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TWI609043B - Resin copper foil, copper-clad laminate and printed wiring board - Google Patents

Resin copper foil, copper-clad laminate and printed wiring board Download PDF

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Publication number
TWI609043B
TWI609043B TW105122437A TW105122437A TWI609043B TW I609043 B TWI609043 B TW I609043B TW 105122437 A TW105122437 A TW 105122437A TW 105122437 A TW105122437 A TW 105122437A TW I609043 B TWI609043 B TW I609043B
Authority
TW
Taiwan
Prior art keywords
resin
copper foil
resin layer
layer
parts
Prior art date
Application number
TW105122437A
Other languages
English (en)
Other versions
TW201716500A (zh
Inventor
米田祥浩
松島敏文
細井俊宏
桑子富士夫
Original Assignee
三井金屬鑛業股份有限公司
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Filing date
Publication date
Application filed by 三井金屬鑛業股份有限公司 filed Critical 三井金屬鑛業股份有限公司
Publication of TW201716500A publication Critical patent/TW201716500A/zh
Application granted granted Critical
Publication of TWI609043B publication Critical patent/TWI609043B/zh

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Classifications

    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/38—Improvement of the adhesion between the insulating substrate and the metal
    • H05K3/386—Improvement of the adhesion between the insulating substrate and the metal by the use of an organic polymeric bonding layer, e.g. adhesive
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    • B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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    • B32B15/088—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyamides
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    • B32B15/09—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyesters
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/748—Releasability
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
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    • B32B2307/752—Corrosion inhibitor
    • B—PERFORMING OPERATIONS; TRANSPORTING
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Description

附樹脂銅箔、覆銅積層板及印刷配線板
本發明係關於附樹脂之銅箔、覆銅積層板及印刷配線板。
作為用於覆銅積層板或印刷配線板之製造的銅箔，已知預浸物等之應提升與樹脂基材的密著性，並於單面上具備樹脂層之附樹脂之銅箔。尚且，預浸物意指於合成樹脂板、玻璃板、玻璃織布、玻璃不織布、紙等之基材使合成樹脂浸漬之複合材料的總稱。
例如專利文獻1(日本專利第5118469號公報)中，揭示於銅箔之單面上具備含有填充劑粒子的樹脂層之附樹脂層銅箔，記載含有填充劑粒子的樹脂層係含芳香族聚醯胺樹脂聚合物、環氧樹脂、及硬化促進劑，且係含以胺系矽烷偶合劑之苯基胺矽烷所處理的填充劑粒子之半硬化樹脂層。
另外，專利文獻2(日本專利第3949676號公報)中，揭示於未施予粗化處理的銅箔之單面上具備確保與樹脂基材的良好貼合密著性之極薄底塗樹脂層的附極薄 接著劑層銅箔，記載使用由20~80重量份之環氧樹脂(含硬化劑)、20~80重量份之芳香族聚醯胺樹脂聚合物、及需要時所添加之硬化促進劑構成的樹脂混合物形成極薄底塗樹脂層。該極薄底塗樹脂層係用以確保與樹脂基材的良好貼合密著性而作為極薄接著劑層發揮功能。
進一步，專利文獻3(國際公開第2013/105650號)中，揭示於銅箔之單面上具備接著劑層的附接著劑層之銅箔，記載接著劑層係相對於聚苯醚化合物100質量部，為由含5質量部以上65質量部以下的苯乙烯丁二烯嵌段共聚物之樹脂組成物構成的層。
不過，印刷配線板係廣泛地用於攜帶用電子機器等電子機器。尤其是伴隨近年攜帶用電子機器等高功能化，進行著應大量的情報之高速處理的信號之高頻化，需求適於高頻用途的印刷配線板。該等高頻用印刷配線板中，期望用以未降低高頻信號的品質而能傳送，降低傳送損失。雖然印刷配線板具備加工至配線圖型之銅箔與絕緣樹脂基材，但是傳送損失係主要是由銅箔所造成導體損失與絕緣樹脂基材所造成電介質損失構成。
〔先行技術文獻〕 〔專利文獻〕
〔專利文獻1〕日本專利第5118469號公報
〔專利文獻2〕日本專利第3949676號公報
〔專利文獻3〕國際公開第2013/105650號
因此，將附樹脂層銅箔採用於高頻用途時，期望能抑制樹脂層所造成電介質損失。為此，需求樹脂層的優異之介電特性，尤其是低介電正切。然而，如引用文獻1及2所揭示之附樹脂層銅箔係能實現與預浸物等的樹脂基材之密著性的提升，介電正切高，因而介電特性劣化，不適合於高頻用途。
本發明者們今般獲得於銅箔之至少單面上具備樹脂層之附樹脂之銅箔中，藉由採用含有環氧樹脂、聚醯亞胺樹脂及芳香族聚醯胺樹脂與同時含有之咪唑系硬化觸媒的樹脂層，樹脂層具有適於高頻用途的優異之介電特性，為覆銅積層板或印刷配線板時，能發揮優異之層間密著性及耐熱性的見識。
因此，本發明的目的在於提供樹脂層具有適於高頻用途的優異之介電特性，為覆銅積層板或印刷配線板時，能發揮優異之層間密著性及耐熱性的附樹脂之銅箔。
根據本發明的一態樣，能提供附樹脂之銅箔，其係於銅箔的至少單面具備樹脂層的附樹脂之銅箔，前述樹脂層含有包含環氧樹脂、聚醯亞胺樹脂、及芳香族聚醯胺樹脂之樹脂混合物與咪唑系硬化觸媒。
根據本發明的其他一態樣，能提供覆銅積層板，其係具備藉由上述態樣之附樹脂之銅箔而成，使前述 樹脂層硬化。
根據本發明的其他一態樣，能提供印刷配線板，其係具備藉由上述態樣的附樹脂之銅箔而成，使前述樹脂層硬化。
10‧‧‧附樹脂之銅箔
12‧‧‧銅箔
14‧‧‧樹脂層
20‧‧‧附樹脂之銅箔
22‧‧‧銅箔
22a‧‧‧電路
24‧‧‧樹脂層
26‧‧‧樹脂基材
28‧‧‧覆銅積層板
〔圖1〕例1~19表示介電特性評估之試料的製作之步驟圖。
〔圖2〕例1~19表示耐熱性評估及銅箔密著性的評估之試料的製作之步驟圖。
附樹脂之銅箔
本發明的附樹脂之銅箔係於銅箔之至少單面上樹脂層具備附樹脂之銅箔。附樹脂之銅箔係樹脂層含有樹脂混合物與咪唑系硬化觸媒。該樹脂混合物係含有環氧樹脂、聚醯亞胺樹脂、及芳香族聚醯胺樹脂。如此一來，藉由採用含有環氧樹脂、聚醯亞胺樹脂及芳香族聚醯胺樹脂與同時含有之咪唑系硬化觸媒的樹脂層，樹脂層具有適於高頻用途的優異之介電特性(低介電正切)，為覆銅積層板或印刷配線板時，能發揮優異之層間密著性及耐熱性。該銅箔及樹脂層間的優異之密著性及耐熱性係製造用以覆銅積層 板或印刷配線板時，防止電路剝落等不利而能實現提升製品生產性。另外，低介電正切係賦予降低電介質損失，其結果能實現降低高頻用途之傳送損失。因此，本發明的附樹脂之銅箔係佳為能適用於作為組網機器的高頻數字化通訊用之印刷配線板用的絕緣層及導體層。該組網機器之例能列舉(i)基站內服務器、路由器等、(ii)公司內組網、(iii)高速攜帶通信的企業系統等。
具體而言，本發明的附樹脂之銅箔係樹脂層硬化的狀態時，樹脂層係頻率1GHz中，佳為具有未達0.020的介電正切，較佳為未達0.015，更佳為未達0.008。尚且，該等介電正切係典型為具有0.001以上的值，更典型為具有0.002以上的值。另外，本發明的附樹脂之銅箔係樹脂層硬化的狀態時，依JIS C6481-1996所測定的樹脂層及銅箔之間的剝離強度為佳為0.20kgf/cm以上，較佳為0.40kgf/cm以上，更佳為0.60kgf/cm以上。尚且，該剝離強度係典型為具有1.4kgf/cm以下的值，更典型為具有1.2kgf/cm以下的值。
樹脂層含有樹脂混合物與咪唑系硬化觸媒。並且，樹脂混合物係含有環氧樹脂、聚醯亞胺樹脂、及芳香族聚醯胺樹脂。
環氧樹脂係只要於分子內具有2個以上的環氧基，能用於電及電子材料用途者就沒有特別限定。環氧樹脂之例係能列舉雙酚A型環氧樹脂、雙酚F型環氧樹脂、雙酚S型環氧樹脂、苯酚酚醛清漆型環氧樹脂、聯苯 酚醛型環氧樹脂、甲酚酚醛清漆型環氧樹脂、脂環式環氧樹脂、縮水甘油胺型環氧樹脂、萘型環氧樹脂、蒽型環氧樹脂、雙環戊二烯型環氧樹脂、及該等任意的組合。保持硬化物的耐熱性之方面而言，佳為芳香族環氧樹脂或多官能環氧樹脂，較佳為酚醛清漆型環氧樹脂、萘型環氧樹脂、甲酚酚醛清漆型環氧樹脂或聯苯酚醛型環氧樹脂。
聚醯亞胺樹脂係附予提升介電特性(尤其是介電正切的降低)。樹脂混合物中聚醯亞胺樹脂的佳含量係相對於環氧樹脂100重量份，為160~340重量份，較佳為200~300重量份，更佳為220~280重量份。為該含量時，邊確保良好耐熱性邊展現優異之介電特性。聚醯亞胺樹脂係只要能獲得所期望的介電特性、密著性及耐熱性就沒有特別限定，從能形成與環氧樹脂良好地相溶之清漆及塗膜方面而言，佳為能溶解於有機溶劑之聚醯亞胺樹脂(以下，又稱為有機溶劑可溶性聚醯亞胺)。能溶解於聚醯亞胺樹脂之該有機溶劑係佳為溶解度參數(SP值)為7.0~17.0者，該有機溶劑之佳例係能列舉甲基乙基酮、甲苯、二甲苯、N-甲基吡咯烷酮、二甲基乙醯胺、二甲基甲醯胺、環戊酮、環己酮、環己烷、甲基環己烷、乙二醇、乙二醇二甲基醚、乙二醇乙酸酯、及該等任意的組合。尤其是從保持硬化後的耐熱性之方面而言，使用分子末端具有至少一個能與環氧基反應之官能基者為佳。具體而言，聚醯亞胺樹脂係作為其末端乃至側鏈之官能基，佳為具有選自由羧基、磺酸基、硫醇基、及酚性羥基構成之 群組的至少1種官能基。藉由具有該等官能基，提升聚醯亞胺樹脂的有機溶劑可溶性及與環氧樹脂的相溶性。另外，熱處理時促進與環氧樹脂之聚合反應，進而，藉由促進聚醯亞胺樹脂彼此之聚合反應，能獲得更耐熱性高、且介電正切低的硬化物。該等之中作為末端或側鏈的官能基使用具有羧基之聚醯亞胺樹脂較佳。
佳有機溶劑可溶性聚醯亞胺能列舉使四羧酸二酐與二胺化合物進行醯亞胺化反應。四羧酸二酐之例能列舉2,2-雙(3,4-二羧基苯基)丙烷二酐、2,2-雙(2,3-二羧基苯基)丙烷二酐、雙(3,4-二羧基苯基)碸二酐、雙(3,4-二羧基苯基)醚二酐、2,2-雙(3,4-二羧基苯基)六氟丙烷二無水物、2,2-雙〔4-(3,4-二羧基苯基)苯〕丙烷二酐、均苯四甲酸二酐、3,3’,4,4’-聯苯四羧酸二酐、2,3,3’，4’-聯苯四羧酸二酐、2,2’,3,3’-聯苯四羧酸二酐、3,3’,4,4’-二苯甲酮四羧酸二酐、2,2’,3,3’-二苯甲酮四羧酸二酐、1,1-雙(3,4-二羧基苯基)乙烷二酐、1,1-雙(2,3-二羧基苯基)乙烷二酐、雙(3,4-二羧基苯基)甲烷二酐、雙(2,3-二羧基苯基)甲烷二酐、1,2,5,6-萘四羧酸二酐、2,3,6,7-萘四羧酸二酐、2,3,5,6-吡啶四羧酸二酐、3,4,9,10-苝四羧酸二酐等、或於該等芳香族環具有烷基或鹵素原子之置換基的化合物、及該等任意的組合等。該等之中就提升樹脂組成物的耐熱性之方面而言，主要為2,2-雙(3,4-二羧基苯基)六氟丙烷二無水物、2,2-雙〔4-(3,4-二羧基苯基)苯〕丙烷二酐、2,3,3’,4’-聯苯四羧酸 二酐、或2,2’,3,3’-聯苯四羧酸二酐之聚醯亞胺樹脂為佳。
另一方面，二胺之例能列舉、3,4’-二胺二苯基硫、4,4’-二胺二苯基硫、3,4’-二胺二苯基醚、4,4’-二胺二苯基醚、3,4’-二胺二苯楓、4,4’-二胺二苯楓、雙〔4-(4-胺苯氧基)苯〕楓、雙〔4-(3-胺苯氧基)苯〕楓、雙(4-胺苯氧基)聯苯、雙〔4-(4-胺苯氧基)苯〕醚、1,4-雙(4-胺苯氧基)苯、1,3-雙(4-胺苯氧基)苯、2,2-雙〔4-(4-胺苯氧基)苯〕六氟丙烷、2,2-雙〔4-(4-胺苯氧基)苯〕丙烷酯、1,3-雙(胺甲基)環己烷及該等任意的組合。
尤其是聚醯亞胺樹脂單體係頻率1GHz中，介電率為2.0~5.0，佳為將介電正切為取得0.001~0.008之範圍的聚醯亞胺樹脂係供給本發明的樹脂組成物，較佳為介電率為2.0~3.0，介電正切為取得0.001~0.005之範圍的聚醯亞胺樹脂。
另外，聚醯亞胺樹脂作為單體之軟化點係就充分地保持硬化物的耐熱性之方面而言，佳為70℃以上，較佳為90℃以上，更佳為120℃以上。軟化點之測定係能依JIS K 7196：2012測定。此處，「聚醯亞胺樹脂單體」意指自聚醯亞胺樹脂所溶解之清漆的溶劑含量為0.1重量%以下時，使溶劑蒸發乾固而得之固化物。另外，能邊保持硬化物之耐熱性邊保持對有機溶劑的溶解性之方面而言，聚醯亞胺樹脂作為單體之玻璃轉移點係130 ℃以上為佳，較佳為150~190℃。該等玻璃轉移點係藉由動態黏彈性測定所特定者。
芳香族聚醯胺樹脂係附予提升樹脂層之耐熱性。樹脂混合物中芳香族聚醯胺樹脂的佳含量係相對於環氧樹脂100重量份，為50~200重量份，較佳為80~150重量份，更佳為90~120重量份。為該等含量時，能邊確保良好介電特性邊展現優異之耐熱性。芳香族聚醯胺樹脂意指藉由芳香族二胺與二羧酸之縮聚合所合成者。用於上述縮聚合之芳香族二胺的例係能列舉3,4’-二胺二苯基醚、4,4’-二胺二苯基醚、4,4’-二胺二苯基甲烷、3,3’-二胺二苯楓、m-二甲苯二胺、3,3’-氧基二苯胺等、及該等任意的組合。另外，用於上述縮聚合之二羧酸的例係能列舉草酸、丙二酸、琥珀酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、鄰苯二甲酸、間苯二甲酸、對苯二甲酸、富馬酸、及該等任意的組合。對芳香族聚醯胺樹脂賦予耐熱性時，佳二羧酸係芳香族二羧酸，芳香族二羧酸之例係能列舉鄰苯二甲酸、間苯二甲酸、對苯二甲酸、富馬酸、及該等任意的組合。尤其是於分子內含有酚性羥基之芳香族聚醯胺樹脂為佳。另外，該等芳香族聚醯胺樹脂係不損及耐熱性的範圍內，作為柔軟鍵於分子內適宜具有對芳香族聚醯胺樹脂賦予可翹性之化學鍵結即可，作為與聚醯胺樹脂之架橋性聚合物合金還能一部分以凝聚狀態存在即可。作為柔軟鍵對芳香族聚醯胺樹脂帶來賦予可翹性之化學鍵結的化合物之例係能列舉例如丁二烯、乙烯-丙 烯共聚物、苯乙烯-丁二烯共聚物、羧酸丁二烯共聚物、丙烯腈-丁二烯共聚物、胺基甲酸乙酯、聚氯丁二烯、聚矽氧烷等。
咪唑系硬化觸媒係與環氧樹脂的硬化反應後作為離子不遊離而作為環氧樹脂之一部分摻入分子結構，能為樹脂層之介電特性或絕緣信頼性優異者。咪唑系硬化觸媒的含量係邊考量樹脂層之組成等諸條件邊適宜決定帶來期望的硬化之量即可，沒有特別限定。咪唑硬化觸媒之例能列舉2-十一烷基咪唑、2-十七烷基咪唑、2-乙基-4-甲基咪唑、2-苯基-4-甲基咪唑、1-氰乙基-2-十一烷基咪唑、1-氰乙基-2-乙基-4-甲基咪唑、2-乙基-4-甲基咪唑、1-氰乙基-2-苯基咪唑、2-苯基-4,5-二羥基甲基咪唑、2-苯基-4-甲基-5-羥基甲基咪唑、2-甲基咪唑、及該等任意的組合。咪唑系硬化觸媒之佳例能列舉2-甲基咪唑、2-乙基-4-甲基咪唑、2-苯基-4-甲基咪唑、2-苯基-4-甲基-5-羥基甲基咪唑，該等之中從樹脂層之半硬化(B階段化)狀態的化學的安定性之方面而言，較佳例能列舉具有苯基之咪唑系硬化觸媒的2-苯基-4-甲基咪唑、2-苯基-4-甲基-5-羥基甲基咪唑。該等之中特佳為能列舉2-苯基-4-甲基-5-羥基甲基咪唑。
依所期望樹脂層還能進一步含有無機填料。藉由無機填料的添加，能期望地降低樹脂層的介電正切。無機填料係能適宜使用能用於樹脂組成物之公知者，沒有特別限定。佳無機填料的例能列舉二氧化矽、氧化鋁、滑 石等之粒子，從降低介電正切之方面而言，特佳為二氧化矽粒子。無機填料的粒徑係沒有特別限定，保持樹脂層之表面平滑性與抑制清漆之混合時的凝聚之方面而言，藉由平均粒徑雷射衍射散射式粒度分布測定所測定之平均粒徑D50為佳為0.01~2.0μm，較佳為0.01~1.0μm，更佳為0.01~0.5μm。樹脂層中無機填料的含量係相對於環氧樹脂、聚醯亞胺樹脂及芳香族聚醯胺樹脂(亦即樹脂固體成分)之總量100重量份，佳為10~100重量份，較佳為10~70重量份，更佳為30~70重量份，特佳為30~50重量份。為該等含量時，介電正切優異，還能回避降低剝離強度。
含有無機填料時，使用施予特定表面處理的填充劑粒子為佳。藉此，使樹脂層與銅箔的密著性更良好，能使該附樹脂層銅箔與預浸物更強固地密著。其結果，能更提升剝離強度，能抑制產生脫層。尤其是佳為填充劑粒子係經矽烷偶合劑進行表面處理者。矽烷偶合劑係能使用胺基官能性矽烷偶合劑、丙烯酸官能性矽烷偶合劑、甲基丙烯酸官能性矽烷偶合劑、環氧官能性矽烷偶合劑、烯烴官能性矽烷偶合劑、巰基官能性矽烷偶合劑、乙烯基官能性矽烷偶合劑等各種矽烷偶合劑。上述中胺基官能性矽烷偶合劑、丙烯酸官能性矽烷偶合劑、甲基丙烯酸官能性矽烷偶合劑、乙烯基官能性矽烷偶合劑等較佳。藉由對於該填充劑粒子相施予上述表面處理，能提升與溶劑之潤濕性，能使填充劑粒子良好地分散於樹脂溶液中。其 結果，能使填充劑粒子均勻地分散於層內而獲得樹脂層。另外，藉由對填充劑粒子施予上述表面處理，而為填充劑粒子與上述樹脂組成物之相溶性良好者，還能為填充劑粒子與樹脂組成物之密著性良好者。胺官能性矽烷偶合劑之例能列舉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、3-三乙氧基矽烷基-N-(1,3-二甲基-亞丁基)丙基胺、N-苯基-3-胺基丙基三甲氧基矽烷等。至於甲基丙烯酸官能性矽烷偶合劑及丙烯酸官能性矽烷偶合劑之例，能列舉3-甲基丙烯醯氧基丙基甲基二甲氧基矽烷、3-甲基丙烯醯氧基丙基三甲氧基矽烷、3-甲基丙烯醯氧基丙基甲基二乙氧基矽烷、3-甲基丙烯醯氧基丙基三乙氧基矽烷、3-丙烯醯氧基丙基三甲氧基矽烷等。乙烯官能性矽烷偶合劑之例，能列舉乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、乙烯基苯基三乙氧基矽烷等。另外，還能使用甲基三甲氧基矽烷、二甲基二甲氧基矽烷、苯基三甲氧基矽烷、甲基三乙氧基矽烷、二甲基二乙氧基矽烷、苯基三乙氧基矽烷等之烷氧基矽烷。使用該等矽烷偶合劑之表面處理方法係沒有特別限定，能使用適當、適宜之方法進行。
樹脂層的厚度係沒有特別限定，佳為0.1~100μm，較佳為0.5~70μm，更佳為1.0~50μm。為該等範圍內的厚度時，藉由塗佈樹脂組成物容易形成樹脂層，同時與銅箔之間也容易確保充分密著性。
樹脂層係還能為以其本身能構成覆銅積層板或印刷配線板之絕緣層。另外，由於樹脂層係作為與覆銅積層板或印刷配線板之預浸物貼合的底塗層，所以於銅箔表面形成者。此時，附樹脂之銅箔的樹脂層係作為底塗層，能提升預浸物與銅箔的密著性。因此，本發明的附樹脂之銅箔係能於樹脂層上具備預浸物。尚且，該等樹脂層係還能為上述樹脂組成物所硬化者，或上述樹脂組成物係能供給作為半硬化(B階段化)狀態之樹脂組成物層，還能供給藉由熱間熱壓之接著硬化作為後步驟。該熱間熱壓能採用予以達到真空後，以溫度150~300℃、溫度保持時間30~300分鐘、壓力10~60kgf/cm2之範圍的條件下進行硬化之真空熱間熱壓法。
銅箔係能為電解製箔或壓延製箔之金屬箔(所謂的生箔)，還能為於至少任一者的面經施予表面處理之表面處理箔的形態。表面處理係為了於金屬箔的表面提升乃至賦予任何性質(例如防銹性、耐濕性、耐藥品性、耐酸性、耐熱性、及與基板之密著性)而進行的各種表面處理。表面處理係能於金屬箔之至少單面進行，還能於金屬箔之兩面進行。對於銅箔相所進行表面處理之例能列舉防銹處理、矽烷處理、粗化處理、阻隔形成處理等。
銅箔之樹脂層側的表面之依JISB0601-2001所測定的十點平均粗糙度Rzjis係2.0μm以下為佳，較佳為1.5μm以下，更佳為1.0μm以下。在於該範圍內時，能期望地降低高頻用途之傳送損失。亦即，藉由愈為高頻時愈 顯著地展現銅箔之表皮效果所增大的銅箔造成降低導體損失，能實現更降低傳送損失。銅箔之樹脂層側的表面之十點平均粗糙度Rzjis的下限值係沒有特別限定，提升與樹脂層的密著性之方面而言，佳為Rzjis係0.005μm以上，較佳為0.01μm以上，更佳為0.05μm以上。
於銅箔之樹脂層側的表面，保持上述十點平均粗糙度Rzjis之數值範圍的範圍中能顯著提升與樹脂層的耐熱密著性之方面而言，佳為形成粒子狀突起。構成該粒子狀突起之金屬係能降低印刷配線板的高頻傳送損失之方面而言，佳為銅。粒子狀突起係能邊確保將與樹脂層之密著性作為物理固著效果，邊將銅箔作為配線層形成時的高頻傳送特性維持高之方面而言，佳為平均粒徑為10~300nm，更佳為50~200nm。另外，從上述之方面而言，佳為粒子狀突起係以40~280個/μm2的面密度存在，較佳為80~250個/μm2。該等粒子狀突起係藉由利用掃描型電子顯微鏡以5,000~50,000倍進行表面觀察而能識別各個粒子。平均粒徑係藉由對於任意20個的粒子之粒子輪廓的面積圓相當徑之平均值能算出。形成粒子狀突起之方法的例能列舉電解處理、噴砂處理、及氧化還原處理，但是從均一形成的粒子之方面而言，佳為電解處理，較佳為銅電解處理。例如電解處理液係藉由使用銅濃度10~20g/L、游離硫酸濃度15~100g/L、9-苯基吖啶濃度100~200mg/L、及氯濃度20~100mg/L的水溶液進行電解電鍍，能良好地形成粒子狀突起。
銅箔的厚度係沒有特別限定，佳為0.1~100μm，較佳為0.15~40μm，更佳為0.2~30μm。在於該等範圍內的厚度時，為形成印刷配線板的配線之一般圖型形成方法，能採用MSAP(Modified‧Semi Additive Process)法、SAP(Semi Additive Process)法、Subtractive process法等工法。然而，銅箔的厚度為例如係10μm以下時等為本發明的附樹脂之銅箔係為了提升操作性能為於具備剝離層及載體的附載體之銅箔的銅箔表面形成樹脂層者。
覆銅積層板
本發明的附樹脂之銅箔係用於印刷配線板用覆銅積層板的製作為佳。亦即，根據本發明的佳態樣，能提供具備上述附樹脂之銅箔覆銅積層板、或使用上述附樹脂之銅箔而獲得之覆銅積層板。此時，使上述附樹脂之銅箔的樹脂層硬化。該覆銅積層板係具備本發明的附樹脂之銅箔及設置於與該附樹脂之銅箔的樹脂層密著之絕緣基材層而成。此時，樹脂層係用以提升與絕緣基材層之密著性作為底塗層發揮功能。附樹脂之銅箔係能設置於絕緣樹脂層之單面，還能設置於兩面。絕緣樹脂層係含有絕緣性樹脂而成。絕緣基材層係佳為經填充玻璃纖維之預浸物、玻璃板、陶瓷板、樹脂薄膜或該等組合。作為預浸物使用的絕緣性樹脂之佳例能列舉環氧樹脂、氰酸酯樹脂、聚醯亞胺樹脂、雙馬來醯亞胺三嗪樹脂(BT樹脂)、聚伸苯醚樹 脂、苯樹脂等。能以複数層構成樹脂層。該等之中意味提升覆銅積層板之傳送特性而言，佳為聚伸苯醚樹脂及聚醯亞胺樹脂，尤其是與本發明的附樹脂之銅箔中的樹脂層之密著性優異者。樹脂薄膜所使用之絕緣樹脂的例能列舉聚醯亞胺樹脂、液晶聚合物等。尚且，能思及各種為了形成覆銅積層板之方法，典型為以於絕緣基材層貼合本發明的附樹脂之銅箔的方法所形成者。其他還能思及於絕緣基材層預先塗佈樹脂層後，於樹脂層的表面貼合銅箔，使絕緣基材層及樹脂層硬化之方法。換言之，本發明的一形態還包含事後具備作為付樹脂之金屬箔的層構成之形態。
印刷配線板
本發明的附樹脂之銅箔佳為用於印刷配線板的製作。亦即，根據本發明的佳態樣，提供具備上述附樹脂之銅箔的印刷配線板、或使用上述附樹脂之銅箔而獲得的印刷配線板。此時，使上述附樹脂之銅箔的樹脂層硬化。根據本態樣之印刷配線板係含有使絕緣樹脂層與銅層依順積層之層構成而成。另外，至於絕緣樹脂層針對覆銅積層板如上述。任一者均印刷配線板係能採用習知之層構成。印刷配線板的具體例能列舉於預浸物的單面或雙面接著本發明的附樹脂之銅箔並硬化而成的積層體上形成電路之單面或雙面印刷配線板，或將該等經多層化之多層印刷配線板等。另外，其他具體例還能列舉為於樹脂薄膜上形成發明的附樹脂之銅箔而形成電路之可撓性印刷配線板、COF、TAB 膠帶、積層多層配線板、於半導體積體電路上交替地重複積層附樹脂之銅箔及形成電路之晶圓上直接增層等。尤其是本發明的附樹脂之銅箔係佳為能適用於作為組網機器中高頻數字化通訊用之印刷配線板用絕緣層及導體層。該組網機器之例能列舉(i)基站內服務器、路由器等、(ii)公司內組網、(iii)高速攜帶通信的企業系統等。
〔實施例〕
藉由以下之例進一步具體地說明本發明。
例1~10及14~19
調製含有樹脂組成物而成的樹脂清漆後，使用該樹脂清漆製造附樹脂之銅箔，並進行評估。具體而言如下述。
(1)樹脂清漆的調製
首先，作為樹脂清漆用原料成分準備以下所示之樹脂成分、咪唑系硬化觸媒及無機填料。尚且，僅例6使用無機填料。
環氧樹脂：新日鐵住金化學股份有限公司製YDCN-704(甲酚酚醛清漆型、環氧當量210g/Eq)
聚醯亞胺樹脂A：荒川化學工業股份有限公司製PIAD-300(末端官能基：羧基、溶劑：環己酮、甲基環己烷及乙二醇二甲基醚的混合液、介電率(1GHz)：2.70、介電正切(1GHz)：0.003、軟化點：140℃)
聚醯亞胺樹脂B：股份有限公司T & K TOKA製P I-2的溶劑稀釋物(末端官能基：羧基、主溶劑：二甲基乙醯胺、介電率(1GHz)：3.0、介電正切(1GHz)：0.018、軟化點：150℃)
芳香族聚醯胺樹脂：日本化藥股份有限公司製BPAM-155(含有酚性羥基之橡膠改性型、羥基當量4000g/Eq)
咪唑系硬化觸媒：四國化成工業股份有限公司製2P4MHZ
無機填料：球狀二氧化矽、Admatechs Corporation製SC1050-DJA(平均粒徑D50=0.3μm、表面胺矽烷處理品)
以表1~3所示之摻合比(重量比)秤重上述樹脂清漆用原料成分。另外，作為有機溶劑混合二甲基乙醯胺25重量份與環戊酮75重量份，製得混合溶劑。將所秤重之樹脂清漆用原料成分及溶劑投入燒瓶，於60℃攪拌使樹脂成分溶解於溶劑，回收樹脂清漆。
(2)樹脂單體之評估
於厚度18μm之電解銅箔的電極面(十點平均粗糙度Rzjis：0.5μm、依JIS B0601-2001測定)以乾燥後塗裝厚度為50μm的厚度塗裝上述(1)所獲得之樹脂清漆。以烘箱使所塗裝之樹脂清漆乾燥，而為半硬化(B階段化)狀態。如圖1所示，製作2片的於銅箔12之單面具備樹脂層14的附樹脂之銅箔10。如圖1所示，積層2片的附樹脂之銅箔10以樹脂層14彼此重疊，之後，熱壓溫度 190℃、溫度保持時間90分鐘、熱壓壓力40kgf/cm2的條件下進行真空熱壓，而樹脂層14為硬化狀態。該經硬化的樹脂層14之厚度為100μm。自熱壓後之積層體蝕刻銅箔而除去，獲得由樹脂層14單獨構成之樹脂薄膜。
<介電特性評估-介電正切>
至於上述所獲得之樹脂薄膜，使用組網分析儀(是德科技股份有限公司製PNA-L N5234A)藉由空洞共振器摂動法測定1GHz之介電正切。依ASTMD2520(JISC2565)進行測定。依以下基準以4階段評估所獲得的介電正切。
評估A：未達0.008(非常良好)
評估B：0.008以上未達0.015(良好)
評估C：0.015以上未達0.020(能接受)
評估D：0.020以上(不良好)
(3)將樹脂層作為底塗層使用之覆銅積層板及評估印刷配線板
(3-1)電解銅箔的製作
藉由以下之方法分別製作厚度為18μm的電解銅箔A~C。
<電解銅箔A>
於硫酸銅溶液中在陰極使用鈦製璇轉電極(表面粗糙度Ra=0.20μm)在陽極使用DSA，以溶液溫度45℃、電 流密度55A/dm2電解，製作原箔。該硫酸銅溶液之組成係銅濃度80g/L、游離硫酸濃度140g/L、3-雙(3-磺丙基)二硫化物濃度30mg/L、二烯丙基二甲基氯化銨聚合物濃度50mg/L、氯濃度40mg/L。之後，對原箔之電解液面依序進行下述(a)~(c)的表面處理。
(a)鋅-鎳覆膜形成
焦磷酸鉀濃度：80g/L
鋅濃度：0.2g/L
鎳濃度：2g/L
液溫：40℃
電流密度：0.5A/dm2
(b)鉻酸鹽層形成
鉻酸濃度：1g/L、pH11
溶液溫度：25℃
電流密度：1A/dm2
(c)矽烷層形成
矽烷偶合劑：3-胺基丙基三甲氧基矽烷(3g/L水溶液)
液處理方法：淋浴處理
所獲得之電解銅箔A的表面處理面係十點平均粗糙度Rzjis為0.5μm(依JIS B0601-2001測定)，沒有粒子狀突起。
<電解銅箔B>
於電解銅箔A的原箔之電解液面側的表面使粒子狀突 起形成，對該粒子狀突起面與電解銅箔A同樣地進行表面處理。藉由硫酸銅溶液(銅濃度：13g/L、游離硫酸濃度55g/L、9-苯基吖啶濃度140mg/L、氯濃度35mg/L)中溶液溫度30℃、電流密度50A/dm2的條件下進行電解形成粒子突起。該電解銅箔B之表面處理面係十點平均粗糙度Rzjis為0.5μm(依照JIS B0601-2001)，粒子狀突起係藉由掃描型電子顯微鏡圖像之平均粒徑為100nm，粒子密度為205個/μm2。
<電解銅箔C>
於電解銅箔A的原箔之電解液面側的表面，使粒子狀突起形成後，與電解銅箔A同樣地進行表面處理。藉由以下之3段階的電解處理形成粒子突起。於硫酸銅溶液(銅濃度：10.5g/L、游離硫酸濃度：220g/L)中溶液溫度30℃、電流密度28A/dm2的條件下進行第1階段之電解處理。於硫酸銅溶液(銅濃度：10.5g/L、游離硫酸濃度：220g/L)中溶液溫度30℃、電流密度16A/dm2的條件下進行第2階段之電解處理。於硫酸銅溶液(銅濃度：70g/L、游離硫酸濃度：220g/L)中溶液溫度52℃、電流密度21A/dm2的條件下進行第3階段之電解處理。所獲得之電解銅箔C的表面處理面係十點平均粗糙度Rzjis為1.8μm(依照JIS B0601-2001)，粒子狀突起係藉由掃描型電子顯微鏡圖像之平均粒徑為1.0μm，粒子密度為1個/μm2。
(3-2)附樹脂之銅箔的製作
於上述所獲得之各電解銅箔的表面處理面以乾燥後塗裝厚度為3.0μm的厚度塗裝上述(1)所獲得的樹脂清漆。以烘箱使所塗裝之樹脂清漆乾燥，為半硬化(B階段化)狀態，而製作於銅箔22的單面具備樹脂層24的附樹脂之銅箔20。
<耐熱性評估-耐熱保持時間>
將預浸物(松下電器產業股份有限公司製MEGTRON-6)積層2片獲得厚度0.2mm之樹脂基材26。如圖2所示，樹脂基材26之兩面上積層2片的附樹脂之銅箔20的樹脂層24側，熱壓溫度190℃、溫度保持時間120分鐘、熱壓壓力30kgf/cm2的條件下進行真空熱壓，將樹脂層24為硬化的狀態獲得覆銅積層板28。如此所硬化的樹脂層24之厚度係3.0μm。尚且，能判斷樹脂層24係覆銅積層板28的製作中發揮功能作為與樹脂基材26連接的底塗層。於耐熱性評估用基板製作使用所獲得的覆銅積層板28。具體而言，將覆銅積層板28切成6.35mm×6.35mm平方。使用熱機械分析裝置(TMA)使加熱至288℃的石英探針與切成覆銅積層板28的表面接觸，而測定直至產生脫層(電路剝離或基材剝離)的時間(分鐘)。依IPC-TM-650(No.2.4.24.1測定該時間。結果係如表1~3所示。
評估AA：120分鐘以上(極好)
評估A：60分鐘以上(非常良好)
評估B：30分鐘以上未達60分鐘(良好)
評估C：10分鐘以上未達30分鐘(能接受)
評估D：未達10分鐘(不良好)
<銅箔密著性-剝離強度>
使用上述所獲得之覆銅積層板28形成剝離強度測定試驗用電路。具體而言，於覆銅積層板28之兩面貼合乾薄膜，形成蝕刻阻劑層。並且，於其兩面之蝕刻阻劑層曝光顯影10mm寬之剝離強度測定試驗用電路，形成蝕刻圖型。之後，以銅蝕刻液進行電路蝕刻，剝離蝕刻阻劑獲得電路22a。將所形成之電路22a自樹脂層24剝離，測定電路22a及樹脂層24之間的剝離強度(kgf/cm)。依JIS C6481-1996測定該剝離強度。結果係如表1~3所示。
評估A：0.60kgf/cm以上(非常良好)
評估B：0.40kgf/cm以上、未達0.60kgf/cm(良好)
評估C：0.20kgf/cm以上、未達0.40kgf/cm(能接受)
評估D：未達0.20kgf/cm(不良好)
<傳送特性評估>
將附樹脂之銅箔20作為最外層，與2片的預浸物(松下電器產業股份有限公司製MEGTRON-6、實厚度68μm)一起積層，製作厚度0.14mm的兩面覆銅積層板 28。之後，藉由將銅箔圖型蝕刻，製作阻抗轉換電路。所選定電路的特性阻抗為50Ω之圖型，測定50GHz中之傳送損失S21(db/cm)。結果係如表3所示。
評估A：-0.55db/cm以上(良好)
評估B：-0.70db/cm以上(能接受)
例11(比較)
使用苯樹脂取代聚醯亞胺樹脂(明和化成股份有限公司製MEH-7500)以外，與例10同樣地調製樹脂清漆及進行各種評估。結果係如表2所示。
例12(比較)
將聚醯亞胺樹脂的摻合比減少至40重量份(相對於環氧樹脂100重量份)，及未添加芳香族聚醯胺樹脂以外，與例1同樣地調製樹脂清漆及進行各種評估。結果係如表2所示。
例13(比較)
未添加聚醯亞胺樹脂，及將芳香族聚醯胺樹脂的摻合比減少至50重量份(相對於環氧樹脂100重量份)以外，與例1同樣地調製樹脂清漆及進行各種評估。結果係如表2所示。

Claims (13)

  1. 一種附樹脂之銅箔，其係於銅箔的至少單面上具備樹脂層的附樹脂之銅箔，前述樹脂層含有包含環氧樹脂、聚醯亞胺樹脂、及芳香族聚醯胺樹脂之樹脂混合物與咪唑系硬化觸媒，其中，相對於前述環氧樹脂100重量份，前述樹脂混合物係將前述聚醯亞胺樹脂含有160~340重量份，且將前述芳香族聚醯胺樹脂含有50~200重量份。
  2. 如請求項1的附樹脂之銅箔，其中，相對於前述環氧樹脂100重量份，前述樹脂混合物係將前述聚醯亞胺樹脂含有200~300重量份，且將前述芳香族聚醯胺樹脂含有80~150重量份。
  3. 如請求項1的附樹脂之銅箔，其中，前述樹脂層係進一步含有無機填料。
  4. 如請求項1的附樹脂之銅箔，其中，前述聚醯亞胺樹脂係作為聚醯亞胺樹脂單體，於頻率1GHz中介電率為2.0~3.0，介電正切為0.001~0.005。
  5. 如請求項1的附樹脂之銅箔，其中，相對於前述環氧樹脂、前述聚醯亞胺樹脂及前述芳香族聚醯胺樹脂之總量100重量份，前述樹脂層係將前述無機填料含有10~100重量份。
  6. 如請求項4的附樹脂之銅箔，其中，前述無機填料係二氧化矽粒子。
  7. 如請求項1的附樹脂之銅箔，其中，前述銅箔之 樹脂層側的表面之依JIS B0601-2001所測定的十點平均粗糙度Rzjis係2.0μm以下。
  8. 如請求項1的附樹脂之銅箔，其中，於前述銅箔之樹脂層側的表面，具備平均粒徑10~300nm的粒子狀突起。
  9. 如請求項1的附樹脂之銅箔，其中，於前述銅箔之樹脂層側的表面，粒子狀突起以40~280個/μm2存在。
  10. 如請求項1的附樹脂之銅箔，其中，在前述樹脂層經硬化之狀態下，前述樹脂層係於頻率1GHz中具有未達0.020的介電正切。
  11. 如請求項1的附樹脂之銅箔，其中，在前述樹脂層經硬化之狀態下，依JIS C6481-1996所測定之前述樹脂層及前述銅箔之間的剝離強度為0.40kgf/cm以上。
  12. 一種覆銅積層板，其係具備如請求項1~11中任一項的附樹脂之銅箔而成，且前述樹脂層係經硬化。
  13. 一種印刷配線板，其係具備如請求項1~11中任一項的附樹脂之銅箔而成，且前述樹脂層係經硬化。
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