TWI778307B - 樹脂組成物、包含其的預浸材、包含其的層疊板、包含其的樹脂覆蓋式金屬箔 - Google Patents

樹脂組成物、包含其的預浸材、包含其的層疊板、包含其的樹脂覆蓋式金屬箔 Download PDF

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TWI778307B
TWI778307B TW108142093A TW108142093A TWI778307B TW I778307 B TWI778307 B TW I778307B TW 108142093 A TW108142093 A TW 108142093A TW 108142093 A TW108142093 A TW 108142093A TW I778307 B TWI778307 B TW I778307B
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Taiwan
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resin
resin composition
organic
inorganic
double bond
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TW108142093A
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TW202028329A (zh
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黃勇善
沈昌補
閔鉉盛
朴惠林
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南韓商Ｌｇ化學股份有限公司
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Abstract

本發明是有關於一種包含黏結劑樹脂及有機-無機複合填 料的樹脂組成物、一種包含樹脂組成物的預浸材、一種包含樹脂組成物的層疊板以及一種包含樹脂組成物的樹脂覆蓋式金屬箔。

Description

樹脂組成物、包含其的預浸材、包含其的層疊 板、包含其的樹脂覆蓋式金屬箔
本發明是有關於一種樹脂組成物、一種包含樹脂組成物的預浸材(prepreg)、一種包含樹脂組成物的層疊板(laminated plate)以及一種包含樹脂組成物的樹脂覆蓋式金屬箔(resin-coated metal foil)。
[相關申請案的交叉參考]
本申請案主張於2018年11月23日向韓國智慧財產局提出申請的韓國專利申請案第10-2018-0146306號的申請日的權益，所述韓國專利申請案的全部揭露內容併入本案供參考。
近來，例如半導體基板、印刷電路板(printed circuit board，PCB)及環氧模製化合物(epoxy molding compound，EMC)等電子部件以及資訊與通訊裝置的訊號頻帶趨於增加。電性訊號的傳輸損耗與介質損耗正切及頻率成比例。因此，較高的頻率會增加傳 輸損耗並導致訊號衰減，從而導致訊號傳輸可靠性的劣化。此外，傳輸損耗被轉換成熱量，且因此，亦可能導致發熱的問題。由於此原因，對在高頻區中具有極低介電損耗正切的絕緣材料的需求正在增長。
此外，隨著當前在半導體裝置及PCB領域中對高積體度、高精細度、高效能等的需求的增加，形勢逐漸改變成需要對半導體裝置進行積體、使印刷電路板具有高密度且同時簡化配線間隔的情況。為滿足該些特性，較佳地使用具有使得傳輸速率能夠增加的低介電係數(permittivity)及用於降低傳輸損耗的低介電損耗特性的材料。
傳統上，為開發此種絕緣材料，已開發出基於聚伸苯基醚(polyphenylene ether，PPE)樹脂(PPE樹脂是具有優異介電性質的熱固性樹脂)的絕緣材料，但是所述絕緣材料具有高熔化黏度(melt viscosity)的問題，在預浸材的可處置性(handleability)、模製可加工性(molding processability)方面存在困難等。此外，將例如多孔填料等有利於低介電性質的填料引入至聚伸苯基醚樹脂中，但是填料的可分散性(dispersibility)低，此導致可加工性(processability)及耐熱性方面的問題，且存在難以以高含量施加填料的問題。
本發明的一目的是提供一種樹脂組成物，所述樹脂組成物會改善黏結劑樹脂與填料之間的相容性，且因此表現出優異的可加工性及耐熱性，且亦同時滿足低熱膨脹係數(coefficient of thermal expansion，CTE)、低介電性質及低介電損耗。
本發明的另一目的是提供一種使用上述樹脂組成物的預浸材、一種使用上述樹脂組成物的層疊板以及一種使用上述樹脂組成物的樹脂覆蓋式金屬箔。
在一個態樣中，提供一種樹脂組成物，所述樹脂組成物包含黏結劑樹脂及有機-無機複合填料，其中所述有機-無機複合填料是其中形成有覆蓋層的有機填料，所述覆蓋層包括利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的無機顆粒。
在另一態樣中，提供一種預浸材，所述預浸材包括：纖維基板；以及所述樹脂組成物，浸漬至纖維基板中。
在又一態樣中，提供一種層疊板，其中層壓有至少二層上述預浸材。
在再一態樣中，提供一種樹脂覆蓋式金屬箔，所述樹脂覆蓋式金屬箔包括金屬箔，且樹脂層位於金屬箔上，且樹脂組成物在所述樹脂層中固化。
在下文中，將更詳細地闡述根據本發明具體實施例的一種樹脂組成物、一種包含樹脂組成物的預浸材、一種包含樹脂組成物的層疊板以及一種包含樹脂組成物的樹脂覆蓋式金屬箔。
在本說明書中，氟系有機填料意指有機填料中含有至少一或多種氟元素的有機填料。
此外，含有含雙鍵官能基的矽烷意指含有含一或多個雙鍵的官能基作為矽烷取代基的矽烷。
此外，(甲基)丙烯酸酯基意在包括丙烯酸酯基與甲基丙烯酸酯基二者。
此外，預浸材意指藉由以下方式而獲得的片狀材料：利用樹脂組成物覆蓋或浸漬纖維基板，且接著藉由加熱而固化至半固化狀態(B階段)。
在本發明的一個實施例中，提供一種樹脂組成物，所述樹脂組成物包含黏結劑樹脂及有機-無機複合填料，其中有機-無機複合填料是其中形成有覆蓋層的有機填料，所述覆蓋層包括利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的無機顆粒。
本發明者已對用於預浸材、層疊板、樹脂覆蓋式金屬箔等的樹脂組成物進行了研究，且藉由實驗發現，使用具有芯-殼結構(core-shell structure)的有機-無機複合填料的樹脂組成物表現出低熱膨脹係數(CTE)、低介電性質及低介電損耗，且亦同時滿足優異的耐熱性及可加工性，所述芯-殼結構由有機填料(芯)及覆蓋層(殼)構成，所述覆蓋層包括利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的無機顆粒。
傳統樹脂組成物中所包含的有機或無機填料在黏結劑樹脂中的可分散性低，且因此導致可加工性、耐熱性等方面的問 題，由此難以以高含量施加填料。
然而，由於有機-無機複合填料在覆蓋層中包括利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的無機顆粒，因此有機-無機複合填料具有顯著優異的可分散性及與黏結劑樹脂的相容性，且因此複合填料不僅會防止可加工性、耐熱性等方面的問題，而且亦會在降低介電性質的同時改善例如吸濕後耐熱性(heat resistance after moisture absorption)等效果。
與具有芯-殼結構的有機-無機複合填料的芯對應的有機填料無特別限制，只要其為此項技術中已知的無機填料即可，但是其可為例如含有氟元素的氟系有機填料。更具體而言，氟系有機填料可為選自由以下組成的群組的一或多者：聚四氟乙烯粉末、四氟乙烯-全氟烷氧基乙烯共聚物(tetrafluoroethylene-perfluoroalkoxyethylene copolymer，PFA)、乙烯-氯三氟乙烯共聚物(ethylene-chlorotrifluoroethylene copolymer)及聚偏氟乙烯(polyfluorovinylidene，PVDF)。
與具有芯-殼結構的有機-無機複合填料的殼對應的覆蓋層包括利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的無機顆粒。
含有含雙鍵官能基的矽烷偶合劑用於改善與黏結劑樹脂的相容性，且其中利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的無機顆粒位於最外部分處的有機-無機複合填料與黏結劑樹脂具有優異的相容性。
含有含雙鍵官能基的矽烷偶合劑意指含有含一或多個雙鍵的官能基作為矽烷偶合劑取代基的矽烷偶合劑。矽烷偶合劑中所含有的含雙鍵官能基可為乙烯基(vinyl group)或(甲基)丙烯酸酯基((meth)acrylate group)。
含有含雙鍵官能基的矽烷偶合劑無特別限制，只要其為此項技術中已知的含有含雙鍵官能基的矽烷偶合劑即可，且其可為例如選自由以下組成的群組的一或多者：乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、對苯乙烯基三甲氧基矽烷、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三乙氧基矽烷及3-丙烯醯氧基丙基三甲氧基矽烷。
此外，無機顆粒無特別限制，只要其為此項技術中已知的無機顆粒且是其表面已利用含有含雙鍵官能基的矽烷偶合劑進行處理的無機顆粒即可。所述無機顆粒的實例包括：二氧化矽，例如天然二氧化矽、熔融二氧化矽、非晶二氧化矽及結晶二氧化矽；水鋁石、氧化鋁、滑石、球形玻璃、碳酸鈣、碳酸鎂、氧化鎂、黏土、矽酸鈣、氧化鈦、氧化銻、玻璃纖維、硼酸鋁、鈦酸鋇、鈦酸鍶、鈦酸鈣、鈦酸鎂、鈦酸鉍、氧化鈦、鋯酸鋇、鋯酸鈣、氮化硼、氮化矽、雲母等。所述無機顆粒的表面利用含有含雙鍵官能基的矽烷偶合劑進行處理。該些無機填料可單獨使用，或者以其中的二或更多者的混合物形式使用。在所述無機填料中，可使用顯示出低熱膨脹係數的熔融二氧化矽。
利用含有含雙鍵官能基的矽烷偶合劑處理無機顆粒的 表面的方法可藉由此項技術中已知的傳統方法來製備。作為一個實例，可藉由將無機顆粒添加至含有矽烷偶合劑的溶液、隨後進行乾燥來製備所述方法，所述矽烷偶合劑含有含雙鍵官能基。
利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的無機顆粒的平均粒度(average particle size)無特別限制，但是例如，平均粒徑(average particle diameter)可為200奈米(nm)或小於200奈米、50至200奈米、50至100奈米或50至70奈米。
製備有機-無機複合填料的方法無特別限制，但是所述方法可藉由對有機填料與利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的無機顆粒進行混合來製備，或者藉由在混合後施加振動來製備。在有機填料的表面上覆蓋利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的無機顆粒的方法可在乾燥狀態下施行。
同時，有機填料與利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的無機顆粒的混合比率不限於此。舉例而言，在有機-無機複合填料中，以100重量份的有機填料計，利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的無機顆粒的含量可為0.001至10重量份、0.005至5重量份或0.01至2重量份。
有機-無機複合填料的平均粒度無特別限制，但是例如，平均粒度可為0.3至5微米(μm)、0.4至4微米或0.5至3微米。若平均粒度小於0.3微米，則存在黏著性(cohesiveness)變高的問題。若平均粒度大於5微米，則可能由於高體積/體積比率而導致難以在生產薄膜時進行應用。
在樹脂組成物中，以100重量份的黏結劑樹脂計，有機-無機複合填料的含量可為20至90重量份、25至85重量份或30至80重量份。
根據一個實施例的樹脂組成物可更包含利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的無機填料。
在樹脂組成物中，以100重量份的黏結劑樹脂計，無機填料的含量可為80重量份或小於80重量份、5至80重量份、10至70重量份、15至60重量份、20至50重量份或25至40重量份。若無機填料的含量過高，則存在介電係數變高的問題。
無機填料是其表面已利用含有含雙鍵官能基的矽烷偶合劑進行處理的無機填料，且無機填料可減小樹脂層與另一層之間的熱膨脹係數(CTE)差異，藉此有效地改善最終產品的彎曲性質、低膨脹性、機械強度(韌性)、較低應力。
無機顆粒無特別限制，只要其為此項技術中已知的無機顆粒且是其表面已利用含有含雙鍵官能基的矽烷偶合劑進行處理的無機顆粒即可。所述無機顆粒的實例包括：二氧化矽，例如天然二氧化矽、熔融二氧化矽、非晶二氧化矽及結晶二氧化矽；水鋁石、氧化鋁、滑石、球形玻璃、碳酸鈣、碳酸鎂、氧化鎂、黏土、矽酸鈣、氧化鈦、氧化銻、玻璃纖維、硼酸鋁、鈦酸鋇、鈦酸鍶、鈦酸鈣、鈦酸鎂、鈦酸鉍、氧化鈦、鋯酸鋇、鋯酸鈣、氮化硼、氮化矽、雲母等。所述無機顆粒的表面利用含有含雙鍵官能基的矽烷偶合劑進行處理。該些無機填料可單獨使用，或者以其中的二或更多者 的混合物形式使用。在所述無機填料中，可使用顯示出低熱膨脹係數的熔融二氧化矽。
製備利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的無機填料的方法無特別限制，且可藉由此項技術中已知的傳統方法來製備。作為一個實例，可藉由將無機顆粒添加至含有矽烷偶合劑的溶液中、隨後進行乾燥來製備所述方法，所述矽烷偶合劑含有含雙鍵官能基。
根據一個實施例的樹脂組成物可包含利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的無機填料以及有機-無機複合填料。藉此，會改善填料與黏結劑樹脂之間的相容性，且因此，可在降低介電性質的同時改善例如吸濕後耐熱性、可加工性及耐熱性等效果。此外，所述樹脂組成物可減小樹脂層與另一層之間的熱膨脹係數(CTE)差異，藉此有效地改善最終產品的彎曲性質、低膨脹性、機械強度(韌性)、較低應力。
根據一個實施例的樹脂組成物中所含有的黏結劑樹脂可無限制地使用，只要其為此項技術中已知的傳統黏結劑樹脂即可，且例如，所述黏結劑樹脂可包括選自由以下組成的群組的一或多者：聚伸苯基醚(polyphenylene ether)樹脂、氰酸酯(cyanate ester)樹脂、雙馬來醯亞胺(bismaleimide)樹脂、丁二烯(butadiene)樹脂、苯氧基(phenoxy)樹脂、聚醯胺醯亞胺(polyamideimide)樹脂、聚醚醯亞胺(polyetherimide)樹脂、聚碸(polysulfone)樹脂、聚醚碸(polyethersulfone)樹脂、聚碳酸酯(polycarbonate) 樹脂及聚醚醚酮(polyether ether ketone)樹脂。
更具體而言，黏結劑樹脂可包括聚伸苯基醚樹脂(a)、雙馬來醯亞胺樹脂(b)、氰酸酯樹脂(c)及/或苯乙烯-丁二烯樹脂(d)。由於該些樹脂與有機-無機複合填料具有更為優異的相容性，因此可在降低介電性質的同時進一步改善吸濕後耐熱性及可加工性。
聚伸苯基醚樹脂(a)可包含在兩端利用烯屬不飽和基(ethylenically unsaturated group)進行官能化的改性伸苯基醚寡聚物或改性聚(伸苯基醚)。在組分(a)兩端官能化的所述兩個烯屬不飽和基可為相同的或不同的。
烯屬不飽和基可為例如：烯基，例如乙烯基、烯丙基、甲基烯丙基、丙烯基、丁烯基、己烯基及辛烯基；環烯基，例如環戊烯基及環己烯基；丙烯酸基、甲基丙烯酸基；或者烯基芳基，例如乙烯基苄基及乙烯基萘基。
製備組分(a)的方法無特別限制，但是例如，可藉由以下方式來製備利用乙烯基苄基進行官能化的組分(a)：將雙官能伸苯基醚寡聚物及氯乙烯基苯溶解於溶劑中，在加熱及攪拌下向其添加鹼以進行反應，且接著對樹脂進行硬化。
藉由凝膠滲透層析(gel permeation chromatograph，GPC)方法得到的組分(a)在聚苯乙烯方面的數目平均分子量(number average molecular weight)可在500至3000克/莫耳(g/mol)或1000至2500克/莫耳範圍內。當組分(a)的數目平均分子量小於 500克/莫耳時，存在使用樹脂組成物形成的預浸材黏合充分的問題。當其超過3000克/莫耳時，在溶劑中的溶解度可能降低。
作為雙馬來醯亞胺樹脂(b)及氰酸酯樹脂(c)，可無特別限制地使用本發明所屬技術領域中眾所習知者。
舉例而言，雙馬來醯亞胺樹脂(b)可為選自由以下組成的群組的一或多種化合物：二苯基甲烷雙馬來醯亞胺，例如4,4’-二苯基甲烷雙馬來醯亞胺；苯基甲烷馬來醯亞胺的寡聚物；伸苯基雙馬來醯亞胺，例如間伸苯基雙馬來醯亞胺；雙酚A二苯基醚雙馬來醯亞胺；3,3’-二甲基-5,5’-二乙基-4,4’-二苯基甲烷雙馬來醯亞胺；4-甲基-1,3-伸苯基雙馬來醯亞胺；以及1,6-雙馬來醯亞胺-(2,2,4-三甲基)己烷。
此外，舉例而言，氰酸酯樹脂(c)可為選自由以下組成的群組的一或多種化合物：酚醛清漆型氰酸酯樹脂、雙環戊二烯型氰酸酯樹脂、雙酚型氰酸酯樹脂及其部分三嗪化預聚物(partially triazinated prepolymer)。
苯乙烯-丁二烯樹脂(d)是苯乙烯與丁二烯的共聚物樹脂，在室溫下是液體，且可具有約5%至50%的苯乙烯含量。此外，苯乙烯-丁二烯樹脂(d)可具有-35℃至0℃或-30℃至-5℃的玻璃轉變溫度(glass transition temperature)(Tg)以及1000至50000克/莫耳或2000至10000克/莫耳的數目平均分子量。
根據一個實施例的樹脂組成物可更包含選自由以下組成的群組的一或多種添加劑：固化劑、阻燃劑、紫外線(ultra-violet， UV)屏蔽劑、調平劑、增稠劑、顏料、分散劑及抗氧化劑。
作為固化劑，可無限制地使用此項技術中已知的傳統固化劑，且舉例而言，所述固化劑可為選自由以下的一或多種固化劑：醯胺系固化劑、聚胺系固化劑、酸酐固化劑、苯酚酚醛清漆型固化劑、聚硫醇固化劑、第三胺固化劑、咪唑固化劑及金屬配位催化劑。具體而言，金屬配位催化劑可為乙酸鈷(II)，其可促進黏結劑樹脂中可能包含的氰酸酯的三嗪鍵合。
以樹脂組成物的總重量計，樹脂組成物中固化劑的含量可為0.1重量%至10重量%、0.2重量%至8重量%或0.5重量%至5重量%。
作為阻燃劑，可無限制地使用此項技術中已知的傳統阻燃劑，且所述阻燃劑的實例可為含有溴或氯的鹵素阻燃劑；磷系阻燃劑，例如磷酸三苯酯、磷酸三甲苯酯(tricresylphosphate)、三-二氯丙基磷酸酯(trisdichloropropyl phosphate)及磷腈；銻系阻燃劑，例如三氧化二銻；由如氫氧化鋁及氫氧化鎂等無機物質構成的阻燃劑。
以樹脂組成物的總重量計，樹脂組成物中阻燃劑的含量可為0.1重量%至10重量%、0.2重量%至8重量%或0.5重量%至5重量%。若阻燃劑的含量小於0.1重量%，則阻燃劑可能無法具有阻燃性，而若阻燃劑的含量超過10重量%，則電性特性可能劣化。
在本發明的另一實施例中，提供一種預浸材，所述預浸 材包括：纖維基板；以及所述樹脂組成物，浸漬至纖維基板中。
纖維基板無特別限制，但是纖維基板的實例可包括選自由以下組成的群組的一或多者：玻璃纖維、玻璃紙、玻璃纖維非織織物(玻璃網(glass web))、玻璃布、芳香族聚醯胺纖維、芳香族聚醯胺紙、聚酯纖維、碳纖維、無機纖維及有機纖維。
纖維基板可利用含有含雙鍵官能基的矽烷偶合劑進行表面處理。
當將樹脂組成物浸漬至利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的纖維基板中時，由於纖維基板與樹脂組成物中所含有的無機填料及有機-無機複合填料二者含有含雙鍵官能基，因此所述二者之間的相容性優異，由此，介電性質得到改善，吸濕後耐熱性及可加工性得到進一步改善，且因此可開發出高頻材料。
利用含有含雙鍵官能基的矽烷偶合劑處理纖維基板的表面的方法可藉由此項技術中已知的傳統方法來製備。利用含有含雙鍵官能基的矽烷偶合劑處理纖維基板的表面的方法可藉由此項技術中已知的常用方法來生產。作為一個實例，可藉由將纖維基板添加至含有矽烷偶合劑的溶液、隨後進行乾燥來製備所述方法，所述矽烷偶合劑含有含雙鍵官能基。
纖維基板的厚度無特別限制，且可例如在0.01至0.3毫米範圍內。
用於生產預浸材的方法無特別限制，且可根據此項技術 中已知的生產方法來製備。
預浸材指代藉由以下方式而獲得的片狀材料：將樹脂組成物覆蓋或浸漬至利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的纖維基板上，且接著藉由加熱固化至半固化狀態(B階段)。此時，加熱溫度及時間無特別限制，且例如，加熱溫度可為約20℃至200℃或70℃至170℃，且加熱時間可在約1至10分鐘範圍內。
除上述方法以外，預浸材可藉由已知的熱熔法、溶劑法或此項技術中已知的類似方法來生產。溶劑法是將樹脂基板浸漬至清漆(varnish)中且接著對其進行乾燥的方法，清漆是藉由將用於預浸材形成的樹脂組成物溶解於有機溶劑中而形成。當採用此種溶劑方法時，一般使用清漆。將樹脂組成物浸漬至纖維基板中的方法的實例可包括將纖維基板浸沒於清漆中的方法、藉由各種覆蓋器將清漆施加至基板的方法、藉由噴塗將清漆噴塗至基板上的方法等。此時，當纖維基板浸沒於樹脂清漆中時，可改善樹脂組成物對纖維基板的可浸漬性(impregnability)，且因此是較佳的。
當製備清漆時，有機溶劑的實例可包括：酮，例如丙酮、甲基乙基酮及環己酮；乙酸酯，例如乙酸乙酯、乙酸丁酯、溶纖劑乙酸酯、丙二醇單甲醚乙酸酯及卡必醇乙酸酯；溶纖劑；卡必醇，例如丁基卡必醇；芳香烴，例如甲苯及二甲苯；二甲基甲醯胺；二甲基乙醯胺；N-甲基吡咯啶酮；四氫呋喃等。作為有機溶劑，可單獨使用一種類型的有機溶劑，或者可以組合形式使用二或更多種 類型的有機溶劑。
此外，熱熔法可為以下一種方法：在所述方法中，將樹脂組成物覆蓋在相對於樹脂組成物具有優異可釋放性(releasability)的釋放紙(release paper)上，而不將樹脂組成物溶解於有機溶劑中且接著層疊於片狀纖維基板上，或者直接藉由鑄模覆蓋器(die coater)進行覆蓋。此外，樹脂組成物可藉由在加熱及按壓條件下對包含熱固性樹脂組成物的黏合膜進行連續熱層疊來生產，所述熱固性樹脂組成物自片狀加強基板的兩側層疊於支架上。
在又一實施例中，提供一種層疊板，其中層壓有至少二層上述一個實施例的上述預浸材。
舉例而言，層疊板可藉由以下方式來生產：層疊上述實施例的預浸材中的一或多者，可選地，在預浸材的一側或兩側上搭疊金屬箔，且接著對所得產品進行加熱及按壓。
層疊板生產期間的加熱及按壓條件無特別限制，但是可在140℃至220℃的溫度範圍內施加70至800磅/平方吋(pounds per square inch，psi)的壓力。在此種範圍內，對於層疊板的層間黏合性、耐熱性、可靠性等而言可為有利的。
此外，作為在層疊板生產期間用於加熱及按壓的裝置，可使用多級壓機、多級真空壓機、連續模製機、高壓釜模製機等，但是上述實施例的層疊板不限於此。
當在層疊板生產期間使用金屬箔時，儘管無特別限制， 但是由銅、鋁、鎳、鎳磷、鎳錫合金、鎳鐵合金、鉛及鉛錫合金中的一或多種金屬製成的金屬箔可作為一個片材或多個片材進行使用。
在本發明的另一實施例中，提供一種樹脂覆蓋式金屬箔，所述樹脂覆蓋金屬箔包括：金屬箔；以及樹脂層，位於金屬箔上，且上述實施例的樹脂組成物在樹脂層中固化。
舉例而言，樹脂覆蓋式金屬箔可藉由以下方式來生產：製備尚未加工成預浸材的樹脂組成物作為清漆，將其覆蓋至金屬箔，隨後進行乾燥。
與用於製備預浸材的清漆組成物相似，用於利用樹脂生產金屬箔的清漆包含溶劑，但是可更包含固化劑、固化催化劑等。
作為金屬箔，可無限制地使用由此項技術中已知的傳統金屬或合金製成的金屬箔。在此種情形中，金屬箔可為銅箔，且可使用的銅箔的實例包括CFL(TZA_B、HFZ_B)、三井(Mitsui)(HSVSP、MLS-G)、日光(Nikko)(RTCHP)、古河(Furukawa)、伊爾新(ILSIN)等。
銅箔包括藉由滾製法(rolling method)及電解法(electrolytic method)生產的所有銅箔。此處，銅箔可經歷防銹處理，以防止其表面被氧化及腐蝕。
在金屬箔中，在樹脂組成物與固化樹脂層接觸的一個表面上亦可形成預定表面粗糙度(Rz)。在此種情形中，表面粗糙度(Rz)無特別限制，但是可例如在0.6至3.0微米範圍內。
此外，金屬箔的厚度無特別限制，但是慮及最終產品的厚度及機械性質，可小於5微米或者為1至3微米。
由於根據本發明的樹脂組成物同時滿足低熱膨脹係數(CTE)、低介電性質、低介電損耗、高耐熱性及優異可加工性，因此使用所述樹脂組成物的預浸材、層疊板、樹脂覆蓋式金屬箔等可容易地提供用於例如汽車、大型電腦及伺服器等組件中。
在下文中，將參照實例更詳細地闡述本發明。然而，該些實例僅用於說明目的，且本發明的範圍不受該些實例所限制。
實例1至4及比較例1至4
根據下表1中所示的組成對黏結劑樹脂、無機填料及有機-無機複合填料進行了混合，並攪拌了4小時以製備實例及比較例的樹脂組成物。
Figure 108142093-A0305-02-0018-1
Figure 108142093-A0305-02-0019-2
-聚伸苯基醚：OPE-2st-1200，可自三菱瓦斯化學股份有限公司(Mitsubishi Gas Chemical Company,Inc.，MGC)獲得
-雙馬來醯亞胺樹脂：BMI-5100，可自大和化成(DAIWA Kasei)獲得
-氰酸酯樹脂：ULL-950S可自龍沙有限公司(Lonza Ltd.)獲得
-苯乙烯-丁二烯橡膠：瑞康181(Ricon181)，可自克雷威利(Cray Valley)獲得
-無機填料：利用乙烯基矽烷(乙烯基三甲氧基矽烷)進行表面處理的漿料型填料(二氧化矽)(固體含量為70%)，平均粒度為0.5微米，SC2050，可自雅都瑪(Admatechs)獲得
-有機-無機複合填料：聚四氟乙烯**覆蓋有二氧化矽*，平均粒度為3微米，比表面積(specific surface area)為1.5平方米/克(m2/g)，可自雅都瑪獲得
*二氧化矽：利用乙烯基矽烷(乙烯基三甲氧基矽烷)進行表 面處理的二氧化矽，平均粒度為150奈米，可自雅都瑪獲得
**聚四氟乙烯，平均粒度為3微米，TFW-3000FK，可自誠新公司(Seishin Corporation)獲得
-phr：是「每百份樹脂(parts per hundred resin)」的縮寫，且是無機填料及有機-無機複合填料的使用單位。具體而言，其是以100重量份的黏結劑樹脂計，無機填料及有機-無機複合填料中的每一者的含量(重量份)。
評價
藉由以下方法評價了實例及比較例的物理性質，且評價結果示於下表2中。
(1)評價用預浸材及層疊體的生產
將實例及比較例的樹脂組成物浸漬至利用乙烯基矽烷進行表面處理的玻璃纖維(厚度為15微米，旭化成(Asahi Kasei)，1017，L-玻璃)中，且接著在130℃至160℃的溫度下乾燥了約3至10分鐘，以製備厚度為30微米的預浸材。
隨後，對所述兩個預浸材進行了層疊，且接著在兩側上按壓銅箔(厚度為12微米，由三井製造)以製備覆銅層疊板(copper-clad laminated plate)。
(2)樹脂流動度(Resin Flow)
在預浸材狀態下，使用蓋壓機(cover press)根據IPC-TM-650 2.3.17試驗方法手冊對樹脂流動度(%)進行了量測及評價。(基於在170℃下乾燥3分鐘)
(3)耐熱性(焊料浮動)
根據IPC-TM-650 2.4.13試驗方法手冊，藉由在288℃下使層疊板在焊料上浮動來評價耐熱性，以量測絕緣層與銅箔之間以及絕緣層與金屬芯或絕緣層之間發生分離現象的時間點。
(4)相對介電係數及介質損耗正切的量測
使用被移除銅箔的層壓板、利用相對介電係數量測裝置(射頻阻抗(RF Impedence)，安捷倫(Agilent))以1吉赫(GHz)的頻率對相對介電係數及介電損耗正切進行了量測。
(5)熱膨脹係數(CTE)
使用被移除銅箔的層疊板量測了熱膨脹係數。具體而言，根據IPC-TM-650.2.4.24試驗方法手冊，藉由熱機械分析儀(thermomechanical analyzer，TMA)Q400(熱分析(thermal analysis，TA)儀器)對熱膨脹係數(ppm/℃)進行量測及評價。
Figure 108142093-A0305-02-0021-3
根據表2，證實了由於實例1至4一起應用無機填料與 有機-無機複合填料，因此實例1至4作為絕緣材料的可靠性優異(由於實例1至4的優異耐熱性及低熱膨脹係數)，且表現出低介電係數。
另一方面，證實了單獨使用30phr含量的無機顆粒的比較例1相較於含有相同量的無機顆粒的實例1及2而言具有較高的介電損耗及較高的熱膨脹係數，且使用75phr含量的無機顆粒的比較例2相較於包含相同量的無機顆粒的實例3及4而言具有較高的介電係數。此外，證實了僅應用有機-無機複合填料的比較例3及4相較於實例而言具有較低的耐熱性及較高的熱膨脹係數。

Claims (11)

  1. 一種樹脂組成物，包含：黏結劑樹脂及填料，所述填料包括有機-無機複合填料及無機填料，其中所述有機-無機複合填料是其中形成有覆蓋層的有機填料，所述覆蓋層包括利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的無機顆粒，以100重量份的所述黏結劑樹脂計，所述有機-無機複合填料的含量為20至90重量份，其中在所述有機-無機複合填料中，以100重量份的所述有機填料計，所述利用含有含雙鍵官能基的矽烷偶合劑進行表面處理的無機顆粒的含量為0.001至10重量份。
  2. 如請求項1所述的樹脂組成物，其中所述黏結劑樹脂包括選自由以下組成的群組的一或多者：聚伸苯基醚樹脂、氰酸酯樹脂、雙馬來醯亞胺樹脂、丁二烯樹脂、苯氧基樹脂、聚醯胺醯亞胺樹脂、聚醚醯亞胺樹脂、聚碸樹脂、聚醚碸樹脂、聚碳酸酯樹脂及聚醚醚酮樹脂。
  3. 如請求項1所述的樹脂組成物，其中所述有機填料是含有氟元素的氟系有機填料。
  4. 如請求項1所述的樹脂組成物，其中所述無機填料利用含有含雙鍵官能基的矽烷偶合劑進行表面處理。
  5. 如請求項1或請求項4所述的樹脂組成物，其中 所述含雙鍵官能基是乙烯基或(甲基)丙烯酸酯基。
  6. 如請求項1所述的樹脂組成物，其中所述樹脂組成物更包含選自由以下組成的群組的一或多者：固化劑、阻燃劑、紫外線屏蔽劑、調平劑、增稠劑、顏料、分散劑及抗氧化劑。
  7. 一種預浸材，包括：纖維基板；以及如請求項1所述的樹脂組成物，浸漬至所述纖維基板中。
  8. 如請求項7所述的預浸材，其中所述纖維基板利用含有含雙鍵官能基的矽烷偶合劑進行表面處理。
  9. 一種層疊板，其中層疊有至少二層如請求項7所述的預浸材。
  10. 如請求項9所述的層疊板，其中所述層疊板在層疊有至少兩層所述預浸材的狀態下被加熱及按壓。
  11. 一種樹脂覆蓋式金屬箔，包括：金屬箔；以及樹脂層，位於所述金屬箔上，且如請求項1所述的樹脂組成物在所述樹脂層中固化。
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