CN106590452B - 一种覆铜板用粘结片 - Google Patents
一种覆铜板用粘结片 Download PDFInfo
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- CN106590452B CN106590452B CN201611051432.0A CN201611051432A CN106590452B CN 106590452 B CN106590452 B CN 106590452B CN 201611051432 A CN201611051432 A CN 201611051432A CN 106590452 B CN106590452 B CN 106590452B
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Abstract
本发明属于通信材料领域，具体涉及一种覆铜板用粘结片。本发明将树脂、无机填料和助剂混合均匀之后，经热压烧结‑车削等工艺而制备得到了面积可控、表面平整、厚度均匀易控、韧性和粘性适宜的粘结片。根据实际应用场景，本发明通过选择合适的树脂和无机填料而制备得到了各类复合粘结片，实现了多种聚合物基、不同介电性能、不同表面结构的半固化片之间的良好复合。尤其是因未使用玻璃纤维等增强材料，粘结片介电性能可调节的范围得以大幅提升，有效增强了粘结片的实用性和普适性。本发明中，粘结片与半固化片之间相容性好、粘结力强，所制备得到的多层板热‑机械性能佳、稳定高、吸湿性低，能满足不同通信领域对覆铜板的各项综合性能要求。
Description
技术领域
本发明属于通信材料领域，具体涉及一种覆铜板用粘结片。
背景技术
现如今，信息电子行业处于高速发展阶段，正逐步成为各国的支柱产业之一。作为信息电子产业关键材料之一的覆铜板，已广泛应用在通信基站、卫星、导航定位系统、自动售货机、电脑、手机等领域。半固化片作为覆铜板的基本组成单元之一，它们之间的复合情况对覆铜板的最终性能至关重要。尤其是新近兴起的可穿戴设备、无人驾驶汽车、无人机和智能机器人等领域对覆铜板的综合性能又提出了更高的要求，有些情况下常常需要将多种聚合物基、不同介电性能、不同表面结构的半固化片复合到一起，以实现覆铜板性能的多元化，可同时在多个频率范围内正常、稳定的工作。粘结片的使用、其自身的性能对半固化片之间的复合效果扮演着极为重要的角色。
美国专利US3676566、US3770566和US4647508均报道了利用商品化的粘结片（如聚酰亚胺-含氟材料复合Kapton系列膜）用于制造高性能的覆铜板。然而，商品化粘结片组成固定、可使用范围小且价格昂贵。中国专利CN101885900A、CN102794949B、CN103731980A、CN105898984A、CN101880441A和CN102558861B等提供了多种覆铜板用粘结片的制备方法，但存在粘结片的介电性能可调范围较窄、固化过程复杂、工艺难以控制而导致生产难度增大，并且由于涉及到多种有机溶剂的使用而导致环境问题和安全问题严重。
发明内容
本发明的目的在于提供一种覆铜板用粘结片及其制备方法。
本发明提供的一种覆铜板用粘结片，其具体制备步骤为：称取树脂、无机填料和助剂，经搅拌混合均匀之后，再经热压烧结-车削工艺制备得到粘结片；所述粘结片的厚度为0.005~5mm。
发明人发现，现有技术中覆铜板用粘结片的制备其均涉及到玻纤布或玻璃纤维等增强材料的使用，或者使用可固化体系做粘结片；前者因增强材料自身介电常数高而致使粘结片的介电性能可调节范围大幅变窄；后者固化过程复杂、工艺难以控制而导致生产难度增大。
本发明将树脂、无机填料和助剂混合均匀之后，经热压烧结-车削等工艺可快速连续地制备得到了面积可控、表面平整、厚度均匀易控、韧性和粘性适宜的粘结片。根据实际应用场景，本发明通过选择合适的树脂和无机填料而制备得到了各类复合粘结片，实现了多种聚合物基、不同介电性能、不同表面结构的半固化片之间的良好复合。尤其是因未使用玻璃纤维等增强材料，大幅提升了粘结片介电性能可调节的范围，有效增强了粘结片的实用性和普适性。本发明中，粘结片与半固化片之间相容性好、粘结力强，所制备得到的多层板热-机械性能佳、稳定高、吸湿性低，能满足不同通信领域对覆铜板的各项综合性能要求。
本发明操作过程简单、普适性强、制备条件温和、生产成本低、易于批量化和规模化生产，具有良好的工业化生产基础和广阔的应用前景。
本发明粘结片与半固化片压合之后得到的多层板在高温下处理5min、重复5次不发生起泡、不分层，且外观、强度和韧性几无变化。Z轴CTE (0~100oC, ppm/oC)为5~475，阻燃性(UL-94)达V1或V0，288oC下耐浸焊性超过20次，高压锅蒸煮后288oC下的耐浸焊性仍超过20次。
本发明中，所述的树脂为含氟树脂（如聚四氟乙烯(PTFE)、聚全氟乙丙烯(FEP、F46)、四氟乙烯-全氟烷氧基乙烯基醚共聚物(PFA)等）、聚烯烃（如聚丙烯、聚丁二烯、聚苯乙烯等）、聚酰胺、聚酰亚胺、聚醚酮、聚醚醚酮、聚碳酸酯、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、聚芳醚砜腈、聚芳硫醚砜腈、聚苯基喹喔啉、酚醛树脂、环氧树脂、氰酸酯树脂、聚酯、聚甲醛、聚脲、聚氨酯、丙烯腈-苯乙烯-丙烯酸酯共聚物、丙烯腈-苯乙烯共聚物、甲基丙烯酸酯-苯乙烯共聚物、丙烯腈-丁二烯-苯乙烯共聚物、乙烯-四氟乙烯共聚物、SEBS、苯乙烯-丁二烯-苯乙烯共聚物、苯乙烯-异戊二烯-苯乙烯共聚物、苯乙烯-聚烯烃-苯乙烯共聚物、苯乙烯-丙烯腈共聚物、丁苯橡胶、丁腈橡胶和纤维素及其衍生物中的一种或多种的混合物。
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、石墨、氧化石墨烯、氟化石墨、滑石粉、云母粉、高岭土和粘土等中的一种或是几种的混合物；所述的无机填料占树脂的0~85wt%。
本发明中，所述的助剂为偶联剂、阻燃剂、抗氧剂和脱模剂中的一种或多种的混合物。
本发明中，所述的偶联剂为硅烷偶联剂（如KH550、KH570等）、钛酸酯偶联剂（如TMC-201、TMC-102、DN-101等）、铝酸酯偶联剂（如SG-Al821、DL-411-A、DL-411-B等）、硼酸酯偶联剂、锆酸酯偶联剂（如ZR-801、ZR-802等）、稀土偶联剂（如DN-903、DN-931等）、磷酸酯偶联剂（如DN-27、DN-37等）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0~5wt%。
本发明中，所述的阻燃剂为磷系阻燃剂（如间苯二酚双(二苯基磷酸酯)、磷酸三苯酯等）、氮系阻燃剂（如氰尿酸三聚氰胺、聚磷酸三聚氰胺等）、铝镁系阻燃剂（如氢氧化镁、氢氧化铝等）、硼锌系阻燃剂（如硼砂、偏硼酸钠、硼酸锌等）、钼锡系阻燃剂（如锡酸锌、氧化钼等）、三氧化二锑及其衍生物中的一种或多种的混合物；其用量为树脂的0~50wt%。
本发明中，所述的抗氧剂为亚磷酸酯类抗氧化剂（如三(2,4-二叔丁基苯基)亚磷酸酯、二(2,6-二叔丁基-4-甲基苯基)季戊四醇二亚磷酸酯等）、受阻酚类抗氧剂（如四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、己二醇[β-(3,5-二叔丁基-4-羟基苯基)丙酸]酯等）、受阻胺类抗氧剂（如二芳基仲胺、酮胺等）、含硫酯类抗氧剂（如硫代二丙酸二月桂酯等）、金属钝化剂（如N,N-二乙酰基己二酰基二酰肼等）、ZnS、ZnO和MgO中的一种或多种的混合物；其用量为树脂的0~3wt%。
本发明中，所述的脱模剂为脂肪酸（如硬脂酸、棕榈酸、月桂酸等）、脂肪酸盐（如硬脂酸钙、硬脂酸锌等）、脂肪酸酯（如硬脂酸硬脂酯、甘油三硬脂酸酯、季戊四醇双硬脂酸酯等）、酰胺类（芥酸酰胺）、石蜡、甘油、凡士林、硅酮粉、硅油（如聚二甲基硅氧烷等）、聚烯烃蜡（如聚乙烯蜡、聚丙烯蜡等）、氧化聚烯烃蜡（如氧化聚乙烯蜡、氧化聚丙烯蜡等）、滑石粉、云母粉、陶土和粘土及其衍生物中的一种或多种的混合物；其用量为树脂的0~5wt%。
本发明中，所述的热压烧结温度为120~430oC、压力为40~200kg/cm2，时间为2~72h。
本发明中，所述的车削速度为10~250m/min，进给量0.005~5mm/r，切削深度0.005~5mm。
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覆铜板用粘结片及其制备方法。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
称取75份PTFE（日本大金PTFE M-18）、75份PFA（杜邦Teflon PFA340）、70份二氧化钛（天津中正华美科技）和1份KH550（南京曙光化工总厂），经高速搅拌机混合均匀之后，在360oC、120 kg/cm2下热压烧结24h之后，经车削得到粘结片，其厚度约0.095~0.105mm；将该粘结片与PTFE板高温压合后得到多层板，随后在300oC下处理5min，重复5次后，可观察到多层板不起泡、不分层，且外观、强度和韧性几无变化。
实施例 2
称取150份PTFE（日本大金PTFE M-18）、10份PFA（杜邦Teflon PFA340）、80份二氧化钛（天津中正华美科技）和2份KH550（南京曙光化工总厂），经高速搅拌机混合均匀之后，在430oC、200 kg/cm2下热压烧结24h之后，经车削得到粘结片，其厚度约0.095~0.105mm；将该粘结片与PTFE板高温压合后得到多层板，随后在300oC下处理5min，重复5次后，可观察到多层板不起泡、不分层，且外观、强度和韧性几无变化。
实施例 3
称取110份PTFE（日本大金PTFE L-5）、30份FEP（日本大金Neoflon FEP NC-1539）、10份乙烯-四氟乙烯共聚物(ETFE)（杜邦Teflon Tefzel ETFE750）、50份二氧化钛（天津中正华美科技）、30份二氧化硅（新沂宏润）和1份KH550（南京曙光化工总厂），经高速搅拌机混合均匀之后，在380oC、150 kg/cm2下热压烧结24h之后，经车削得到粘结片，其厚度约0.0105~0.115mm；将该粘结片与PTFE板高温压合后得到多层板，随后在300oC下处理5min，重复5次后，可观察到多层板不起泡、不分层，且外观、强度和韧性几无变化。
实施例 4
称取45份PTFE（日本大金PTFE L-5）、15份乙烯-四氟乙烯共聚物(ETFE) （杜邦Teflon Tefzel ETFE750）、70份聚苯醚（沙比克PPO640）、20份ABS树脂（奇美PA-717C）、70份氧化铝（淄博恒邦）、1份KH550（南京曙光化工总厂）、0.8份抗氧剂225（Ciba精化）、10份双酚A-双（二苯基磷酸酯）（常州常宇化工）和0.5份硬脂酸锌（河北庆保塑料助剂加工有限公司），经高速搅拌机混合均匀之后，在270oC、130 kg/cm2下热压烧结12h之后，再在350oC、150kg/cm2下热压烧结12h，随后经车削得到粘结片，其厚度约0.010~0.110mm；将该粘结片两面分别覆上PTFE板和聚苯醚板，高温压合后得到多层板，随后在240oC下处理5min，重复5次后，可观察到多层板不起泡，粘结片与PTFE板和聚苯醚板复合处均不分层，且外观、强度和韧性几无变化。
实施例 5
将40份聚苯醚树脂（沙比克PPO640）、70份聚苯乙烯（奇美PG-383）、20份氧化硅（新沂宏润）、20份氧化钛（天津中正华美科技）、0.5份硅烷偶联剂KH550（南京曙光化工总厂）、1份抗氧剂1010（南京米兰化工）、1份费托蜡（日本精蜡株式会社FT115）、30份氢氧化铝（潍坊远东橡塑科技）和2份双酚A-双（二苯基磷酸酯）（BDP，常州常宇化工）经高速搅拌混合均匀。经高速搅拌机混合均匀之后，在220oC、110 kg/cm2下热压烧结16h之后，再在280oC、140 kg/cm2下热压烧结8h，随后经车削得到粘结片，其厚度约0.105~0.110mm；将该粘结片两面分别覆上聚苯醚板，高温压合后得到多层板，随后在160oC下处理5min，重复5次后，可观察到多层板不起泡，粘结片和聚苯醚板复合处均不分层，且外观、强度和韧性几无变化。
实施例 6
称取95份聚苯醚（沙比克PPO640）、30份聚丙烯（燕山石化K9026）、25份ABS树脂（奇美PA-717C）、70份氧化铝（淄博恒邦）、1份KH550（南京曙光化工总厂）、1份抗氧剂225（Ciba精化）、6份双酚A-双（二苯基磷酸酯）（常州常宇化工）和0.5份硬脂酸锌（河北庆保塑料助剂加工有限公司），经高速搅拌机混合均匀之后，在260oC、130 kg/cm2下热压烧结16h之后，再在300oC、150 kg/cm2下热压烧结8h，随后经车削得到粘结片，其厚度约0.095~0.105mm；将该粘结片两面分别覆上聚苯醚板，高温压合后得到多层板，随后在210oC下处理5min，重复5次后，可观察到多层板不起泡、不分层，且外观、强度和韧性几无变化。
实施例 7
称取90份聚苯醚（沙比克PPO640）、50份ASA树脂（奇美PW-978B）、20份ABS树脂（奇美PA-717C）、50份氧化铝（淄博恒邦）、10份氧化硅（新沂宏润）、1份KH550（南京曙光化工总厂）、1份抗氧剂225（Ciba精化）、5份双酚A-双（二苯基磷酸酯）（常州常宇化工）、10份氢氧化铝（潍坊远东橡塑科技）和0.5份硬脂酸锌（河北庆保塑料助剂加工有限公司），经高速搅拌机混合均匀之后，在220oC、120 kg/cm2下热压烧结16h之后，再在280oC、150 kg/cm2下热压烧结8h，随后经车削得到粘结片，其厚度约0.105~0.115mm；将该粘结片两面分别覆上聚苯醚板和FR-4板，高温压合后得到多层板，随后在190oC下处理5min，重复5次后，可观察到多层板不起泡，粘结片与FR-4板和聚苯醚板复合处均不分层，且外观、强度和韧性几无变化。
实施例 8
称取90份聚苯乙烯（奇美PG-383）、20份ASA树脂（奇美PW-978B）、10份ABS树脂（奇美PA-717C）、1份抗氧剂225（Ciba精化）、10份双酚A-双（二苯基磷酸酯）（常州常宇化工）、0.5份KH550（南京曙光化工总厂）、50份氢氧化铝（潍坊远东橡塑科技）和0.5份硬脂酸锌（河北庆保塑料助剂加工有限公司），经高速搅拌机混合均匀之后，在120oC、40 kg/cm2下热压烧结16h之后，再在180oC、100 kg/cm2下热压烧结8h，随后经车削得到粘结片，其厚度约0.105~0.115mm；将该粘结片两面分别覆上聚苯醚板，高温压合后得到多层板，随后在120oC下处理5min，重复5次后，可观察到多层板不起泡，粘结片与聚苯醚板复合处均不分层，且外观、强度和韧性几无变化。
实施例 9
将50份聚苯醚树脂（沙比克PPO640）、30份聚苯乙烯（奇美PG-383）、30份ASA树脂（奇美PW-978B）、20份氧化硅（新沂宏润）、20份氧化钛（天津中正华美科技）、0.8份硅烷偶联剂KH550（南京曙光化工总厂）、1份抗氧剂1010（南京米兰化工）、1份硅酮粉（凯杰高分子塑料增韧材料有限公司）、30份氢氧化铝（潍坊远东橡塑科技）和2份双酚A-双（二苯基磷酸酯）（BDP，常州常宇化工）经高速搅拌混合均匀。经高速搅拌机混合均匀之后，在190oC、130 kg/cm2下热压烧结12h之后，再在260oC、150kg/cm2下热压烧结12h，随后经车削得到粘结片，其厚度约0.110~0.115mm；将该粘结片两面分别覆上聚苯醚板和FR-4板，高温压合后得到多层板，随后在170oC下处理5min，重复5次后，可观察到多层板不起泡，粘结片和聚苯醚板复合处均不分层，且外观、强度和韧性几无变化。
对比例1
在不适用粘结片的情况下，将PTFE板经与实施例1一样的工艺压合制备得到多层板。
对比例2
在不适用粘结片的情况下，将PTFE板和聚苯醚板经与实施例4一样的工艺压合制备得到多层板。
对比例3
在不适用粘结片的情况下，将聚苯醚板经与实施例5一样的工艺压合制备得到多层板。
对比例4
在不适用粘结片的情况下，将聚苯醚板与FR-4板经与实施例7一样的工艺压合制备得到多层板。
相比于传统工艺，本发明通过调节车削工艺参数可快速简便地调节粘结片的面积和厚度，由此制备得到的粘结片均匀性佳。车削工艺应用广泛、普适性强。针对不同的应用场景，本发明选用合适的树脂材料、无机填料和加工助剂，优化组合，使得粘结片的介电性能、韧性和粘性等适宜相应的使用场合，实现可与多种聚合物基、不同介电性能、不同表面结构的半固化片之间的良好复合。半固化片之间相容性好、粘结力强，所制备得到的多层板热-机械性能佳、稳定高、吸湿性低，能满足不同通信领域对覆铜板的各项综合性能要求。此外，本发明操作过程简单、普适性强、制备条件温和、生产成本低、易于批量化和规模化生产，具有良好的工业化生产基础和广阔的应用前景。
注：以上均为特征值；Z轴CTE由IPC TM-650 2.4.24 Mettler 3000 TMA测试得到。
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 (6)
1.一种覆铜板用粘结片，其特征在于覆铜板用粘结片的具体制备步骤为：称取树脂、无机填料和助剂，经搅拌混合均匀之后，再经热压烧结-车削工艺而制备得到粘结片；所述粘结片的厚度为0.005~5mm；
所述的树脂为聚烯烃、聚酰胺、聚酰亚胺、聚醚酮、聚醚醚酮、聚碳酸酯、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、聚芳醚砜腈、聚芳硫醚砜腈、聚苯基喹喔啉、酚醛树脂、环氧树脂、氰酸酯树脂、聚酯、聚甲醛、聚脲、聚氨酯、丙烯腈-苯乙烯-丙烯酸酯共聚物、丙烯腈-苯乙烯共聚物、甲基丙烯酸酯-苯乙烯共聚物、丙烯腈-丁二烯-苯乙烯共聚物、乙烯-四氟乙烯共聚物、SEBS、苯乙烯-丁二烯-苯乙烯共聚物、苯乙烯-异戊二烯-苯乙烯共聚物、苯乙烯-聚烯烃-苯乙烯共聚物、苯乙烯-丙烯腈共聚物、丁苯橡胶、丁腈橡胶和纤维素及其衍生物中的一种或多种的混合物；
所述的无机填料为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、石墨、氧化石墨、氟化石墨、滑石粉、云母粉、高岭土和粘土中的一种或是几种的混合物；所述的无机填料占树脂的0~85wt%；
所述的热压烧结温度为120~430oC、压力为40~200kg/cm2，时间为2~72h；
所述的车削速度为10~250m/min，进给量0.005~5mm/r，切削深度0.005~5mm。
2.如权利要求1所述的覆铜板用粘结片，其特征在于所述的助剂为偶联剂、阻燃剂、抗氧剂和脱模剂中的一种或多种的混合物。
3.如权利要求2所述的覆铜板用粘结片，其特征在于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0~5wt%。
4.如权利要求2所述的覆铜板用粘结片，其特征在于所述的阻燃剂为磷系阻燃剂、氮系阻燃剂、铝镁系阻燃剂、硼锌系阻燃剂、钼锡系阻燃剂、三氧化二锑及其衍生物中的一种或多种的混合物；其用量为树脂的0~50wt%。
5.如权利要求2所述的覆铜板用粘结片，其特征在于所述的抗氧剂为亚磷酸酯类抗氧化剂、受阻酚类抗氧剂、受阻胺类抗氧剂、含硫酯类抗氧剂、金属钝化剂、ZnS、ZnO和MgO中的一种或多种的混合物；其用量为树脂的0~3wt%。
6.如权利要求2所述的覆铜板用粘结片，其特征在于所述的脱模剂为脂肪酸、脂肪酸盐、脂肪酸酯、酰胺类、石蜡、甘油、凡士林、硅酮粉、硅油、聚烯烃蜡、氧化聚烯烃蜡、滑石粉、云母粉、陶土和粘土及其衍生物中的一种或多种的混合物；其用量为树脂的0~5wt%。
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