CN117343656A - 一种覆铜板用无布型软质低介电粘结片及其制备方法 - Google Patents
一种覆铜板用无布型软质低介电粘结片及其制备方法 Download PDFInfo
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Abstract
本发明提供了一种覆铜板用无布型软质低介电粘结片，由PTFE支撑膜以及分别贴合于PTFE支撑膜两面的热固性树脂层组成；所述PTFE支撑膜由以下重量百分比的原料制成：PTFE乳液20～70％，陶瓷粉20～70％，润湿剂5～8％，表面活性剂2～5％；所述热固性树脂层由以下重量百分比的原料制成：热固性碳氢树脂60～70％，填料20～30％，过氧化物引发剂2～5％，抗氧剂3～5％，偶联剂2～3％。本发明还提供了该覆铜板用无布型软质低介电粘结片的制备方法。本发明提供的覆铜板用无布型软质低介电粘结片的材质柔软，且介电性能较好。
Description
技术领域
本发明涉及一种粘结片，特别是涉及一种覆铜板用无布型软质低介电粘结片及其制备方法。
背景技术
目前，国内外的PTFE覆铜板高频板压合所用的粘结片大多是玻纤布加热固树脂加陶瓷填充类型的材料。此类粘结片有三个缺点：一是玻纤布的经纬纱造成材料有方向性，不利于高频信号的传输；二是玻纤布本身的介电常数和介电损耗均较高，影响了高频材料的传输速度与信号完整性；三是玻纤布是主要由SiO2、CaO等成分组成，材质比较硬，在多层压合过程中容易压伤电阻，进而造成线路中的阻值变化超标。
近年来随着通讯行业的发展，PTFE覆铜板行业发展迅猛竞争激烈。PTFE板材由原先仅可用于双面板的无填充的玻纤布加PTFE纯树脂的板材，逐步发展到适用于多层压合的有陶瓷填充的PTFE高频板材，同时电阻铜箔的使用越来越广泛，相应地用于多层压合的低介电粘结片的需求也越来越多，因此，有必要研发出一款无布复合型软质超低介电损耗的粘结片产品。
中国专利申请CN202211005708.7公开了“一种低介电、高Tg的碳氢粘结片及其制备的高频覆铜板”，所述碳氢粘结片由如下重量份的原材料组成：碳氢树脂25-50份，硅微粉5-30，中空硅微粉5-40份，阻燃剂10-30份，偶联剂0.1-10份，抗氧剂0.1-10份，交联剂1-10份，交联助剂0.5-5份。该发明提供的粘结片同样属于玻纤布型，存在会影响高频材料的传输速度、材质较硬等问题。
发明内容
本发明要解决的技术问题是提供一种覆铜板用无布型软质低介电粘结片，其材质柔软，且介电性能较好。
为解决上述技术问题，本发明的技术方案是：
一种覆铜板用无布型软质低介电粘结片，由PTFE支撑膜以及分别贴合于PTFE支撑膜两面的热固性树脂层组成；所述PTFE支撑膜由以下重量百分比的原料制成：PTFE乳液20～70％，陶瓷粉20～70％，润湿剂5～8％，表面活性剂2～5％；所述热固性树脂层由以下重量百分比的原料制成：热固性碳氢树脂60～70％，填料20～30％，过氧化物引发剂2～5％，抗氧剂3～5％，偶联剂2～3％。
进一步地，本发明所述陶瓷粉为二氧化硅粉、二氧化钛粉或氧化铝粉，陶瓷粉的平均粒径为25～50μm。
进一步地，本发明所述润湿剂为聚丙烯酸钠。
进一步地，本发明所述表面活性剂为十二烷基硫酸钠。
进一步地，本发明所述热固性碳氢树脂为苯乙烯-丁二烯-苯乙烯共聚物。
进一步地，本发明所述填料为超细二氧化硅，填料的平均粒径为0.1～0.5μm。
进一步地，本发明所述过氧化物引发剂为过氧化苯甲酸叔丁酯，抗氧剂为抗氧剂168，偶联剂为硅烷偶联剂KH-550。
上述覆铜板用无布型软质低介电粘结片的制备方法包括以下步骤：
S1.按重量百分比称取PTFE支撑膜的各原料，将各原料混合均匀得到混合乳液，将混合乳液涂覆于载体膜表面，380℃下烘烤至混合乳液完全固化成膜后剥离得到PTFE支撑膜；
S2.将步骤S1所得PTFE支撑膜置于等离子设备中，等离子处理2-4分钟后取出得到粗化PTFE支撑膜；
S3.将金属钠加入四氢呋喃与萘的混合液中，室温搅拌2小时后得到处理液，将步骤S2所得粗化PTFE支撑膜浸入处理液中静置5-10分钟，取出后浸入丙酮溶液中静置3-5分钟，取出后用去离子水洗净，105℃下烘干得到活化PTFE支撑膜；
S4.按重量百分比称取热固性树脂层的各原料，将各原料混合均匀得到胶液，将胶液均匀涂覆于步骤S3所得活化PTFE支撑膜的两面，120-160℃下烘烤20-30分钟得到覆铜板用无布型软质低介电粘结片。
进一步地，本发明所述步骤S2中，等离子处理时使用的气体为氩气或氦气，压力为5-10Pa。
进一步地，本发明所述步骤S3中，金属钠、四氢呋喃、萘的比例为3g:250mL:32g，丙酮溶液的浓度为5mol/L。
与现有技术相比，本发明具有以下有益效果：
(1)本发明提供的覆铜板用无布型软质低介电粘结片是使用具有陶瓷粉填充的PTFE膜作为支撑膜，在两边涂上热固型树脂胶液，经过烘干后得到的像三明治结构的软质粘结片，既可以保证材料具有良好的介电性能，同时具有热固性和热塑性高频材料性能，还具有优秀的层间粘结力，满足热应力、热冲击的性能要求，可以广泛用于PTFE高频板的多层压合，也能适用于碳氢板、高速板、FR4板、电阻板、铜箔的多层压合；此外，本发明在未固化前材质柔软，层压时对电阻铜箔的电阻层的碰撞挤压极低，在电阻板的压合中不会压伤铜箔，确保了电阻值稳定，非常适合电阻板的应用。
(2)本发明使用大粒径、低介电的陶瓷粉作为PTFE支撑膜的填充物，既保证了支撑膜的强度、尺寸稳定性，又保证了材料本身的介电性能；此外，本发明使用超细二氧化硅作为热固性树脂层的填料，填料的平均粒径小于电阻铜箔电阻层的1μm的厚度，在压合过程中不会伤害电阻铜箔中的电阻材料。
(3)本发明制备方法中PTFE支撑膜在涂胶前采用了等离子处理(用等离子设备的高压使氩气或氦气产生等离子，等离子轰击PTFE支撑膜的表面，表面氧原子含量增加，氟原子含量降低，使其水接触角由110°下降到43°左右，同时在PTFE膜表面引入含活性气体元素的官能团，增加表面自由能，改善表面惰性)以及使用高氧化性的药水(钠萘四氢呋喃)进行腐蚀处理，双重表面处理有效保证了PTFE支撑膜与热固性树脂层之间的界面粘结力(在经过高温热冲击后不会出现分层的情况)。
具体实施方式
下面将结合具体实施例来详细说明本发明，在此本发明的示意性实施例及其说明用来解释本发明，但并不作为对本发明的限定。
实施例1：
覆铜板用无布型软质低介电粘结片，由厚度为75μm的PTFE支撑膜以及分别贴合于PTFE支撑膜两面、厚度为45mm的热固性树脂层组成；PTFE支撑膜由以下重量百分比的原料制成：PTFE乳液20％，平均粒径为25～50μm的二氧化硅粉70％，聚丙烯酸钠5％，十二烷基硫酸钠5％；热固性树脂层由以下重量百分比的原料制成：苯乙烯-丁二烯-苯乙烯共聚物70％，平均粒径为0.1～0.5μm的超细二氧化硅20％，过氧化苯甲酸叔丁酯2％，抗氧剂1685％，硅烷偶联剂KH-550 3％。
实施例1的制备方法包括以下步骤：
S1.按重量百分比称取PTFE支撑膜的各原料，将各原料混合均匀得到混合乳液，将混合乳液涂覆于载体膜表面，380℃下烘烤至混合乳液完全固化成膜后剥离得到PTFE支撑膜；
S2.将步骤S1所得PTFE支撑膜置于等离子设备中，使用氩气5Pa压力下等离子处理4分钟后取出得到粗化PTFE支撑膜；
S3.将金属钠加入四氢呋喃与萘的混合液中，金属钠、四氢呋喃、萘的比例为3g:250mL:32g，室温搅拌2小时后得到处理液，将步骤S2所得粗化PTFE支撑膜浸入处理液中静置5分钟，取出后浸入浓度为5mol/L的丙酮溶液中静置3分钟，取出后用去离子水洗净，105℃下烘干得到活化PTFE支撑膜；
S4.按重量百分比称取热固性树脂层的各原料，将各原料混合均匀得到胶液，将胶液均匀涂覆于步骤S3所得活化PTFE支撑膜的两面，120℃下烘烤30分钟得到覆铜板用无布型软质低介电粘结片。
实施例2
覆铜板用无布型软质低介电粘结片，由厚度为65μm的PTFE支撑膜以及分别贴合于PTFE支撑膜两面、厚度为55mm的热固性树脂层组成；PTFE支撑膜由以下重量百分比的原料制成：PTFE乳液50％，平均粒径为25～50μm的二氧化钛粉40％，聚丙烯酸钠7％，十二烷基硫酸钠3％；热固性树脂层由以下重量百分比的原料制成：苯乙烯-丁二烯-苯乙烯共聚物65％，平均粒径为0.1～0.5μm的超细二氧化硅25％，过氧化苯甲酸叔丁酯3％，抗氧剂1684％，硅烷偶联剂KH-550 3％。
实施例2的制备方法包括以下步骤：
S1.按重量百分比称取PTFE支撑膜的各原料，将各原料混合均匀得到混合乳液，将混合乳液涂覆于载体膜表面，380℃下烘烤至混合乳液完全固化成膜后剥离得到PTFE支撑膜；
S2.将步骤S1所得PTFE支撑膜置于等离子设备中，使用氦气7Pa压力下等离子处理3分钟后取出得到粗化PTFE支撑膜；
S3.将金属钠加入四氢呋喃与萘的混合液中，金属钠、四氢呋喃、萘的比例为3g:250mL:32g，室温搅拌2小时后得到处理液，将步骤S2所得粗化PTFE支撑膜浸入处理液中静置7分钟，取出后浸入浓度为5mol/L的丙酮溶液中静置4分钟，取出后用去离子水洗净，105℃下烘干得到活化PTFE支撑膜；
S4.按重量百分比称取热固性树脂层的各原料，将各原料混合均匀得到胶液，将胶液均匀涂覆于步骤S3所得活化PTFE支撑膜的两面，140℃下烘烤25分钟得到覆铜板用无布型软质低介电粘结片。
实施例3
覆铜板用无布型软质低介电粘结片，由厚度为60μm的PTFE支撑膜以及分别贴合于PTFE支撑膜两面、厚度为60mm的热固性树脂层组成；PTFE支撑膜由以下重量百分比的原料制成：PTFE乳液70％，平均粒径为25～50μm的氧化铝粉20％，聚丙烯酸钠8％，十二烷基硫酸钠2％；热固性树脂层由以下重量百分比的原料制成：苯乙烯-丁二烯-苯乙烯共聚物60％，平均粒径为0.1～0.5μm的超细二氧化硅30％，过氧化苯甲酸叔丁酯5％，抗氧剂168 3％，硅烷偶联剂KH-550 2％。
实施例3的制备方法包括以下步骤：
S1.按重量百分比称取PTFE支撑膜的各原料，将各原料混合均匀得到混合乳液，将混合乳液涂覆于载体膜表面，380℃下烘烤至混合乳液完全固化成膜后剥离得到PTFE支撑膜；
S2.将步骤S1所得PTFE支撑膜置于等离子设备中，使用氩气10Pa压力下等离子处理2分钟后取出得到粗化PTFE支撑膜；
S3.将金属钠加入四氢呋喃与萘的混合液中，金属钠、四氢呋喃、萘的比例为3g:250mL:32g，室温搅拌2小时后得到处理液，将步骤S2所得粗化PTFE支撑膜浸入处理液中静置10分钟，取出后浸入浓度为5mol/L的丙酮溶液中静置5分钟，取出后用去离子水洗净，105℃下烘干得到活化PTFE支撑膜；
S4.按重量百分比称取热固性树脂层的各原料，将各原料混合均匀得到胶液，将胶液均匀涂覆于步骤S3所得活化PTFE支撑膜的两面，160℃下烘烤20分钟得到覆铜板用无布型软质低介电粘结片。
对比例1
与实施例1不同的是制备方法不包括步骤S2，步骤S3中使用的步骤S2所得粗化PTFE支撑膜替换为步骤S1所得PTFE支撑膜，即PTFE支撑膜在涂胶前不进行等离子处理。
对比例2
与实施例1不同的是制备方法不包括步骤S3，步骤S4中使用的步骤S3所得活化PTFE支撑膜替换为步骤S2所得粗化PTFE支撑膜，即PTFE支撑膜在涂胶前不进行腐蚀处理。
实验例：性能测试
将实施例1-3以及对比例1-2制得的覆铜板用无布型软质低介电粘结片进行性能测试，测试结果如表1所示。
介电性能测试的测试仪器为矢量网络分析仪，测试标准参考IPC-TM-650标准，测试方法为***式谐振腔法，测试条件为室温，谐振频率10GHz。
热冲击性能测试的测试标准参考GB/T 15727-1995标准，测试条件为288℃，10s，6次。
剥离性能测试的测试仪器为铜箔抗剥强度测试仪，测试标准参考IPC-TM-650标准，测试条件为速度25mm/min，跨距50mm，样品尺寸90mm×120mm。
表1
从表1可以看出，实施例1-3的介电性能、热冲击性能、剥离强度均较好。对比例1、2的制备步骤与实施例1不同，与实施例1相比，对比例1、2的介电性能、剥离强度相差无几，而在热冲击性能测试时出现了分层的情况，说明本发明采用的等离子处理、腐蚀处理均能有效提高PTFE支撑膜与热固性树脂层之间的界面粘结力。
上述实施例仅例示性说明本发明的原理及其功效，而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下，对上述实施例进行修饰或改变。因此，举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变，仍应由本发明的权利要求所涵盖。
Claims (10)
1.一种覆铜板用无布型软质低介电粘结片，其特征在于：由PTFE支撑膜以及分别贴合于PTFE支撑膜两面的热固性树脂层组成；所述PTFE支撑膜由以下重量百分比的原料制成：PTFE乳液20～70％，陶瓷粉20～70％，润湿剂5～8％，表面活性剂2～5％；所述热固性树脂层由以下重量百分比的原料制成：热固性碳氢树脂60～70％，填料20～30％，过氧化物引发剂2～5％，抗氧剂3～5％，偶联剂2～3％。
2.根据权利要求1所述的一种覆铜板用无布型软质低介电粘结片，其特征在于：所述陶瓷粉为二氧化硅粉、二氧化钛粉或氧化铝粉，陶瓷粉的平均粒径为25～50μm。
3.根据权利要求1所述的一种覆铜板用无布型软质低介电粘结片，其特征在于：所述润湿剂为聚丙烯酸钠。
4.根据权利要求1所述的一种覆铜板用无布型软质低介电粘结片，其特征在于：所述表面活性剂为十二烷基硫酸钠。
5.根据权利要求1所述的一种覆铜板用无布型软质低介电粘结片，其特征在于：所述热固性碳氢树脂为苯乙烯-丁二烯-苯乙烯共聚物。
6.根据权利要求1所述的一种覆铜板用无布型软质低介电粘结片，其特征在于：所述填料为超细二氧化硅，填料的平均粒径为0.1～0.5μm。
7.根据权利要求1所述的一种覆铜板用无布型软质低介电粘结片，其特征在于：所述过氧化物引发剂为过氧化苯甲酸叔丁酯，抗氧剂为抗氧剂168，偶联剂为硅烷偶联剂KH-550。
8.根据权利要求1～7任意一项所述的一种覆铜板用无布型软质低介电粘结片的制备方法，其特征在于：包括以下步骤：
S1.按重量百分比称取PTFE支撑膜的各原料，将各原料混合均匀得到混合乳液，将混合乳液涂覆于载体膜表面，380℃下烘烤至混合乳液完全固化成膜后剥离得到PTFE支撑膜；
S2.将步骤S1所得PTFE支撑膜置于等离子设备中，等离子处理2-4分钟后取出得到粗化PTFE支撑膜；
S3.将金属钠加入四氢呋喃与萘的混合液中，室温搅拌2小时后得到处理液，将步骤S2所得粗化PTFE支撑膜浸入处理液中静置5-10分钟，取出后浸入丙酮溶液中静置3-5分钟，取出后用去离子水洗净，105℃下烘干得到活化PTFE支撑膜；
S4.按重量百分比称取热固性树脂层的各原料，将各原料混合均匀得到胶液，将胶液均匀涂覆于步骤S3所得活化PTFE支撑膜的两面，120-160℃下烘烤20-30分钟得到覆铜板用无布型软质低介电粘结片。
9.根据权利要求8所述的一种覆铜板用无布型软质低介电粘结片的制备方法，其特征在于：所述步骤S2中，等离子处理时使用的气体为氩气或氦气，压力为5-10Pa。
10.根据权利要求8所述的一种覆铜板用无布型软质低介电粘结片的制备方法，其特征在于：所述步骤S3中，金属钠、四氢呋喃、萘的比例为3g:250mL:32g，丙酮溶液的浓度为5mol/L。
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