CN115139602A - 一种低介电常数、低介电损耗、高Tg覆铜板的制备方法 - Google Patents
一种低介电常数、低介电损耗、高Tg覆铜板的制备方法 Download PDFInfo
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Abstract
本发明公开了一种低介电常数、低介电损耗、高Tg覆铜板的制备方法，包括如下步骤：(1)制备树脂胶液：按重量份数计，将50‑80份聚苯醚树脂、30‑80份氰酸酯，10‑25份SMA树脂，1‑8份双马来酰亚胺树脂0.1‑10份交联固化剂、0.1‑1份硅烷偶联剂、0‑1份表面分散剂、5‑20份增韧剂、100‑220份溶剂，20‑50份阻燃剂，60‑100份填充材料混合，乳化搅拌均匀；(2)制备半固化片；(3)制备低介电常数、低介电损耗、高Tg覆铜板。本发明制得的覆铜板板材的介电常数(Dk)≤3.9(10GHz)，介电损耗(Df)≤0.005(10GHz)，Tg≥220℃，T288可达到120min以上不分层，具有非常低的介电常数、介电损耗、较高耐热性，适应高频高速电路板的高层设计。
Description
技术领域
本发明属于覆铜板生产技术领域，具体涉及一种低介电常数、低介电损耗、高Tg覆铜板的制备方法。
背景技术
随着5G通讯技术的广泛普及，电子产品日新月异，为了满足整机电子产品信号的高速高质量传输，必须在CCL(铜箔基板)的介电特性上表现得优秀(具有低介电常数性等)。特别是在高频高速高热条件下，要求它的介电特性能够保持稳定。原来在覆铜板上普遍应用的环氧及其固化体系由于本身有很大的介电损耗和一般的尺寸稳定性，限制了它在高频高速高密度互联领域的应用。国外很多先进国家纷纷开发出了各种高性能的树脂材料，如聚苯醚，氰酸酯树脂，双马来酰亚胺树脂，PI，SMA,PTFE等，以满足电子通讯技术的发展要求，这些树脂的合理应用，在覆铜板研发上具有重要意义。
专利CN 110181903A公布了一种以双酚A型氰酸酯和呋喃树脂为主体树脂的树脂组合物，可达到Dk≤3.9(10GHz)，Df≤0.009(10GHz)，150℃<Tg<160℃的效果。
专利CN 107234851B公布了一种以低分子量聚苯醚和双酚A改性型氰酸酯为主体树脂的改性树脂PPO/CE组合物，得到Dk≥3，但Df普遍较大，最小的Df>0.01，未做Tg说明。
专利CN 110421928B公布了一种以改性环氧树脂和苯并恶嗪为主体树脂的树脂组合物，达到了DK为3.5-3.8(10GHz),Df为0.007-0.009(10GHz)，Tg为155℃-160℃。
上述专利中使用不同的树脂体系，达到了一定效果，但Df、Dk值没有同时降低或Tg不够高。
发明内容
本发明针对上述现有技术存在的不足，提供一种低介电常数、低介电损耗、高Tg覆铜板的制备方法，制得的覆铜板板材的介电常数(Dk)≤3.9(10GHz)，介电损耗(Df)≤0.005(10GHz)，Tg≥220℃，T288可达到120min以上不分层，具有非常低的介电常数、介电损耗、较高耐热性，适应高频高速电路板的高层设计。
具体技术方案如下：
低介电常数、低介电损耗、高Tg覆铜板的制备方法，包括如下步骤：
(1)制备树脂胶液：按重量份数计，将50-80份聚苯醚树脂、30-80份氰酸酯，10-25份SMA树脂，1-8份双马来酰亚胺树脂0.1-10份交联固化剂、0.1-1份硅烷偶联剂、0-1份表面分散剂、5-20份增韧剂、100-220份溶剂，20-50份阻燃剂，60-100份填充材料混合，乳化搅拌均匀，得到树脂胶液；
(2)将低介电电子级玻璃纤维布浸渍在步骤(1)制得的树脂后，经过100-200℃的上胶机，制得半固化片，控制含胶量为45％-55％；
(3)取若干张步骤(2)制得的半固化片叠加在一起，双面各覆有一张铜箔，得板材；将板材与不锈钢板上下对应叠合，送入真空压机，在100-250℃、70-150kgf/cm2条件下热压150-300min，制得低介电常数、低介电损耗、高Tg覆铜板。
在上述技术方案的基础上，本发明还可做如下改进：
进一步，步骤(1)中，所述双马来酰亚胺树脂，可以提前溶解于溶剂中配制成溶液，促进其快速溶解；
步骤(1)中，所述交联固化剂所述交联固化剂为DCP(过氧化二异丙苯)、双25(2,5-二甲基-2,5-二(叔丁基过氧化)己烷)中的至少一种。
步骤(1)中，表面分散剂为BYK W-903、BYK W-904中的至少一种；所述硅烷偶联剂为KH-570，所述溶剂为甲苯、丙酮、丁酮、二甲苯中的至少一种。
步骤(1)中，所述增韧剂为苯酚联苯型环氧树脂和氢化的丁苯橡胶的至少一种。
步骤(1)中，所述阻燃剂为十溴二苯醚、十溴二苯乙烷或溴代三嗪中的至少一种。
步骤(1)中，所述填充材料为二氧化硅、空心玻璃球、电子级E玻璃粉、表面分散剂或硅烷偶联剂处理的球形和角形纳米非晶态硅微粉中的至少一种，粒径为0.5-20μm。
在步骤(2)中，所述低介电电子级玻纤布需要经过硅烷偶联剂处理，为E玻纤布或NE玻纤布的任意一种；半固化片胶化时间控制在120-150秒。
优选地，所述聚苯醚树脂可以使用低分子量(Mw:2000-3000)双官能丙烯酸封端聚苯醚低聚物。所述SMA树脂可以使用苯乙烯：马来酸酐共聚摩尔比为6：1，Mw:5000～6500的共聚物，所述硅微粉中SiO2含量达99.9％，粒径平均为3-5μm，最大粒径不超过20μm；所述E玻璃粉的D90≤8μm，最大粒径不超过12μm；所述填充材料最后添加。
进一步，步骤(3)中，可根据不同厚度要求调整半固化片的数量，将板材与不锈钢板上下对应叠合后，先铺高耐热毛毡，再送入真空压机，热压时间优选180-200min，制得低介电常数、低介电损耗、高Tg覆铜板。
与现有技术相比，本发明的有益效果如下：
(1)本发明将硅烷偶联剂处理过的低介电型的E-GLASS玻纤布浸渍特制树脂胶液，其树脂胶液中的聚苯醚树脂在降低介电损耗、提高玻璃化转变温度和增加韧性、降低吸湿性等方面均有良好表现、非常适合于与其它不饱和单体或树脂进行自由基聚合反应；
(2)本发明中的氰酸酯不但能大幅提高覆铜板的耐热性、阻燃性，并大幅度降低了基材的介电常数和介电损耗；
(3)本发明中的阻燃剂由于独特的自熄功能，具有较高的热分解温度和阻燃效果，可以达到UL-94VO级阻燃性能，阻燃性能大大优于传统阻燃体系；且发烟及有毒气体少，是一种环境友好型阻燃材料，能满足欧盟RollS指令及WEEE指令的要求；
(4)本发明的胶液中加入的填充剂，如球形和角形硅和超细电子级E玻璃粉，粒径小，分散性好，介电性能优秀，介电常数很小，制得的PCB板具有较低的成型收缩率、热膨胀系数和很好的尺寸稳定性，而浸渍使用的玻纤布也是低介电型的E-glass玻纤布；
(5)本发明制得制得的覆铜板板材的介电常数(Dk)≤3.9(10GHz)，介电损耗(Df)≤0.005(10GHz)，Tg≥220℃，T288可达到120min以上不分层，具有非常低的介电常数、介电损耗、较高耐热性，适应高频高速电路板的高层设计。
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，所用的计量单位为重量份。
实施例1
一种低介电常数、低介电损耗、高Tg覆铜板的制备方法，包括如下步骤：
(1)制备树脂胶液：按重量份数计，将50份聚苯醚树脂(低分子量(Mw:2000-3000)双官能丙烯酸封端聚苯醚低聚物)、60份氰酸酯，25份SMA树脂(Mw:6000,苯乙烯：马来酸酐共聚比例6：1)，3份双马来酰亚胺树脂，3份交联固化剂DCP、0.5份硅烷偶联剂KH-570、表面分散剂BYK W-904 0.5份，10份增韧剂氢化的丁苯橡胶、70份甲苯，70份二甲苯，20份丁酮，30份阻燃剂十溴二苯醚(含溴量81％-83％)，50份硅烷偶联剂处理的高纯超细球形纳米非晶态硅微粉(SiO2含量达99.9％，粒径平均为3-5μm，最大粒径不超过20μm)，50份超细电子级E玻璃粉(D90≤8μm，最大粒径不超过12μm)混合。
乳化搅拌均匀；
(2)将经过硅烷偶联剂处理的低介电型的电子级2116玻璃纤维布浸渍在步骤(1)制得的树脂胶液中，经过170℃的上胶机，胶化时间控制在140±5秒，制得半固化片，含胶量控制45％-55％；
(3)取6张步骤(2)制得的半固化片叠加在一起，双面各覆有一张18μm铜箔，得板材；将板材与不锈钢板上下对应叠合，铺高耐热毛毡，送入真空压机，在225℃、120kgf/cm2条件下热压180min，制得低介电常数、低介电损耗、高Tg的覆铜板。
实施例2
一种低介电常数、低介电损耗、高Tg覆铜板的制备方法，包括如下步骤：
(1)制备树脂胶液：按重量份数计，将80份聚苯醚树脂(低分子量(Mw:2000-3000)双官能丙烯酸封端聚苯醚低聚物)、40份氰酸酯，15份SMA树脂(Mw:6000,苯乙烯：马来酸酐共聚比例6：1)，3份双马来酰亚胺树脂(购买自日本Daiwakasei)、0.6份硅烷偶联剂KH-570、0.6份表面分散剂BYK W-903、5份增韧剂苯酚联苯型环氧树脂(产自圣泉)、3份交联固化剂DCP，50份甲苯，50份丁酮，20份阻燃剂十溴二苯醚(含溴量81％-83％)，60份填充材料硅烷偶联剂处理的高纯超细角形纳米非晶态硅微粉(SiO2含量达99.9％，粒径平均为3-5μm，最大粒径不超过20μm)混合，乳化搅拌均匀；
(2)将经过硅烷偶联剂处理的低介电型的电子级2116玻璃纤维布浸渍在步骤(1)制得的树脂胶液中，经过180℃的上胶机，胶化时间控制在140±5秒，制得半固化片，控制含胶量50±5％；
(3)取6张步骤(2)制得的半固化片叠加在一起，双面各覆有一张18μm铜箔，得板材；将板材与不锈钢板上下对应叠合，铺高耐热毛毡，送入真空压机，在235℃、150kgf/cm2条件下热压200min，制得低介电常数、低介电损耗、高Tg的覆铜板。
实施例3
一种低介电常数、低介电损耗、高Tg覆铜板的制备方法，包括如下步骤：
(1)制备树脂胶液：按重量份数计，将50份聚苯醚树脂(低分子量(Mw:2000-3000)双官能丙烯酸封端聚苯醚低聚物)、60份氰酸酯，25份SMA树脂(Mw:6000,苯乙烯：马来酸酐共聚比例6：1)，3份双马来酰亚胺树脂，3份交联固化剂DCP、0.5份硅烷偶联剂KH-570、0.5份分散剂BYK W-904,10份增韧剂氢化的丁苯橡胶、70份甲苯，70份二甲苯，20份丁酮，30份阻燃剂十溴二苯醚(含溴量81％-83％)，50份分散剂处理的高纯超细球形、角形1：1混合的纳米非晶态硅微粉(SiO2含量达99.9％，粒径平均为3-5μm，最大粒径不超过20μm)，50份超细电子级E玻璃粉(D90≤8μm，最大粒径不超过12μm)混合。乳化搅拌均匀；
(2)将经过硅烷偶联剂处理的低介电型的电子级2116玻璃纤维布浸渍在步骤(1)制得的树脂胶液中，经过170℃的上胶机，胶化时间控制在140±5秒，制得半固化片，含胶量控制45％-55％；
(3)取6张步骤(2)制得的半固化片叠加在一起，双面各覆有一张18μm铜箔，得板材；将板材与不锈钢板上下对应叠合，铺高耐热毛毡，送入真空压机，在225℃、120kgf/cm2条件下热压180min，制得低介电常数、低介电损耗、高Tg的覆铜板。
对比例1
对比例1与实施例3的区别在于将氰酸酯换为双环戊二烯环氧树脂。
测试方法说明：
1、介电常数：分离柱式介电谐振器测量法，IPC TM-650 2.5.5.13；
2、介电损耗：分离柱式介电谐振器测量法，IPC TM-650 2.5.5.13；
3、Tg(℃)：差示扫描热量法(DSC)，IPC TM-650；
4、T288(min)：热机械分析法(TMA)，IPC TM-650。
实施例1-3和对比例1所得样品的各项性能测试实验数据如表1所示。
表1实施例1-3和对比例1所得样品的各项性能测试实验数据对照表
| 介电常数 | 介电损耗 | Tg(℃) | T288(min) | |
| 实施例1 | 3.80393 | 0.00476 | 227 | >120 |
| 实施例2 | 3.80955 | 0.00482 | 223 | >120 |
| 实施例3 | 3.79320 | 0.00474 | 225 | >120 |
| 对比例1 | 4.79413 | 0.00796 | 195 | 55 |
由表1可以看出，实施例1-3制得的覆铜板板材的介电常数小于3.9，介电损耗小于0.005，T288可达到120min不分层。相比于对比例1，实施例1-3制备的覆铜板，介电常数、介电损耗、Tg、T288的测试效果均优异很多，证明本发明制备的覆铜板具有较低的介电常数、较低的介电损耗、较高的Tg和较高的耐热性。
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 (9)
1.一种低介电常数、低介电损耗、高Tg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：按重量份数计，将50-80份聚苯醚树脂、30-80份氰酸酯，10-25份SMA树脂，1-8份双马来酰亚胺树脂0.1-10份交联固化剂、0.1-1份硅烷偶联剂、0-1份表面分散剂、5-20份增韧剂、100-220份溶剂，20-50份阻燃剂，60-100份填充材料混合，乳化搅拌均匀，得到树脂胶液；
(2)将低介电电子级玻璃纤维布浸渍在步骤(1)制得的树脂后，经过100-200℃的上胶机，制得半固化片，控制含胶量为45％-55％；
(3)取若干张步骤(2)制得的半固化片叠加在一起，双面各覆有一张铜箔，得板材；将板材与不锈钢板上下对应叠合，送入真空压机，在100-250℃、70-150kgf/cm2条件下热压150-300min，制得低介电常数、低介电损耗、高Tg覆铜板。
2.根据权利要求1所述的制备方法，其特征在于，步骤(1)中，所述交联固化剂为DCP(过氧化二异丙苯)、双25(2,5-二甲基-2,5-二(叔丁基过氧化)己烷)中的至少一种。
3.根据权利要求1所述的制备方法，其特征在于，步骤(1)中，所述表面分散剂为BYK W-903、BYK W-904中的至少一种；所述硅烷偶联剂为KH-570，所述溶剂为甲苯、丙酮、丁酮、二甲苯中的至少一种。
4.根据权利要求1所述的制备方法，其特征在于，步骤(1)中，所述增韧剂为苯酚联苯型环氧树脂和氢化的丁苯橡胶的至少一种。
5.根据权利要求1所述的制备方法，其特征在于，步骤(1)中，所述阻燃剂为十溴二苯醚、十溴二苯乙烷或溴代三嗪中的至少一种。
6.根据权利要求1所述的制备方法，其特征在于，所述填充材料为二氧化硅、空心玻璃球、电子级E玻璃粉、表面分散剂或硅烷偶联剂处理的球形和角形纳米非晶态硅微粉中的至少一种，粒径为0.5-20μm。
7.根据权利要求1所述的制备方法，其特征在于，在步骤(2)中，所述低介电电子级玻纤布需要经过硅烷偶联剂处理，为E玻纤布或NE玻纤布的任意一种。
8.根据权利要求1所述的制备方法，其特征在于，所述聚苯醚树脂为低分子量双官能丙烯酸封端聚苯醚低聚物，Mw为2000-3000。
9.根据权利要求1所述的制备方法，其特征在于，所述SMA树脂为苯乙烯：马来酸酐共聚摩尔比为6：1、Mw为5000～6500的共聚物。
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