CN110978724B - 一种高频高速覆铜板的制作方法 - Google Patents

一种高频高速覆铜板的制作方法 Download PDF

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CN110978724B
CN110978724B CN201911245916.2A CN201911245916A CN110978724B CN 110978724 B CN110978724 B CN 110978724B CN 201911245916 A CN201911245916 A CN 201911245916A CN 110978724 B CN110978724 B CN 110978724B
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copper
clad plate
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resin
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陈刚
刘传兵
何梦瑜
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Zhejiang Yuanji New Material Co.,Ltd.
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Abstract

本发明涉及一种高频高速覆铜板的制作方法，包括以下步骤：S1：按比例取用原料备用；S2：将步骤S1中的原料按比例加入高剪切反应釜，正常搅拌5～10小时，再一边搅拌一边加入填充粉料，填充粉料加完后再开启高速剪切电机高速搅拌2～4小时，得到胶水；S3：用电子1080纤维玻璃布涂上步骤S2中得到的胶水，然后在烘箱烘烤5～10分钟制成半固化片；S4：将步骤S3中得到的半固化片进行裁切，然后将裁切的半固化片上下两侧与铜箔配成叠层，在叠层的上下两侧再层叠上钢板，然后放入压机中，在135～230℃下压合4小时，压力为80～450N。本发明具有提高覆铜板的电性能的效果。

Description

一种高频高速覆铜板的制作方法
技术领域
本发明涉及覆铜板生产的技术领域，尤其是涉及一种高频高速覆铜板的制作方法。
背景技术
覆铜箔层压板是将电子玻纤布或其它增强材料浸以树脂，一面或双面覆以铜箔并经热压而制成的一种板状材料，简称为覆铜板。
现有的覆铜板生产工艺如授权公告号为CN101921457B的中国发明专利公开了一种用于生产覆铜板的材料及生产工艺，包括玻璃纤维布、环氧树脂和铜箔，环氧树脂为磷/氮系环氧树脂，在上述环氧树脂内添加有无机阻燃剂，在无机阻燃剂中包括有氢氧化铝粉末与矽粉末；玻璃纤维布由无捻开纤玻璃纤维编织而成。由于在该覆铜板材料中的环氧树脂材料中，用超细氢氧化铝粉末和超软矽粉末作为阻燃剂原料，代替了现有技术中使用溴化树脂等卤素作为阻燃剂原料，从而解决了由于普通型覆铜板的阻燃体系为含溴树脂体系，溴化物燃烧产生对人类和环境有害的二噁英物质问题。
上述中的现有技术方案存在以下缺陷：现有技术中用于生产覆铜板的材料中的环氧树脂通常为双酚A型环氧树脂，因为双酚A型环氧树脂含有较多极性基团，制作的环氧覆铜板介电常数与介质损耗正切值高，所以使用双酚A型环氧树脂制作的覆铜板满足不了5G高频高速信号传输要求。
发明内容
本发明的目的是提供一种高频高速覆铜板的制作方法，通过采用液态聚丁二烯环氧树脂作为基体树脂，减少树脂中的极性基团，从而提高树脂基板的电性能。
本发明的上述发明目的是通过以下技术方案得以实现的：
一种高频高速覆铜板的制作方法，其特征在于：包括以下步骤：
S1：按比例取用原料备用，原料包括以下重量百分比的组分：
Figure BDA0002307622880000011
Figure BDA0002307622880000021
S2：将步骤S1中的原料按比例加入高剪切反应釜，正常搅拌5～10小时，再一边搅拌一边加入填充粉料，填充粉料的加入量与液态聚丁二烯环氧树脂加入量的质量比为(0.3～0.8)∶1，填充粉料加完后再开启高速剪切电机高速搅拌2～4小时，得到胶水；
S3：用电子1080纤维玻璃布涂上步骤S2中得到的胶水，然后在烘箱烘烤5～10分钟制成半固化片；
S4：将步骤S3中得到的半固化片进行裁切，然后将裁切的半固化片上下两侧与铜箔配成叠层，在叠层的上下两侧再层叠上钢板，然后放入压机中，在135～230℃下压合4小时，压力为80～450N。
通过采用上述技术方案，覆铜板的原料采用液态聚丁二烯环氧树脂作为主体树脂，代替现有技术中的双酚A型环氧树脂，可以满足覆铜板的制作工艺要求，同时液态聚丁二烯环氧树脂上的极性基团比双酚A型环氧树脂少，而且含有较多的非极性的双键，制作得到的覆铜板的介电常数和介质损耗正切值较低，电性能优良；苯乙烯树脂可与液态聚丁二烯环氧树脂中的不饱和键进行交联反应，从而使得苯乙烯与液态聚丁二烯环氧树脂交联形成网状
线型酚醛树脂具有高强度、尺寸稳定性好、抗冲击、抗蠕变、抗溶剂等优点，线型酚醛树脂的加入后可以与液态聚丁二烯环氧树脂发生开环交联反应，提高液态聚丁二烯环氧树脂的结构强度，同时赋予更好的抗冲击、抗蠕变等性能。顺丁烯二酸酐用作固化剂成分，对液态聚丁二烯环氧树脂和线型酚醛树脂起到固化交联的作用，而且可以提高交联后的新聚合物的黏合力。促进剂主要起到催化开环交联反应的作用。
原料通过高剪切反应釜进行反应，高剪切反应釜可以将加入的填充粉料粉碎成细小的微粒，然后分散在连续的液相介质中，形成均匀而稳定的混合体。然后再用玻璃布进行涂覆得到半固化片，在通过压机将铜箔热压到半固化片上，从而得到覆铜板。
本发明进一步设置为：所述原料中还添加有苯并恶嗪树脂，所述原料中各组分按重量百分比计为下表：
Figure BDA0002307622880000031
通过采用上述技术方案，苯并恶嗪树脂在加热以及促进剂的共同作用下，会生成含氮类似酚醛树脂的网状物，其具有普通热固性酚醛树脂或热塑性酚醛树脂的耐热性和阻燃性的同时，树脂在成型固化过程中没有小分子释放，所有得到的成品孔隙率低，不易产生裂纹。而且苯并恶嗪树脂的加入使得基体树脂的玻璃化转变温度提高，耐热性能提高更加明显。
本发明进一步设置为：所述原料中还添加有熔融结晶形二氧化硅，所述原料中各组分按重量百分比计为下表：
Figure BDA0002307622880000032
通过采用上述技术方案，熔融结晶形二氧化硅从晶型的二氧化硅转变为非晶型的玻璃熔体，熔融的二氧化硅的热膨胀系数小，可以改变半固化片在压片过程中的流变性，可以提高固化体系的最低熔融粘度，以改善在压合过程中体系流胶大的问题。同时熔融结晶形二氧化硅添加后的半固化片的最低熔融粘度较其他形状的二氧化硅更大，对于体系的流变性影响更大，效果更好。
本发明进一步设置为：所述原料中还添加有十溴二苯乙烷和DOPO，所述原料中各组分按重量百分比计为下表：
Figure BDA0002307622880000041
通过采用上述技术方案，十溴二苯乙烷作为阻燃剂添加到树脂当中可以显著提高覆铜板的阻燃性能。而且十溴二苯乙烷在受热裂解或者燃烧时，不产生有毒的多溴代二苯并二恶烷及多溴代二苯并呋喃，对环境不会造成危害。十溴二苯乙烷在体系中也相当稳定，可以得到循环使用。DOPO与原料一同加入时，DOPO会与环氧基发生亲核反应，使得DOPO作为支链引入，对液态聚丁二烯环氧树脂的主体结构起到阻燃的作用。同时苯并恶嗪树脂与含磷环氧树脂同时存在时，能实现N-P复合阻燃的效果，进一步提高覆铜板的阻燃性能。
根据权利要求1所述的一种高频高速覆铜板的制作方法，其特征在于：所述促进剂包括以下重量百分比的组分：
Figure BDA0002307622880000042
通过采用上述技术方案，树脂在固化时需要较高的固化温度和较长的固化时间，为节约能源、缩短生产周期，需要向体系中添加固化促进剂。咪唑类化合物分子结构中含有仲胺活泼氢原子，本身可以作环氧树脂中温固化剂，其分子中同时存在叔胺氮原子，也可以作为酸酐/环氧树脂体系的亲核型促进剂。2-甲基咪唑、二甲基苯胺、DMP-30和甲基四氢苯酐具有较好的相容性，可以相互之间进行补足，从而对于树脂固化体系起到多重促进的作用，提高固化效率。
本发明进一步设置为：所述溶剂选用甲苯、苯、二甲苯、丙酮、乙酸乙酯、乙酸丁酯中的一种或多种。
本发明进一步设置为：所述填充粉料包括以下重量百分比的组分：
勃姆石 20～50％；
高岭土 20～30％；
碳酸钙 20～50％。
通过采用上述技术方案，填料具有增容的作用，填料可以代替部分树脂，在一定程度上可以起到降低制造成本。勃姆石、高岭土和碳酸钙填料可以协同提高板材的性能，显著提高覆铜板的尺寸稳定性，降低热膨胀系数，提高板材的耐热性、阻燃性、冲孔性和弯曲强度。同时无机填料的加入可以控制上胶所用胶液的粘度，降低半固化片的流动度，改善覆铜板的生产工艺，减少后续压合过程的流胶，提高板材厚度的均匀性和外观的平整度。
综上所述，本发明的有益技术效果为：
1.通过采用液态聚丁二烯环氧树脂作为覆铜板基板的基体树脂，使得覆铜板的介电常数和介质损耗正切值降低，电性能提高；
2.通过添加苯并恶嗪树脂、十溴二苯乙烷和DOPO，使得覆铜板的阻燃性能得到提高。
具体实施方式
以下对本发明作进一步详细说明。
实施例1：
本发明公开的一种高频高速覆铜板的制作方法，包括以下步骤：
S1：按比例取用原料备用，原料包括以下重量百分比的组分：
Figure BDA0002307622880000051
Figure BDA0002307622880000061
其中，
促进剂包括以下重量百分比的组分：2-甲基咪唑40％、二甲基苯胺30％、DMP-3020％、甲基四氢苯酐10％。
S2：将步骤S1中的原料按比例加入高剪切反应釜，正常搅拌5小时，再一边搅拌一边加入填充粉料，填充粉料的加入量与液态聚丁二烯环氧树脂加入量的质量比为0.3∶1，填充粉料加完后再开启高速剪切电机高速搅拌2小时，得到胶水；
S3：用电子1080纤维玻璃布涂上步骤S2中得到的胶水，然后在温度120℃的烘箱内烘烤5分钟制成半固化片；
S4：将步骤S3中得到的半固化片进行裁切，然后将裁切的半固化片上下两侧与铜箔配成叠层，在叠层的上下两侧再层叠上钢板，然后放入压机中，在135℃下压合4小时，压力为450N。
实施例2～11与实施例1的区别在于原料中各组分按重量百分比计为下表。
Figure BDA0002307622880000062
Figure BDA0002307622880000071
Figure BDA0002307622880000072
Figure BDA0002307622880000081
实施例16～27实施例与实施例1的区别在于促进剂中各组分按重量百分比计为下表。
Figure BDA0002307622880000082
实施例28～36实施例与实施例1的区别在于溶剂中各组分按重量百分比计为下表。
Figure BDA0002307622880000083
Figure BDA0002307622880000091
对比例
对比例1与实施例1的区别在于液态聚丁二烯环氧树脂采用双酚A型环氧树脂代替；
对比例2与实施例1的区别在于原料中未添加十溴二苯乙烷；
对比例3与实施例1的区别在于原料中未添加DOPO；
对比例4与实施例1的区别在于原料中未添加苯并恶嗪树脂；
对比例5与实施例1的区别在于原料中未添加DOPO和苯并恶嗪树脂。
检测方法
1、采用GB/T 12636-1990《微波介质基片复介电常数带状线测试方法》对实施例1～5以及对比例1在10GHZ下进行检测，检测结果如下表。
实施例 介电常数(10GHZ)
实施例1 3.2
实施例2 3.3
实施例3 3.3
实施例4 3.4
实施例5 3.5
对比例1 3.9
结论：通过上表的数据可以看出，实施例1～5与对比例1的介电常数测试结果可知，采用液态聚丁二烯环氧树脂制作而成的覆铜板的介电常数明显降低。而通过实施例1～5的结果对比可以得知，液态聚丁二烯环氧树脂含量的改变使得介电常数的值受到影响，说明液态聚丁二烯环氧树脂对于降低介电常数具有很好的效果。
2、阻燃测试
将实施例1、6、7、8以及对比例2～5中的覆铜板用明火点燃，通过观测覆铜板的燃烧状况判断覆铜板的阻燃能力，根据火焰的熄灭时间从长到短分为1～10级。
实施例 燃烧状况
实施例1 6
实施例6 7
实施例7 8
实施例8 8
对比例2 5
对比例3 4
对比例4 4
对比例5 3
结论：通过上表的数据可以看出，实施例1、6、7、8的阻燃性能明显比对比例2～5好，说明苯并恶嗪树脂、DOPO和十溴二苯乙烷对于覆铜板的阻燃能力都有一定的提高作用。而通过对比例2～5的对比可以得知，苯并恶嗪树脂和DOPO之间存在协同促进提高阻燃能力的作用。
本具体实施方式的实施例均为本发明的较佳实施例，并非依此限制本发明的保护范围，故：凡依本发明的结构、形状、原理所做的等效变化，均应涵盖于本发明的保护范围之内。

Claims (4)

1.一种高频高速覆铜板的制作方法，其特征在于：包括以下步骤：
S1：按比例取用原料备用，原料包括以下重量百分比的组分：
液态聚丁二烯环氧树脂40-55%；
线型酚醛树脂5-15%；
顺丁烯二酸酐 5-10%；
苯乙烯树脂 5-25%；
苯并恶嗪树脂5-20%； DOPO 5-10%；
十溴二苯乙烷 5-10%；
熔融结晶型 二氧化硅 5-20%；
促进剂0.1-1%；
溶剂5-10%；
S2：将步骤S1中的原料按比例加入高剪切反应釜，正常搅拌5～10小时，再一边搅拌一边加入填充粉料，填充粉料的加入量与液态聚丁二烯环氧树脂加入量的质量比为(0 .3～0.8)∶1，填充粉料加完后再开启高速剪切电机高速搅拌2～4小时，得到胶水；
S3：用电子1080纤维玻璃布涂上步骤S2中得到的胶水，然后在烘箱烘烤5～10分钟制成半固化片；
S4：将步骤S3中得到的半固化片进行裁切，然后将裁切的半固化片上下两侧与铜箔配成叠层，在叠层的上下两侧再层叠上钢板，然后放入压机中，在135～230℃下压合4小时，压力为80～450N。
2.根据权利要求1所述的一种高频高速覆铜板的制作方法，其特征在于：所述促进剂包括以下重量百分比的组分：
2-甲基咪唑40-60%；
二甲基苯胺 10-30%；
DMP-30 20-40%；
甲基四氢苯酐10-30%。
3.根据权利要求1所述的一种高频高速覆铜板的制作方法，其特征在于：所述溶剂选用甲苯、苯、二甲苯、丙酮、乙酸乙酯、乙酸丁酯中的一种或多种。
4.根据权利要求1所述的一种高频高速覆铜板的制作方法，其特征在于：所述填充粉料包括以下重量百分比的组分：
勃姆石 20～50％；
高岭土 20～30％；
碳酸钙 20-50%。
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