TW202300573A - 多孔質聚醯亞胺膜 - Google Patents

多孔質聚醯亞胺膜 Download PDF

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TW202300573A
TW202300573A TW111114775A TW111114775A TW202300573A TW 202300573 A TW202300573 A TW 202300573A TW 111114775 A TW111114775 A TW 111114775A TW 111114775 A TW111114775 A TW 111114775A TW 202300573 A TW202300573 A TW 202300573A
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porous polyimide
polyimide film
dielectric loss
loss factor
less
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TW111114775A
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三島慧
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日商日東電工股份有限公司
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Priority claimed from JP2022014324A external-priority patent/JP2022165379A/ja
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Publication of TW202300573A publication Critical patent/TW202300573A/zh

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Abstract

本發明提供一種即使浸漬於水中亦可抑制介電損耗因數上升之多孔質聚醯亞胺膜。多孔質聚醯亞胺膜於25℃、相對濕度50%之氛圍下靜置24小時後之介電損耗因數T1與於25℃之氛圍下於水中浸漬24小時後之介電損耗因數T2之差為0.0030以下。

Description

多孔質聚醯亞胺膜
本發明係關於一種多孔質聚醯亞胺膜。
已知一種由二胺成分與酸二酐成分之反應產物形成之多孔質聚醯亞胺膜(例如，參照下述專利文獻1)。專利文獻1之實施例中，二胺成分包含苯二胺(PDA)及氧二苯胺(ODA)。 [先前技術文獻] [專利文獻]
[專利文獻1]國際專利WO2018/186486號
[發明所欲解決之問題]
多孔質聚醯亞胺膜根據用途及目的而浸漬於水中。要求多孔質聚醯亞胺膜即使浸漬於水中亦抑制介電損耗因數上升。
然而，專利文獻1揭示之多孔質聚醯亞胺膜存在無法滿足上述要求之問題。
本發明提供一種即使浸漬於水中亦可抑制介電損耗因數上升之多孔質聚醯亞胺膜。 [解決問題之技術手段]
本發明(1)包含一種多孔質聚醯亞胺膜，其於25℃、相對濕度50%之氛圍下靜置24小時後之介電損耗因數T1與於水中25℃之氛圍下浸漬24小時後之介電損耗因數T2之差為0.0030以下。
本發明(2)包含如(1)之多孔質聚醯亞胺膜，其中上述介電損耗因數T2為0.0060以下。
本發明(3)包含如(1)或(2)之多孔質聚醯亞胺膜，其中以UL94標準進行阻燃性試驗時之判定為V-0以上。 [發明之效果]
本發明之多孔質聚醯亞胺膜於水中浸漬後之介電損耗因數T2與於氛圍下靜置後之介電損耗因數T1之差為0.0030以下。因此，即使將多孔質聚醯亞胺膜浸漬於水中亦可抑制介電損耗因數上升。
＜多孔質聚醯亞胺膜＞ 對本發明之多孔質聚醯亞胺膜進行說明。多孔質聚醯亞胺膜具有厚度。多孔質聚醯亞胺膜於面方向上延伸。面方向與厚度方向正交。
多孔質聚醯亞胺膜為多孔質。多孔質聚醯亞胺膜例如具有獨立氣泡結構及/或連續氣泡結構。從確實地抑制浸漬於水中後之介電損耗因數T2上升之觀點出發，多孔質聚醯亞胺膜較佳為具有獨立氣泡結構。
＜於氛圍下靜置後之多孔質聚醯亞胺膜之介電損耗因數T1＞ 多孔質聚醯亞胺膜於25℃、相對濕度50%之氛圍下靜置24小時後之多孔質聚醯亞胺膜之介電損耗因數T1並無限定。再者，靜置之開始時間並無限定。具體而言，可於製造出多孔質聚醯亞胺膜後立刻開始實施靜置，又，可於得到流通之多孔質聚醯亞胺膜時開始實施靜置。
上述多孔質聚醯亞胺膜之介電損耗因數T1係用以獲得用於求出與後述於水中浸漬「24小時」後之介電損耗因數T2之差之基準的介電損耗因數，因此靜置時間設定為與介電損耗因數T2之測定時間之24小時相同之「24小時」。
再者，剛製造完成或得到時之介電損耗因數T0、即靜置24小時前之介電損耗因數T0與靜置24小時後之介電損耗因數T1實質上相同。具體而言，靜置前之介電損耗因數T0與靜置後之介電損耗因數T1之差抑制在例如0.0001以下、進而0.00001以下。
對多孔質聚醯亞胺膜於25℃、相對濕度50%之氛圍下靜置24小時後之多孔質聚醯亞胺膜之介電損耗因數T1進行調整，以使後述差為期望上限以下。具體而言，多孔質聚醯亞胺膜於25℃、相對濕度50%之氛圍下靜置24小時後之多孔質聚醯亞胺膜之介電損耗因數T1例如為0.0028以下，較佳為0.0025以下，更佳為0.0020以下，進而較佳為0.0015以下，特佳為0.0010以下，最佳為0.0008以下。於氛圍下靜置後之介電損耗因數T1之下限並無限定。於氛圍下靜置後之介電損耗因數T1例如超過0.0000，進而為0.0001以上。
使用共振器於10 GHz測定靜置後之多孔質聚醯亞胺膜之介電損耗因數T1。又，上述介電損耗因數T0及測定均與上述相同。
＜於水中浸漬後之多孔質聚醯亞胺膜之介電損耗因數T2＞ 多孔質聚醯亞胺膜於25℃之氛圍下於水中浸漬24小時後之多孔質聚醯亞胺膜之介電損耗因數T2並無限定。對上述於水中浸漬後之多孔質聚醯亞胺膜之介電損耗因數T2進行調整，使下述說明之介電損耗因數之差為期望上限以下。再者，可於製造出多孔質聚醯亞胺膜後立即開始實施浸漬，又，可於得到流通之多孔質聚醯亞胺膜時開始實施浸漬。具體而言，多孔質聚醯亞胺膜於25℃之氛圍下於水中浸漬24小時後之上述多孔質聚醯亞胺膜之介電損耗因數T2例如為0.0060以下，較佳為0.0050以下，更佳為0.0040以下，進而較佳為0.0038以下，特佳為0.0030以下，最佳為0.0025以下，進而0.0020以下較為合適。於水中浸漬後之多孔質聚醯亞胺膜之介電損耗因數T2之下限並無限定。於水中浸漬後之多孔質聚醯亞胺膜之介電損耗因數T2例如超過0.0000，進而為0.0001以上。
＜多孔質聚醯亞胺膜之兩個介電損耗因數之差＞ 本發明中，於25℃、相對濕度50%之氛圍下靜置24小時後之上述介電損耗因數T1與於25℃之氛圍下於水中浸漬24小時後之上述介電損耗因數T2之差為0.0030以下。
若介電損耗因數之上述差超過0.0030，則多孔質聚醯亞胺膜浸漬於水中時無法充分抑制多孔質聚醯亞胺膜之介電損耗因數上升。
再者，若多孔質聚醯亞胺膜浸漬於水中，則介電損耗因數存在上升之傾向，因此介電損耗因數之上述差由從於水中浸漬後之介電損耗因數T2減去於氛圍下靜置後之介電損耗因數T1獲得之值(T2－T1)表示。
介電損耗因數之上述差較佳為0.0025以下，更佳為0.0018以下。
介電損耗因數之上述差之下限並無限定。上述差例如超過0.0000，進而為0.0001以上、0.001以上、0.0013以上、0.0015以上。
＜介電損耗因數以外之物性＞ 10 GHz下之多孔質聚醯亞胺膜之介電常數並無限定。10 GHz下之多孔質聚醯亞胺膜之介電常數例如為2.50以下，較佳為2.00以下，更佳為1.80以下，進而較佳為1.75以下，特佳為1.70以下，最佳為1.60以下。若多孔質聚醯亞胺膜之介電常數為上述上限以下，則具有低介電常數之多孔質聚醯亞胺膜可較好地用於例如第五代(5G)標準之無線通信及/或高速軟性印刷基板(FPC)。又，10 GHz下之多孔質聚醯亞胺膜之介電常數超過1.00。多孔質聚醯亞胺膜之介電常數係使用共振器進行測定。
多孔質聚醯亞胺膜之孔隙率並無限定。多孔質聚醯亞胺膜之孔隙率例如為50%以上，較佳為60%以上，更佳為65%以上，又，例如為95%以下，較佳為80%以下，更佳為70%以下。若多孔質聚醯亞胺膜之孔隙率為上述下限以上，則可降低兩個介電常數。若多孔質聚醯亞胺膜之孔隙率為上述上限以下，則能確保多孔質聚醯亞胺膜之機械強度，操作性優異。
多孔質聚醯亞胺膜之孔隙率係藉由向下式插入介電常數而求出。
多孔質聚醯亞胺膜之介電常數＝空氣之介電常數×孔隙率＋聚醯亞胺樹脂之介電常數×(1－孔隙率)
多孔質聚醯亞胺膜之平均孔徑例如為10 μm以下，較佳為5 μm以下，又，例如為0.1 μm以上，較佳為1 μm以上，更佳為2 μm以上。平均孔徑係藉由剖面SEM照片之圖像解析進行測定。
以阻燃性UL94標準對多孔質聚醯亞胺膜進行阻燃性試驗時之判定例如為V-2以上，較佳為V-1以上，更佳為V-0。若阻燃性試驗之判定為上述基準以上，則多孔質聚醯亞胺膜之阻燃性優異。
多孔質聚醯亞胺膜之厚度並無限定。多孔質聚醯亞胺膜之厚度例如為2 μm以上，較佳為5 μm以上，又，例如為1,000 μm以下，較佳為500 μm以下。
＜多孔質聚醯亞胺膜之原料＞ 多孔質聚醯亞胺膜例如係二胺成分與酸二酐成分之反應產物。換言之，多孔質聚醯亞胺膜之原料例如含有二胺成分及酸二酐成分。
＜二胺成分＞ 二胺成分含有芳香族二胺及/或脂肪族二胺。芳香族二胺及/或脂肪族二胺係二胺成分中之主要成分。
＜芳香族二胺＞ 該芳香族二胺如下述式(1)所示。
[化1]
Figure 02_image001
(式中，Y係選自由單鍵、-COO-、-S-、-CH(CH 3)-、-C(CH 3) 2-、-CO-、-NH-及-NHCO-所組成之群中之至少一個。)
＜芳香族二胺之種類＞ 具體而言，作為二胺成分，可列舉Y為單鍵之4,4'-二胺基聯苯、Y為-COO-之4-胺基苯基-4-胺基苯甲酸酯、Y為-S-之雙(4-胺基苯基)硫醚、Y為-CH(CH 3)-之4,4'-二胺基二苯基乙烷、Y為-C(CH 3) 2-之4,4'-二胺基二苯基丙烷、Y為-CO-之4,4'-二胺基二苯甲酮、Y為-NH-之4,4'-二胺基苯胺、及Y為-NHCO-之4,4'-二胺基苯甲醯苯胺。從進一步降低多孔質聚醯亞胺膜之介電損耗因數之差之觀點出發，較佳可列舉4-胺基苯基-4-胺基苯甲酸酯。再者，4-胺基苯基-4-胺基苯甲酸酯有時僅簡稱為APAB。上述芳香族二胺可單獨使用或併用。從進一步減小上述介電損耗因數之差之觀點及提高阻燃性之觀點出發，較佳可列舉單獨使用APAB。
二胺成分中之芳香族二胺之莫耳分率例如為5莫耳%以上，較佳為10莫耳%以上，更佳為15%以上，又，例如為75莫耳%以下，較佳為60莫耳%以下，更佳為40莫耳%以下。
＜脂肪族二胺＞ 脂肪族二胺含有長鏈之烷基，另一方面，可於分子內含有環狀部分。作為脂肪族二胺，例如可列舉六亞甲基二胺、1,3-雙(胺基甲基)環己烷、及二聚二胺。作為脂肪族二胺，較佳可列舉二聚二胺。二聚二胺係例如用一級胺基取代二聚酸含有之兩個羧基而獲得之胺化合物。二聚酸係不飽和脂肪酸之二聚物。作為不飽和脂肪酸，例如可列舉油酸。二聚二胺例如於日本專利特開2020-172667及日本專利特開2018-168369號公報中有所記載。作為二聚二胺，可使用市售品，具體而言，使用PRIAMINE系列(Croda公司製造)。
二胺成分中之脂肪族二胺之莫耳分率例如為5莫耳%以上，較佳為10莫耳%以上，更佳為15%以上，又，例如為75莫耳%以下，較佳為50莫耳%以下，更佳為30莫耳%以下。
可併用芳香族二胺及脂肪族二胺，又，可單獨使用芳香族二胺，亦可單獨使用脂肪族二胺。較佳可列舉單獨使用芳香族二胺，較佳可列舉單獨使用脂肪族二胺。
＜其他二胺成分＞ 除上述芳香族二胺及/或脂肪族二胺以外，二胺成分可含有例如第2芳香族二胺及第3芳香族二胺。第2芳香族二胺及第3芳香族二胺係二胺成分中之副成分。
＜第2芳香族二胺＞ 第2芳香族二胺含有單個芳香環。作為第2芳香族二胺，例如可列舉苯二胺、二甲基苯二胺、及乙基甲基苯二胺。從機械強度之觀點出發，較佳可列舉苯二胺。作為苯二胺，例如可列舉鄰苯二胺、間苯二胺、及對苯二胺。作為苯二胺，較佳可列舉對苯二胺。對苯二胺有時僅簡稱為PDA。
二胺成分中之第2芳香族二胺之莫耳分率例如為10莫耳%以上，較佳為20莫耳%以上，又，例如為95莫耳%以下，較佳為75莫耳%以下，更佳為65莫耳%以下。
＜第3芳香族二胺＞ 第3芳香族二胺含有複數個芳香環及配置於該等之間之醚鍵或單鍵。作為第3芳香族二胺，例如可列舉氧二苯胺及二胺基二甲基聯苯(又稱為聯甲苯胺)。作為氧二苯胺，例如可列舉3,4'-氧二苯胺及4,4'-氧二苯胺。作為二胺基二甲基聯苯，例如可列舉4,4'-二胺基-2,2'-二甲基聯苯(又稱為間聯甲苯胺)及4,4'-二胺基-3,3'-二甲基聯苯(又稱為鄰聯甲苯胺)。從減小上述介電損耗因數之差之觀點及提高阻燃性之觀點出發，較佳可列舉氧二苯胺，更佳可列舉4,4'-氧二苯胺(又稱為4,4'-二胺基二苯醚)。4,4'-氧二苯胺有時僅簡稱為ODA。
二胺成分中之第3芳香族二胺之莫耳分率例如為5莫耳%以上，較佳為10莫耳%以上，又，例如為95莫耳%以下，較佳為30莫耳%以下。
可併用第2芳香族二胺及第3芳香族二胺，又，可單獨使用第2芳香族二胺，又，可單獨使用第3芳香族二胺。較佳為併用第2芳香族二胺及第3芳香族二胺。
相對於第2芳香族二胺與第3芳香族二胺之總計100莫耳份，上述芳香族二胺及脂肪族二胺之總計莫耳份(較佳為芳香族二胺或脂肪族二胺之莫耳份)例如為5莫耳份以上，較佳為10莫耳份以上，更佳為20莫耳份以上，又，例如為100莫耳份以下，較佳為50莫耳份以下，更佳為30莫耳份以下。
＜酸二酐成分＞ 酸二酐成分例如含有包含芳香環之酸二酐。作為包含芳香環之酸二酐，例如可列舉芳香族四羧酸二酐。作為芳香族四羧酸二酐，例如可列舉苯四羧酸二酐、二苯甲酮四羧酸二酐、聯苯四羧酸二酐、聯苯碸四羧酸二酐、及萘四羧酸二酐。
作為苯四羧酸二酐，例如可列舉苯-1,2,4,5-四羧酸二酐。作為二苯甲酮四羧酸二酐，例如可列舉3,3'-4,4'-二苯甲酮四羧酸二酐及2,2'-3,3'-二苯甲酮四羧酸二酐。作為聯苯四羧酸二酐，例如可列舉3,3'-4,4'-聯苯四羧酸二酐、2,2'-3,3'-聯苯四羧酸二酐、2,3,3',4'-聯苯四羧酸二酐、及3,3',4,4'-二苯醚四羧酸二酐。作為聯苯碸四羧酸二酐，例如可列舉3,3',4,4'-聯苯碸四羧酸二酐。作為萘四羧酸二酐，例如可列舉2,3,6,7-萘四羧酸二酐、1,2,5,6-萘四羧酸二酐、1,2,4,5-萘四羧酸二酐、及1,4,5,8-萘四羧酸二酐。
從機械強度之觀點出發，作為酸二酐成分，較佳可列舉苯四羧酸二酐及聯苯四羧酸二酐，更佳可列舉苯-1,2,4,5-四羧酸二酐及3,3'-4,4'-聯苯四羧酸二酐。再者，由於苯-1,2,4,5-四羧酸二酐亦稱為均苯四甲酸二酐，因此有時僅簡稱為PMDA。3,3'-4,4'-聯苯四羧酸二酐有時僅簡稱為BPDA。
酸二酐成分可單獨使用或併用。較佳可列舉單獨使用苯四羧酸，較佳可列舉併用苯四羧酸二酐及聯苯四羧酸二酐。更佳可列舉單獨使用BPDA，更佳可列舉併用BPDA及PMDA。
當併用苯四羧酸二酐及聯苯四羧酸二酐時，相對於苯四羧酸二酐100莫耳份，聯苯四羧酸二酐之莫耳份例如為5莫耳份以上，較佳為10莫耳份以上，更佳為20莫耳份以上，又，例如為200莫耳份以下，較佳為100莫耳份以下，更佳為50莫耳份以下，進而較佳為30莫耳份以下。
二胺成分之胺基(-NH 2)之莫耳量與酸二酐成分之酸酐基(-CO-O-CO-)之莫耳量例如為等量。
其次，參照圖1說明多孔質聚醯亞胺膜1之製造方法。
該方法中，例如，首先準備包含金屬之基材膜2(括號及假想線)。基材膜2於面方向上延伸。作為金屬，例如可列舉銅、鐵、銀、金、鋁、鎳、及該等之合金(不鏽鋼、青銅)。作為金屬，較佳可列舉銅。基材膜2之厚度例如為0.1 μm以上，較佳為1 μm以上，又，例如為100 μm以下，較佳為50 μm以下。
其次，製備包含聚醯亞胺樹脂之前驅物、多孔化劑、成核劑、及溶劑之清漆，繼而，將清漆塗佈於基材膜2之厚度方向之一個面，形成塗膜。清漆中之多孔化劑、成核劑、及溶劑之種類及調配比率等例如於國際專利WO2018/186486號中有所記載。
聚醯亞胺樹脂之前驅物係上述二胺成分與酸二酐成分之反應產物。為製備聚醯亞胺樹脂之前驅物，調配上述二胺成分、上述酸二酐成分、及溶劑，製備清漆，對該清漆進行加熱，製備前驅物溶液。繼而，於前驅物溶液中調配成核劑及多孔化劑，製備多孔前驅物溶液。
其後，將多孔前驅物溶液塗佈於基材膜2之厚度方向之一個面，形成塗膜。
其後，加熱塗膜使其乾燥，藉此形成前驅物膜。藉由上述加熱，進行溶劑之除去，且製備以成核劑為核之具有聚醯亞胺樹脂前驅物與多孔化劑之相分離結構的前驅物膜。
其後，例如，藉由將超臨界二氧化碳用作溶劑之超臨界萃取法，從前驅物膜中萃取出(提取或除去)多孔化劑。
其後，加熱前驅物膜使其硬化，形成包含聚醯亞胺樹脂之多孔質聚醯亞胺膜1。多孔質聚醯亞胺膜1形成於基材膜2之厚度方向之一個面。
其後，視需要如圖1之實線所示除去基材膜2。例如，使用剝離液溶解基材膜2。作為剝離液，例如可列舉FeCl 3。藉此，獲得多孔質聚醯亞胺膜1。再者，製造後述金屬層積層板10時，保留上述基材膜2作為第1金屬層3，不將其除去。
＜用途＞ 其次，如圖1之假想線及實線所示，說明具備多孔質聚醯亞胺膜1之金屬層積層板10。該金屬層積層板10具備多孔質聚醯亞胺膜1、及以假想線表示之兩個金屬層3、4。
多孔質聚醯亞胺膜1包含於金屬層積層板10中。即，多孔質聚醯亞胺膜1用於以下說明之兩個金屬層3、4之積層。
兩個金屬層3、4包含第1金屬層3及第2金屬層4。第1金屬層3配置於多孔質聚醯亞胺膜1之厚度方向之另一面。作為第1金屬層3之材料，可列舉基材膜2所例示之金屬。較佳可列舉銅。第1金屬層3之厚度例如為0.1 μm以上，較佳為1 μm以上，又，例如為100 μm以下，較佳為50 μm以下。
第2金屬層4配置於多孔質聚醯亞胺膜1之厚度方向之一個面。再者，第2金屬層4可經由未圖示之接著劑層配置於多孔質聚醯亞胺膜1之厚度方向之一個面。作為第2金屬層4之材料，可列舉基材膜2所例示之金屬。第2金屬層4之厚度與第1金屬層3之厚度相同。
對金屬層積層板10之製造方法進行說明。首先，在製造過程中，於具備基材膜2及多孔質聚醯亞胺膜1之積層體20之厚度方向之一個面配置第2金屬層4。另一方面，由於基材膜2包含金屬，因此直接保留基材膜2作為第1金屬層3(轉用作第1金屬層3)。藉此，獲得具備多孔質聚醯亞胺膜1、及分別配置於其厚度方向之一個面及另一面之第2金屬層4及第1金屬層3的金屬層積層板10。
其後，例如，藉由蝕刻等，將第1金屬層3及第2金屬層4形成為圖案。
根據用途及目的，於上述圖案形成前、形成中、及/或形成後，對金屬層積層板10進行加壓。具體而言，對金屬層積層板10進行熱壓。
該金屬層積層板10用於例如第五代(5G)標準之無線通信及/或高速軟性印刷基板(FPC)。
＜一實施方式之作用效果＞ 多孔質聚醯亞胺膜1於水中浸漬後之介電損耗因數T2與於氛圍下靜置後之介電損耗因數T1之差為0.0030以下。因此，即使將多孔質聚醯亞胺膜1浸漬於水中，亦可抑制介電損耗因數上升。其結果，多孔質聚醯亞胺膜1用於需耐水性之用途中。
又，若於水中浸漬後之多孔質聚醯亞胺膜1之介電損耗因數T2為0.0060以下，則多孔質聚醯亞胺膜1可較好地用於需耐水性之用途中。
又，若以UL94標準對多孔質聚醯亞胺膜1進行阻燃性試驗時之判定為V-0以上，則多孔質聚醯亞胺膜1之阻燃性優異。 [實施例]
以下示出了實施例及比較例，進而具體說明本發明。再者，本發明並不限定於任何實施例及比較例。又，以下記載中使用之調配比率(含有比率)、物性值、參數等具體數值可由上述「實施方式」中記載之與該等對應之調配比率(含有比率)、物性值、參數等該記載之上限(定義為「以下」、「未達」之數值)或下限(定義為「以上」、「超過」之數值)代替。
＜實施例1＞ 於具備攪拌機及溫度計之反應裝置中加入PDA(第2芳香族二胺)64.88 g(0.60莫耳)、ODA(第3芳香族二胺)40.05 g(0.20莫耳)、及APAB(式(1)所示之Y為-COO-之芳香族二胺)45.65 g(0.20莫耳)，並添加N-甲基-2-吡咯啶酮(NMP)2300 g作為溶劑，於40℃攪拌20分鐘，製備PDA、ODA及APAB之NMP溶液。再者，NMP溶液含有二胺成分1.00莫耳。
其次，於上述NMP溶液中加入3,3'-4,4'-聯苯四羧酸二酐(BPDA)294.2 g(1.00莫耳)，進而添加N-甲基-2-吡咯啶酮(NMP)18 g，升溫至80℃後，攪拌10小時，獲得聚醯亞胺前驅物溶液。
相對於聚醯亞胺前驅物溶液之固形物成分100質量份，添加作為成核劑之中值粒徑1 μm以下之PTFE粉末3質量份、作為多孔化劑之重量平均分子量為400之聚氧乙烯二甲醚(日油(股)製等級：MM400)150質量份、及2-甲咪唑(四國化成工業(股)製2Mz-H)4質量份，獲得多孔前驅物溶液。將所得多孔前驅物溶液塗佈於包含銅之基材膜2，形成塗膜。其後，將塗膜於135℃乾燥15分鐘，製作前驅物膜。
藉由將該前驅物膜於60℃浸漬於加壓至30 MPa之二氧化碳、並流通4小時，促進多孔化劑之萃取除去、殘存NMP之相分離、及多孔之形成。其後，對二氧化碳進行減壓。
其後，將前驅物膜於真空下、390℃之溫度下加熱大約185分鐘，促進殘存成分之除去及醯亞胺化，藉此獲得配置於基材膜2之厚度方向之一個面的多孔質聚醯亞胺膜1。其後，將基材膜2及多孔質聚醯亞胺膜1(積層體20)浸漬於FeCl 3溶液中，除去基材膜2。
表1中記載了各成分之g數及質量份數。表2中記載了二胺成分及酸二酐成分之莫耳分率。
＜實施例2至實施例4及比較例1＞ 以與實施例1相同之方式，製造多孔質聚醯亞胺膜1。但根據表1及表2更改了配方。再者，表1中，DMAc係作為溶劑之二甲基乙醯胺。
＜評估＞ 對實施例2至實施例4及比較例1各自之多孔質聚醯亞胺膜1測定下述項目。該等之結果(然而，平均孔徑除外)示於表2。
＜介電損耗因數T1＞ 測定多孔質聚醯亞胺膜1之介電損耗因數T1。具體而言，將剛製造完成之多孔質聚醯亞胺膜1於25℃、相對濕度50%之氛圍下靜置24小時。 其後，利用共振器以頻率10 GHz測定多孔質聚醯亞胺膜1。
＜介電損耗因數T2＞ 測定多孔質聚醯亞胺膜1之介電損耗因數T2。具體而言，將剛製造完成之多孔質聚醯亞胺膜1於25℃之氛圍下於水中浸漬24小時。其後，利用共振器以頻率10 GHz測定多孔質聚醯亞胺膜1。
＜介電損耗因數T0＞ 測定實施例1之剛製造完成之多孔質聚醯亞胺膜1之介電損耗因數T0。其結果，確認剛製造完成之多孔質聚醯亞胺膜1之介電損耗因數T0與製造後靜置24小時後之多孔質聚醯亞胺膜1之介電損耗因數T1相同。
＜介電常數＞ 利用共振器以頻率10 GHz測定剛製造完成之多孔質聚醯亞胺膜1之介電常數。
＜孔隙率＞ 將上述求得之介電常數插入下式，求出多孔質聚醯亞胺膜1之孔隙率。
多孔質聚醯亞胺膜之介電常數＝空氣之介電常數×孔隙率＋聚醯亞胺樹脂之介電常數×(1－孔隙率)
＜平均孔徑＞ 藉由剖面SEM照片之圖像解析，測定實施例1及比較例1各自之多孔質聚醯亞胺膜1之平均孔徑。
其結果，實施例1之多孔質聚醯亞胺膜1之平均孔徑為3.6 μm。另一方面，比較例1之多孔質聚醯亞胺膜1之平均孔徑為5.3 μm。
＜阻燃性試驗＞ 以UL94標準對多孔質聚醯亞胺膜1進行阻燃性試驗。基於以下基準，評估由試驗所獲得之判定。 ○：判定為V-0以上。 ×：未判定為V-0以上。
[表1]
表1
調配內容物 實施例1 實施例2 實施例3 實施例4 比較例1
二胺成分 主要成分 芳香族二胺 APAB(g) 45.65 - - - -
脂肪族二胺 PRIAMINE 1075(g) - 21.4 10.7 - -
PRIAMINE 1074(g) - - - 2.79 -
副成分 第2芳香族二胺 PDA(g) 64.88 17.3 19.47 - 129.77
第3芳香族二胺 ODA(g) 40.05 - - - 60.07
聯甲苯胺(g) - - - 13.52 -
酸二酐成分 聯苯四羧酸二酐 BPDA(g) 294.22 58.84 58.84 4.06 441.33
苯四羧酸二酐 PMDA(g) - - - 12.02 -
溶劑 NMP(g) 2300 505 460 - 3264
DMAc(g) - - - 168 -
多孔化劑 聚氧乙烯二甲醚(相對於聚醯亞胺前驅物溶液之固形物成分100份之質量份數) 150 120 120 120 200
[表2]
表2
   實施例1 實施例2 實施例3 實施例4 比較例1
二胺成分 主要成分 芳香族二胺 APAB(mol%) 20 - - - -
脂肪族二胺 PRIAMINE 1075(mol%) - 20 10 - -
PRIAMINE 1074(mol%) - - - 10 -
副成分 第2芳香族二胺 PDA(mol%) 60 80 90 - 80
第3芳香族二胺 ODA(mol%) 20 - - - 20
聯甲苯胺(mol%) - - - 90 -
酸二酐成分 聯苯四羧酸二酐 BPDA(mol%) 100 100 100 20 100
苯四羧酸二酐 PMDA(mol%) - - - 80 -
孔隙率(%) 69 69 61 55 81
介電常數 1.70 1.67 1.93 1.97 1.49
介電損耗因數 T0(剛製造完成) 0.0038 - - - -
T1(製造後於氛圍下靜置24小時) 0.0022 0.0005 0.0019 0.0027 0.0029
T2(製造後於水中浸漬24小時) 0.0038 0.0015 0.0039 0.0044 0.0060
介電損耗因數之差 T2-T1 0.0016 0.0011 0.0020 0.0018 0.0031
阻燃性 UL94 V-0 ○ × × × ○
再者，上述發明作為本發明例示之實施方式而提供，但其僅為例示，不應限定性地進行解釋。該技術領域之業者顯而易見之本發明之變化例包含於後述權利要求之範圍中。
1:多孔質聚醯亞胺膜 2:基材膜 3:第1金屬層 4:第2金屬層 10:金屬層積層板 20:積層體
圖1係本發明之多孔質聚醯亞胺膜之一實施方式之剖視圖。
1:多孔質聚醯亞胺膜
2:基材膜
3:第1金屬層
4:第2金屬層
10:金屬層積層板
20:積層體

Claims (3)

  1. 一種多孔質聚醯亞胺膜，其於25℃、相對濕度50%之氛圍下靜置24小時後之介電損耗因數T1與於25℃之氛圍下於水中浸漬24小時後之介電損耗因數T2之差為0.0030以下。
  2. 如請求項1之多孔質聚醯亞胺膜，其中上述介電損耗因數T2為0.0060以下。
  3. 如請求項1或2之多孔質聚醯亞胺膜，其中以UL94標準進行阻燃性試驗時之判定為V-0以上。
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