CN112210749A - 一种mpi覆铜板的制备方法及其制备的mpi覆铜板 - Google Patents
一种mpi覆铜板的制备方法及其制备的mpi覆铜板 Download PDFInfo
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Abstract
本发明涉及一种电子材料制备领域，特别是涉及一种MPI覆铜板的制备方法及其制备的MPI覆铜板。本发明制备方法包括：(1)MPI薄膜表面预处理；(2)将表面预处理过的MPI薄膜放入银离子溶液中进行金属离子接枝改性；(3)将改性后的薄膜通过低能离子束系统沉积金属种子层；(4)将金属种子层通过低能离子束系统沉积金属层。本发明通过化学接枝法可以直接活化MPI薄膜表面，可在聚合物表面获得带有金属银离子的官能团，获得致密性高的覆铜层，大大提高了提高MPI薄膜与铜金属层的结合力。
Description
技术领域
本发明涉及一种电子材料制备领域，特别是涉及一种MPI覆铜板的制备方法及其制备的MPI覆铜板。
背景技术
5G通讯针对覆铜板在高频、低传输损耗、高密度、高集成化等方面提出了迫切的需求。目前应用较多的软板基材主要是PI，但是由于PI基材的介电常数和损耗因子较大、吸潮性较大、可靠性较差，因此PI软板的高频传输损耗严重、结构特性较差，已经无法适应当前的高频高速趋势。因此出现了LCP材料和MPI材料。MPI材料就是改进配方的聚酰亚胺天线，MPI因为是非结晶性的材料，所以操作温度宽，在低温压合铜箔下易操作，表面能够与铜较易接着，且成本低。MPI高频挠性覆铜板主要应用在高频信号传输的FPC天线板上，终端运用于5G手机、物联网、智能家居、无人驾驶、VR技术等。现有单面或双面的无胶挠性覆铜板(FCCL)主要制备技术为制备工艺有涂布法、压合法及溅镀法三种，但传统的制备方法难以制备12微米以下覆铜板，或者金属层与MPI基材的结合力不高。
CN110691469A公开了一种高频线路板新型材料层结构的涂布成型方法及其制品，具体公开了将铜箔放到涂布机上，以铜箔为基底，在铜箔上涂布合成液态薄膜；将涂布有合成液态薄膜的铜箔送至隧道烤炉内分段烘烤，在铜箔上形成固化薄膜，获得单面板；将单面板放到涂布机上，在单面板的固化薄膜上涂覆上一层合成液态高频材料层；将涂覆有合成液态高频材料层的单面板送至隧道烤炉内，单面板上的合成液态高频材料层变成半固化高频材料层，获得高频线路板新型材料层结构。该技术方案直接使用涂布法，但减薄铜箔的成本高，而且无法实现在超薄铜箔上直接进行涂覆，整体结合力也不高。
CN110655789A公开了低介电低损耗的5G应用材料及其制备方法，包括位于中间的MPI 材料层，以及包覆在MPI材料层上下两侧的LCP材料层，其中MPI材料层的厚度是25-75um， LCP材料层的厚度为12.5-50um。该技术方案制备方法包括使低介电低损耗的5G应用材料，在干燥惰性气体的保护下采用远红外加热的方式，与基材结合，因此，尽管该方法结合了 LCP材料和MPI材料的优缺点，材料的结合力还是不够，存在改进的空间。
综上所述，现有技术仍缺乏一种结合力高的MPI超薄无胶覆铜板。
发明内容
本发明目的是针对现有技术的不足，通过化学接枝法直接活化MPI薄膜表面，通过化学接枝，可在聚合物表面获得带有金属银离子的官能团，提高MPI薄膜与基材的结合力，本发明的详细技术方案如下所述。
一种MPI覆铜板的制备方法，包括以下步骤：
(1)MPI薄膜表面预处理；
(2)将表面预处理过的MPI薄膜放入银离子溶液中进行金属离子接枝改性；
(3)将改性后的薄膜通过低能离子束系统沉积金属种子层；
(4)将金属种子层通过低能离子束系统沉积金属层。
MPI薄膜在NaOH溶液中水解，对MPI薄膜进行表面改性，薄膜表层酰亚胺基团断裂生成酰亚胺酸和酰亚胺酸钠盐。在AgNO，溶液中Na+与Ag+交换。详细的化学反应路线如下所示。
本发明主要利用化学接枝法改变表面化学态。为使MPI薄膜表面具有良好的活性，采用碱性溶液对MPI薄膜进行化学改性，MPI薄膜表面在NaOH溶液中发生水解，表层酰亚胺基团断裂生成酰亚胺酸和酰亚胺酸钠盐，在AgNO3溶液中实现Na+和Ag+间的离子交换,形成含有银离子的接枝，随后在MPI薄膜表进行面低能离子束沉积实现表面金属化，最后通过低能离子束系统在MPI基体上直接进行覆铜，致密性高，并且结合力高，可实现1-10微米的铜箔的制备，成本可控，工艺环保。
本发明中离子能量小于等于5keV为低能离子束，大于5keV为高能离子束。
作为优选，所述步骤(2)中银离子浓度为2-4g/L，反应时间为离子交换时间30-40min。本发明要采用碱性溶液对MPI薄膜进行化学改性，提高改性的离子交换效率。
作为优选，所述步骤(3)中金属种子层为银金属层，厚度为10-200nm。金属种子层主要是起到承上启下的作用，使用银金属在之前离子交换形成的含有银离子的接枝进行沉积，可以提高沉积的效率，提高整体的结合力。
作为优选，所述步骤(3)中金属种子层包括第一金属层和第二金属层，所述第一金属层为银金属层，厚度为10-100nm，所述第二金属层为过渡金属层，所述过渡金属层的金属为Ti、Ni、Cr、Co、Cu中的一种，所述过渡金属层厚度为10-100nm。由于金属银比较贵重，因此可以使用少量银，然后使用与银接触较好的金属，在形成一层较厚的金属层。
作为优选，所述步骤(3)中沉积负偏压为15V-150V，沉积电流为40-120A，束流强度为0.5-5A。
作为优选，所述步骤(4)中沉积金属层为Cu层，厚度为1-10μm。本发明是为了制备MPI薄膜覆铜板，通过金属种子层后再沉积金属层，能够有效提高沉积效果，并且提升MPI薄膜与铜金属层的结合力。
作为优选，所述步骤(4)中沉积负偏压为0V-200V，沉积电流为40-120A，束流强度为0.5-5A。
作为优选，所述步骤(1)中预处理步骤为：将MPI薄膜去离子水超声清洗10min，放入1-3mol/L NaOH溶液中室温浸泡15-60min，取出，用大量去离子水冲洗干净，烘干待用。MPI薄膜通过使用碱液清洗杂质，提高沉积效率和成功率。
本发明保护一种5G用MPI覆铜板，根据所述的制备方法制备而成。
作为优选，所述金属层与所述MPI基材的剥离强度大于或等于0.7N/mm。0.7N/mm的结合力，能够远远满足覆铜板的结合力要求。
本发明的有益效果有：
(1)本发明通过化学接枝法可以直接活化MPI薄膜表面，通过化学接枝，可在聚合物表面获得带有金属银离子的官能团，提高MPI薄膜与铜金属层的结合力；
(2)本发明通过低能离子束技术制备种子层，低能离子束系统引出的纯离子束带有一定能量，可以与接枝获得的Ag离子官能团的MPI表面实现高结合，低能离子束技术具有高的离子密度可获得致密性高的种子层及覆铜层；
(3)本发明结合力高，成本可控，工艺环保，可实现1-10微米的铜箔的制备，市场前景广阔。
具体实施方式
下面对本发明的具体实施方式作进一步说明：
实施例
实施例1
一种5G用MPI覆铜板的制备方法，通过以下步骤制备而成：
(1)MPI薄膜表面预处理，取尺寸为200mm*600mm的MPI薄膜，去离子水超声清洗10min，随后放入3mol/L NaOH溶液中室温浸泡30min，取出，用大量去离子水冲洗干净，烘干待用；
(2)金属离子接枝，将表面预处理过的MPI薄膜放人2g/L AgNO3溶液中进行离子交换，离子交换时间为30min，取出薄膜用大量去离子水清洗干净；
(3)将改性后的薄膜通过低能离子束系统沉积金属种子层，沉积负偏压为100V，沉积电流为50A，束流强度为3A，所述种子金属层为银金属层，厚度为100nm；
(4)在银金属层表面通过低能离子束系统沉积金属层，沉积负偏压为150V，沉积电流为100A，束流强度为4A，沉积金属为Cu，金属Cu层厚度为5μm。
实施例2
一种5G用MPI覆铜板的制备方法，通过以下步骤制备而成：
(1)MPI薄膜表面预处理，取尺寸为200mm*600mm的MPI薄膜，去离子水超声清洗10min，随后放入3mol/L NaOH溶液中室温浸泡30min，取出，用大量去离子水冲洗干净，烘干待用；
(2)金属离子接枝，将表面预处理过的MPI薄膜放人2g/L AgNO3溶液中进行离子交换，准确控制离子交换时间30min，取出薄膜用大量去离子水清洗干净。
(3)通过低能离子束系统沉积金属种子层，先沉积第一金属层，也就是银金属层，沉积负偏压为100V，沉积电流为50A，束流强度为3A，厚度为20nm，然后沉积第二金属层，沉积负偏压、沉积电流、束流强度不变，第二金属层为Ti金属层，厚度为100nm；
(4)通过低能离子束系统沉积金属层，沉积负偏压为150V，沉积电流为100A，束流强度为4A，沉积金属为Cu，金属Cu层厚度为5μm。
实施例3-实施例4，对比实施例1-对比实施例4的制备方法与实施例1和实施例2大体相同，因此简化描述，主要参数如表1所示。
表1实施例和对比实施例的主要参数表
测试实施例
将实施例和对比实施例进行剥离强度测试和粗糙度测试。剥离强测试方法为，采用90 度剥离强度试验机进行测试。粗糙度测试采用粗糙度测试仪，依据《国家标准GB/T3505-09》。测量结果如表2所示。
表2测试结果表
通过数据证明，(1)由实施例1-4与对比实施例1-3可知，本发明获得的MPI薄膜覆铜板能够有效提高MPI与金属层的结合力；
(2)由实施例1-4与对比实施例1-2可知，进行金属离子接枝能够有效提高结合力；
(3)由实施例1-4与对比实施例3可知，种子金属层能够提高结合力。
(4)由实施例3与对比实施例4可知，需进行NaOH溶液的前处理，才能够形成有效的金属离子接枝层。
(5)由实施例4与对比实施例5可知，NaOH溶液浓度会影响表面粗糙度。
根据上述说明书的揭示和教导，本发明所属领域的技术人员还可以对上述实施方式进行变更和修改。因此，本发明并不局限于上面揭示和描述的具体实施方式，对发明的一些修改和变更也应当落入本发明的权利要求的保护范围内。此外，尽管本说明书中使用了一些特定的术语，但这些术语只是为了方便说明，并不对本发明构成任何限制。
Claims (10)
1.一种MPI覆铜板的制备方法，其特征在于，包括以下步骤：
(1)MPI薄膜表面预处理；
(2)将表面预处理过的MPI薄膜放入银离子溶液中进行金属离子接枝改性；
(3)将改性后的薄膜通过低能离子束系统沉积金属种子层；
(4)将金属种子层通过低能离子束系统沉积金属层。
2.根据权利要求1所述的制备方法，其特征在于，所述步骤(2)中银离子浓度为2-4g/L，反应时间为30-40min。
3.根据权利要求2所述的制备方法，其特征在于，所述步骤(3)中金属种子层为银金属层，厚度为10-200nm。
4.根据权利要求1或2所述的制备方法，其特征在于，所述步骤(3)中金属种子层包括第一金属层和第二金属层，所述第一金属层为银金属层，厚度为10-100nm，所述第二金属层为过渡金属层，所述过渡金属层的金属为Ti、Ni、Cr、Co、Cu或其合金中的一种，所述过渡金属层厚度为10-100nm。
5.根据权利要求2或3所述的制备方法，其特征在于，所述步骤(3)中沉积负偏压为15V-150V，沉积电流为40-120A，束流强度为0.5-5A。
6.根据权利要求5所述的制备方法，其特征在于，所述步骤(4)中沉积金属层为Cu层，厚度为1-10μm。
7.根据权利要求6所述的制备方法，其特征在于，所述步骤(4)中沉积负偏压为0V-200V，沉积电流为40-120A，束流强度为0.5-5A，沉积温度100-150℃。
8.根据权利要求1所述的制备方法，其特征在于，所述步骤(1)中预处理为：将MPI薄膜去离子水超声清洗1-2小时，放入1-3mol/L NaOH溶液中室温浸泡15-60min，取出，用大量去离子水冲洗干净，烘干待用。
9.一种MPI覆铜板，其特征在于，根据权利要求1-8任一项所述的制备方法制备而成。
10.根据权利要求9所述的MPI覆铜板，其特征在于，所述金属层与MPI薄膜的剥离强度大于或等于0.7N/mm。
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