TWI532818B - 連接材料與半導體裝置 - Google Patents
連接材料與半導體裝置 Download PDFInfo
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- TWI532818B TWI532818B TW098114221A TW98114221A TWI532818B TW I532818 B TWI532818 B TW I532818B TW 098114221 A TW098114221 A TW 098114221A TW 98114221 A TW98114221 A TW 98114221A TW I532818 B TWI532818 B TW I532818B
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- TW
- Taiwan
- Prior art keywords
- connecting material
- acrylate
- weight
- metal particles
- methacrylate
- Prior art date
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- 239000000463 material Substances 0.000 title claims description 120
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- 239000004332 silver Substances 0.000 claims description 16
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Classifications
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- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/30—Assembling printed circuits with electric components, e.g. with resistor
- H05K3/32—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits
- H05K3/321—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits by conductive adhesives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- C09J9/02—Electrically-conducting adhesives
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- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
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- H01L23/48—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor
- H01L23/488—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor consisting of soldered or bonded constructions
- H01L23/495—Lead-frames or other flat leads
- H01L23/49503—Lead-frames or other flat leads characterised by the die pad
- H01L23/49513—Lead-frames or other flat leads characterised by the die pad having bonding material between chip and die pad
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- H01L24/83—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a layer connector
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Description
本發明是有關於一種導熱性及黏著性優異的連接材料及使用此連接材料的半導體裝置。更詳細而言,本發明是有關於一種適用於將積體電路(Integrated Circuit,IC)、大規模積體電路(Lafge-Scale Integrated Circuit,LSI)、發光二極體(Light-Emitting Diode,LED)等的半導體元件黏著於導線架(lead frame)、陶瓷配線板、玻璃環氧配線板、聚醯亞胺配線板等的基板上的連接材料及使用此連接材料的半導體裝置。
於製造半導體裝置時,作為使半導體元件與導線架(支持構件)黏著的方法,有如下方法:於環氧系樹脂(epoxy resin)、聚醯亞胺系樹脂(polyimide resin)等的樹脂中分散銀粉等的填充劑並製成糊狀(例如銀糊),將此糊狀物質用作黏著劑。
根據此方法,使用點膠機(dispenser)或印刷機、打印機(Stamping Machine)等將糊狀黏著劑塗佈於導線架的晶片座(die pad)上之後,對半導體元件進行黏晶(die bonding),藉由加熱硬化而使此半導體元件黏著,製成半導體裝置。
對於此半導體裝置,進一步藉由密封材料將外部密封而製成半導體封裝之後,焊接安裝於配線基板上。由於最近的安裝要求高密度以及高效率,故焊接安裝的主流是將半導體裝置的導線架直接焊接於基板上的表面安裝法。
於此表面安裝時,使用藉由紅外線等對整個基板進行加熱的回流焊(reflow soldering),封裝被加熱到大於等於200℃的高溫。此時,若封裝的內部特別是黏著劑層中存在水分,則此水分會氣化而進入至晶片座與密封材料之間,導致封裝內產生裂痕(回焊裂痕(reflow crack))。
此回焊裂痕會使半導體裝置的可靠性明顯下降,故成為深刻的問題及技術課題,對於多被用於將半導體元件與半導體支持構件黏著的黏著劑而言,追求以高溫時的黏著強度為首的可靠性。
進而,近年來隨著半導體元件的高速化及高積體化的發展,除了先前以來一直需求的黏著強度等的可靠性以外,為了確保半導體裝置的動作穩定性而需求高散熱特性。即,為了解決上述技術課題,業者需求一種將散熱構件(導線架)與半導體元件接合的黏著劑所使用的兼具高黏著強度與高導熱性的連接材料。
又,作為相較於先前的利用金屬粒子彼此的接觸的導電性黏著劑而達成更高的散熱性的方法之一,提出有如下的導電性黏著劑:使用燒結性優異且平均粒徑為小於等於0.1 μm的金屬奈米粒子,或者在大於等於200℃的高溫下使金屬微粒子燒結。如上所述的先前技術例如記載於專利文獻1~專利文獻5中。
先前,作為確保黏著劑的高導熱性的方法,一直採用大量填充導熱率高的銀粒子的方法。又,亦有如下示例:使用低熔點金屬,藉由金屬鍵結來形成導熱通道及與被黏著體進行金屬化(metalize),藉此確保了高導熱化及室溫下的強度。進而,亦正在推進使用金屬奈米粒子的導電性黏著劑的研究。
專利文獻1:日本專利特開2006-073811號公報
專利文獻2:日本專利特開2006-302834號公報
專利文獻3:日本專利特開2005-093996號公報
專利文獻4:日本專利特開平11-066953號公報
專利文獻5:日本專利特開2006-083377號公報
然而,先前的大量填充導熱率高的銀粒子的方法中,為了確保近年來的功率IC、LED所需的大於等於20 W/m.K的導熱率,需要銀粒子填充量達到大於等於95重量份的量非常多的銀粒子。
當銀粒子填充量變多時,黏度上升,由此於點膠(dispense)時會產生拉絲等,而存在無法確保操作性的問題,當為了確保操作性而大量添加溶劑時,存在產生空隙或殘存溶劑導致黏著強度下降的問題。
又,於使用低熔點金屬並藉由金屬鍵結來形成導熱通道及與被黏著體進行金屬化的方法中,於將功率IC或LED等的封裝(package,PKG)安裝於基板上時,於回焊爐內暴露在260℃下,而存在由於此熱歷程而導致接合部再熔融、無法獲得連接可靠性的問題。
進而,於使用金屬奈米粒子的方法中,雖然可避免接合部再熔融的問題,但是如下情況等成問題:為了製作奈米尺寸的金屬粒子,要耗費大量成本;或者為了獲得金屬奈米粒子的分散穩定性,需要大量的表面保護材料;另外,為了將金屬奈米粒子燒結,必須施加大於等於200℃的高溫或者負荷。
因此,本發明之目的在於提供一種連接材料及使用此連接材料的半導體裝置,上述連接材料即便於未施加負荷且於小於等於200℃的硬化溫度下接合時亦具有高導熱率,且即便於260℃下加熱硬化體時亦具有充分的黏著強度。
鑒於上述情況,本發明提供一種連接材料,此連接材料含有藉由X射線光電子分光法(X-ray Photoelectron Spectroscopy)測定的氧的狀態比率小於15%的金屬粒子。根據此連接材料,即便於未施加負荷且在小於等於200℃的硬化溫度下接合時亦具有高導熱率,且即便於260℃下加熱硬化體時亦具有充分的黏著強度。
上述金屬粒子較好的是實施了將表面的氧化膜去除的處理及使用表面保護材料的表面處理的金屬粒子。
上述金屬粒子的平均粒徑較好的是大於等於0.1 μm、小於等於50 μm,又,較好的是在小於等於200℃下燒結的金屬粒子。
本發明的連接材料較好的是更含有揮發性成分或黏合成分而形成。
又,本發明提供一種連接材料,其含有黏合劑(A)、填料(B)及添加劑(C),並且將填料(B)與添加劑(C)以與連接材料中的重量比相同的重量比混合並進行加熱成型所得的成型體的導熱率達到大於等於40 W/mK。根據此連接材料,可具有操作性優異的黏度,且可維持黏著強度並提高導熱率。
再者,上述所謂「加熱成型」,是指成型為既定大小之後於180℃下加熱處理1小時,又,上述所謂「導熱率」,是指藉由實施例中記載的方法測定的導熱率。
上述添加劑(C)的含量較好的是相對於100重量份的黏合劑(A)為1重量份~100重量份。
進而,本發明提供一種半導體裝置,其具有經由上述本發明的連接材料而將半導體元件與半導體元件搭載用支持構件黏著的結構。
根據本發明,可提供一種連接材料及使用此連接材料的半導體裝置,上述連接材料即便於未施加負荷且在小於等於200℃的硬化溫度下接合時亦具有高導熱率,且即便於260℃下加熱硬化體時亦具有充分的黏著強度。上述連接材料適宜用作導電性連接材料、導電性黏著劑或黏晶材料。
為讓本發明之上述特徵和優點能更明顯易懂,下文特舉實施例,並配合所附圖式作詳細說明如下。
本發明的連接材料含有藉由X射線光電子分光法測定的氧的狀態比率小於15%的金屬粒子。
於上述金屬粒子中,氧的狀態比率較好的是小於10%,更好的是小於5%。
X射線光電子分光法的分析裝置例如可使用Surface Science Instrument公司的S-Probe ESCA Model 2803,照射X射線可使用AlKα線。所謂「狀態比率」,是指測定樣品中的特定元素的濃度,是以根據元素強度使用裝置配套的相對感度係數(relative sensitivity coefficient)計算出的值來表示。再者,藉由X射線光電子分光法測定的金屬粒子的氧的狀態比率成為金屬粒子表面上的氧化膜的量的指標。
作為上述金屬粒子,可使用各種公知的金屬粒子。例如可列舉:金、鉑、銀、銅、鎳、鈀、鐵、鋁等的導電性粉體等,又,該些金屬粒子可單獨使用,或者可將兩種或兩種以上組合使用。其中,特別是銀及銅在價格、導電性及導熱性等的方面而言較為理想。
上述金屬粒子的平均粒徑較理想的是大於等於0.1 μm小於等於50 μm。平均粒徑小於0.1 μm的粒子存在製造成本增大的傾向,平均粒徑超過50 μm的粒子存在粒子間的空隙大而導熱率下降的傾向。
上述金屬粒子較好的是實施了將表面的氧化膜去除的處理及使用表面保護材料的表面處理的金屬粒子。
藉由使用上述金屬粒子可獲得上述本發明的效果的原因雖然未必明瞭,但根據圖1~圖6的示意圖來說明本發明者等人的研究。
首先,於對表面氧化膜少的金屬粒子實施了使用表面保護材料的表面處理之情形時,被認為成為如圖1所示的狀態。即,被認為成為如下狀態:於塊狀金屬3上存在稍許殘留的氧化膜2,並且以避開氧化膜2的方式而由表面保護材料1覆蓋塊狀金屬3。
於此情形時,藉由在小於等於200℃下進行加熱,如圖2所示,由於表面保護材料1脫離、活性塊狀金屬3的表面露出,故此活性表面與其他金屬粒子的活性表面接觸,藉此促進燒結,而形成金屬粒子彼此的金屬鍵結(metallic bonding)的通道。被認為,含有此種金屬粒子的連接材料即便在小於等於200℃下進行加熱時亦具有高導熱率。
另一方面,於如圖3所示的氧化膜2多的金屬粒子之情形時,若在小於等於200℃下進行加熱,則如圖4所示,雖然表面保護材料1脫離,但因金屬粒子的表面廣泛地被氧化膜2所覆蓋,故被認為難以引起金屬粒子彼此的燒結。
相對於此,即便於使用氧化膜2多的金屬粒子之情形時,當實施了去除表面氧化膜2的處理及使用表面保護材料的表面處理時,如圖5所示,可獲得氧化膜2不存在而塊狀金屬3的整個表面被表面保護材料4所覆蓋的狀態的金屬粒子。
於此情形時,藉由與圖1所示的金屬粒子同樣地在小於等於200℃下進行加熱,表面保護材料4脫離,活性塊狀金屬3的表面露出,故此活性表面與其他金屬粒子的活性表面接觸,藉此促進燒結,而形成金屬粒子彼此的金屬鍵結的通道。此時,由於活性塊狀金屬3的表面的露出面積較圖1的金屬粒子更廣,因此被認為能進一步促進燒結,並被認為可獲得更高的導熱率。
進而,本發明者等人亦確立了如下的金屬粒子表面處理法:將金屬粒子的氧化膜的量減少或者完全去除,並防止金屬粒子的再氧化及凝聚。以下示出此方法。
首先,於溶解、分散有表面保護材料的酸性溶液中添加金屬粒子,一方面進行攪拌並且去除氧化膜,一方面進行表面保護。
接著,過濾溶液而取出金屬粒子,然後使用溶劑來清洗物理吸附於金屬粒子表面的表面保護材料或酸成分。其後,對金屬粒子進行減壓乾燥藉此去除多餘的溶劑,獲得乾燥狀態的經表面處理的金屬粒子。
再者,於去除氧化膜的製程中,於不含表面保護材料的酸性溶液中進行氧化膜處理之情形時,金屬粒子彼此凝聚,因而無法獲得具有與氧化膜處理前的粒子同等的平均粒徑的粉體狀金屬粒子。為了防止金屬粒子的凝聚,較好的是於酸性溶液中添加表面保護材料,來同時進行氧化膜去除與表面處理。
酸性溶液並無限制,酸可使用硫酸、硝酸、鹽酸、乙酸、磷酸等。酸的稀釋溶劑亦並無限制,較理想的是與酸的相容性良好且表面保護材料的溶解性及分散性優異的溶劑。
關於酸性溶液的酸的濃度,為了去除氧化膜,於將酸性溶液整體設為100重量份時,酸性溶液的酸的濃度較理想的是大於等於1重量份,於含有氧化膜較厚的金屬粒子之情形時,酸性溶液的酸的濃度更理想的是大於等於5重量份。
又,若酸的濃度過濃,則會導致金屬大量地溶解於溶液中,故酸的濃度較理想的是小於等於50重量份,為了防止粒子彼此凝聚,酸的濃度更理想的是小於等於40重量份。
表面保護材料較理想的是具有良好地吸附於金屬表面的末端官能基的化合物。例如可列舉具有羥基、羧基、胺基、硫醇基、雙硫基的化合物,較好的是具有硫醇基的化合物。藉由使用該些表面保護材料,可防止再氧化或粒子的凝聚。
又,為了進一步高度防止金屬粒子的再氧化或多餘的有機物的吸附汚染,較理想的是化合物的主骨架具有緊密地填充保護材料般的直鏈烷烴骨架。
烷烴骨架更理想的是碳數為大於等於4個,以藉由碳鏈之間的分子間力而緊密填充。
又,為了在小於等於200℃的低溫度下燒結金屬粒子,更理想的是表面保護材料自金屬表面脫離的溫度低於200℃的碳數為小於等於18個的烷烴骨架。
具有硫醇基且主骨架為直鏈烷烴骨架的化合物例如可列舉:具有1至18個碳原子的乙硫醇、正丙硫醇、異丙硫醇、正丁硫醇、異丁硫醇、第三丁硫醇、戊硫醇、己硫醇,十二硫醇、十八硫醇之類的硫醇或環烷硫醇,環烷硫醇可列舉:具有5至7個碳原子的環戊硫醇、環己硫醇或環庚硫醇之類的硫醇等。
關於酸性溶液中的表面保護材料的濃度,於將酸性溶液整體設為100重量份時,為了防止金屬粒子彼此的凝聚,酸性溶液中的表面保護材料的濃度較理想的是大於等於0.0001重量份,為了防止表面保護材料過剩地物理吸附於金屬粒子,酸性溶液中的表面保護材料的濃度較理想的是小於等於0.1重量份。
關於上述金屬粒子於連接材料中的比例,於將連接材料整體設為100重量份時,為了提高導熱率,上述金屬粒子於連接材料中的比例較理想的是大於等於80重量份,為了達成與高溫焊料同等或較之更高的導熱率,上述金屬粒子於連接材料中的比例更理想的是大於等於87重量份。
又,為了將連接材料製成糊狀,於將連接材料整體設為100重量份時,金屬粒子的比例較理想的是小於等於99重量份,為了提高點膠機或印刷機中的操作性,金屬粒子的比例更理想的是小於等於95重量份。
本發明中所使用的揮發性成分只要是對與金屬粒子的混合物施加既定的熱歷程時金屬粒子燒結的成分則無特別限制。
揮發性成分的一例可列舉:乙二醇丁醚(ethylene glycol butyl ether)、乙二醇苯醚、二乙二醇甲醚、二乙二醇***、二乙二醇丁醚、二乙二醇異丁醚、二乙二醇己醚、三乙二醇甲醚、二乙二醇二甲醚、二乙二醇二***、二乙二醇二丁醚、二乙二醇丁基甲基醚、二乙二醇異丙基甲基醚、三乙二醇二甲醚、三乙二醇丁基甲基醚、乙二醇***乙酸酯、乙二醇丁醚乙酸酯、二乙二醇***乙酸酯、二乙二醇丁醚乙酸酯、丙二醇丙醚、二丙二醇甲醚、二丙二醇***、二丙二醇丙醚、二丙二醇丁醚、二丙二醇二甲醚、三丙二醇甲醚、三丙二醇二甲醚、二丙二醇甲醚乙酸酯、3-甲基-3-甲氧基丁醇、乳酸乙酯、乳酸丁酯、γ-丁內酯、α-松脂醇(α-terpineol)、異佛酮(isophorone)、對異丙基甲苯(paracymene)、1,3-二甲基-2-咪唑啶酮(1,3-dimethyl-2-imidazolidinone)、苯甲醚(anisole)、二甲亞碸、六甲基磷醯胺(hexamethylphosphoramide)、間甲酚、鄰氯苯酚、溶纖劑乙酸酯(cellosolve acetate)、N-甲基-2-吡咯啶酮、N,N-二甲基乙醯胺、N,N-二甲基甲醯胺、環丁碸、四氫呋喃、二氧陸圜、乙二醇二甲醚(Monoglyme)、二乙二醇二甲醚(diglyme)、苯、甲苯、二甲苯、甲基乙基酮、甲基溶纖劑、溶纖劑乙酸酯、環己酮等。
上述揮發性成分可使用一種,或者視需要可將兩種或兩種以上的成分混合使用。關於揮發性成分的含量,為了提高導熱性,當將連接材料整體設為100重量份時,揮發性成分的含量較理想的是小於等於20重量份。
本發明中所使用的黏合成分(黏合劑(A))包含有機高分子化合物或其前驅物,視需要亦可包含反應性稀釋劑、硬化劑、用以提高硬化性的硬化促進劑、用以緩和應力的可撓劑、用以提高操作性的稀釋劑、黏著力提昇劑、潤濕性提昇劑、消泡劑及用以實現低黏度化的反應性稀釋劑中的一種或一種以上。再者,本發明的連接材料亦可包含此處列舉的化合物以外的成分。
上述有機高分子化合物或其前驅物並無特別限制,例如較好的是熱固性樹脂或其前驅物。上述樹脂例如可列舉:環氧樹脂、丙烯酸系樹脂、順丁烯二醯亞胺樹脂、氰酸酯樹脂或其前驅物等。
上述之中,丙烯酸系樹脂、順丁烯二醯亞胺樹脂等的可進行聚合的具有乙烯性碳-碳雙鍵的化合物或環氧樹脂,耐熱性及黏著性優異,且藉由使用適當之溶劑可製成液狀故操作性優異,就該些方面而言較佳。上述樹脂可單獨使用,或者可將兩種或兩種以上組合使用。
於使用環氧樹脂作為上述熱固性樹脂之情形時,較好的是併用硬化劑、硬化促進劑。上述環氧樹脂較好的是1分子中具有大於等於2個的環氧基的化合物,例如可列舉由雙酚A、雙酚F、雙酚AD等與表氯醇(epichlorohydrin)衍生的環氧樹脂等。
此種化合物只要是1分子中具有大於等於2個的環氧基的化合物則並無特別限制,例如可列舉:雙酚A型環氧樹脂[AER-X8501(旭化成工業(股),商品名)、R-301(Yuka Shell Epoxy(股),商品名)、YL-980(Yuka Shell Epoxy(股),商品名)]、雙酚F型環氧樹脂[YDF-170(東都化成(股),商品名)]、雙酚AD型環氧樹脂[R-1710(三井石油化學工業(股),商品名)]、苯酚酚醛清漆型環氧樹脂[N-730S(大日本油墨化學工業(股),商品名)、Quatrex-2010(陶氏化學公司,商品名)]、甲酚酚醛清漆型環氧樹脂[YDCN-702S(東都化成(股),商品名)、EOCN-100(日本化藥(股),商品名)]、多官能環氧樹脂[EPPN-501(日本化藥(股),商品名)、TACTIX-742(陶氏化學公司,商品名)、VG-3010(三井石油化學工業(股),商品名)、1032S(Yuka Shell Epoxy(股),商品名)]、具有萘骨架的環氧樹脂[HP-4032(大日本油墨化學工業(股),商品名)]、脂環式環氧樹脂[EHPE-3150、CEL-3000(泰金化學工業(股),商品名)、DME-100(新日本理化(股),商品名)]、脂肪族環氧樹脂[W-100(新日本理化(股),商品名)]、胺型環氧樹脂[ELM-100(住友化學工業(股),商品名)、YH-434L(東都化成(股),商品名)、TETRAD-X、TETRAC-C(三菱瓦斯化學(股),商品名)]、間苯二酚型環氧樹脂[DENACOL EX-201(長瀨化成工業(股),商品名)]、新戊二醇型環氧樹脂[DENACOL EX-211(長瀨化成工業(股),商品名)]、己二醇型環氧樹脂[DENACOL EX-212(長瀨化成工業(股),商品名)]、乙二醇-丙二醇型環氧樹脂[DENACOL EX-810、DENACOL EX-811、DENACOL EX-850、DENACOL EX-851、DENACOL EX-821、DENACOL EX-830、DENACOL EX-832、DENACOL EX-841、DENACOL EX-861(長瀨化成工業(股),商品名)]、下述通式(I)所表示的環氧樹脂[E-XL-24、E-XL-3L(三井東壓化學(股),商品名)]等。又,亦可將該些環氧樹脂適當組合使用。
(式中,a表示0~5的整數)。
又,環氧樹脂亦可包含1分子中僅具有一個環氧基的環氧化合物(反應性稀釋劑)。此種環氧化合物是以不阻礙本發明的連接材料的特性的範圍而使用,較好的是以相對於環氧樹脂總量為0~30重量%的範圍而使用。
此種環氧化合物的市售品可列舉:PGE(日本化藥(股),商品名)、PP-101(東都化成(股),商品名)、ED-502、ED-509、ED-509S(旭電化工業(股),商品名)、YED-122(Yuka Shell Epoxy(股),商品名)、KBM-403(信越化學工業(股),商品名)、TSL-8350、TSL-8355、TSL-9905(東芝矽膠(股),商品名)等。
又,環氧樹脂硬化劑並無特別限制,例如可列舉:苯酚酚醛清漆樹脂[H-1(明和化成(股),商品名)、VR-9300(三井東壓化學(股),商品名)]、苯酚芳烷基樹脂[XL-225(三井東壓化學(股),商品名)]、烯丙基化苯酚酚醛清漆樹脂[AL-VR-9300(三井東壓化學(股),商品名)]、下述通式(II)所表示的特殊酚樹脂[PP-700-300(日本石油化學(股),商品名)]、雙酚F、雙酚A、雙酚AD、烯丙基化雙酚F、烯丙基化雙酚A、烯丙基化雙酚AD、二氰基二醯胺、下述通式(III)所表示的二元酸二醯肼[ADH、PDH、SDH(均為Japan Hydrazine Company(股),商品名)]、由環氧樹脂與胺化合物的反應產物所形成的微膠囊型硬化劑[NOVACURE(旭化成工業(股),商品名)]等。又,亦可將該些硬化劑適當組合使用。
(式中,R1表示甲基、乙基等的碳數為1~6的烷基,R2表示氫或甲基、乙基等的碳數為1~6的烷基,b表示2~4的整數)。
(式中,R3表示間伸苯基、對伸苯基等的2價芳香族烴基,碳數為2~12的直鏈或支鏈的伸烷基)。
相對於100重量份的環氧樹脂,環氧樹脂硬化劑的調配量較好的是設為0.01重量份~90重量份,更好的是設為0.1重量份~50重量份。若環氧樹脂硬化劑的調配量小於0.01重量份,則存在硬化性下降的傾向,若環氧樹脂硬化劑的調配量超過90重量份,則存在黏度上升而操作性下降的傾向。
於本發明的連接材料中,視需要可添加硬化促進劑。硬化促進劑可列舉:有機硼鹽化合物[EMZ.K、TPPK(北興化學工業(股),商品名)]、三級胺類或其鹽[DBU、U-CAT 102、U-CAT 106、U-CAT 830、U-CAT 840、U-CAT 5002(SAN-APRO公司,商品名)]、咪唑類[CUREZOL、2P4MHZ、C17Z、2PZ-OK(四國化成(股),商品名)]等。
環氧樹脂硬化劑及視需要添加的硬化促進劑可分別單獨使用,又,亦可將多種環氧樹脂硬化劑及硬化促進劑適當組合使用。相對於100重量份的環氧樹脂,硬化促進劑的調配量較好的是小於等於20重量份。
本發明中所使用的可進行聚合的具有乙烯性碳-碳雙鍵的化合物可列舉丙烯酸酯化合物或甲基丙烯酸酯化合物等,此化合物是1分子中具有大於等於1個的丙烯基或甲基丙烯基的化合物,較好的是使用下述通式(IV)~通式(XIII)所表示的化合物。
通式(IV)所表示的化合物,
(式中,R4表示氫或甲基,R5表示碳數為1~100、較好的是碳數為1~36的具有2價脂肪族或環狀結構的脂肪族烴基)。
通式(IV)所表示的化合物可列舉:丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、丙烯酸異丙酯、丙烯酸正丁酯、丙烯酸異丁酯、丙烯酸第三丁酯、丙烯酸戊酯、丙烯酸異戊酯、丙烯酸己酯、丙烯酸庚酯、丙烯酸辛酯、丙烯酸-2-乙基己酯、丙烯酸壬酯、丙烯酸癸酯、丙烯酸異癸酯、丙烯酸十二烷酯、丙烯酸十三烷酯、丙烯酸十六烷酯、丙烯酸十八烷酯、丙烯酸異十八烷酯、丙烯酸環己酯、丙烯酸異冰片酯、丙烯酸三環[5.2.1.02.6]癸酯等的丙烯酸酯化合物,甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丙酯、甲基丙烯酸異丙酯、甲基丙烯酸正丁酯、甲基丙烯酸異丁酯、甲基丙烯酸第三丁酯、甲基丙烯酸戊酯、甲基丙烯酸異戊酯、甲基丙烯酸己酯、甲基丙烯酸庚酯、甲基丙烯酸辛酯、甲基丙烯酸-2-乙基己酯、甲基丙烯酸壬酯、甲基丙烯酸癸酯、甲基丙烯酸異癸酯、甲基丙烯酸十二烷酯、甲基丙烯酸十三烷酯、甲基丙烯酸十六烷酯、甲基丙烯酸十八烷酯、甲基丙烯酸異十八烷酯、甲基丙烯酸環己酯、甲基丙烯酸異冰片酯、甲基丙烯酸三環[5.2.1.02.6]癸酯等的甲基丙烯酸酯化合物。
通式(V)所表示的化合物,
(式中,R4及R5表示與通式(IV)中的R4及R5相同的基)。
通式(V)所表示的化合物有:丙烯酸-2-羥乙酯、丙烯酸-2-羥丙酯、甲基丙烯酸-2-羥乙酯、甲基丙烯酸-2-羥丙酯等。
通式(VI)所表示的化合物,
(式中,R4表示與通式(IV)中的R4相同的基,R6表示氫、甲基或苯氧基甲基,R7表示氫、碳數為1~6的烷基、二環戊烯基、苯基或苯甲醯基,b表示1~50的整數)。
通式(VI)所表示的化合物可列舉:二乙二醇丙烯酸酯、聚乙二醇丙烯酸酯、聚丙二醇丙烯酸酯、丙烯酸-2-甲氧基乙酯、丙烯酸-2-乙氧基乙酯、丙烯酸-2-丁氧基乙酯、甲氧基二乙二醇丙烯酸酯、甲氧基聚乙二醇丙烯酸酯、丙烯酸二環戊烯氧基乙酯、丙烯酸-2-苯氧基乙酯、苯氧基二乙二醇丙烯酸酯、苯氧基聚乙二醇丙烯酸酯、丙烯酸-2-苯甲醯氧基乙酯、丙烯酸-2-羥基-3-苯氧基丙酯等的丙烯酸酯化合物,二乙二醇甲基丙烯酸酯、聚乙二醇甲基丙烯酸酯、聚丙二醇甲基丙烯酸酯、甲基丙烯酸-2-甲氧基乙酯、甲基丙烯酸-2-乙氧基乙酯、甲基丙烯酸-2-丁氧基乙酯、甲氧基二乙二醇甲基丙烯酸酯、甲氧基聚乙二醇甲基丙烯酸酯、甲基丙烯酸二環戊烯氧基乙酯、甲基丙烯酸-2-苯氧基乙酯、苯氧基二乙二醇甲基丙烯酸酯、苯氧基聚乙二醇甲基丙烯酸酯、甲基丙烯酸-2-苯甲醯氧基乙酯、甲基丙烯酸-2-羥基-3-苯氧基丙酯等的甲基丙烯酸酯化合物等。
通式(VII)所表示的化合物,
[式中,R4表示與通式(IV)中的R4相同的基,R8表示苯基、腈基、-Si(OR9)3(R9表示碳數為1~6的烷基)、
(R10、R11及R12分別獨立表示氫或碳數為1~6的烷基,R13表示氫或碳數為1~6的烷基或苯基),c表示0、1、2或3的數]。
上述通式(VII)及(VII')所表示的化合物有:丙烯酸苄酯、丙烯酸-2-氰基乙酯、γ-丙烯醯氧基丙基三甲氧基矽烷、丙烯酸縮水甘油酯、丙烯酸四氫糠酯、丙烯酸四氫吡喃酯、丙烯酸二甲基胺基乙酯、丙烯酸二乙基胺基乙酯、丙烯酸-1,2,2,6,6-五甲基哌啶酯、丙烯酸-2,2,6,6-四甲基哌啶酯、磷酸丙烯醯氧基乙酯、酸式磷酸丙烯醯氧基乙基苯酯、氫化鄰苯二甲酸-β-丙烯醯氧基乙酯、氫化琥珀酸-β-丙烯醯氧基乙酯等的丙烯酸酯化合物,甲基丙烯酸苄酯、甲基丙烯酸-2-氰基乙酯、γ-甲基丙烯醯氧基丙基三甲氧基矽烷、甲基丙烯酸縮水甘油酯、甲基丙烯酸四氫糠酯、甲基丙烯酸四氫吡喃酯、甲基丙烯酸二甲基胺基乙酯、甲基丙烯酸二乙基胺基乙酯、甲基丙烯酸-1,2,2,6,6-五甲基哌啶酯、甲基丙烯酸-2,2,6,6-四甲基哌啶酯、磷酸甲基丙烯醯氧基乙酯、酸式磷酸甲基丙烯醯氧基乙基苯酯等的甲基丙烯酸酯,氫化鄰苯二甲酸-β-甲基丙烯醯氧基乙酯、氫化琥珀酸-β-甲基丙烯醯氧基乙酯等的甲基丙烯酸酯化合物等。
通式(VIII)所表示的化合物,
(式中,R4及R5表示與通式(IV)中的R4及R5相同的基)。
通式(VIII)所表示的化合物有:乙二醇二丙烯酸酯、1,4-丁二醇二丙烯酸酯、1,6-己二醇二丙烯酸酯、1,9-壬二醇二丙烯酸酯、1,3-丁二醇二丙烯酸酯、新戊二醇二丙烯酸酯、二聚醇二丙烯酸酯(dimerdiol acrylate)等的二丙烯酸酯化合物,乙二醇二甲基丙烯酸酯、1,4-丁二醇二甲基丙烯酸酯、1,6-己二醇二甲基丙烯酸酯、1,9-壬二醇二甲基丙烯酸酯、1,3-丁二醇二甲基丙烯酸酯、新戊二醇二甲基丙烯酸酯、二聚醇二甲基丙烯酸酯等的二甲基丙烯酸酯化合物。
通式(IX)所表示的化合物,
(式中,R4表示與通式(IV)中的R4相同的基,R6、b與通式(VI)中的R6、b相同)。
通式(IX)所表示的化合物有:二乙二醇二丙烯酸酯、三乙二醇二丙烯酸酯、四乙二醇二丙烯酸酯、聚乙二醇二丙烯酸酯、三丙二醇二丙烯酸酯、聚丙二醇二丙烯酸酯等的二丙烯酸酯化合物,二乙二醇二甲基丙烯酸酯、三乙二醇二甲基丙烯酸酯、四乙二醇二甲基丙烯酸酯、聚乙二醇二甲基丙烯酸酯、三丙二醇二甲基丙烯酸酯、聚丙二醇二甲基丙烯酸酯等的二甲基丙烯酸酯化合物等。
通式(X)所表示的化合物,
(式中,R4表示與通式(IV)中的R4相同的基,R14及R15分別獨立表示氫或甲基)。
通式(X)所表示的化合物有:1莫耳的雙酚A、雙酚F或雙酚AD與2莫耳的丙烯酸縮水甘油酯的反應產物,1莫耳的雙酚A、雙酚F或雙酚AD與2莫耳的甲基丙烯酸縮水甘油酯的反應產物等。
通式(XI)所表示的化合物,
(式中,R4表示與通式(IV)中的R4相同的基,R14及R15表示與通式(X)中的R14及R15相同的基,R16及R17分別獨立表示氫或甲基,d及e分別獨立表示1~20的整數)。
通式(XI)所表示的化合物有:雙酚A、雙酚F或雙酚AD的聚氧化乙烯加成物的二丙烯酸酯,雙酚A、雙酚F或雙酚AD的聚氧化丙烯加成物的二丙烯酸酯,雙酚A、雙酚F或雙酚AD的聚氧化乙烯加成物的二甲基丙烯酸酯,雙酚A、雙酚F或雙酚AD的聚氧化丙烯加成物的二甲基丙烯酸酯等。
通式(XII)所表示的化合物,
(式中,R4表示與通式(IV)中的R4相同的基,R18、R19、R20及R21分別獨立表示氫或甲基,f表示1~20的整數)。
通式(XII)所表示的化合物有:雙(丙烯醯氧基丙基)聚二甲基矽氧烷、雙(丙烯醯氧基丙基)甲基矽氧烷-二甲基矽氧烷共聚物、雙(甲基丙烯醯氧基丙基)聚二甲基矽氧烷、雙(甲基丙烯醯氧基丙基)甲基矽氧烷-二甲基矽氧烷共聚物等。
通式(XIII)所表示的化合物,
(式中,R4表示與通式(IV)中的R4相同的基,g、h、i、j及k分別獨立表示大於等於1、較好的是1~10的數)。
通式(XIII)所表示的化合物有:使加成有順丁烯二酸酐的聚丁二烯與分子內具有羥基的丙烯酸酯化合物或甲基丙烯酸酯化合物反應所得的反應產物及其氫化物,只要是1分子中具有大於等於1個的丙烯基或甲基丙烯基的化合物則並無特別限制,例如有MM-1000-80、MAC-1000-80(均為日本石油化學(股)商品名)等。
可進行聚合的具有乙烯性碳-碳雙鍵的化合物可單獨使用上述化合物,或者將兩種或兩種以上的上述化合物組合使用。
於使用具有乙烯性碳-碳雙鍵的化合物作為上述熱固性樹脂之情形時,較好的是併用自由基起始劑作為硬化劑觸媒。自由基起始劑並無特別限制,就空隙等的方面而言較好的是過氧化物,又,就連接材料的硬化性及黏度穩定性的方面而言,較好的是過氧化物的分解溫度為70℃~170℃。
自由基起始劑的具體例可列舉:1,1,3,3-四甲基過氧基-2-乙基己酸酯(1,1,3,3-tetramethylperoxy-2-ethylhexanoate)、1,1-雙(第三丁基過氧基)環己烷、1,1-雙(第三丁基過氧基)環十二烷、過氧化間苯二甲酸-二-第三丁酯(di-tert-butylperoxyisophthalate)、過氧化苯甲酸第三丁酯、過氧化二異丙苯、過氧化第三丁基異丙苯、2,5-二甲基-2,5-二(第三丁基過氧基)己烷、2,5-二甲基-2,5-二(第三丁基過氧基)己炔、過氧化氫異丙苯(cumenehydroperoxide)等。
相對於可進行聚合的具有乙烯性碳-碳雙鍵的化合物的總量100重量份,自由基起始劑的調配量較好的是0.1重量份~10重量份,尤其好的是0.5重量份~5重量份。
上述黏合成分可使用一種,或者可視需要將兩種或兩種以上的成分混合使用。於將連接材料整體設為100重量份時,黏合成分的含量較理想的是3重量份~30重量份。
可撓劑的例子可列舉液狀聚丁二烯(宇部興產公司製造的「CTBN-1300×31」、「CTBN-1300×9」等的丙烯腈丁二烯共聚物,較好的是分子內具有選自環氧基、羧基、胺基及乙烯基中的至少一種或一種以上的官能基。
丙烯腈丁二烯共聚物可預先與上述環氧樹脂以環氧樹脂:丙烯腈丁二烯共聚物=10:90~90:10(重量份)的比率於80℃~120℃下反應20分鐘~6小時左右。反應時,視需要可使用丁基溶纖劑、卡必醇(carbitol)、乙酸丁基溶纖劑、乙酸卡必醇、乙二醇二***、α-松脂醇等的沸點相對較高的有機溶劑。
丙烯腈丁二烯共聚物的數量平均分子量較好的是500~10000。若分子量小於500,則存在晶片翹曲的減少效果差的傾向,若分子量超過10000,則存在連接材料的黏度上升而操作性差的傾向。數量平均分子量是藉由蒸氣壓浸透法(Vapor Pressure Osmometry)測定的值或藉由凝膠滲透層析法(Gel Permeation ChromatograPhy,GPC)利用標準聚苯乙烯的校正曲線來進行測定(以下稱作GPC法)的值。
又,環氧化聚丁二烯較好的是環氧當量為100(g/eq)~500(g/eq)。若環氧當量小於100,則存在黏度增大而連接材料的操作性下降的傾向,若環氧當量超過500,則存在加熱時的黏著強度下降的傾向。再者,環氧當量是藉由過氯酸法而求出的。環氧化聚丁二烯亦可使用分子內具有羥基的環氧化聚丁二烯。
環氧化聚丁二烯的數量平均分子量較好的是500~10000。若分子量小於500,則存在晶片翹曲的減少效果差的傾向,若分子量超過10000,則存在連接材料的黏度上升而操作性差的傾向。數量平均分子量是藉由GPC法測定的值。
可撓劑具有緩和由於將半導體元件與導線架黏著而產生的應力的效果。於將有機高分子化合物及其前驅物的總量設為100重量份時,可撓劑通常是添加0~500重量份。
於本發明的連接材料中,視需要可進一步適當添加氧化鈣、氧化鎂等的吸濕劑,矽烷偶合劑、鈦酸酯偶合劑、鋁偶合劑、鋁鋯偶合劑(zircoaluminate coupling agent)等的黏著力提昇劑,非離子系界面活性劑、氟系界面活性劑等的潤濕性提昇劑,矽油(silicone oil)等的消泡劑,無機離子交換體等的離子捕捉劑(ion-trap agent),聚合抑制劑等。
此處,矽烷偶合劑例如可列舉:乙烯基三(β-甲氧基乙氧基)矽烷、乙烯基三乙氧基矽烷、乙烯基三甲氧基矽烷、γ-甲基丙烯醯氧基丙基三甲氧基矽烷、β-(3,4-環氧環己基)乙基三甲氧基矽烷、γ-縮水甘油氧基丙基三甲氧基矽烷、γ-縮水甘油氧基丙基甲基二乙氧基矽烷、N-苯基-γ-胺基丙基三甲氧基矽烷、γ-巰基丙基三甲氧基矽烷、六甲基二矽氮烷(hexamethyl disilazane)、N,O-雙(三甲基矽烷基)乙醯胺、N-甲基-3-胺基丙基三甲氧基矽烷、4,5-二氫咪唑丙基三乙氧基矽烷、γ-巰基丙基三乙氧基矽烷、γ-巰基丙基甲基二甲氧基矽烷、3-氰基丙基三甲氧基矽烷、甲基三(甲基丙烯醯氧基乙氧基)矽烷、甲基三(縮水甘油氧基)矽烷、2-乙基己基膦酸-2-乙基己酯(2-ethylhexyl-2-ethylhexyl-phosphonate)、γ-縮水甘油氧基丙基甲基二甲氧基矽烷、乙烯基三乙醯氧基矽烷、γ-苯胺基丙基三甲氧基矽烷、γ-巰基丙基甲基二甲氧基矽烷、γ-甲基丙烯醯氧基丙基甲基二甲氧基矽烷、N-三甲基矽烷基乙醯胺、二甲基三甲基矽烷基胺、二乙基三甲基矽烷基胺、三甲基矽烷基咪唑、三甲基矽烷基異氰酸酯、二甲基矽烷基二異氰酸酯、甲基矽烷基三異氰酸酯、乙烯基矽烷基三異氰酸酯、苯基矽烷基三異氰酸酯、四異氰酸酯矽烷、乙氧基矽烷三異氰酸酯等。
上述鈦酸酯偶合劑例如可列舉:異丙基三異硬脂醯基鈦酸酯(isopropyl tri-isostearoyl titanate)、異丙基三辛醯基鈦酸酯、異丙基二甲基丙烯醯基異硬脂醯基鈦酸酯、異丙基三(十二烷基)苯磺醯基鈦酸酯、異丙基異硬脂醯基二丙烯基鈦酸酯、異丙基三(二辛基磷醯氧基)鈦酸酯(isopropyl tri(dioctylphosphate)titanate)、異丙基三異丙苯基苯基鈦酸酯、異丙基三(二辛基焦磷醯氧基)鈦酸酯(isopropyl tri(dioctylpyrophosphate)titanate)、四異丙基雙(二辛基亞磷醯氧基)鈦酸酯、四辛基雙[二(十三烷基)亞磷醯氧基]鈦酸酯(tetraoctyl bis[di(tridecyl)Phosphite]titanate)、四(2,2-二烯丙氧基甲基-1-丁基)雙[二(十三烷基)]亞磷醯氧基鈦酸酯、二異丙苯基苯氧基乙醯氧基鈦酸酯、雙(二辛基焦磷醯氧基)氧基乙醯氧基鈦酸酯、二異硬脂醯基鈦酸乙二酯(di-isostearoyl ethylene titanate)、雙(二辛基焦磷醯氧基)鈦酸乙二酯、二異丙氧基雙(2,4-戊二醯氧基)鈦(IV)、二異丙基雙三乙醇胺基鈦酸酯、乳酸鈦、乙醯乙酸酯鈦酸酯(acetoacetic ester titanate)、二異丙氧基雙(乙醯丙酮)鈦、二正丁氧基雙(三乙醇胺)鈦、二羥基雙(乳酸)鈦(dihydroxy bis(lactato)titanium)、異丙氧基辛二醇鈦(titanium-iso-propoxyoctylene glycolate)、硬脂酸鈦、單硬脂酸三正丁氧基鈦、乳酸乙酯鈦(titanium lactate ethyl ester)、三乙醇胺鈦(titanium triethanol aminato)等。
作為聚合抑制劑,例如可列舉:醌類、對苯二酚、硝基/亞硝基化合物、胺類、多氧基化合物、對第三丁基鄰苯二酚、苦味酸(picric acid)、二硫代苯甲醯基二硫醚(dithiobenzoyl disulfide)等的含硫化合物、氯化銅、二苯基苦味肼、三-對硝基苯基甲基、三苯基四聯氮基(triphenyl verdazyl)、氧化N-(3-N-氧基苯胺基-1,3-二甲基亞丁基)苯胺(N-(3-N-oxyanilino-1,3-dimethyl butylidene)anilinoxide)等,但並不限定於該些化合物。
於本發明的連接材料中,視需可要進一步添加滲出抑制劑。滲出抑制劑例如有:全氟辛酸、辛醯胺、油酸等的脂肪酸、丙烯酸全氟辛基乙酯、矽酮等。
上述填料(B)可使用各種公知的填料,例如可使用金、鉑、銀、銅、鎳、鈀、鐵、鋁等的導電性粉體。又,該些填料可單獨使用,或者可將兩種或兩種以上組合使用。其中,特別是銀及銅於價格、導電性及導熱性等的方面而言較為理想。
上述添加劑(C)可使用上述揮發性成分或表面保護劑。
製造上述連接材料時,適當組合攪拌器、擂潰器、三輥研磨機、行星式混合機(planetary mixer)等的分散、溶解裝置,將金屬粒子、揮發性成分及黏合劑連同視需要添加的稀釋劑等一併或分步地視需要進行加熱並加以混合、溶解、碎粒混練或分散,製成均勻的糊狀即可。
圖7是表示使用本發明的連接材料而製造的半導體裝置的一例的示意剖面圖。圖7所示的半導體裝置包含:三個導線架(散熱體)12a、12b、12c,於導線架12a上經由本發明的連接材料13而連接的晶片(發熱體)11,以及對該些構件進行鑄模的鑄模樹脂15。晶片11經由2根金屬線14而分別連接於導線架12b、12c。
圖8是表示使用本發明的連接材料而製造的半、導體裝置的其他例的示意剖面圖。圖7所示的半導體裝置包含:基板16,以包圍基板的方式形成的兩個導線架17,於導線架17上經由本發明的連接材料13而連接的LED晶片18,以及將該些構件加以密封的透光性樹脂19。LED晶片18經由金屬線14而連接於導線架17。
本發明的半導體裝置是藉由使用本發明的連接材料將半導體元件黏著於支持部材上而獲得。將半導體元件黏
著於支持部材上之後,視需要進行打線接合工程及密封工程。
支持構件例如可列舉:42合金導線架、銅導線架、預鍍鈀導線架(palladium pre-plated Lead-frames,Pd-PPF)等的導線架,玻璃環氧基板(由玻璃纖維強化環氧樹脂形成的基板)、順丁烯二醯亞胺-三嗪(Bismaleimide-Triazine,BT)基板(使用由氰酸酯單體及其低聚物與順丁烯二醯亞胺所形成的BT樹脂的基板)等的有機基板。
使用本發明的連接材料將半導體元件黏著於導線架等的支持構件上時,可藉由如下方式來進行:首先,於支持構件上藉由點膠法、網版印製法、衝壓法等而塗佈連接材料,然後對半導體元件進行壓接,其後使用烘箱(oven)或加熱塊(heat block)等的加熱裝置進行加熱硬化。加熱硬化通常是藉由在100℃~200℃下加熱5秒~10小時而進行的。進而,經由打線接合工程之後,藉由通常的方法進行密封,藉此可獲得製作完畢的半導體裝置。
實施例
以下,藉由實施例詳細說明本發明,但本發明並不限於實施例。實施例及參考例中使用的材料是以如下方式製作或取得。
(1)環氧樹脂溶液:將7.5重量份的YDF-170(東都化成(股),商品名,雙酚F型環氧樹脂,環氧當量=170)及7.5重量份的YL-980(Yuka Shell Epoxy(股),商品名,雙酚A型環氧樹脂,環氧當量=185)加熱到80℃,持續攪拌1小時,獲得均勻的環氧樹脂溶液。
(2)硬化促進劑:2PZCNS-PW(四國化成工業(股),商品名,咪唑)1.1重量份;(3)揮發性成分:二丙二醇甲醚乙酸酯(以下稱作DMPA)(泰金化學(股))、甲苯(關東化學(股))、γ-丁內酯(三協化學(股));(4)金屬粒子:K-0082P(METALOR,商品名,銀粉,平均粒徑為1.6 μm,氧的狀態比率為4%),AgF10S(德力化學研究所(股),商品名,銀粉,平均粒徑為10 μm,氧的狀態比率為15%)
又,按照以下順序製作對AgF10S實施了氧化膜去除及表面處理的表面處理Ag粉。
以80重量份的乙醇(關東化學(股))將28重量份的鹽酸(關東化學(股))稀釋,調整酸性溶液。於該酸性溶液中添加0.29重量份的十八硫醇(東京化成工業(股))作為表面保護材料,從而製備表面處理液。
於該表面處理液中添加AgF10S,保持於40℃之狀態攪拌1小時,以進行氧化膜去除及表面處理。其後,藉由過濾而去除表面處理液,添加40℃的乙醇而對表面處理Ag粉進行清洗。
進而,藉由過濾而去除乙醇的清洗液,並將此清洗、過濾工程反覆進行10次左右,而將物理吸附於表面處理Ag粉表面上的十八硫醇及鹽酸去除。
最後,對清洗後的表面處理Ag粉進行減壓乾燥,由此去除乙醇,獲得乾燥狀態的表面處理Ag粉。所獲得的表面處理Ag粉的氧的狀態比率為0%,確認到氧化膜已被完全去除。
使用擂潰機將材料(1)及(2)混練10分鐘,而獲得黏合成分。
接著,以表1所示的調配比例添加材料(3)及(4)並使用擂潰機混練15分鐘,獲得連接材料。
藉由下示方法來觀察連接材料的特性。將金屬粒子、揮發性成分及黏合成分的組成、以及特性的測定結果示於表1及表2。
(1)切變強度:將0.2 mg的連接材料塗佈於鍍Ag的Cu導線架(焊盤部:10 mm×5 mm)上,並於其上方黏著2 mm×2 mm的鍍Ag的Cu晶片(厚度為0.15 mm),進而於加熱板(HHP-401)上於180℃下加熱處理1小時。
對其使用萬能型黏合力測試機(Bond Tester)(DAGE公司製造,4000系列),以500 μm/s之測定速度、100 μm之測定高度,測定於260℃下加熱30秒之後的剪切強度(切變強度)(MPa)。
(2)連接材料硬化物的導熱率:於180℃下對上述連接材料加熱處理1小時,獲得10 mm×10 mm×1 mm的試驗片。藉由雷射閃光法(NETZSCH公司製造,LFA 447,25℃)測定此試驗片的熱擴散率,進而根據此熱擴散率、藉由示差掃描熱量測定裝置(Perkin Elmer公司製造的Pyris1)獲得的比熱容量以及藉由阿基米德法(Archimedes method)獲得的比重的積,來計算出25℃時的連接材料的硬化物導熱率(W/m.K)。
如表1及表2所示表明,實施例1~實施例3的由表面處理Ag粉及揮發性成分所構成的連接材料表現出大於等於70 W/m.K的高導熱率、以及於260℃下為大於等於7 MPa的高切變強度。相對於此,由參考例1~參考例3表明,由氧的狀態比率為大於等於15%的Ag粉(AgF10S)及揮發性成分所構成的連接材料,因在180℃下不進行金屬粒子彼此的燒結,故無法製作導熱率測定用的試驗片,亦未表現出切變強度。
又,由參考例4表明,由氧的狀態比率為大於等於15%的Ag粉(AgF10S)、揮發性成分及黏合成分所構成的連接材料,導熱率低至小於等於3 W/m.K,但實施例4的由表面處理Ag粉、揮發性成分及黏合成分所構成的連接材料在維持了切變強度的狀態下表現出大於等於20 W/m.K的高導熱率。
進而,由參考例5表明,由氧的狀態比率為大於等於15%的AgF10S及黏合成分所構成的連接材料,導熱率低至小於等於2 W/m.K,但實施例5的由表面處理AgF10S及黏合成分所構成的連接材料在維持了切變強度的狀態下表現出大於等於20 W/m.K的高導熱率。
再者,由實施例6及實施例7表明,由氧的狀態比率為10%的表面處理AgF5S、揮發性成分及黏合成分所構成的連接材料與參考例6及參考例7所示的由氧的狀態比率為大於等於20%的AgF5S、揮發性成分及黏合成分所構成的連接材料相比,表現出更高的導熱率及切變強度。
(實施例8~實施例14及參考例8~參考例11)
準備下述黏合劑(A)、填料(B)及添加劑(C)。
黏合劑(A):
黏合劑(A)是藉由如下方式而製備:使用擂潰機,將37.6重量份的環氧樹脂溶液(A1)、9.2重量份的丙烯腈丁二烯共聚物(A2)、18.4重量份的環氧化聚丁二烯(A3)、1.8重量份的環氧樹脂硬化劑(A4)、0.8重量份的硬化促進劑(A5)、18.2重量份的稀釋劑(A6)、14.7重量份的甲基丙烯酸酯化合物(A7)及0.5重量份的自由基起始劑(A8)混練10分鐘。
環氧樹脂溶液(A1):將7.5重量份的YDF-170(東都化成股份有限公司,商品名,雙酚F型環氧樹脂,環氧當量=170)及7.5重量份的YL-980(日本環氧樹脂股份有限公司,商品名,雙酚A型環氧樹脂,環氧當量=185)加熱到80℃,持續攪拌1小時,獲得均勻的環氧樹脂溶液。
丙烯腈丁二烯共聚物(A2):CTBNX-1300×9(宇部興產股份有限公司,商品名,羧基末端丙烯腈丁二烯共聚物)
環氧化聚丁二烯(A3):E-1000-8.0(日本石油化學股份有限公司,商品名)環氧樹脂硬化劑(A4):二氰基二醯胺
硬化促進劑(A5):C17Z(四國化成股份有限公司,商品名,咪唑)
稀釋劑(A6):PP-101(東都化成股份有限公司,商品名,烷基苯基縮水甘油醚)
甲基丙烯酸酯化合物(A7):乙二醇二甲基丙烯酸酯自由基起始劑(A8):過氧化二異丙苯
填料(B):AgC-224(福田金屬箔粉股份有限公司,商品名,銀粉,平均粒徑為10 μm)
SPQ05J(三井金屬礦業股份有限公司,商品名,銀粉,平均粒徑為0.85 μm)
SA1507(METALOR,商品名,銀粉,平均粒徑為15 μm)
添加劑(C):二丙二醇甲醚
甲苯
丙二醇甲醚乙酸酯
十二硫醇
以表3所示的調配比例來混合所準備的黏合劑(A)、填料(B)及添加劑(C),並使用擂潰機混練15分鐘之後,於小於等於5托(Torr)下進行混練,從而獲得實施例8~實施例14及參考例8~參考例11的連接材料。
藉由下述方法測定實施例8~實施例14及參考例8~參考例11的連接材料的特性、及填料(B)與添加劑(C)的混合物成型體的特性。將其結果示於表3。
(1)黏度:使用電液動力(electrohydrodynamic,EHD)型旋轉黏度計(東京計器公司製造),測定連接材料於250℃時的0.5 rpm的黏度(Pa.s)。
(2)晶片切變強度(剪切強度):將約0.2 mg的連接材料塗佈於鍍鈀導線架(PPF,焊盤部:10 mm×8 mm)上,於其上方壓接2 mm×2 mm的矽晶片(厚度為0.4 mm),進而使用潔淨烘箱(clean oven)(ESPEC公司製造)於180℃下加熱處理1小時。對其使用萬能型黏合力測試機(DAGE公司製造,4000系列),以500 μm/s的測定速度、120 μm的測定高度,測定於260℃下加熱30秒之後的剪切強度(MPa)。
(3)填料(B)與添加劑(C)的混合物成型體的導熱率:以表3所示的調配比例來調配填料(B)與添加劑(C)以使總重量達到20 g,並使用研缽等進行混練。將所生成的粉體狀或糊狀的混合物成型為10 mm×10 mm×1 mm,並於180℃下加熱處理1小時。藉由雷射閃光法(NETZSCH公司製造,LFA 447,25℃)測定此成型物的熱擴散率,進而根據此熱擴散率、藉由示差掃描熱量測定裝置(Perkin Elmer公司製造的Pyris1)獲得的比熱容量以及藉由阿基米德法獲得的比重的積,來計算出25℃時的填料(B)與添加劑(C)的混合物成型體的硬化物的導熱率(W/m.K)。
(4)連接材料的硬化物的導熱率:將上述連接材料於180℃下加熱處理1小時,獲得10 mm×10 mm×1 mm的試驗片。藉由雷射閃光法(NETZSCH公司製造,LFA 447,25℃)測定此試驗片的熱擴散率,進而根據此熱擴散率、藉由示差掃描熱量測定裝置(Perkin Elmer公司製造的Pyris1)獲得的比熱容量以及藉由阿基米德法獲得的比重的積,來計算出25℃時的連接材料的硬化物導熱率(W/m.K)。
根據實施例8~實施例14的連接材料,可具有操作性優異的黏度,並且可維持黏著強度並提高導熱率。不含添加劑的參考例8的連接材料,填料(B)與添加劑(C)的混合物成型體的導熱率低,且連接材料的硬化體的導熱率亦低。不含添加劑的參考例9的連接材料,雖然連接材料的硬化物的導熱率相對較高,但是因填料(B)的含有比率高,故連接材料的黏度高。參考例10的連接材料雖然含有添加劑,但填料(B)與添加劑(C)的混合物成型體的導熱率低,故連接材料的硬化體的導熱率低。參考例11的連接材料雖然含有添加劑,且連接材料的硬化體的導熱率高,但填料(B)與添加劑(C)的混合物成型體的導熱率低,且連接材料的黏度高。
雖然本發明已以實施例揭露如上,然其並非用以限定本發明,任何所屬技術領域中具有通常知識者,在不脫離本發明之精神和範圍內,當可作些許之更動與潤飾,故本發明之保護範圍當視後附之申請專利範圍所界定者為準。
1、4‧‧‧表面保護材料
2‧‧‧氧化膜
3‧‧‧塊狀金屬
11‧‧‧晶片
12a、12b、12c‧‧‧導線架
13‧‧‧連接材料
14‧‧‧金屬線
15‧‧‧鑄模樹脂
16‧‧‧基板
17‧‧‧導線架
18‧‧‧晶片
19‧‧‧透光性樹脂
圖1是對表面氧化膜少的金屬粒子實施了使用表面保護材料的表面處理之後的金屬粒子的示意圖。
圖2是表示圖1中所示的金屬粒子的表面保護材料脫離、金屬粒子彼此燒結之狀態的示意圖。
圖3是對表面氧化膜多的金屬粒子實施了使用表面保護材料的表面處理之後的金屬粒子的示意圖。
圖4是表示圖3中所示的金屬粒子的表面保護材料脫離、但金屬粒子彼此無法燒結之狀態的示意圖。
圖5是對氧化膜多的金屬粒子實施了去除表面氧化膜的處理及使用表面保護材料的表面處理之後的金屬粒子的示意圖。
圖6是表示圖5中所示的金屬粒子的表面保護材料脫離、金屬粒子彼此燒結之狀態的示意圖。
圖7是表示本發明的半導體裝置的一例的示意剖面
圖。
圖8是表示本發明的半導體裝置的其他例的示意剖面圖。
11...晶片
12a、12b、12c...導線架
14...金屬線
15...鑄模樹脂
Claims (6)
- 一種連接材料,此連接材料含有藉由X射線光電子分光法測定的氧的狀態比率小於15%的銀粒子,上述銀粒子的平均粒徑為大於等於0.1μm且小於等於50μm。
- 如申請專利範圍第1項所述之連接材料,其中上述銀粒子是實施了將其表面的氧化膜去除的處理及使用表面保護材料的表面處理的銀粒子。
- 如申請專利範圍第1項或第2項所述之連接材料,其中上述銀粒子是於小於等於200℃下可燒結的銀粒子。
- 如申請專利範圍第1項或第2項所述之連接材料,此連接材料是更含有揮發性成分或黏合成分而成的。
- 如申請專利範圍第3項所述之連接材料,此連接材料是更含有揮發性成分或黏合成分而成的。
- 一種半導體裝置,此半導體裝置具有經由如申請專利範圍第1項至第5項中任一項所述之連接材料而將半導體元件與半導體元件搭載用支持構件黏著的結構。
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EP2278593A4 (en) | 2013-08-28 |
CN104962214A (zh) | 2015-10-07 |
KR101311681B1 (ko) | 2013-09-25 |
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JPWO2009133897A1 (ja) | 2011-09-01 |
US20110101543A1 (en) | 2011-05-05 |
KR20100137581A (ko) | 2010-12-30 |
US8421247B2 (en) | 2013-04-16 |
JP2015057825A (ja) | 2015-03-26 |
JP6056821B2 (ja) | 2017-01-11 |
WO2009133897A1 (ja) | 2009-11-05 |
JP5921808B2 (ja) | 2016-05-24 |
CN102017016A (zh) | 2011-04-13 |
EP2278593A1 (en) | 2011-01-26 |
JP2016135843A (ja) | 2016-07-28 |
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