CN108219434A - 一种热固性树脂组合物、预浸料以及层压板 - Google Patents
一种热固性树脂组合物、预浸料以及层压板 Download PDFInfo
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- CN108219434A CN108219434A CN201711440192.8A CN201711440192A CN108219434A CN 108219434 A CN108219434 A CN 108219434A CN 201711440192 A CN201711440192 A CN 201711440192A CN 108219434 A CN108219434 A CN 108219434A
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Classifications
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Abstract
本发明公开了一种热固性树脂组合物、预浸料以及层压板。其中,热固性树脂组合物包括如下组分:(1)40‑60重量份聚苯醚,所述聚苯醚为两端为环氧基团的聚苯醚,其数均分子量为3000‑10000;(2)30‑50重量份活性酯低聚物,所述活性酯低聚物为DCPD型活性酯;(3)10‑20重量份有机硅高分子,所述有机硅高分子为环氧功能化的聚硅氧烷。本发明的热固性树脂组合物具有很好的活性和浸润性,其制备的预浸料和层压板具有良好的介电性能、耐热性、阻燃性、韧性及加工性等优点。
Description
技术领域
本发明属于电子基材技术领域,特别是涉及一种可用作电子基材覆铜板的热固性树脂组合物、预浸料以及层压板。
背景技术
如今,随着全球信息技术向数字化、网络化迅速发展,超大容量的信息传输和超快速度、超高密度的信息处理,已成为信息及通信设备(ICT)技术发展所追求的目标。这也对电路基板的耐热性、吸水性、耐化学性、机械性能、尺寸稳定性和介电性能等综合性能提出了更高的要求。而现有环氧树脂及酚醛树脂系统的材料已经无法满足近阶段的应用,特别是高速印刷电路板的应用。
为了改善铜箔层压板绝缘层的介电特性,如介电常数(Dielectric constant,Dk)以及耗散因子(Dissipation factor,Df),一般会在树脂组合物内添加介电特性良好的高分子聚合物。聚苯醚(PPO或PPE)树脂就是一种介电性能良好的树脂且被广泛用于高速覆铜板领域。但常规聚苯醚树脂由于分子太大,由其组成的树脂组合物涂覆于玻纤布制备覆铜板所需要的半固化片时,聚苯醚浸润玻纤布的效果不佳,压合基板会有气泡产生,影响基板外观及介电性能。
松下专利CN102361903A公开了采用低分子量的羟基封端的聚苯醚与多官能环氧制备树脂组合物,再将玻纤布浸胶制备半固化片,虽然解决了聚苯醚与玻纤布的浸润性,但羟基封端的低分子量聚苯醚反应活性差,不利于后期的压板固化反应。
中山台光电子专利CN102516530A公开了一种由高分子量聚苯醚与环氧树脂催化反应制备得到的环氧基改性聚苯醚,以及其与其它环氧树脂组合得到的环氧改性聚苯醚树脂组合物。上述专利虽然一定程度上改善了聚苯醚的反应活性,但其与其它环氧树脂组合固化,没有使用介电性能优异的环氧固化剂,对于改善压合基板的介电性能效果不明显,此外,环氧溶液加热催化改性聚苯醚,工艺较复杂,大大限制了覆铜板的生产效率。
生益科技专利CN104761719A提供了一种含有聚苯醚主链的双端基多官能活性酯,并用其固化环氧制备树脂组合物,该专利引入聚苯醚结构的同时采用低介电性能的环氧固化剂固化环氧,制备低介电的覆铜板。然而,将活性酯基团接在聚苯醚两端的做法,限制了活性酯结构多变性的优势,不利于后期树脂组合物的优化以及提高压合基板的综合性能,例如介电、耐热、增韧、阻燃等性能。
综上,现有的可用于电子基板的热固性树脂以及用其制作预浸料或者压层板存在介电性能不高,耐热性能或阻燃性能需要改善,工艺复杂,生产效率不高等问题。
发明内容
本发明的目的在于提供一种热固性树脂组合物、预浸料以及层压板。本发明的树脂组合物具有很好的活性、浸润性,其制备的预浸料和层压板具有良好的介电性能、耐热性、阻燃性、韧性及加工性能等优点。
为了达到上述的目的,本发明提供一种热固性树脂组合物,其包括如下组分:
(1)40-60重量份聚苯醚,所述聚苯醚的两端为环氧基团,数均分子量为3000-10000,所述聚苯醚的链段占聚苯醚总摩尔比40%-90%;
(2)30-50重量份活性酯低聚物,所述活性酯低聚物为DCPD型活性酯;
(3)10-20重量份有机硅高分子,所述有机硅高分子为环氧功能化的聚硅氧烷。
在上述树脂组合物中,所述两端为环氧基团的聚苯醚的结构式如下:
式(1)中Y包括至少一个碳、至少一个氧、至少一个苯环或以上组合物,X为相同或不同,表示-COO-、-CH2-,或-CH2O-,a、b为1以上的整数,R1、R2、R3、R4相同或不同,表示H、OH,C1-C10烷基,或C1-C10烯烃。
在上述树脂组合物中,所述活性酯低聚物的结构式如下:
式(2)中:X为苯环或萘环,R1、R2相同或不同,表示氢原子或碳原子数为1-10的烷基,n为0或1,m为1或2。
在上述树脂组合物中,所述有机硅高分子结构式如下:
式(3)中:X为相同或不同,选自-COO-、-CH2-,或-CH2O-,R1为C1-C10烷基,n为大于1且小于15的整数。
在上述树脂组合物中,进一步包括环氧树脂固化剂。
进一步地,热固性树脂组合物还可以包括胺系化合物、酰胺系化合物、酸酐系化合物、酚系化合物作为共固化剂。
进一步地,可根据需要在热固性树脂组合物中适当组合使用固化促进剂,例如磷系化合物、叔胺、二甲基氨基吡啶、咪唑、有机酸金属盐、Lewis酸、胺络盐等。尤其用作积层材料、电路基板用途时,从耐热性、介电特性、耐焊性考虑,优选二甲基氨基吡啶、咪唑。
在上述树脂组合物中,不包含反应型或添加型含卤阻燃剂;可以在不降低电路基板可靠性的范围内配混不含卤素原子的非卤素系阻燃剂,优选磷系阻燃剂,例如磷酸酯化合物、膦酸化合物、次膦酸化合物、氧化膦化合物、正膦化合物、有机系含氮磷化合物、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物、10-(2,5-二羧基苯基)-9,10-二氢-9-氧杂-10磷菲-10-氧化物、二(3-胺苯基)苯基氧膦或三(3-胺苯基)氧化膦等磷系阻燃剂。
在上述树脂组合物中,进一步地,还包括填料,例如氧化铝、氢氧化铝、氮化铝、氮化硼、勃姆石、滑石、云母、高岭土、轻质碳酸钙、氢氧化镁、熔融二氧化硅、硅微粉、球形二氧化硅、粘土、硼酸锌中的一种或多种。
在上述树脂组合物中,进一步地,还包括:相容剂、界面活性剂、分散剂、溶剂、增韧剂中的一种或多种。
本发明还提供一种预浸料,其包括增强材料及通过浸渍干燥后附着在其上的上述热固性树脂组合物。
本发明还提供一种覆金属箔层压板,其包括至少一张如上所述的预浸料及压覆在预浸料一侧或两侧的金属箔。
本发明具有以下技术特点:
(1)本发明采用DCPD型活性酯固化低分子量环氧化的聚苯醚,很好地利用了活性酯固化环氧减少二次羟基生成的优势,提高了固化体系的介电性能,同时活性酯的DCPD结构也使固化体系保持了高耐热性、低水解性及优异的尺寸稳定性。
(2)本发明直接使用低分子量环氧化聚苯醚不仅省略了合成改性的复杂环节,而且使聚苯醚对玻纤布的浸润性得到改善,同时环氧化后的聚苯醚还具有较佳的反应活性,能很好地将低介电常数的聚苯醚链段引入固化体系提高体系的介电性能。
(3)本发明引入具有环氧反应基团的有机硅柔性树脂,使树脂组合物具有较好韧性的同时改善阻燃性能,且不会降低耐热性能。
具体实施方式
为了更好地说明本发明,便于理解本发明的技术方案,本发明的典型但非限制性的实施案例如下:
具体实施方式中实施例所用原料来源和产品名称如表1所示:
表1实施案例1-6所用原料
(一)热固性树脂组合物的制备:
将聚苯醚与溶剂混合,搅拌至聚苯醚完全溶解后,再依次加入有机硅高分子和活性酯低聚物,最后加入填料或阻燃剂等添加剂,将混合物搅拌混合均匀,即得到热固性树脂组合物。
(二)预浸料的制备
将上一步制备得到的热固性树脂组合物用溶剂调节体系固含量55wt%-60wt%而制成胶液,使用该胶液浸渍增强材料,如玻璃纤维布,将浸渍好的玻璃纤维布在150℃的烘箱中加热干燥1-8分钟即制成预浸料。
(三)覆金属箔层压板的制备
使用上述的6片预浸料和2片1盎司(35μm厚度)的金属箔叠合在一起,通过热压机层压,从而压制成双面金属箔的层压板。所述的热压机层压步骤工艺条件如下:①层压的升温速率,在料温80-120℃时通常应控制在2-3℃/min;②层压的压力设置,外层料温在120-150℃施加满压,满压压力为350psi左右;③固化时,控制料温在200℃,并保温100min。所述的金属箔为铜箔、镍箔、铝箔、SUS箔等。
(四)覆金属箔层压板的性能测定
玻璃化转变温度(Tg)按IPC-TM-6502.4.25测试标准;
耐浸焊性按IPC-TM-650 2.4.13.1标准测试,观察分层起泡时间;
吸水性(%)按IPC-TM-650 2.6.2.1标准测试;
燃烧性按UL-94标准测试;
介电常数和介电损耗按照GB/T 1409-2006(测量电气绝缘材料在工频、音频、高频下电容率和介质损耗因数的推荐方法)标准测定;
剥离强度按照GB/T 4722-92(印制电路用覆铜箔层压板)标准测定。
实施例1-6:改变热固性树脂组合物原料以及原料含量,通过上述制备方法制成覆金属箔层压板,并依据上述性能测定标准测试层压板的玻璃化转变温度、介电常数、介电损耗因素、吸水性、耐热性、阻燃性等性能,结果如表2所示。
表2各实施例比较例的配方组成及其物性数据
上述实施案例中所涉及的原材料用量及配比均为重量配比,各原料如无特殊说明,均可通过市售取得。
从表2中实施例1-3可以看出,热固性树脂组合物中环氧化聚苯醚分子量越大其制成的层压板的介电性能越好,但是随着环氧化聚苯醚的Mn增大,体系的交联密度降低,热性能有所降低,因此,选择分子量适中的环氧化聚苯醚的树脂组合物可制备介电性能优异、耐热性良好的层压板。
从表2中实施例4-5可以看出,用带DCPD链段的活性酯固化环氧化聚苯醚得到的热固性树脂组合物具有更好的介电性能及耐热性;
从表2中实施例4,实施例6比较来看,带环氧活性基团的甲基苯基聚硅氧烷不仅改善了阻燃性能,还保障了热性能没有下降。
综上,本发明提供的树脂组合物制备的层压板具有良好介电性能、良好的耐热性及阻燃性等综合性能。
以上实施例的说明只是用于帮助理解本发明方法及其核心思想。应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以对本发明进行若干改进和修饰,这些改进和修饰也落入本发明权利要求保护范围内。
Claims (10)
1.一种热固性树脂组合物,其特征在于,包括如下组分:
(1)40-60重量份聚苯醚,所述聚苯醚为两端为环氧基团的聚苯醚,其数均分子量为3000-10000;
(2)30-50重量份活性酯低聚物,所述活性酯低聚物为DCPD型活性酯;
(3)10-20重量份有机硅高分子,所述有机硅高分子为环氧功能化的聚硅氧烷。
2.如权利要求1所述的热固性树脂组合物,其特征在于,所述聚苯醚的结构式如下:
式(1)中Y包含至少一个碳、至少一个氧、至少一个苯环或以上组合物,X为相同或不同,表示-COO-、-CH2-,或-CH2O-,a、b为1以上的整数,R1、R2、R3、R4相同或不同,表示H,OH,C1-C10烷基,或C1-C10烯烃。
3.如权利要求1所述的热固性树脂组合物,其特征在于,所述活性酯低聚物的结构式如下:
式(2)中:X为苯环或萘环,R1、R2相同或不同,表示氢原子或碳原子数为1-10的烷基,n为0或1,m为1或2。
4.如权利要求1所述的热固性树脂组合物,其特征在于,所述有机硅高分子结构式如下:
式(3)中:X为相同或不同,选自-COO-、-CH2-,或-CH2O-,R1为C1-C10烷基,n为大于1且小于15的整数。
5.如权利要求1所述的热固性树脂组合物,其特征在于,热固性树脂组合物进一步包括环氧树脂固化剂。
6.如权利要求1所述的热固性树脂组合物,其特征在于,热固性树脂组合物进一步包括共固化剂和/或固化促进剂,所述共固化剂为胺系化合物、酰胺系化合物、酸酐系化合物、酚系化合物中的一种或多种,所述固化促进剂为磷系化合物、叔胺、二甲基氨基吡啶、咪唑、有机酸金属盐、Lewis酸、胺络盐中的一种或多种。
7.如权利要求1所述的热固性树脂组合物,其特征在于,热固性树脂组合物还包括阻燃剂和/或填料,所述阻燃剂为非卤素系阻燃剂,所述填料选自氧化铝、氢氧化铝、氮化铝、氮化硼、勃姆石、滑石、云母、高岭土、轻质碳酸钙、氢氧化镁、熔融二氧化硅、硅微粉、球形二氧化硅、粘土、硼酸锌中的一种或多种。
8.如权利要求1所述的热固性树脂组合物,其特征在于,热固性树脂组合物还包括相容剂、界面活性剂、分散剂、溶剂、增韧剂中的一种或多种。
9.一种预浸料,其包括增强材料及通过浸渍干燥后附着在其上的如权利要求1-8任一项所述的热固性树脂组合物。
10.一种覆金属箔层压板,其包括至少一张如权利要求9所述的预浸料及压覆在预浸料一侧或两侧的金属箔。
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Denomination of invention: A thermosetting resin composition, prepreg, and laminated board Effective date of registration: 20231128 Granted publication date: 20200131 Pledgee: Agricultural Bank of China Limited Hangzhou Yuhang Branch Pledgor: ZHEJIANG HUAZHENG NEW MATERIAL GROUP Co.,Ltd. Registration number: Y2023980067733 |