TW202411305A - 樹脂組成物、接著劑、塗覆劑、硬化物、接著片材、附樹脂之銅箔、覆銅積層板及印刷配線板 - Google Patents
樹脂組成物、接著劑、塗覆劑、硬化物、接著片材、附樹脂之銅箔、覆銅積層板及印刷配線板 Download PDFInfo
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- TW202411305A TW202411305A TW112134024A TW112134024A TW202411305A TW 202411305 A TW202411305 A TW 202411305A TW 112134024 A TW112134024 A TW 112134024A TW 112134024 A TW112134024 A TW 112134024A TW 202411305 A TW202411305 A TW 202411305A
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- resin composition
- bis
- resin
- copper foil
- heat resistance
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- 239000011342 resin composition Substances 0.000 title claims abstract description 64
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- 239000011889 copper foil Substances 0.000 title claims abstract description 51
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Classifications
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- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
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- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
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Abstract
本發明提供一種樹脂組成物,在作為接著劑使用時,賦予接著性、焊料耐熱性、耐濕熱性及耐遷移性優異的硬化物,此外在使用硬化物作為樹脂膜時,亦表現出優異的焊料耐熱性及高儲能模量。本發明關於一種樹脂組成物、接著劑、塗覆劑、硬化物、接著片材、附樹脂之銅箔、覆銅積層板及印刷配線板,該樹脂組成物係含有:聚醯亞胺(A)、由通式(1)表示之交聯劑(B)、以及(B)成分以外之硬化劑(C),該聚醯亞胺(A)為含有芳香族四羧酸酐(a1)及含二聚物二胺之二胺(a2)之單體群的反應物。
(在式(1)中,X
1、X
2以及X
3各自獨立地表示具有1個以上的環氧骨架之基團。)
Description
本發明係關於樹脂組成物、接著劑、塗覆劑、硬化物、接著片材、附樹脂之銅箔、覆銅積層板以及印刷配線板。
聚醯亞胺通常為使四羧酸酐與二胺反應而得之產物,具有耐熱性、密著性及機械特性等各種性能。因此,被用於半導體用之保護膜、絕緣密封膜、以及柔性印刷配線板、印刷電路板等之接著劑等各種各樣的用途。
此外,近年來,為了高速地傳輸、處理大容量的訊息,使用高頻的電訊號,但由於高頻訊號非常容易衰減,因而即使對於前述多層配線板而言亦需要設法儘量抑制傳輸損耗,從此點考慮具有低介電特性(低介電常數、低介電損耗角正切)之聚醯亞胺係有用的。
作為此種技術,本發明人為了形成具有絕緣膜、接著劑層與銅箔之覆銅積層體中之接著劑層,已揭示一種含有具有四羧酸殘基及源自於二聚酸之二胺殘基之聚醯亞胺及交聯成分之接著劑組成物(專利文獻1)。該聚醯亞胺由於具有芳香環,因此表現出優異的焊料耐熱性。
作為各用途中之目前的課題可列舉以下3個。
1.該技術中,作為接著劑組成物中之交聯成分之一配合有多官能環氧樹脂。然而,此種環氧樹脂中通常作為製造步驟上的雜質包含氯成分,若以此種組成物來製作配線板,則會在高濕環境下因對銅電路的端子間施加電壓而從陽極側析出溶出的銅,容易產生電路短路之被稱作離子遷移的現象。
2.該技術中,作為覆銅積層板中之熱可塑性聚醯亞胺組成物配合有異氰酸酯,在製作覆銅積層板時需要280℃以上的高溫。
3.作為製造聚醯亞胺膜之代表性方法,可列舉流延法。該方法中,在支撐基材上塗佈聚醯胺酸溶液並進行乾燥,利用熱處理進行醯亞胺化後,剝離支撐基材而形成。但是,熱處理中若非300~400℃如此非常高的溫度,則不會推進醯亞胺化。
[先前技術文獻]
[專利文獻]
[專利文獻1]日本特開2018-121807號公報
[發明所欲解決之技術問題]
本發明之目的在於提供一種樹脂組成物,在作為接著劑使用時,賦予接著性、焊料耐熱性、耐濕熱性及耐遷移性優異的硬化物,此外在使用硬化物作為樹脂膜時,亦表現出優異的焊料耐熱性及高儲能模量。
[技術手段]
本發明人進行深入研究後,發現可以解決前述課題,從而完成本發明。即,在本發明中,提供以下內容。
1.一種樹脂組成物,其含有:聚醯亞胺(A)、由通式(1)表示之交聯劑(B)、以及(B)成分以外之硬化劑(C),前述聚醯亞胺(A)為含有芳香族四羧酸酐(a1)及含二聚物二胺之二胺(a2)之單體群的反應物;
〔化1〕
(在式(1)中,X
1、X
2以及X
3各自獨立地表示具有1個以上的環氧骨架之基團。)
2.如前項1所述之樹脂組成物,其中,前述(C)成分為選自聚醯胺多胺、聚醚多胺及三聚物三胺所成群中之1種以上。
3.如前項1或2所述之樹脂組成物,其中,前述樹脂組成物進一步含有無機填料。
4.一種接著劑,其含有如前項1所述之樹脂組成物。
5.一種塗覆劑,其含有如前項1所述之樹脂組成物。
6.一種硬化物,其含有選自如前項1所述之樹脂組成物、如前項4所述之接著劑、以及如前項5所述之塗覆劑所成群中之1種以上。
7.一種接著片材,其在支撐膜之至少單面上具有如前項6所述之硬化物。
8.一種附樹脂之銅箔,其含有如前項6所述之硬化物或如前項7所述之接著片材、以及銅箔。
9.一種覆銅積層板,其含有如前項8所述之附樹脂之銅箔、以及銅箔或絕緣性片材。
10.一種印刷配線板,其在如前項9所述之覆銅積層板的銅箔面具有電路圖案。
[發明之效果]
本發明之樹脂組成物,在作為接著劑使用時,賦予接著性、焊料耐熱性、耐濕熱性及耐遷移性優異的硬化物,此外在使用硬化物作為樹脂膜時,亦表現出優異的焊料耐熱性及高儲能模量。此外,本發明之樹脂組成物利用聚醯亞胺以及交聯劑的組合,亦可以在比以往更低的溫度下硬化。
本發明之樹脂組成物含有:聚醯亞胺(A)(以下,稱為(A)成分。)、由通式(1)表示之交聯劑(B)(以下,稱為(B)成分。)、以及(B)成分以外之硬化劑(C)(以下,稱為(C)成分。),該聚醯亞胺(A)為含有芳香族四羧酸酐(a1)(以下,稱為(a1)成分。)及含二聚物二胺之二胺(a2)(以下,稱為(a2)成分。)之單體群的反應物。
〔化1〕
(在式(1)中,X
1、X
2以及X
3各自獨立地表示具有1個以上的環氧骨架之基團。)
(A)成分係聚醯亞胺,並且係用以使樹脂組成物的層(以下,稱為硬化物層。)表現出低介電常數及低介電損耗角正切之成分。
作為(a1)成分,可列舉例如:2,2’,3,3’-聯苯四甲酸二酐、2,3’,3,4’-聯苯四甲酸二酐、3,3’,4,4’-聯苯四甲酸二酐、均苯四甲酸二酐、1,2,3,4-苯四甲酸酐、3,3’,4,4’-二苯基碸四甲酸二酐、4,4’-氧基二鄰苯二甲酸酐、4,4’-[丙-2,2-二基雙(1,4-伸苯基氧基)]二鄰苯二甲酸二酐、2,2’,3,3’-二苯甲酮四甲酸二酐、2,3,3’,4’-二苯甲酮四甲酸二酐、3,3’,4,4’-二苯甲酮四甲酸二酐、2,3’,3,4’-二苯基醚四甲酸二酐、雙(2,3-二羧基苯基)醚二酐、雙(2,3-二羧基苯基)甲烷二酐、雙(3,4‐二羧基苯基)甲烷二酐、1,1-雙(2,3-二羧基苯基)乙烷二酐、1,1-雙(3,4-二羧基苯基)乙烷二酐、2,2-雙(2,3-二羧基苯基)丙烷二酐、2,2-雙(3,4-二羧基苯基)丙烷二酐、雙(2,3-二羧基苯氧基苯基)碸二酐、雙(3,4-二羧基苯氧基苯基)碸二酐、1,4,5,8-萘四甲酸酐、2,3,6,7-萘四甲酸酐、2,3,6,7-蒽四甲酸二酐、1,2,5,6-萘四甲酸二酐、1,4,5,8-萘四甲酸二酐、2,3,6,7-萘四甲酸二酐、4,8-二甲基-1,2,3,5,6,7-六氫萘-1,2,5,6-四甲酸二酐、2,2-雙(3,4-二羧基苯基)六氟丙烷二酐、2,2-雙(3,3’,4,4’-四羧基苯基)四氟丙烷二酐等。此等可以單獨使用亦可並用2種以上。
其中,作為(a1)成分,從硬化物層的可撓性、焊料耐熱性之觀點而言,理想為由下述通式(2)表示之物質。
〔化2〕
(式(2)中,X表示單鍵、-SO
2-、-CO-、-O-、-O-C
6H
4-C(CH
3)
2-C
6H
4-O-、-C(CH
3)
2-、-O-C
6H
4-SO
2-C
6H
4-O-、-C(CHF
2)
2-、-C(CF
3)
2-、-COO-(CH
2)
p-OCO-、或-COO-H
2C-HC(-O-C(=O)-CH
3)-CH
2-OCO-,p表示1~20的整數。)
作為由通式(2)表示之物質,可列舉例如:2,2’,3,3’-聯苯四甲酸二酐、3,3’,4,4’-聯苯四甲酸二酐、3,3’,4,4’-二苯基碸四甲酸二酐、3,3’,4,4’-二苯甲酮四甲酸二酐、3,3’,4,4’-二苯基醚四甲酸二酐、2,2-雙(3,4-二羧基苯基)六氟丙烷二酐、2,2-雙(3,3’,4,4’-四羧基苯基)四氟丙烷二酐、4,4’-[丙-2,2-二基雙(1,4-伸苯基氧基)]二鄰苯二甲酸二酐、2,2-雙(2,3-二羧基苯基)丙烷二酐、2,2-雙(3,4-二羧基苯基)丙烷二酐、2,2’-雙(3,4-二羧基苯氧基苯基)碸二酐等。此等可以單獨使用亦可並用2種以上。其中,從(A)成分在有機溶劑中良好溶解之觀點而言,理想為2,2-雙(3,4-二羧基苯基)六氟丙烷二酐、4,4’-[丙-2,2-二基雙(1,4-伸苯基氧基)]二鄰苯二甲酸二酐。
構成(A)成分之單體群100莫耳%中的(a1)成分的使用量,通常為10~90莫耳%,理想為25~75莫耳%。
此外,構成(A)成分之單體群100莫耳%中的由通式(2)表示之四羧酸酐的使用量,通常為10~90莫耳%,理想為25~75莫耳%。
(a1)成分100莫耳%中的由通式(2)表示之四羧酸酐的使用量,通常為10~100莫耳%,理想為50~100莫耳%。
(a2)成分為含二聚物二胺之二胺。
二聚物二胺係指將二聚酸的全部羧基取代為一級胺基或一級胺基甲基而得的產物(例如,參照日本特開平9-12712號公報)。在此,二聚酸係指主要含有將油酸、亞油酸、亞麻酸等不飽和脂肪酸二聚化而得的碳數36的二元酸的物質,並根據其精製程度含有碳數18的單體酸、碳數54的三聚酸、碳數20~90的聚合脂肪酸。又,雖然前述二聚酸含有雙鍵,但亦可以藉由例如氫化反應而使不飽和度降低。
作為前述二聚物二胺,可列舉例如由下述通式(3)表示之物質。又,在通式(3)中,理想m+n=6~17,理想p+q=8~19,虛線部分意指碳-碳單鍵或碳-碳雙鍵。
〔化3〕
此外,作為二聚物二胺的市售品,可列舉:「Versamine551」、「Versamine552」(以上為Cognis Japan股份有限公司製),「PRIAMINE1073」、「PRIAMINE1074」、「PRIAMINE1075」(以上為Croda Japan股份有限公司製)等。此等市售品中,「Versamine551」、「PRIAMINE1074」含有由下述式(3-1)表示之化合物,「Versamine552」、「PRIAMINE1073」、「PRIAMINE1075」係含有由下述式(3-2)表示之化合物之二聚物二胺。
〔化4〕
〔化5〕
又,在二聚物二胺中,可以含有源自前述單體酸、三聚酸及/或聚合脂肪酸之胺,作為其等的含量,在二聚物二胺中為10重量%以下,理想為5重量%以下,更理想為3重量%以下,進一步理想為2重量%以下。
此外,二聚物二胺可以直接使用市售品,亦可以使用對市售品實施蒸餾等精製處理的產物。
構成(A)成分之單體群100莫耳%中的二聚物二胺的使用量,通常為5莫耳%以上,理想為25~75莫耳%。
此外,(a2)成分100莫耳%中的二聚物二胺的使用量,通常為10莫耳%以上,理想為30~100莫耳%。
此外,作為(a2)成分,亦可以含有二聚物二胺以外之二胺(a2-1)(以下,稱為(a2-1)成分。)。作為(a2-1)成分,例如可以含有脂肪族二胺、脂環族二胺、芳香族二胺、二胺基醚、二胺基聚矽氧烷。又,對於此等胺,不包括二聚物二胺。
作為脂肪族二胺,可列舉例如:乙二胺、1,3-二胺基丙烷、1,4-二胺基丁烷、1,5-二胺基戊烷、1,6-二胺基己烷、1,7-二胺基庚烷、1,8-二胺基辛烷、1,9-二胺基壬烷、1,10-二胺基癸烷、1,11-二胺基十一烷、1,12-二胺基十二烷等。
作為脂環族二胺,可列舉例如:二胺基環己烷、二胺基二環己基甲烷、二甲基二胺基二環己基甲烷、二胺基二環己基丙烷、四甲基二胺基二環己基甲烷、1,3-雙(胺基甲基)環己烷、1,4-雙(胺基甲基)環己烷、雙(4-胺基環己基)甲烷、二胺基雙環[2.2.1]庚烷、雙(胺基甲基)-雙環[2.2.1]庚烷、3(4),8(9)-雙(胺基甲基)三環[5.2.1.0(2,6)]癸烷、異佛爾酮二胺等。
作為芳香族二胺,可列舉例如:
2,2’-二胺基聯苯、3,3’-二胺基聯苯、4,4’-二胺基聯苯、2,2’-二甲基-4,4’-二胺基聯苯、2,2’-二乙基-4,4’-二胺基聯苯、2,2’-二正丙基-4,4’-二胺基聯苯等二胺基聯苯;
2,2-雙[4-(3-胺基苯氧基)苯基]丙烷、2,2-雙[4-(4-胺基苯氧基)苯基]丙烷等雙胺基苯氧基苯基丙烷;
3,3’-二胺基二苯基醚、3,4’-二胺基二苯基醚、4,4’-二胺基二苯基醚等二胺基二苯基醚;
對苯二胺、間苯二胺等苯二胺;
3,3’-二胺基二苯基硫醚、3,4’-二胺基二苯基硫醚、4,4’-二胺基二苯基硫醚等二胺基二苯基硫醚;
3,3’-二胺基二苯基碸、3,4’-二胺基二苯基碸、4,4’-二胺基二苯基碸等二胺基二苯基碸;
3,3’-二胺基二苯甲酮、3,4’-二胺基二苯甲酮、4,4’-二胺基二苯甲酮等二胺基二苯甲酮;
3,3’-二胺基二苯基甲烷、3,4’-二胺基二苯基甲烷、4,4’-二胺基二苯基甲烷、雙[4-(3-胺基苯氧基)苯基]甲烷等二胺基二苯基甲烷;
2,2-二(3-胺基苯基)丙烷、2,2-二(4-胺基苯基)丙烷、2-(3-胺基苯基)-2-(4-胺基苯基)丙烷等二胺基苯基丙烷;
2,2-二(3-胺基苯基)-1,1,1,3,3,3-六氟丙烷、2,2-二(4-胺基苯基)-1,1,1,3,3,3-六氟丙烷、2-(3-胺基苯基)-2-(4-胺基苯基)-1,1,1,3,3,3-六氟丙烷等二胺基苯基六氟丙烷;
1,1-二(3-胺基苯基)-1-苯基乙烷、1,1-二(4-胺基苯基)-1-苯基乙烷、1-(3-胺基苯基)-1-(4-胺基苯基)-1-苯基乙烷等二胺基苯基苯基乙烷;
1,3-雙(3-胺基苯氧基)苯、1,3-雙(4-胺基苯氧基)苯、1,4-雙(3-胺基苯氧基)苯、1,4-雙(4-胺基苯氧基)苯等雙胺基苯氧基苯;
1,3-雙(3-胺基苯甲醯基)苯、1,3-雙(4-胺基苯甲醯基)苯、1,4-雙(3-胺基苯甲醯基)苯、1,4-雙(4-胺基苯甲醯基)苯等雙胺基苯甲醯基苯;
1,3-雙(3-胺基-α,α-二甲基苄基)苯、1,3-雙(4-胺基-α,α-二甲基苄基)苯、1,4-雙(3-胺基-α,α-二甲基苄基)苯、1,4-雙(4-胺基-α,α-二甲基苄基)苯等雙胺基二甲基苄基苯;
1,3-雙(3-胺基-α,α-二-三氟甲基苄基)苯、1,3-雙(4-胺基-α,α-二-三氟甲基苄基)苯、1,4-雙(3-胺基-α,α-二-三氟甲基苄基)苯、1,4-雙(4-胺基-α,α-二-三氟甲基苄基)苯等雙胺基二-三氟甲基苄基苯;
4,4’-雙(3-胺基苯氧基)聯苯、4,4’-雙(4-胺基苯氧基)聯苯、雙[1-(3-胺基苯氧基)]聯苯等胺基苯氧基聯苯;
雙[4-(3-胺基苯氧基)苯基]酮、雙[4-(4-胺基苯氧基)苯基]酮等胺基苯氧基苯基酮;
雙[4-(3-胺基苯氧基)苯基]硫醚、雙[4-(4-胺基苯氧基)苯基]硫醚等胺基苯氧基苯基硫醚;
雙[4-(3-胺基苯氧基)苯基]碸、雙[4-(4-胺基苯氧基)苯基]碸等胺基苯氧基苯基碸;
雙[4-(3-胺基苯氧基)苯基]醚、雙[4-(4-胺基苯氧基)苯基]醚等胺基苯氧基苯基醚;
2,2-雙[4-(3-胺基苯氧基)苯基]丙烷、2,2-雙[3-(3-胺基苯氧基)苯基]-1,1,1,3,3,3-六氟丙烷、2,2-雙[4-(4-胺基苯氧基)苯基]-1,1,1,3,3,3-六氟丙烷等胺基苯氧基苯基丙烷;
1,3-雙[4-(3-胺基苯氧基)苯甲醯基]苯、1,3-雙[4-(4-胺基苯氧基)苯甲醯基]苯、1,4-雙[4-(3-胺基苯氧基)苯甲醯基]苯、1,4-雙[4-(4-胺基苯氧基)苯甲醯基]苯等雙(胺基苯氧基苯甲醯基)苯;
1,3-雙[4-(3-胺基苯氧基)-α,α-二甲基苄基]苯、1,3-雙[4-(4-胺基苯氧基)-α,α-二甲基苄基]苯、1,4-雙[4-(3-胺基苯氧基)-α,α-二甲基苄基]苯、1,4-雙[4-(4-胺基苯氧基)-α,α-二甲基苄基]苯等雙(胺基苯氧基-α,α-二甲基苄基)苯;
4,4’-雙[4-(4-胺基苯氧基)苯甲醯基]二苯基醚等雙[(胺基芳氧基)苯甲醯基]二苯基醚;
4,4’-雙[4-(4-胺基-α,α-二甲基苄基)苯氧基]二苯甲酮等雙(胺基-α,α-二甲基苄基苯氧基)二苯甲酮;
4,4’-雙[4-(4-胺基-α,α-二甲基苄基)苯氧基]二苯基碸等雙[胺基-α,α-二甲基苄基苯氧基]二苯基碸;
4,4’-雙[4-(4-胺基苯氧基)苯氧基]二苯基碸等雙[胺基苯氧基苯氧基]二苯基碸;
3,3’-二胺基-4,4’-二苯氧基二苯甲酮、3,3’-二胺基-4,4’-二聯苯氧基二苯甲酮等二胺基二芳氧基二苯甲酮;
3,3’-二胺基-4-苯氧基二苯甲酮、3,3’-二胺基-4-聯苯氧基二苯甲酮等二胺基芳氧基二苯甲酮;
1-(4-胺基苯基)-2,3-二氫-1,3,3-三甲基-1H-茚-5-胺、9,9-雙(4-胺基苯基)芴等。
作為二胺基醚,可列舉例如雙(胺基甲基)醚、雙(2-胺基乙基)醚、雙(3-胺基丙基)醚、雙[(2-胺基甲氧基)乙基]醚、雙[2-(2-胺基乙氧基)乙基]醚、雙[2-(3-胺基丙氧基)乙基]醚、1,2-雙(胺基甲氧基)乙烷、1,2-雙(2-胺基乙氧基)乙烷、1,2-雙[2-(胺基甲氧基)乙氧基]乙烷、1,2-雙[2-(2-胺基乙氧基)乙氧基]乙烷、乙二醇雙(3-胺基丙基)醚、二乙二醇雙(3-胺基丙基)醚、三乙二醇雙(3-胺基丙基)醚等。
作為二胺基聚矽氧烷,可列舉例如α,ω-雙(2-胺基乙基)聚二甲基矽氧烷、α,ω-雙(3-胺基丙基)聚二甲基矽氧烷、α,ω-雙(4-胺基丁基)聚二甲基矽氧烷、α,ω-雙(5-胺基戊基)聚二甲基矽氧烷、α,ω-雙[3-(2-胺基苯基)丙基]聚二甲基矽氧烷、α,ω-雙[3-(4-胺基苯基)丙基]聚二甲基矽氧烷等。
此等(a2-1)成分可以單獨使用亦可並用2種以上。其中,從硬化物層表現出優異的焊料耐熱性之觀點而言,理想為脂環族二胺、芳香族二胺,更理想為芳香族二胺。
構成(A)成分之單體群100莫耳%中的(a2-1)成分的使用量,通常為90莫耳%以下,理想為50莫耳%以下。
此外,(a2)成分100莫耳%中的(a2-1)成分的使用量,通常為90莫耳%以下,理想為70莫耳%以下。
本發明之(A)成分可以藉由各種習知的製造方法而得到。作為其製造方法,可列舉例如包含以下步驟之方法等:以溫度理想為30~120℃左右、更理想為60~100℃左右、並且時間理想為0.1~2小時左右、更理想為0.1~0.5小時左右的條件,使含有(a1)成分及(a2)成分之單體群進行複加成反應而得到複加成物之步驟;在理想為80~250℃左右、更理想為100~170℃左右的溫度下,以理想為0.5~50小時左右、更理想為1~20小時左右的條件,使所得之複加成物進行醯亞胺化反應,即脫水閉環反應之步驟。又,(a1)成分及(a2)成分的混合方法、順序等沒有特別限定。
又,在進行醯亞胺化反應之步驟中,可以使用各種習知的反應催化劑、脫水劑及有機溶劑,此等可以單獨使用亦可並用2種以上。
作為反應催化劑,可列舉例如三乙胺等脂肪族三級胺;二甲基苯胺等芳香族三級胺;吡啶、甲基吡啶、異喹啉等雜環式三級胺等。此外,脫水劑可列舉:乙酸酐等脂肪族羧酸酐、苯甲酸酐等芳香族羧酸酐等。
作為有機溶劑,可列舉例如:
N-甲基-2-吡咯烷酮、N,N-二甲基甲醯胺、N,N-二乙基甲醯胺、N,N-二甲基乙醯胺、N,N-二乙基乙醯胺、二氮雜雙環十一烯等氮系有機溶劑;
甲基乙基酮、甲基正丙基酮、甲基異丙基酮、正丁基甲基酮、異丁基甲基酮、二乙基酮、乙基正丙基酮、乙基異丙基酮、正丁基乙基酮、二正丙基酮等脂肪族酮;
環丙基甲基酮、環丁酮、環丁基甲基酮、環戊酮、環己酮、甲基環己酮等脂環族酮;
甲酸正丙酯、甲酸異丙酯、甲酸正丁酯、甲酸異丁酯、甲酸正戊酯、甲酸異戊酯、乙酸乙酯、乙酸正丙酯、乙酸異丙酯、乙酸正丁酯、乙酸異丁酯、乙酸正戊酯、乙酸異戊酯、丙酸甲酯、丙酸乙酯、丙酸正丙酯、丙酸異丙酯、丙酸正丁酯等脂肪族酯;
碳酸二甲酯、碳酸甲乙酯、碳酸二乙酯等碳酸烷基酯;
環丙烷羧酸甲酯、環丙烷羧酸乙酯、環丁烷羧酸甲酯等脂環族酯;
乙基正丙基醚、二正丙基醚、二異丙基醚、1,2-二甲氧基乙烷、1,1-二乙氧基乙烷、1,2-二乙氧基乙烷、1,2-二甲氧基丙烷、2,2-二甲氧基丙烷、1,1-二乙氧基丙烷、2,2-二乙氧基丙烷等脂肪族醚;
四氫呋喃、二噁烷等環狀醚;
甲醇、乙醇、正丙醇、異丙醇、1-甲氧基-2-丙醇、三級丁基醇等醇;
2-甲基戊烷、3-乙基戊烷、正己烷、2-甲基己烷、3-甲基己烷、3-乙基己烷、正庚烷、2-甲基庚烷、3-甲基庚烷、4-甲基庚烷、3-乙基庚烷、正辛烷、2-甲基辛烷、3-甲基辛烷、4-甲基辛烷等脂肪族烴;
甲基環戊烷、乙基環戊烷、正丙基環戊烷、異丙基環戊烷、正丁基環戊烷、異丁基環戊烷、環己烷、甲基環己烷、乙基環己烷、1,1-二甲基環己烷、1-乙基-3-甲基環己烷、環庚烷等脂環族烴;
苯、甲苯、二甲苯等芳香族烴;二甲基亞碸等。此等可以單獨使用亦可組合2種以上。
此外,調節有機溶劑的使用量以使得反應濃度為5~60質量%,理想為20~50質量%。
(A)成分的醯亞胺閉環率,從得到軟化點及柔軟性均高的(A)成分之觀點而言,理想為90~100%,更理想為95~100%左右。
推定此是因為,藉由使(A)成分的醯亞胺閉環率為前述範圍,(A)成分容易形成硬鏈段及軟鏈段的結構,從而軟化點及柔軟性均變高。在此,「醯亞胺閉環率」,係指(A)成分的聚醯亞胺中的環狀醯亞胺鍵的含量,例如可以藉由NMR、IR分析等各種光譜手段來確定。
作為(A)成分的物性,例如重量平均分子量理想為10,000~100,000。此外,(A)成分的數平均分子量理想為5,000~50,000。重量平均分子量及數平均分子量例如以藉由凝膠滲透層析(GPC)測定而得的聚苯乙烯換算值的形式來求出。
本發明的(A)成分的軟化點理想為50~250℃左右,更理想為80~200℃左右。又,軟化點係指在使用市售的測定器(裝置名:「ARES-2KSTD-FCO-STD」,Rheometric Scientific公司製)等進行測定而得的儲能模量的曲線中,儲能模量開始降低的溫度。
(B)成分為由通式(1)表示之交聯劑,藉由與(A)成分以及後述之(C)成分的組合,例如可以發揮以下的效果的任意1種以上。
(1)可以使樹脂組成物在低溫下硬化。
(2)硬化物表現出優異的接著性、焊料耐熱性及耐遷移性。
(3)在使用硬化物作為樹脂膜時表現出優異的焊料耐熱性及高儲能模量。
〔化1〕
(在式(1)中,X
1、X
2以及X
3各自獨立地表示具有1個以上的環氧骨架之基團。)
式(1)中,作為X
1、X
2以及X
3的基團,各自獨立地可列舉例如:縮水甘油基、2,3-環氧丙基、3,4-環氧丁基、2-(3,4-環氧環己基)乙基、由通式(1-1)表示之具有烷基、環氧基、烷基如此並列的結構之基團、由通式(1-2)表示之具有烷基、環氧基、烷基、環氧基、烷基如此並列的結構之基團等。
〔化6〕
(式(1-1)中,Y
1、Y
2各自獨立地為1~15的整數。)
〔化7〕
(式(1-2)中,Z
1、Z
2、Z
3各自獨立地為1~15的整數。)
作為(B)成分(即由通式(1)表示之交聯劑)的市售品,可列舉例如「Sansocizer E-2000H」、「Sansocizer E-9000H」(以上為新日本理化股份有限公司製)、「Adekacizer O-130P」、「Adekacizer O-180P」(以上為ADEKA股份有限公司製)、「Epocizer W-100-EL」(DIC股份有限公司製)、「Kapox S-6」(花王股份有限公司製)、「Newcizer 510R」(日油股份有限公司製)等,「Sansocizer E-2000H」為含有由下述式(1-3)表示之化合物的環氧樹脂。
〔化8〕
作為(B)成分的含量,從易於發揮前述的效果之方面而言,以不揮發成分換算,相對於(A)成分100重量份,理想為1~15重量份,更理想為3.5~10重量份,進一步理想為3.5~7重量份。又,不揮發成分意指除去水、有機溶劑等揮發成分後殘留的成分。
(C)成分為(B)成分以外的硬化劑,由於能夠促進(A)成分與(B)成分的反應,因此能夠在較低溫度下硬化,所得的硬化物亦表現出優異的焊料耐熱性。在此,硬化劑意指具有進行硬化的功能之成分,可分類為在該硬化劑與該硬化劑以外的成分發生反應的同時進行硬化之硬化劑(非交聯性硬化劑)及在前述的硬化的基礎上硬化劑之間發生自交聯之硬化劑(交聯性硬化劑、交聯劑)。
作為(C)成分,可列舉例如環氧樹脂、苯并噁嗪、雙馬來醯亞胺、氰酸酯、多異氰酸酯、磷化合物、酸酐、胺、咪唑、胍、酚樹脂、活性酯等。此等可以單獨使用亦可組合2種以上。
作為環氧樹脂,例如列舉苯酚酚醛清漆型環氧樹脂、甲酚酚醛清漆型環氧樹脂、雙酚A型環氧樹脂、雙酚F型環氧樹脂、雙酚S型環氧樹脂、氫化雙酚A型環氧樹脂、氫化雙酚F型環氧樹脂、二苯乙烯型環氧樹脂、含三嗪骨架之環氧樹脂、含芴骨架之環氧樹脂、線狀脂肪族環氧樹脂、脂環式環氧樹脂、縮水甘油胺型環氧樹脂、三酚甲烷型環氧樹脂、烷基改性三酚甲烷型環氧樹脂、聯苯型環氧樹脂、含雙環戊二烯骨架之環氧樹脂、含萘骨架之環氧樹脂、芳基伸烷基型環氧樹脂、四縮水甘油基苯二甲基二胺、作為前述環氧化物之二聚酸改性物之二聚酸改性環氧化物、二聚酸二縮水甘油基酯等。
作為環氧樹脂的市售品,可列舉「jER828」、「jER834」、「jER807」、「jER604」、「jER630」、「jER871」、「jER872」(以上為三菱化學股份有限公司製),「ST-3000」、「YD-172-X75」(以上為日鐵化學材料(NIPPON STEEL Chemical & Material)股份有限公司製),「CELLOXIDE 2021P」(大賽璐(Daicel)股份有限公司製),「TETRAD-X」(三菱瓦斯化學股份有限公司製),「NC-513」、「NC-514S」、「NC-547」(以上為卡德萊股份有限公司(Cardolite Corp.)製)等。
作為苯并噁嗪,可列舉例如:6,6-(1-甲基亞乙基)雙(3,4-二氫-3-苯基-2H-1,3-苯并噁嗪)、6,6-(1-甲基亞乙基)雙(3,4-二氫-3-甲基-2H-1,3-苯并噁嗪)等。又,噁嗪環的氮上可以鍵結有苯基、甲基、環己基等。
作為苯并噁嗪的市售品,可列舉「苯并噁嗪F-a型」、「苯并噁嗪P-d型」(以上為四國化成工業股份有限公司製)、「RLV-100」(AIR WATER股份有限公司製)等。
作為雙馬來醯亞胺,可列舉例如:
N,N’-伸乙基雙馬來醯亞胺、N,N’-三亞甲基雙馬來醯亞胺、N,N’-四亞甲基雙馬來醯亞胺、N,N’-五亞甲基雙馬來醯亞胺、N,N’-六亞甲基雙馬來醯亞胺、N,N’-六亞甲基雙甲基馬來醯亞胺、N,N-七亞甲基雙馬來醯亞胺、N,N-八亞甲基雙馬來醯亞胺、1,6’-雙馬來醯亞胺-(2,2,4-三甲基)己烷、1,1’-(癸烷-1,10-二基)雙(1H-吡咯-2,5-二酮)等N,N’-伸烷基雙馬來醯亞胺類;
N,N’-二環己基甲烷雙馬來醯亞胺、1,1’-[(4-己基-3-辛基環己烷-1,2-二基)雙(辛烷-1,8-二基)]雙(1H-吡咯-2,5-二酮)、1,1’-(環己烷-1,10-二基)雙(1H-吡咯-2,5-二酮)、1,1’-[4,4’-亞甲基雙(環己烷-1,4-二基)]雙(1H-吡咯-2,5-二酮)等具有環烷烴之雙馬來醯亞胺類;
N,N’-二甲苯雙馬來醯亞胺、N,N’-甲苯雙馬來醯亞胺、N,N’-苯二甲基雙馬來醯亞胺、N,N’-間伸苯基雙馬來醯亞胺、N,N’-對伸苯基雙馬來醯亞胺、4-甲基-1,3-伸苯基雙馬來醯亞胺等伸苯基雙馬來醯亞胺類;
1,1’-[亞甲基雙(1,4-伸苯基)]雙(1H-吡咯-2,5-二酮)、1,1’-[亞甲基雙(2-乙基-6-甲基-1,4-伸苯基)]雙(1H-吡咯-2,5-二酮)、1,1’-(1,3-伸苯基)雙(1H-吡咯-2,5-二酮)等雙伸苯基雙馬來醯亞胺類;
N,N’-(4,4’-二苯基甲烷)雙馬來醯亞胺、N,N’-4,4’-[3,3’-二甲基二苯基甲烷]馬來醯亞胺、N,N’-4,4’-[3,3’-二乙基二苯基甲烷]馬來醯亞胺、N,N’-(4,4’-二苯基丙烷)雙馬來醯亞胺、N,N’-二苯基環己烷雙馬來醯亞胺、3,3’-二甲基-5,5’-二乙基-4,4-二苯基甲烷雙馬來醯亞胺、N,N’-(4,4’-二苯基甲烷)雙馬來醯亞胺、N,N’-4,4’-[3,3’-二甲基二苯基甲烷]馬來醯亞胺、N,N’-4,4’-[3,3’-二乙基二苯基甲烷]馬來醯亞胺、N,N’-(4,4’-二苯基丙烷)雙馬來醯亞胺、N,N’-二苯基環己烷雙馬來醯亞胺、3,3’-二甲基-5,5’-二乙基-4,4’-二苯基甲烷雙馬來醯亞胺、N,N’-二苯基醚雙馬來醯亞胺、1,3-雙(3-馬來醯亞胺苯氧基)苯、1,3-雙(3-馬來醯亞胺苯氧基)苯、1,3-雙(4-馬來醯亞胺苯氧基)苯、N,N’-3,3’-二苯基碸雙馬來醯亞胺、N,N’-4,4’-二苯基碸雙馬來醯亞胺、N,N’-二氯二苯基雙馬來醯亞胺、1,1’-[2,2’-雙(三氟甲基){1,1’-聯苯}-4,4’-二基]雙[1H-吡咯-2,5-二酮]等N,N’-二苯基雙馬來醯亞胺類;
2,2-雙[4-(4-馬來醯亞胺苯氧基)苯基]丙烷、2,2-雙[4-(4-馬來醯亞胺苯氧基)苯基]六氟丙烷、2,2-雙[3-甲基-4-(4-馬來醯亞胺苯氧基)苯基]丙烷、2,2-雙[3-甲基-4-(4-馬來醯亞胺苯氧基)苯基]六氟丙烷、2,2-雙[3,5-二甲基-4-(4-馬來醯亞胺苯氧基)苯基]丙烷、2,2-雙[3,5-二甲基-4-(4-馬來醯亞胺苯氧基)苯基]六氟丙烷、2,2-雙[3-乙基-4-(4-馬來醯亞胺苯氧基)苯基]丙烷、2,2-雙[3-乙基-4-(4-馬來醯亞胺苯氧基)苯基]六氟丙烷等雙(苯氧基苯基)烷烴類等。此等可以單獨使用亦可組合2種以上。
此外,作為雙馬來醯亞胺的市售品,可列舉「BMI」、「BMI-70」、「BMI-80」(以上為KI化成股份有限公司製);「BMI-1000」、「BMI-1000H」、「BMI-1100」、「BMI-1100H」、「BMI-2000」、「BMI-2300」、「BMI-3000」、「BMI-3000H」、「BMI-4000」、「BMI-5100」、「BMI-7000」、「BMI-7000H」、「BMI-TMH」(以上為大和化成股份有限公司製)等。
此外,作為雙馬來醯亞胺,亦可以使用由前述的二聚物二胺衍生之雙馬來醯亞胺(以下,稱為具有二聚物二胺骨架的馬來醯亞胺類)。作為該馬來醯亞胺的市售品,可列舉例如「BMI-689」、「BMI-689C」、「BMI-1400」、「BMI-1500」、「BMI-1550」、「BMI-1700」、「BMI-2500」、「BMI-2560」、「BMI-3000-C」、「BMI-3000J」、「BMI-3000 Solution」、「BMI-5000P」、「BMI-5000T」、「BMI-6000」、「BMI-6100」(以上為Designer Molecule Inc.製)等。
作為氰酸酯,可列舉例如2-烯丙基苯酚氰酸酯、4-甲氧基苯酚氰酸酯、2,2-雙(4-異氰酸基苯基)-1,1,1,3,3,3-六氟丙烷、雙酚A氰酸酯、二烯丙基雙酚A氰酸酯、4-苯基苯酚氰酸酯、1,1,1-參(4-氰氧基苯基)乙烷、4-枯基苯酚氰酸酯、1,1-雙(4-氰氧基苯基)乙烷、4,4’-雙酚氰酸酯、及2,2-雙(4-氰氧基苯基)丙烷等。
作為氰酸酯的市售品,可列舉「PRIMASET BTP-6020S」(Lonza Japan股份有限公司製)等。
作為多異氰酸酯,可列舉例如:
亞甲基二異氰酸酯、二亞甲基二異氰酸酯、三亞甲基二異氰酸酯、四亞甲基二異氰酸酯、五亞甲基二異氰酸酯、六亞甲基二異氰酸酯、七亞甲基二異氰酸酯、八亞甲基二異氰酸酯、九亞甲基二異氰酸酯、十亞甲基二異氰酸酯等直鏈脂肪族二異氰酸酯;
三甲基伸丁基二異氰酸酯、三甲基伸戊基二異氰酸酯、三甲基六亞甲基二異氰酸酯等支鏈脂肪族多異氰酸酯;
二環己基甲烷-4,4’-二異氰酸酯、異佛爾酮二異氰酸酯、伸環戊基二異氰酸酯、1,4-伸環己基二異氰酸酯、伸環庚基二異氰酸酯、降莰烯二異氰酸酯、降莰烯甲烷二異氰酸酯、金剛烷二異氰酸酯、環己烷-1,4-二基雙(亞甲基)二異氰酸酯、3,5,5-三甲基伸環己基二異氰酸酯、三伸環癸基二異氰酸酯、氫化苯二甲基二異氰酸酯、氫化甲苯二異氰酸酯、氫化四甲基苯二甲基二異氰酸酯、氫化二苯基甲烷二異氰酸酯、氫化二甲基二苯基甲烷二異氰酸酯、氫化萘二異氰酸酯等脂環族多異氰酸酯;
苯二甲基二異氰酸酯、甲苯二異氰酸酯、伸苯基二異氰酸酯、四甲基苯二甲基二異氰酸酯、二苯基甲烷二異氰酸酯、二甲基二苯基甲烷二異氰酸酯、間四甲基苯二甲基二異氰酸酯、萘二異氰酸酯等芳香族多異氰酸酯等。
此外,作為多異氰酸酯,前述多異氰酸酯的縮二脲體、異氰脲酸酯體、脲基甲酸酯體、加成物亦可以使用。此等多異氰酸酯可以單獨使用亦可組合2種以上。
作為多異氰酸酯的市售品,例如:
就縮二脲體而言,可列舉「Duranate 24A-100」、「Duranate 22A-75P」、「Duranate 21S-75E」(以上為旭化成股份有限公司製)、「Desmodur N3200A」(以上為住友拜耳聚胺酯股份有限公司製)等,
就異氰脲酸酯體而言,可列舉「Duranate TPA-100」、「Duranate TKA-100」、「Duranate MFA-75B」、「Duranate MHG-80B」(以上為旭化成股份有限公司製)、「Coronate HXR」(東曹(TOSOH)股份有限公司製)、「Takenate D-131N」、「Takenate D204EA-1」、「Takenate D-127N」(以上為三井化學股份有限公司製)、「VESTANAT T1890/100」(EVONIK JAPAN股份有限公司製)等,
就脲基甲酸酯體而言,可列舉「Takenate D-178N」(三井化學股份有限公司製)等,
就加成物而言,可列舉「Duranate P301-75E」(旭化成股份有限公司製)、「Takenate D110N」、「Takenate D160N」(以上為三井化學股份有限公司製)、「Coronate L」(東曹股份有限公司製)等。
作為磷化合物,可列舉例如三丁基膦、苯基膦、二苯基膦、甲基二苯基膦、三苯基膦、硼酸鏻化合物、四苯基硼酸四苯基鏻、四苯基硼酸正丁基鏻、癸酸四丁基鏻、硫氰酸(4-甲基苯基)三苯基鏻、硫氰酸四苯基鏻、硫氰酸丁基三苯基鏻等。此等可以單獨使用亦可組合2種以上。
作為酸酐,可列舉例如琥珀酸酐、鄰苯二甲酸酐、馬來酸酐、偏苯三甲酸酐、均苯四甲酸酐、六氫鄰苯二甲酸酐、3-甲基六氫鄰苯二甲酸酐、4-甲基六氫鄰苯二甲酸酐、4-甲基六氫鄰苯二甲酸酐及六氫鄰苯二甲酸酐的混合物、四氫鄰苯二甲酸酐、甲基-四氫鄰苯二甲酸酐、納迪克酸酐、甲基納迪克酸酐、降莰烷-2,3-二甲酸酐、甲基降莰烷-2,3-二甲酸酐、甲基環己烯二甲酸酐、3-十二烯基琥珀酸酐、辛烯基琥珀酸酐等。此等可以單獨使用亦可組合2種以上。
作為胺,可列舉例如前述的二聚物二胺、(a2-1)成分、三乙胺、三丁胺、三伸乙基二胺、二伸乙基三胺、三伸乙基四胺、四伸乙基五胺等脂肪族胺;
三乙醇胺、二甲胺基乙醇等胺基醇;
三聚物三胺等脂環族胺;
1,3-胺基苯、苄基二甲胺、1,3-雙(胺基甲基)苯、2,4,6-參(二甲基胺基甲基)苯酚等芳香族胺。
4-二甲基胺基吡啶、N-胺基乙基呱嗪、1,8-二氮雜雙環[5,4,0]-十一碳烯等雜環胺;
聚醯胺多胺、聚醚多胺、聚酯多胺等。此等可以單獨使用或組合2種以上。
作為咪唑,可列舉例如2-甲基咪唑、1,2-二甲基咪唑、2-乙基-4-甲基咪唑、2-十一基咪唑、2-十七基咪唑、2-苯基咪唑、2-苯基-4-甲基咪唑、1-苄基-2-甲基咪唑、1-苄基-2-苯基咪唑、1-氰乙基-2-甲基咪唑、1-氰乙基-2-十一基咪唑、1-氰乙基-2-乙基-4-甲基咪唑、1-氰乙基-2-苯基咪唑、2-乙基-4-甲基咪唑四苯基硼酸鹽、1-氰乙基-2-十一基咪唑偏苯三甲酸鹽、1-氰乙基-2-苯基咪唑偏苯三甲酸鹽、2,4-二胺基-6-[2’-甲基咪唑基-(1’)]-乙基-均三嗪、2,4-二胺基-6-[2’-十一基咪唑基-(1’)]-乙基-均三嗪、2,4-二胺基-6-[2’-乙基-4’-甲基咪唑基-(1’)]-乙基-均三嗪、2,4-二胺基-6-[2’-甲基咪唑基-(1’)]-乙基-均三嗪異氰脲酸加成物、2-苯基咪唑異氰脲酸加成物、2-苯基-4,5-二羥甲基咪唑、2-苯基-4-甲基-5-羥甲基咪唑、2,3-二氫-1H-吡咯[1,2-a]苯并咪唑、1-十二基-2-甲基-3-苄基咪唑氯化物、2-甲基咪唑啉、2-苯基咪唑啉等。此等可以單獨使用亦可組合2種以上。
作為胍,例如列舉雙氰胺、1-甲基胍、1-乙基胍、1-環己基胍、1-苯基胍、1-(鄰甲苯基)胍、二甲基胍、二苯基胍、三甲基胍、四甲基胍、五甲基胍、1,5,7-三氮雜雙環[4.4.0]癸-5-烯、7-甲基-1,5,7-三氮雜雙環[4.4.0]癸-5-烯、1-甲基雙胍、1-乙基雙胍、1-正丁基雙胍、1-正十八基雙胍、1,1-二甲基雙胍、1,1-二乙基雙胍、1-環己基雙胍、1-烯丙基雙胍、1-苯基雙胍、1-(鄰甲苯基)雙胍等。此等可以單獨使用亦可組合2種以上。
作為酚樹脂,可列舉例如苯酚酚醛清漆樹脂、甲酚酚醛清漆樹脂、雙酚A型酚醛清漆樹脂、三嗪改性苯酚酚醛清漆樹脂、含酚性羥基之磷腈等。此等可以單獨使用亦可組合2種以上。
作為活性酯,可列舉例如日本特開2019-183071號中記載之含有雙環戊二烯基二酚結構之物質、含有萘結構之物質、苯酚酚醛清漆之乙醯化物、苯酚酚醛清漆之苯甲醯化物等。此等可以單獨使用亦可組合2種以上。
作為活性酯的市售品,例如列舉:
作為含有雙環戊二烯基二酚結構之物質的「EXB9451」、「EXB9460」、「EXB9460S」、「HPC-8000」、「HPC-8000H」、「HPC-8000-65T」、「HPC-8150-62T」、「HPC-8000H-65MT」、「HPC-8000L-65MT」、「EXB-8000L」、「EXB-8000L-65MT」、「EXB-8150-65T」(以上為DIC股份有限公司製);
作為含有萘結構之物質的「EXB9416-70BK」(DIC股份有限公司製);
作為苯酚酚醛清漆之乙醯化物的「DC808」(三菱化學股份有限公司製);
作為苯酚酚醛清漆之苯甲醯化物的「YLH1026」、「YLH1030」、「YLH1048」(以上為三菱化學股份有限公司製)等。
活性酯可以使用藉由各種習知的方法而製造的物質,作為其例子,可列舉日本專利第5152445號公報中所記載之使多官能酚化合物與芳香族羧酸類發生反應而得的物質等。
前述的(C)成分可以單獨使用亦可組合2種以上。其中,從硬化物表現出優異的耐熱性之觀點而言,理想為胺,更理想為聚醯胺多胺、聚醚多胺、三聚體三胺。
作為聚醯胺多胺的市售品,可列舉例如「VEGECHEM GREEN V115」、「VEGECHEM GREEN V125」、「VEGECHEM GREEN V140」、「VEGECHEM GREEN V150」、「VEGECHEM GREEN V1460」、「VEGECHEM GREEN V1480」、「VEGECHEM GREEN G250」、「VEGECHEM GREEN G747」(以上為築野食品工業股份有限公司製)、「LUCKAMIDE TD-960」、「LUCKAMIDE TD-984」、「LUCKAMIDE TD-982」(以上為DIC股份有限公司製)等。
作為聚醚多胺的市售品,可列舉例如「PEG#1000 Diamine」(日油股份有限公司製)、「JEFFAMINE」系列(例如「JAFFAMINE D-230」、「JAFFAMINE T-403」等)(HUNTSMAN公司製)、「Baxxodur」系列(BASF公司製)等。
三聚物三胺係將作為油酸等不飽和脂肪酸的三聚物之三聚酸(參照日本特表2013-505345號公報等)的全部羧基取代為一級胺基而得的產物。作為市售品,可列舉「PRIAMINE1071」、「PRIAMINE1073」(以上為Croda Japan股份有限公司製)等。
作為(C)成分的含量,從易於發揮前述的效果之方面而言,以不揮發成分換算,相對於(A)成分100重量份,理想為0.5~10重量份,更理想為0.9~7重量份,進一步理想為1~5重量份。
本發明之樹脂組成物亦可以進一步含有無機填料。
作為無機填料,可列舉例如二氧化矽填料、磷系填料、氟系填料、無機離子交換體填料等。又,二氧化矽填料亦可以使用其表面經矽烷偶聯劑等處理劑改性的二氧化矽填料。此等可以單獨使用亦可組合2種以上。
作為無機填料的市售品,可列舉例如「FB-3SDC」、「SFP-20M」(以上為電化(DENKA)股份有限公司製)、「SC-2500-SPJ」、「SC-2500-SXJ」、「SC-2500-SVJ」、「SC-2500-SEJ」(以上為ADMATECHS股份有限公司製)、「Exolit OP935」(Clariant Chemicals(日文:クラリアントケミカルズ)股份有限公司製)、「KTL-500F」(喜多村股份有限公司製)、「IXE」(東亞合成股份有限公司製)等。
作為無機填料的含量,從硬化物易於為低介電損耗角正切、並且在作為樹脂膜使用時易於提高儲能模量之觀點而言,以不揮發成分換算,相對於(A)成分100重量份,理想為5~70重量份,更理想為10~60重量份,進一步理想為10~50重量份。
本發明之樹脂組成物亦可以進一步含有磷系阻燃劑。
磷系阻燃劑,可列舉聚磷酸或磷酸酯、不具有酚性羥基之磷腈衍生物等。該磷腈衍生物之中,基於阻燃性、耐熱性、耐滲出性等觀點,理想環狀磷腈衍生物。作為環狀磷腈衍生物的市售品,可列舉「SPB-100」(大塚化學股份有限公司製)、「Rabitle FP-300B」(伏見製藥所股份有限公司製)等。
作為磷系阻燃劑的含量,以不揮發成分換算,相對於(A)成分100重量份,理想為0.01~5重量份。
本發明之樹脂組成物中,亦可以含有由通式:W-Si(R
1)
a(OR
2)
3-a(式中,W表示含有與酸酐基反應的官能基之基團,R
1表示氫或碳數1~8的烴基,R
2表示碳數1~8的烴基,a表示0、1或2。)表示之反應性烷氧基矽基化合物。藉由反應性烷氧基矽基化合物,可以將樹脂組成物的層維持為低介電特性,同時調節其熔融黏度。其結果,可以提高該樹脂組成物的層與支撐體的界面密著力(所謂的錨固效應),並且可以抑制從該支撐體的邊緣產生的該硬化層的滲出。
前述通式的W中所含之反應性官能基,可列舉:胺基、環氧基及硫醇基等。
W含有胺基之化合物,可列舉:N-2-(胺基乙基)-3-胺基丙基甲基二甲氧基矽烷、N-2-(胺基乙基)-3-胺基丙基三甲氧基矽烷、3-胺基丙基三甲氧基矽烷、3-胺基丙基三乙氧基矽烷及3-脲基丙基三烷氧基矽烷等。作為W含有環氧基之化合物,可列舉例如:2-(3,4-環氧環己基)乙基三甲氧基矽烷、3-環氧丙氧基丙基甲基二甲氧基矽烷、3-環氧丙氧基丙基三甲氧基矽烷、3-環氧丙氧基丙基甲基二乙氧基矽烷及3-環氧丙氧基丙基三乙氧基矽烷等。作為W含有硫醇基之化合物,可列舉例如:3-巰基丙基三甲氧基矽烷、3-巰基丙基三乙氧基矽烷、3-巰基丙基甲基二甲氧基矽烷及3-巰基丙基甲基二乙氧基矽烷等。此等之中,從反應性及流動控制的效果良好之方面而言,理想W含有胺基之化合物。
作為反應性烷氧基矽基化合物的含量,以不揮發成分換算,相對於(A)成分100重量份,理想為0.01~5重量份。
本發明之樹脂組成物亦可以進一步含有前述的有機溶劑。作為有機溶劑的含量,較佳係將樹脂組成物的不揮發成分濃度理想調節為20~40重量%、更理想調節為25~35重量%。
本發明之樹脂組成物亦可以含有並非(A)成分、(B)成分、(C)成分、無機填料、磷系阻燃劑、反應性烷氧基矽基化合物、有機溶劑中之任一者之物質作為添加劑。
作為添加劑,可列舉例如開環酯化反應催化劑、脫水劑、增塑劑、耐候劑、抗氧化劑、熱穩定劑、潤滑劑、抗靜電劑、增白劑、著色劑、導電劑、脫模劑、表面處理劑、黏度調節劑、無機顏料、有機顏料等。
作為前述添加劑的含量,以不揮發成分換算,相對於(A)成分100重量份,可列舉小於1重量份、小於0.1重量份、小於0.01重量份、0重量份等。
本發明之樹脂組成物可以藉由在將(A)成分、(B)成分及(C)成分,根據需要之無機填料、磷系阻燃劑、反應性烷氧基矽基化合物、有機溶劑以及添加劑加入後進行混合的同時使之溶解而得到。
[接著劑]
本發明中,含有前述樹脂組成物之接著劑亦是實施型態之一。由此,硬化物成為接著性、焊料耐熱性及耐遷移性優異的產品。
[塗覆劑]
本發明中,含有前述樹脂組成物之塗覆劑亦是實施型態之一。由此,可以在低溫下硬化,硬化物表現出優異的接著性、焊料耐熱性及低介電特性,此外在使用硬化物作為樹脂膜時,成為表現出優異的焊料耐熱性及高儲能模量的物品。
[硬化物]
本發明中,含有選自前述樹脂組成物、前述接著劑以及前述塗覆劑所成群中之1種以上之硬化物亦是實施型態之一。作為硬化物的製造方法,可列舉包含以下步驟之方法等:將前述樹脂組成物塗敷於適當的支撐體之步驟;藉由加熱使有機溶劑揮發從而使樹脂組成物硬化之步驟;將該支撐體剝離之步驟等。此外,硬化物的厚度理想為3~40μm。作為支撐體,可列舉剝離紙、剝離膜、後述之支撐膜等。此外,在製造前述硬化物時,亦可以並用前述樹脂組成物與前述樹脂組成物以外的各種習知的樹脂組成物。此外對於所得之硬化物,亦可以剝離支撐體後作為樹脂膜使用。
[接著片材]
本發明之接著片材係在支撐膜的至少單面含有本發明之硬化物。
前述接著片材例如可以藉由在支撐膜之上塗敷本發明之樹脂組成物並經由加熱進行硬化、或者將本發明之硬化物貼合在支撐膜之上而得到。
前述支撐膜,可列舉聚醯亞胺;聚酯;聚醯亞胺-二氧化矽混成物;聚乙烯;聚丙烯;聚對苯二甲酸乙二酯;聚萘二甲酸乙二酯;聚甲基丙烯酸甲酯樹脂;聚苯乙烯樹脂;聚碳酸酯樹脂;丙烯腈-丁二烯-苯乙烯樹脂;由對苯二甲酸乙二酯、苯酚、鄰苯二甲酸、羥基萘甲酸等與對羥基苯甲酸得到的芳香族系聚酯樹脂(所謂的液晶聚合物;「Vecstar」(Kuraray股份有限公司製)等);環烯烴聚合物;氟系樹脂(聚四氟乙烯(PTFE);全氟烷氧基烷烴(PFA)、聚偏二氟乙烯(PVDF)等)等。聚醯亞胺含有本發明之前述聚醯亞胺膜。
在將本發明之樹脂組成物塗敷於前述支撐膜時,作為其塗敷方法,可列舉例如使用逗號式塗佈機、模塗機、刮刀塗佈機、唇式塗佈機等塗佈機等。作為塗敷層的厚度,在乾燥後理想為1~100μm左右,更理想為3~50μm左右。此外,該接著片材之硬化物層亦可以由各種保護膜進行保護。
[附樹脂之銅箔]
本發明之附樹脂之銅箔係包含本發明之硬化物或接著片材以及銅箔。具體而言,其係將本發明之樹脂組成物塗敷至銅箔並加熱硬化而得者,或者將本發明之硬化物貼合至銅箔而得者。作為銅箔,可列舉例如壓延銅箔、電解銅箔,亦可以使用實施各種表面處理(粗化、防鏽化等)之銅箔。防鏽化處理,可列舉使用含有Ni、Zn、Sn等的鍍液之鍍處理、鉻酸鹽處理等所謂的鏡面化處理。
作為銅箔的厚度,理想為1~100μm左右,更理想為2~38μm左右。此外,作為塗敷手段,可列舉出前述方法。
此外,附樹脂之銅箔之樹脂組成物的層或硬化物可以是在加熱下部分硬化或完全硬化的物體。部分硬化之樹脂組成物的層或硬化物處於被稱為所謂的乙階的狀態。此外,作為樹脂組成物的層或硬化物的厚度,理想為0.5~30μm左右。此外,亦可以進一步將樹脂組成物的層貼合至該附樹脂之銅箔的銅箔,製成兩面附樹脂之銅箔。
[覆銅積層板]
本發明之覆銅積層板係包含本發明之附樹脂之銅箔以及銅箔或絕緣性片材。覆銅積層板亦被稱為CCL(覆銅層壓板,Copper Clad Laminate)。具體而言,覆銅積層板係將前述附樹脂之銅箔在加熱下壓接於各種習知的銅箔或絕緣性片材的至少單面或兩面而得的材料。在貼合於單面的情況下,可以在另一面壓接與前述附樹脂之銅箔不同的材料。此外,該覆銅積層板中之附樹脂之銅箔、銅箔及絕緣性片材的張數沒有特別限定。
在一個實施型態中,絕緣性片材理想為預浸料或前述支撐膜。預浸料係指使樹脂浸滲於玻璃布等增強材料並使其硬化至B階段而得到的片狀材料(JIS C 5603)。該樹脂使用本發明之樹脂組成物、酚樹脂、環氧樹脂、聚酯樹脂、液晶聚合物、芳香族聚醯胺樹脂等絕緣性樹脂。作為絕緣性片材的厚度,理想為20~500μm左右。作為加熱、壓接條件,理想為150~280℃左右(更理想為170℃~240℃左右),以及理想為0.5~20MPa左右(更理想為1~8MPa左右)。
[印刷配線板]
本發明之印刷配線板係在本發明之覆銅積層板的銅箔面具有電路圖案。對於在覆銅積層板的銅箔面形成電路圖案的圖案化手段,可列舉:減成法、半加成法。作為半加成法,可列舉以下方法:利用抗蝕劑膜對覆銅積層板的銅箔面進行圖案化後,進行電解鍍銅,除去抗蝕劑,並利用鹼液進行蝕刻。此外,該印刷配線板中的電路圖案層的厚度沒有特別限定。此外,亦可以藉由將該印刷配線板作為芯,並在其之上積層相同的印刷配線板或其他習知的印刷配線板或者印刷電路板從而得到多層基板。積層時,可以並用前述樹脂組成物與前述樹脂組成物以外的其他習知的樹脂組成物。此外,多層基板中的積層數沒有特別限定。此外,每次積層可以插設通孔,並對內部進行鍍處理。前述電路圖案的線寬/線距比理想為1μm/1μm~100μm/100μm左右。此外,前述電路圖案的高度亦理想為1~50μm左右。
[實施例]
以下,列舉實施例對本發明具體地進行說明,但本發明並不特別限定於此等例子。此外,只要沒有特別聲明,「%」均為質量基準。
製造例1
在具備攪拌機、分水器、溫度計及氮氣導入管的反應容器中,投入3,3’,4,4’-二苯甲酮四羧酸二酐(商品名:「BTDA」,EVONIK INDUSTRIES公司製。以下,稱為BTDA。)210.00g、環己酮1008.00g及甲基環己烷201.60g,加熱至60℃。接著,慢慢地添加二聚物二胺(商品名:「PRIAMINE1075」,Croda Japan股份有限公司製。以下,亦記為PRIAMINE1075)318.41g、聚二甲基矽氧烷(商品名:「KF-8010」,信越化學工業股份有限公司製)27.31g後,在120℃歷時14小時進行醯亞胺化反應,由此得到聚醯亞胺(A-1)的溶液(不揮發成分30%)。
製造例2
在與製造例1同樣的反應容器中,投入4,4’-[丙-2,2-二基雙(1,4-伸苯基氧基)]二鄰苯二甲酸二酐(商品名:「BisDA-1000」,SABIC 創新塑膠日本(SABIC Innovative Plastics Japan)有限責任公司製。以下,稱為BisDA。)280.00g、環己酮794.64g及甲基環己烷158.93g,加熱至70℃。接著,慢慢地添加4,4’-二胺基苯基醚(商品名:「ODA」,和歌山精化工業股份有限公司製)71.88g及二聚物二胺(PRIAMINE1075)83.08g後,在110℃歷時12小時進行醯亞胺化反應,由此得到聚醯亞胺(A-2)的溶液(不揮發成分30%)。
製造例3
在與製造例1同樣的反應容器中,投入210.00g的BTDA、環己酮1006.32g及甲基環己烷201.26g,加熱至60℃。接著,慢慢地添加二聚物二胺(PRIAMINE1075)340.02g後,在120℃歷時14小時進行醯亞胺化反應,由此得到聚醯亞胺樹脂(A-3)的溶液(不揮發成分30%)。
製造例4
在與製造例1同樣的反應容器中,投入280.00g的BisDA-1000、乙二醇二甲基醚371.38g及甲苯866.56g,加熱至70℃。接著,慢慢地添加二聚物二胺(PRIAMINE1075)276.92g後,在140℃歷時12小時進行醯亞胺化反應,由此得到聚醯亞胺樹脂(A-4)的溶液(不揮發成分30%)。
實施例1-1
將作為聚醯亞胺之(A-1)333.3g(不揮發成分100.0g)、作為(B)成分之交聯劑之具有甘油三酯基的多官能環氧樹脂(商品名:「Sansocizer E-2000H」,新日本理化股份有限公司製)5.3g(不揮發成分5.3g)、作為硬化劑之聚醯胺多胺(商品名:「VEGECHEM GREEN V-150」,築野食品工業股份有限公司製)1.6g(不揮發成分1.6g)、作為有機溶劑之甲基乙基酮87.4g混合,充分攪拌,得到不揮發成分25%之樹脂組成物(1)。
實施例1-2~1-10,比較例1-1~1-5
變更為表1所示之組成,利用與實施例1-1同樣的方法進行操作,分別得到樹脂組成物(1)。
<接著片材的製作>
以乾燥後的厚度成為25μm的方式,利用間隙塗佈機將各實施例及比較例的樹脂組成物(1)塗敷於市售的聚醯亞胺膜(商品名:「Kapton 100EN」;膜厚25μm,熱膨脹係數:15ppm/℃,東麗杜邦(DU PONT-TORAY)股份有限公司製)(以下,稱為Kapton。)後,在150℃乾燥5分鐘,分別得到接著片材(Kapton/硬化物層)。
<覆銅積層板(1)的製作>
將前述接著片材(Kapton/硬化物層)的硬化物層側重疊於市售的電解銅箔(商品名「F2-WS」,古河電氣工業股份有限公司製)(膜厚18μm)的鏡面側,製作積層體(Kapton/硬化物層/電解銅箔)。接著,置於加壓用支撐體之上,從上方向隔著由相同原材料得到的支撐體在壓力10MPa、溫度100℃的條件下加熱加壓30秒後,在溫度170℃熱硬化30分鐘,由此分別製作覆銅積層板(1)。
<接著強度>
對於前述覆銅積層板(1),根據JIS C 6481(柔性印刷配線板用覆銅積層板的試驗方法),測定剝離強度(N/mm)。結果示於表1。
<焊料耐熱性>
將前述覆銅積層板(1)在溫度23℃、濕度50%的恆溫室中放置24小時後,以銅箔側為下,漂浮於288℃的焊料浴,確認有無發泡,並按照以下基準進行評價。結果示於表1。
(評價基準)
〇:外觀無變化
△:在覆銅積層板的一半有發泡、膨脹、剝離
×:在覆銅積層板的整體有發泡、膨脹、剝離
<耐濕熱性>
將前述覆銅積層板(1)放入溫度85℃、濕度85%的恆溫恆濕機後,經過1000小時後取出。根據JIS C 6481(柔性印刷配線板用覆銅積層板的試驗方法),測定剝離強度(N/mm)。結果示於表1。
<耐遷移性>
在市售的單面附銅箔之聚醯亞胺膜(商品名:「Pyralux TAS124500」,DUPONT公司製)形成電路寬度/電路間距離(L/S)=20μm/40μm的梳形的銅電路(以下,稱作附PI之覆銅積層板。)。將前述接著片材(Kapton/硬化物層)的硬化物層側重疊於附PI之覆銅積層板的銅電路側。接著,置於加壓用支撐體之上,從上方向隔著由相同原材料得到的支撐體在壓力10MPa、溫度100℃的條件下加熱加壓30秒後,在溫度170℃熱硬化30分鐘,由此製作評價用基板。對所得之上述評價用基板在溫度85℃、濕度85%(相對濕度)的條件下施加30V的電壓500小時,並按照以下基準進行評價。又,對於比較例1-1之具有樹脂組成物的接著片材未進行評價。
(評價基準)
〇:即使經過500小時以上亦未觀察到短路
×:在小於500小時時觀察到短路
〔表1〕
※對於各成分的重量份,以不揮發成分重量表示。
聚醯亞胺(重量份) | 交聯劑(重量份) | 硬化劑(重量份) | 接著強度(N/mm) | 焊料耐熱性 | 耐濕熱性 | 耐遷移性 | ||||
實施例1-1 | A-1 | 100 | B-1 | 5.3 | C-1 | 1.6 | 1.0 | 〇 | 1.1 | 〇 |
實施例1-2 | A-1 | 100 | B-1 | 11.1 | C-1 | 3.4 | 1.1 | △ | 1.0 | 〇 |
實施例1-3 | A-3 | 100 | B-1 | 4.4 | C-1 | 1.4 | 1.2 | 〇 | 1.0 | 〇 |
實施例1-4 | A-3 | 100 | B-1 | 8.8 | C-1 | 2.7 | 1.1 | 〇 | 1.1 | 〇 |
實施例1-5 | A-4 | 100 | B-1 | 3.3 | C-1 | 1.0 | 1.3 | 〇 | 0.9 | 〇 |
實施例1-6 | A-4 | 100 | B-1 | 6.6 | C-1 | 2.0 | 1.2 | 〇 | 1.0 | 〇 |
實施例1-7 | A-1 | 100 | B-1 | 5.3 | C-2 | 1.8 | 1.0 | 〇 | 0.8 | 〇 |
實施例1-8 | A-1 | 100 | B-1 | 5.3 | C-3 | 3.3 | 0.9 | 〇 | 0.9 | 〇 |
實施例1-9 | A-1 | 100 | B-1 | 5.3 | C-1 | 3.2 | 1.0 | 〇 | 1.0 | 〇 |
實施例1-10 | A-1 | 100 | B-1 | 5.3 | C-1 | 4.9 | 1.0 | 〇 | 0.8 | 〇 |
比較例1-1 | E-1 | 100 | B-1 | 11.1 | C-1 | 3.4 | 0.1 | × | 0.1 | - |
比較例1-2 | A-1 | 100 | F-1 | 2.2 | C-1 | 1.6 | 0.6 | 〇 | 0.3 | × |
比較例1-3 | A-1 | 100 | F-2 | 2.7 | C-1 | 1.6 | 0.4 | 〇 | 0.4 | × |
比較例1-4 | A-1 | 100 | B-1 | 5.3 | - | 0.9 | × | 0.3 | 〇 | |
比較例1-5 | A-1 | 100 | - | C-1 | 1.6 | 0.9 | × | 0.2 | 〇 |
表1中所示之符號分別表示以下的化合物。
(聚醯亞胺)
・A-1:製造例1的聚醯亞胺
・A-3:製造例3的聚醯亞胺
・A-4:製造例4的聚醯亞胺
・E-1:氫化苯乙烯系樹脂(商品名「塔夫泰克(日文:タフテック)H1062」,旭化成股份有限公司製)
(交聯劑)
・B-1:具有甘油酯骨架之多官能環氧樹脂(商品名:「Sansocizer E-2000H」,新日本理化股份有限公司製)
・F-1:多官能環氧樹脂(商品名:「TETRAD-X」,三菱瓦斯化學股份有限公司製)
・F-2:多官能環氧樹脂(商品名:「jER604」,三菱化學股份有限公司製
(硬化劑)
・C-1:聚醯胺多胺(商品名:「VEGECHEM GREEN V-150」,築野食品工業股份有限公司製)
・C-2:聚醚多胺(商品名:「JAFFAMINE T-403」,HUNTSMAN公司製)
・C-3:三聚物三胺(商品名:「PRIAMINE1071」,Croda Japan股份有限公司製)
實施例2-1
將作為聚醯亞胺之(A-2)333.3g(不揮發成分100.0g)、作為(B)成分之交聯劑之具有甘油三酯基的環氧樹脂(商品名:「Sansocizer E-2000H」,新日本理化股份有限公司製)5.9g(不揮發成分5.9g)、作為硬化劑之三聚物三胺(商品名:「PRIAMINE1071」,Croda Japan股份有限公司製)3.6g(不揮發成分3.6g)、作為有機溶劑之環己酮204.7g混合,充分攪拌,得到不揮發成分20%的樹脂組成物(2)。
實施例2-2~2-6,比較例2-1~2-5
變更為表2所示的組成,利用與實施例2-1同樣的方法進行操作,分別得到樹脂組成物(2)。
<硬化物層(1)的製作>
以乾燥後的厚度成為4μm的方式,利用間隙塗佈機將各實施例及比較例的樹脂組成物(2)塗敷於剝離紙(三榮化研(Sun A. Kaken)股份有限公司製)後,在150℃乾燥5分鐘後,剝下剝離紙,分別得到硬化物層(1)。
<相對介電常數及介電損耗角正切的測定>
將前述硬化物層(1)置於加壓用支撐體之上,進一步在硬化物層(1)側隔著相同的加壓用支撐體在壓力6MPa、220℃的條件下加熱加壓30秒從而進行硬化,由此製作熱硬化後之接著片材(支撐體/硬化物層/支撐體)。從該硬化物層(1)除去加壓用的支撐體,對於硬化物層(1),利用以下的方法,算出相對介電常數(Dk)及介電損耗角正切(Df)。
使用網路分析儀(是德科技(Keysight Technologies)公司製,裝置名:「P5003A」)及測定頻率10.124GHz的分離柱介電質共振器(split post dielectric resonator,QWED公司製),測定沒有任何插入的共振器本體的共振頻率及其峰的Q值。
接著,將前述接著劑層裁切成4cm×5cm從而製作試驗片後,以總厚度成為100μm以上的方式重疊複數片試驗片並插入至共振器內後,測定插入試驗片時的共振頻率及Q值。
相對介電常數(Dk)係由共振器本體與插入試驗片時的共振頻率之差算出,介電損耗角正切(Df)係由共振器本體與插入試驗片時的Q值之差以及共振頻率之差算出。結果示於表2。
<接著片材的製作>
以乾燥後的厚度成為4μm的方式,利用間隙塗佈機將各實施例和比較例的樹脂組成物(2)塗敷於市售的聚醯亞胺膜(商品名:「Kapton 100EN」,膜厚25μm,熱膨脹係數15ppm/℃,東麗杜邦股份有限公司製)(以下,稱為Kapton。)後,在150℃乾燥5分鐘,分別得到接著片材(Kapton/硬化物層)。
<覆銅積層板(2)的製作>
將前述接著片材(Kapton/硬化物層)的硬化物層側重疊於市售的電解銅箔(商品名「F2-WS」,古河電氣工業股份有限公司製)(膜厚18μm)的鏡面側,製作積層體(Kapton/硬化物層/電解銅箔)。接著,置於加壓用支撐體之上,從上方向隔著由相同原材料得到的支撐體在壓力6MPa、溫度220℃的條件下加熱加壓30秒,由此分別製作覆銅積層板(2)。
<貼合>
確認上述覆銅積層板(2)的外觀,按照以下基準進行評價。結果示於表2。
〇:在覆銅積層板上沒有間隙、膨脹
×:在覆銅積層板上有間隙、膨脹
<接著強度>
對於前述覆銅積層板(2),利用與前述同樣的方法測定剝離強度(N/mm)。結果示於表2。
<焊料耐熱性>
對於前述覆銅積層板(2),利用與前述同樣的方法評價焊料耐熱性。結果示於表2。
〔表2〕
※對於各成分的重量份,以不揮發成分重量表示。
聚醯亞胺 (重量份) | 交聯劑 (重量份) | 硬化劑 (重量份) | 無機填料 (重量份) | 貼合 | 相對介電常數 Dk | 介電損耗角正切 Df | 接著強度 (N/mm) | 焊料耐熱性 | |||||
實施例2-1 | A-2 | 100 | B-1 | 5.9 | C-3 | 3.6 | - | 〇 | 2.8 | 0.0039 | 1.1 | 〇 | |
實施例2-2 | A-2 | 100 | B-1 | 3.0 | C-3 | 7.2 | - | 〇 | 2.8 | 0.0045 | 1.0 | △ | |
實施例2-3 | A-2 | 100 | B-1 | 5.9 | C-3 | 7.2 | - | 〇 | 2.8 | 0.0044 | 0.7 | 〇 | |
實施例2-4 | A-2 | 100 | B-1 | 3.0 | C-2 | 2.0 | - | 〇 | 2.8 | 0.0035 | 0.5 | △ | |
實施例2-5 | A-2 | 100 | B-1 | 5.9 | C-3 | 3.6 | D-1 | 12.2 | 〇 | 2.8 | 0.0040 | 1.1 | 〇 |
實施例2-6 | A-2 | 100 | B-1 | 5.9 | C-3 | 3.6 | D-1 | 46.9 | 〇 | 3.0 | 0.0036 | 1.2 | 〇 |
比較例2-1 | A-2 | 100 | F-1 | 1.3 | C-3 | 3.6 | - | 〇 | 2.8 | 0.0044 | 0.2 | △ | |
比較例2-2 | A-2 | 100 | F-2 | 1.5 | C-3 | 3.6 | - | 〇 | 2.7 | 0.0040 | 0.4 | × | |
比較例2-3 | A-2 | 100 | - | C-3 | 3.6 | - | 〇 | 2.9 | 0.0045 | 0.4 | × | ||
比較例2-4 | A-2 | 100 | B-1 | 3.0 | - | - | × | - | |||||
比較例2-5 | A-2 | 100 | F-1 | 1.3 | C-2 | 2.0 | - | 〇 | 2.8 | 0.0038 | 0.4 | × |
表2中所示的符號分別表示以下的化合物。
(聚醯亞胺)
・A-2:製造例2的聚醯亞胺
(交聯劑)
・B-1:具有甘油酯骨架之多官能環氧樹脂(商品名:「Sansocizer E-2000H」,新日本理化股份有限公司製)
・F-1:多官能環氧樹脂(商品名:「TETRAD-X」,三菱瓦斯化學股份有限公司製)
・F-2:多官能環氧樹脂(商品名:「jER604」,三菱化學股份有限公司製)
(硬化劑)
・C-2:聚醚多胺(商品名:「JAFFAMINE T-403」,HUNTSMAN公司製)
・C-3:三聚物三胺(商品名:「PRIAMINE1071」,Croda Japan股份有限公司製)
(無機填料)
・D-1:苯基改性二氧化矽(商品名:「ADMAFINE SC2500-SPJ」,Admatechs股份有限公司製)
實施例3-1
將作為聚醯亞胺之(A-2)333.3g(不揮發成分100.0g)、作為(B)成分之交聯劑之具有甘油三酯基的環氧樹脂(商品名:「Sansocizer E-2000H」,新日本理化股份有限公司製)3.0g(不揮發成分3.0g)、作為硬化劑之聚醯胺多胺(商品名:「VEGECHEM GREEN V-150」,築野食品工業股份有限公司製)1.6g(不揮發成分1.6g)、作為有機溶劑之環己酮185.1g混合,充分攪拌,得到不揮發成分20%的樹脂組成物(3)。
實施例3-2~3-9,比較例3-1~3-2
變更為表3所示的組成,利用與實施例3-1同樣的方法進行操作,分別得到樹脂組成物(3)。
<硬化物層(2)的製作>
以乾燥後的厚度成為12μm的方式,利用間隙塗佈機將各實施例及比較例的樹脂組成物(3)塗敷於剝離紙(三榮化研(Sun A. Kaken)股份有限公司製)後,在150℃乾燥5分鐘,接著在170℃乾燥30分鐘後,剝下剝離紙,得到硬化物層(2)。
<焊料耐熱性>
將前述硬化物層(2)重疊於市售的電解銅箔(商品名「F2-WS」,古河電氣工業股份有限公司製)(膜厚18μm)的鏡面側,以銅箔側為下表面,漂浮於288℃的焊料浴,確認硬化物層的形狀及向銅箔的貼合性,按照以下基準進行評價。結果示於表3。
(評價基準)
○:沒有形狀的變化,並且亦沒有向銅箔的黏合
△:雖然沒有形狀的變化,然而有向銅箔的黏合
×:有形狀的變化,並且亦有向銅箔的黏合
<儲能模量>
在動態黏彈性測定裝置(裝置名:「DMA7100」、日立Hightech Science股份有限公司製)安裝裁割為20mm×40mm的附樹脂之銅箔,在間隔20mm、升溫速度10mm/min、頻率1Hz的條件下進行試驗而算出儲能模量(E’)。數值越高則表示結果越好。結果示於表3。將1.0×10
5Pa以上設為良好。
〔表3〕
※對於各成分的重量份,以不揮發成分重量表示。
聚醯亞胺 (重量份) | 交聯劑 (重量份) | 硬化劑 (重量份) | 無機填料(重量份) | 焊料耐熱性 | 儲能模量 (Pa) | |||||
實施例3-1 | A-2 | 100 | B-1 | 3.0 | C-1 | 1.6 | - | 〇 | 3.0×10 6 | |
實施例3-2 | A-2 | 100 | B-1 | 4.5 | C-1 | 1.6 | - | 〇 | 4.5×10 6 | |
實施例3-3 | A-2 | 100 | B-1 | 1.5 | C-1 | 1.6 | - | △ | 2.1×10 5 | |
實施例3-4 | A-2 | 100 | B-1 | 3.0 | C-1 | 2.4 | - | 〇 | 4.0×10 6 | |
實施例3-5 | A-2 | 100 | B-1 | 3.0 | C-1 | 0.8 | - | △ | 1.0×10 5 | |
實施例3-6 | A-2 | 100 | B-1 | 3.0 | C-2 | 2.0 | - | 〇 | 4.0×10 6 | |
實施例3-7 | A-2 | 100 | B-1 | 3.0 | C-3 | 3.6 | - | 〇 | 2.2×10 6 | |
實施例3-8 | A-2 | 100 | B-1 | 3.0 | C-4 | 2.8 | - | △ | 2.9×10 6 | |
實施例3-9 | A-2 | 100 | B-1 | 3.0 | C-1 | 1.6 | D-2 | 26.1 | 〇 | 5.5×10 6 |
比較例3-1 | A-2 | 100 | - | C-1 | 1.6 | - | × | 1.0×10 4 | ||
比較例3-2 | A-2 | 100 | B-1 | 3.0 | - | - | × | 2.1×10 5 | ||
表3中所示的符號分別表示以下的化合物。
(聚醯亞胺)
・A-2:製造例2的聚醯亞胺
(交聯劑)
・B-1:具有甘油酯骨架的多官能環氧樹脂(商品名:「Sansocizer E-2000H」,新日本理化股份有限公司製)
(硬化劑)
・C-1:聚醯胺多胺(商品名:「VEGECHEM GREEN V-150」,築野食品工業股份有限公司製)
・C-2:聚醚多胺(商品名:「JAFFAMINE T-403」,HUNTSMAN公司製)
・C-3:三聚物三胺(商品名:「PRIAMINE1071」,Croda Japan股份有限公司製)
・C-4:活性酯(商品名:「EPICLON HPC-8000L」,DIC股份有限公司製)
(無機填料)
・D-2:熔融二氧化矽(商品名:「FB-3SDC」,電化(DENKA)股份有限公司製)
Claims (10)
- 一種樹脂組成物,其含有:聚醯亞胺(A)、由通式(1)表示之交聯劑(B)以及(B)成分以外之硬化劑(C),該聚醯亞胺(A)為含有芳香族四羧酸酐(a1)及含二聚物二胺之二胺(a2)之單體群的反應物; 〔化1〕 (在式(1)中,X 1、X 2以及X 3各自獨立地表示具有1個以上的環氧骨架之基團)。
- 如請求項1所述之樹脂組成物,其中,該(C)成分為選自聚醯胺多胺、聚醚多胺及三聚物三胺所成群中之1種以上。
- 如請求項1或2所述之樹脂組成物,其中,該樹脂組成物進一步含有無機填料。
- 一種接著劑,其含有如請求項1所述之樹脂組成物。
- 一種塗覆劑,其含有如請求項1所述之樹脂組成物。
- 一種硬化物,其含有選自如請求項1所述之樹脂組成物、如請求項4所述之接著劑以及如請求項5所述之塗覆劑所成群中之1種以上。
- 一種接著片材,其在支撐膜之至少單面上具有如請求項6所述之硬化物。
- 一種附樹脂之銅箔,其含有: 如請求項6所述之硬化物或如請求項7所述之接著片材、以及 銅箔。
- 一種覆銅積層板,其含有: 如請求項8所述之附樹脂之銅箔、以及 銅箔或絕緣性片材。
- 一種印刷配線板,其在如請求項9所述之覆銅積層板的銅箔面具有電路圖案。
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