TW201623454A - 無鹵無磷矽樹脂組合物以及使用它的預浸料、層壓板和印製電路板 - Google Patents

無鹵無磷矽樹脂組合物以及使用它的預浸料、層壓板和印製電路板 Download PDF

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TW201623454A
TW201623454A TW104111512A TW104111512A TW201623454A TW 201623454 A TW201623454 A TW 201623454A TW 104111512 A TW104111512 A TW 104111512A TW 104111512 A TW104111512 A TW 104111512A TW 201623454 A TW201623454 A TW 201623454A
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parts
resin
resin composition
vinyl
organic
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TW104111512A
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TWI585160B (zh
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xiao-sheng Su
Su-Wen Ye
guo-fang Tang
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Shengyi Technology Guangdong Co Ltd
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Abstract

本發明提供了一種無鹵無磷矽樹脂組合物以及使用它的預浸料、層壓板和印製電路板。以固體重量計，所述矽樹脂組合物包括：有機矽樹脂50~90份，端乙烯基矽油20~80份，增粘劑0.1~5份，填料0~60份，催化劑0.0001~0.5份，抑制劑0.00001~0.1份，其中交聯劑中的Si-H與有機矽樹脂中的Si-Vi摩爾比為1.0~1.7。本發明的樹脂組合物的樹脂主體為熱固性矽樹脂，以此製備的層壓板具有優異的耐熱性和阻燃性，同時具有非常低的介電常數（Dk）和介電損耗(Df)。

Description

無鹵無磷矽樹脂組合物以及使用它的預浸料、層壓板和印製電路板
本發明涉及一種無鹵無磷、低介電熱固性樹脂組合物及由其制得的預浸料、層壓板、覆銅板以及印製電路板
隨著資訊產業的高速發展，現代高頻通信的發展對材料的電性能提出了越來越高的要求，在高頻電路上應用的覆銅板必須具備良好的介電性能，要求板材具有更低的介電常數和較小的介電損耗。通常情況下，線路板導線內的信號傳播速度V＝K*C/ε2，其中C為光速，ε為介電常數，K是一個常數，由此可以看出，ε越小，則傳播速度越快。另外，信號傳播中的傳輸損失與導體內損失及介質內損失有關，導體內損失與ε平方根成正比，介質內損失與ε平方根及損耗角正切有關。因此使用低介電常數和低介電損耗的基板材料，有助於信號的高速傳播和減小信號損失。
而目前普通的FR-4在1GHz條件下的介電常數（Dk）在4.3~4.8，其介電損耗（Df）在0.02~0.025，無法滿足高頻信號傳輸的速度及信號傳輸的完整性。
由於矽樹脂大分子主鏈的外面具有一層非極性的有機基團，以及大分子鏈具有分子對稱性，所以具有優良的電氣絕緣性能，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，同時在在200℃以下仍可維持恒定，可作為在350℃下使用的超高頻絕緣材料。在矽樹脂的多種固化方式中，鉑催化-CH=CH2與-Si-H反應條件溫和，在固化時無小分子放出，不會產生氣泡，具有非常優越的電性能。
鑒於此，本發明的目的在於提供一種無鹵無磷、低介電的矽樹脂組合物以及使用它的預浸料、層壓板、覆銅板以及印製電路板，其可以在保持良好的阻燃性能下同時具有優良的介電性能。
為了達到上述目的，本發明採用了如下技術方案：
一種矽樹脂組合物，以固體重量份計，所述矽樹脂組合物包括：
有機矽樹脂：50~90份；
端乙烯基矽油：20~80份；
催化劑：0.0001~0.5份；
抑制劑：0.00001~0.1份。
優選地，所述矽樹脂組合物還包括交聯劑，交聯劑與有機矽樹脂交聯。
優選地，交聯劑為甲基含氫矽油、甲基苯基含氫矽油、甲基含氫矽樹脂或甲基苯基含氫矽樹脂中的任意一種或者至少兩種的混合物；所述交聯劑中的Si-H(矽氫)與有機矽樹脂中的Si-Vi(矽乙烯基)摩爾比為1.0~1.7，例如1.05、1.1、1.15、1.2、1.25、1.3、1.35、1.4、1.45、1.5、1.55、1.6或1.65。Si-H（矽氫）與Si-Vi（矽乙烯基）摩爾比理想計算為1.0，但由於交聯劑中的Si-H（矽氫）在高溫反應時自身易產生氫氣脫去Si-H，因而在實際應用時Si-H與Si-Vi摩爾比會高一些，但Si-H與Si-Vi摩爾比不能太高，否則產生氫氣會增多，導致固化後層壓板出現孔洞，因而與Si-H與Si-Vi摩爾比在1.0-1.7合適，且優選為1.2~1.6。
優選地，所述交聯劑的含氫品質分數為0.5~1.6%，例如0.6%、0.7%、0.8%、0.9%、1.0%、1.1%、1.2%、1.3%、1.4%或1.5%，優選0.7~1.3%。
在本發明中，交聯劑的量是通過Si-H（矽氫）/Si-Vi（矽乙烯基）摩爾比與有機矽樹脂的乙烯基含量和品質份數進行計算而得。
在本發明中，所述有機矽樹脂的含量例如為53份、56份、59份、63份、67份、71份、75份、79份、83份、86份或89份。
所述端乙烯基矽油的含量例如為24份、28份、32份、36份、40份、44份、48份、52份、56份、60份、64份、68份、72份或76份。
所述催化劑的含量例如為0.0001份、0.0005份、0.001份、0.005份、0.01份、0.05份、0.1份、0.3份或0.5份。
所述抑制劑的含量例如為0.00003份、0.00005份、0.0001份、0.0005份、0.001份、0.005份、0.01份、0.05份或0.09份。
本發明的矽樹脂組合物的固化方式為：和在鉑催化劑的催化作用下，反應生成交聯網狀結構而得，具體反應式如下：
在本發明中，所述有機矽樹脂為熱固性矽樹脂，包括甲基乙烯基矽樹脂或/和甲基苯基乙烯基矽樹脂，這兩種樹脂可通過交聯劑進行加成反應，反應時無小分子等副產物產生，電性能優越。同時，乙烯基品質分數越低，樹脂越傾向於矽橡膠，固化後硬度越低，影響層壓板使用，而乙烯基品質分數越高，樹脂熱固性越好，但樹脂越脆，力學性能降低，因而有機矽樹脂中的乙烯基品質分數為0.5~8.0%，例如1%、1.5%、2%、2.5%、3%、3.5%、4%、4.5%、5%、5.5%、6%、6.5%、7%或7.5%，優選乙烯基品質分數為1.0~6.0%。
在本發明中，所述端乙烯基矽油為樹脂組合物的活性稀釋劑，包括甲基端乙烯基矽油或/和甲基苯基端乙烯基矽油，端乙烯基矽油本身會參加反應，當端乙烯基矽油粘度越低時，稀釋和溶解矽樹脂效果越好，但固化後易發脆，而端乙烯基矽油粘度越高，可以對矽樹脂起到增韌的效果，同時對矽樹脂的稀釋作用降低，因而其粘度為200~10000mPa.s，優選粘度為500~8000 mPa.s。
在本發明中，所述矽樹脂組合物還包括催化劑，所述催化劑為鉑催化劑，優選為鉑-甲基乙烯基絡合物或/和鉑-甲基苯基乙烯基絡合物，優選催化劑的粘度為100m~10000mPa.s。
在本發明中，所述抑制劑為含炔基化合物、含多乙烯基化合物、含N有機化合物、含P有機化合物或含S有機化合物中的任意一種或者至少兩種的混合物。
在本發明中，所述矽樹脂組合物還包括增粘劑。
在本發明中，所述增粘劑為含有-OCH3、-OCH2CH3、、、或-CH=CH2 中的任意一種或者至少兩種的組合的有機化合物。該類有機化合物在樹脂組合物中主要是提高與銅箔的剝離強度。
所述增粘劑的含量為0.1~5份，例如為0.5份、1份、1.5份、2份、2.5份、3份、3.5份、4份或4.5份。
在本發明中，所述矽樹脂組合物還包括填料0~60份；所述填料為氧化鋁、氫氧化鋁、二氧化矽、氧化鋅、雲母粉、氮化鋁、氮化硼、碳化矽、硫酸鋇、二氧化鈦、硼酸鋅、氣相二氧化矽、滑石粉、氫氧化鎂或勃母石中的任意一種或者至少兩種的混合物。
所述填料的含量例如為5份、14份、18份、22份、26份、30份、34份、38份、42份、46份、50份、54份或58份。
在本發明，所述填料的粒徑沒有特別限定，但優選10μm以下，更優選為5μm以下。
優選地，所述矽樹脂組合物按重量分數包括：
有機矽樹脂：50~90份；
端乙烯基矽油：20~80份；
增粘劑：0.1~5份；
填料： 0~60份 ；
催化劑：0.0001~0.5份；
抑制劑：0.00001~0.1份；
其中，有機矽樹脂的交聯劑為甲基含氫矽油、甲基苯基含氫矽油、甲基含氫矽樹脂或甲基苯基含氫矽樹脂中的任意一種或者至少兩種的混合物；交聯劑中的Si-H與有機矽樹脂中的Si-Vi摩爾比為1.0~1.7。
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，可以舉出甲苯、二甲苯、正己烷、環己烷或異丙醇等。
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矽樹脂組合物。
示例中的預浸料的製備方法為：
將有機矽樹脂溶於端乙烯基矽油中，配以交聯劑、抑制劑、催化劑、增粘劑、填料以及任選地助劑而成有機矽樹脂組合物浸漬于增強材料如片狀玻纖纖維基材中，在一定的壓力和溫度下直接壓制而成。
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，其通過將至少一張如上所述的預浸料加熱加壓成型得到。
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。
與已有技術相比，本發明具有如下有益效果：
本發明以有機矽樹脂作為主體樹脂，配以合適量的端乙烯基矽油、交聯劑、增粘劑、填料、催化劑、抑制劑以及任選地助劑得到矽樹脂組合物，以該矽樹脂組合物製備的層壓板具有優異的力學性能、耐熱性和阻燃性，在無鹵無磷的情況下達到V-0阻燃，同時具有非常低的介電常數（Dk）和介電損耗(Df)。
下面通過具體實施方式來進一步說明本發明的技術方案。
實施例1
按照Si-H（矽氫）/Si-Vi(矽乙烯基)=1.6(摩爾比)設計配方，稱取甲基苯基乙烯基矽樹脂90份（乙烯基品質分數為1.0%），溶入30份粘度為500mPa.s的甲基苯基端乙烯基矽油中，溶解均勻後加入4.10份甲基苯基含氫矽油（含氫品質分數為1.3%）和0.1份增粘劑，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15份3.5μm粒徑的矽微粉，室溫下攪拌1h，乳化20min，得矽樹脂組合物。
用此矽樹脂組合物浸漬重量為104g/cm2 的玻璃纖維布，並直接將8片預浸料重疊，在該層疊體上下表面配置35μ的電解銅箔，在200℃、表面壓力10kgf/cm2 、30mmHg以下的真空下進行180min的加壓成型，獲得厚度為1.0mm的雙面覆銅層壓板。
實施例2
按照Si-H/Si-Vi=1.2(摩爾比)設計配方，稱取甲基乙烯基矽樹脂70份（乙烯基品質分數為3.5%），溶入50份粘度為3000mPa.s的甲基端乙烯基矽油中，溶解均勻後加入10.9份甲基含氫矽油（含氫品質分數為1.0%）和0.5份增粘劑，高速攪拌均勻後稱取0.005份己炔醇，攪拌30min後加入0.00005份鉑-甲基乙烯基絡合物，繼續攪拌30min後加入10份5μm粒徑的矽微粉和15份3.5μm氧化鋁，室溫下攪拌1h，乳化20min，得矽樹脂組合物。
除了使用該樹脂組合物外，與實施例1同樣進行，獲得厚度為1.0mm的雙面覆銅層壓板。
實施例3
按照Si-H/Si-Vi=1.5(摩爾比)設計配方，稱取甲基乙烯基矽樹脂50份（乙烯基品質分數為7.5%），溶入70份粘度為8000mPa.s的甲基端乙烯基矽油中，溶解均勻後加入26.1份甲基含氫矽油（含氫品質分數為0.8%）和0.1份增粘劑，高速攪拌均勻後稱取0.1份四甲基四乙烯基環四矽氧烷（D4vi），攪拌30min後加入0.0001份鉑-甲基乙烯基絡合物，繼續攪拌30min後加入50份5μm粒徑的矽微粉，室溫下攪拌1h，乳化20min，得矽樹脂組合物。
除了使用該樹脂膠液外，與實施例1同樣進行，獲得厚度為1.0mm的雙面覆銅層壓板。
比較例1
按照Si-H/Si-Vi=1.9(摩爾比)設計配方，替換實施例1中的Si-H（矽氫）/Si-Vi(矽乙烯基)=1.6(摩爾比)，其餘不變。
按照Si-H（矽氫）/Si-Vi(矽乙烯基)=1.9(摩爾比)設計配方，稱取甲基苯基乙烯基矽樹脂90份（乙烯基品質分數為1.0%），溶入30份粘度為500mPa.s的甲基苯基端乙烯基矽油中，溶解均勻後加入4.87份甲基苯基含氫矽油（含氫品質分數為1.3%）和0.1份增粘劑，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15份3.5μm粒徑的矽微粉，室溫下攪拌1h，乳化20min，得矽樹脂組合物。
除了使用該樹脂組合物外，與實施例1同樣進行，獲得厚度為1.0mm的雙面覆銅層壓板。
比較例2
用甲基乙烯基矽樹脂90份（乙烯基含量為10.0%）替代實施例1中的甲基苯基乙烯基矽樹脂90份（乙烯基含量為1.0%），其餘不變。
按照Si-H/Si-Vi=1.2(摩爾比)設計配方，稱取甲基乙烯基矽樹脂70份（乙烯基品質分數為10.0%），溶入50份粘度為3000mPa.s的甲基端乙烯基矽油中，溶解均勻後加入31.1份甲基含氫矽油（含氫品質分數為1.0%）和0.5份增粘劑，高速攪拌均勻後稱取0.00005份己炔醇，攪拌30min後加入0.005份鉑-甲基乙烯基絡合物，繼續攪拌30min後加入10份5μm粒徑的矽微粉和15份3.5μm氧化鋁，室溫下攪拌1h，乳化20min，得矽樹脂組合物。
除了使用該樹脂組合物外，與實施例1同樣進行，獲得厚度為1.0mm的雙面覆銅層壓板。
比較例3
用1.5份甲基含氫矽油（含氫量為0.8%）替代實施例3中的15.3份甲基含氫矽油（含氫量為0.8%），其餘不變。
按照Si-H/Si-Vi=0.7(摩爾比)設計配方，稱取甲基乙烯基矽樹脂50份（乙烯基品質分數為7.5%），溶入70份粘度為8000mPa.s的甲基端乙烯基矽油中，溶解均勻後加入12.2份甲基含氫矽油（含氫品質分數為0.8%）和0.1份增粘劑，高速攪拌均勻後稱取0.1份四甲基四乙烯基環四矽氧烷（D4vi），攪拌30min後加入0.0001份鉑-甲基乙烯基絡合物，繼續攪拌30min後加入50份5μm粒徑的矽微粉，室溫下攪拌1h，乳化20min，得矽樹脂組合物。
除了使用該樹脂膠液外，與實施例1同樣進行，獲得厚度為1.0mm的雙面覆銅層壓板。
比較例4
稱取甲基苯基矽樹脂70.0份溶於50.0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0.005份乙醯丙酮鋁和0.5份增粘劑，繼續攪拌30min後加入10份5μm粒徑的矽微粉和15份3.5μm氧化鋁，室溫下攪拌1h，乳化20min，得矽樹脂組合物。用此矽樹脂組合物浸漬重量為104g/cm2的玻璃纖維布，在烘箱中用170℃烘烤5min得半固化片。
除了使用該半固化片，與實施例1同樣進行，獲得厚度為1.0mm的雙面覆銅層壓板。
確認效果測試：
1、介電性能測試
平板電容測試方法參照IPC TM650 2.5.5.9進行，SPDR測試方法參照IPC TM650 2.5.5.13進行。
2、燃燒性測試
依據UV94法測試。
3、彎曲強度測試
參照IPC-TM-650 2.4.4(12/94B版)進行。
4、表觀情況
外觀檢測：用肉眼觀察覆銅箔層壓板表面；
內部檢測：進行切片製作，並用掃描電鏡進行觀察，測試結果如下：
表1 覆銅箔層壓板測試結果
物性分析：從測試結果看，實施例1-3具有非常低的Dk/Df，有助於信號的高速傳播和減少信號損失，同時達到無鹵無磷阻燃，力學性能也較優越。而比較例1與實施例1相比，Si-H/Si-Vi=1.9(摩爾比)，含氫矽油的量過量，在高溫下釋放氫氣，導致層壓板內部有少量氣泡和孔洞；比較例2與實施例2相比，乙烯基含量為10.0份，通過計算含氫矽油的量為31.1份，乙烯基含量過大導致樹脂固化後質脆，力學性能降低；而比較例3與實施例3相比，Si-H/Si-Vi=0.7(摩爾比)，含氫矽油的量無法使乙烯基矽樹脂固化完全，導致層壓板硬度低，力學性能差，且銅箔表面易起皺紋；比較例4為縮合型矽樹脂，由於固化時會放出小分子，電性能較乙烯基矽樹脂差。
從實施例4和比較例5測試結果可看出，由於加成型矽樹脂反應時無小分子放出具有更好的耐電壓性能且具有更好的耐浸焊性能，並且加成型矽樹脂使用活性稀釋劑對環境無污染，同時對矽樹脂能起到良好的增韌效果，樹脂層不掉粉不開裂。
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 (9)

  1. 一種矽樹脂組合物，其特徵在於，以固體重量份計，所述矽樹脂組合物包括： 　　有機矽樹脂：50~90份； 　　端乙烯基矽油：0~80份； 　　催化劑：0.0001~0.5份； 　　抑制劑：0.00001~0.1份。
  2. 如申請專利範圍第1項所述的矽樹脂組合物，其特徵在於，所述有機矽樹脂為甲基乙烯基矽樹脂或/和甲基苯基乙烯基矽樹脂，且有機矽樹脂中的乙烯基品質分數為0.5~8.0%，優選乙烯基品質分數為1.0~6.0%； 優選地，所述矽樹脂組合物還包括交聯劑； 優選地，交聯劑為甲基含氫矽油、甲基苯基含氫矽油、甲基含氫矽樹脂或 甲基苯基含氫矽樹脂中的任意一種或者至少兩種的混合物； 　　優選地，交聯劑中的Si-H與有機矽樹脂中的Si-Vi摩爾比為1.0~1.7； 　　優選地，交聯劑中的Si-H與有機矽樹脂中的Si-Vi摩爾比為1.2~1.6； 　　優選地，交聯劑的含氫品質分數為0.5~1.6%，優選0.7~1.3%； 　　優選地，所述端乙烯基矽油為甲基端乙烯基矽油或/和甲基苯基端乙烯基矽油，其粘度為200~10000mPa.s，優選粘度為500~8000 mPa.s。
  3. 如申請專利範圍第1或2項所述的矽樹脂組合物，其特徵在於，所述矽樹脂組合物還包括增粘劑0.1~5份； 優選地，所述增粘劑為含有-OCH3 、-OCH2 CH3 、、、或 -CH=CH2 中的任意一種或者至少兩種的組合的有機化合物； 優選地，所述矽樹脂組合物還包括填料0~60份； 優選地，所述填料為氧化鋁、氫氧化鋁、二氧化矽、氧化鋅、雲母粉、氮化 鋁、氮化硼、碳化矽、硫酸鋇、二氧化鈦、硼酸鋅、氣相二氧化矽、滑石粉、氫氧化鎂或勃母石中的任意一種或者至少兩種的混合物； 優選地，所述填料的粒徑為10μm以下，優選為5μm以下； 優選地，所述催化劑為鉑催化劑，優選為鉑-甲基乙烯基絡合物或/和鉑-甲基 苯基乙烯基絡合物； 優選地，所述催化劑的粘度為100~10000mPa.s； 優選地，所述抑制劑為含炔基化合物、含多乙烯基化合物、含N有機化合物、 含P有機化合物或含S有機化合物中的任意一種或者至少兩種的混合物。
  4. 如申請專利範圍第1至3項中任一項所述的矽樹脂組合物，其特徵在於，所述矽樹脂組合物按重量分數包括： 　　有機矽樹脂：50~90份； 　　端乙烯基矽油：20~80份； 　　增粘劑：0.1~5份； 　　填料：0~60份 ； 　　催化劑 ：0.0001~0.5份； 　　抑制劑：0.00001~0.1份； 　　其中，有機矽樹脂的交聯劑為甲基含氫矽油、甲基苯基含氫矽油、甲基含氫矽樹脂或甲基苯基含氫矽樹脂中的任意一種或者至少兩種的混合物；交聯劑中的Si-H與有機矽樹脂中的Si-Vi摩爾比為1.0~1.7。
  5. 一種樹脂膠液，其特徵在於，其是將如申請專利範圍第1至4項中任一項所述的矽樹脂組合物溶解或分散在溶劑中得到。
  6. 一種預浸料，其特徵在於，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申請專利範圍第1至4項中任一項所述的矽樹脂組合物。
  7. 一種層壓板，其特徵在於，所述層壓板含有至少一張所述的預浸料。
  8. 一種覆銅箔層壓板，其特徵在於，所述覆銅箔層壓板包括至少一張疊合的如申請專利範圍第6項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。
  9. 一種印製電路板，其特徵在於，所述印製電路板包括至少一張如申請專利範圍第6項所述的預浸料。
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