CN108891102A - 一种可交联氟树脂改性的半固化片及其制备的热固型覆铜板 - Google Patents
一种可交联氟树脂改性的半固化片及其制备的热固型覆铜板 Download PDFInfo
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- CN108891102A CN108891102A CN201810473844.6A CN201810473844A CN108891102A CN 108891102 A CN108891102 A CN 108891102A CN 201810473844 A CN201810473844 A CN 201810473844A CN 108891102 A CN108891102 A CN 108891102A
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Classifications
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Landscapes
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
- Reinforced Plastic Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
本涉及一种可交联氟树脂改性的半固化片及其制备的热固型覆铜板，本发明中，氟树脂与基体树脂之间存在着化学交联结构，使其在拥有与传统的氟树脂改性覆铜板相当的介电性能、热稳定性、化学稳定性和铜箔剥离强度的基础上，表现出更高的机械强度和硬度、更低的热膨胀系数，适合于制作多层高频覆铜板，可满足当下高频、高速通信领域对覆铜板材料的功能多元化和复杂化的各项性能要求。因此，本发明具有良好的工业化生产基础和广阔的应用前景。
Description
技术领域
本发明属于通信材料领域，具体涉及一种可交联氟树脂改性的半固化片及其制备的热固型覆铜板。
背景技术
以环氧树脂、酚醛树脂和氰酸酯树脂为代表的热固型树脂的热机械性能高、热膨胀系数低、物美价廉、加工方便、通用性强，常用来制作覆铜板的基材。然而，其过高的介电常数和介质损耗，限制了它们均只能在低频下使用，已不能满足当下高频高速通信领域对基板材料的各项性能要求。后人们又逐步开发出以聚丁二烯、端乙烯基修饰的聚芳醚等为代表的热固型碳氢树脂为基体的覆铜板，在确保原有热固型树脂性能优势的基础上，进一步提升了板材在高频领域的介电性能。
氟树脂拥有其他聚合物无法比拟的低介电常数（≤2.20）、低介质损耗（≤0.001）、高热稳定性和化学稳定性、较宽频率范围内稳定的介电性能等优势，是一种理想的覆铜板基体材料和基体添加改性剂。然而，迄今为止，在几乎所有的氟树脂改性覆铜板中，氟树脂均是以一种有机填料的形式简单共混在各类基体树脂中，这虽有利于覆铜板的介电性能和热稳定性，但对板材整体的机械强度和硬度贡献不大。最近，《ACS大分子快报》（2015, 4,197-201）和《ACS应用材料与表面》（2016, 8, 11516-11525）报道了以磺化全氟烷氧基乙烯基醚为大分子引发剂引发烯烃类单体聚合这一现象，并揭示了磺化全氟烷氧基乙烯基醚主链/侧链上的CF官能团、侧链上的CF3官能团和侧链醚键附近的CF2官能团均可作为ATRP引发位点这一本质。然而，至今尚未有人以此制备得到可交联氟树脂并将其用于改性热固型覆铜板，以期在基体树脂和氟树脂之间建立化学交联结构，从而获得综合性能更高的全新的氟树脂改性的热固型覆铜板。
发明内容
本发明的目的在于提供一种可交联氟树脂改性的半固化片及其制备的热固型覆铜板。
本发明以全氟烷氧基乙烯基醚共聚物为ATRP大分子引发剂引发乙烯基类可交联化合物聚合，制得可交联氟树脂的分散液；在低温环境下，向该分散液中加入无机填料、阻燃剂、偶联剂和引发剂，充分混合均匀后再加入可交联基体树脂的溶液，经絮凝沉降法制得复合糊状物；随后，将该复合糊状物于干净平板上刮涂成膜，经烘烤-半固化、剥离等步骤制得可交联氟树脂改性的半固化介质片；最后，将半固化介质片、膜和覆于其表面的铜箔一起压合，制备得到了一种热固型覆铜板。
本发明提供的一种可交联氟树脂改性的半固化片及其制备的热固型覆铜板，其具体制备步骤为：
（1）向氟树脂乳液中加入乙烯基类可交联化合物和联吡啶，搅拌均匀后，重复冷冻-脱气-溶解等三步骤，以除去体系中的氧气；随后再加入ATRP催化剂，继续重复冷冻-脱气-溶解等三步骤，以进一步除去体系中的氧气；在40~100℃、剧烈搅拌下反应6~240h后，经搅拌-透析处理得到可交联氟树脂的均匀分散液；
（2）向上述均匀分散液中加入无机填料、阻燃剂、偶联剂和引发剂，于50℃以下环境中搅拌均匀后，紧接着加入可交联基体树脂的溶液，迅速拌匀后待其絮凝沉降，随后倒去溶剂，得到复合糊状物；
（3）将该复合糊状物于干净的平板上刮涂成膜，经烘烤-半固化、剥离等步骤制备得到可交联氟树脂改性的半固化介质片；
（4）最后，将上述半固化介质片、膜和覆于表面的铜箔叠合在一起，经层压工艺制备得到了一种热固型覆铜板。
本发明中，所述的氟树脂乳液为四氟乙烯-全氟烷氧基乙烯基醚共聚物（PFA）及其衍生物中的一种或几种混合物的乳液，固含量为20~70wt/v%，粘度9~45mPa·s (25℃)；所述的氟树脂占所述半固化介质片的1~80wt%。
本发明中，所述的乙烯基类可交联化合物为分子结构中含有两个或两个以上反应型碳碳双键的小分子化合物中的一种或几种的混合物，其用量为氟树脂的0.1~5000wt%。
本发明中，所述联吡啶的用量为氟树脂的0.02wt‰~3wt%。
本发明中，所述的ATRP催化剂为卤化铜CuX（X为Br或Cl）、苄基卤化物、α-溴代酯、α-卤代酮和α-卤代腈中的一种或几种的混合物，其用量为乙烯基类可交联化合物的0.01wt‰~5wt%。
本发明中，所述的无机填料为SiO2、Al2O3、TiO2、ZnO、MgO、Bi2O3、AlN、Si3N4、SiC、Al(OH)3、Mg(OH)2、BaxSr1-xTiO3(x=1~0)、Mg2TiO4、Bi2(TiO3)3、PbTiO3、NiTiO3、CaTiO3、ZnTiO3、Zn2TiO4、BaSnO3、Bi2(SnO3)3、CaSnO3、PbSnO3、MgSnO3、SrSnO3、ZnSnO3、BaZrO3、CaZrO3、PbZrO3、MgZrO3、SrZrO3、ZnZrO3、氧化石墨、氟化石墨、滑石粉、云母粉、高岭土、粘土、实心玻璃微珠、空心玻璃微珠、玻璃纤维和玄武岩纤维中的一种或是几种的混合物，其用量占半固化介质片的0.5~60wt%。
本发明中，所述的阻燃剂为铝镁系阻燃剂、硼锌系阻燃剂、钼锡系阻燃剂、溴系阻燃剂、三氧化二锑、磷系阻燃剂和氮系阻燃剂及其衍生物中的一种或多种的混合物；所述的阻燃剂占半固化介质片的1~65wt%。
本发明中，所述的偶联剂为硅烷偶联剂、钛酸酯偶联剂、铝酸酯偶联剂、硼酸酯偶联剂、锆酸酯偶联剂、稀土偶联剂、磷酸酯偶联剂和磺酰叠氮偶联剂及其衍生物中的一种或多种的混合物，其用量占无机填料的0.01~5wt%。
本发明中，所述的引发剂为能在氟树脂乳液或可交联基体树脂溶液中溶解的过氧化物、偶氮化物和氧化还原体系等自由基引发剂中的一种或几种的混合物，其半衰期10h的分解温度≥50℃；所述引发剂的用量占可交联氟树脂的0.01~5wt%。
本发明中，所述的可交联基体树脂为分子结构中含有反应型碳碳双键的聚合物树脂中的一种或几种的混合物，其用量占半固化介质片的5~95wt%。
本发明中，所述氟树脂乳液的溶剂为可以均匀分散氟树脂、但不能溶解所述可交联基体树脂的溶剂中的一种或几种的混合物；其特征还在于步骤（3）中所述可交联基体树脂溶液的溶剂为可以溶解可交联基体树脂、但不能溶解或分散氟树脂的溶剂中的一种或几种的混合物。
本发明中，所述的平板为陶瓷基或者金属基材料中的一种或几种的复合材料。
本发明中，所述的烘烤-半固化过程分为两个阶段，第一阶段烘烤干燥温度为40~120℃，时间为0.5~10min；第二阶段烘烤干燥温度为120~250℃，时间为0.5~120min。
本发明中，所述的膜为含氟聚合物、聚酰亚胺、聚烯烃、聚芳烃、聚酰胺、聚醚酮、聚醚醚酮、聚芳醚、聚芳硫醚、聚芳醚砜、聚芳硫醚砜、聚芳醚酮、聚芳硫醚酮、聚醚砜酮、聚芳醚腈砜、聚芳硫醚腈砜、聚苯基喹喔啉、酚醛树脂、环氧树脂、氰酸酯树脂、聚碳酸酯、聚氨酯和聚甲醛及其衍生物中的一种或多种的混合物。
本发明中，所述层压工艺的层压温度为150~340℃，层压压力为50~170kg/cm2，层压时间为0.5~24h；其中，半固化介质片的张数≥1，膜的张数≥0，铜箔的张数为1或2；所述氟树脂改性的热固型覆铜板的厚度控制在0.1~10mm之间。
在传统的氟树脂改性覆铜板中，氟树脂仅作为一种有机填料存在于基体之中，虽有利于覆铜板的介电性能和热稳定性，但对板材整体的机械强度和硬度贡献不大。而在本发明中，氟树脂与基体树脂之间存在着化学交联结构，使其在拥有与传统的氟树脂改性覆铜板相当的介电性能、热稳定性、化学稳定性和铜箔剥离强度的基础上，表现出更高的机械强度和硬度、更低的热膨胀系数，适合于制作多层高频覆铜板，可满足当下高频、高速通信领域对覆铜板材料的功能多元化和复杂化的各项性能要求。因此，本发明具有良好的工业化生产基础和广阔的应用前景。
具体实施方式
以下通过实施例进一步详细说明本发明提供的一种可交联氟树脂改性的半固化片及其制备的热固型覆铜板。然而，该实施例仅仅是作为提供说明而不是限定本发明。
实施例 1
向85份四氟乙烯-全氟烷氧基乙烯基醚共聚物乳液（杜邦Teflon® PFAD 335D，固含量60%）中加入9份二乙烯基苯和0.28份联吡啶，搅拌均匀后，重复冷冻-脱气-溶解步骤三次以除去体系中的氧气；随后，向上述体系中加入0.45份CuBr，同法重复冷冻-脱气-溶解步骤三次以进一步除去体系中的氧气，在85℃、剧烈搅拌下反应32h后，再经搅拌-透析得到二乙烯基苯接枝PFA的分散液；接着加入5份SiO2（新沂宏润）、20份阻燃剂氢氧化镁（美国雅宝MAGNIFIN H-5）、60份TiO2（天津中正华美科技）、0.65份硅烷偶联剂KH550（南京曙光化工总厂）和0.24份偶氮二异丁脒盐酸盐（润兴光电V-50），在20℃下搅拌均匀后紧接着加入150份45wt%聚丁二烯的DMF溶液（克雷威利Ricon142）并剧烈搅拌均匀，后待其絮凝沉淀直至不再出现白色粘稠沉淀物，倒去溶剂、得到复合糊状物；将该复合糊状物于干净的玻璃平板上刮成厚度约为0.81mm的膜，在70℃下烘烤5min后，再于220℃下继续烘烤40min，待其自然降至室温后，将膜从玻璃片上剥离，得到半固化介质片；取1张该半固化介质片和2张loz铜箔，在压力为120~150kg/cm2、温度为330℃的情况下层压8h，制得氟树脂改性热固型聚丁二烯基覆铜板。
实施例 2
二乙烯基苯接枝PFA的分散液和复合糊状物的制备方法与实施例1相同；将复合糊状物于干净的玻璃平板上刮成厚度约为0.29mm厚的膜，在70℃下烘烤2min后，再于210℃下继续烘烤20min，待其自然降至室温后，将膜从玻璃片上剥离，得到半固化介质片；取2张该半固化介质片、1张PTFE膜和2张loz铜箔，在压力为120~150kg/cm2、温度为330℃的情况下层压8h，制得氟树脂改性热固型聚丁二烯基覆铜板。
实施例 3
二乙烯基苯接枝PFA的分散液与实施例1相同；接着加入5份SiO2（新沂宏润）、20份阻燃剂氢氧化镁（美国雅宝MAGNIFIN H-5）、60份TiO2（天津中正华美科技）、0.65份硅烷偶联剂KH550（南京曙光化工总厂）和0.24份偶氮二异丁脒盐酸盐（润兴光电V-50），在20℃下搅拌均匀后紧接着加入150份45wt%端乙烯基修饰聚苯醚的DMF溶液（Sabic SA9000）并剧烈搅拌均匀，后待其絮凝沉淀直至不再出现白色粘稠沉淀物，倒去溶剂、得到复合糊状物；将该复合糊状物于干净的不锈钢平板上刮成厚度约为0.81mm厚的膜，在70℃下烘烤5min后，再于230℃下继续烘烤35min，待其自然降至室温后，将膜从玻璃片上剥离，得到半固化介质片；取1张该半固化介质片和2张loz铜箔，在压力为110~140kg/cm2、温度为340℃的情况下层压8h，制得氟树脂改性热固型聚苯醚基覆铜板。
如表1所示，本发明在氟树脂与基体树脂之间建立起化学交联结构，使其在拥有优异的介电性能、热稳定性、化学稳定性和铜箔剥离强度的基础上，表现出较高的机械强度和硬度以及较低的热膨胀系数，可用于制作多层高频覆铜板，以满足当下高频、高速通信领域对覆铜板材料的功能多元化和复杂化的各项性能要求。因此，本发明具有良好的工业化生产基础和广阔的应用前景。
以上实施例并非对本发明中组合物的含量作任何限制。凡是依据本发明的技术实质或组合物成份或含量对以上实施例所作的任何细微修改、等同变化与修饰，均仍属于本发明技术方案的范围内。
Claims (8)
1.一种可交联氟树脂改性的半固化片及其制备的热固型覆铜板，其特征在于其具体制备步骤为：
（1）向氟树脂乳液中加入乙烯基类可交联化合物和联吡啶，搅拌均匀后，重复冷冻-脱气-溶解等三步骤，以除去体系中的氧气；随后再加入ATRP催化剂，继续重复冷冻-脱气-溶解等三步骤，以进一步除去体系中的氧气；在40~100℃、剧烈搅拌下反应6~240h后，经搅拌-透析处理得到可交联氟树脂的均匀分散液；
（2）向上述均匀分散液中加入无机填料、阻燃剂、偶联剂和引发剂，于50℃以下环境中搅拌均匀后，紧接着加入可交联基体树脂的溶液，迅速拌匀后待其絮凝沉降，随后倒去溶剂，得到复合糊状物；
（3）将该复合糊状物于干净的平板上刮涂成膜，经烘烤-半固化、剥离等步骤制备得到可交联氟树脂改性的半固化介质片；
（4）最后，将上述半固化介质片、膜和覆于表面的铜箔叠合在一起，经层压工艺制备得到了一种氟树脂改性的热固型覆铜板。
2.根据权利要求1所述的一种可交联氟树脂改性的半固化片及其制备的热固型覆铜板，其特征在于步骤（1）中所述的氟树脂乳液为四氟乙烯-全氟烷氧基乙烯基醚共聚物（PFA）及其衍生物中的一种或几种混合物的乳液，固含量为20~70wt/v%，25℃时粘度9~45mPa·s；所述的氟树脂占所述半固化介质片的1~80wt%；
所述的乙烯基类可交联化合物为分子结构中含有两个或两个以上反应型碳碳双键的小分子化合物中的一种或几种的混合物，其用量为氟树脂的0.1~5000wt%；
所述联吡啶的用量为氟树脂的0.02wt‰~3wt%；
所述的ATRP催化剂为卤化铜CuX（X为Br或Cl）、苄基卤化物、α-溴代酯、α-卤代酮和α-卤代腈中的一种或几种的混合物，其用量为乙烯基类可交联化合物的0.01wt‰~5wt%。
3.根据权利要求1所述的一种可交联氟树脂改性的半固化片及其制备的热固型覆铜板，其特征在于步骤（2）中所述的无机填料为SiO2、Al2O3、TiO2、ZnO、MgO、Bi2O3、AlN、Si3N4、SiC、BN、Al(OH)3、Mg(OH)2、BaTiO3、SrTiO3、Mg2TiO4、Bi2(TiO3)3、PbTiO3、NiTiO3、CaTiO3、ZnTiO3、Zn2TiO4、BaSnO3、Bi2(SnO3)3、CaSnO3、PbSnO3、MgSnO3、SrSnO3、ZnSnO3、BaZrO3、CaZrO3、PbZrO3、MgZrO3、SrZrO3、ZnZrO3、氧化石墨、氟化石墨、滑石粉、云母粉、高岭土、粘土、实心玻璃微珠、空心玻璃微珠、玻璃纤维和玄武岩纤维中的一种或是几种的混合物，其用量占半固化介质片的0.5~60wt%；
所述的阻燃剂为铝镁系阻燃剂、硼锌系阻燃剂、钼锡系阻燃剂、溴系阻燃剂、三氧化二锑、磷系阻燃剂和氮系阻燃剂及其衍生物中的一种或多种的混合物；所述的阻燃剂占半固化介质片的1~65wt%；
所述的偶联剂为硅烷偶联剂、钛酸酯偶联剂、铝酸酯偶联剂、硼酸酯偶联剂、锆酸酯偶联剂、稀土偶联剂、磷酸酯偶联剂和磺酰叠氮偶联剂及其衍生物中的一种或多种的混合物，其用量占无机填料的0.01~5wt%；
所述的引发剂为能在氟树脂乳液或可交联基体树脂溶液中溶解的过氧化物、偶氮化物和氧化还原体系等自由基引发剂中的一种或几种的混合物，其半衰期10h的分解温度≥50℃；所述引发剂的用量占可交联氟树脂的0.01~5wt%。
4.根据权利要求1所述的一种可交联氟树脂改性的半固化片及其制备的热固型覆铜板，其特征在于步骤（2）中所述的可交联基体树脂为分子结构中含有反应型碳碳双键的聚合物树脂中的一种或几种的混合物，其用量占半固化介质片的5~95wt%。
5.根据权利要求1所述的一种可交联氟树脂改性的半固化片及其制备的热固型覆铜板，其特征在于步骤（1）中所述氟树脂乳液的溶剂为可以均匀分散氟树脂、但不能溶解所述可交联基体树脂的溶剂中的一种或几种的混合物；其特征还在于步骤（3）中所述可交联基体树脂溶液的溶剂为可以溶解可交联基体树脂、但不能溶解或分散氟树脂的溶剂中的一种或几种的混合物。
6.根据权利要求1所述的一种可交联氟树脂改性的半固化片及其制备的热固型覆铜板，其特征在于步骤（3）中所述的平板为陶瓷基或者金属基材料中的一种或几种的复合材料；
所述的烘烤-半固化过程分为两个阶段，第一阶段烘烤干燥温度为40~120℃，时间为0.5~10min；第二阶段烘烤干燥温度为120~250℃，时间为0.5~120min。
7.根据权利要求1所述的一种可交联氟树脂改性的半固化片及其制备的热固型覆铜板，其特征在于步骤（4）中所述的膜为含氟聚合物、聚酰亚胺、聚烯烃、聚芳烃、聚酰胺、聚醚酮、聚醚醚酮、聚芳醚、聚芳硫醚、聚芳醚砜、聚芳硫醚砜、聚芳醚酮、聚芳硫醚酮、聚醚砜酮、聚芳醚腈砜、聚芳硫醚腈砜、聚苯基喹喔啉、酚醛树脂、环氧树脂、氰酸酯树脂、聚碳酸酯、聚氨酯和聚甲醛及其衍生物中的一种或多种的混合物。
8.根据权利要求1所述的一种可交联氟树脂改性的半固化片及其制备的热固型覆铜板，其特征在于步骤（4）中所述层压工艺的层压温度为150~340℃，层压压力为50~170kg/cm2，层压时间为0.5~24h；其中，半固化介质片的张数≥1，膜的张数≥0，铜箔的张数为1或2；所述氟树脂改性的热固型覆铜板的厚度控制在0.1~10mm之间。
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