TW201730276A - 熱傳導性矽酮組合物以及半導體裝置 - Google Patents
熱傳導性矽酮組合物以及半導體裝置 Download PDFInfo
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- TW201730276A TW201730276A TW105131982A TW105131982A TW201730276A TW 201730276 A TW201730276 A TW 201730276A TW 105131982 A TW105131982 A TW 105131982A TW 105131982 A TW105131982 A TW 105131982A TW 201730276 A TW201730276 A TW 201730276A
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Abstract
本發明提供一種具有優異的熱傳導性的熱傳導性矽酮組合物。其包含下述成分(A)和成分(B):成分(A)為有機聚矽氧烷,其以下述平均組成式(1)所表示,且在25℃下的運動黏度為10~100000mm2/s。〔式中R1表示選自氫原子、羥基或碳原子數為1~18的飽和或不飽和一價烴基中的一種或二種以上基團,a滿足1.8≦a≦2.2。〕,成分(B)為銀粉末,其振實密度為3.0g/cm3以上,比表面積為2.0m2/g以下。相對於100質量份的成分(A),成分(B)的配合量為300~11000質量份。R1aSiO(4-a)/2 (1)
Description
本發明涉及熱傳導性優異的矽酮組合物以及半導體裝置。
由於多數的電子部件在使用中放熱,為了確實地發揮該電子部件的功能,需要從該電子部件去除熱。尤其是被用於個人計算機的CPU等的集成電路元件,由於操作頻率的高速化導致熱值增大,從而散熱對策則成為重要的問題。
人們提出了眾多的散放出上述熱的方法。特別是提出了在放熱量多的電子部件中,於電子部件和散熱體等的部件之間借助熱傳導性潤滑脂和熱傳導性片材的熱傳導性材料進行放熱的方法。
在日本特開平2-153995號公報(專利文獻1)中,公開了將一定粒徑範圍的球狀六方晶系氮化鋁粉配合在特定的有機聚矽氧烷中的矽酮潤滑脂組合物;在日本特開平3-14873號公報(專利文獻2)中,公開了組合細粒徑的氮化鋁粉和粗粒徑的氮化鋁粉的熱傳導性有機矽氧烷組合物;在日本特開平10-110179號公報(專利文獻3)中,公開了組合氮化鋁粉和氧化鋅粉的熱傳導性矽酮潤滑脂組合物;在日本特開2000-63872號公報(專利文獻4)中,公開了使用用有機矽烷處理了的氮化鋁粉的熱傳導性潤滑脂組合物。
氮化鋁的熱傳導率為70~27OW/mK,由此作為熱傳導性高的材料,有
熱傳導率900~2000W/mK的金剛石°在日本特開2002-30217號公報(專利文獻5)中,公開了使用了矽酮樹脂、金剛石、氧化鋅以及分散劑的熱傳導性矽酮組合物。
另外,在日本特開2000-63873號公報(專利文獻6)和日本特開2008-222776號公報(專利文獻7)中,公開了於矽油等的基礎油中混合了金屬鋁粉的熱傳導性潤滑脂組合物。
進一步,還公開了將熱傳導率高的銀粉作為填充劑使用的日本專利3130193號公報(專利文獻8)和日本專利3677671號公報(專利文獻9)等。
但是,以上所有的熱傳導性材料和熱傳導性潤滑脂針對最近的CPU等的集成電路元件的放熱量皆為不充分的熱傳導性材料。
專利文獻1日本特開平2-153995號公報
專利文獻2日本特開平3-14873號公報
專利文獻3日本特開平10-110179號公報
專利文獻4日本特開2000-63872號公報
專利文獻5日本特開2002-30217號公報
專利文獻6日本特開2000-63873號公報
專利文獻7日本特開2008-222776號公報
專利文獻8日本專利3130193號公報
專利文獻9日本專利3677671號公報
因此,本發明的目的在於,提供一種發揮良好的放熱效果的熱傳導性矽酮組合物。
為了達到上述目的,本發明人們依據精心研究的結果,找出了通過將具有特定的振實密度和比表面積的銀粉混合在特定的有機聚矽氧烷中,從而能夠飛躍性地提高熱傳導性的方法,進而完成了本發明。
即,本發明為提供以下的熱傳導性矽酮組合物等的發明。
<1>一種熱傳導性矽酮組合物,其包含:下述成分(A)和成分(B),其中,成分(A)為以下述平均組成式(1)表示,且在25℃的運動黏度為10~100000mm2/s的有機聚矽氧烷,R1 aSiO(4-a)/2 (1)式中,R1表示選自氫原子、羥基或碳原子數為1~18的飽和或不飽和一價烴基中的一種或二種以上基團,a滿足1.8≦a≦2.2,成分(B)為振實密度3.0g/cm3以上、比表面積為2.0m2/g以下的銀粉,相對於100質量份的成分(A),其為300~11000質量份。
<2>如<1>之熱傳導性矽酮組合物,其中,成分(B)的銀粉的縱橫比為2.0以上且150.0以下。
<3>如<1>或<2>之熱傳導性矽酮組合物,其中,部分或全部成分(A)為:
成分(C),在1個分子中至少含有2個與矽原子鍵合的烯基之有機聚矽氧烷;和/或成分(D),在1個分子中至少含有2個與矽原子鍵合的氫原子之有機氫聚矽氧烷。
<4>如<1>或<2>之熱傳導性矽酮組合物,其進一步含有固化催化劑。
<5>如<1>或<2>所述的熱傳導性矽酮組合物,其進一步含有作為成分(E)的有機矽烷,該作為成分(E)的有機矽烷以下述式(2)所表示,R2 bSi(OR3)4-b (2)式中,R2表示選自任選具有取代基的飽和或不飽和的一價烴基、環氧基、丙烯基以及甲基丙烯基中的1種或2種以上基團、R3表示一價烴基、b滿足1≦b≦3,並且,相對於100質量份的成分(A),所述作為成分(E)的有機矽烷的含量為0~10質量份。
<6>一種半導體裝置,其為具備放熱性電子部件和散熱體的半導體裝置,且<1>或<2>之熱傳導性矽酮組合物介於上述放熱性電子部件和散熱體之間。
<7>一種半導體裝置的製造方法,該方法具有如下步驟:於放熱性電子部件和散熱體之間,在施加0.01MPa以上的壓力狀態下將<1>或<2>所述的熱傳導性矽酮組合物加熱至80℃以上。
本發明的熱傳導性矽酮組合物由於具有優異的熱傳導性,因此對半導體裝置為有用。
1‧‧‧基板
2‧‧‧放熱性電子部件(CPU)
3‧‧‧熱傳導性矽酮組合物層
4‧‧‧散熱體(蓋)
圖1為表示本發明的半導體裝置的一例的縱剖面概略圖。
以下,對本發明的熱傳導性矽酮組合物加以詳細地說明。
成分(A):
為成分(A)的有機聚矽氧烷為以下述平均組成式(1)所表示,且在25℃下的運動黏度為10~100000mm2/s的有機聚矽氧烷。
R1 aSiO(4-a)/2 (1)
〔式中,R1表示選自氫原子、羥基或碳原子數為1~18的飽和或不飽和一價烴基中的一種或二種以上基團,a滿足1.8≦a≦2.2。〕
在上述式(1)中,作為以R1表示的碳原子數為1~18的飽和或不飽和的一價烴基,可列舉例如,甲基、乙基、丙基、己基、辛基、癸基、十二烷基、十四烷基、十六烷基以及十八烷基等的烷基;環戊基、環己基等的環烷基;乙烯基、烯丙基等的烯基;苯基、甲苯基等的芳基;2-苯乙基、2-甲基-2-苯乙基等的芳烷基;3,3,3-三氟丙基、2-(全氟丁基)乙基、2-(全氟辛基)乙基以及對氯苯基等的鹵化烴基。如果將本發明的矽酮組合物作為潤滑脂使用,從作為矽酮潤滑脂組合物所要求的濃稠度的觀點考慮,a優選為在1.8~2.2的範圍,特別優選為在1.9~2.1的範圍。
另外,在本發明中使用的有機聚矽氧烷在25℃下的運動黏度如果低於
10mm2/s,則在製成組合物時容易出現滲油,如果高於100000mm2/s,則在製成組合物時的黏度增高,其不易操作,因此,其黏度需要在25℃下為10mm2/s~100000mm2/s,特別優選為30mm2/s~10000mm2/s。需要說明的是,有機聚矽氧烷的運動黏度為在25℃下用奧斯特瓦爾德黏度計所測定的值。
成分(C)和成分(D)
成分(A)的全部或一部分優選為作為成分(C)的在1個分子中至少含有2個與矽原子鍵合的烯基之有機聚矽氧烷和/或作為成分(D)的在1個分子中至少含有2個與矽原子鍵合的氫原子之有機氫聚矽氧烷。
作為成分(C)的含有與矽原子鍵合的烯基之有機聚矽氧烷為在一分子中平均具有2個以上(通常為2~50個)、優選為2~20個、更優選為2~10個左右的與矽原子鍵合的烯基之有機聚矽氧烷。作為成分(C)的有機聚矽氧烷中的烯基,可列舉例如,乙烯基、烯丙基、丁烯基、戊烯基、己烯基、庚烯基等。其中,尤其優選為乙烯基。成分(C)中的烯基,其既可與分子鏈末端的矽原子鍵合,也可與非分子鏈末端部位的矽原子鍵合,並且可同時與分子鏈末端部位的矽原子和非分子鏈末端部位的矽原子鍵合。
在為成分(C)的有機聚矽氧烷中,作為除烯基以外的與矽原子鍵合的有機基,可列舉例如,甲基、乙基、丙基、丁基、戊基、己基以及庚基等的烷基;苯基、甲苯基、二甲苯基以及萘基等的芳基;苄基、苯乙基等的芳烷基;氯甲基、3-氯丙基以及3,3,3-三氟丙基等的鹵化烷基等。其中,尤其優選為甲基、苯基。
作為這樣的成分(C)的分子結構,雖可列舉,例如直鏈狀、具有部分支
鏈的直鏈狀、環狀、支鏈狀、三維網狀等,但優選為基本上主鏈由二有機矽氧烷單元(D單元)的重複所構成,且分子鏈兩末端用三有機矽氧基封端的直鏈狀二有機聚矽氧烷;或為該直鏈狀的二有機聚矽氧烷和支鏈狀或三維網狀的有機聚矽氧烷的混合物。
為成分(D)的有機氫聚矽氧烷,為在一分子中至少含有2個(通常為2~300個)、優選為2~100個左右的與矽原子鍵合的氫原子(即,SiH基)的有機氫聚矽氧烷,也可為直鏈狀、支鏈狀、環狀或三維網狀結構的樹脂狀物的任意一種。成分(D)中的氫原子,其既可與分子鏈末端的矽原子鍵合,也可與非分子鏈末端部位的矽原子鍵合,並且可同時與分子鏈末端部位的矽原子和非分子鏈末端部位的矽原子鍵合。
在為成分(D)的有機氫聚矽氧烷中,作為氫原子以外的已與矽原子鍵合的有機基團,可列舉例如,為甲基、乙基、丙基、丁基、戊基、己基以及庚基等的烷基;苯基、甲苯基、二甲苯基以及萘基等的芳基;苄基、苯乙基等的芳烷基;氯甲基、3-氯丙基、3,3,3-三氟丙基等的鹵化烷基等。其中,尤其優選為甲基、苯基。
另外,在添加以成分(A)的平均組成式(1)所表示的有機聚矽氧烷的同時,也可配合以下述式(3)表示的具有水解性基的有機聚矽氧烷(K)。該水解性有機聚矽氧烷的含量,相對於成分(A)優選為0~20質量%的量,更優選為0~10質量%的量。
(在式(3)中,R4為碳原子數1~6的烷基、R5彼此獨立地為碳原子數1~18的飽和或不飽和的非取代或取代的一價烴基,c為5~120。)
以上述式(3)所示的有機聚矽氧烷輔助將粉末高填充於矽酮組合物中。另外,還可通過該有機聚矽氧烷對粉末的表面進行疏水化處理。
在上述式(3)中,R4為碳原子數1~6的烷基、例如,可列舉甲基、乙基、丙基等的碳原子數1~6的烷基等,但特別優選為甲基、乙基。R5彼此獨立地為碳原子數1~18、優選為碳原子數1~10的飽和或不飽和的非取代或取代的一價烴基。作為該一價烴基,可列舉例如,甲基、乙基、丙基、己基、辛基、癸基、十二烷基、十四烷基、十六烷基以及十八烷基等烷基;環戊基和環己基等的環烷基;乙烯基和烯丙基等的烯基;苯基和甲苯基等的芳基;2-苯乙基和2-甲基-2-苯乙基等的芳烷基;或用氟、溴、氯等鹵原子、氰基等取代這些基團的一部分或所有的氫原子而成的基團,例如,可列舉3,3,3-三氟丙基、2-(全氟丁基)乙基、2-(全氟辛基)乙基、對氯苯基等。其中,特別優選為甲基。在上述式(3)中,c為5~120的整數,優選為10~90的整數。
成分(B):
成分(B)為,振實密度為3.0g/cm3以上,比表面積為2.0m2/g以下的銀粉。
為成分(B)的銀粉的振實密度如果小於3.0g/cm3,則不能夠提升成分(B)對於組合物的填充率,從而組合物的黏度上升,導致操作性變劣,因此,
以在3.0g/cm3~10.0g/cm3的範圍為宜。優選為4.5g/cm3~10.0g/cm3的範圍,更優選為6.0g/cm3~10.0g/cm3的範圍。
為成分(B)的銀粉的比表面積如果大於2.0m2/g,則不能夠提升對於組合物的填充率,從而組合物的黏度上升,導致操作性變劣,因此,以在0.08m2/g~2.0m2/g的範圍為宜。優選為0.08m2/g~1.0m2/g的範圍,更優選為0.08m2/g~0.5m2/g的範圍。
需要說明的是,本說明書所記載的振實密度為,稱量出100g銀粉,用漏斗柔和地灑落在100ml量筒中後,將該量筒載置於振實密度測定儀上,並以落差距離20mm、60次/分鐘的速度振擊銀粉600次,從而從已壓縮的銀粉的容積而算出的值。
另外,比表面積為稱取約2g銀粉作為樣品,在60±5℃條件下脫氣10分鐘後,使用比表面積自動測定裝置(BET法)測定了總表面積,其後,稱量樣品,用下述公式(4)進行計算而算出的值。
比表面積(m2/g)=總表面積(m2)/樣品量(g) (4)
為成分(B)的銀粉的縱橫比以2.0~150.0為宜,優選為3.0~100.0的範圍,更優選為3.0~50.0的範圍為宜。所謂縱橫比是指粒子的長徑和短徑的比率(長徑/短徑)。作為其測定方法,例如,可以拍攝粒子的電子顯微鏡的照片,從該照片測定粒子的長徑和短徑,從而算出縱橫比。粒子的大小能夠用從上面拍攝的電子顯微鏡的照片進行測定。將該從上面拍攝的電子顯微鏡的照片中的大的直徑作為長徑進行測定。相對於該長徑的短徑作為粒子的厚度。但粒子的厚度不能使用該從上面拍攝的電子顯微鏡
的照片進行測定。測定粒子厚度,在拍攝電子顯微鏡的照片時將放置粒子的試樣台傾斜安裝,從上面拍攝電子顯微鏡的照片,用試樣台的傾斜角度進行補正,從而可以算出粒子的厚度。具體說來,在用電子顯微鏡拍攝多枚擴大數千倍的照片後,任意測定100個粒子的長徑和短徑,然後算出長徑和短徑的比率(長徑/短徑),從而得出了平均值。
為成分(B)的銀粉的粒徑雖無特別地限制,但平均粒徑優選為在0.2~50μm的範圍,更優選為1.0~30μm的範圍為宜。平均粒徑為,用微型藥勺取1~2勺銀粉於100ml燒杯中,再加入約60ml異丙醇,在用超聲波均化器使銀粉分散1分鐘後,可通過激光衍射式粒度分析儀測定的以體積為基準的體積平均粒徑[MV]。需要說明的是,其測定時間為30秒。
用於本發明的銀粉的製備方法並無特別地限定,可列舉例如,電解法、粉碎法、熱處理法、霧化法、還原法等。在此,既可直接使用通過上述方法所得到的銀粉,也可使用通過在滿足上述數值的範圍的條件下進行粉碎而得到的銀粉。在粉碎銀粉時,其裝置並無特別地限定,例如可列舉搗碎機、球磨機、振動磨機、錘磨機、軋輥機、研缽等的公知的裝置。其優選為搗碎機、球磨機、振動磨機、錘磨機。
成分(B)的配合量,相對於成分(A)的100質量份為300~11000質量份。成分(B)的配合量相對於成分(A)的100質量份,若少於300質量份、則所得到的組合物的熱傳導率變劣;成分(B)的配合量相對於成分(A)的100質量份,若多於11000質量份,則組合物的流動性變劣,從而操作性變劣。成分(B)的配合量,相對於成分(A)的100質量份優選為300~5000質量份、更優選為500~5000質量份的範圍。
另外,本發明的熱傳導性矽酮組合物,除成分(B)以外,在不有損於本發明的效果的範圍內,也可兼顧含有無機化合物粉末和/或有機化合物材料。無機化合物粉末其優選為熱傳導率高的無機化合物粉末,可列舉,例如選自鋁粉末、氧化鋅粉末、氧化鈦粉末、氧化鎂粉末、氧化鋁粉末、氫氧化鋁粉末、氮化硼粉末、氮化鋁粉末、金剛石粉末、金粉末、銅粉末、炭粉末、鎳粉末、銦粉末、鎵粉末、金屬矽粉末以及二氧化矽粉末中的1種或2種以上。有機化合物材料也優選為熱傳導率高的有機化合物材料。可列舉,例如選自碳素纖維、石墨烯、石墨、碳納米管以及碳材料中的1種或2種以上。這些無機化合物粉末和有機化合物材料的表面,可根據需要用有機矽烷、有機矽氮烷、有機聚矽氧烷以及有機氟化合物等進行疏水化處理。無機化合物粉末和有機化合物材料的平均粒徑,由於不論是小於0.5μm還是大於100μm,其對於所得到的組合物的填充率都得不到提高,因此,其優選為0.5~100μm範圍,特別優選為1~50μm的範圍。另外,碳素纖維的長度由於不論是小於10μm還是大於500μm,其對於所得到的組合物的填充率都得不到提高,因此,其優選為10~500μm範圍,特別優選為30~300μm的範圍。無機化合物粉末和有機化合物材料的配合量,相對於成分(A)的100質量份若高於3000質量份、則流動性變劣,從而操作性變劣,因此,優選為0~3000質量份、特別優選為0~2000質量份。
固化催化劑:
另外,本發明組合物通過配合固化催化劑能夠形成固化性組合物。本發明組合物如果通過矽氫化反應進行固化的情況下,作為成分(A),添加成分(C)、成分(D)以及鉑族催化劑。相對於成分(C)的烯基1摩爾,優選成分(D)
的配合量為使成分(D)的與矽原子鍵合的氫原子為0.1~10摩爾範圍內的量,進一步優選使成分(D)的與矽原子鍵合的氫原子為0.1~5摩爾範圍內的量,特別優選為使成分(D)的與矽原子鍵合的氫原子為0.1~3.0摩爾範圍內的量。
鉑族催化劑為用於促進本發明組合物的固化的催化劑。可列舉例如,氯鉑酸、氯鉑酸的醇溶液、鉑的鏈烯絡合物、鉑的烯基矽氧烷絡合物以及鉑的羰基絡合物。
在本發明的組合物中,鉑族催化劑的含量為對本發明的組合物的固化所必需的量,即為所謂的催化劑量。具體說來,相對於(A)成分,本成分中的鉑金屬優選為以質量單位計在0~500ppm範圍內的量,特別優選為在0~200ppm範圍內的量。
另外,為了調節本發明組合物的固化速度,從而提高操作性,可含有固化反應抑制劑。該固化反應抑制劑可列舉為,2-甲基-3-丁炔-2-醇、2-苯基-3-丁炔-2-醇、1-乙炔基-1-環己醇等的乙炔類化合物;3-甲基-3-戊烯-1-炔、3,5-二甲基-3-己烯-1-炔等的烯-炔化合物;其它的肼類化合物、膦類化合物、硫醇類化合物等。該固化反應抑制劑的含量並無限定,其優選為相對於(A)成分100質量份在0.0001~1.0質量份的範圍內。
另外,在通過縮合反應固化本發明組合物的情況下,其優選在組合物中作為固化劑含有於一分子中具有至少3個與矽原子鍵合的水解性基團的矽烷或矽氧烷低聚物;以及作為固化催化劑含有縮合反應用催化劑。在此,作為矽原子鍵合水解性基團,可例示烷氧基、烷氧烷氧基、醯氧基、酮肟基、鏈烯氧基、氨基、氨氧基以及醯胺基。另外,除上述的水解性基外,在該矽烷的矽原子上,還可鍵合例如,與上述同樣的直鏈狀烷
基、支鏈狀烷基、環狀烷基、烯基、芳基、芳烷基以及鹵化烷基。作為這樣的矽烷或矽氧烷低聚物,可列舉例如,四乙氧基矽烷、甲基三乙氧基矽烷、乙烯基三乙氧基矽烷、甲基三(甲基乙基酮肟)矽烷、乙烯基三乙醯氧基矽烷、乙基正矽酸鹽、乙烯基三(異丙烯氧基)矽烷。
該矽烷或矽氧烷低聚物的含量,為使本發明的組合物固化所必需的量,具體說來,相對於(A)成分100質量份,優選為在0.01~20質量份的範圍內,特別優選為在0.1~10質量份的範圍內。
另外,縮合反應用催化劑為任意成分,例如,在將具有氨氧基、氨基、酮肟基等的水解性基團的矽烷作為固化劑使用的情況下可不為必需。作為這樣的縮合反應用催化劑,可列舉例如,四丁基鈦酸酯、四異丙基鈦酸酯等的有機鈦酸酯;二異丙氧基雙(乙醯醋酸酯)鈦、二異丙氧基雙(乙醯醋酸酯)鈦等的有機鈦螯合物化合物;三(乙醯丙酮)鋁、三(乙醯乙酸乙酯)鋁等的有機鋁化合物;四(乙醯丙酮)鋯、四丁酸鋯等的有機鋯化合物;二丁基二辛酸錫、二丁基二月桂酸錫、丁基-2-乙基己酸錫等的有機錫化合物;萘酸錫、油酸錫、丁酸錫、萘酸鈷、硬脂酸鋅等的有機羧酸的金屬鹽;己胺、磷酸十二胺等的胺化合物以及其鹽;苄基三乙基乙酸銨等的季銨鹽;醋酸鉀等的鹼金屬的低級脂肪酸鹽;二甲基羥胺、二乙基羥胺等的二烷基羥胺;含有胍基的有機矽化合物。
在本發明的組合物中,該縮合反應用催化劑的含量為任意量。在進行配合時,具體說來,相對於(A)成分100質量份,優選為在0.01~20質量份的範圍內,特別優選為在0.1~10質量份的範圍內。
另外,本發明的組合物如果通過利用有機過氧化物的自由基
反應進行固化,其固化催化劑優選使用有機過氧化物。作為該有機過氧化物,可列舉例如,苯甲醯過氧化物、二(對甲基苯甲醯)過氧化物、二(鄰甲基苯甲醯)過氧化物、二異丙苯過氧化物、2,5-二甲基-2,5-雙(叔丁基)己烷過氧化物、二叔丁基過氧化物、苯甲酸叔丁酯過氧化物以及1,1-二(叔丁基過氧化)環已烷。該有機過氧化物的含量為本發明組合物的固化所需要的量,具體說來,相對於(A)成分100質量份,優選為在0.1~5質量份的範圍內。
成分(E):
進一步,在本發明的組合物中,作為成分(E)也可以配合以下述式(2)表示的有機矽烷。
R2 bSi(OR3)4-b (2)
〔在式(2)中,R2表示選自任選具有取代基的飽和或不飽和的一價烴基、環氧基、丙烯基以及甲基丙烯基中的1種或2種以上的基團、R3表示為一價烴基、b滿足1≦b≦3。〕
作為上述式(2)的R2,可列舉例如,甲基、乙基、丙基、己基、辛基、壬基、癸基、十二烷基以及十四烷基等的烷基;環烷基烯基;丙烯基;環氧基;環戊基和環己基等的環烷基;乙烯基和烯丙基等的烯基;苯基和甲苯基等的芳基;2-苯乙基和2-甲基-2-苯乙基等的芳烷基;3.3.3-三氟丙基、2-(全氟丁基)乙基、2-(全氟辛基)乙基、對氯苯基等的鹵化烴基等。作為一價烴基的取代基,可列舉丙烯醯氧基、甲基丙烯醯氧基等。另外,b為1~3。作為R3,可列舉甲基、乙基、丙基、丁基、戊基以及己基等的碳原子數為1~6的1種或2種以上的烷基。其中,特別優選為甲基和乙基。
作為成分(E)的以式(2)所表示的有機矽烷的具體例子,可例
舉如下。
C10H21Si(OCH3)3
C12H25Si(OCH3)3
C12H25Si(OC2H5)3
C10H21Si(CH3)(OCH3)2
C10H21Si(C6H6)(OCH3)2
C10H21Si(CH3)(OC2H5)2
C10H21Si(CH=CH2)(OCH3)2
C10H21Si(CH2CH2CF3)(OCH3)2、
CH2=C(CH3)COOC8H16Si(OCH3)3
在添加該有機矽烷的情況下,其添加量為相對於(A)成分100質量份,以添加0.1~20質量份的範圍為宜,更優選為添加0.1~10質量份的範圍。
本發明的矽酮組合物的製備方法只要是遵循以往的矽酮組合物的製備方法即可,並無特殊的限制。例如,可通過將上述(A)成分和(B)成分以及根據需要的其他成分用三輥混合機、雙輥混合機、行星式攪拌機(全部為井上製作所(股份有限公司)製造的混合機的註冊商標)、高速攪拌機(瑞穗工業(股份有限公司)製造的混合機的註冊商標)、HIVIS DISPER混合機(PRIMIX Corporation製造混合機的註冊商標)等的混合機進行混合30分鐘~4小時而製備。另外,根據需要,也可在50~150℃範圍的溫度下邊加熱邊進行混合。
本發明的熱傳導性矽酮組合物,其在25℃下所測定的絕對
黏度為10~600Pa.s,優選為50~500Pa.s,更優選為50~400Pa.s。通過將絕對黏度控制在上述範圍內,可提供良好的潤滑脂,且操作性優異。該絕對黏度可通過用上述配合量調整各成分而獲得。上述絕對黏度為使用股份有限公司馬爾科姆公司製造的型號PC-1TL(10rpm)而進行測定所得到的結果。
對以上述的方式所得到的熱傳導性矽酮組合物,在施加0.01MPa以上的壓力的狀態下加熱至80℃以上,從而使本發明的熱傳導性矽酮組合物固化。如此得到的固化物的性狀並無限定,例如,可列舉凝膠狀、低硬度的橡膠狀或高硬度的橡膠狀。
半導體裝置:
本發明的半導體裝置,其特徵在於,本發明的熱傳導性矽酮組合物介於放熱性電子部件的表面和放熱體之間。本發明的熱傳導性矽酮組合物,其優選為以10~200μm的厚度介於上述兩者之間。
圖1示出了代表性構造,但本發明並不被限定於此。本發明的熱傳導性矽酮為於圖1中的3所示者。
在製造本發明的半導體裝置的方法中,其優選為在放熱性電子部件和放熱體之間,在施加0.01MPa以上的壓力的狀態下,將本發明的熱傳導性矽酮組合物加熱至80℃以上的方法。此時,所施加的壓力,優選為0.01MPa以上,特別優選為0.05MPa~100MPa,更優選為0.1MPa~100MPa。加熱溫度需要為80℃以上。優選為90℃~300℃,更優選為100℃~300℃,進一步優選為120℃~300℃。
基於進一步明確本發明的效果的目的,通過實施例和比較例
對本發明進行更為詳細地說明,但本發明並不被這些實施例限制。
以下述的方法進行了有關涉及本發明的效果的試驗。
在25℃下,使用馬爾科姆黏度計(型號PC-1TL)測定了組合物的絕對黏度。
在將實施例1~13和比較例1~8的各種組合物分別澆鑄在6mm厚的模具內,且在施加0.1MPa的壓力的狀態下於170℃加熱後,均在25℃條件下,通過京都電子工業股份有限公司製造的TPS-2500S測定了熱傳導率。有關實施例14、15,在將各組合物澆鑄在6mm厚的模具內,且在23±2℃/50±5%RH條件下放置7天後,通過京都電子工業股份有限公司製造的TPS-2500S,在25℃條件下測定了熱傳導率。
準備了形成組合物的以下各種成分。
成分(A)
A-1:兩末端用二甲基乙烯基甲矽烷基所封端,在25℃下的運動黏度為600mm2/s的二甲基聚矽氧烷
A-2:由((CH3)3SiO1/2)單元和((CH3)2SiO)單元構成、在25℃下的運動黏度為5000mm2/s的有機聚矽氧烷
A-3:以下述式表示的有機氫聚矽氧烷
A-4:兩末端用羥基所封端,在25℃下的運動黏度為5000mm2/s的二甲基聚矽氧烷
A-5(比較例):由包括((CH3)3SiO1/2)單元和((CH3)2SiO)單元構成的運動黏度為200000mm2/s的有機聚矽氧烷
成分(B)
B-1:振實密度為6.2g/cm3、比表面積為0.48m2/g、縱橫比為13的銀粉
B-2:振實密度為6.4g/cm3、比表面積為0.28m2/g、縱橫比為8的銀粉
B-3:振實密度為9.0g/cm3、比表面積為0.16m2/g、縱橫比為30的銀粉
B-4:振實密度為3.0g/cm3、比表面積為2.0m2/g、縱橫比為50的銀粉
B-5(比較例):振實密度為2.3g/cm3、比表面積為2.3m2/g、縱橫比為1的銀粉
B-6(比較例):振實密度為3.3g/cm3、比表面積為2.11m2/g、縱橫比為1的銀粉
B-7(比較例):振實密度為2.8g/cm3、比表面積為1.8m2/g、縱橫比為2的銀粉
成分(K)
K-1:以下述式表示的有機聚矽氧烷
成分(E)
E-1:以下述式表示的有機矽烷
成分(F)固化催化劑
F-1:鉑-二乙烯基四甲基二矽氧烷絡合物的A-1溶液,且作為鉑原子含有1wt%
成分(G)固化反應抑制劑
G-1:1-乙炔基-1-環己醇
成分(H)固化催化劑
H-1:過氧化物(日本油脂股份有限公司製造商品名:PERHEXA®C)
成分(I)固化劑
I-1:乙烯基三(異丙烯氧基)矽烷
成分(J)縮合反應用催化劑
J-1:四甲基胍基丙基三甲氧基矽烷
實施例1~15和比較例1~8
按下述表1~3所示的組成且按如下所示方法進行混合,從而獲得了實施例1~15和比較例1~8的組合物。
即,將成分(A)、成分(K)以及成分(E)放在5公升行星式攪拌機(井上製作所股份有限公司製造)內,再加入成分(B),在25℃條件下混合1.5小時。然後再添加成分(F)、成分(G)、成分(H)、成分(I)或成分(J),並將其混合至均勻。
1‧‧‧基板
2‧‧‧放熱性電子部件(CPU)
3‧‧‧熱傳導性矽酮組合物層
4‧‧‧散熱體(蓋)
Claims (7)
- 一種熱傳導性矽酮組合物,其包含:下述成分(A)和成分(B),其中,成分(A)為以下述平均組成式(1)表示,且在25℃的運動黏度為10~100000mm2/s的有機聚矽氧烷,R1 aSiO(4-a)/2 (1)式中,R1表示選自氫原子、羥基或碳原子數為1~18的飽和或不飽和一價烴基中的一種或二種以上基團,a滿足1.8≦a≦2.2,成分(B)是振實密度為3.0g/cm3以上、比表面積為2.0m2/g以下的銀粉,相對於100質量份的成分(A),其為300~11000質量份。
- 如申請專利範圍第1項之熱傳導性矽酮組合物,其中,成分(B)的銀粉的縱橫比為2.0以上且150.0以下。
- 如申請專利範圍第1或2項之熱傳導性矽酮組合物,其中,部分或全部成分(A)為:成分(C),在1個分子中至少含有2個與矽原子鍵合的烯基之有機聚矽氧烷;和/或成分(D),在1個分子中至少含有2個與矽原子鍵合的氫原子之有機氫聚矽氧烷。
- 如申請專利範圍第1或2項之熱傳導性矽酮組合物,其進一步含有固化催化劑。
- 如申請專利範圍第1或2項之熱傳導性矽酮組合物,其進一步含有作為成分(E)的有機矽烷, 該作為成分(E)的有機矽烷以下述通式(2)所表示,R2 bSi(OR3)4-b (2)式中,R2表示選自任選具有取代基的飽和或不飽和的一價烴基、環氧基、丙烯基以及甲基丙烯基中的1種或2種以上基團、R3表示一價烴基、b滿足1≦b≦3,並且,相對於100質量份的成分(A),含有0~10質量份上述作為成分(E)的有機矽烷。
- 一種半導體裝置,其為具備放熱性電子部件和散熱體的半導體裝置,且申請專利範圍第1或2項之熱傳導性矽酮組合物介於上述放熱性電子部件和散熱體之間。
- 一種半導體裝置的製造方法,該方法具有如下步驟:於放熱性電子部件和散熱體之間,在施加0.01MPa以上的壓力的狀態下將申請專利範圍第1或2項之熱傳導性矽酮組合物加熱至80℃以上。
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