TW201429691A - 複合材料之結合 - Google Patents

複合材料之結合 Download PDF

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Publication number
TW201429691A
TW201429691A TW102142725A TW102142725A TW201429691A TW 201429691 A TW201429691 A TW 201429691A TW 102142725 A TW102142725 A TW 102142725A TW 102142725 A TW102142725 A TW 102142725A TW 201429691 A TW201429691 A TW 201429691A
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Taiwan
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composite
prepreg
curing
adhesive
bonding
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TW102142725A
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English (en)
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Leonard A Macadams
Dalip K Kohli
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Cytec Ind Inc
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Publication of TW201429691A publication Critical patent/TW201429691A/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • 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
    • B29C70/30—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
    • B29C65/4805—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding characterised by the type of adhesives
    • B29C65/483—Reactive adhesives, e.g. chemically curing adhesives
    • B29C65/4835—Heat curing adhesives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
    • B29C65/52—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding characterised by the way of applying the adhesive
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/72—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the structure of the material of the parts to be joined
    • B29C66/721—Fibre-reinforced materials
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/73—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset
    • B29C66/737—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the state of the material of the parts to be joined
    • B29C66/7375—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the state of the material of the parts to be joined uncured, partially cured or fully cured
    • B29C66/73753—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the state of the material of the parts to be joined uncured, partially cured or fully cured the to-be-joined area of at least one of the parts to be joined being partially cured, i.e. partially cross-linked, partially vulcanized
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    • B29C66/73—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset
    • B29C66/739—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of the parts to be joined being a thermoplastic or a thermoset
    • B29C66/7394—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of at least one of the parts being a thermoset
    • B29C66/73941—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of at least one of the parts being a thermoset characterised by the materials of both parts being thermosets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • 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
    • B29C70/06—Fibrous reinforcements only
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
    • C09J5/02—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving pretreatment of the surfaces to be joined
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
    • B29C65/14—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
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    • B29C65/1403—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation characterised by the type of electromagnetic or particle radiation
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/71—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the composition of the plastics material of the parts to be joined
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/72—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the structure of the material of the parts to be joined
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    • B29C66/7212—Fibre-reinforced materials characterised by the composition of the fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/72—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the structure of the material of the parts to be joined
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    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
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    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/73—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset
    • B29C66/731—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the intensive physical properties of the material of the parts to be joined
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    • C09J2400/00—Presence of inorganic and organic materials
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    • F16B11/00—Connecting constructional elements or machine parts by sticking or pressing them together, e.g. cold pressure welding
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  • General Engineering & Computer Science (AREA)
  • Reinforced Plastic Materials (AREA)
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Abstract

本發明揭示一種複合結合方法。將兩個基於樹脂之可固化複合基板中之至少一者部分地固化至至少10%但小於75%完全固化之固化程度。然後使用該等複合基板之間之可固化黏著劑使其彼此接合。對該等接合基板實施共固化以形成結合之複合結構，藉此該黏著劑以化學方式結合至且以機械方式擴散有該等複合基板之樹脂基質，從而在該黏著劑與每一複合基板之間得到化學結合界面。另外，結合可在接合表面上存在污染物下發生。

Description

複合材料之結合
纖維增強之聚合複合物係高性能結構材料，其已用於製作需要高強度及/或低重量及抗侵蝕環境性之結構部件。該等結構部件之實例包含飛機組件(例如尾、翼、機身、螺旋槳)、汽車部件、風刃等。纖維會增強基質樹脂，從而承受由複合物支撐之大部分負荷，而樹脂基質承受由複合物支撐之小部分負荷且亦將負荷自破裂纖維轉移至完整纖維。以此方式，該等聚合複合物可支撐大於基質樹脂或纖維可單獨支撐之負荷的負荷。另外，藉由以特定幾何形狀或定向修整增強纖維，可有效設計複合物以最小化重量及體積。
黏著結合在傳統上用作在製造一級及二級飛機結構中接合結構組件之方法。通常，組合使用結構黏著劑與機械緊固件(例如鉚釘、螺絲及螺栓)以安全且可靠地固定結構材料。除二級組件之情形外，很少使用結構黏著劑作為接合結構部件之唯一機制。黏著結合部件展現優於藉由機械緊固件接合之部件之顯著優點，包含：較輕重量、減小之應力集中、耐久性、較低部件計數等。然而，在航空工業中廣泛使用結構黏著劑面臨由黏著結合接點之可靠性及結合線品質問題所致之較大阻礙。為增加黏著劑之使用以作為唯一結合主源，需要證實可在製造環境中使用膜黏著劑作為產生具有特殊結合線品質再現性之可靠結合之方法。
本文揭示B階化結合方法，其容許在無需單獨表面製備步驟下來結合複合基板。
圖1展示CYCOM 5320-1基於環氧之樹脂之差示掃描熱量測定計(DSC)分析。
圖2展示CYCOM 5320-1基於環氧之樹脂在275℉、300℉及325℉下之DSC跡線。
圖3展示CYCOM 5320-1基於環氧之樹脂在250℉下之DSC跡線。
圖4係展示藉由階化結合形成之結合結構之界面之顯微影像。
圖5係展示二級結合結構之界面之顯微影像。
對於接合由纖維增強之聚合複合物製得之複合部件而言，習用黏著結合方法包含共固化、共結合及二級結合。
「二級結合」係藉由黏著結合將預固化複合部件接合至一起，其中僅黏著劑發生固化。此結合方法通常需要在結合表面處表面製備每一先前固化之複合部件。表面製備通常由以下部分組成：施加剝離夾層、使用研磨介質噴粒、電漿處理或一些產生結合位點以促進黏著劑與複合物之間之機械聯鎖之其他製程。舉例而言，在預固化複合部件之金屬結合及二級結合(此係用於飛機制造之典型結合製程)中，黏著劑主要經由機械聯鎖機制進行結合，其中黏著劑流入複合物表面處之微通道中，且以機械方式使黏附體彼此固定。
「共結合」涉及藉由黏著結合將預固化複合部件接合至未固化複合部件，其中黏著劑及未固化複合部件在結合期間同時固化。如上述二級結合中所闡述，預固化複合物在黏著結合之前需要額外表面製備步驟。此結合方法之缺點在於，預固化複合物並不以化學方式結合至黏著劑且未固化預浸體複合物可難以處置及成型為複雜部件。
「共固化」涉及藉由同時固化及結合來接合未固化複合部件，其中複合部件與黏著劑一起固化，從而得到化學結合。然而，難以應用此技術來結合未固化預浸體以製作具有複雜形狀之較大結構部件。未固化預浸體難以處置且缺乏自支撐所需之剛性。因此，難以在具有複雜三維形狀之工具上組裝及結合未固化預浸體。
在工業中眾所周知，脫模材料係常見污染物，其可破壞黏著結合機制且導致在複合結構中之結合接點處損失強度。脫模材料(例如天然或合成材料，包含聚矽氧、礦物油、蠟、脂肪酸衍生物、二醇、氟化烴等)通常形成於模具上以用於促進模製層壓結構自形成其之模具之釋放。出於此原因以及為消除來自其他材料之污染之可能，在黏著結合之前對複合基板實施表面製備處理以增加機械粗糙度及/或清洗表面之污染物。表面製備通常由以下部分組成：施加剝離夾層、噴粒或一些產生結合位點以促進黏著劑與複合物之間之機械聯鎖之其他製程。
在並無化學結合下，在結合接點負載剝離力或在長時間段內暴露於環境下或處於此兩種情形下時，存在所謂的「弱結合」條件。黏著失效指示在基板與黏著材料之間缺乏化學結合，其可視為所有測試類型中之不可接受之失效模式。期望研發將黏著膜完全整合至複合結構中從而藉由形成化學鍵來產生連續「無黏著劑」結構(亦即在界面區域處並無明晰黏著層)之結合技術。
已發現，在黏著結合之前將可固化或未固化複合基板階化至特定固化等級(至少10%但小於75%、較佳地25%-70%或25%-50%或40%-60%)會致使複合基板免於污染(例如脫模化學物質)，且容許進行無需習用表面製備之結合製程。在某些階化等級(至少10%但小於75%)下，複合基板展現用於組裝目的之足夠剛性，但其中之基質樹脂能夠在最終固化/黏著結合期間發生彈性變形。因基質樹脂在階化之後並 未完全固化，故在最終固化階段期間基質樹脂材料與黏著劑之間可發生化學結合及交纏，由此在複合基板之間之界面處得到改良之物理及化學結合。
本文所揭示之階化結合製程係附加於任一可在製造個別預浸體期間實施之先前部分固化。若在預浸體製造期間部分地固化，則用於習用預浸體之固化等級通常小於10%。在該低固化等級下，預浸體仍具有高黏著及懸垂特性且並無剛性。
擬藉由本文所揭示階化結合製程結合之初始複合基板係由嵌入或浸漬有可固化基質樹脂之增強纖維構成之基板。在一實施例中，可固化(包含未固化)複合基板係選自未固化或可固化預浸體及預浸體疊層。此背景中所用之術語「可固化」係指未固化條件或具有小於10%之固化等級。
本文所揭示之結合方法係經由複合基板之B階段固化在複合基板與黏著劑之間產生共價化學鍵的易用方法。此方式能夠組合化學結合(經由共固化結合達成)與二級結合之處理優點。
另外，階化操作在結合之前穩定複合物之基質樹脂，由此改良複合材料之處置及組裝。階化有助於將材料之玻璃轉變溫度(Tg)升至足夠高以使得延長階化複合基板之室溫儲存。測試已指示，完全固化之結合基板展現改良之機械性質，例如高搭接剪切強度。
根據一實施例，本揭示內容之B階化結合製程可包括：a)提供至少兩個未固化複合基板，每一複合基板包括浸漬有可固化聚合樹脂基質之織造或非織造增強纖維；b)將複合基板部分地固化至至少10%但小於75%完全固化(例如25%-70%)之固化程度；c)在複合基板中之至少一者上施加可固化黏著劑；d)使用複合基板之間之黏著劑使基板彼此接合；及 e)完全共固化接合基板以形成在所有成份之間含有化學鍵之完全結合之複合結構。
在完全固化後，黏著劑以化學方式結合至且以機械方式擴散有複合基板之聚合樹脂基質，從而在黏著劑與每一複合基板之間得到化學結合界面。在一較佳實施例中，在未固化複合基板並無任何中間表面處理下實施步驟(a)-(d)以產生紋理化表面或增加/影響表面形態。
本文所用之「表面製備」係指產生結合位點以促進黏著劑與複合基板之間之機械聯鎖之表面處理，例如施加剝離夾層、噴粒、電漿暴露或一些以物理方式改質/粗糙化/紋理化表面之其他製程。
發生於部分地固化之複合基板與黏著劑之間之「化學鍵形成」定義如下：在存在於黏著劑基質中之反應性部分與複合物基質中之化學反應性基團之間形成鍵。該等化學鍵形成於存在於黏著劑及複合物基質中之反應性成份之間。舉例而言，在複合基板之基質樹脂及黏著劑含有環氧樹脂及胺固化劑時，可自複合物基質樹脂中之環氧化物基團與黏著劑中之胺基團之反應形成共價鍵且反之亦然。
本文所用之術語「固化(cure及curing)」涵蓋聚合材料之聚合及/或交聯。可藉由各種製程(包含但不限於加熱、暴露於紫外光及暴露於輻射)來實施固化。
可藉由使用差示掃描熱量測定(DSC)來測定B階化之部分固化程度(或等級)。可藉由以等溫方式或以動態方式將複合材料在指定溫度下加熱設定時間來量測DSC。維持溫度直至複合材料完全固化為止。對反應峰之放熱熱進行積分使得可在溫度下時間與固化程度之間建立直接關聯。
複合基板及預浸體
此背景中之複合基板係指纖維增強之樹脂複合物，包含預浸體或預浸體疊層(例如彼等用於製備航空複合結構者)。本文所用之術語 「預浸體」係指浸漬有可固化基質樹脂之纖維材料層(例如單向紗束或膠帶、非織造氈或織物夾層)。本文所用之術語「預浸體疊層」係指以堆疊配置安置之複數個預浸體夾層。可人工或藉由自動化製程(例如自動化膠帶安置(ATL))來實施安置製程。疊層內之預浸體夾層可相對於彼此以所選定向進行定位。舉例而言，預浸體疊層可包括具有單向纖維構造之預浸體夾層，其中纖維相對於疊層之最大尺寸(例如長度)以所選角度((例如0°、45°或90°)進行定向。應進一步理解，在某些實施例中，預浸體可具有纖維構造(例如單向纖維、多向纖維及織造織物)之任一組合。
可藉由使用基質樹脂系統灌注或浸漬連續纖維或織造織物從而產生材料之柔韌及黏性片材來製造預浸體。此通常稱為預浸製程。可指定纖維之確切規格、其定向及樹脂基質之調配物以達成用於預期預浸體用途之最佳性能。亦可根據需求指定每平方米之纖維體積。
在預浸時，使用基質樹脂以受控方式浸漬增強纖維且然後冷凍以抑制樹脂之聚合。然後運送經冷凍預浸體且儲存於冷凍條件下直至需要時為止。在自預浸體製造複合部件時，將預浸體解凍至室溫，切割至適當大小，且在模製工具上組裝。在置於適當位置後，在壓力下將預浸體固結及固化以達成具有最少空隙之所需纖維體積分數。
本文所用之術語「浸漬」係指將可固化基質樹脂材料引入增強纖維中以使用樹脂部分地或完全囊封纖維。用於製備預浸體之基質樹脂可採取樹脂膜或液體之形式。另外，基質樹脂在結合之前呈可固化/未固化狀態。可藉由施加熱及/或壓力來促進浸漬。
作為實例，浸漬方法可包含：(1)連續移動纖維穿過熔融浸漬基質樹脂組合物之(加熱)浴以完全或實質上完全浸濕纖維；或(2)抵靠平行或以織物夾層形式配置之連續單向纖維壓製頂部 及底部樹脂膜。
增強纖維
用於製作複合基板(或預浸體)之增強纖維可採取以下形式：短切纖維、連續纖維、絲、紗束、束、片材、夾層及其組合。連續纖維可進一步採用單向(在一個方向上對準)、多向(在不同方向上對準)、非織造、織造、針織、縫合、捲繞及編織組態以及捲毛玻璃氈、氈墊及短切氈結構中之任一者。織造纖維結構可包括複數條織造紗束，每一紗束由複數條絲(例如數千條絲)構成。在其他實施例中，紗束可藉由跨紗束縫線、緯編***針織縫線或少量樹脂黏合劑(例如熱塑性樹脂)保持於適當位置。
纖維組合物包含但不限於玻璃(包含電氣玻璃或E-玻璃)、碳、石墨、芳族聚醯胺、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。
為製作高強度複合材料(例如用於航空及汽車應用)，增強纖維較佳具有大於3500MPa之拉伸強度。
基質樹脂
通常，樹脂基質含有一或多種熱固性樹脂作為主要組份與少量添加劑之組合，該等添加劑係(例如)固化劑、觸媒、共單體、流變性控制劑、增黏劑、流變性改良劑、無機或有機填充劑、熱塑性或彈性體增韌劑、穩定劑、抑制劑、顏料/染料、阻燃劑、反應性稀釋劑及彼等熟習此項技術者熟知用於在固化之前或之後修改樹脂基質之性質之其他添加劑。
熱固性樹脂可包含但不限於環氧樹脂、不飽和聚酯樹脂、雙馬來醯亞胺、聚醯亞胺、氰酸酯、酚系物等。在一實施例中，樹脂基質係基於環氧之樹脂調配物，其含有一或多種多官能環氧樹脂(亦即聚環氧化物)作為主要聚合組份。
適宜環氧樹脂包含芳族二胺、芳族單一級胺、胺基酚、多元酚、多元醇、多羧酸之聚縮水甘油基衍生物。適宜環氧樹脂之實例包含雙酚(例如雙酚A、雙酚F、雙酚S及雙酚K)之聚縮水甘油基醚；及基於甲酚及苯酚之酚醛樹脂之聚縮水甘油基醚。
添加固化劑及/或觸媒可增加固化速率及/或降低基質樹脂之固化溫度。熱固性樹脂之固化劑適宜地選自已知固化劑，例如胍(包含經取代胍)、脲(包含經取代脲)、三聚氰胺樹脂、胍胺衍生物、胺(包含一級及二級胺、脂肪族及芳族胺)、醯胺、酐(包含多羧酸酐)及其混合物。
增韌劑可包含熱塑性及彈性體聚合物及聚合顆粒(例如核-殼橡膠顆粒、聚醯亞胺顆粒、聚醯胺顆粒)。
無機填充劑可包含發菸二氧化矽、石英粉末、氧化鋁、扁平狀填充劑(例如雲母)、滑石粉或黏土(例如高嶺土)。
黏著劑
用於結合複合基板之黏著劑係適於與未固化複合基板共固化之可固化組合物。可固化黏著劑組合物可包括一或多種熱固性樹脂、固化劑及/或觸媒及視情況增韌劑、填充劑材料、流動控制劑、染料等。熱固性樹脂包含但不限於環氧樹脂、不飽和聚酯樹脂、雙馬來醯亞胺、聚醯亞胺、氰酸酯、酚系物等。
可用於可固化黏著劑組合物之環氧樹脂包含每分子具有複數個環氧基團之多官能環氧樹脂，例如彼等針對基質樹脂所揭示者。
固化劑可包含(例如)胍(包含經取代胍)、脲(包含經取代脲)、三聚氰胺樹脂、胍胺衍生物、胺(包含一級及二級胺、脂肪族及芳族胺)、醯胺、酐及其混合物。適宜固化劑包含基於胺之潛伏性固化劑，其可在大於160℉(71℃)、較佳地大於200℉(例如350℉)之溫度下活化。適宜基於胺之潛伏性固化劑之實例包含二氰二胺(DICY)、胍 胺、胍、胺基胍及其衍生物。尤其適宜之基於胺之潛伏性固化劑係二氰二胺(DICY)。
固化加速劑可與基於胺之潛伏性固化劑結合使用以促進環氧樹脂與基於胺之固化劑之間的固化反應。適宜固化加速劑可包含經烷基及芳基取代之脲(包含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脲。雙脲之一實例係2,4-甲苯脲(二甲基脲)。作為實例，二氰二胺可與與經取代雙脲(作為固化加速劑)組合使用。
增韌劑可包含熱塑性或彈性體聚合物及聚合顆粒(例如核-殼橡膠顆粒)。無機填充劑可包含發菸二氧化矽、石英粉末、氧化鋁、扁平狀填充劑(例如雲母)、滑石粉或黏土(例如高嶺土)。
在一實施例中，黏著劑係在高於200℉(93℃)(例如350℉(176.7℃))之溫度下可固化之基於環氧之組合物。
結合結構
在一實施例中，將複數個未固化或可固化預浸體夾層(具有小於10%之固化程度)安置於工具上且部分地固化至25%-75%之固化等級，由此形成第一B階化預浸體疊層。工具可具有非平面三維模製表面以用於將預浸體成型為期望組態。模製表面可塗覆有脫模材料(例如基於矽之膜)。亦以相同方式形成第二B階化預浸體疊層。接下來，以黏著方式使B階化疊層彼此接合，其中工具側彼此面對且其間存在可固化黏著膜。然後將所得總成固化以形成整合複合結構。預浸體疊層中之基質樹脂及黏著劑在此最終固化步驟中同時完全固化。應指出，將B階化預浸體疊層直接自工具取出用於結合而並無任何中間表面改質處理。
在另一實施例中，將複數個未固化預浸體夾層安置於工具上且部分地固化至25%-75%之固化等級，由此形成第一B階化預浸體疊層。工具可具有非平面三維模製表面以用於將預浸體成型為期望組 態。模製表面可塗覆有脫模材料(例如基於矽之膜)。然後使B階化疊層以黏著方式接合至未固化預浸體夾層或預浸體疊層，其中疊層之工具側面向未固化預浸體夾層/疊層。在完全固化後，以化學方式結合所得總成。
可藉由一起或單獨使用高壓釜(加熱壓力器皿)或非高壓釜製程或任一施加熱及壓力之其他習用製程來實施如本文所揭示黏著結合之複合基板或預浸體壓層之固化結合。
作為實例，可使用真空袋設置進行該固化結合。在此設置中，將複合壓層組裝於工具上，將真空袋置於整個複合壓層上方且在整個複合壓層周圍密封，且將壓層與工具一起置於高壓釜中以固化壓層。在固化期間，向真空袋施加真空，且將高壓釜加壓以將壓層壓實於工具之上表面上。在完成固化製程之後，自工具取出經壓實及固化之複合壓層。
在非高壓釜(OOA)處理中，將擬固化壓層包封於真空袋殼體內且僅經受真空壓力(並無高壓釜壓力)。然後在並不使用高壓釜下加熱壓層。此處理方式亦稱為僅真空袋(VBO)處理。
可使用真空袋設置或僅真空袋(VBO)自預浸體形成成型複合結構。舉例而言，產生具有三維表面之模具且然後將形成複合結構之預浸體夾層安置於模具表面上。然後藉由使用聚合膜(例如耐龍(nylon)，使用塑膠條帶將其密封至模具周邊)覆蓋組件來固結預浸體疊層。然後向包封空間施加真空且大氣壓會固結疊層。在固結後，將模具與預浸體疊層一起置於高壓釜或烘箱中進行固化。
在某些實施例中，完全固化之結合之複合結構展現在約室溫(75℉或24℃)下大於4,000psi(27.6MPa)及在250℉(121℃)下大於3,000psi(20.7MPa)之黏著結合強度，如藉由搭接剪切測試使用ASTM D1002所量測。另外，結合之複合結構提供內聚失效且展現大約650 J/m2或更大之模式I斷裂韌度，如藉由G1c測試根據ASTM D5528所測定。
搭接剪切測試測定在單搭接接點樣品上測試時黏著結合材料之剪切強度。使用黏著劑將兩種測試樣品結合至一起且如所指定進行固化。將測試樣品置於通用測試機器之夾鉗中且以預定負載速率(loading rate)拉動直至失效為止。
斷裂韌度係闡述含有裂縫之材料抵抗斷裂之能力之性質，且係用於航空應用之材料之最重要性質之一。斷裂韌度係表示在存在裂縫時材料之抗脆性斷裂性之定量方式。可將斷裂韌度量化為應變能釋放率(Gc)，其係每單位新產生斷裂表面積在斷裂期間所耗散之能量。Gc包含GIC(模式1-開口模式)。下標「Ic」表示模式I裂縫開口，其係在垂直於裂縫之法向拉伸應力下形成。
實例
提供下列實例以用於闡釋可如何測定固化等級及結合複合結構之各種實施例之目的，但其並不意欲限制本揭示內容之範圍。
測定固化等級
在下列實例中，使用DSC來測定達成期望階化程度之複合物熱固化循環。使用TA儀器Q20 DSC藉由以等溫方式或以動態方式將試樣在指定溫度下於鋁坩堝中加熱設定時間來量測DSC。維持溫度直至複合物完全固化為止。對反應峰之放熱熱進行積分使得可在溫度下時間與固化程度之間建立直接關聯。圖1展示CYCOM 5320-1(來自Cytec Industries公司之環氧基質/碳纖維預浸體膠帶)之代表性DSC結果。圖2及圖3展示用於測定固化程度之CYCOM 5320-1之其他DSC跡線。
使用TA儀器AR200 EX流變儀以扭轉模式及3℃/min之斜坡速率自40℃至300℃來進行動態機械量測。將試樣固化成2”×0.5”×0.125”樣品且以3%發生應變。使用TA儀器TMA Q400來測定熱機械分析 (TMA)。自40℃至200℃以10℃ min-1之掃描速率使用曲向探針在0.100N之所施加恆定負荷下來實施TMA實驗。軟化溫度(Ts)取為TMA跡線上探針位移之起始溫度。
複合物製作 共固化
藉由將10個環氧樹脂/碳纖維預浸體膠帶夾層以0°單向設計安置於工具上來結合共固化之結合面板(其用作對照樣品)。將FM 309-1黏著劑(可在350℉下固化之基於環氧之黏著劑，其自Cytec Industries公司獲得)置於預浸體膠帶頂部且將呈0°單向配置之10個膠帶預浸體夾層置於其頂部。然後在僅真空袋或高壓釜固化製程中藉由遵循所提示之複合物固化循環特徵來共固化整個總成。
二級結合及階化複合結合
藉由以0°單向設計安置10個環氧樹脂/碳纖維預浸體膠帶夾層來製作二級結合及階化結合之複合面板(呈12”×12”試件形式)。向工具表面施加脫模材料且使其與複合面板在製作期間直接接觸。然後使用非高壓釜(OOA)方法(其中在固化期間使用真空袋方案來生成複合面板之外部壓力)或高壓釜來將複合面板完全固化或部分地階化以達成期望固化等級。為顯示階化結合之複合面板抵抗污染之能力，容許脫模材料在後續黏著結合期間保留於複合物之表面上。
黏著複合結合
使用上文在「共固化」下詳述之程序來製備共固化面板。
使用FM 309-1黏著劑固化特徵(3℉ min-1至350℉且在40psi下保持90min)來進行複合面板之二級結合。
藉由在3℉/min下加熱至350℉且在40psi下保持120min來結合階化複合面板(25%、50%及75%)。藉由將黏著劑施加至已暴露於脫模材料之工具側來實施黏著結合。並不使用表面製備。
機械性質
根據ASTM D 5528來實施G1c測試。藉由遵循ASTM D 1002來實施0.5”搭接剪切測試。
實例1
在此實例中，使用CYCOM 5320-1預浸體來製作結合之複合面板且根據如上所述之共固化、階化結合及二級結合製程進行結合。將結合之面板切割至適當大小且加以測試以測定G1c及0.5”搭接剪切。結果展示於下表1中。
如可自上表1看到，搭接剪切強度顯著降低，此乃因階化複合面板之固化等級有所增加。共固化面板之搭接剪切值在75℉及250℉下分別為4872psi及4015psi。25%固化及50%固化下之階化面板具有類似室溫性能(在25%固化下為3845psi且在50%固化下為3890psi)，但25%階化材料在250℉下之強度顯著高於50%階化面板。已預固化至75%之面板展現在75℉下562psi及在250℉下513psi之極差性能，而二級結合面板展示在上述黏著劑與複合物之間並未黏著。為加以對比，亦展示共固化搭接剪切結果。
階化複合面板對於G1c性質之效應亦較為顯著，如自表1可看到。階化面板具有1694J/m2之室溫G1c值(在25%階化時)及1679J/m2之G1c值(在50%階化時)。階化至75%及100%固化等級之階化面板並不展示黏著，因此對於彼等試樣並不量測G1c。另外，斷裂機制在階化面板 中主要係內聚。
實例2
在此實例中，使用不同於CYCOM 5320-1之環氧樹脂/碳纖維預浸體來製作複合面板，且使用如上所述之共固化、階化結合及二級結合製程進行結合。將G1c及0.5”搭接剪切面板切割至適當大小且加以測試。結果展示於下表2中。
上表展示25%及50%階化面板能夠經由表面污染進行結合。75%及二級階化面板亦完全固化，但並不在表面上保留足夠化學活性官能基以經由表面污染形成共價鍵。
界面擴散
使用FM 309-1膜黏著劑來結合兩個階化至25%固化等級之基於CYCOM 5320之預浸體面板。使用上述FM 3090-1固化特徵來結合複合物，且在顯微鏡下研究複合物-黏著劑界面。圖4係展示在50×放大率下複合物-黏著劑界面之顯微影像。如在圖4之顯微影像中可看到，複合物-黏著劑界面展示在黏著劑與複合樹脂之間發生交纏。並不存在明顯邊界，但代之以在纖維與黏著劑之間存在黏著劑與複合樹脂之混合區。結合之結構容許基質樹脂物理擴散至黏著劑及複合物中，從而樹脂交纏基本上消除了黏著劑-複合物界面。此展示交纏提供了在黏著劑與複合物之間發生共價結合之物理路徑。
為加以對比，亦使用相同FM 309-1膜黏著劑來結合兩個完全固 化(亦即100%固化)之基於CYCOM 5320之預浸體面板。圖5係展示在50×放大率下複合物-黏著劑界面之顯微影像。可自圖5看到明晰障壁或界面，此表明在黏著劑與複合樹脂之間並無交纏。

Claims (18)

  1. 一種複合結合方法，其包括：a)形成至少兩個可固化複合基板，每一複合基板包括增強纖維及可固化樹脂基質；b)將該等複合基板部分地固化至至少10%但小於75%之固化程度；c)在該等複合基板中之至少一者上施加可固化黏著劑；d)使用該等複合基板之間之該可固化黏著劑使該等基板彼此接合；及e)完全共固化該等接合之複合基板以形成結合之複合結構，藉此，在共固化後，該黏著劑以化學方式結合至且以機械方式擴散有該等複合基板之該樹脂基質，從而在該黏著劑與每一複合基板之間得到化學結合界面。
  2. 如請求項1之方法，其中步驟(b)中之該固化程度在25%至70%固化之範圍內。
  3. 如請求項1之方法，其中步驟(b)中之該固化程度在25%至50%固化之範圍內。
  4. 如請求項1之方法，其中步驟(b)中之該固化程度在40%至60%之範圍內。
  5. 如請求項1之方法，其中在並無以物理方式改質該等可固化複合基板之表面之任何中間表面處理下來實施步驟(a)至(d)。
  6. 如請求項5之方法，其中該中間表面處理包含施加剝離夾層及以物理方式粗糙化或紋理化該表面之處理。
  7. 如請求項1之方法，其中該完全固化之結合之複合結構展現在約75℉(或24℃)下大於4,000psi(27.6MPa)及在250℉(或121℃) 下大於3,000psi(20.7MPa)之黏著結合強度，如藉由搭接剪切測試使用ASTM D1002所量測。
  8. 如請求項1之方法，其中該完全固化之結合之複合結構提供內聚失效且展現大約650J/m2或更大之模式I斷裂韌度，如藉由G1c測試根據ASTM D5528所測定。
  9. 如請求項1之方法，其中每一可固化複合基板係包括複數個預浸體夾層之預浸體疊層，每一預浸體夾層包括浸漬有可固化熱固性基質樹脂之增強纖維層。
  10. 如請求項1之方法，其中該熱固性基質樹脂包括一或多種環氧樹脂及固化劑。
  11. 如請求項10之方法，其中該可固化黏著劑包括一或多種環氧樹脂及固化劑。
  12. 如請求項9之方法，其中每一預浸體疊層係形成於非平面三維模製表面上且該預浸體疊層之至少一部分與該模製表面貼合。
  13. 如請求項12之方法，其中該模製表面上具有脫模塗層，且其中在並無去除該等預浸體疊層上之殘餘脫模塗層之任何中間步驟下實施該等預浸體疊層之該接合，且結合可在該等預浸體疊層之該等接合表面上存在污染物下發生。
  14. 如請求項12之方法，其中在與該模製表面接觸之側彼此面對下接合該等預浸體疊層。
  15. 一種複合結合方法，其包括：a)形成兩個可固化複合基板，每一複合基板包括增強纖維及可固化樹脂基質；b)將該等複合基板中之一者部分地固化至至少10%但小於75%之固化程度； c)在該等複合基板中之至少一者上施加可固化黏著劑；d)使用該等複合基板之間之該可固化黏著劑使該等基板彼此接合；及e)共固化該等接合之複合基板以形成完全固化之結合之複合結構，藉此，在共固化步驟(e)後，該黏著劑以化學方式結合至且以機械方式擴散有該等複合基板之該樹脂基質，從而在該黏著劑與每一複合基板之間得到化學結合界面。
  16. 如請求項15之方法，其中在步驟(b)部分地固化之該複合基板係包括複數個預浸體夾層之預浸體疊層，每一預浸體夾層包括浸漬有可固化熱固性基質樹脂之增強纖維層。
  17. 如請求項16之方法，其中該預浸體疊層係形成於上面具有脫模塗層之非平面三維模製表面上，且該預浸體疊層之至少一部分與該模製表面貼合，在步驟(d)，該預浸體疊層之與該模製表面接觸之側接合至另一複合基板，且在並無去除該預浸體疊層上之殘餘脫模塗層之任何中間步驟下實施該等複合基板之該接合。
  18. 如請求項15之方法，其中步驟(b)中之該固化程度在25%至70%固化之範圍內。
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JP6212129B2 (ja) 2017-10-11
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US20160214328A1 (en) 2016-07-28
CA2892082A1 (en) 2014-05-30
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US20140144568A1 (en) 2014-05-29
CN104837605A (zh) 2015-08-12
AU2013348225A1 (en) 2015-05-28
WO2014081652A2 (en) 2014-05-30
RU2618055C2 (ru) 2017-05-02
JP2016501145A (ja) 2016-01-18
EP2922685A2 (en) 2015-09-30
MX2015006612A (es) 2015-08-05
BR112015012020A2 (pt) 2017-07-11
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EP2922685B1 (en) 2019-04-17
WO2014081652A3 (en) 2015-04-09

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