CN116970275A - 树脂组合物、半固化片及其制备方法、覆铜板及其制备方法和印制电路板 - Google Patents
树脂组合物、半固化片及其制备方法、覆铜板及其制备方法和印制电路板 Download PDFInfo
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- CN116970275A CN116970275A CN202310541199.8A CN202310541199A CN116970275A CN 116970275 A CN116970275 A CN 116970275A CN 202310541199 A CN202310541199 A CN 202310541199A CN 116970275 A CN116970275 A CN 116970275A
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- Prior art keywords
- prepreg
- copper
- clad plate
- parts
- resin composition
- Prior art date
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Landscapes
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- Laminated Bodies (AREA)
Abstract
本申请实施例涉及覆铜板技术领域,尤其是涉及一种树脂组合物、半固化片及其制备方法、覆铜板及其制备方法和印制电路板。树脂组合物包括氰酸酯80‑200份、双马来酰亚胺20‑80份、二烯丙基双酚A5‑50份、固化催化剂0.1‑5份、硅烷偶联剂0.1‑1份、硅微粉100‑300份、勃姆石10‑80份和含磷阻燃剂10‑80份。将氰酸酯和双马来酰亚胺复配使用可以提高半固化片的耐热性能、降低半固化片的介电常数和介电损耗。二烯丙基双酚A用于提高氰酸酯/双马来酰亚胺树脂体系的韧性。固化催化剂用于提高氰酸酯/双马来酰亚胺树脂体系的固化效率。硅微粉用于降低半固化片的介电常数和介电损耗。勃姆石和含磷阻燃剂用于提高半固化片的阻燃性能。
Description
技术领域
本申请实施例涉及覆铜板技术领域,尤其是涉及一种树脂组合物、半固化片及其制备方法、覆铜板及其制备方法和印制电路板。
背景技术
由于电子设备的高频化发展,覆铜板必须具有更低的介电常数才能满足高频化的要求。此外,如军事领域,还对覆铜板提出了重量更轻、力学性能更好等特殊要求。
现有技术的高频覆铜板大部分由增强纤维对热固性树脂进行增强而得到。目前能够用于高频覆铜板制造的树脂材料主要有聚四氟乙烯树脂、环氧树脂、氰酸酯树脂等。可以发现,聚四氟乙烯基覆铜板成型工艺复杂、所得覆铜板密度大、力学性能差;而普通环氧树脂基覆铜板由于介质损耗较大,不能满足高频数据传输要求,必须选用适合的材料并进行改性以降低覆铜板的介质损耗。
发明内容
为了改善覆铜板的介电性能,本申请实施例提供一种树脂组合物、半固化片及其制备方法、覆铜板及其制备方法和印制电路板,能够使覆铜板具有较低的介电损耗。
在本申请的第一方面,提供了一种树脂组合物,按照重量份计,所述树脂组合物包括以下组分:氰酸酯80-200份;双马来酰亚胺20-80份;二烯丙基双酚A5-50份;固化催化剂0.1-5份;硅烷偶联剂0.1-1份;硅微粉100-300份;勃姆石10-80份;含磷阻燃剂10-80份。
在本申请的实施例中,将氰酸酯和双马来酰亚胺复配使用可以提高半固化片的耐热性能、降低半固化片的介电常数和介电损耗。二烯丙基双酚A用于提高氰酸酯/双马来酰亚胺树脂体系的韧性。固化催化剂用于提高氰酸酯/双马来酰亚胺树脂体系的固化效率。硅微粉用于降低半固化片的介电常数和介电损耗。勃姆石和含磷阻燃剂用于提高半固化片的阻燃性能。本申请实施例提供的半固化片和覆铜板不但具有较低的介电常数和较低的介电损耗,还具有良好的耐热性能和无卤阻燃性能。
在一些实施例中,所述氰酸酯为双酚A型氰酸酯,所述双马来酰亚胺为二苯甲烷双马来酰亚胺。
在一些实施例中,所述固化催化剂为二月桂酸二丁基锡。
在一些实施例中,按照重量份计,所述树脂组合物还包括:有机溶剂100-200份。
在本申请的第二方面,还提供了一种半固化片,所述半固化片包括增强材料和包覆所述增强材料的树脂层,所述树脂层的原材料为第一方面所述的树脂组合物。
在一些实施例中,所述增强材料为玻璃纤维布。
在本申请的第三方面,还提供了一种半固化片的制备方法,所述方法包括以下步骤:取第一方面所述的树脂组合物;将增强材料浸渍在所述树脂组合物中;加热浸渍后的所述增强材料,以使所述增强材料上的所述树脂组合物半固化,从而形成所述半固化片。
在本申请的第四方面,还提供了一种覆铜板,所述覆铜板包括第二方面所述的半固化片和设置于所述半固化片单面或双面的导电金属片。
在本申请的第五方面,还提供了一种覆铜板的制备方法,所述方法包括:将第二方面所述的半固化片的单面或双面覆上导电金属片,将所述半固化片和所述导电金属片压合成型,从而形成所述覆铜板。
在本申请的第六方面,还提供一种印制电路板,所述印制电路板包括第四方面所述的覆铜板和设置于所述覆铜板的电子元件。
应当理解,发明内容部分中所描述的内容并非旨在限定本公开的关键或重要特征,亦非用于限制本公开的范围。本公开的其他特征通过以下的描述将变得容易理解。
附图说明
为了更清楚地说明本发明实施例的技术方案,下面将对本发明实施例中所需要使用的附图作简单地介绍。显而易见地,下面所描述的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1是实施例1的热膨胀系数测试结果图;
图2是实施例2的热膨胀系数测试结果图;
图3是实施例1的玻璃化转变温度测试结果图;
图4是实施例2的玻璃化转变温度测试结果图。
具体实施方式
下文将参考附图中示出的若干示例性实施例来描述本公开的原理和精神。应当理解,描述这些具体的实施例仅是为了使本领域的技术人员能够更好地理解并实现本公开,而并非以任何方式限制本公开的范围。在以下描述和权利要求中,除非另有定义,否则本文中使用的所有技术和科学术语具有与所属领域的普通技术人员通常所理解的含义。
如本文所使用的,术语“包括”及其类似用语应当理解为开放性包含,即“包括但不限于”。术语“基于”应当理解为“至少部分地基于”。术语“一个实施例”或“该实施例”应当理解为“至少一个实施例”。术语“第一”、“第二”等等可以指代不同的或相同的对象,并且仅用于区分所指代的对象,而不暗示所指代的对象的特定空间顺序、时间顺序、重要性顺序。
覆铜箔层压板(Copper Clad Laminate,CCL)是将电子玻纤布或其它增强材料浸以树脂,一面或双面覆以铜箔并经热压而制成的一种板状材料,简称为覆铜板。各种不同形式、不同功能的印制电路板,都是在覆铜板上有选择地进行加工、蚀刻、钻孔及镀铜等工序,制成不同的印制电路。对印制电路板主要起互连导通、绝缘和支撑的作用,对电路中信号的传输速度、能量损失和特性阻抗等有很大的影响,因此,印制电路板的性能、品质、制造中的加工性、制造水平、制造成本以及长期的可靠性及稳定性在很大程度上取决于覆铜板。
传统的覆铜板主要是用来制造印制电路板,以对电子元器件起到支撑和互相连接、互相绝缘的作用,被称为印制电路板的重要基础材料。它是所有电子整机,包括航空、航天、遥感、遥测、遥控、通讯、计算机、工业控制、家用电器、甚至高级儿童玩具等等一切电子产品,都不可缺少的重要电子材料。随着科技水平的不断提高,近年来有些特种电子覆铜板也用来直接制造印制电子元件。
由于电子产品的小型、轻量及薄型化,迫使印制电路板必须具备各种高质量、高技术特性,使印制电路板制造技术直接涉及到当代多种高新技术,其主要、最重要的材料——覆铜板,也就必须随之具备各种高质量和高技术特性。
随着半导体器件的高度集成以及封装工艺的精细化,印制电路板线路的高密度化,连接和安装技术的进步,电子器件显著地向小型化、高频化、高速数字化、高可靠性的方向发展,特别是应用在高频的移动通讯领域。作为电子器件基材的印制电路板,近期有向多层化、超细化线路的趋势发展,从而信号的传输速度必须越来越快,信号的频率也越来越高,因此这也要求作为信号传输载体的印制电路板材料必须降低其介电常数,同时材料的介电损耗因子也要足够低,从而使信号在传输过程中的损耗较小。原来常规的FR-4覆铜板一直使用环氧树脂作为主体树脂,但环氧树脂的介电性能已不能满足要求,因此需使用替代环氧体系的材料。
另一方面,之前一直作为印制电路板主要阻燃材料的具有良好阻燃效果的含卤素化合物因其对环境影响较大,并且各国对环境要求越来越高,已有不少卤素阻燃阻燃剂被禁止使用,因此为避免使用该种对环境有害的卤素阻燃剂,开发并使用无卤素并具有良好阻燃效果的环保阻燃剂已成为当务之急。
基于此,本申请实施例提供一种树脂组合物、半固化片及其制备方法、覆铜板及其制备方法和印制电路板,能够使覆铜板具有低介电损耗、低热膨胀系数、高耐热性和较好的无卤阻燃等特征。为了便于读者理解本申请,下面结合具体的实施例进行说明。
本申请实施例提供一种树脂组合物,该树脂组合物用于制备覆铜板,按照重量份计,所述树脂组合物包括以下组分:
氰酸酯(Cyanate Ester,CE)是含有两个及两个以上氰酸酯基团的酚的衍生物,在热及催化剂的作用下发生三聚环化反应生成高交联密度、无极性的芳氧基三嗪环结构,正是该种结构使得氰酸酯具有优异的介电性能。固化的氰酸酯同时还具有较好的阻燃、高玻璃化转变温度、低收缩率、低吸湿率、良好的粘结性能及低发烟和耐烧蚀等性能,是高性能树脂基复合材料的基体材料,在电子、宇航、军工等许多领域有着广泛的应用前景,特别是高频印制电路板、结构材料及天线涂层等方面有较大的发展前景。
在一些实施例中,氰酸酯具体可以是双酚A型氰酸酯、双酚E型氰酸酯、双酚F型氰酸酯、双酚M型氰酸酯、四甲基双酚F型氰酸酯、双环戊二烯双酚A型氰酸酯中的至少一种。具体地,在本申请的某些实施例中,当氰酸酯为双酚A型氰酸酯时,得到的覆铜板的介电性能、耐热性能和阻燃性能等性能最好。
双马来酰亚胺是一种典型的耐热型热固性树脂,具有优越的加工性能、粘结性、电绝缘性、耐疲劳性、高强度以及耐湿热等性能。双马来酰亚胺的性能及应用不仅与其结构组成有关,而且深受固化方式和工艺等的影响。
在本申请的某些实施例中,当双马来酰亚胺为二苯甲烷双马来酰亚胺时,得到的覆铜板的介电性能、耐热性能和阻燃性能等性能最好。
相对于使用单一的氰酸酯或使用单一的双马来酰亚胺树脂,本申请实施例通过将氰酸酯与双马来酰亚胺树脂进行复配使用,可以提高覆铜板的综合性能,例如,介电性能、耐热性能和阻燃性能等。
虽然氰酸酯与环氧树脂等热固性树脂相比,其耐冲击性能较好,但其韧性仍不能满足要求,需对其进行改性,通常采用具有较高的热性能的热塑性树脂对其进行改性。在本申请的实施例中,通过二烯丙基双酚A对氰酸酯/双马来酰亚胺树脂体系进行改性,可以提高氰酸酯/双马来酰亚胺树脂体系的韧性。
在本申请的实施例中,为了提高氰酸酯/双马来酰亚胺树脂体系的固化效率,采用二月桂酸二丁基锡作为固化催化剂。加入适量的二月桂酸二丁基锡不仅可以提高基体树脂的固化效率,而且可以改善氰酸酯/双马来酰亚胺树脂基覆铜板的韧性和介电性能等。
在一些实施例中,硅烷偶联剂例如可以是KH-560。
在本申请的实施例中,硅微粉有助于降低覆铜板的介电损耗。勃姆石有助于降低覆铜板的介电损耗,还有助于提高覆铜板的阻燃性能。在一些实施例中,硅微粉具体可以是球形硅微粉(也即,球硅)。
在一些实施例中,含磷阻燃剂包括磷腈化合物、磷酸酯化合物、氮磷阻燃剂、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物或二乙基磷酸铝阻燃剂中的至少一种。
在一些实施例中,按照重量份计,所述树脂组合物还包括:100-200份的有机溶剂。有机溶剂例如可以是丙酮、丁酮和/或环己酮等。在本申请的某些实施例中,有机溶剂具体为丁酮。
第二方面,本申请实施例还提供了一种半固化片,该半固化片包括增强材料和包覆该增强材料的树脂层,且树脂层的原材料为上述实施例提供的的树脂组合物。
在一些实施例中,增强材料包括石英纤维布、玻璃纤维布、芳纶纤维布和/或碳纤维布。具体地,在一些实施例中,当增强材料为玻璃纤维布时覆铜板的综合性能最好。
第三方面,本申请实施例还提供了一种半固化片的制备方法,该方法包括以下步骤:取上述实施例提供的树脂组合物;将增强材料浸渍在树脂组合物中;加热浸渍后的增强材料,以使增强材料上的树脂组合物半固化,从而形成半固化片。
在一些实施例中,半固化片的制备方法具体包括以下步骤:将型氰酸酯、双马来酰亚胺、二烯丙基双酚A和二月桂酸二丁基锡加入装有丁酮的容器中;75℃-85℃加热条件下,通过搅拌的方式使容器中的混合物混合均匀,然后在容器中添加硅微粉、硅烷偶联剂、勃姆石和含磷阻燃剂,继续搅拌1.5h-2.5h,得到胶液。用胶液浸渍玻璃纤维布后,将包覆有胶液的玻璃纤维布置于155℃-165℃下预固化10-15min后,得到半固化片;其中,玻璃纤维布的厚度可以是35μm左右。
第四方面,本申请实施例还提供了一种覆铜板,该覆铜板包括上述实施例提供的半固化片和设置于所述半固化片单面或双面的导电金属片。半固化片的层数可以是一层或多层。导电金属片具体可以是铜片。
第五方面,本申请实施例还提供了一种覆铜板的制备方法,该方法包括:将上述实施例提供的半固化片的单面或双面覆上导电金属片,将半固化片和导电金属片压合成型,从而形成覆铜板。
在一些实施例中,覆铜板的制备方法具体包括以下步骤:
在半固化片的至少一侧表面叠加导电金属片(例如铜箔)后,再使叠合后的半固化片和导电金属片在承受2MPa-3MPa压力的条件下,先于175℃-185℃固化1.5h-2.5h,再于205℃-215℃固化1.5h-2.5h、最后于235℃-245℃固化1.5h-2.5h,从而得到覆铜板。
第六方面,本申请实施例还提供一种印制电路板,所述印制电路板包括第四方面所述的覆铜板和设置于所述覆铜板的电子元件。
在本申请的实施例中,将氰酸酯和双马来酰亚胺复配使用可以提高半固化片的耐热性能、降低半固化片的介电常数和介电损耗。二烯丙基双酚A用于提高氰酸酯/双马来酰亚胺树脂体系的韧性。固化催化剂用于提高氰酸酯/双马来酰亚胺树脂体系的固化效率。硅微粉用于降低半固化片的介电常数和介电损耗。勃姆石和含磷阻燃剂用于提高半固化片的阻燃性能。本申请实施例提供的半固化片和覆铜板不但具有较低的介电常数和较低的介电损耗,还具有良好的耐热性能和无卤阻燃性能。
下面提供挠性覆铜板的若干实施例。
实施例1
将100重量份的双酚A型氰酸酯、25重量份的二苯甲烷双马来酰亚胺、15重量份的二烯丙基双酚A、0.28重量份的二月桂酸二丁基锡加入装有150重量份丁酮的容器中;80℃加热条件下搅拌容器中的混合物,使混合物混合均匀;然后,在容器中添加200重量份的硅微粉、0.6重量份的硅烷偶联剂KH-560、50重量份的勃姆石和50重量份的含磷阻燃剂继续搅拌2h,得到胶液A。
用此胶液A浸渍厚度为35μm左右的玻璃纤维布1067,将包覆有胶液A的玻璃纤维布在160℃下进行10min-15min的预固化,得到半固化片。再在半固化片的上下两侧表面叠加12μm厚的铜箔,在2.5MPa压力下,依次按照180℃下加热2h、210℃下加热2h,以及在240℃条件下加热2h的温度时间固化程序对叠加的铜箔和半固化进行加热加压,得到白色覆铜板A。
实施例2
将100重量份的双酚A型氰酸酯、25重量份的二苯甲烷双马来酰亚胺、15重量份的二烯丙基双酚A和0.28重量份的二月桂酸二丁基锡加入装有150重量份丁酮的容器中;80℃加热条件下搅拌容器中的混合物,使容器中的混合物混合均匀;然后在容器中添加150重量份的硅微粉、50重量份的二氧化钛、0.6重量份的硅烷偶联剂KH-560、50重量份的勃姆石和50重量份的含磷阻燃剂继续搅拌2h,得到胶液B。
用胶液B浸渍厚度为35μm左右的玻纤布1067,将包覆有胶液B的玻璃纤维布置于160℃下进行10-15min的预固化,得到半固化片。再在半固化片上下叠加12μm厚的铜箔,在2.5MPa压力下,依次按照180℃下加热2h、210℃下加热2h,以及在240℃条件下加热2h的温度时间固化程序对叠加的铜箔和半固化进行加热加压,得到白色覆铜板B。
表一出示了实施例1和实施例2使用的树脂组合物的配方和覆铜板的性能测试结果。需要说明的是:在进行热膨胀系数测试和玻璃化转变温度测试时,需要刻蚀掉实施例1的覆铜板A上的铜箔之后得到半固化片A,并对半固化片A进行热膨胀系数测试和玻璃化转变温度测试;以及,需要刻蚀掉实施例2的覆铜板B上的铜箔之后得到半固化片B,并对半固化片B进行热膨胀系数测试和玻璃化转变温度测试。
表一:实施例1和实施例2使用的树脂组合物的配方和覆铜板的性能测试结果。
图1和图2分别出示了实施例1和实施例2的热膨胀系数测试结果图。由图1和图2可知:实施例1和实施例2的膨胀系数(CTE)的测试结果分别为14.58ppm/℃和14.18ppm/℃。
图3和图4分别出示了实施例1和实施例2的玻璃化转变温度测试结果图。由图1和图2可知:实施例1和实施例2的玻璃化转变温度(Tg)的测试结果分别为290℃和279℃。由于实施例2的二氧化钛和硅微粉在混合的时候没有分散均匀,导致在树脂体系中出现不良界面,所以实施例2的耐热性偏低于实施例1。
本申请实施例1的覆铜板的Tg高达290℃,热膨胀系数CTE低至14ppm/℃,介电常数(DK)为3.76,介电损耗(DF)低至0.006。因此,本申请实施例1的覆铜板适用于当前高频、高速印制电路板(PCB)的设计,而且可以大大提高了封装效率和PCB板的可靠性。
最后应说明的是:以上实施例仅用以说明本发明的技术方案,而非对其限制;在本发明的思路下,以上实施例或者不同实施例中的技术特征之间也可以进行组合,步骤可以以任意顺序实现,并存在如上所述的本发明的不同方面的许多其它变化,为了简明,它们没有在细节中提供;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。
Claims (10)
1.一种树脂组合物,其特征在于,按照重量份计,所述树脂组合物包括以下组分:
2.根据权利要求1所述的树脂组合物,其特征在于,所述氰酸酯为双酚A型氰酸酯;
所述双马来酰亚胺为二苯甲烷双马来酰亚胺。
3.根据权利要求1或2所述的树脂组合物,其特征在于,所述固化催化剂为二月桂酸二丁基锡。
4.根据权利要求3所述的树脂组合物,其特征在于,按照重量份计,所述树脂组合物还包括:
有机溶剂100-200份。
5.一种半固化片,其特征在于,所述半固化片包括增强材料和包覆所述增强材料的树脂层,所述树脂层的原材料为权利要求1-4任一项所述的树脂组合物。
6.根据权利要求4或5所述的半固化片,其特征在于,所述增强材料为玻璃纤维布。
7.一种半固化片的制备方法,其特征在于,所述方法包括以下步骤:
取权利要求1-4任意一项所述的树脂组合物;
将增强材料浸渍在所述树脂组合物中;
加热浸渍后的所述增强材料,以使所述增强材料上的所述树脂组合物半固化,从而形成所述半固化片。
8.一种覆铜板,其特征在于,所述覆铜板包括权利要求5或6任一项所述的半固化片和设置于所述半固化片单面或双面的导电金属片。
9.一种覆铜板的制备方法,其特征在于,所述方法包括:
将权利要求5或6任意一项所述的半固化片的单面或双面覆上导电金属片,将所述半固化片和所述导电金属片压合成型,从而形成所述覆铜板。
10.一种印制电路板,其特征在于,所述印制电路板包括权利要求8所述的覆铜板和设置于所述覆铜板的电子元件。
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