TWI464749B - 傳導性組合物 - Google Patents

傳導性組合物 Download PDF

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Publication number
TWI464749B
TWI464749B TW099125523A TW99125523A TWI464749B TW I464749 B TWI464749 B TW I464749B TW 099125523 A TW099125523 A TW 099125523A TW 99125523 A TW99125523 A TW 99125523A TW I464749 B TWI464749 B TW I464749B
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Taiwan
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conductive composition
metal
sintering aid
type
silver
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TW099125523A
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TW201126541A (en
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Raymond L Dietz
Maciej Patelka
Akito Yoshii
Pawel Czubarow
Takashi Sakamoto
Yukinari Abe
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Diemat Inc
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Description

傳導性組合物
本發明大體上係關於導熱性組合物。
本申請案係基於2006年5月8日申請之臨時申請案60/799,068之申請案第11/801156號之部份延續。
本發明係關於特別適用於將高密度、微電路電子組件黏合於基板之熱增強黏著膏。
多年來，將高密度、微電路組件附著在基板上，諸如將矽晶粒附著在陶瓷板上已係電子工業之一重要態樣。通常，已知利用沉積於晶粒與基板間的晶粒附著膏。一般而言，晶粒附著膏包括填料、黏著劑與載體。填料係經選擇以賦予最終黏合層所需之傳導性、電阻性或介電性。黏著劑係經選擇以於晶粒與基板之間形成強黏合。載體將所有的組份保持在流體、均勻混合物中，其允許糊膏輕易施用於晶粒-基板界面。在熱處理總成後，其亦具有在晶粒與基板間遷移之適宜揮發性。在沉積糊膏及裝配晶粒與基板後，一般加熱該總成以熔化黏著劑並驅除載體。冷卻時，晶粒緊緊地附接於基板。
主動組件之功率密度持續上升，導致越來越需要較高導熱性之黏著劑來附接此等組件。先前此等需求已由先前技術(包括美國專利第6,111,005號與第6,140,402號)中所描述之技術滿足。此等專利描述一種包括利用懸浮於非溶劑中之粉末狀有機聚合物樹脂以及高度導熱性填料的技術。粉末狀樹脂之類型係視應用而變化。就大面積組件的附著而言，其中與基板之熱膨脹係數(CTE)不匹配亦較大，故併入低模量熱塑性聚合物以處理在黏著劑之黏合線處產生之剪切應力。就較小面積組件而言，其中與基板之膨脹不匹配較低，故於具有填料之黏著劑組合物中使用熱固性或熱塑性與熱固性聚合物粉末之組合。使用較高模量聚合物亦會增加導熱率。
美國專利第6,265,471號描述再更高的導熱率技術，其中使高度傳導性填料懸浮於溶於易揮發溶劑中的液態環氧樹脂中。此技術使導熱率增加至超越美國專利第6,111,005號與第6,140,402號中所述之先前技術。不幸的是，當固化或交聯時，熱固性液態樹脂系統之彈性模量係相對較高。因此，此技術之應用受限於小面積組件附著及/或CTE與組件緊密匹配之基板，通常為半導體晶粒。在以上所述技術中所述之先前技術清楚顯示黏著劑之模量與導熱性間的線性關係。美國專利第6,111,005號與第6,140,402號中所述之低模量黏著劑導熱性較低，而美國專利第6,265,471號中所述之較高模量黏著劑導熱性較高。隨著較高功能半導體裝置大小及功率的增加，黏著劑對高導熱性與低模量兩者的需求亦增加，需要此等黏著劑來吸收由晶粒與高膨脹、高導熱性基板間之熱膨脹不匹配所引起之黏合線剪切應力。在市場中之一廣泛應用係將大面積覆晶微處理器裝置附著於高膨脹、高導熱性散熱器。此應用需求高傳導性與低模量性質兩者。迄今為止，於此應用中使用美國專利第6,111,005、6,140,402及6,265,471號中所述之一系列黏著劑。然而，微處理器裝置之功率密度增大，且因此對具有再更好之熱性質以及低彈性模量的黏著劑的需求增加。
本發明提供夠強但仍足夠彈性以將大面積矽晶粒黏合於更易膨脹基板而不引起過多應力，且仍能提供較當前技術顯著更高之熱性質的晶粒附著膏。本發明亦提供一種用於附接較小組件之具有顯著增強熱性質的黏著劑，其中固化黏著劑之模量較高。本發明亦提供一種可藉由工業設備及製程在無重大修飾下施用並產生黏合線及藉此加工之黏著膏。本發明亦提供組件與基板間可通過工業黏附標準之充足黏附。此外，由於熱塑性樹脂可重覆地熔融及固化，故本發明之彼等實施例可再次加工且適用於多晶片模組技術。
具體言之，本發明提供基本上包括以下組份之黏著膏：(A)約2-20重量百分比之有機聚合物樹脂；(B)高達30重量百分比之易揮發液體；及(C)約5-98重量百分比之無機填料，其中該填料係以顆粒形式存在且至少約80%之填料顆粒之特徵為圓形邊緣且實質上無扁平表面。
附圖係用以進一步闡述根據本發明之各種實施例且用以解釋根據本發明之各種原理及優點，其中在所有個別視圖中，相同的參考數字指示相同或功能相近之元件且其與以下詳細說明一起併入及形成說明書之部份。
技術熟練者當瞭解圖中之元件係為簡明及清晰而闡述且並不一定係按比例繪製。例如，圖中一些元件之尺寸可相對其他元件放大，以助於改善理解本發明之實施例。
在此文件中，諸如第一及第二、頂部及底部及其類似者之關係術語可僅用以區分一實體或行為與另一實體或行為，而並不一定係要求或暗指此等實體或行為間之任何實際的此關係或次序。術語「包括」、「包含」或其任何其他變形係意欲涵蓋非排他性的包含，以致包括一列元素之製程、方法、物件或裝置不僅僅包括彼等元素，而且可包括此製程、方法、物件或裝置未清楚列出或固有之其他元素。經「包括一......」處理之元素並不排除在包括該元素的該製程、方法、物件或裝置中存在額外的相同元素。
美國專利第6,111,005與6,265,471號描述本發明之黏著膏之主要組份的詳細描述。關鍵差異係較佳在燒結助劑之存在下，以球形銀粉取代黏著劑組合物中之銀薄片。相較具有銀薄片之相同膏，球形粉末產生高度燒結、更密實的結構。此產生體電阻率之不預期的下降及導熱率之增加。此外，黏著力增加，其容許減少樹脂含量(較高的銀對樹脂比)，其進一步增加導熱率。
用於本發明之黏著膏的無機填料係以顆粒形式存在。至少約80%之填料顆粒(且較佳實質上所有的填料顆粒)之特徵為圓形邊緣，且實質上無扁平表面。大體上球形顆粒為尤佳。無機填料亦最好係實質上無表面活性劑。可用於本發明之填料顆粒之代表係可獲自Metalor Technologies USA(Attlebro,Mass.) K82P及P318-8之彼等。
無機填料較佳係與至少一種燒結助劑(亦即增強填料燒結之任何添加劑)組合使用。代表性的燒結助劑包括金屬樹脂酸鹽及銀氧化物。燒結助劑通常係以固化材料之約0.1至0.5重量百分比之濃度存在。
雖然未完全理解電及熱性質的預料外之增加，但咸信其係歸因於球形相較先前用於此類塑膠中之薄片幾何形狀之更佳的填充及點接觸。亦咸信重要的是不存在於薄片製造過程中所存在的會在薄片之表面上留下殘餘物的表面活性劑或潤滑劑。此有機層傾向於熱隔離一個薄片與另一薄片。
在先前所述之粉末樹脂技術中，當加熱該總成時，樹脂粉末熔化且與其他顆粒聚結並朝著黏合線界面遷移。此粉末熔化會在黏合線中留下空隙，下文稱為「黏合脫落」(BDO)。據認為此BDO空隙之分佈或孔隙度係黏合線之關鍵性質，並控制由經黏合之兩組件之膨脹不匹配所產生的剪切應力。此等孔之尺寸與數量係樹脂之量、聚合物粉末尺寸分佈的直接函數。在無孔的情況下，本發明提供自身彈性模量高之高度燒結銀填料。來自粉末狀樹脂熔化之孔的分佈會減小固化黏合線的彈性模量。樹脂離開產生孔。因此，最終孔隙度係粉末狀樹脂之起始體積之函數。
在封圍指定體積之所有表面中，球體具有最小表面積，且在具有指定表面積之所有密閉表面中，其封圍最大體積。因此，針對指定體積之填料，球體間之接觸數量將比薄片的數量少。由於主要的導熱路徑係通過填料之整體，故就最高熱流而言，每單位體積填料的顆粒接觸量應保持為最低。填料之填充密度係決定熱流之另一關鍵因素。此填充密度可藉由如以下實例所述之球體的粒度分佈而增強。
本發明黏著膏較佳進一步包括高達約3.0重量%之還原劑。可使用廣泛種類之還原劑，包括有機、無機、有機金屬或鹽化合物。可使用之還原劑的代表例為肼、苯肼、N,N-二乙基羥基胺、磷酸羥胺(HAP)、硫酸羥胺(HAS)、硫酸氫銨、磷酸氫銨(AUP)、磷酸二氫銨、硝酸銨及硫酸銨。
其他類球形亦可用於本發明中。在數學中，類球形係藉由使橢圓繞著其主軸之一旋轉而獲得之三維空間中的二次曲面。因此，球體係產生橢圓為圓的類球形之一特例。
為闡述本發明，將填料、樹脂及易揮發液體之組合結合於膏中。由其主要組份製備黏著劑及其之應用及使用方法充分利用技術中熟知之各種方法及設備。可在技術中已知之設備中混合主要組份用於製備膏。於以上引述及參考之先前技術中描述此方法之細節。
本發明之晶粒附著黏著劑一般係用於將微電路電子組件附著於基板。通常而言，此包括製備本發明之黏著膏；接著將該膏施用於基板之表面以形成黏合線，及將電子組件置於黏合線上，以使該膏係置於電子組件與基板之間；然後加熱該總成至足夠高溫度歷時足夠長時間，以使有機熱塑性樹脂軟化及變為流體，但不分解，且液體自膏中去揮發；然後冷卻經熱處理之總成至熱塑性聚合物變為固體以下之溫度，由此藉由無空隙黏合線將微電路電子組件黏合於基板。當使用熱固性樹脂作為部份或全部有機聚合物(而非作為顆粒)時，處理溫度應足夠高以使樹脂交聯。
為示範本發明，先將膏刮片塗布於玻璃面上，以及沉積於陶瓷基板上，隨後再將晶粒置於濕黏著劑上。所有固化係在最高200攝氏度下進行30分鐘。固化後，施加垂直於晶粒側面的力直至晶粒剪切離開基板。此力以psi記錄作為受測試特定組合物之黏著力值。量測載玻片上之黏著劑條的電阻並以微歐姆-cm記錄為體電阻率。由於熱傳送之機構係藉由電子進行，其係與導電相同之機構，故此電阻率值與導熱率有強烈關聯。由於電阻與導熱率之間的關係，故將進一步測試以電阻率值作為指標之該等組合物之導熱率。導熱率量測係藉由已知之雷射閃光方法進行。
如本文所用，表述「實質上由......組成」意指該組合物可包括除主要組份(稱為組份)以外之額外組份，其條件為額外組份不係以足以減損本發明之可操作性的量存在。
現藉由本發明之特定代表性實施例之實例闡述本發明，其中除非另有指明，否則所有的份、比例及百分比係以重量計。實例係僅為闡述性，且熟習此項技術者將明瞭本發明之修飾與對等物。
實例1-25及比較實例A-D
在下表1中的實例中，藉由以上所述之步驟製備膏，並闡述填料形態對電阻率的影響。
下表2中之實例闡述金屬樹脂酸鹽對黏著膏的電阻率及導熱率的影響。
下表3中之實例闡述填料載量對電阻率的影響。
下表4中之實例闡述粉末狀樹脂系統中之填料形態對電阻率及導熱率的影響。實例14表示本發明之最佳實施例。
下表5中之實例闡述環氧樹脂系統中之填料形態對電阻率及導熱率的影響。
下表6中之實例闡述另一環氧樹脂系統中之填料形態對電阻率及導熱率的影響。
如實例所述，在存在樹脂酸Ag鹽作為燒結助劑下，包括Ag之球形顆粒會得到顯著較低的電阻及較高導熱率，雖然其關係並非始終為線性。
下表8中之實例闡述在固化期間的壓力對界面熱阻的影響。
已發現加入較小百分比之具有顆粒直徑小於200奈米之極細(奈米級)銀顆粒以及燒結助劑會導致進一步增加的熱性能。圖1顯示已加入至根據本發明實施例的傳導性組合物的奈米級銀顆粒的SEM顯微圖。奈米級銀顆粒係球形。圖2顯示圖1中所示顆粒之粒度分佈。在此情況下，平均粒度係124奈米。或者，可使用奈米級Au、Cu、Sn、Pd或Pt替代奈米級銀。
燒結助劑適宜為金屬化合物，且可例如包括有機金屬、金屬-有機鹽、金屬硫醇及/或樹脂酸鹽。根據特定實施例，燒結助劑包括與例如由銀製造之傳導性填料顆粒相同之金屬。可用作燒結助劑的金屬硫醇之實例包括第三-十二烷基硫醇銀及二乙基二硫代胺基甲酸銀。可使用之其他有機金屬化合物之實例包括雙-(η1 -4-苯基-η2 -1-丁烯)銀(I)。可用作燒結助劑的金屬-有機鹽化合物之實例包括六氟戊二酮根環辛二烯銀(I)錯合物、新癸酸銀、2,4-五氟丙酸銀、2,4-戊二酮銀、甲苯磺酸銀。根據特定實施例，樹脂酸鹽係傳導性組合物之至少0.25重量%。根據特定實施例，具有直徑小於200奈米之傳導性(例如銀)顆粒係傳導性組合物之至少1重量%。
在特定實施例中，此等微細傳導性顆粒係與具有大於300奈米，且在一些情況下大於10微米之平均直徑的較大傳導性顆粒組合使用。當混合兩種類型具有兩種不同形態的較大顆粒時，獲得良好性能。已發現組合具有縱橫比小於1.3：1的顆粒形式稱為本文所界定之「球形」形態較大顆粒與具有約5之縱橫比但本文更寬廣界定為具有介於3：1與10：1間之縱橫比的顆粒的厚板形顆粒得到經改良之熱性質。圖3係顯示用於根據本發明實施例之傳導性組合物中的「球形」形態較大顆粒之SEM顯微圖，及圖4係已用於根據本發明實施例之傳導性組合物中的厚板形微米級顆粒之SEM。圖3所示之「球形」顆粒具有0.7-1.9 m2 /g之表面積，4.9-6.0克/cc之敲緊密度及1.7微米之平均粒度，粒度範圍為0.9至2.7微米。更通常而言，「球形」顆粒較佳具有大於0.5微米之粒度。圖4所示之厚板形顆粒具有0.05-0.15 m2 /g之表面積，5.5-7.1克/cc之敲緊密度及18微米之平均粒度，粒度範圍為8至36微米。更通常而言，在本發明之實施例中，可有利地使用具有大於10微米之平均粒度的厚板形顆粒。
較佳使用大約等量(以重量計)之圖3所示之「球形」形態顆粒及圖4所示之厚板形顆粒。通常「球形」對厚板形較大顆粒之重量比係介於40：60與60：40之間。
下表9提供顯示加入奈米銀與燒結助劑(例如樹脂酸鹽)兩者相比僅利用此等成份中之任一者的優點的資訊。表中之表值係以W/mK為單位之導熱率。如所示，加入5重量%之奈米銀及0.45重量%(基於未經固化組合物之總重量)之樹脂酸銀得到58 W/mK之導熱率，而加入5%之奈米銀但無樹脂酸銀得到僅為7 W/mK之導熱率及加入5%之樹脂酸銀但無奈米銀得到僅為19 W/mK之導熱率。用於此等測試中之樹脂酸銀係基於第三-十二烷基硫醇銀。表9係基於傳導性組合物，其除了表9所示之組份以外，亦包括圖3及圖4所示之「球形」與厚板形態較大銀粉末之50/50混合物、聚酯樹脂黏合劑及直鏈石蠟基之易揮發載劑。
圖5與圖6係表9中之四種傳導性組合物之SEM顯微圖。圖5、6中之顯微圖的佈局(以橫向定向之頁面)對應於表9中之表值佈局。圖5顯示放大2,000倍之傳導性組合物及圖6顯示放大50,000倍之傳導性組合物。在50,000倍下，明顯可見包括5%奈米銀及5%樹脂酸銀之組合物(示於右下方)，在很大程度上銀係包含於相連基質中。咸信銀之此更相連基質係獲得較高導熱率之原因。
如在以上所述之實施例之情況下，包括奈米級顆粒之傳導性組合物可進一步有利地包括諸如以上所述的樹脂黏合劑與易揮發液體。根據特定實施例，奈米級傳導性顆粒佔傳導性組合物之0.1%至10%，微米級傳導性顆粒佔至少75%，樹脂黏合劑佔2%至25%及易揮發載劑佔5%至15%。
加入金屬樹脂酸鹽(例如樹脂酸銀)而不加入奈米級銀得到導熱率之顯著增加，此對某些應用具可行性及競爭性。圖7係導熱率對樹脂酸鹽之百分比(相對於未經固化之傳導性組合物之重量)之圖。導熱率自0%樹脂酸鹽下之8 W/mK增加至0.9%樹脂酸鹽下之43 W/mK。此數據係基於除了樹脂酸鹽外，尚包括「球形」及厚板微銀粉末之50/50混合物、聚酯樹脂黏合劑、及具有約150克/莫耳易揮發載劑之分子量之直鏈石蠟的調配物。使用由BASF(East Newark,NJ)製造之硫醇銀樹脂酸鹽。
在本發明之典型實施例中，傳導性組合物之導熱率係與導電性相關。此歸因於導熱率很大程度因金屬填料內之電子遷移率而上升之事實。傳導性組合物之一些應用要求導熱性及一些應用要求導電性。一些應用可能要求兩者。其中導電性係主要需求的應用係利用傳導性組合物於形成面板上之導電性電路跡線。該等應用可使用在易揮發載體中包括奈米級銀及樹脂酸鹽的傳導性組合物配方。在特定實施例中，不需要其他之成份。此傳導性組合物可例如藉由篩網印刷施用於基板。組合物之燃燒溫度係相對低，此意指可使用包括具有較低耐熱性之基板之較寬廣範圍的基板。
在前述說明書中，已描述本發明之具體實施例。然而，熟悉技術人士瞭解可在不脫離如以下申請專利範圍中提出的本發明範圍下作出各種修飾及變化。因此，說明書與圖係應視為闡述性而非限制意義，且所有諸等修飾係意欲包含於本發明之範圍內。不應將益處、優點、問題解決方案及會導致任何益處、優點或解決方案出現或變得更加顯著的任何要素解釋為任何或全部申請專利範圍之關鍵、必需或必要特徵或要素。本發明僅係由隨附申請專利範圍，包括在此申請案之待審期間作出之任何修訂及如發出之彼等申請專利範圍的所有對等物所界定。
圖1係用於根據本發明之實施例的傳導性組合物中的奈米銀之顯微圖。
圖2係圖1所示之奈米銀的粒度分佈。
圖3係用於根據本發明之實施例的傳導性組合物中的厚板形微米尺寸銀顆粒的顯微圖。
圖4係用於根據本發明之實施例的傳導性組合物中的球形微米尺寸銀顆粒的顯微圖。
圖5係以2,000x放大率顯示四種不同傳導性組合物彼此相比的四張顯微圖之矩陣。
圖6係顯示如圖5所示之相同傳導性組合物但在50,000x放大率下之四張顯微圖之矩陣。
圖7係導熱率對樹脂酸鹽之百分比(相對於未經固化之傳導性組合物之重量)之圖。
(無元件符號說明)

Claims (28)

  1. 一種傳導性組合物，其包括：第一類型金屬顆粒；及金屬化合物燒結助劑，其中該金屬化合物燒結助劑包括金屬硫醇。
  2. 如請求項1之傳導性組合物，其中該第一類型金屬顆粒具有小於200奈米之平均直徑。
  3. 如請求項1之傳導性組合物，其中該第一類型金屬顆粒及該金屬化合物燒結助劑包括選自由Ag、Au、Cu、Sn、Pd及Pt組成之群的共同金屬。
  4. 如請求項1之傳導性組合物，其進一步包括樹脂黏合劑。
  5. 如請求項4之傳導性組合物，其進一步包括易揮發液體。
  6. 如請求項5之傳導性組合物，其中該第一類型金屬顆粒構成該傳導性組合物之0.1重量%至10重量%，該第二類型金屬顆粒構成該傳導性組合物之至少75重量%，該樹脂黏合劑構成2至25%及該易揮發液體佔5至15%。
  7. 如請求項5之傳導性組合物，其中該樹脂黏合劑係不溶於該易揮發液體中。
  8. 一種傳導性組合物，其包括：第一類型金屬顆粒；及金屬化合物燒結助劑，其中該燒結助劑包括樹脂酸鹽。
  9. 如請求項8之傳導性組合物，其中該樹脂酸鹽係以至少0.25%之量存在於該傳導性組合物中。
  10. 如請求項8或9之傳導性組合物，其中該第一類型金屬顆粒具有小於200奈米之平均直徑。
  11. 如請求項8或9之傳導性組合物，其中該第一類型金屬顆粒及該金屬化合物燒結助劑包括選自由Ag、Au、Cu、Sn、Pd及Pt組成之群的共同金屬。
  12. 一種傳導性組合物，其包括：第一類型金屬顆粒；金屬化合物燒結助劑；及具有大於0.5微米之平均直徑的第二類型金屬顆粒，其中該第一類型金屬顆粒具有小於200奈米之平均直徑，且該第二類型金屬顆粒具有介於3：1與10：1間之縱橫比。
  13. 如請求項12之傳導性組合物，其進一步包括具有至少0.5微米之平均直徑及具有小於1.3：1之縱橫比的第三類型金屬顆粒。
  14. 如請求項12或13之傳導性組合物，其中該第一類型金屬顆粒及該金屬化合物燒結助劑包括選自由Ag、Au、Cu、Sn、Pd及Pt組成之群的共同金屬。
  15. 如請求項12或13之傳導性組合物，其中該第一類型金屬顆粒包括銀且該金屬化合物燒結助劑包括銀。
  16. 如請求項12或13之傳導性組合物，其中該金屬化合物燒結助劑包括有機金屬化合物。
  17. 如請求項12或13之傳導性組合物，其中該金屬化合物燒結助劑包括金屬有機化合物。
  18. 如請求項12或13之傳導性組合物，其中該金屬化合物燒結助劑包括金屬有機鹽化合物。
  19. 如請求項12或13之傳導性組合物，其中該金屬化合物燒結助劑包括金屬硫醇。
  20. 如請求項12或13之傳導性組合物，其中該金屬化合物燒結助劑包括選自由六氟戊二酮根環辛二烯銀(I)錯合物、新癸酸銀、2,4-五氟丙酸銀、2,4-戊二酮銀及甲苯磺酸銀組成之群的化合物。
  21. 如請求項12或13之傳導性組合物，其中該金屬化合物燒結助劑包括雙-(η1 -4-苯基-η2 -1-丁烯)銀(I)。
  22. 如請求項12或13之傳導性組合物，其中該金屬化合物燒結助劑包括選自由第三-十二烷基硫醇銀及二乙基二硫代胺基甲酸銀組成之群的化合物。
  23. 如請求項12或13之傳導性組合物，其中該燒結助劑包括樹脂酸鹽。
  24. 如請求項23之傳導性組合物，其中該樹脂酸鹽係以至少0.25%之量存在於該傳導性組合物中。
  25. 如請求項12或13之傳導性組合物，其中該第一類型金屬顆粒構成該傳導性組合物之至少1重量%。
  26. 如請求項25之傳導性組合物，其中該金屬化合物燒結助劑構成該傳導性組合物之至少0.25重量%。
  27. 如請求項12或13之傳導性組合物，其中該第二類型金屬 顆粒具有大於10微米之平均直徑。
  28. 如請求項12或13之傳導性組合物，其中該第二類型金屬顆粒包括銀。
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