CN113844130A - 一种高Tg高频覆铜板的制备方法 - Google Patents
一种高Tg高频覆铜板的制备方法 Download PDFInfo
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- CN113844130A CN113844130A CN202111066807.1A CN202111066807A CN113844130A CN 113844130 A CN113844130 A CN 113844130A CN 202111066807 A CN202111066807 A CN 202111066807A CN 113844130 A CN113844130 A CN 113844130A
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- Inorganic Chemistry (AREA)
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Abstract
本发明属于覆铜板生产技术领域,尤其涉及一种高Tg高频覆铜板的制备方法。本发明中双酚A型环氧树脂中的环氧基和羟基赋予树脂反应性,使树脂固化物具有很强的内聚力和粘接力;醚键和羟基是极性基团,有助于提高树脂浸润性和粘附力;苯环赋予聚合物耐热性和刚性;异丙撑基减小分子间作用力,赋予树脂一定韧性从而提高玻璃化转变温度。本发明工艺压制所得的覆铜板具有较高玻璃化转变温度(Tg)>215℃、DK≤3.8、Df≤0.007、热分层时间(T288)>120min,基本可以满足5G通信所用电子产品以及智能设备的使用要求。
Description
技术领域
本发明属于覆铜板生产技术领域,尤其涉及一种高Tg高频覆铜板的制备方法。
背景技术
为了适应电子工业的快速发展以及人工智能产业的不断成熟,家电、通讯工具以及智能穿戴设备也正不断的在向小、轻、薄的方向发展,印制电路板(PCB)基板的性能也不断地进步。而其中,5G技术的发展拉动了高速高频覆铜板的快速发展。目前在玻璃布基覆铜板总量中FR-4覆铜板的生产量占总产的90%以上。5G建设中需要的毫米波(30-300GHZ)决定覆铜板基材必须是高频覆铜板才能满足频段要求,所以说毫米波这项技术需要更多的宏基站,进而加大了对高频覆铜板的需求。5G建设过程中所需的另一项技术MassiveMIMO也将刺激了高频覆铜板的不断研发,该项技术的发展意味着天线振子、馈电网络系统将使用更多的高频覆铜板。另外为解决5G信号覆盖不足的问题,将大量建设微小基站,更是全方位的刺激高速高频覆铜板的全面发展。
高Tg印制板当温度升高到某一区域时,基板将由“玻璃态”转变为“橡胶态”,此时的温度称为该板的玻璃化温度(Tg)。也就是说,Tg是基材保持刚性的最高温度(℃)。普通PCB基板材料在高温下,不但产生软化、变形、熔融等现象,同时还表现在机械、电气特性的急剧下降,一般板材的Tg为130度以上,高Tg一般大于170度,中等Tg约大于150度。通常Tg≥170℃的PCB印制板,称作高Tg印制板。基板的Tg提高了,印制板的耐热性、耐潮湿性、耐化学性、耐稳定性等特征都会提高和改善。Tg值越高,板材的耐温度性能越好,尤其在无铅制程中,高Tg应用比较多。高Tg意味的是高耐热性。随着电子工业的飞跃发展,特别是以计算机为代表的电子产品,向着高功能化、高多层化发展,需要PCB基板材料的更高的耐热性作为重要的保证。以SMT、CMT为代表的高密度安装技术的出现和发展,使PCB在小孔径、精细线路化、薄型化方面,越来越离不开基板高耐热性的支持。所以一般的FR-4与高Tg的FR-4的区别是在热态下,特别是在吸湿后受热下,其材料的机械强度、尺寸稳定性、粘接性、吸水性、热分解性、热膨胀性等各种性能存在差异,高Tg产品的这些性能明显要优于普通的PCB基板材料。
发明内容
本发明针对上述现有技术存在的不足,目的在于提供一种高Tg高频覆铜板的制备方法,本发明制备的覆铜板玻璃化转变温度达到215℃以上,热分层时间大于1200s,介电常数在3.6-3.9之间,介质损耗低于0.007,热分层时间(T288)>120min。
为实现以上目的,采用的具体技术方案如下:
一种高Tg高频覆铜板的制备方法,包括如下步骤:
(1)制备树脂胶液:按重量份计,将10~50份DCPD型环氧树脂、9~25份双酚A型环氧树脂、3~20份DDS固化剂、0.1~0.8份咪唑类催化剂、10~30份无机填料、10~60份无卤阻燃填料加入溶剂中,在充分搅拌下,乳化分散均匀2小时后制备得到树脂胶液;
(2)将玻璃纤维布浸渍在步骤(1)制得的树脂后,经过150-170℃烘烤4~7min,制得粘结片;
(3)取若干张步骤(2)制得的粘结片叠合在一起,一面或双面覆以18~35μm铜箔,得板材;将板材放置在不锈钢板之间,然后置于真空压机中,在10~40kgf/cm2、170~220℃条件下热压120~180分钟制成。
其中,所述咪唑类催化剂为2-甲基咪唑、2-乙基-4-甲基咪唑、2-苯基咪唑、DMAP中的至少一种;所述无机填料为滑石粉、硅微粉、云母粉、钛白粉中的至少一种;所述无卤阻燃填料为氢氧化铝、氮系阻燃剂、磷系阻燃剂、三氧化二锑、氢氧化镁中的至少一种;所述溶剂为丙酮、丁酮、甲苯、二甲苯、丙二醇单甲醚、环已酮中的至少一种。
优选的,所用玻璃纤维布型号为1035或2116。
优选的,步骤(1)中胶液的凝胶时间为260秒~390秒,胶液固体含量为50~70%(171℃)。
优选的,步骤(2)中粘结片的树脂流动度为15~35%,含胶量为40~70%,凝胶时间为150~190秒(171℃),所述的含胶量是指浸胶用树脂乳液纯固体占浸胶料片重量的百分比,所述的流动度是指浸胶用树脂乳液在1.4MPa、171±2℃流出的重量占浸胶用树脂乳液总重量的百分比。
与现有技术相比,本发明的有益效果是:
(1)本发明中双酚A型环氧树脂中的环氧基和羟基赋予树脂反应性,使树脂固化物具有很强的内聚力和粘接力;醚键和羟基是极性基团,有助于提高树脂浸润性和粘附力;苯环赋予聚合物耐热性和刚性;异丙撑基减小分子间作用力,赋予树脂一定韧性从而提高玻璃化转变温度。
(2)本发明中用DDS固化剂固化环氧树脂,可以提高产品的玻璃化转变温度、耐热性、尺寸稳定性,保证低吸水率和Low Dk/Df等。
(3)本发明工艺压制所得的覆铜板具有较高玻璃化转变温度(Tg)>215℃、DK≤3.8、Df≤0.007、热分层时间(T288)>120min,基本可以满足5G通信所用电子产品以及智能设备的使用要求。
具体实施方式
以下结合实例对本发明的原理和特征进行描述,所举实例只用于解释本发明,并非用于限定本发明的范围。
具体实施方式中,所述的“份”均为重量份。
实施例1
(1)制备树脂胶液:取DCPD型环氧树脂20份(环氧当量210~290g/eq),双酚A型环氧树脂17份(环氧当量180~260g/eq),DDS固化剂13份,DMAP0.21份,硅微粉15份,磷系阻燃剂10份,氮系阻燃剂10份,加入丁酮、二甲苯的溶剂中,在充分搅拌下配置成固体含量为66%的树脂溶液。
(2)用型号为1035和2116玻纤布浸渍上述树脂溶液,经170℃烘烤6分钟,制成粘结片。粘结片含胶量为55±5%,树脂的流动度为25±4%。
(3)取6片粘结片,叠合整齐,双面覆以18μm铜箔,放置在不锈钢板之间,然后置于真空压机中,在175±3℃、35kgf/cm2条件下热压180分钟,制成双面覆铜板。
实施例2
(1)制备树脂胶液:取DCPD型环氧树脂25份,双酚A型环氧树脂15份(环氧当量180~260g/eq),DDS固化剂15份,2-甲基咪唑0.21份,DMAP0.11份,氢氧化铝15份,磷系阻燃剂10份,加入丙酮、丙二醇单甲醚的溶剂中,在充分搅拌下配置成固体含量为66%的树脂溶液。
(2)用型号为1035和2116玻纤布浸渍上述树脂溶液,经170℃烘烤6分钟,制成粘结片。粘结片含胶量为52±4%,树脂的流动度为24±3%。
(3)取6片粘结片,叠合整齐,双面覆以18μm铜箔,放置在不锈钢板之间,然后放于真空压机中,在190±6℃、40kgf/cm2条件下热压180分钟,制成双面覆铜板。
实施例3
(1)制备树脂胶液:取DCPD型环氧树脂25份,双酚A型环氧树脂18份(环氧当量180~260g/eq),DDS固化剂12份,2-乙基-4-甲基咪唑0.20份,DMAP 0.17份,氢氧化镁18份,磷系阻燃剂9份,钛白粉10份,加入适量丙酮、丁酮、二甲苯做溶剂,在充分搅拌下配置成固体含量为66%的树脂溶液。
(2)用型号为1035和2116玻纤布浸渍上述树脂溶液,经170℃烘烤9分钟,制成粘结片。粘结片含胶量为53±3%,树脂的流动度为25±3%。
(3)取6片粘结片,叠合整齐,双面覆以18μm铜箔,放置在不锈钢板之间,然后放于真空压机中,在185±3℃、40kgf/cm2条件下热压180分钟,制成双面覆铜板。
对比例1
(1)制备树脂胶液:取苯并噁嗪环氧树脂29份,苯酚-芳烷基环氧树脂13份,含磷酚醛树脂25份,2-乙基咪唑0.14份,三氧化二锑30份,硅微粉10份,加入适量丙酮、丁酮、二甲苯做溶剂,在充分搅拌下配置成固体含量为65%的树脂溶液。
(2)用型号为1035和2116玻纤布浸渍上述树脂溶液,经170℃烘烤7分钟,制成粘结片。粘结片含胶量为55±3%,树脂的流动度为21±3%。
(3)取6片粘结片,叠合整齐,双面覆以18μm铜箔,放置在不锈钢板之间,然后放于真空压机中,在220±3℃、40kgf/cm2条件下热压180分钟,制成双面覆铜板。
对比例2
(1)制备树脂胶液:取苯并噁嗪环氧树脂29份,DCPD型环氧树脂22份,邻甲酚型酚醛环氧树脂11份,咪唑0.11份,硅微粉14份,氢氧化铝10份,加入适量丙酮、丙二醇单甲醚做溶剂,在充分搅拌下配置成固体含量为65%的树脂溶液。
(2)用1035和2116玻纤布浸渍上述树脂溶液,经170℃烘烤7分钟,制成粘结片。粘结片含胶量为55±4%,树脂的流动度为25±4%。
(3)取6片粘结片,叠合整齐,双面覆以18μm铜箔,放置在不锈钢板之间,然后放于真空压机中,在220±3℃、40kgf/cm2条件下热压180分钟,制成双面覆铜板。
测试
对实施例1~3以及对比例1~2制备得到的覆铜板进行以下测试,测试结果如表1所示。
(1)玻璃化转变温度(Tg),测试方法采用差示扫描量热仪分析(DSC)
(2)热膨胀系数(CTE),测试方法采用热机械分析法(TMA)
(3)热分解温度(Td),测试方法采用热重分析法(TGA)
(4)燃烧性,依据美国UL94垂直燃烧法测定
(5)热分层时间(T288),测试方法采用热机械分析法(TMA)
(6)剥离强度,测试方法按照IPC-TM-650 2.4.9测量
(7)介电常数(Dk)和介质损耗(Df),测试方法按照ASTM-D150和IPC-TM-6502.5.5.9测量
(8)加工性测试方法按照IPC-TM-650 2.4.7测量
(9)耐浸焊性测试方法IPC-TM-650 2.6.8测量
表1.实施例1~3与对比例1~2所得覆铜板的性能对比
由表1可以看出,与对比例1~2相比,实施例1~3树脂组合物制备的覆铜板具有高Tg、Tg能达到215℃以上,高耐热性、低吸水性、热分层时间(T288)>120min、良好的介电性能等优良的综合性能,且达到无卤阻燃要求,具有良好的加工性能。
以上所述仅为本发明的较佳实施例,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (7)
1.一种高Tg高频覆铜板的制备方法,其特征在于,包括如下步骤:
(1)制备树脂胶液:按重量份计,将10~50份DCPD型环氧树脂、9~25份双酚A型环氧树脂、3~20份DDS固化剂、0.1~0.8份咪唑类催化剂、10~30份无机填料、10~60份无卤阻燃填料加入溶剂中,在充分搅拌下制备得到树脂胶液;
(2)将玻璃纤维布浸渍在步骤(1)制得的树脂后,经过150-170℃烘烤4~7min,制得粘结片;
(3)取若干张步骤(2)制得的粘结片叠合在一起,一面或双面覆以18~35μm铜箔,得板材;将板材放置在不锈钢板之间,然后置于真空压机中,在10~40kgf/cm2、170~220℃条件下热压120~180分钟制成。
2.根据权利要求1所述的制备方法,其特征在于,所述咪唑类催化剂为2-甲基咪唑、2-乙基-4-甲基咪唑、2-苯基咪唑、DMAP中的至少一种。
3.根据权利要求1或2所述的制备方法,其特征在于,所述无机填料为滑石粉、硅微粉、云母粉、钛白粉中的至少一种。
4.根据权利要求1所述的制备方法,其特征在于,所述无卤阻燃填料为氢氧化铝、氮系阻燃剂、磷系阻燃剂、三氧化二锑、氢氧化镁中的至少一种。
5.根据权利要求1所述的制备方法,其特征在于,所述溶剂为丙酮、丁酮、甲苯、二甲苯、丙二醇单甲醚、环已酮中的至少一种。
6.根据权利要求1所述的制备方法,其特征在于,步骤(1)中胶液的凝胶时间为260秒~390秒,胶液固体含量为50~70%(171℃)。
7.根据权利要求1所述的制备方法,其特征在于,步骤(2)中粘结片的树脂流动度为15~35%,含胶量为40~70%,凝胶时间为150~190秒(171℃)。
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