二複合基材係同時固化。
- 如請求項21之結合方法,其中該等第一及第二可固化基質樹脂包含經選擇以不同速率影響固化之不同固化劑。
- 一種結合方法,其包括:(a)提供包含經第一可固化基質樹脂灌注或浸漬之強化纖維之第一複合基材;(b)將樹脂薄膜施覆於該第一複合基材之表面上,該樹脂薄膜 係自第二可固化基質樹脂形成,該第二可固化基質樹脂係經調配以比該第一可固化基質樹脂更慢之速率固化;(c)使該第一複合基材及該樹脂薄膜共固化,直至該第一複合基材完全固化而該樹脂薄膜保持部分固化,從而提供具有化學活性官能基之可結合表面;(e)用該等複合基材間之可固化黏著性薄膜使該固化之第一複合基材連接至第二複合基材,其中該可固化黏著性薄膜包含可與該第一複合基材之可結合表面上之化學活性官能基反應之化學活性官能基;及(f)使該黏著性薄膜固化以形成共價結合之結構。
- 如請求項25之結合方法,其中該第二複合基材在連接至該固化之第一複合基材前係固化。
- 如請求項25之結合方法,其中該第二複合基材在連接至該第一複合基材前係未固化或部分固化,及在(f)之固化期間,該黏著性薄膜及該第二複合基材係同時固化。
- 如請求項25之結合方法,其中該等第一及第二可固化基質樹脂包含經選擇以不同速率影響固化之不同固化劑。
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RU2017119030A (ru) | 2018-12-05 |
US9789646B2 (en) | 2017-10-17 |
US20160121591A1 (en) | 2016-05-05 |
AU2015343586A1 (en) | 2017-05-04 |
CN107207749A (zh) | 2017-09-26 |
AU2015343586B2 (en) | 2019-05-09 |
KR20170081663A (ko) | 2017-07-12 |
JP6660397B2 (ja) | 2020-03-11 |
TWI652171B (zh) | 2019-03-01 |
CN107207749B (zh) | 2021-03-16 |
EP3227363A1 (en) | 2017-10-11 |
RU2708209C2 (ru) | 2019-12-04 |
EP3227363B1 (en) | 2020-10-07 |
BR112017009032A2 (pt) | 2018-02-06 |
ES2842278T3 (es) | 2021-07-13 |
BR112017009032B1 (pt) | 2021-10-26 |
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