CN115210077A - 覆铜箔层压板用低介电复合膜及包括其的覆铜箔层压板 - Google Patents
覆铜箔层压板用低介电复合膜及包括其的覆铜箔层压板 Download PDFInfo
- Publication number
- CN115210077A CN115210077A CN202080097785.2A CN202080097785A CN115210077A CN 115210077 A CN115210077 A CN 115210077A CN 202080097785 A CN202080097785 A CN 202080097785A CN 115210077 A CN115210077 A CN 115210077A
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- CN
- China
- Prior art keywords
- polyimide
- low dielectric
- clad laminate
- composite film
- copper clad
- Prior art date
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Images
Classifications
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Abstract
本发明涉及用于覆铜箔层压板(CCL)的低介电复合膜，更具体地，涉及具有显着低的介电常数和介电损耗和优异的机械性能、还呈现显着低热膨胀系数效果的用于覆铜箔层压板的低介电复合膜及包括其的低介电覆铜箔层压板。
Description
技术领域
本发明涉及用于覆铜箔层压板(CCL)的低介电复合膜，更具体地，涉及具有显着低的介电常数和介电损耗和优异的机械性能、还呈现显着低热膨胀系数效果的用于覆铜箔层压板的低介电复合膜及包括其的低介电覆铜箔层压板。
背景技术
10秒下载1GB的时代，也就是说5G网络(5G Networks)时代正在开启。在国际消费者家用电器博览会2017(CES 2017)，英特尔宣布全球首款5G调制解调器，并预测基于千兆级速度，自动驾驶汽车、物联网、无线宽带等各个领域都会出现创新，如此，移动电信公司已经在转向第五代移动通信。国际电信联盟(ITU)于2015年10月召开无线电通信大会，将5G的正式技术名称定为“国际移动通信(International Mobile Telecommunication，IMT)-2020”。5G为“第五代移动通信(5th generation mobile communications)”的缩写。
根据国际电信联盟给出的定义，5G是最高下载速度为20Gbps，最低下载速度为100Mbps的移动通信技术。此外，能够为1km2半径内的100万台设备提供物联网(IoT)服务，即使在时速为500km的高速列车上也应该可以实现自由通信。5G下载速度比作为目前移动通信速度的300Mbps快70倍以上，比一般LTE快280倍。这是可以在10秒内下载1GB电影的速度。5G不仅仅关心传输速度。不仅传输速度，响应速度也显着提高。如果数据传输速度是一次可以通过多少数据的指标，响应速度就衡量小数据通过所需的时间。在4G，响应速度提高到10ms至50ms(毫秒，千分之一秒)。在5G，上述响应速度会更快10倍左右。得益于此，5G将被积极导入到必须与中央服务器之间不断收发大量数据的自动驾驶汽车和物联网领域中。
另一方面，与使用2GHz以下频率的4G不同，5G使用28GHz的超高频带频率。移动通信系统中发射和接收的信号是无线电波，目前正在建设中的5G使用3.5GHz和28GHz的高频段，与4G相比使用明显更高的高频段，因此，衍射特性比4G更低(直线度强)，电波到达距离短，由于这些通信特性，需要设置比4G更多的基站或中继器。
电信号具有随着频率增加，传输损耗增加的特性。在以往的低介电薄膜和覆铜箔层压板的情况下，无法达到所需水平的低介电常数和介电损耗，因此不能最小化或防止高频段的信号干扰，即使表现预定的低介电常数，也存在机械性能降低或热膨胀系数高的问题。
因此，迫切需要开发一种具有显着低的介电常数和介电损耗、优异的机械性能及显着低的热膨胀系数的材料。
发明内容
技术问题
本发明是鉴于上述问题而研制的，其目的在于提供具有显着低的介电常数和介电损耗和优异的机械性能、还呈现显着低热膨胀系数效果的用于覆铜箔层压板的低介电复合膜及包括其的低介电覆铜箔层压板。
解决问题的方案
为了解决上述问题，本发明提供一种用于覆铜箔层压板的低介电复合膜，该低介电复合膜包括芯层，上述芯层通过包括包含膨胀聚四氟乙烯(ePTFE)并具有多个气孔的多孔基材以及聚酰亚胺类化合物而形成，上述芯层包括填充在上述多孔基材的气孔中的聚酰亚胺类基体。
根据本发明的一实施例，相对于上述芯层的总重量，上述多孔基材的含量可以为20重量％至85重量％。
此外，相对于上述芯层的总体积，上述多孔基材的含量可以为15体积％至80体积％。
此外，上述芯层还可包括聚酰亚胺类层，上述聚酰亚胺类层设置在上述多孔基材的上表面和下表面中的至少一个表面上且来源于上述聚酰亚胺类基体。
并且，相对于上述芯层的总体积，上述聚酰亚胺类层的含量可以为8体积％至80体积％。
另外，上述多孔基材的MD方向的抗拉强度与TD方向的抗拉强度之比可以为1：0.4至1：2.5。
并且，上述聚酰亚胺类层的总厚度与上述多孔基材的厚度之比可以为1:0.2至1:12。
此外，上述芯层可以在上述多孔基材的上表面和下表面上分别包括第一聚酰亚胺类层和第二聚酰亚胺类层，上述第一聚酰亚胺类层和第二聚酰亚胺类层的厚度比可以为1:0.5至1:1.5。
此外，上述聚酰亚胺类基体的根据下述测量方法1测量的酰亚胺化率可以为90％以上。
[测量方法1]
将在380℃下酰亚胺化60分钟的基准样品的酰亚胺化率假定为100％，通过红外光谱仪对聚酰亚胺类基体的1,700㎝-1波长和1,615㎝-1波长处的峰大小进行测量后，根据下述数学式1计算PI指数，然后根据下述数学式2计算酰亚胺化率。
[数学式1]
PI指数＝1,700㎝-1波长处的峰面积(PI峰)/1,615㎝-1波长处的峰面积(PAA峰)
[数学式2]
酰亚胺化率(％)＝(聚酰亚胺类基体的PI指数/基准样品的PI指数)×100(％)
此外，可以在上述芯层的一面或两面上进一步包括粘合层。
此外，上述聚酰亚胺类基体可以通过对将二酐和二胺聚合形成的聚酰胺酸进行酰亚胺化而形成，上述二酐包括选自由BPDA(3,3’,4,4’-联苯四甲酸二酐(3,3’,4,4’-Biphenyltetracarboxylic dianhydride))、PMDA(均苯四酸二酐(Pyromelliticdianhydride))、ODPA(4,4’-氧双邻苯二甲酸酐(4,4’-oxydiphthalic anhydride))、BTDA(二苯甲酮-3,3’,4,4’-四羧酸二酐(3,3’,4,4’-benzophenone tetracarboxylicdianhydride))、BPADA(2,2-双[4-(3,4-二羧基苯氧基)苯基]丙烷二酐(2,2-Bis[4-(3,4-Dicarboxyphenoxy)Phenyl]Propane Dianhydride))、TAHQ(对-亚苯基-双苯偏三酸酯二酐(Ditricarboxylic anhydride hydroquinone ester))、6FDA(2,2-双-(3,4-二羧基苯基)六氟丙烷二酐(2,2-bis(3,4-anhydrodicarboxyphenyl)hexafluoropropane))、CBDA(环丁烷-1,2,3,4-四羧酸二酐(cyclobutane-1,2,3,4-tetracarboxylic dianhydride))及CHDA(1,2,4,5-环己烷四羧酸二酐(1,2,4,5-Cyclohexanetetracarboxylic Dianhydride))组成的组中的至少一种，上述二胺包括选自由pPDA(对苯二胺(paraphenylene diamine))、ODA(4,4’-氧二苯胺(4,4’-Oxydianiline))、TPE-R(1,3-双(4-氨基苯氧基)苯(1,3-Bis(4-aminophenoxy)benzene))、TPE-Q(1,4-双(4-氨基苯氧基)苯(1,4-Bis(4-aminophenoxy)benzene))、BAPP(2,2-双[4-(4-氨基苯氧基苯基)]丙烷(2,2-Bis[4-(4-aminophenoxy)Phenyl]Propane))、M-Tolidine(4,4’-二氨基-2,2’-二甲基联苯(2,2’-Dimethyl-4,4’-diaminobiphenyl))、O-Tolidine(4,4’-二氨基-3,3’-二甲基联苯(3,3’-Dimethyl-4,4’-diaminobiphenyl))、TFDB(2,2’-双三氟甲基-4,4’-二氨基联苯(2,2’-bis(trifluoromethyl)-[1,1’-biphenyl]-4,4’-diamine))及HFBAPP(2,2-双[4-(4-氨基苯氧基)苯基]六氟丙烷(2,2-Bis[4-(4-aminophenoxy)phenyl]hexafluoropropane))组成的组中的至少一种。
此外，相对于上述芯层和粘合层的总体积，上述粘合层的含量可以为2体积％至40体积％。
并且，上述聚酰亚胺类基体可以包括氟类颗粒和陶瓷颗粒中的至少一种。
并且，上述氟类颗粒可以包括选自由氟乙烯(PTFE)、全氟烷氧基共聚物(PFA，MFA，perfluoroalkoxy copolymer)、氟化乙烯丙烯共聚物(FEP，fluorinated ethylenepropylene copolymer)、乙烯-四氟乙烯共聚物(ETFE，ethylene tetrafluoroethylenecopolymer)及乙烯-氯三氟乙烯共聚物(ECTFE，ethylene chlorotrifluoroethylenecopolymer)组成的组中的至少一种。
并且，上述陶瓷颗粒可以为包括选自由B、Na、Mg、Al、Si、P、K、Ca及Ti组成的组中的至少一种元素的陶瓷颗粒。
并且，上述陶瓷颗粒可以包括中空陶瓷颗粒和非中空陶瓷颗粒中的至少一种。
此外，本发明提供一种低介电覆铜箔层压板，该低介电覆铜箔层压板包括：芯层，通过包括包含膨胀聚四氟乙烯并具有多个气孔的多孔基材以及聚酰亚胺类化合物而形成，上述芯层包括填充在上述多孔基材的气孔的聚酰亚胺类基体；铜箔，设置在上述芯层的一面或两面上；及粘合层，介于上述芯层和铜箔之间。
发明的效果
根据本发明的用于覆铜箔层压板的低介电复合膜及包括其的低介电覆铜箔层压板具有显着低的介电常数和介电损耗、优异的机械性能及显着低的热膨胀系数。
附图说明
图1为根据本发明的一实施例的用于覆铜箔层压板的低介电复合膜的剖面图，
图2为根据本发明的另一实施例的用于覆铜箔层压板的低介电复合膜的剖面图，
图3为根据本发明的一实施例的用于覆铜箔层压板的低介电覆铜箔层压板的剖面图。
具体实施方式
用于实施发明的最佳方式
以下，参照附图来对本发明的实施例进行详细说明，以使本发明所属技术领域的普通技术人员轻松实现本发明。本发明可通过多种不同的实施方式实现，并不限定于在本说明书中所说明的实施例。为了明确说明本发明，在附图中省略了与说明无关的部分，在说明书全文中，对于相同或相似的结构要素赋予相同的附图标记。
如图1和图2所示，根据本发明的低介电复合膜1000、1001包括芯层100，上述芯层100包括包含多个气孔的多孔基材10和填充在上述多孔基材的各气孔中的聚酰亚胺类基体。
上述多孔基材执行支撑低介电复合膜的功能，并执行表现低介电性能的功能，并且包括膨胀聚四氟乙烯。
上述多孔基材的MD方向的抗拉强度与TD方向的抗拉强度之比可以为1:0.4至1:2.5，优选第，MD方向的抗拉强度与TD方向的抗拉强度之比可以为1:0.8至1:1.7。若MD方向的抗拉强度与TD方向的抗拉强度之比小于1:0.4或大于1:2.5，则低介电复合膜可能由于对各个方向的收缩和应力差异而发生变形。
此外，上述聚酰亚胺类基体执行表现出低介电性能和降低热膨胀系数的功能。
如上所述，上述聚酰亚胺类基体部分地或完全地封闭上述多孔基材10的多个气孔，优选地，可以封闭上述多孔基材10的所有多个气孔。
另一方面，上述聚酰亚胺类基体可以通过对将二酐和二胺聚合形成的聚酰胺酸进行酰亚胺化而形成，上述二酐包括选自由BPDA(3,3’,4,4’-联苯四甲酸二酐(3,3’,4,4’-Biphenyltetracarboxylic dianhydride))、PMDA(均苯四酸二酐(Pyromelliticdianhydride))、ODPA(4,4’-氧双邻苯二甲酸酐(4,4’-oxydiphthalic anhydride))、BTDA(二苯甲酮-3,3’,4,4’-四羧酸二酐(3,3’,4,4’-benzophenone tetracarboxylicdianhydride))、BPADA(2,2-双[4-(3,4-二羧基苯氧基)苯基]丙烷二酐(2,2-Bis[4-(3,4-Dicarboxyphenoxy)Phenyl]Propane Dianhydride))、TAHQ(对-亚苯基-双苯偏三酸酯二酐(Ditricarboxylic anhydride hydroquinone ester))、6FDA(2,2-双-(3,4-二羧基苯基)六氟丙烷二酐(2,2-bis(3,4-anhydrodicarboxyphenyl)hexafluoropropane))、CBDA(环丁烷-1,2,3,4-四羧酸二酐(cyclobutane-1,2,3,4-tetracarboxylic dianhydride))及CHDA(1,2,4,5-环己烷四羧酸二酐(1,2,4,5-Cyclohexanetetracarboxylic Dianhydride))组成的组中的至少一种，上述二胺包括选自由pPDA(对苯二胺(paraphenylene diamine))、ODA(4,4’-氧二苯胺(4,4’-Oxydianiline))、TPE-R(1,3-双(4-氨基苯氧基)苯(1,3-Bis(4-aminophenoxy)benzene))、TPE-Q(1,4-双(4-氨基苯氧基)苯(1,4-Bis(4-aminophenoxy)benzene))、BAPP(2,2-双[4-(4-氨基苯氧基苯基)]丙烷(2,2-Bis[4-(4-aminophenoxy)Phenyl]Propane))、M-Tolidine(4,4’-二氨基-2,2’-二甲基联苯(2,2’-Dimethyl-4,4’-diaminobiphenyl))、O-Tolidine(4,4’-二氨基-3,3’-二甲基联苯(3,3’-Dimethyl-4,4’-diaminobiphenyl))、TFDB(2,2’-双三氟甲基-4,4’-二氨基联苯(2,2’-bis(trifluoromethyl)-[1,1’-biphenyl]-4,4’-diamine))及HFBAPP(2,2-双[4-(4-氨基苯氧基)苯基]六氟丙烷(2,2-Bis[4-(4-aminophenoxy)phenyl]hexafluoropropane))组成的组中的至少一种，优选地，上述二酐包括选自由BPDA(3,3’,4,4’-联苯四甲酸二酐(3,3’,4,4’-Biphenyltetracarboxylic dianhydride))、PMDA(均苯四酸二酐(Pyromelliticdianhydride))、ODPA(4,4’-氧双邻苯二甲酸酐(4,4’-oxydiphthalic anhydride))、BTDA(二苯甲酮-3,3’,4,4’-四羧酸二酐(3,3’,4,4’-benzophenone tetracarboxylicdianhydride))及6FDA(2,2-双-(3,4-二羧基苯基)六氟丙烷二酐(2,2-bis(3,4-anhydrodicarboxyphenyl)hexafluoropropane))组成的组中的至少一种，上述二胺包括选自由pPDA(对苯二胺(paraphenylene diamine))、ODA(4,4’-氧二苯胺(4,4’-Oxydianiline))及TFDB(2,2’-双三氟甲基-4,4’-二氨基联苯(2,2’-bis(trifluoromethyl)-[1,1’-biphenyl]-4,4’-diamine))组成的组中的至少一种。
另一方面，上述聚合可以在包括选自由DMF(N,N-二甲基甲酰胺(N,N-dimethylformamide))、DMAc(N,N-二甲基乙酰胺(N,N-dimethylacetamide))、NMP(1-甲基-2-吡咯烷酮(1-methyl-2-pyrrolidone)、NEP(N-乙基-2-吡咯烷酮(N-ethyl-2-pyrrolidone))、GBL(γ-丁内酯(γ-butyrolactone))、GVL(γ-戊内酯(γ-valerolactone))、DVL(δ-戊内酯(δ-valerolactone))、碳酸亚乙酯(Ethylenecarbonate)、碳酸亚丙酯(Propylene carbonate)、间甲酚(m-cresol)、对甲酚(p-cresol)、苯乙酮(Acetophenone)、THF(四氢呋喃(Tetrahydrofuran))、二甲氧基乙烷、二乙氧基乙烷、二丁醚、二甘醇二甲醚、甲基异丁基酮、二异丁基酮、环己酮、甲基乙基酮、丙酮、丁醇、乙醇、二甲苯、甲苯及氯苯组成的组中的至少一种的溶剂下进行。
具体而言，可以通过下面将描述的方法来形成上述聚酰亚胺类基体。此时，以使用BPDA和PMDA作为上述二酐、使用pPDA和ODA作为二胺的例子来说明下面将描述的方法。
首先，在室温和氮气氛下，将pPDA和ODA完全溶解在用于一般聚酰亚胺聚合的极性非质子溶剂中，在15分钟至45分钟内加入在两种酸二酐中的BPDA。将上述溶液搅拌5分钟至15分钟后，在15分钟至45分钟内加入PMDA。之后，在0℃至60℃的反应温度下进行反应8小时至24小时，以制备聚酰胺酸溶液。此时，上述聚酰胺酸溶液的固含量可以为5重量％至25重量％，优选地，固含量可以为10重量％至20重量％，上述聚酰胺酸溶液在25℃下的粘度可以为2000cps至5000cps，优选地，粘度可以为2500cps至4500cps。用预定的过滤器对上述聚酰胺酸溶液进行过滤，制备浸渍溶液。之后，将多孔基材浸渍于浸渍溶液中，使得上述多孔基材内部的所有气孔被上述浸渍溶液堵塞，然后先在65℃至95℃下进行一次干燥1分钟至10分钟，然后在100℃至140℃下进行二次干燥5分钟至15分钟，以除去溶剂，从而制备包括多孔基材和聚酰胺酸的复合膜，上述聚酰胺酸被包含在上述多孔基材的气孔和两面。最后，通过在170℃至260℃下进行一次热处理且在240℃至360℃下进行二次热处理，将聚酰胺酸酰亚胺化，从而可以制备包含多孔基材10和聚酰亚胺类基体的低介电复合膜1000、1001。此时，为了使膜的抽缩和卷曲(curl)的发生最小化，可以通过拉幅机(辊拉伸机)设备在横向(TD)拉伸条件下进行热处理。
另一方面，相对于上述芯层100的总重量，上述多孔基材10的含量可以为20重量％至85重量％，优选地，可以为60重量％80重量％。若相对于上述芯层的总重量，上述多孔基材的含量小于20重量％，则低介电复合膜和低介电覆铜箔层压板的介电常数和介电损耗增加，难以用作5G高频用基板材料，若上述多孔基材的含量超过85重量％，则可能会出现机械强度降低的问题。
此外，相对于上述芯层100的总体积，上述多孔基材10的含量可以为15体积％至80体积％，优选地，可以为50体积％至75体积％。若相对于上述芯层的总体积，上述多孔基材的含量小于15体积％，则可能会发生介电常数和介电损耗增加的问题，若上述多孔基材的含量超过80体积％，则可能会出现机械强度降低的问题。
另一方面，上述芯层100还可包括聚酰亚胺类层20a、20b，上述聚酰亚胺类层20a、20b设置在上述多孔基材10的上表面和下表面中的至少一个表面上且来源于上述聚酰亚胺类基体。
此时，由于上述聚酰亚胺类层来源于上述聚酰亚胺类基体，因此它可以通过包含与上述聚酰亚胺类基体的聚酰亚胺类化合物相同的化合物来形成。
另一方面，相对于上述芯层100的总体积，上述聚酰亚胺类层20a、20b的含量可以为8体积％至80体积％，优选地，可以为10体积％至40体积％。若相对于上述多孔基材和聚酰亚胺类基体的总体积，上述聚酰亚胺类层的含量小于8体积％，则可能会发生机械强度降低的问题，若上述含量超过80体积％，则可能会发生介电常数和介电损耗增加的问题。
此外，上述聚酰亚胺类层20a、20b的总厚度与上述多孔基材10的厚度之间的厚度比可以为1:0.2至1:12，优选地，厚度比可以为1:4至1:11.5。若上述聚酰亚胺类层的总厚度与上述多孔基材的厚度之间的厚度比小于1:0.2，则可能会发生介电常数和介电损耗增加的问题，若上述厚度比超过1:12，则可能会出现机械强度降低的问题。
另一方面，如图1和图2所示，在上述芯层100中，在上述多孔基材10的上表面和下表面上可以分别包括第一聚酰亚胺类层20a和第二聚酰亚胺类层20b。具体而言，在上述多孔基材10的上表面上可以包括上述第一聚酰亚胺类层20a，在上述多孔基材10的下表面上可以包括上述第二聚酰亚胺类层20b。
此时，上述第一聚酰亚胺类层20a与第二聚酰亚胺类层20b的厚度比可以为1:0.5至1:1.5，优选地，厚度比可以为1:0.7至1:1.3。若上述厚度比超出上述范围，则发生层间应力不均匀，导致复合膜和/或覆铜箔层压板发生卷曲，并且可能由于过度的内应力而发生变形。
另一方面，上述聚酰亚胺类基体的根据下述测量方法1测量的酰亚胺化率可以为90％以上，优选地，根据下述测量方法1测量的酰亚胺化率可以为95％以上。
[测量方法1]
将在380℃下酰亚胺化60分钟的基准样品的酰亚胺化率假定为100％，通过红外光谱仪对聚酰亚胺类基体的1,700㎝-1波长和1,615㎝-1波长处的峰大小进行测量后，根据下述数学式1计算PI指数，然后根据下述数学式2计算酰亚胺化率。
[数学式1]
PI指数＝1,700㎝-1波长处的峰面积(PI峰)/1,615㎝-1波长处的峰面积(PAA峰)
[数学式2]
酰亚胺化率(％)＝(聚酰亚胺类基体的PI指数/基准样品的PI指数)×100(％)
若根据上述测量方法1测量的酰亚胺化率小于90％，则介电常数和介电损耗可能会增加，且会出现热膨胀系数增加的问题。
此时，上述PI指数可以根据下述数学式3计算，但本发明不限于此。
[数学式3]
PI指数＝1,700㎝-1波长处的峰面积(PI峰)/1,510㎝-1波长处的峰面积(PI，PAA峰)
另一方面，如图2所示，根据本发明的一实施例的低介电复合膜1001在上述芯层100的一面或两面上还可包括粘合层200。
上述粘合层200执行将下面将描述的覆铜箔层压板所具备的铜箔固定在低介电复合膜上的功能。作为上述粘合层，只要是由本领域中可常用的粘合层材料形成的粘合层，就可以不受限制地应用，优选地，可以为选自由环氧类粘合层、热塑性聚酰亚胺类粘合层、有机硅类粘合层及丙烯酸类粘合层组成的组中的至少一种粘合层。
另一方面，相对于上述芯层100和粘合层200的总体积，上述粘合层200的含量可以为2体积％至40体积％，优选地，可以为4体积％至30体积％。若相对于上述芯层100和粘合层200的总体积，上述粘合层200的含量小于2体积％，则铜箔与聚酰亚胺类基体之间的粘合力不足，导致在低介电覆铜箔层压板中发生层间剥离现象，机械性能降低，若粘合层的含量大于40体积％，则可能会出现介电常数和介电损耗增加的问题。
另一方面，根据本发明的另一实施例，上述聚酰亚胺类基体可以包括氟类颗粒和陶瓷颗粒中的至少一种。
作为上述氟类颗粒，只要是在本领域中可常用的氟类颗粒，就可以不受限制地使用，优选地，上述氟类颗粒可以包括选自由氟乙烯(PTFE)、全氟烷氧基共聚物(PFA，MFA，perfluoroalkoxy copolymer)、氟化乙烯丙烯共聚物(FEP，fluorinated ethylenepropylene copolymer)、乙烯-四氟乙烯共聚物(ETFE，ethylene tetrafluoroethylenecopolymer)及乙烯-氯三氟乙烯共聚物(ECTFE，ethylene chlorotrifluoroethylenecopolymer)组成的组中的至少一种。
此外，作为上述陶瓷颗粒，只要是在本领域中可常用的陶瓷颗粒，就可以不受限制地使用，优选地，上述陶瓷颗粒可以包括选自由B、Na、Mg、Al、Si、P、K、Ca及Ti组成的组中的至少一种元素。在这种情况下，上述陶瓷颗粒的组成可以包括上述元素，且包括上述元素的方法可以根据目的而变化，例如通过在表面掺杂上述元素而形成等，在本发明中对此没有特别限制。
并且，上述陶瓷颗粒可以包括包含中空部的中空陶瓷颗粒和非中空颗粒状的陶瓷颗粒中的至少一种。
另一方面，根据上述氟类颗粒和/或陶瓷颗粒的大小，包含在上述多孔基材内部的聚酰亚胺类基体中不存在上述颗粒，而可以仅在聚酰亚胺层存在上述颗粒，但本发明不限于此。
如图3所示，根据本发明的低介电覆铜箔层压板2000包括：芯层100，包括：多孔基材10，具有多个气孔；及聚酰亚胺类基体，填充在上述多孔基材的气孔中；铜箔300，设置在上述芯层100的一面或两面上；及粘合层200，介于上述芯层和铜箔之间。
上述铜箔300可以是具有本领域常用的已知规格的铜箔，在本发明中对此没有特别限制。
用于实施发明的方式
将通过以下实施例更详细说明本发明，但以下实施例不应解释为限制本发明的范围，而应解释为有助于理解本发明。
[实施例]
<实施例1：用于覆铜箔层压板的低介电复合膜的制备>
首先，在氮气气氛下，将pPDA和ODA加入到作为聚合溶剂的DMAc中，在室温下完全溶解，然后在30分钟内加入BPDA。搅拌上述溶液10分钟后，在30分钟内加入PMDA。之后，通过在20℃以下的温度下进行反应16小时来制备聚酰胺酸溶液。由此得到固含量为15重量％、在25℃下粘度为3500cps的聚酰胺酸溶液，然后用韩国Chungsoo Technofil公司的MINIFLOW过滤器(CTS-CAP10 A级)进行过滤，最后制备固含量为15重量％的浸渍溶液。
之后，将作为厚度为40μm的膨胀聚四氟乙烯的包括多个气孔的多孔基材浸渍到在上面制备的浸渍溶液中，以堵塞多孔基材的所有多个气孔，然后，为了去除溶剂，在80℃的温度下进行一次干燥5分钟，在120℃的温度下进行二次干燥10分钟。此时，上述多孔基材的MD方向的抗拉强度为30MPa，TD方向的抗拉强度为25MPa，MD方向的抗拉强度与TD方向的抗拉强度之比为1：0.8。
此后，通过在250℃的温度下进行一次热处理10分钟且在350℃的温度下进行二次热处理5分钟来使聚酰胺酸酰亚胺化，从而制备如图1所示的包括多孔基材和聚酰亚胺类基体的低介电复合膜。此时，为了使膜的抽缩和卷曲的发生最小化，通过拉幅机(辊拉伸机)设备在横向拉伸条件下进行热处理。
在制备的低介电复合膜中，第一聚酰亚胺类层和第二聚酰亚胺类层的厚度分别为5μm，相对于制备的低介电复合膜的总重量，多孔基材的含量为73重量％，相对于制备的低介电复合膜的总体积，多孔基材的含量为64体积％，聚酰亚胺类层的含量为25体积％。此外，在所制备的低介电复合膜中，根据下述测量方法1测量的聚酰亚胺类基体的酰亚胺化率为98％。
[测量方法1]
使用傅里叶变换红外光谱(FT-IR)分析酰亚胺化率，将在380℃下酰亚胺化60分钟的基准样品的酰亚胺化率假定为100％，通过红外光谱仪对聚酰亚胺类基体的1,700㎝-1波长和1,615㎝-1波长处的峰大小进行测量后，根据下述数学式1计算PI指数，然后根据下述数学式2计算酰亚胺化率。
[数学式1]
PI指数＝1,700㎝-1波长处的峰面积(PI峰)/1,615㎝-1波长处的峰面积(PAA峰)
[数学式2]
酰亚胺化率(％)＝(聚酰亚胺类基体的PI指数/基准样品的PI指数)×100(％)
<实施例2至13及比较例1至2>
除了改变多孔基材的重量百分比、体积百分比、聚酰亚胺类层的体积百分比、聚酰亚胺类层的总厚度和多孔基材的厚度之间的厚度比、聚酰亚胺类基体的酰亚胺化率、是否包含多孔基材以及是否包含聚酰亚胺类基体等之外，其余以与实施例1相同的方法进行制备，从而制备出如表1至表3所示的低介电复合膜。
<实验例1>
对于根据实施例和比较例制备的各个低介电复合膜的以下物理性能进行评价，将其结果示于表1至表3中。
1.介电常数和介电损耗测量
对于各个低介电复合膜，使用网络分析仪(E8364A(45MHz～50GHz)，美国安捷伦科技公司(Agilent Technologies，Inc.))来通过谐振腔(Resonant cavity)测量薄膜型样品的千兆赫(GHz)区域的介电常数和介电损耗。
2.机械性能评价
对于各个低介电复合膜，使用万能试验机(Universal Testing Machine，UTM)根据ASTM-D882标准测量抗张强度。
3.热膨胀系数测量
对于各个低介电复合膜，使用热机械分析仪(Pyris Diamond TMA，美国珀金埃尔默仪器公司(Perkin Elmer instrument))测量热膨胀系数。在30℃至400℃范围的温度下，在氮气流下以10℃/分钟的升温条件进行测量，然后计算出在50℃至250℃之间的平均值。
表1
表2
表3
从上述表1至表3可以看出，都满足根据本发明的多孔基材的重量百分比、体积百分比、聚酰亚胺类层的体积百分比、聚酰亚胺类层的总厚度和多孔基材的厚度之间的厚度比、聚酰亚胺类基体的酰亚胺化率、是否包含多孔基材以及是否包含聚酰亚胺类基体等条件的实施例1、3、4、8、11及12与不满足其中至少一个条件的实施例2、5、6、7、9、10、13及比较例1至2相比，介电常数和介电损耗显着低，机械性能优异，同时表现出热膨胀系数低的效果。
另一方面，比较例2的热膨胀系数过高，无法进行测量。
<实施例14至19>
除了将实施例1的作为二酐的BPDA和PMDA改变为BPDA和ODPA(实施例14)、BPDA和BTDA(实施例15)、BPDA和6FDA(实施例16)、PMDA和ODPA(实施例17)、PMDA和BTDA(实施例18)、PMDA和6FDA(实施例19)之外，其余以与实施例1相同的方法制备低介电复合膜。
<实施例20至21>
除了将实施例1的作为二胺的pPDA和ODA改变为pPDA和TFDB(实施例20)、ODA和TFDB(实施例21)之外，其余以与实施例1相同的方法制备低介电复合膜。
<实施例22至24>
除了将实施例1的作为二酐的BPDA和PMDA改变为6FDA(实施例22)、ODPA(实施例23)、BTDA(实施例24)并分别单独应用来制备聚酰胺酸之外，其余以与实施例1相同的方法制备低介电复合膜。
<实施例25至26>
除了将实施例1的作为二胺的pPDA和ODA分别改为TFDB(实施例25)、BAPP(实施例26)并分别单独应用来制备聚酰胺酸之外，其余以与实施例1相同的方法制备低介电复合膜。
<实验例2>
对于根据实施例14至26制备的各个低介电复合膜的以下物理性能进行评价，将其结果示于表4和表5中。
1.介电常数和介电损耗测量
对于各个低介电复合膜，使用网络分析仪(E8364A(45MHz～50GHz)，美国安捷伦科技公司(Agilent Technologies，Inc.))来通过谐振腔测量薄膜型样品的千兆赫区域的介电常数和介电损耗。
2.机械性能评价
对于各个低介电复合膜，使用万能试验机(Universal Testing Machine，UTM)根据ASTM-D882标准测量抗张强度。
3.热膨胀系数测量
对于各个低介电复合膜，使用热机械分析仪(Pyris Diamond TMA，美国珀金埃尔默仪器公司(Perkin Elmer instrument))测量热膨胀系数。在30℃至400℃范围的温度下，在氮气流下以10℃/分钟的升温条件进行测量，然后计算出在50℃至250℃之间的平均值。
表4
表5
从上述表4和表5可以看出，满足根据本发明的二酐和二胺类型的实施例14至21与不满足它们的实施例22至26相比具有显着低的介电常数和介电损耗，且同时表现出优异的机械性能和低热膨胀系数的效果。
<制备例1>
在根据实施例1制备的低介电复合膜的上表面上涂布含有潜伏性固化剂和丙烯酸树脂的单液型环氧溶液，然后在100℃的温度下干燥，以制备包括厚度为6μm的粘合层的低介电复合膜。其中，相对于100重量份的单液型环氧树脂，包括10重量份的作为潜在固化剂的双氰胺(dicyandiamide，DICY)和丙烯酸树脂。此时，相对于所制备的低介电复合膜的总体积，粘合层的含量为6体积％。
<制备例2至6>
除了改变相对于低介电复合膜的总体积的粘合层的体积百分比之外，其余以与制备例1相同的方式制备如下表6所示的低介电复合膜。
<实验例3>
对于根据上述制备例1至6制备的低介电复合膜的以下物理性能进行评价，将其结果示于下表6中。
1.介电常数和介电损耗测量
对于各个低介电复合膜，使用网络分析仪(E8364A(45MHz～50GHz)，美国安捷伦科技公司(Agilent Technologies，Inc.))来通过谐振腔测量薄膜型样品的千兆赫区域的介电常数和介电损耗。
2.粘合强度测量
对于根据制备例的各个低介电复合膜，根据IPC-TM-650 2.4.9.1的评价规格，对在沿90度方向拉起时铜层剥离的时间点进行测量和评价。
表6
从上述表6可以看出，满足根据本发明的粘合层的体积百分比和聚酰亚胺类层的体积百分比的制备例1、3及4与不满足它们的制备例2、6相比同时表现出介电常数和介电损耗显著低且粘合强度优异的效果。
如上对本发明的一实施例进行说明，但本发明的主旨并不限于本发明中的实施例，本领域的技术人员在相同主旨范围内，可通过对构成要件的附加、修改、删除、增加等容易地提出其它实施例，而这些属于本发明的主旨范围。
Claims (17)
1.一种用于覆铜箔层压板的低介电复合膜，其特征在于，包括芯层，上述芯层通过包括包含膨胀聚四氟乙烯并具有多个气孔的多孔基材以及聚酰亚胺类化合物而形成，上述芯层包括填充在上述多孔基材的气孔中的聚酰亚胺类基体。
2.根据权利要求1所述的用于覆铜箔层压板的低介电复合膜，其特征在于，相对于上述芯层的总重量，上述多孔基材的含量为20重量％至85重量％。
3.根据权利要求1所述的用于覆铜箔层压板的低介电复合膜，其特征在于，相对于上述芯层的总体积，上述多孔基材的含量为15体积％至80体积％。
4.根据权利要求1所述的用于覆铜箔层压板的低介电复合膜，其特征在于，上述芯层还包括聚酰亚胺类层，上述聚酰亚胺类层设置在上述多孔基材的上表面和下表面中的至少一个表面上且来源于上述聚酰亚胺类基体。
5.根据权利要求4所述的用于覆铜箔层压板的低介电复合膜，其特征在于，相对于上述芯层的总体积，上述聚酰亚胺类层的含量为8体积％至80体积％。
6.根据权利要求1所述的用于覆铜箔层压板的低介电复合膜，其特征在于，上述多孔基材的MD方向的抗拉强度与TD方向的抗拉强度之比为1：0.4至1：2.5。
7.根据权利要求4所述的用于覆铜箔层压板的低介电复合膜，其特征在于，上述聚酰亚胺类层的总厚度与上述多孔基材的厚度之比为1:0.2至1:12。
8.根据权利要求4所述的用于覆铜箔层压板的低介电复合膜，其特征在于，上述芯层在上述多孔基材的上表面和下表面上分别包括第一聚酰亚胺类层和第二聚酰亚胺类层，上述第一聚酰亚胺类层和第二聚酰亚胺类层的厚度比为1:0.5至1:1.5。
9.根据权利要求1所述的用于覆铜箔层压板的低介电复合膜，其特征在于，上述聚酰亚胺类基体的根据下述测量方法1测量的酰亚胺化率为90％以上：
[测量方法1]
将在380℃下酰亚胺化60分钟的基准样品的酰亚胺化率假定为100％，通过红外光谱仪对聚酰亚胺类基体的1,700cm-1波长和1,615cm-1波长处的峰大小进行测量后，根据下述数学式1计算PI指数，然后根据下述数学式2计算酰亚胺化率：
[数学式1]
PI指数＝1,700cm-1波长处的峰面积(PI峰)/1,615cm-1波长处的峰面积(PAA峰)
[数学式2]
酰亚胺化率(％)＝(聚酰亚胺类基体的PI指数/基准样品的PI指数)×100(％)。
10.根据权利要求1所述的用于覆铜箔层压板的低介电复合膜，其特征在于，在上述芯层的一面或两面上进一步包括粘合层。
11.根据权利要求1所述的用于覆铜箔层压板的低介电复合膜，其特征在于，上述聚酰亚胺类基体通过对将二酐和二胺聚合形成的聚酰胺酸进行酰亚胺化而形成，
上述二酐包括选自由3,3’,4,4’-联苯四甲酸二酐、均苯四酸二酐、4,4’-氧双邻苯二甲酸酐、二苯甲酮-3,3’,4,4’-四羧酸二酐、2,2-双[4-(3,4-二羧基苯氧基)苯基]丙烷二酐、对-亚苯基-双苯偏三酸酯二酐、2,2-双-(3,4-二羧基苯基)六氟丙烷二酐、环丁烷-1,2,3,4-四羧酸二酐及1,2,4,5-环己烷四羧酸二酐组成的组中的至少一种，
上述二胺包括选自由对苯二胺、4,4’-氧二苯胺、1,3-双(4-氨基苯氧基)苯、1,4-双(4-氨基苯氧基)苯、2,2-双[4-(4-氨基苯氧基苯基)]丙烷、4,4’-二氨基-2,2’-二甲基联苯、4,4’-二氨基-3,3’-二甲基联苯、2,2’-双三氟甲基-4,4’-二氨基联苯及2,2-双[4-(4-氨基苯氧基)苯基]六氟丙烷组成的组中的至少一种。
12.根据权利要求10所述的用于覆铜箔层压板的低介电复合膜，其特征在于，相对于上述芯层和粘合层的总体积，上述粘合层的含量为2体积％至40体积％。
13.根据权利要求4所述的用于覆铜箔层压板的低介电复合膜，其特征在于，上述聚酰亚胺类基体包括氟类颗粒和陶瓷颗粒中的至少一种。
14.根据权利要求13所述的用于覆铜箔层压板的低介电复合膜，其特征在于，上述氟类颗粒包括选自由氟乙烯、全氟烷氧基共聚物、氟化乙烯丙烯共聚物、乙烯-四氟乙烯共聚物及乙烯-氯三氟乙烯共聚物组成的组中的至少一种。
15.根据权利要求13所述的用于覆铜箔层压板的低介电复合膜，其特征在于，上述陶瓷颗粒为包括选自由B、Na、Mg、Al、Si、P、K、Ca及Ti组成的组中的至少一种元素的陶瓷颗粒。
16.根据权利要求13所述的用于覆铜箔层压板的低介电复合膜，其特征在于，上述陶瓷颗粒包括中空陶瓷颗粒和非中空陶瓷颗粒中的至少一种。
17.一种低介电覆铜箔层压板，其特征在于，包括：
芯层，通过包括包含膨胀聚四氟乙烯并具有多个气孔的多孔基材以及聚酰亚胺类化合物而形成，上述芯层包括填充在上述多孔基材的气孔的聚酰亚胺类基体；
铜箔，设置在上述芯层的一面或两面上；及
粘合层，介于上述芯层和铜箔之间。
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|---|---|---|---|
| KR1020200115972A KR102268708B1 (ko) | 2020-09-10 | 2020-09-10 | 동박적층판(ccl)용 저유전 복합필름 및 이를 포함하는 저유전 동박적층판(ccl) |
| KR10-2020-0115972 | 2020-09-10 | ||
| PCT/KR2020/016692 WO2022055028A1 (ko) | 2020-09-10 | 2020-11-24 | 동박적층판(ccl)용 저유전 복합필름 및 이를 포함하는 저유전 동박적층판(ccl) |
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| EP (1) | EP4212336A1 (zh) |
| JP (1) | JP7465365B2 (zh) |
| KR (1) | KR102268708B1 (zh) |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024117799A1 (ko) * | 2022-11-30 | 2024-06-06 | 피아이첨단소재 주식회사 | 블렌딩된 폴리이미드 필름 및 이의 제조방법 |
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| Publication number | Publication date |
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| JP2023518535A (ja) | 2023-05-02 |
| JP7465365B2 (ja) | 2024-04-10 |
| KR102268708B1 (ko) | 2021-06-25 |
| EP4212336A1 (en) | 2023-07-19 |
| WO2022055028A1 (ko) | 2022-03-17 |
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