TWI624202B - 用於金層黏著之含有助熔劑或還原劑的銀燒結組合物 - Google Patents

用於金層黏著之含有助熔劑或還原劑的銀燒結組合物 Download PDF

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TWI624202B
TWI624202B TW102125632A TW102125632A TWI624202B TW I624202 B TWI624202 B TW I624202B TW 102125632 A TW102125632 A TW 102125632A TW 102125632 A TW102125632 A TW 102125632A TW I624202 B TWI624202 B TW I624202B
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哈利 理查 庫達
茱麗葉 葛蕾絲 山雀斯
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漢高智慧財產控股公司
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Abstract

本發明係關於一種可燒結傳導組合物，其包含(i)微米或次微米級銀薄片或粉末及(ii)助熔劑或氧化溶劑或過氧化物。該組合物可用於在未施加壓力的情況下於

Description

用於金層黏著之含有助熔劑或還原劑的銀燒結組合物
包含黏著樹脂及導電填充劑之傳導黏著組合物係用於半導體封裝件及微電子裝置之製造及組裝中，以用於機械黏接積體電路裝置及其基板並於其間建立導電性及導熱性。最常用的導電填充劑係銀薄片。在該等傳導組合物中使用黏著樹脂之原因係銀薄片通常無法使半導體或微電子裝置充分黏著至其基板上。然而，該樹脂的存在會限制銀的高導熱性及導電性。
目前，僅包含銀而無樹脂的傳導組合物係藉由熱壓縮結合(或無壓力結合)黏著至銀或金基板。然而，常用於製造電子裝置的基板係銅引線框，且銀不容易與銅形成金屬間結合。雖然已使用焊料，但在高功率及高溫應用中，焊料在於高溫或接近其熔融溫度的溫度下循環時係無效。此外，焊料需要存在助熔劑，其在形成金屬間結合後留下助熔殘餘物，因此需要對基板進行清潔步驟。
具有一種可燒結及黏著至銅且可高強度地黏著至現可獲得的銀及金基板的不含黏著樹脂的銀組合物將係有利。
本發明係關於一種傳導組合物，其包含(i)微米或次微米級銀薄片及(ii)助熔劑或氧化溶劑或過氧化物且不含有機樹脂。該助熔劑、過氧化物或氧化溶劑將經選擇以在燒結溫度下充分揮發以使該組合物 於燒結後無殘餘物殘留。此組合物係於250℃或更低的溫度下燒結，且可在未施加壓力的情況下與銅基板形成金屬間結合。在另一實施例中，本發明係一種包含第一銀或金基板、燒結組合物及選自銅、銀或金的第二基板的組合件，其中該包含銀薄片及氧化溶劑或過氧化物或助熔劑的燒結組合物係佈置於該第一及第二基板之間。
微米或次微米級銀薄片係市售且具有用於防止凝聚的脂肪酸潤滑劑及/或界面活性劑塗層。銀薄片製造商常用的潤滑劑包括硬脂酸、異硬脂酸、月桂酸、癸酸、油酸、棕櫚酸或經胺(例如咪唑)中和的脂肪酸。該潤滑劑及/或界面活性劑的移除促進該傳導組合物中的銀薄片與選定金屬基板之間形成金屬間結合，且可藉由使用氧化溶劑或過氧化物來完成。
適宜氧化溶劑之實例係酮、酯、二醇醚及醇。此等係由於具有高溶解力及效果而用於移除銀顆粒及基板表面上的有機物。氧化溶劑包括乙酸2-(2-乙氧基乙氧基)乙酯、丙二醇單乙醚、乙酸丁基乙氧基乙酯、二乙二醇單丁醚乙酸酯、二乙二醇、二丙二醇、單丁醚乙酸酯及碳酸丙二酯。其他適宜溶劑包括環酮，例如環辛酮、環庚酮及環己酮。當存在該氧化溶劑時，其含量將係至多該總組合物之約15重量%(但非0%)。
適宜過氧化物之實例包括過氧2-乙基己酸第三丁酯、過氧新癸酸第三丁酯、過氧化二月桂醯基、過辛酸第三丁酯、過氧2-乙基己酸1,1,3,3-四甲基丁酯、過氧化二第三丁基、2,5-雙-(第三丁基過氧基)-2,5-二甲基己烷及過氧化二異丙苯、過氧化二第三戊基。當存在過氧化物時，其含量將係該總組合物之0至2.0重量%(較佳0.0至1.0重量 %)。
助熔劑及還原劑(下文稱為助熔劑)係用作自金屬薄片或基板之金屬表面移除氧化物的化學清潔劑。助熔劑可於高溫下顯示極強還原性，由此防止金屬氧化物形成。助熔劑及還原劑可用於銀粉、銀薄片及塗覆銀之顆粒(例如塗覆銀之銅及塗覆銀之玻璃)上。適宜助熔劑之實例包括2,2,6,6-四甲基-哌啶氧、4,4’-二硫二丁酸、琥珀酸、8-羥基喹啉、次氮基三甲基膦酸、三乙醇胺、戊二酸、蘋果酸、酒石酸、乙醯丙酮、甘油、二硫蘇糖醇、1,2,3-三羥基苯。當存在助熔劑時，其含量將係該總組合物之0.0至10.0重量%(較佳0.5至5.0重量%)。
包含銀薄片及上述氧化溶劑、過氧化物或助熔劑中之一者的傳導組合物係於室溫下製得，沈積於基板上，與第二基板接觸，且隨後加熱至銀的燒結溫度以使該兩個基板黏著在一起。
當此等組合物用於半導體製造時，其等在未使用任何有機樹脂的情況下於燒結後具有充分黏著性以使塗覆金屬之晶粒黏著至塗覆金屬之基板。特定言之，該等組合物可用於使塗覆銀或金之半導體晶粒黏著至銅引線框。在一些實施例中，本發明組合物將於小於250℃的溫度下燒結。在其他實施例中，本發明組合物將於小於200℃的溫度下燒結。無需壓力即可引起燒結。在燒結溫度下，該等銀薄片上的潤滑劑及/或界面活性劑及該組合物中使用的溶劑、過氧化物或助熔劑係經燒除，僅留下燒結銀。
可設計各種燒結曲線時間表以適應從業者的需求。大尺寸晶粒可需要較低溫度及較長時間之燒結曲線，以使溶劑移除更緩慢，由此確保無空隙接合線。文中已提供典型燒結曲線，然而應瞭解預期其他類似燒結曲線將同樣有效。燒結曲線之實例包括：(i)自室溫歷時30分鐘斜升至220℃，接著維持於220℃下60分鐘；(ii)自室溫歷時15分鐘斜升至110℃，接著維持於110℃下60分鐘，接著維持於240℃下60分 鐘；(iii)自室溫歷時30分鐘斜升至250℃，接著維持於250℃下60分鐘；(iv)就較高燒結溫度而言，歷時60分鐘斜升至300℃，接著維持於300℃下2小時。無需壓力即可以此等燒結曲線完成本發明組合物之燒結。
在另一實施例中，本發明係一種包含第一銀或金基板、燒結組合物及選自銅、銀或金的第二基板之組合件，其中該包含銀薄片及氧化溶劑或過氧化物或助熔劑之燒結組合物係佈置於該第一及第二基板之間。
發現本發明銀黏著劑可用於需要高功率密度的電子工業用組合封裝件(例如彼等用於半導體、汽車、高電壓及太陽能電池應用中者)中。
實例
實例1.
在此實例中，製備以下樣品並進行測試方案。使用具有助熔劑之組合物及不含助熔劑之對照組合物製備樣品。將該等組合物於小型雙離心混合器(Speedmixer®)中以1000rpm混合60秒且隨後以1500rpm混合30秒。使所有樣品接受自周圍溫度歷時30分鐘斜升至250℃並於250℃下維持60分鐘之燒結。不使用壓力。
使用具有可達到350℃之加熱器安裝板且實現至少50kg力的Dage 4000系列晶粒剪切測試儀測量晶粒剪切。將該等組合物塗佈至3X3mm2塗覆銀之晶粒上並使其接觸半導體工業中常用的裸露銅引線框、塗覆銀之銅引線框及塗覆金之銅引線框。根據上述燒結曲線使該等樣品燒結。晶粒剪切目標值係大於或等於1.0Kg/mm2。
使用Agilent 34401A數位萬用錶或QuadTech 1689 RLC Digibridge測量體積電阻率。測試載體係載玻片，其上塗佈有根據上述燒結曲線燒結的50微米X 0.25mm X 25.4mm銀黏著劑。就有效性及可重複性 而言，測試至少3個樣品多次，且匯總結果並取平均值。
使用Holometrix Micro Flash雷射熱性質儀測量導熱性。該等測試樣品係根據上述燒結曲線燒結之0.5mm X 12.5mm的獨立銀黏著劑圓盤。就有效性及重複性而言，測量至少兩個樣品多次並匯總結果及取平均值。
使用具有錐板CP51的Brookfield DV-III於25.0℃下進行黏度測量。以1.92sec-1及19.2sec-1之剪切速率測量黏度。
藉由TA儀器Q20於自25℃以10℃/min斜升至350℃下測量DSC。
本發明樣品及對照樣品之組成(以重量份(pbw)計)及性能測試結果係描述於下表中：
該等結果顯示具有含助熔劑、氧化溶劑及過氧化物的組合物之所有引線框均具有較高晶粒剪切強度。
實例2.
在此實例中，該等銀燒結組合物不含助熔劑且其中一者不含過氧化物。兩種樣品均包含氧化溶劑。該TNA晶粒係鈦-鎳-塗覆銀之矽晶粒。Ag-LF係銀引線框。Cu-LF係銅引線框及PPF-LF係鎳-鈀-金閃蒸(金表面)引線框。RT係室溫。如實例1中所述般進行性能測試。數據顯示基本上由銀薄片及氧化溶劑組成之組合物將燒結並提供足以用於商業應用之晶粒剪切強度。
實例3.
在此實例中，如下表中所示來製備調配物：一種調配物包含過氧化物及氧化溶劑；一種僅包含氧化溶劑；且一種僅包含助熔劑。除 該表中所示者以外，如實例1中所述般進行性能測試，且其顯示基本上由銀薄片及助熔劑(或銀薄片及氧化溶劑)組成之調配物將燒結並提供足以用於商業應用之晶粒剪切強度。
數據顯示不存在過氧化物對具有助熔劑之燒結調配物之性能無顯著影響。
實例4.
在此實例中，如下表中所示來製備調配物：一種調配物包含氧化溶劑；一種調配物僅包含過氧化物；且一種調配物僅包含助熔劑。除該表中所示者以外，如實例1中所述般進行性能測試，且其顯示基本上由銀薄片及助熔劑(或銀薄片及氧化溶劑)組成之調配物將燒結並提供用於商業應用之充分熱及電性能及一些晶粒剪切強度條件。

Claims (6)

  1. 一種傳導黏著組合物，其係由下列所組成：(i)微米或次微米級銀薄片，其包含脂肪酸潤滑劑及/或界面活性劑塗層；(ii)助熔劑，其係選自由以下組成之群：2,2,6,6-四甲基-哌啶氧、4,4’-二硫二丁酸、琥珀酸、8-羥基喹啉、次氮基三甲基膦酸、三乙醇胺、戊二酸、蘋果酸、酒石酸、乙醯丙酮、二硫蘇糖醇及1,2,3-三羥基苯；(iii)過氧化物；及(iv)氧化溶劑，其係選自由以下組成之群：乙酸2-(2-乙氧基乙氧基)乙酯、丙二醇單乙醚、二乙二醇單丁醚乙酸酯、單丁醚乙酸酯及碳酸丙二酯。
  2. 如請求項1之傳導黏著組合物，其中該助熔劑係以佔該總組合物之0.1至10.0重量%的含量存在於該組合物中。
  3. 如請求項1之傳導黏著組合物，其中該氧化溶劑係以佔該總組合物之0.1至15.0重量%的含量存在。
  4. 如請求項1之傳導黏著組合物，其中過氧化物係存在且係選自由以下組成之群：過氧2-乙基己酸第三丁酯、過氧新癸酸第三丁酯、過氧化二月桂醯基、過辛酸第三丁酯、過氧2-乙基己酸1,1,3,3-四甲基丁酯、過氧化二第三丁基、2,5-雙-(第三丁基過氧基)-2,5-二甲基己烷及過氧化二異丙苯及過氧化二第三戊基。
  5. 如請求項4之傳導黏著組合物，其中該過氧化物係以佔該總組合物之高於0.0及至多1.0重量%的含量存在。
  6. 一種組合件，其包含第一銀基板、傳導黏著組合物及選自銅、銀或金的第二基板，其中該傳導黏著組合物係由下列所組成： (i)微米或次微米級銀薄片，其包含脂肪酸潤滑劑及/或界面活性劑塗層；(ii)助熔劑，其係選自由以下組成之群：2,2,6,6-四甲基-哌啶氧、4,4’-二硫二丁酸、琥珀酸、8-羥基喹啉、次氮基三甲基膦酸、三乙醇胺、戊二酸、蘋果酸、酒石酸、乙醯丙酮、二硫蘇糖醇及1,2,3-三羥基苯；(iii)過氧化物；及(iv)氧化溶劑，其係選自由以下組成之群：乙酸2-(2-乙氧基乙氧基)乙酯、丙二醇單乙醚、二乙二醇單丁醚乙酸酯、單丁醚乙酸酯及碳酸丙二酯；且該組合物係佈置於該第一及第二基板之間。
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