CN116333491B - 一种适用于高速通信的无卤树脂组合物及其应用 - Google Patents
一种适用于高速通信的无卤树脂组合物及其应用 Download PDFInfo
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Abstract
本发明涉及高速通信领域,具体涉及一种适用于高速通信的无卤树脂组合物及其应用,针对现有邻苯二甲腈树脂介电性能不理想的情况下,添加SMA树脂,降低组合物的Dk值,添加氰酸酯降低产品的Df和加工可靠性,加入PTFE微粉,降低层压板的Dk和Df。
Description
技术领域
本发明涉及高速通信领域,具体涉及一种适用于高速通信的无卤树脂组合物及其构成的层压板与制备方法。
背景技术
随着电子信息产业的飞速发展,产品的微型化、高集成化、多功能化,数字电路的传输、读取、处理速度越来越快,对低介电常数材料更加依赖。一般将具有低传输信号损耗特性的高速数字线路板用基板材料,称为高速电路用基板材料。目前,高速基材中最常用的低介电常数基材是聚苯醚,它具有较低的介电常数和介电损耗,但是其耐温性、热膨胀系数以及尺寸稳定性相对较差,而且微电子领域应用的聚苯醚被国外企业垄断,售价昂贵。用邻苯二甲腈树脂开发的覆铜板材料,在耐温性、尺寸稳定性、阻燃性能以及热膨胀系数等方面有很大的优势。但是其介电常数和介质损耗方面不及聚苯醚树脂。
现有专利CN109517197A提供一种腈基树脂覆铜板,介电常数为4.7(3GHz),介电损耗为0 .009(3GHz);无法跟上电子信息快发展对材料的要求,其介电性能需要提升。
发明内容
本发明的目的在于,提供一种无卤树脂组合物,此树脂组合物可达到欧盟RoSH指令要求的无卤化要求,由此树脂组合物制造的预浸料及由单张或多张预浸料叠加金属箔制造的覆金属箔层压板,其介电常数、介质损耗低,可用于5G通信材料。
为了解决上述技术问题,本发明采用如下技术方案:
一种适用于高速通信的无卤树脂组合物,包括邻苯二甲腈树脂、萘环型环氧树脂、SMA树脂、氰酸酯、PTFE微粉。
针对现有邻苯二甲腈树脂介电性能不理想以及玻璃化转变温度高的情况下,添加SMA树脂,降低组合物的Dk值和板材的韧性,添加氰酸酯降低产品的Df,加入PTFE微粉,降低层压板的Dk和Df,并且提高了板材的加工性能。
但添加的比例不能过大,会影响的板材的热膨胀系数和高多层加工能力。
优选的,所述无卤树脂组合物还包括含磷阻燃剂和填料。
优选的,所述邻苯二甲腈树脂树脂、所述萘环型环氧树脂、所述SMA树脂、所述氰酸酯树脂、所述PTFE微粉、所述含磷阻燃剂、所述填料的重量比为100:(10~50):(5~35):(10~40):(50~100) : (5~25):(50~150)。
优选的,所述邻苯二甲腈树脂树脂、所述萘环型环氧树脂、所述SMA树脂、所述氰酸酯树脂、所述PTFE微粉、所述含磷阻燃剂、所述填料的重量比为100:40:20:20: 100: 10:100。
优选的,所述氰酸酯树脂包括双酚A型氰酸酯树脂、酚醛型氰酸酯树脂中的一种或多种。
一种上述无卤树脂组合物的应用,用于制备预浸料或层压板。
优选的,所述预浸料包括所述无卤树脂组合物、所述无卤树脂组合物浸渗或涂布了的基材中的一种或多种。
优选的,所述层压板包括层压板、及压覆于所述层压板的一侧或两侧的金属箔,所述层压板包括数片相贴合的粘结片,所述粘结片采用所述无卤树脂组合物制成。
优选的,所述层压板的制备包括:将所述无卤树脂组合物加入丁酮溶剂中,搅拌混合均匀得到固体含量为60~70wt%的胶液,然后使用基材浸胶,经170℃烘箱中烘5min制得半固化片;将8片所述半固化片层叠,上下一侧或两侧各覆盖一张厚度为18微米金属铜箔,置于真空热压机中,210~235℃温度下压合140min,压制得到所述层压板。
优选的,所述基材包括自由E玻璃纤维布、T玻璃纤维布、S玻璃纤维布、Q玻璃纤维布、有机纤维、有机薄膜中的一种或多种。
与现有技术相比较,实施本发明,具有如下有益效果:
1.邻苯二甲腈树脂与体系较难共混,所选用搭配的其他原材料是经过不断试验摸索而优选出。在试验过程中,分别将聚苯醚和碳氢树脂加入邻苯二甲腈树脂中,但是出现体系不相融的情况,不能制得表面无缺陷的板材。而大多数的环氧体系树脂引入邻苯二甲腈树脂后,介电性能差,且板材表面容易出现斑纹,表明体系相溶性差。而本发明通过长期的研究,意外发现通过优选的环氧树脂、氰酸酯以及SMA树脂,与邻苯二甲腈树脂共混后,具有极好的相容性,用该增强材料预浸经烘烤及压板后所制得的板材,其表面无裂纹和斑纹和其他外观缺陷。
2.其他共混的原材料比例不同对板材的性能有很大的影响。配方中添加萘环型环氧树脂,可提高板材的耐热性能,提高剥离强度,提高阻燃性能。但如果添加过量,板材的介电性能下降,玻璃化转变温度降低。配方中的PTFE微粉,可以降低介电性能,添加过量,则导致玻璃强度显著下降,热膨胀系数增大。配方中的SMA树脂可以降低板材Dk值,添加过多,则影响板材的耐热性能。配方中的氰酸酯可以降低板材的Df值,添加过量,则会导致板材的PCT不合格。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚,下面将结合具体实施例对本发明作进一步地详细描述。
效果例1
一种腈基无卤树脂组合物,以固体重量计,包括如下组分,参见表1所示:
表1
注:上表中,1g=1重量份,各组分分别为:
腈基树脂A1:邻苯二甲腈树脂(成都科宜高分子科技有限公司)
环氧树脂B1:联苯型环氧树脂(NC3000H,日本化药株式会社)
环氧树脂B2:萘环型环氧树脂(HP-9900H,日本DIC株式会社)
环氧树脂B3:DCPD型环氧树脂(HP-7200H,日本DIC株式会社)
SMA树脂C1:苯乙烯—马来酸酐共聚物(EF-60,法国克雷威利)
SMA树脂C2:苯乙烯—马来酸酐共聚物(EF-30,法国克雷威利)
氰酸酯树脂D1:双酚A型氰酸酯树脂(BA-3000S,美国龙沙)
氰酸酯树脂D2:酚醛型氰酸酯树脂(PT-30S,美国龙沙)
含磷阻燃剂FR1:磷系阻燃剂(SPB-100,日本大塚)
PTFE微粉F1:聚四氟乙烯微粉(L-640A,南京天诗新材料)
二氧化硅F2:球形表面改性二氧化硅(VF02510,浙江三时纪新材科技有限公司)
效果例2
按照表1中的组分含量加入丁酮溶剂中,搅拌混合均匀得到固体含量为63wt%的胶液,然后使用2116玻璃纤维布浸胶,经170℃烘箱中烘5min制得半固化片。采用上述半固化片制得层压板,其制造方法包括如下步骤:将8片上述制得的半固化片层叠,上下各覆盖一张厚度为18微米金属铜箔,置于真空热压机中,在225℃温度下压合140min,制得1.0mm厚度的覆铜箔层压板。
表2分别是对实施例1~3和对比例1~7制备的层压板进行性能测试,结果如下表所示:
表2
性能测试:
性能测试方法如下:
玻璃化转变温度(Tg):采用DMA法进行测试,按照IPC-TM-650 2.4.24.2方法进行测试。
剥离强度:按照IPC-TM-650 2 .4 .8方法进行测试。
PCT:按照IPC-TM-650 2 .6 .23方法进行测试。
介电性能(Dk/Df):按照IPC-TM-650 2 .5 .5 .9方法进行测试,频率为3GHz。
Float漂锡T288:将含铜样品漂在288℃锡炉中,记录爆板分层时间,若受热120分钟后仍未爆板,则记录为“>120”分钟无爆板。
Y轴CTE:按照IPC-TM-650 2 .4 .24方法进行测试。
阻燃性:按照IPC-TM-650 2 .3 .10方法进行测试。
次表面外观:将制得样品蚀刻表面的铜箔,观察表面外观。表面平滑,颜色分布均匀,无其他缺陷为合格。
从表2的数据可知,相比于现有技术样品介电常数(Dk)通常在5上下,运用本发明获得的实施例1~3的样品能调整到3~4之间。更重要的是,相对于现有平均0.09左右的介电损耗(Df),而实施例1~3成功将介电损耗降低到了0.07附近,获得了预料不到的效果。并且,采用本发明提供的邻苯二甲腈无卤树脂组合物配方,还具有阻燃性能可达UL94V0级别,耐热性强,剥离强度高,低热膨胀等优异性能。
从表2的数据还可知,配方中添加萘环型环氧树脂,可提高板材的耐热性能,提高剥离强度,提高阻燃性能。但如果添加过量,板材的介电性能下降,玻璃化转变温度降低。配方中的PTFE微粉,可以降低介电性能,添加过量,则导致玻璃强度显著下降,热膨胀系数增大。配方中的SMA树脂可以降低板材Dk值,添加过多,则影响板材的耐热性能。配方中的氰酸酯可以降低板材的Df值,添加过量,则会导致板材的PCT不合格。
以上所揭露的仅为本发明的较佳实施例而已,当然不能以此来限定本发明之权利范围,因此依本发明权利要求所作的等同变化,仍属本发明所涵盖的范围。
Claims (8)
1.一种适用于高速通信的无卤树脂组合物,其特征在于,所述无卤树脂组合物包括邻苯二甲腈树脂、萘环型环氧树脂、SMA树脂、氰酸酯树脂、PTFE微粉;所述无卤树脂组合物还包括含磷阻燃剂和填料;所述邻苯二甲腈树脂、所述萘环型环氧树脂、所述SMA树脂、所述氰酸酯树脂、所述PTFE微粉、所述含磷阻燃剂、所述填料的重量比为100:(10~50):(5~35):(10~40):(50~100) : (5~25):(50~150)。
2.根据权利要求1所述适用于高速通信的无卤树脂组合物,其特征在于,所述邻苯二甲腈树脂、所述萘环型环氧树脂、所述SMA树脂、所述氰酸酯树脂、所述PTFE微粉、所述含磷阻燃剂、所述填料的重量比为100:40:20:20: 100: 10:100。
3.根据权利要求1所述适用于高速通信的无卤树脂组合物,其特征在于,所述氰酸酯树脂包括双酚A型氰酸酯树脂、酚醛型氰酸酯树脂中的一种或多种;所述填料包括二氧化硅。
4.一种根据权利要求1所述适用于高速通信的无卤树脂组合物的应用,其特征在于,用于制备预浸料或层压板。
5.根据权利要求4所述应用,其特征在于,所述预浸料包括所述无卤树脂组合物、所述无卤树脂组合物浸渗或涂布了的基材中的一种或多种。
6.根据权利要求4所述应用,其特征在于,所述层压板包括层压板、及压覆于所述层压板的一侧或两侧的金属箔,所述层压板包括数片相贴合的粘结片,所述粘结片采用所述无卤树脂组合物制成。
7.根据权利要求6所述应用,其特征在于,所述层压板的制备包括:将所述无卤树脂组合物加入丁酮溶剂中,搅拌混合均匀得到固体含量为60~70wt%的胶液,然后使用基材浸胶,经170℃烘箱中烘5min制得半固化片;将8片所述半固化片层叠,上下一侧或两侧各覆盖一张厚度为18微米金属铜箔,置于真空热压机中,210~235℃温度下压合140min,压制得到所述层压板。
8.根据权利要求5或7所述应用,其特征在于,所述基材包括自由E玻璃纤维布、T玻璃纤维布、S玻璃纤维布、Q玻璃纤维布、有机纤维、有机薄膜中的一种或多种。
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