TWI651387B - 用於大型晶粒半導體封裝之導電黏晶薄膜及供其製備之組合物 - Google Patents

用於大型晶粒半導體封裝之導電黏晶薄膜及供其製備之組合物 Download PDF

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TWI651387B
TWI651387B TW103125744A TW103125744A TWI651387B TW I651387 B TWI651387 B TW I651387B TW 103125744 A TW103125744 A TW 103125744A TW 103125744 A TW103125744 A TW 103125744A TW I651387 B TWI651387 B TW I651387B
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group
composition
epoxy resin
maleimide
conductive
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TW103125744A
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TW201512367A (zh
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周溥剛
吉娜 洪
莎希 古普塔
安德魯 賴博
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漢高智慧財產控股公司
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    • H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L24/31—Structure, shape, material or disposition of the layer connectors after the connecting process
    • H01L24/32—Structure, shape, material or disposition of the layer connectors after the connecting process of an individual layer connector
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • C08L63/10—Epoxy resins modified by unsaturated compounds
    • C—CHEMISTRY; METALLURGY
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    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
    • C08G59/32—Epoxy compounds containing three or more epoxy groups
    • C08G59/34—Epoxy compounds containing three or more epoxy groups obtained by epoxidation of an unsaturated polymer
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    • C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
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Abstract

本文提供具有有利性質之導電黏晶薄膜，其用於各種應用中，例如，用於製備大型晶粒半導體封裝。本文亦提供可用於製備該等薄膜之調配物，以及製備該等調配物之方法。在本發明之其他態樣中，提供自本發明組合物製備之導電網狀物。在其他態樣中，本發明進一步係關於包含該等黏著至其適宜基板之導電黏晶薄膜之物件。

Description

用於大型晶粒半導體封裝之導電黏晶薄膜及供其製備之組合物
本發明係關於導電黏晶薄膜及可用於製備該等薄膜之調配物。在一個態樣中，本發明係關於製備該等調配物之方法。在另一態樣中，本發明係關於自本發明組合物製備之導電網狀物及製備該等導電網狀物之方法。在又一態樣中，本發明係關於包含黏著至適宜基板之本發明導電黏晶薄膜之物件，及製備該等物件之方法。
根據本發明，提供具有有利性質之導電黏晶薄膜，其用於大型晶粒半導體封裝中。本發明亦提供可用於製備該等薄膜之調配物，以及製備該等調配物之方法。
根據本發明之另一態樣，提供自本發明組合物製備之導電網狀物。在某些態樣中，本發明係關於包含該等黏著至其適宜基板之導電黏晶薄膜之物件。
根據本發明，提供包含以下之組合物：第一馬來醯亞胺、納特醯亞胺(nadimide)或衣康醯亞胺 (itaconimide)，其中該第一馬來醯亞胺、納特醯亞胺或衣康醯亞胺具有芳香族主鏈，且該第一馬來醯亞胺、納特醯亞胺或衣康醯亞胺之主鏈上醯亞胺部分之取代程度為該主鏈之每重複單元之至少0.5個醯亞胺部分，第二馬來醯亞胺、納特醯亞胺或衣康醯亞胺，其中該第二馬來醯亞胺、納特醯亞胺或衣康醯亞胺具有撓性脂肪族或脂肪族/芳香族主鏈，其中該第二馬來醯亞胺、納特醯亞胺或衣康醯亞胺之主鏈包括直鏈或具支鏈烴基區段，其中每一烴基區段具有至少20個碳，第一環氧樹脂，其中該第一環氧樹脂係橡膠或彈性體改質的，第二環氧樹脂，其中該第二環氧樹脂具有撓性脂肪族或脂肪族/芳香族主鏈，其中該第二環氧樹脂之主鏈包括直鏈或具支鏈烴基區段，其中每一烴基區段具有至少20個碳，導電填料，固化劑；及因此視情況非反應性有機稀釋劑；其中：當在260℃下藉由動力機械分析(DMA)測試時，該組合物在固化時具有小於約1GPa之模數。
在某些實施例中，第一馬來醯亞胺、納特醯亞胺或衣康醯亞胺之主鏈上醯亞胺部分之取代程度為該主鏈之每重複單元至少0.8個醯亞胺部分；在某些實施例中，第一馬來醯亞胺、納特醯亞胺或衣康醯亞胺之主鏈上之取代程度為該主鏈之每重複單元至少1個醯亞胺部分。
在某些實施例中，用於實踐本發明所涵蓋之第一馬來醯亞胺、納特醯亞胺或衣康醯亞胺分別具有以下結構：
其中：m為1至15，p為0至15，每一R2獨立地選自氫或低碳數烷基，且J係單價或多價基團，其係選自：-具有約6個至最多約300個範圍內之碳原子之芳香族烴基或經取代之芳香族烴基物質，其中芳香族烴基物質係選自芳基、烷基芳基、芳基烷基、芳基烯基、烯基芳基、芳基炔基或炔基芳基；-具有約6個至最多約300個範圍內之碳原子之芳香族伸烴基或經取代之芳香族伸烴基物質，其中芳香族伸烴基物質係選自伸芳基、烷基伸芳基、芳基伸烷基、芳基伸烯基、烯基伸芳基、芳基伸炔基或炔基伸芳基，-具有約6個至最多約300個範圍內之碳原子之雜環或經取代之雜環物質，-聚矽氧烷，或-聚矽氧烷-聚胺基甲酸酯嵌段共聚物，以及上述物質中之一或多者與選自以下之連接體之組合：共價鍵、-O-、-S-、-NR-、-NR-C(O)-、-NR-C(O)-O-、-NR-C(O)-NR-、-S-C(O)-、-S-C(O)-O-、-S-C(O)-NR-、-O-S(O)2-、-O-S(O)2-O-、-O-S(O)2-NR-、-O-S(O)-、-O-S(O)-O-、-O-S(O)-NR-、-O-NR-C(O)-、-O-NR-C(O)-O-、-O-NR-C(O)-NR-、-NR-O-C(O)-、-NR-O-C(O)-O-、-NR-O-C(O)-NR-、-O-NR-C(S)-、-O-NR-C(S)-O-、-O-NR-C(S)-NR-、-NR-O-C(S)- 、-NR-O-C(S)-O-、-NR-O-C(S)-NR-、-O-C(S)-、-O-C(S)-O-、-O-C(S)-NR-、-NR-C(S)-、-NR-C(S)-O-、-NR-C(S)-NR-、-S-S(O)2-、-S-S(O)2-O-、-S-S(O)2-NR-、-NR-O-S(O)-、-NR-O-S(O)-O-、-NR-O-S(O)-NR-、-NR-O-S(O)2-、-NR-O-S(O)2-O-、-NR-O-S(O)2-NR-、-O-NR-S(O)-、-O-NR-S(O)-O-、-O-NR-S(O)-NR-、-O-NR-S(O)2-O-、-O-NR-S(O)2-NR-、-O-NR-S(O)2-、-O-P(O)R2-、-S-P(O)R2-或-NR-P(O)R2-；其中每一R獨立地為氫、烷基或經取代之烷基。
在本發明之一些實施例中，上述馬來醯亞胺、納特醯亞胺或衣康醯亞胺之J為雜環、氧基雜環、硫基雜環、胺基雜環、羧基雜環、氧基芳基、硫基芳基、胺基芳基、羧基芳基、雜芳基、氧基雜芳基、硫基雜芳基、胺基雜芳基、羧基雜芳基、氧基烷基芳基、硫基烷基芳基、胺基烷基芳基、羧基烷基芳基、氧基芳基烷基、硫基芳基烷基、胺基芳基烷基、羧基芳基烷基、氧基芳基烯基、硫基芳基烯基、胺基芳基烯基、羧基芳基烯基、氧基烯基芳基、硫基烯基芳基、胺基烯基芳基、羧基烯基芳基、氧基芳基炔基、硫基芳基炔基、胺基芳基炔基、羧基芳基炔基、氧基炔基芳基、硫基炔基芳基、胺基炔基芳基或羧基炔基芳基、氧基伸芳基、硫基伸芳基、胺基伸芳基、羧基伸芳基、氧基烷基伸芳基、硫基烷基伸芳基、胺基烷基伸芳基、羧基烷基伸芳基、氧基芳基伸烷基、硫基芳基伸烷基、胺基芳基伸烷基、羧基芳基伸烷基、氧基芳基伸烯基、硫基芳基伸烯基、胺基芳基伸烯基、羧基芳基伸烯基、氧基烯基伸芳基、硫基烯基伸芳基、胺基烯基伸芳基、羧基烯基伸芳基、氧基芳基伸炔基、硫基芳基伸炔基、胺基芳基伸炔基、羧基芳基伸炔基、氧基炔基伸芳基、硫基炔基伸芳基、胺基炔基伸芳基、羧基炔基伸芳基、伸雜芳基、氧基伸雜芳基、硫基伸雜芳基、胺基伸雜芳基、羧基伸雜芳基、含有雜原子之二價或多價環狀部分、含有氧基雜原子之二價或多價環狀部分、含有硫基雜原子之二 價或多價環狀部分、含有胺基雜原子之二價或多價環狀部分，或含有羧基雜原子之二價或多價環狀部分。
供本文使用所涵蓋之第一馬來醯亞胺、納特醯亞胺或衣康醯亞胺之實例包括：
在某些實施例中，供本文使用所涵蓋之第二馬來醯亞胺、納特 醯亞胺或衣康醯亞胺之主鏈含有直鏈或具支鏈烴基區段，其中每一烴基區段具有至少30個碳，藉此增強其撓性。
在某些實施例中，供本文使用所涵蓋之第二馬來醯亞胺、納特醯亞胺或衣康醯亞胺分別具有以下結構：
其中：m為1至15，p為0至15，每一R2獨立地選自氫或低碳數烷基，且J係單價或多價基團，其係選自：-具有約20個至最多約500個範圍內之碳原子之非芳香族烴基或經取代之非芳香族烴基物質，其中非芳香族烴基物質係選自烷基、烯基、炔基、環烷基或環烯基；-具有約20個至最多約500個範圍內之碳原子之非芳香族伸烴基或經取代之非芳香族伸烴基物質，其中非芳香族伸烴基物質係選自伸烷基、伸烯基、伸炔基、伸環烷基或伸環烯基，-具有約20個至最多約500個範圍內之碳原子之雜環或經取代之雜環物質，-聚矽氧烷，或-聚矽氧烷-聚胺基甲酸酯嵌段共聚物，以及上述物質中之一或多者與選自以下之連接體之組合：共價鍵、-O-、-S-、-NR-、-NR-C(O)-、-NR-C(O)-O-、-NR-C(O)-NR-、-S-C(O)-、-S-C(O)-O-、-S-C(O)-NR-、-O-S(O)2-、-O-S(O)2-O-、-O-S(O)2-NR- 、-O-S(O)-、-O-S(O)-O-、-O-S(O)-NR-、-O-NR-C(O)-、-O-NR-C(O)-O-、-O-NR-C(O)-NR-、-NR-O-C(O)-、-NR-O-C(O)-O-、-NR-O-C(O)-NR-、-O-NR-C(S)-、-O-NR-C(S)-O-、-O-NR-C(S)-NR-、-NR-O-C(S)-、-NR-O-C(S)-O-、-NR-O-C(S)-NR-、-O-C(S)-、-O-C(S)-O-、-O-C(S)-NR-、-NR-C(S)-、-NR-C(S)-O-、-NR-C(S)-NR-、-S-S(O)2-、-S-S(O)2-O-、-S-S(O)2-NR-、-NR-O-S(O)-、-NR-O-S(O)-O-、-NR-O-S(O)-NR-、-NR-O-S(O)2-、-NR-O-S(O)2-O-、-NR-O-S(O)2-NR-、-O-NR-S(O)-、-O-NR-S(O)-O-、-O-NR-S(O)-NR-、-O-NR-S(O)2-O-、-O-NR-S(O)2-NR-、-O-NR-S(O)2-、-O-P(O)R2-、-S-P(O)R2-或-NR-P(O)R2-；其中每一R獨立地為氫、烷基或經取代之烷基。
在某些實施例中，上述馬來醯亞胺、納特醯亞胺或衣康醯亞胺之J係氧基烷基、硫基烷基、胺基烷基、羧基烷基、氧基烯基、硫基烯基、胺基烯基、羧基烯基、氧基炔基、硫基炔基、胺基炔基、羧基炔基、氧基環烷基、硫基環烷基、胺基環烷基、羧基環烷基、氧基環烯基、硫基環烯基、胺基環烯基、羧基環烯基、雜環、氧基雜環、硫基雜環、胺基雜環、羧基雜環、氧基伸烷基、硫基伸烷基、胺基伸烷基、羧基伸烷基、氧基伸烯基、硫基伸烯基、胺基伸烯基、羧基伸烯基、氧基伸炔基、硫基伸炔基、胺基伸炔基、羧基伸炔基、氧基伸環烷基、硫基伸環烷基、胺基伸環烷基、羧基伸環烷基、氧基伸環烯基、硫基伸環烯基、胺基伸環烯基、羧基伸環烯基、含有雜原子之二價或多價環狀部分、含有氧基雜原子之二價或多價環狀部分、含有硫基雜原子之二價或多價環狀部分、含有胺基雜原子之二價或多價環狀部分，或含有羧基雜原子之二價或多價環狀部分。
供本文使用所涵蓋之第二馬來醯亞胺、納特醯亞胺、衣康醯亞胺之實例包括：
在某些實施例中，供本文使用所涵蓋之第一環氧樹脂係環氧化之羧基封端之丁二烯-丙烯腈(CTBN)寡聚物或聚合物。
在某些實施例中，環氧化之CTBN寡聚物或聚合物係具有以下結構之寡聚或聚合前體之含環氧基衍生物：HOOC[(Bu)x(ACN)y]mCOOH
其中：每一Bu係丁烯部分(例如，1,2-丁二烯基或1,4-丁二烯基)，每一ACN係丙烯腈部分，Bu單元及ACN單元可無規或以嵌段形式排列， x及y中之每一者大於0，前提係x+y之總和=1，x：y之比率在約10：1至1：10之範圍內，且m在約20至約100之範圍內。
如熟悉此項技術者可易於認識到，環氧化之CTBN寡聚物或聚合物可以各種方式製得，例如藉由CTBN之羧酸基團與環氧樹脂間之反應(經由鏈延伸反應)自(1)羧基封端之丁二烯/丙烯腈共聚物、(2)環氧樹脂及(3)雙酚A製得： 及諸如此類。
第一環氧樹脂(即，橡膠或彈性體改質的環氧樹脂)之實例包括自以下各項製得之環氧化之CTBN寡聚物或聚合物：(1)羧基封端之丁二烯/丙烯腈共聚物，(2)環氧樹脂及(3)如上所述之雙酚A；HyproTM環氧基官能丁二烯-丙烯腈聚合物(先前為Hycar® ETBN)，及諸如此類。
橡膠或彈性體改質的環氧樹脂包括以下各項之環氧化衍生物：(a)共軛二烯之均聚物或共聚物，其具有30,000至400,000或更高之重量平均分子量(Mw)，如美國專利第4,020,036號(該案之全部內容係以引用方式併入本文中)中所闡述，其中共軛二烯每分子含有4至11個碳原子(例如1,3-丁二烯、異戊二烯及諸如此類)；(b)表鹵代醇均聚物、兩種或更多種表鹵代醇單體之共聚物，或表鹵代醇單體與氧化物單體之共聚物，其數量平均分子量(Mn)自約800至約50,000變化，如美國專利第4,101,604號(該案之全部內容係以引用方式併入本文中)中所闡述；(c)烴聚合物，包括乙烯/丙烯共聚物及乙烯/丙烯與至少一種非 共軛二烯之共聚物(例如乙烯/丙烯/己二烯/降莰二烯)，如美國專利第4,161,471號中所闡述；或(d)共軛二烯丁基彈性體，例如由85重量%至99.5重量%之C4-C5烯烴以及約0.5重量%至約15重量%之具有4至14個碳原子之共軛多烯烴組成之共聚物，異丁烯及異戊二烯之共聚物，其中組合在該共聚物中之大部分異戊二烯單元具有共軛二烯不飽和現象(例如參見，美國專利第4,160,759號；該案之全部內容係以引用方式併入本文中)。
在某些實施例中，第二環氧樹脂係環氧化聚丁二烯二縮水甘油醚寡聚物或聚合物。
在某些實施例中，供本文使用所涵蓋之環氧化聚丁二烯二縮水甘油醚寡聚物具有以下結構：
其中：R1及R2各自獨立地為H或低碳數烷基，R3為H、飽和或不飽和烴基或環氧基，每一寡聚物中存在至少1個上述含有環氧基之重複單元及至少一個上述烯屬重複單元，且當存在時，存在1至10個範圍內之每一重複單元，且n在2至150之範圍內。
在某些實施例中，用於實踐本發明所涵蓋之環氧化聚丁二烯二縮水甘油醚寡聚物或聚合物具有以下結構：
其中R係H、OH、低碳數烷基、環氧基、環氧乙烷取代之低碳數烷基、芳基、烷芳基及諸如此類。
供本文使用所涵蓋之第二環氧樹脂(即，具有撓性主鏈之環氧樹脂)之實例包括：
及諸如此類。
在一些實施例中，本發明調配物中可包括其他環氧樹脂材料。當包括在本發明調配物中時，涵蓋多種環氧基官能化樹脂以供本文使用，例如，基於雙酚A之環氧樹脂(例如，Epon Resin 834)、基於雙酚F之環氧樹脂(例如，RSL-1739)、基於苯酚-清漆型酚醛樹脂之多官能 環氧樹脂、二環戊二烯型環氧樹脂(例如，Epiclon HP-7200L)、萘型環氧樹脂及諸如此類，以及其任兩種或更多種之混合物。
供本文使用所涵蓋之例示性環氧基官能化樹脂包括環脂肪族醇之二環氧化合物、氫化雙酚A(作為Ep合金5000市售)、六氫鄰苯二甲酸酐之二官能環脂肪族縮水甘油酯(作為Ep合金5200市售)、Epiclon EXA-835LV、Epiclon HP-7200L及諸如此類，以及其任兩種或更多種之混合物。
適宜用作本發明調配物之可選其他組份之習用環氧樹脂材料之其他實例包括：
及諸如此類。
用於實踐本發明所涵蓋之導電填料包括銀、鎳、鈷、銅、金、鈀、鉑、碳黑、碳纖維、石墨、碳奈米管、鋁、銦錫氧化物、銀塗覆 之銅、銀塗覆之鋁、銀塗覆之石墨、鎳塗覆之石墨、鉍、錫、鉍-錫合金、金屬塗覆之玻璃球體、銀塗覆之纖維、銀塗覆之球體、銻摻雜之錫氧化物、碳奈米管、導電奈米填料、該等金屬之合金及諸如此類，以及其任兩種或更多種之混合物。
用於實踐本發明所涵蓋之固化劑包括脲、脂肪族及芳香族胺、聚醯胺、咪唑、二氰二胺、醯肼、脲-胺混合固化系統、自由基起始劑、有機鹼、過渡金屬觸媒、苯酚、酸酐、路易斯酸(Lewis acid)、路易斯鹼及諸如此類。例如參見，美國專利第5,397,618號，該案之全部內容係以引用方式併入本文中。
例示性自由基起始劑包括過氧酯、過氧碳酸酯、氫過氧化物、烷基過氧化物、芳基過氧化物、偶氮化合物及諸如此類。
非反應性稀釋劑在存在時包括芳香族烴(例如，苯、甲苯、二甲苯及諸如此類)、飽和烴(例如，己烷、環己烷、庚烷、十四烷)、氯化烴(例如，二氯甲烷、氯仿、四氯化碳、二氯乙烷、三氯乙烯及諸如此類)、醚(例如，乙醚、四氫呋喃、二噁烷、乙二醇醚、乙二醇之單烷基或二烷基醚及諸如此類)、酯(例如，乙酸乙酯、乙酸丁酯、甲氧基乙酸丙酯及諸如此類)；二元酯、α-帖品醇、β-帖品醇、煤油、鄰苯二甲酸二丁酯、丁基卡必醇、丁基卡必醇乙酸酯、卡必醇乙酸酯、乙基卡必醇乙酸酯、己二醇、高沸點醇及其酯、乙二醇醚、多元醇(例如，聚乙二醇、丙二醇、聚丙二醇及諸如此類)、酮(例如，丙酮、甲基乙基酮及諸如此類)、醯胺(例如，二甲基甲醯胺、二甲基乙醯胺及諸如此類)、雜芳香族化合物(例如，N-甲基吡咯啶酮及諸如此類)。
供本發明使用所涵蓋之非反應性稀釋劑之量可在很大範圍內變化，只要所採用之量足以溶解及/或分散本發明組合物之組份即可。當存在時，所用非反應性稀釋劑之量通常在組合物之約2重量%至最多約25重量%之範圍內。在某些實施例中，非反應性稀釋劑之量在總 組合物之約5重量%至最多20重量%之範圍內。在一些實施例中，非反應性稀釋劑之量在總組合物之約10重量%至最多約18重量%之範圍內。
如熟悉此項技術者易於認識到，在某些實施例中，本發明組合物中實質上不含稀釋劑。即使曾經存在稀釋劑，其通常係在完成對本發明組合物之操作(例如，藉由作為薄膜塗覆於適宜基板上)後去除。
在某些實施例中，本發明組合物進一步包含至多約4wt%丙烯酸系聚合物。用於實踐本發明所涵蓋之丙烯酸酯在業內眾所周知。例如參見美國專利第5,717,034號，該案之全部內容係以引用方式併入本文中。例示性丙烯酸系聚合物之分子量在約100,000至最多約1,000,000之範圍內且Tg在約-40℃至最高約20℃之範圍內。在某些實施例中，供本文可選使用所涵蓋之丙烯酸系聚合物之分子量在約200,000至最多約900,000之範圍內且Tg在約-40℃至最高約20℃之範圍內。
在某些實施例中，本發明組合物進一步包含至多約4wt%聚胺基甲酸酯、聚矽氧烷或諸如此類。
如本文所使用，「聚胺基甲酸酯」係指由有機單元結合有胺甲酸酯(亦稱為「胺基甲酸酯」)連接體之鏈構成之聚合物。聚胺基甲酸酯聚合物可藉由使異氰酸酯與多元醇反應形成。用於製備聚胺基甲酸酯之異氰酸酯及多元醇二者通常每分子含有平均兩個或更多個官能基。
如本文所使用，「聚矽氧烷」係指聚矽氧樹脂、寡聚物及聚合物、聚矽氧橋接之聚合物及具有化學式[R2SiO] n 之混合型無機-有機聚合物，其中R係有機基團，例如甲基、乙基、苯基或諸如此類。該等材料由無機矽-氧主鏈(…-Si-O-Si-O-Si-O-…)以及附接至四配位矽原子之有機側基(R)組成。
在某些實施例中，本發明組合物視情況進一步包含一或多種流 動添加劑、黏著力促進劑、導電性添加劑、流變改質劑或諸如此類，以及其任兩種或更多種之混合物。
如本文所使用，「流動添加劑」係指矽聚合物、丙烯酸乙酯/丙烯酸2-乙基己基酯共聚物、酮肟磷酸酯之羥烷基銨鹽及諸如此類，以及其任兩種或更多種之組合。
本發明組合物之每一組份之量可在很大範圍內變化。例示性組合物包含：至少1wt%之該第一馬來醯亞胺、納特醯亞胺或衣康醯亞胺，至少1wt%之該第二馬來醯亞胺、納特醯亞胺或衣康醯亞胺，至少2wt%之該第一環氧樹脂(即，該橡膠或彈性體改質的環氧樹脂)，至少0.5wt%之該第二環氧樹脂(即，該環氧樹脂具有撓性脂肪族或脂肪族/芳香族主鏈)，至少70wt%之該導電填料，至少0.3wt%之該固化劑，視情況至多4wt%之丙烯酸系聚合物，及因此視情況至多25wt%之非反應性有機稀釋劑。
在一些實施例中，本發明組合物之每一組份之量在約以下之範圍內：1-6wt%之該第一馬來醯亞胺、納特醯亞胺或衣康醯亞胺，1-8wt%之該第二馬來醯亞胺、納特醯亞胺或衣康醯亞胺，2-15wt%之該第一環氧樹脂(即，該橡膠或彈性體改質的環氧樹脂)，0.5-8wt%之該第二環氧樹脂(即，該環氧樹脂具有撓性脂肪族或脂肪族/芳香族主鏈)，70-95wt%之該導電填料， 0.3-4wt%之該固化劑，視情況至多4wt%之丙烯酸系聚合物，及因此視情況至多25wt%之非反應性有機稀釋劑。
在一些實施例中，本發明組合物之每一組份之量在約以下之範圍內：2-4wt%之該第一馬來醯亞胺、納特醯亞胺或衣康醯亞胺，3-6wt%之該第二馬來醯亞胺、納特醯亞胺或衣康醯亞胺，6-12wt%之該第一環氧樹脂(即，該橡膠或彈性體改質的環氧樹脂)，1-5wt%之該第二環氧樹脂(即，該環氧樹脂具有撓性脂肪族或脂肪族/芳香族主鏈)，80-85wt%之該導電填料，0.5-3wt%之該固化劑，視情況至多4wt%之丙烯酸系聚合物，及因此視情況至多25wt%之非反應性有機稀釋劑。
本發明組合物提供多種有用性能性質。例如，當在適宜的10×10mm銅基板墊上以0.2mm之厚度施加本發明組合物並在200℃下固化60分鐘時，該組合物經歷小於58微米之翹曲。
在本發明之某些實施例中，提供製備本文所闡述組合物之方法。本發明方法包含使所涵蓋之組份組合經受高剪切力混合達足以獲得實質上均質摻合物之時間。
在本發明之某些實施例中，將如本文所闡述之組合物施加至適宜基板(例如，釋放襯墊)上，然後在升高之溫度下實施b分段以自該組合物去除實質上所有溶劑。
在本發明之某些實施例中，提供包含在去除實質上所有來自上述b分段組合物之溶劑/稀釋劑後獲得之反應產物之導電黏晶薄膜。
本文所涵蓋之例示性導電黏晶薄膜包括在將該組合物在約160-230℃範圍內之溫度下固化約30分鐘至2小時範圍內之時間時所產生之薄膜。在一些實施例中，導電黏晶薄膜包括在將本發明組合物在約175-200℃範圍內之溫度下固化約1小時時所產生者。
本發明導電黏晶薄膜在固化後在動態蒸氣吸附分析儀中暴露於85℃及85%相對濕度時通常吸收小於約1.2重量%之水分。在一些實施例中，本發明導電黏晶薄膜在固化後在動態蒸氣吸附分析儀中暴露於85℃及85%相對濕度時吸收小於約0.7重量%之水分。
本發明導電黏晶薄膜在固化後通常具有小於約40℃之Tg(如藉由熱機械分析(TMA)所測定)；在一些實施例中，如藉由TMA測得之Tg小於約20℃。熱機械分析(TMA)係用於研究當材料之性質隨溫度改變時之該等材料性質之技術。在本文實例1中參見其例示性方案。
另一選擇為，本發明導電黏晶薄膜在固化後通常具有小於約100℃之Tan δ Tg(如藉由動力機械分析(DMA)測得)；在一些實施例中，Tan δ Tg小於約80℃。動力機械分析係用於測定聚合物之黏彈性之技術。在本文實例1中參見其例示性方案。
本發明導電黏晶薄膜在固化後亦可參考其拉力模數來表徵；在一些實施例中，本發明薄膜之拉力模數(在260℃下)小於1GPa；在一些實施例中，拉力模數(在260℃下)小於500Mpa。
本發明導電黏晶薄膜在固化後亦可參考其熱晶粒剪切力來表徵；在一些實施例中，該固化薄膜在260℃下之熱晶粒剪切力為至少0.5kg/mm2；在一些實施例中，該薄膜之熱晶粒剪切力為至少0.8kg/mm2。
本發明導電黏晶薄膜在固化後亦可參考其在85℃及85%相對濕度下暴露約3天後在260℃下之熱濕晶粒剪切力來表徵；在一些實施例中，該薄膜在暴露於該等條件後之熱濕晶粒剪切力為至少0.5 kg/mm2；在一些實施例中，該薄膜在暴露於該等條件後之熱濕晶粒剪切力為至少0.65kg/mm2。
根據本發明之另一實施例，提供製備導電黏晶薄膜之方法，該方法包含在將上述組合物施加至適宜基板後去除實質上所有來自該上述組合物之溶劑/稀釋劑。
根據本發明之又一實施例，提供製備導電黏晶薄膜之方法，該方法包含在將上述組合物施加至適宜基板後在其可選b分段後固化該上述組合物。在一些實施例中，較佳者係在固化上述組合物前實施b分段。
供本文使用所涵蓋之適宜基板包括引線框架、經設計用於半導體封裝之層壓基板(例如，BT基板、FR4基板及諸如此類)、聚對苯二甲酸乙二酯、聚甲基丙烯酸甲酯、聚乙烯、聚丙烯、聚碳酸酯、環氧樹脂、聚醯亞胺、聚醯胺、聚酯、玻璃及諸如此類。
如本文所使用，「引線框架」包含由銅或銅合金組成之基底板及形成於基底板之上(或兩個)表面上之保護性塗層。保護性塗層由至少一種選自由金、金合金、銀、銀合金、鈀或鈀合金組成之群之金屬構成，且其具有約10-500埃(angstrom)之厚度。保護性塗層係藉由適宜方式(例如，藉由蒸氣沈積)而形成。可藉助蒸氣沈積或濕法電鍍在基底板之表面與保護性塗層之間形成中間的鎳或鎳合金塗層。中間塗層之適宜厚度在約50-20,000埃之範圍內。例如參見，美國專利第5,510,197號，該案之全部內容係以引用方式併入本文中。
根據本發明之又一實施例，提供包含黏著至適宜基板之如本文所闡述之導電黏晶薄膜之物件。
可在固化導電黏晶薄膜與基板之黏著力方面描述本發明物件；通常黏著力在260℃下為至少約0.5kg/mm2；在一些實施例中，黏著力在260℃下為至少約0.8kg/mm2。
亦可在固化導電黏晶薄膜之Tg方面描述本發明物件，且Tg(如藉由熱機械分析(TMA)測得)通常小於約40℃；在一些實施例中，Tg小於約20℃。
另一選擇為，可參考固化導電黏晶薄膜之Tan δ Tg描述本發明物件；通常，本發明物件之導電黏晶薄膜具有小於約100℃之Tan δ Tg(如藉由動力機械分析(DMA)測得)；在一些實施例中，Tg小於約80℃。
可參考該固化導電黏晶薄膜在260℃下之拉力模數進一步描述本發明物件；通常，拉力模數小於約1GPa；在一些實施例中，拉力模數小於約500MPa。
如熟悉此項技術者可易於認識到，本發明物件之尺寸可在廣泛範圍內變化。本發明調配物之具體優點係其適於製備大型晶粒。例示性物件通常具有至少6mm2之表面積，且其可為2.5×2.5mm，或3×3mm，或4×4mm，或5×5mm，或6×6mm，或7×7mm，或8×8mm，或9×9mm，或10×10mm或諸如此類。
根據本發明之又一實施例，提供製備導電網狀物之方法，該方法包含：以預定圖案將如本文所闡述之組合物施加至適宜基板，且此後固化該組合物。
根據本發明之再一實施例，提供如本文所闡述製備之導電網狀物。
藉由以下非限制性實例闡釋本發明之各個態樣。該等實例係出於闡釋性目的而非對本發明之任一實踐進行限制。應瞭解，可作出各種修改形式而不背離本發明之精神及範圍。熟悉此項技術者易於知曉如何合成或在商業上獲得本文所闡述之試劑及組份。
實例1
試樣製備
藉由合併表1中所述之組份如下製備比較調配物及本發明調配物。
漿液製備
如下將固體樹脂預溶解於適宜溶劑中。將所需量之有機組份稱重至容器中，手動混合約5分鐘，然後添加足夠溶劑以填充5-25%之容器。利用高速混合機使預混合繼續約5-10分鐘。然後，將所需量之填料添加至容器中，並使其內容物經受高速混合(約1000-3000rpm)達約一個小時。藉由使所得漿液經受減壓達約1-10分鐘而將其脫氣。
薄膜製備
藉由使用塗覆機器將漿液傾倒於清潔製備之表面上製備導電薄膜。隨後，在甑式烘箱中加熱漿液以產生穩定的塗層薄膜，該薄膜充分接合至基板(釋放襯墊)。然後，將覆蓋襯墊施加至薄膜上以保護其表面。在一些情形下，可在熱量及壓力下合意的層壓薄膜以促進實質上均勻薄膜塗層之形成。
使調配物A、B及C中之每一者經受多種分析。
TMA
例如，使約1-2mm厚之5×5mm試樣經受30-45分鐘之自室溫至200℃之斜坡升溫，在200℃下維持一個小時，然後在具有膨脹夾具之Perkin-Elmer儀器上利用20mN之外加力經受熱機械分析(TMA)。加熱/冷卻/保持參數概述於下文中：
1.以20℃/min自5℃加熱至200℃
2.以50℃/min自200℃冷卻至-85℃
3.在-85℃下保持5min
4.以10℃/min自-85℃加熱至250℃。
在第二加熱運行上實施數據收集；所收集數據用於測定玻璃過渡溫度(Tg)、熱膨脹係數1(CTE1)及熱膨脹係數2(CTE2)。
DMA
採用TA Instruments TA-Q800在TA-Q800上使用平邊拉力薄膜夾具對薄膜試樣實施拉力模數之DMA分析。試樣尺寸為約(24×8×0.2mm)。藉由使試樣經受30-45min之自室溫至200℃之斜坡固化該等試樣，然後在200℃下浸泡約1h。
以5.0℃/min之斜坡速率以-70℃開始至最高300℃實施DMA。對於應變幅度，頻率為10Hz且施加5微米。結果示於表2中。
表2中所述之結果表明，利用基於本發明調配物之測試薄膜獲得極佳性能性質(例如，低水分吸收，優良黏著力，低翹曲，低Tg，低模數)。
實例2
翹曲測試方法
使測試載具(QFN12×12 PPF引線框架，8mm×8mm×300μm厚的晶粒在9.9mm×9.9mm墊上)經受30min斜坡+於200℃下保持60min之固化，並量測所得翹曲。結果示於表3中。
表3中所述之結果表明，本發明調配物較缺乏一或多種供本文使用所涵蓋之組份之調配物遠遠更不易於翹曲。
實例3
MSL測試
根據JEDEC標準J-STD-20在以下條件下測定MSL(水分敏感度等級)：MSL1：85℃及85%相對濕度保持168小時；MSL2：85℃及60%相對濕度保持168小時；且MSL3：30℃及60%相對濕度保持192小時。
結果概述於下文中：
上述結果之綜述揭示，僅本發明調配物(例如，調配物C)能夠滿足MSL1標準所需之較嚴格條件。
實例4
熱循環測試
在室溫與200℃之間利用30分鐘斜坡升溫及於200℃下之60分鐘保持使其上具有8×8×0.3mm晶粒之12×12mm封裝經受板級溫度循環達2000個循環。結果概述於下文中。
上述結果之綜述揭示，本發明調配物(例如，調配物C)在經受多個溫度循環時表現得非常好，其較缺乏一或多種為本發明調配物所需之組份之比較調配物提供遠遠更好之黏著力。
除彼等在本文所顯示及所闡述者外，熟習此項技術者根據上述闡述應明瞭本發明之各種修改形式。該等修改形式亦意欲屬隨附申請專利範圍之範圍內。
本說明書中所提及之專利及公開案指示熟習本發明所屬領域技術者之熟習程度。該等專利及公開案係以引用方式併入本文中，其併入程度如同每一個別申請案或公開案明確地且個別地以引用方式併入本文中一般。
上述闡述闡釋本發明之具體實施例，而並非意欲在實踐本發明時進行限制。以下申請專利範圍(包括其所有等效形式)意欲界定本發明之範圍。

Claims (23)

  1. 一種組合物，其包含：第一馬來醯亞胺，其中該第一馬來醯亞胺具有芳香族主鏈，且該第一馬來醯亞胺之該主鏈上醯亞胺部分之取代程度為該主鏈之每重複單元至少0.5個醯亞胺部分，第二馬來醯亞胺，其中該第二馬來醯亞胺具有撓性脂肪族或脂肪族/芳香族主鏈，其中該第二馬來醯亞胺之該主鏈包括直鏈或具支鏈烴基區段，其中每一烴基區段具有至少20個碳，第一環氧樹脂，其中該第一環氧樹脂係橡膠或彈性體改質的，第二環氧樹脂，其中該第二環氧樹脂具有撓性脂肪族或脂肪族/芳香族主鏈，其中該第二環氧樹脂之該主鏈包括直鏈或具支鏈烴基區段，其中每一烴基區段具有至少20個碳，導電填料，固化劑；及因此視情況非反應性有機稀釋劑；其中：當在260℃下藉由動力機械分析(DMA)測試時，該組合物在固化時具有小於1GPa之模數。
  2. 如請求項1之組合物，其中該第一馬來醯亞胺之該主鏈上醯亞胺部分之該取代程度為該主鏈之每重複單元至少0.8個醯亞胺部分。
  3. 如請求項1之組合物，其中該第一馬來醯亞胺具有以下結構： 其中：m為1至15，每一R2獨立地選自氫或低碳數烷基，且J係單價或多價基團，其係選自：具有6個至300個範圍內之碳原子之芳香族烴基或經取代之芳香族烴基物質，其中該芳香族烴基物質係選自芳基、烷基芳基、芳基烷基、芳基烯基、烯基芳基、芳基炔基或炔基芳基；具有6個至300個範圍內之碳原子之芳香族伸烴基或經取代之芳香族伸烴基物質，其中該芳香族伸烴基物質係選自伸芳基、烷基伸芳基、芳基伸烷基、芳基伸烯基、烯基伸芳基、芳基伸炔基或炔基伸芳基，具有6個至300個範圍內之碳原子之雜環或經取代之雜環物質，聚矽氧烷，或聚矽氧烷-聚胺基甲酸酯嵌段共聚物，以及上述物質中之一或多者與選自以下之連接體之組合：共價鍵、-O-、-S-、-NR-、-NR-C(O)-、-NR-C(O)-O-、-NR-C(O)-NR-、-S-C(O)-、-S-C(O)-O-、-S-C(O)-NR-、-O-S(O)2-、-O-S(O)2-O-、-O-S(O)2-NR-、-O-S(O)-、-O-S(O)-O-、-O-S(O)-NR-、-O-NR-C(O)-、-O-NR-C(O)-O-、-O-NR-C(O)-NR-、-NR-O-C(O)-、-NR-O-C(O)-O-、-NR-O-C(O)-NR-、-O-NR-C(S)-、-O-NR-C(S)-O-、- O-NR-C(S)-NR-、-NR-O-C(S)-、-NR-O-C(S)-O-、-NR-O-C(S)-NR-、-O-C(S)-、-O-C(S)-O-、-O-C(S)-NR-、-NR-C(S)-、-NR-C(S)-O-、-NR-C(S)-NR-、-S-S(O)2-、-S-S(O)2-O-、-S-S(O)2-NR-、-NR-O-S(O)-、-NR-O-S(O)-O-、-NR-O-S(O)-NR-、-NR-O-S(O)2-、-NR-O-S(O)2-O-、-NR-O-S(O)2-NR-、-O-NR-S(O)-、-O-NR-S(O)-O-、-O-NR-S(O)-NR-、-O-NR-S(O)2-O-、-O-NR-S(O)2-NR-、-O-NR-S(O)2-、-O-P(O)R2-、-S-P(O)R2-或-NR-P(O)R2-；其中每一R獨立地為氫、烷基或經取代之烷基。
  4. 如請求項1之組合物，其中該第二馬來醯亞胺之該主鏈含有直鏈或具支鏈烴基區段，其中每一烴基區段具有至少30個碳，藉此增強其撓性。
  5. 如請求項1之組合物，其中該第一環氧樹脂係環氧化之羧基封端之丁二烯-丙烯腈(CTBN)寡聚物或聚合物。
  6. 如請求項5之組合物，其中該環氧化之CTBN寡聚物或聚合物係具有以下結構之寡聚或聚合前體之含有環氧基之衍生物：HOOC[(Bu)x(ACN)y]mCOOH其中：每一Bu係丁烯部分，每一ACN係丙烯腈部分，該等Bu單元及該等ACN單元可無規或以嵌段形式排列，x及y中之每一者大於0，前提係x+y之總和=1，x：y之比率在10：1至1：10之範圍內，且m在20至100之範圍內。
  7. 如請求項1之組合物，其中該第二環氧基係環氧化聚丁二烯二縮水甘油醚寡聚物。
  8. 如請求項7之組合物，其中該環氧化聚丁二烯二縮水甘油醚寡聚 物具有以下結構： 其中：R1及R2各自獨立地為H或低碳數烷基，R3為H、飽和或不飽和烴基或環氧基，每一寡聚物中存在至少1個上述含有環氧基之重複單元及至少一個上述烯屬重複單元，且當存在時，存在1至10個範圍內之每一重複單元，且n在2至150之範圍內。
  9. 如請求項7之組合物，其中該環氧化聚丁二烯二縮水甘油醚寡聚物具有以下結構： 其中R為H、OH、低碳數烷基、環氧基、環氧乙烷取代之低碳數烷基、芳基或烷芳基。
  10. 如請求項1之組合物，其進一步包含至多4wt%之選自丙烯酸系聚合物、聚胺基甲酸酯或聚矽氧烷之另一聚合部分。
  11. 如請求項10之組合物，其中該另一聚合部分係具有100,000至1,000,000範圍內之分子量及-40℃至最高20℃範圍內之Tg之丙烯酸系聚合物。
  12. 如請求項1之組合物，其中該組合物在以0.2mm之厚度施加於10×10mm銅基板墊上並在200℃下固化60分鐘時經歷小於58微米之翹曲。
  13. 如請求項1之組合物，其中該組合物在固化後在動態蒸氣吸附分析儀中暴露於85之相對濕度及85℃時之吸水率小於1wt%。
  14. 如請求項1之組合物，其中該組合物包含：1-6wt%之該第一馬來醯亞胺，1-8wt%之該第二馬來醯亞胺，2-15wt%之該第一環氧樹脂，0.5-8wt%之該第二環氧樹脂，70-95wt%之該導電填料，0.3-4wt%之該固化劑，視情況至多4wt%之選自丙烯酸系聚合物、聚胺基甲酸酯或聚矽氧烷之另一聚合部分，及因此視情況至多25wt%之非反應性有機稀釋劑。
  15. 一種製備如請求項1之組合物之方法，該方法包含使各組份之組合經受高剪切力混合達足以獲得實質上均質之摻合物之時間。
  16. 一種導電黏晶薄膜，其包含在自如請求項1之組合物去除實質上所有溶劑/稀釋劑後所獲得之反應產物。
  17. 如請求項16之導電黏晶薄膜，其中使該組合物在160℃至230℃範圍內之溫度下固化30分鐘至2小時範圍內之時間。
  18. 如請求項17之導電黏晶薄膜，其中該薄膜：在動態蒸氣吸附分析儀中暴露於85℃及85%相對濕度時吸收少於1.2重量%之水分；具有小於40℃之Tg(如藉由熱機械分析(TMA)測得)；具有小於100℃之Tan δ Tg(如藉由動力機械分析(DMA)測得)；具有在260℃下小於1GPa之拉力模數；具有在260℃下至少0.5kg/mm2之晶粒剪切力；及/或在85℃及85%相對濕度下暴露3天後具有在260℃下至少0.5kg/mm2之晶粒剪切力。
  19. 一種製備導電黏晶薄膜之方法，該方法包含在將如請求項1之組 合物施加至基板後對該組合物實施b分段。
  20. 如請求項19之方法，其中該基板係選自引線框架、經設計用於半導體封裝之層壓基板、聚對苯二甲酸乙二酯、聚甲基丙烯酸甲酯、聚乙烯、聚丙烯、聚碳酸酯、環氧樹脂、聚醯亞胺、聚醯胺、聚酯或玻璃。
  21. 一種物件，其包含黏著至其基板之如請求項16之導電黏晶薄膜。
  22. 如請求項21之物件，其進一步包含晶粒，其中該晶粒之尺寸為至少2.5×2.5mm。
  23. 一種製備導電網狀物之方法，該方法包含：以預定圖案將如請求項1之組合物施加至基板，視情況自該組合物去除溶劑/稀釋劑，及此後固化該組合物。
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