TW201731965A - 樹脂組成物、接合體及半導體裝置 - Google Patents

樹脂組成物、接合體及半導體裝置 Download PDF

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TW201731965A
TW201731965A TW105134080A TW105134080A TW201731965A TW 201731965 A TW201731965 A TW 201731965A TW 105134080 A TW105134080 A TW 105134080A TW 105134080 A TW105134080 A TW 105134080A TW 201731965 A TW201731965 A TW 201731965A
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Taiwan
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silver
resin
resin composition
ratio
young
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TW105134080A
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TWI701279B (zh
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赤池寛人
山和彦
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三菱綜合材料股份有限公司
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L24/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
    • H01L24/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • 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
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
    • C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
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Abstract

本發明之樹脂組成物為，具有黏合劑樹脂，與表面導入官能基之銀被覆粒子，又，前述銀被覆粒子之楊氏率(a)與硬化後的前述黏合劑樹脂之楊氏率(b)的比(a/b)為0.1~2.0，前述銀被覆粒子之楊氏率(a)為0.05~2.0GPa。

Description

樹脂組成物、接合體及半導體裝置
本發明係有關，例如絕緣電路基板等搭載半導體元件時可使用的樹脂組成物，及使用該樹脂組成物接合之接合體與半導體裝置。
本申請書係基於2015年10月29日於日本申請之特願2015-212947號、2016年7月29日於日本申請之特願2016-150723號主張優先權，且援用其內容。
LED及動力組件等之半導體裝置中，備有由導電材料所形成之電路層上接合半導體元件的結構。
為了控制風力發電、電動汽車、油電混合車等所使用之大電力控制用的動力半導體元件，會具有較大發熱量。因此有關搭載上述動力半導體元件的基板，目前為止係廣泛使用備有例如由AlN(氮化鋁)、Al2O3(氧化鋁)等所形成之陶瓷基板，與配置於該陶瓷基板一方表面上由具有優良導電性之金屬等所形成的電路層之動力組件用基板。
又，陶瓷基板另一表面形成金屬層之物也被提供作為動力組件用基板用。
此時將半導體元件安裝於電路層上時，例如係使用導電性接著劑等之樹脂組成物。樹脂組成物係藉由熱等而硬化，因此將樹脂組成物塗佈於欲接著部分後進行硬化，可接著構件等。該類樹脂組成物已知一般為，含有黏合劑樹脂與導電性粒子之樹脂組成物。
例如專利文獻1曾揭示，黏合劑樹脂係使用以環氧樹脂為主成分之樹脂，導電性粒子係使用銀粉的樹脂組成物。專利文獻1中，係藉由樹脂黏合劑另外添加環氧化丁二烯-苯乙烯共聚物，以緩和由樹脂組成物硬化所形成之接著層的應力。
又，例如專利文獻2曾揭示，黏合劑樹脂含有環氧化合物，導電性粒子係使用鎳粉或鍍銀粉的樹脂組成物。專利文獻2中，係藉由使用鈦或鋯之有機金屬錯合物作為黏合劑樹脂硬化用之觸媒，以抑制因熱循環而使導電性惡化。
先前技術文獻 專利文獻
[專利文獻1]特許第4872220號公報
[專利文獻2]特許第5651913號公報
但專利文獻1及專利文獻2所揭示之樹脂組成物中，由該樹脂組成物硬化所形成之接著層會因各材料之熱膨脹率差，而使熱應力局部性集中於接著層內部。因此會有因熱應力集中而導致接著層發生裂痕，而降低耐久性及信賴性之問題。
有鑑於上述事情，本發明之目的為，提供可形成緩和熱應力之局部性集中的接著層之樹脂組成物，及使用該樹脂組成物接合所得之接合體與半導體裝置。
為了解決前述課題，本發明一態樣之樹脂組成物為，特徵係具有黏合劑樹脂，與表面導入官能基之銀被覆粒子，又，前述銀被覆粒子之楊氏率(a)與硬化後的前述黏合劑樹脂之楊氏率(b)的比(a/b)為0.1~2.0，前述銀被覆粒子之楊氏率(a)為0.05~2.0GPa。
由此構成之樹脂組成物因前述銀被覆粒子之楊氏率(a)與硬化後的前述黏合劑樹脂之楊氏率(b)的比(a/b)為0.1~2.0，故黏合劑樹脂之楊氏率與銀被覆粒子之楊氏率之間不會產生較大差異，可抑制熱應力之局部性集中，而抑制接著層發生裂痕。
又，因前述銀被覆粒子之楊氏率(a)為0.05~2.0GPa，故確保接著層之剛性的同時，可抑制接著層硬化至必要以上之程度。
又，本發明一態樣之樹脂組成物較佳為，前述銀被覆粒子之楊氏率(a)與硬化後的前述黏合劑樹脂之楊氏率(b)的比(a/b)為0.4~2.0，前述銀被覆粒子之楊氏率(a)為0.2~2.0GPa。
此時因前述銀被覆粒子之楊氏率(a)與硬化後的前述黏合劑樹脂之楊氏率(b)的比(a/b)為0.4~2.0，故可進一步抑制熱應力之局部性集中，而確實抑制接著層發生裂痕。又，因前述銀被覆粒子之楊氏率(a)為0.05~2.0GPa，故可進一步確保接著層之剛性，同時確實抑制接著層硬化至必要以上之程度。
又，本發明一態樣之樹脂組成物中，前述官能基較佳為由環氧基、羧基、羰基、胺基、醯胺基、亞胺基、咪唑基及巰基所成群中所選出。
此時導入銀被覆粒子之表面的官能基為，可與黏合劑樹脂具有優良親和性，提高黏合劑樹脂與銀被覆粒子之密合性。
本發明一態樣之接合體為，特徵係接合第一構件與第二構件所得之接合體中，前述第一構件與前述第二構件之間介有前述樹脂組成物。
由此構成之接合體因第一構件與第二構件之間介有前述樹脂組成物，故既使該接合體負荷熱循環，也可抑制樹脂組成物發生裂痕，而使第一構件與第二構件具有優良接合信賴性。
本發明一態樣之半導體裝置為，特徵係備有 絕緣層一方表面上配置電路層之絕緣電路基板，與接合於前述電路層中前述絕緣層之相反側的表面上之半導體元件的半導體裝置中，前述電路層與前述半導體元件之間介有前述樹脂組成物。
由此構成之半導體裝置因電路層與半導體元件之間介有前述樹脂組成物，故既使該半導體裝置負荷熱循環，也可抑制樹脂組成物發生裂痕，而使電路層與半導體元件具有優良接合信賴性。
藉由本發明可提供，可形成緩和熱應力之局部性集中的接著層之樹脂組成物，及使用該樹脂組成物接合所得之接合體與半導體裝置。
1‧‧‧動力組件
3‧‧‧半導體元件
10‧‧‧動力組件用基板
12‧‧‧電路層
30‧‧‧導電接合層
圖1為使用本實施形態之樹脂組成物的動力組件(半導體裝置)之概略說明圖。
實施發明之形態
下面將詳細說明本發明一實施形態的樹脂組成物，及使用該樹脂組成物所得之半導體裝置(動力組件)。又，為了易明白以下說明用之圖面的特徵，方便上係擴大特徵部位表示，非限定於使各構成要素之尺寸比例 等與實際相同。
<樹脂組成物>
首先將說明本發明一實施形態之樹脂組成物的構成。本實施形態之樹脂組成物大致係由黏合劑樹脂與銀被覆粒子所構成。
本實施形態之樹脂組成物係藉由加熱而硬化形成接著層。於所欲接著之部分形成接著層後，接著第一構件與第二構件，可構成接合體。本實施形態之樹脂組成物可含有稀釋劑(溶劑)。含有稀釋劑之樹脂組成物可提升流動性，而易塗佈於第一構件或第二構件等之形成接著層用的部分。
黏合劑樹脂係藉由交聯或稀釋劑揮發而硬化以形成接著層。黏合劑樹脂可為藉由硬化而形成接著層之樹脂，無特別限定。具體之黏合劑樹脂如，環氧樹脂、苯酚樹脂、胺基甲酸酯樹脂、聚矽氧樹脂、丙烯酸樹脂、聚醯亞胺樹脂，及該等被改質所得之樹脂等。黏合劑樹脂可單獨使用上述樹脂，或二種以上併用。又，黏合劑樹脂可含有熱塑性樹脂。
<樹脂組成物中之黏合劑樹脂>
樹脂組成物所含有之作為黏合劑樹脂用的環氧樹脂如，雙酚型、聯苯型、聯苯混合型、萘型、甲酚酚醛清漆型、二環戊二烯型、三酚乙烷型、四酚乙烷型環氧樹脂。
上述環氧樹脂之硬化劑較佳為，一般所使用之咪唑類、三級胺類或含有氟化硼之路易斯酸，或其化合物、苯酚系硬化劑、酸酐系硬化劑、二氰二醯胺等之潛在性硬化劑。咪唑類如，2-甲基咪唑、2-乙基-4-甲基咪唑、2-苯基咪唑、2-苯基-4-甲基咪唑、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-苯基咪唑三聚異氰酸加成物等。三級胺類如，哌啶、苄基二胺、二乙基胺基丙基胺、異佛爾酮二胺、二胺基二苯基甲烷等。含有氟化硼之路易斯酸如，氟化硼單乙基胺等之氟化硼之胺錯合物。苯酚系硬化劑如，苯酚酚醛清漆樹脂、對二甲苯苯酚樹脂、二環戊二烯苯酚樹脂等。酸酐系硬化劑如，酞酸酐、四氫酞酸酐、六氫酞酸酐等。
又，環氧樹脂於必要時可添加硬化促進劑。硬化促進劑如，1-苄基-2-甲基咪唑等之咪唑類及其鹽類、1,8-二氮雜二環[5.4.0]十一-7-烯等之三級胺及其鹽類、三苯基膦等之有機膦化合物及其鹽類、辛酸鋅、辛酸錫、烷氧基鈦等之有機金屬鹽、鉑、鈀等之貴金屬類等。
樹脂組成物所含有之作為黏合劑樹脂用的苯酚樹脂可為熱硬化型中任何結構之物，但以甲醛/苯酚之莫耳比為1~2之範圍為佳。該熱硬化型苯酚樹脂之重量平均分子量較佳為300~5000，更佳為1000~4000。
樹脂組成物所含有之作為黏合劑樹脂用的胺基甲酸酯樹脂可使用一般作為接著用之物。具體如，聚醇系胺基甲酸酯樹脂、聚酯系胺基甲酸酯樹脂、聚己內醯胺 系胺基甲酸酯樹脂、聚醚系胺基甲酸酯樹脂、聚碳酸酯系胺基甲酸酯樹脂、胺基甲酸酯丙烯酸酯樹脂等，該等可單獨或組合使用。又，必要時可添加異氰酸酯、嵌段異氰酸酯等之硬化劑。
樹脂組成物所含有之作為黏合劑樹脂用的聚矽氧樹脂可為一般作為接著用之物，可使用附加型及縮合型中任何一種結構之物。
該聚矽氧樹脂具體如，各種有機聚矽氧烷、改質聚矽氧烷、彈性體改質聚矽氧烷、室溫硬化型聚矽氧烷橡膠等，該等可單獨或組合使用。
樹脂組成物所含有之作為黏合劑樹脂用的丙烯酸樹脂可使用一般所使用之熱硬化型、光聚合型、溶劑蒸發型之物。例如丙烯酸-mevamido樹脂、聚甲基丙烯酸甲酯樹脂、丙烯酸-苯乙烯共聚物、聚矽氧改質丙烯酸樹脂、環氧改質丙烯酸樹脂等，該等可單獨或組合使用。又，必要時可以異氰酸酯等之熱硬化劑、烷基苯酮系光聚合引發劑等作為硬化劑用。
樹脂組成物所含有之作為黏合劑樹脂用的聚醯亞胺樹脂可使用一般所使用之物。例如芳香族聚醯亞胺、脂環式聚醯亞胺、聚醯亞胺矽氧烷、環氧改質聚醯亞胺、感光性聚醯亞胺等，該等可單獨或組合使用。
上述環氧樹脂、苯酚樹脂、胺基甲酸酯樹脂、丙烯酸樹脂、聚矽氧樹脂或聚醯亞胺樹脂可抑制樹脂組成物因經時變化而使品質惡化，同時會因主鏈具有剛直 骨架而使硬化物具有優良耐熱性及耐濕性，因此可提升所形成之電極等的耐久性。樹脂組成物中黏合劑樹脂之比例換算為硬化物中之體積比例時，較佳為25~75體積%。黏合劑樹脂之比例未達下限值時，會使密合性不良而不宜。超過上限值時會降低導電性等而不宜。
<樹脂組成物中之稀釋劑>
稀釋劑如，乙二醇單乙基醚、乙二醇單丁基醚、丙二醇單甲基醚、丙二醇單乙基醚、丙二醇單-n-丁基醚、二乙二醇單乙基醚、二乙二醇單丁基醚、二丙二醇單甲基醚、二丙二醇單丁基醚、三丙二醇單甲基醚等之醚醇系溶劑及該等之乙酸酯系溶劑、乙二醇、丙二醇、萜品醇、石油溶劑、甲苯等之芳香族烴系溶劑、十二烷等之脂肪族烴系溶劑、二甲基甲醯胺、N-甲基-2-吡咯烷酮、二甲基亞碸、二丙酮醇、二甲基乙醯胺、γ-丁內酯、水、反應性稀釋劑等。
該等可依據與黏合劑樹脂之相溶性而選擇，聚矽氧樹脂特佳為石油溶劑及甲苯，聚醯亞胺樹脂特佳為N-甲基-2-吡咯烷酮，苯酚樹脂、胺基甲酸酯樹脂、環氧樹脂特佳為乙基卡必醇乙酸酯、丁基卡必醇乙酸酯、α-萜品醇。該等溶劑可單獨或複數種組合使用。
相對於黏合劑樹脂及其混合物，於不阻礙導電性、熱傳導性、密合性、形狀保持性之範圍內可混合添加物。添加物如，矽烷偶合劑、鈦偶合劑、銀奈米粒子、 增黏劑、分散劑、難燃劑、消泡劑及防氧化劑等。
硬化後之黏合劑樹脂的楊氏率較佳為0.1~5.0GPa，更佳為0.5~2.0GPa。藉由黏合劑樹脂之楊氏率為0.1GPa以上時，可抑制因外力施加於接合體所造成的接合體變形。又，藉由黏合劑樹脂之楊氏率為5.0GPa以下時，可緩和溫度變化時之熱應力。
又，硬化後之黏合劑樹脂的楊氏率例如可藉由下述方法測定。首先使用輥塗機或棒塗機等將含有黏合劑樹脂之溶劑塗佈於基板上後，加熱使黏合劑樹脂硬化，而於基板上使黏合劑樹脂被膜(接著層)成膜。其次相對於成膜後之被膜，使用微小壓入硬度試驗機(例如耶里歐公司製「ENT-1100」等)測定楊氏率。
銀被覆粒子為，將導電性及熱傳導性賦予樹脂組成物。銀被覆粒子係含有成為核之粒子(母粒子)，與設置於粒子表面之錫吸附層，與被覆於鍚吸附層表面之銀被覆層，與導入銀被覆層表面之官能基。
粒子之形狀可依據所希望之樹脂組成物的液流性而選擇，例如包含完整之球形粒子、橢圓般近似球形之粒子、表面有若干凹凸之粒子、扁平狀粒子、磷片狀粒子、棒狀粒子等。
粒子無特別限定，具體如丙烯酸樹脂粒子、苯乙烯樹脂粒子、苯酚樹脂粒子、聚矽氧樹脂粒子、聚矽氧橡膠粒子、聚醯亞胺樹脂粒子、氟橡膠粒子等。
樹脂粒子之平均粒徑較佳為0.5~40μm。樹脂 粒子之粒徑的粒度分布會依所希望之含有銀被覆粒子樹脂組成物的液流性而異，為了將觸變性賦予含有銀被覆粒子樹脂組成物較佳為，使粒度分布幅寬為一定範圍內。
藉由使樹脂粒子之平均粒徑為0.5μm以上，可縮小樹脂粒子之表面積。因此可減少為了得到作為導電性及熱傳導性填料用所必須之導電性及熱傳導性的銀含量。又，藉由使樹脂粒子之平均粒徑為40μm以下，易使含有銀被覆粒子樹脂組成物被應用於各種塗佈、印刷方法。
又，平均粒徑可藉由下述方法測定。首先使用掃描型電子顯微鏡(例如日立高科技公司製「SU-1500」等)，藉由程式(品名：PC SEM等)，以倍率：2000~5000倍測定300個樹脂粒子之直徑。其次由所得之測定值算出樹脂粒子之直徑的平均值，得平均粒徑。
於樹脂粒子之表面設置錫吸附層。錫吸附層為，含有錫之二價離子。藉由樹脂粒子之表面設置錫吸附層，可藉由無電解電鍍法以銀被覆錫吸附層之表面。
銀之被覆量(含量)可依據樹脂粒子之平均粒徑與所希望之導電性而決定。具體上銀之被覆量較佳如，相對於銀被覆粒子100質量份的銀含量為2~88質量份，更佳為2~80質量份。
藉由使相對於銀被覆粒子100質量份之銀含量為2質量份以上，於分散作為導電性填料用之銀被覆粒子時易取得銀相互間之接點，而賦予充分之導電性。又，藉由使銀含量為88質量份以下，可使比重較小且抑制成本增加。
銀被覆粒子之導電性較佳為，粉體體積電阻為1×10-2Ω‧cm以下，更佳為3×10-3Ω‧cm以下。
藉由使粉體體積電阻為1×10-2Ω‧cm以下，可降低電阻值而適用為導電性材料及熱傳導性材料。
又，粉體體積電阻為，將試料粉末(銀被覆粒子)放入壓力容器後，以9.8MPa進行壓縮，得壓粉體後藉由數據多重計器測定該壓粉體之電阻值所得之值。
此時以單方向將1個銀被覆粒子之粒徑壓縮20%後，壓縮方向之電阻值較佳為100Ω以下。又，以單方向將1個銀被覆粒子之粒徑壓縮50%後，壓縮方向之電阻值較佳為10Ω以下。
藉由使用表面處理劑(塗覆劑)等將官能基導入銀被覆層之表面。導入銀被覆層之表面的官能基較佳為，與黏合劑樹脂具有較高親和性之官能基。具體如，環氧基、羧基、羰基、胺基、醯胺基、亞胺基、咪唑基、巰基等。
藉由導入上述官能基，可提高黏合劑樹脂與銀被覆粒子之親和性，而提升黏合劑樹脂與銀被覆粒子之密合性，故可形成緩和熱應力之局部性集中的接著層。
銀被覆粒子之楊氏率較佳為0.05~2.0GPa，更佳為0.2~2.0GPa，特佳為0.5~1.5GPa。藉由使銀被覆粒子之楊氏率為0.05GPa以上，可抑制樹脂組成物混練時發生銀被覆粒子變形，而減少內部殘留應力，及抑制發生空隙或裂痕。又，藉由使銀被覆粒子之楊氏率為2.0 GPa以下，可將樹脂組成物塗膜之楊氏率保持於一定值以下，而減少溫度變化時之熱應力。
又，銀被覆粒子之楊氏率例如可使用微小壓縮試驗機(例如島津製作所製「MCT-2000」等)測定。
本實施形態之樹脂組成物較佳為，使銀被覆粒子之楊氏率(a)與硬化後的黏合劑樹脂之楊氏率(b)的比(a/b)為0.4~2.0，更佳為0.6~1.5。
使楊氏率之比(a/b)為0.4~2.0之範圍時，可形成緩和熱應力之局部性集中的接著層。因此藉由本實施形態之樹脂組成物所形成的接著層可具有優良之耐熱循環性。
其次將詳細說明上述樹脂組成物之製造方法。
首先為了調製銀被覆粒子，而將樹脂粒子加入錫化合物之水溶液中進行攪拌。其後濾取樹脂粒子進行水洗。藉此可於樹脂粒子表面設置錫吸附層。
此時錫化合物可使用氯化亞錫、氟化亞錫、溴化亞錫、碘化亞錫等。使用氯化亞錫時，錫化合物之水溶液中的氯化亞錫含量較佳為30~100g/dm3。氯化亞錫含量為30g/dm3以上時，易形成均勻之錫吸附層。又，氯化亞錫含量為100g/dm3以下時，易抑制氯化亞錫中之不可避不純物之量。又，錫化合物之水溶液可含有至飽和狀之氯化亞錫。
又，錫化合物之水溶液較佳為，相對於氯化亞錫1g而含有鹽酸0.5~2cm3。鹽酸含量為0.5cm3以上 時，可提升氯化亞錫之溶解性，且抑制錫被水解。鹽酸含量為2cm3以下時，不會過度降低錫化合物之水溶液的pH，可使樹脂粒子有效率吸附錫。
又，錫化合物之水溶液的溫度可為20~45℃，較佳為20~35℃，更佳為25~35℃，最佳為27~35℃。
藉由使錫化合物之水溶液的溫度為20℃以上，可抑制降低水溶液之活性，而使錫化合物充分附著於樹脂粒子上。又，藉由使錫化合物之水溶液的溫度為45℃以下，可抑制錫化合物氧化，而使水溶液安定，故可使錫化合物充分附著於樹脂粒子上。藉由20~45℃之水溶液使錫化合物附著於樹脂粒子時，既使相對於由密合性較差之丙烯酸系樹脂或苯乙烯系樹脂所形成之微粒子，也可析出具有適當結晶徑之銀結晶粒子。因此可形成具有優良密合性及細緻性之銀被覆層。又，因銀被覆層具有優良密合性及細緻性，故可減少粒徑被壓縮10%時之壓縮方向的電阻值。
又，攪拌時間可依據錫化合物之水溶液的溫度及錫化合物之含量而適當決定，但較佳為0.5~24小時。
其次藉由無電解電鍍法形成錫吸附層之表面被覆銀的銀被覆層。藉此可得銀被覆粒子。無電解電鍍法如，(1)將設有錫吸附層之樹脂粒子浸漬於含有錯合劑、還原劑等之水溶液後，滴入銀鹽水溶液的方法， (2)將設有錫吸附層之樹脂粒子浸漬於含有銀鹽、錯合劑之水溶液後，滴入還原劑水溶液的方法，(3)將設有錫吸附層之樹脂粒子浸漬於含有銀鹽、錯合劑、還原劑等之水溶液後，滴入苛性鹼水溶液之方法。
此時銀鹽可使用硝酸銀或銀溶解於硝酸所得之物等。錯合劑可使用氨、伸乙基二胺四乙酸、伸乙基二胺四乙酸四鈉、硝基三乙酸、三伸乙基四胺合物六乙酸、硫基硫酸鈉、琥珀酸鹽、琥珀酸亞胺酯、檸檬酸鹽或碘化物鹽等之鹽類。還原劑可使用甲醛水、葡萄糖、咪唑、羅謝爾鹽(酒石酸鈉鉀)、肼及其衍生物、氫醌、L-抗壞血酸或甲酸等。還原劑較佳為甲醛，更佳為至少含有甲醛之二種以上還原劑的混合物，最佳為含有甲醛與葡萄糖之還原劑的混合物。
其次以鹼洗淨液洗淨銀被覆粒子之表面再進行真空乾燥。其後相對於乾燥後之銀被覆粒子投入表面處理劑進行混練，而將官能基導入銀被覆粒子之表面。
又，表面處理劑為，例如將環氧基導入銀被覆粒子之表面時可使用含有環氧基之矽烷偶合劑、含有羧基之縮水甘油醚、含有胺基之縮水甘油醚等。又，例如導入羧基時可使用含有羧基之矽烷偶合劑、硬化蓖麻油等之脂肪類、丙酸、月桂酸、羥基月桂酸、肉豆蔻酸、羥基肉豆蔻酸、棕櫚酸、羥基棕櫚酸、硬脂酸、羥基硬脂酸、丙烯酸、油酸、亞油酸等之脂肪酸、羥基脂肪酸及該等之鹽類等，或含有該等之溶液。又，例如導入羰基時可使用前 述導入羧基用之表面處理劑、尿素、脂肪酸酯類、芳香族酯類、低分子量胺基甲酸酯等。又，例如導入胺基時可使用含有胺基之矽烷偶合劑、己基胺等之脂肪族胺、六伸甲基二胺等之二胺類，導入醯胺基時可使用含有醯胺基之矽烷偶合劑、丙烯醯胺、肽類、N,N-二甲基甲醯胺、乙醯胺等之脂肪族醯胺類。又，導入亞胺基時可使用含有亞胺基之矽烷偶合劑、脈、脒類、聚伸乙基亞胺等。導入咪唑基時可使用咪唑、甲基咪唑等之烷基咪唑、苯基咪唑、鹵化咪唑、咪唑羧酸、羥基甲基咪唑、咪唑鎓鹽、各種咪唑衍生物及該等之鹽。導入巰基時可使用含有巰基之矽烷偶合劑、十二烷硫醇等之鏈烷硫醇類、十八烷基二硫化物等之烷基二硫化合物、硫甘醇酸及其鹽類、硫乙酸及其鹽類等。
其次將黏合劑樹脂、熱硬化劑與硬化促進劑加入溶劑中，攪拌調製黏合劑混合液。又，黏合劑樹脂僅可使用於添加硬化劑及硬化促進劑後或溶劑乾燥時無需混合。此時溶劑可使用乙二醇單乙基醚、乙二醇單丁基醚、丙二醇單甲基醚、丙二醇單乙基醚、丙二醇單-n-丁基醚、二乙二醇單乙基醚、二乙二醇單丁基醚、二丙二醇單甲基醚、二丙二醇單丁基醚、三丙二醇單甲基醚等之醚醇系溶劑及該等之乙酸酯系溶劑、乙二醇、丙二醇、萜品醇、石油溶劑、芳香族烴系溶劑、脂肪族烴系溶劑等，溶劑之種類可因應與樹脂之相溶性而決定，可單獨或複數種組合使用。
其次使用行星攪拌機或三座輥混合機等混練藉由上述步驟調製所得之表面導入官能基之銀被覆粒子與黏合劑混合液，製造本實施形態之樹脂組成物。
<半導體裝置(動力組件)>
其次將以圖1說明使用本實施形態之樹脂組成物的半導體裝置一例之動力組件。
該動力組件1為，備有配置電路層12之動力組件用基板10，與電路層12之表面介有導電接合層30(接著層)接合的半導體元件3，與冷卻器40。
動力組件用基板10為，備用構成絕緣層之陶瓷基板11，與配置於該陶瓷基板11之一方表面(圖1之上面)上的電路層12，與配置於陶瓷基板11另一表面(圖1之下面)上的金屬層13。
陶瓷基板11為，防止電路層12與金屬層13之間的電接續之物，係由絕緣性較高之AlN(氮化鋁)構成。又，陶瓷基板11之厚度設定於0.2~1.5mm之範圍內，本實施形態係設定為0.635mm。
電路層12係藉由陶瓷基板11之一方表面上，接合具有導電性之金屬板所形成。本實施形態中，電路層12係藉由，由純度為99.99mass%以上之鋁(所得的4N鋁)的壓延板所形成之鋁板接合陶瓷基板11所形成。
金屬層13係藉由陶瓷基板11另一表面上，接合金屬板所形成。本實施形態中，金屬層13與電路層 12相同係藉由，由純度為99.99mass%以上之鋁(所謂的4N鋁)的壓延板所形成之鋁板接合陶瓷基板11所形成。
冷卻器40為，冷卻前述動力組件用基板10之物，其備有接合動力組件用基板10之天板部41，與由該天板部41往下垂設之散熱片42，與冷卻媒體(例如冷卻水)流通用之通路43。冷卻器40(天板部41)較佳為熱傳導性良好之材質構成，本實施形態係由A6063(鋁合金)構成。
又，本實施形態中冷卻器40之天板部41與金屬層13之間設有，由鋁或鋁合金或含有鋁之複合材(例如AlSiC等)所形成之緩衝層15。
又，圖1所示之動力組件1中，電路層12與半導體元件3之間，係藉由上述本實施形態之樹脂組成物形成導電接合層30(接著層)。
使用分配器或網版印刷浮標將厚10~100μm之本實施形態的樹脂組成物塗佈於電路層12之表面後，層合半導體元件3，再以溫度100~200℃、保持時間0.5~2.0小時之條件硬化形成導電接合層30，而接合電路層12與半導體元件3。
如以上之構成本實施形態的樹脂組成物，可使銀被覆粒子之楊氏率(a)與硬化後的黏合劑樹脂之楊氏率(b)的比(a/b)為0.1~2.0，銀被覆粒子之楊氏率(a)為0.05~2.0GPa，因此可形成緩和熱應力之局部性集中的導電接合層30(接著層)。
又，藉由本實施形態之樹脂組成物，可將環氧基、羧基、羰基、胺基、醯胺基、亞胺基、咪唑基、巰基導入銀被覆粒子之表面上，因此可提高黏合劑樹脂與銀被覆粒子之親和性。故可提高黏合劑樹脂與銀被覆粒子之密合性，而形成緩和熱應力之局部性集中的導電接合層30(接著層)。
本實施形態之動力組件1因係使用本實施形態之樹脂組成物形成導電接合層30，以接合電路層12與半導體元件3，故既使該動力組件1負荷熱循環時，也可抑制導電接合層30發生裂痕，得優良之半導體元件3與動力組件用基板10的接合信賴性。
以上係詳述本發明之實施形態，但具體結構非限定為該實施形態，也包括未脫離本發明要旨之範圍內的設計等。
例如接合對象物非限定於半導體元件，可使用上述樹脂組成物接合任意之第一構件與第二構件而構成接合體。
又，本實施形態中係以動力組件為例說明半導體裝置，但非限定於此，可為LED等之其他半導體裝置。
又，係以由鋁構成電路層之物進行說明，但非限定於此，可由銅等之其他導電材料所構成。
另外係以由AlN所形成之陶瓷基板為例說明絕緣層，但非限定於此，可由Al2O3、Si3N4、絕緣樹脂等其他絕緣體所構成。
實施例
下面將舉實施例及比較例詳細說明本發明之效果，但本發明非限定於下述實施例。
<調製樹脂組成物> [本發明例1]
首先為了調製銀被覆粒子，係使用容量1dm3之容量瓶以水將氯化亞錫15g、35%鹽酸15cm3稀釋為(定容)為1dm3後保溫為25℃。將平均粒徑10μm之丙烯酸樹脂粒子(母粒子)25g加入該水溶液後攪拌1小時。其後濾取樹脂粒子再水洗。藉此使樹脂粒子之表面設有錫吸附層。
其次將伸乙基二胺四乙酸四鈉(錯合劑)220.0g、氫氧化鈉50g、甲醛水(還原劑)100cm3溶解於水20dm3中，製作含有錯合劑及還原劑之水溶液。又，混合硝酸銀40g、25%氨水42cm3、水200cm3，製作含有硝酸銀之水溶液。
其次將設有錫吸附層之樹脂粒子浸漬於含有錯合劑及還原劑之水溶液中。
其後攪拌水溶液的同時滴入含有硝酸銀之水溶液，使所得銀被覆粒子中之銀的比例為50質量%般將銀被覆於設有錫吸附層之樹脂粒子上，製作銀被覆粒子。其後水洗銀被覆粒子再乾燥。測定乾燥後之銀被覆粒子的平均粒徑。結果如表1所示。又，銀被覆粒子之平均粒徑係藉由 與前述樹脂粒子之平均粒徑的測定方法相同之方法測定。
其次以鹼洗淨液對所得銀被覆粒子40g進行表面洗淨，再真空乾燥。其後將乾燥之銀被覆粒子投入乙醇1dm3中進行超音波分散後，再投入表1所示作為表面處理劑用之物10g中，攪拌下將表1所示之官能基導入銀被覆粒子的表面上。以乙醇洗淨該乙醇分散液中的銀被覆粒子後乾燥，得導入官能基之銀被覆粒子的乾燥粉。
此時係以下述方法測定銀被覆粒子之楊氏率。
使用微小壓縮試驗機(島津製作所製「MCT-2000」)以設定為，使最大荷重為粒子破壞強度之60%般的狀態進行負荷-除荷試驗，得荷重-位移曲線。使用 壓縮強度=2.8×荷重/(π×粒子直徑×粒子直徑)之式將該荷重-位移曲線中之荷重轉換為壓縮強度，又，以粒子直徑除以位移而轉換為偏差，得壓縮強度-位移曲線。以該壓縮強度-位移曲線中，除荷曲線之最大荷重值(破壞強度之60%)至破壞強度之55%的線形領域中傾斜度作為楊氏率之值。又，由20個粒子算出由此所得之楊氏率的平均值，作為銀被覆粒子之楊氏率。測定結果如表2所示。
其次以表1所示之溶劑稀釋表1所示之黏合劑樹脂與添加劑(硬化劑)，同時使用取泡練太郎(新吉公司)混合，得黏合劑混合液。
使用所得之黏合劑混合液，以下述方法測定 硬化後的黏合劑樹脂之楊氏率。
首先將黏合劑混合液塗佈於不銹鋼(SUS)基板上後，以溫度180℃下1小時之條件加熱所得的塗佈膜，使SUS基板上形成樹脂被膜。其次以下述方法測定所得樹脂被膜(硬化後之黏合劑樹脂)之楊氏率。
使用微小壓入硬度試驗機(耶里歐公司製「ENT-1100」)，於25℃之環境下以設定為最大荷重30mgf之狀態進行負荷-除荷試驗，得荷重-位移曲線。以最小二乘法近似除荷曲線中由除荷開始至15mgf之曲線的直線與荷重-位移曲線之橫軸的交點為h1[μm]，以最大位移[μm]-h1[μm]之值為h2[μm]，由下述式求取楊氏率。
楊氏率E[GPa]=0.0532/(h1×h2)
以樹脂被膜上20處由此測得之楊氏率的平均值作為黏合劑之楊氏率。測定結果如表2所示。
其次使硬化後的樹脂組成物中銀被覆粒子與黏合劑樹脂之體積比為1：1的比例計量上述步驟調製之銀被覆粒子與黏合劑混合液，使用取泡練太郎(新吉公司)混合。使用三座輥混合機混練所得混合物後加入表1所示之溶劑，將樹脂組成物之黏度調整為表2所示。黏度係採用，以電流計(日本TA計器公司DHR3)使用20mm平面板極測定之回轉速度1rpm時的黏度。
[本發明例2]
首先為了調製銀被覆粒子，使用容量1dm3之容量瓶 以水將氯化亞錫15g、35%鹽酸15cm3稀釋(定容)為1dm3後保溫於25℃。將平均粒徑35μm且粒徑之變動係數2.1%的丙烯酸樹脂粒子50g加入該水溶液後攪拌1小時。其後濾取樹脂粒子再水洗。藉此使樹脂粒子之表面設有錫吸附層。
其次將伸乙基二胺四乙酸四鈉(錯合劑)10.7g、氫氧化鈉2.5g及甲醛水(還原劑)5cm3溶解於水2dm3中，製作含有錯合劑及還原劑之水溶液。又，混合硝酸銀1.7g、25%氨水2cm3、水10cm3，製作含有硝酸銀之水溶液。
其次將設有錫吸附層之樹脂粒子浸漬於含有錯合劑及還原劑之水溶液中。
其後攪拌水溶液的同時滴入含有硝酸銀之水溶液，使粒子中銀之比例為2質量%般的銀被覆於設有錫吸附層之樹脂粒子上，製作銀被覆粒子。其後水洗銀被覆粒子再乾燥。
其次以鹼洗淨液洗淨銀被覆粒子50g之表面後進行真空乾燥。其後相對於乾燥後之銀被覆粒子投入表1所示之作為表面處理劑用之物10g，混練而將表1所示之官能基導入銀被覆粒子之表面上。
除了使用上述所製作之銀被覆粒子外，與本發明例1相同製作樹脂組成物。
[本發明例3~10及比較例1]
本發明例3~10及比較例1中係使用表1所示之銀被覆粒子的母粒子，製作銀被覆粒子中銀之比例為表1所示之量的銀被覆粒子。除了使用該製得之銀被覆粒子外，與本發明例1相同製作樹脂組成物。
<信賴性試驗>
相對於所製作之樹脂組成物進行信賴性試驗。具體為，首先將所製作之樹脂組成物塗佈於鋁基板2枚上，使其厚度為100μm後，以溫度150℃加熱1小時使樹脂組成物硬化而接合該組鋁基板，得試驗片。其次使用熱循環試驗機(ESPEC公司製「TSD-100」)，以-45℃~125℃之範圍相對於該試驗片實施循環1000次之熱循環試驗。循環試驗後相對於試驗片評估接合率。
又，接合率評估方法為，以超音波探傷像觀察熱循環試驗前後之試驗片接著界面，再藉由畫像解析測定接合面積及剝離面積，求取初期接合率(熱循環試驗前之接合率)與熱循環後接合率(熱循環試驗後之接合率)。又，係藉由下述式求取初期接合率及熱循環後接合率(單位：%)。
初期接合率=熱循環試驗前之接合面積/(熱循環試驗前之接合面積+熱循環試驗前之剝離面積)×100
熱循環後接合率=(熱循環試驗前之接合面積-熱循環試驗後之剝離面積)/熱循環試驗前之接合面積×100
銀被覆粒子之楊氏率(a)為本發明之範圍外的比較例1及3、銀被覆粒子之楊氏率(a)與硬化的黏合劑之楊氏率(b)的比(a/b)為本發明之範圍外的比較例2、4及銀被覆粒子之表面未導入官能基的比較例5，均會大幅降低熱循環後之接合率。
相對地銀被覆粒子之表面導入官能基，銀被覆粒子之楊氏率(a)及銀被覆粒子之楊氏率(a)與硬化的黏合劑之楊氏率(b)的比(a/b)為本發明之範圍內的本發明例1~10，確認熱循環後之接合率均比比較例高。
產業上利用可能性
本發明之樹脂組成物可形成緩和熱應力之局部性集中的接著層，例如可使用於半導體元件搭載於絕緣電路基板等場合。
1‧‧‧動力組件
3‧‧‧半導體元件
10‧‧‧動力組件用基板
11‧‧‧陶瓷基板
12‧‧‧電路層
13‧‧‧金屬層
15‧‧‧緩衝層
30‧‧‧導電接合層
40‧‧‧冷卻器
41‧‧‧天板部
42‧‧‧散熱片
43‧‧‧通路

Claims (5)

  1. 一種樹脂組成物，其特徵為，具有黏合劑樹脂，與表面導入官能基之銀被覆粒子，又，前述銀被覆粒子之楊氏率(a)與硬化後的前述黏合劑樹脂之楊氏率(b)的比(a/b)為0.1~2.0，前述銀被覆粒子之楊氏率(a)為0.05~2.0GPa。
  2. 如請求項1之樹脂組成物，其中前述銀被覆粒子之楊氏率(a)與硬化後的前述黏合劑樹脂之楊氏率(b)的比(a/b)為0.4~2.0，前述銀被覆粒子之楊氏率(a)為0.2~2.0GPa。
  3. 如請求項1或2之樹脂組成物，其中前述官能基係由環氧基、羧基、羰基、胺基、醯胺基、亞胺基、咪唑基及巰基所成群中所選出。
  4. 一種接合體，其特徵為，接合第一構件與第二構件所形成之接合體中，前述第一構件與前述第二構件之間介有如請求項1至3中任一項之樹脂組成物。
  5. 一種半導體裝置，其特徵為，備有絕緣層一方表面配置電路層之絕緣電路基板，與接合於前述電路層中前述絕緣層之相反側表面的半導體元件之半導體裝置中，前述電路層與前述半導體元件之間介有如請求項1至3中任一項之樹脂組成物。
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