TWI531617B - 一種有機矽樹脂組合物及使用其之預浸料、層壓板、覆銅板以及鋁基板 - Google Patents
一種有機矽樹脂組合物及使用其之預浸料、層壓板、覆銅板以及鋁基板 Download PDFInfo
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Description
本發明涉及一種有機矽樹脂組合物,具體涉及一種高耐熱、無鹵無磷和低熱膨脹係數的有機矽樹脂組合物及使用其之預浸料、層壓板、覆銅板以及鋁基板。
隨著電子訊息技術的飛速發展,PCB越來越向高密度、高可靠、多層化、低成本和自動化連續生產的方向發展,對PCB用基板的耐熱性及可靠性提出了更高的要求。而一直以來以環氧樹脂為主體的FR-4由於耐高溫性差的缺點,在要求耐高溫以及高可靠性電路的應用已經力不從心。
矽樹脂是一種熱固性樹脂,其最突出的性能之一是優異的熱氧化穩定性。這主要是由於矽樹脂是以Si-O-Si為骨架,因此分解溫度高,可在200-250℃下長期使用而不分解或變色,並且配合耐熱填料能耐更高溫度。
同時矽樹脂具有優異的電絕緣性能,由於矽樹脂不含極性基團,故其介電常數及介電損耗角正切值在寬廣的溫度範圍及頻率範圍內變化很小,同時矽樹脂具有優越的電氣絕緣性。由於矽樹脂的可碳化成分較
少,故其耐電弧及耐電暈性能也十分突出。矽樹脂具有突出的耐候性,是任何一種有機樹脂所望塵莫及的。即使在紫外線強烈照射下,矽樹脂也耐泛黃。
目前,為了賦予層壓板阻燃性,使用並用溴系阻燃劑的配方。可是,由於近來對環境問題的呼聲的提高,渴求不使用鹵系化合物的樹脂組合物,進一步進行著代替鹵系阻燃劑的磷化合物研究。磷化合物在燃燒時也可能產生膦等有毒化合物,因此期望開發出即使不使用鹵系化合物和磷化合物也具有阻燃性、且具有低的熱膨脹係數的層壓板。而矽樹脂在不加入鹵素及含磷阻燃劑時其本身也具有非常好的阻燃性能。
鑒於矽樹脂高耐熱、無鹵無磷阻燃、兼備優越的電絕緣性能、突出的耐候性能、同時固化完全的矽樹脂還具有非常低的熱膨脹係數(<2.0%),配合功能性填料其性能會更加優越。因此,用矽樹脂體系製成層壓板正好滿足市場需求一種高耐熱的無鹵無磷(高的玻璃化轉變溫度>200℃,低的Z軸方向的膨脹係數<2.0%)的高性能印製電路用覆銅箔層壓板。
鑒於此,本發明的目的之一在於提供一種有機矽樹脂組合物,其具有高耐熱性、無鹵阻燃以及低膨脹係數等優點。
為了達到上述目的,本發明採用了如下技術手段:
一種有機矽樹脂組合物,所述有機矽樹脂組合物按重量份數包括:縮合型矽樹脂 100份;催化劑 0.0001~2份;助劑 0.001~10份。
所述催化劑的含量例如為0.0005份、0.001份、0.005份、0.01份、0.05份、0.1份、0.5份、0.9份、1.3份、1.7份、1.9份。
所述助劑的含量例如為0.001份、0.005份、0.01份、0.05份、0.1份、0.5份、1份、1.5份、2份、2.5份、3份、3.5份、4份、4.5份、5份、5.5份、6份、6.5份、7份、7.5份、8份、8.5份、9份或9.5份。
在本發明中,所述縮合型矽樹脂主要為甲基矽樹脂、甲基苯基矽樹脂或苯基矽樹脂中的任意一種或者至少兩種的混合物。
在本發明中,所述縮合型矽樹脂為脫水縮合、脫醇縮合或脫氫縮合中的任意一種,其反應結構如下所示:
在本發明中,所述縮合型矽樹脂為R/Si=1.0~1.7(例如1.1、1.2、1.3、1.4、1.5、1.6或1.7)(摩爾比)和Ph/(Me+Ph)=0~1.0(例如0.1、0.2、0.3、0.4、0.5、0.6、0.7、0.8、0.9或1.0)(摩爾比)的甲基矽樹脂、甲基苯基矽樹脂或苯基矽樹脂中的任意一種或者至少兩種的混合物,其中Ph代表苯基基團,Me代表甲基基團,R代表有機官能團-CH3、-Ph、-OCH3、-OCH2CH3、-H或-OH。在縮合型矽樹脂中,R/Si(摩爾比)過小,Ph/Si(摩
爾比)過低,矽樹脂固化後柔軟性差,漆膜變硬,而R/Si(摩爾比)過大,Ph/Si(摩爾比)過高層壓板硬度低,固化慢,熱固性低,故所述縮合型矽樹脂較佳為R/Si=1.2~1.7(摩爾比)且Ph/(Me+Ph)=0.2-0.6(摩爾比)的甲基苯基矽樹脂。
在本發明中,所述催化劑為環烷酸鋅、環烷酸錫、環烷酸鈷、環烷酸鐵、環烷酸鈰、羧酸鋅、羧酸錫、羧酸鈷、羧酸鐵、羧酸鈰、全氟磺酸、氯化磷腈、胺類、季銨堿、辛酸鋅、異辛酸鋅、鈦酸酯或胍類化合物等中的任意一種或者至少兩種的組合。
在本發明中,所述助劑包括矽烷偶聯劑、鈦酸酯偶聯劑或分散劑中的任意一種或者至少兩種的混合物。
在本發明中,所述有機矽樹脂組合物還包括填料。
在本發明中,所述填料包括二氧化矽、氧化鋁、氫氧化鋁、氮化硼、氮化鋁、硫酸鋇、雲母粉、硼酸鋅、二氧化鈦、雲母粉、氮化矽或碳化矽中的任意一種或者至少兩種的混合物。
在本發明中,所述填料的含量為0~60重量份,例如5重量份、10重量份、15重量份、20重量份、25重量份、30重量份、35重量份、40重量份、45重量份、50重量份、55重量份、60重量份。
示例性的一種有機矽樹脂組合物,所述有機矽樹脂組合物按重量份數包括:縮合型矽樹脂 100份
催化劑 0.0001~2.0份
助劑 0.001~10份
填料 0~60份。
理想地,所述有機矽樹脂組合物按重量份數包括:縮合型矽樹脂 100份;催化劑 0.0005~1.5份;助劑 0.005~5份;填料 0~50份。
本發明所述的“包括”,意指其除所述組份外,還可以包括其他組份,這些其他組份賦予所述有機矽樹脂組合物不同的特性。除此之外,本發明所述的“包括”,還可以替換為封閉式的“為”或“由……組成”。
例如,所述有機矽樹脂組合物還可以含有各種添加劑,作為具體例,可以舉出阻燃劑、抗氧劑、熱穩定劑、抗靜電劑、紫外線吸收劑、顏料、著色劑或潤滑劑等。這些各種添加劑可以單獨使用,也可以兩種或者兩種以上混合使用。
本發明的目的之二在於提供一種樹脂膠液,其是將如上所述的有機矽樹脂組合物溶解或分散在溶劑中得到。
作為本發明中的溶劑,沒有特別限定,作為具體例,可以舉出甲醇、乙醇、丁醇等醇類,乙基溶纖劑、丁基溶纖劑、乙二醇-甲醚、卡必醇、丁基卡必醇等醚類,丙酮、丁酮、甲基乙基甲酮、甲基異丁基甲酮、環己酮等酮類,甲苯、二甲苯、均三甲苯等芳香族烴類,乙氧基乙基乙酸酯、醋酸乙酯等酯類,N,N-二甲基甲醯胺、N,N-二甲基乙醯胺、N-甲基-2-吡咯烷酮等含氮類溶劑。上述溶劑可以單獨使用一種,也可以兩種或者兩
種以上混合使用,較佳係甲苯、二甲苯、均三甲苯等芳香族烴類溶劑與丙酮、丁酮、甲基乙基甲酮、甲基異丁基甲酮、環己酮等酮類熔劑混合使用。
本發明的目的之三在於提供一種預浸料,其包括增強材料及通過含浸乾燥後附著在增強材料上的如上所述的有機矽樹脂組合物。
示例性的預浸料的製備方法為:以如上所述的有機矽樹脂組合物重量100份計算,加入甲苯或者二甲苯等有機溶劑製成固含量為50~70%(重量比)的樹脂膠液,由增強材料如玻纖布浸漬該樹脂膠液,然後在120~190℃下烘烤2~15分鐘製備而得。
本發明的目的之四在於提供一種層壓板,所述層壓板含有至少一張如上所述的預浸料。
本發明的目的之五在於提供一種覆銅箔層壓板,所述覆銅箔層壓板包括至少一張疊合的如上所述的預浸料及壓覆在疊合後的預浸料的一側或兩側的銅箔。
本發明目的之六在於提供一種鋁基覆銅板,包括銅箔層和鋁基層,銅箔層和鋁基層間設有絕緣層,所述絕緣層由如上所述的有機矽樹脂組合物,並添加導熱填料製成。
所述導熱填料為三氧化鋁、二氧化矽、碳化矽、氮化硼、氮化鋁或氧化鎂中的任意一種或者至少兩種的混合物。
與已有技術相比,本發明具有如下之功效:(1)本發明通過將矽樹脂、催化劑以及助劑複配,得到的有機矽樹脂組合物具有高耐熱(T300>60min)、無鹵無磷、低熱膨脹係數(其熱膨脹係數(CTE)小於1.0%)及較高的剝離強度的特點;
(2)本發明的有機矽樹脂組合物具有無鹵無磷、低煙、低毒、自熄和環保等優點,為層壓板及覆銅板在阻燃領域提供了新思路和新方法;(3)本發明的製備過程所有的工藝及設備為普通FR-4通用型,完全可以利用現有的生產設備來實施本發明,非常有利於產品的產業化。
下面通過具體實施方式來進一步說明本發明的技術手段。
實施例1
稱取R/Si=1.1(摩爾比),Ph/(Ph+Me)=0(摩爾比)的甲基矽樹脂100.0份,溶於60.0份甲苯溶劑中,攪拌使其完全溶解。待矽樹脂溶解完全後,加入異辛酸鋅0.0001份,矽烷偶聯劑γ-(2,3-環氧丙氧基)丙基三甲氧基矽烷(美國,道康寧公司提供)0.001份,攪拌混合均勻得到膠液。選取平整光潔、厚度為0.1mm的E-玻纖布,均勻塗覆上述膠液,在烘箱中用170℃烘烤5min得半固化片。將8張上述半固化片疊加,上下附上35μm的銅箔,置於真空熱壓機中在3MPa壓力和220℃溫度下壓製3h得到層壓板。
實施例2
稱取R/Si=1.4(摩爾比),Ph/(Ph+Me)=0.5(摩爾比)的甲基苯基矽樹脂100.0份溶於70.0份甲苯溶劑中,攪拌使其完全溶解。待矽樹脂溶解完全後,加入矽微粉23.0份,乙醯丙酮鈷0.1份,矽烷偶聯劑γ-甲基丙烯醯氧基丙基三甲氧基矽烷偶聯劑1.5份(湖北武大有機矽新材料股份有限公司提供),攪拌
均勻得膠液。
除了使用該樹脂膠液外,與實施例1同樣進行,獲得預浸料和厚度為1.0mm的雙面覆銅層壓板。
實施例3
稱取R/Si=1.7(摩爾比),Ph/(Ph+Me)=1.0(摩爾比)的苯基矽樹脂100.0份溶於100.0份甲苯溶劑中,攪拌使其完全溶解。待矽樹脂溶解完全後,加入氧化鋁50份,鈦酸酯1.5份,矽烷偶聯劑γ-甲基丙烯醯氧基丙基三甲氧基矽烷8.7份(湖北武大有機矽新材料股份有限公司提供),攪拌均勻得膠液。
除了使用該樹脂膠液外,與實施例1同樣進行,獲得預浸料和厚度為1.0mm的雙面覆銅層壓板。
實施例4
稱取R/Si=1.1(摩爾比),Ph/(Ph+Me)=0(摩爾比)的甲基矽樹脂60.0份和R/Si=1.7(摩爾比),Ph/(Ph+Me)=0.9(摩爾比)的甲基苯基矽樹脂40.0份,溶於85.0份甲苯溶劑中,攪拌使其完全溶解。待矽樹脂溶解完全後,加入氧化鋁25.0份,矽微粉10.0份,乙醯丙酮鈷0.08份,矽烷偶聯劑γ-甲基丙烯醯氧基丙基三甲氧基矽烷偶聯劑1.5份(湖北武大有機矽新材料股份有限公司提供),攪拌均勻得膠液。
除了使用該樹脂膠液外,與實施例1同樣進行,獲得預浸料和厚度為1.0mm的雙面覆銅層壓板。
對比例1
稱取甲基苯基乙烯基矽樹脂100份(乙烯基含量為1.0%),溶入70份溶劑中,溶解均勻後加入3.1份甲基苯基含氫矽油(含氫量為1.2%),高速攪拌
均勻後稱取0.001份己炔醇,攪拌30min後加入0.01份鉑-甲基苯基乙烯基絡合物,繼續攪拌30min後加入矽烷偶聯劑γ-甲基丙烯醯氧基丙基三甲氧基矽烷偶聯劑1.5份(湖北武大有機矽新材料股份有限公司提供),23份矽微粉,室溫下攪拌1h,乳化20min,得矽樹脂膠液。
除了使用該樹脂膠液外,與實施例1同樣進行,獲得預浸料和厚度為1.0mm的雙面覆銅層壓板。
對比例2
稱取R/Si=1.4(摩爾比),Ph/(Ph+Me)=0.5(摩爾比)的甲基苯基矽樹脂100.0份溶於70.0份甲苯溶劑中,攪拌使其完全溶解。待矽樹脂溶解完全後,加入矽微粉70.0份,乙醯丙酮鈷0.1份,矽烷偶聯劑γ-甲基丙烯醯氧基丙基三甲氧基矽烷偶聯劑1.5份(湖北武大有機矽新材料股份有限公司提供),攪拌均勻得膠液。
除了使用該樹脂膠液外,與實施例1同樣進行,獲得預浸料和厚度為1.0mm的雙面覆銅層壓板。
對比例3
稱取R/Si=1.7(摩爾比),Ph/(Ph+Me)=1.0(摩爾比)的苯基矽樹脂100.0份溶於100.0份甲苯溶劑中,攪拌使其完全溶解。待矽樹脂溶解完全後,加入氧化鋁50份,鈦酸酯1.5份,矽烷偶聯劑γ-甲基丙烯醯氧基丙基三甲氧基矽烷12.0份(湖北武大有機矽新材料股份有限公司提供),攪拌均勻得膠液。
除了使用該樹脂膠液外,與實施例1同樣進行,獲得預浸料和厚度為1.0mm的雙面覆銅層壓板。
對比例4
稱取R/Si=1.9(摩爾比),Ph/(Ph+Me)=1.0(摩爾比)的苯基矽樹脂100.0份溶於100.0份甲苯溶劑中,攪拌使其完全溶解。待矽樹脂溶解完全後,加入氧化鋁50份,鈦酸酯1.5份,矽烷偶聯劑γ-甲基丙烯醯氧基丙基三甲氧基矽烷8.7份(湖北武大有機矽新材料股份有限公司提供),攪拌均勻得膠液。
除了使用該樹脂膠液外,與實施例1同樣進行,獲得預浸料和厚度為1.0mm的雙面覆銅層壓板。
效果確認:
(1)Z-膨脹係數(CTE)的測試(熱機械分析方法)
測試方法:使用IPC-TM-650 2.4.24,測試數據見下表。
(2)熱分層時間(T300)(熱機械分析方法)
測試方法:使用IPC-TM-650 2.4.24.1,測試數據見下表。
(3)燃燒等級
測試方法:參照美國UL94標準,測試數據見下表。
(4)剝離強度測試
測試方法:使用IPC-TM-650 2.4.8方法進行測試,測試數據請見下表。
物性分析:
從上表的數據可以看出,實施例1~4同時具有非常低的熱膨脹係數,高的熱分層時間,無鹵無磷阻燃及具有較好的剝離強度,滿足覆銅箔層壓板的需求。而對比例1與實施例2相比,由於矽樹脂為甲基苯基乙烯基矽樹脂,使用加成型固化方法,固化後膨脹係數大,剝離強度低,且阻燃效果也不突出;而對比例2與實施例2相比,填料含量超出範圍,導致與銅箔的剝離強度降低,熱分層時間減少;對比例3與實施例3相比,助劑的使用量不在保護範圍,由於助劑多為小分子,加入量過多使得層壓板在高溫下小分子放出來較多,使得熱膨脹係數增大,同時分層時間縮短;對比例4與實施例3相比,R/Si值超出範圍,R/Si越大,樹脂交聯密度越低,越傾向於熱塑性樹脂,使得熱膨脹係數上升,高溫下穩定性下降,熱分層時間降低。
申請人聲明,本發明通過上述實施例來說明本發明的詳細方法,但本發明並不局限於上述詳細方法,即不意味著本發明必須依賴上述詳細方法才能實施。所屬技術領域的技術人員應該明瞭,對本發明的任何改進,對本發明產品各原料的等效替換及輔助成分的添加、具體方式的選擇等,均落在本發明的保護範圍和公開範圍之內。
Claims (12)
- 一種有機矽樹脂組合物,其特徵係所述有機矽樹脂組合物按重量份數包括:縮合型矽樹脂 100份;催化劑 0.0001~2份;助劑 0.001~10份;填料 0~60重量份;其中所述縮合型矽樹脂係R/Si=1.0~1.7(摩爾比)和Ph/(Me+Ph)=0~1.0(摩爾比)的甲基矽樹脂、甲基苯基矽樹脂或苯基矽樹脂中的任意一種或者至少兩種的混合物,其中Ph代表苯基基團,Me代表甲基基團,R代表有機官能團-CH3、-Ph、-OCH3、-OCH2CH3、-H或-OH。
- 如申請專利範圍第1項所述之有機矽樹脂組合物,其中,所述縮合型矽樹脂係R/Si=1.2~1.7(摩爾比)且Ph/(Me+Ph)=0.2-0.6(摩爾比)的甲基苯基矽樹脂。
- 如申請專利範圍第1項所述之有機矽樹脂組合物,其中,所述催化劑係環烷酸鋅、環烷酸錫、環烷酸鈷、環烷酸鐵、環烷酸鈰、羧酸鋅、羧酸錫、羧酸鈷、羧酸鐵、羧酸鈰、全氟磺酸、氯化磷腈、胺類、季銨堿、辛酸鋅、異辛酸鋅、鈦酸酯或胍類化合物等中的 任意一種或者至少兩種的組合。
- 如申請專利範圍第1項所述之有機矽樹脂組合物,其中,所述助劑包括矽烷偶聯劑、鈦酸酯偶聯劑或分散劑中的任意一種或者至少兩種的混合物。
- 如申請專利範圍第1至4項中任一項所述之有機矽樹脂組合物,其中,所述填料係包括二氧化矽、氧化鋁、氫氧化鋁、氮化硼、氮化鋁、硫酸鋇、雲母粉、硼酸鋅、二氧化鈦、滑石粉、氮化矽或碳化矽中的任意一種或者至少兩種的混合物。
- 如申請專利範圍第1-4項中任一項所述之有機矽樹脂組合物,其中,所述有機矽樹脂組合物按重量份數包括:縮合型矽樹脂 100份;催化劑 0.0005~1.5份;助劑 0.005~5份填料 0~50份。
- 一種樹脂膠液,其特徵為其係將如申請專利範圍第1-6項中任一項所述之有機矽樹脂組合物溶解或分散在溶劑中得到。
- 一種預浸料,其特徵為其係包括增強材料及通過含浸乾燥後附著在增強材料上的如申請專利範圍第1-6項中任一項所述之有機矽樹脂組合物。
- 一種層壓板,其特徵為所述層壓板係含有至少一張如申請專利範圍第8項所述之預浸料。
- 一種覆銅箔層壓板,其特徵為所述覆銅箔層壓板係包括至少一張疊合的如申請專利範圍第8項所述之預浸料及壓覆在疊合後的預浸料的一側或兩側的銅箔。
- 一種鋁基覆銅板,包括銅箔層和鋁基層,銅箔層和鋁基層間塗有絕緣層,其特徵為所述絕緣層係由如申請專利範圍第1-6項中任一項所述之矽樹脂組合物,並添加導熱填料製成。
- 如申請專利範圍第11項所述之鋁基覆銅板的製造方法,其中,其係包括如下步驟:(1)按組分比例配製矽樹脂組合物,並添加導熱填料,攪拌均勻,製成導熱膠液;(2)將配製好的導熱膠液塗覆於銅箔上,在烘箱中用170℃烘烤5min得半固化塗覆銅箔;(3)將鋁板與(2)所述的塗覆銅箔疊合在一起,置於真空狀態下分步升溫升壓製得鋁基覆銅板。
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