CN107498891B - 一种基于三明治结构的聚醚醚酮电磁屏蔽复合材料及其制备方法 - Google Patents
一种基于三明治结构的聚醚醚酮电磁屏蔽复合材料及其制备方法 Download PDFInfo
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- 229920002530 polyetherether ketone Polymers 0.000 title claims abstract description 128
- 239000004696 Poly ether ether ketone Substances 0.000 title claims abstract description 107
- 239000002131 composite material Substances 0.000 title claims abstract description 81
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 69
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- 239000002041 carbon nanotube Substances 0.000 claims abstract description 61
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- 229920001721 polyimide Polymers 0.000 claims description 17
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- 238000002844 melting Methods 0.000 claims description 10
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- 239000004697 Polyetherimide Substances 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- 229920006393 polyether sulfone Polymers 0.000 claims description 6
- 239000004695 Polyether sulfone Substances 0.000 claims description 4
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- -1 ether ketone Chemical class 0.000 claims description 3
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- 238000007792 addition Methods 0.000 description 4
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- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 description 2
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
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- 229920001169 thermoplastic Polymers 0.000 description 1
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Abstract
一种基于三明治结构的聚醚醚酮电磁屏蔽复合材料及其制备方法,属于电磁屏蔽技术领域,该复合材料适用于电磁屏蔽和微波吸收等领域。是将干燥后的聚醚醚酮粒料挤出成膜,得到聚醚醚酮薄膜;将粘结剂和碳纳米管混合后,得到含有粘结剂的碳纳米管;将含有粘结剂的碳纳米管平铺在聚醚醚酮薄膜上,热压得到聚醚醚酮复合膜;将所需数量的聚醚醚酮复合膜及聚醚醚酮薄膜按照三明治结构进行热压,降至室温后得到基于三明治结构的聚醚醚酮电磁屏蔽复合材料。复合材料随着碳纳米管层的增加,电磁屏蔽性能增强。在三层碳纳米管层时厚度仅为280μm,拉伸强度为70MPa以上,电磁屏蔽性能在8.2~40GHz频率范围内达到35dB以上。
Description
技术领域
本发明属于电磁屏蔽技术领域,具体涉及一种基于三明治结构的聚醚醚酮电磁屏蔽复合材料及其制备方法。该复合材料适用于电磁屏蔽和微波吸收等领域。
背景技术
伴随着电子化、信息化的快速发展,电磁波作为信息传播的重要载体的同时也带来了十分严重的电磁污染。对电子电器设备的正常使用、无线电通信系统以及人类神经中枢等产生很大危害,更对国家安全带来严重影响。为了防止电磁污染带来的危害,开发高性能的电磁屏蔽材料变得尤为迫切。
目前,常见的一类电磁屏蔽材料是将导电填料和树脂基体进行物理共混得到导电复合材料。传统的导电填料主要是金属系填料,比如金属纳米线和纳米粒子,它们具有较高导电率,在30MHz~1.5GHz频率范围内具有较好的屏蔽效果。相较于金属系填料,碳系填料则在8.2~40GHz频率范围内具有较好的屏蔽效果。
聚醚醚酮(PEEK)是一种主链由大量苯环、醚键和羰基重复连接构成的聚合物,具有耐高温、高强度、耐化学腐蚀、抗蠕变和高阻燃性等性能,是一种综合性能优异的特种工程塑料,被广泛应用于航空航天、汽车、医疗器械等领域。但是,PEEK除了浓硫酸以外,几乎不溶于其它常规有机溶剂,因此只能采用熔融加工方式,在加工过程中填料的自身团聚以及填料与基体树脂弱的相容性使填料难于在PEEK基体实现均匀分散,故而制备聚醚醚酮电磁屏蔽复合材料的报道较少。
中国专利CN102321338A公开了一种聚醚醚酮基复合电磁屏蔽材料及其制备方法,其主要是将碳纳米管、碳纤维、导电石墨等用聚醚砜包覆后作为导电填料加入到聚醚醚酮基体树脂中制备成电磁屏蔽材料,导电填料经过包覆改性之后对分散性有所改善。但随着导电填料的加入,在加工过程中导电填料增加会使得材料粘度增加,给加工造成困难,难于实现导电填料高含量的加入。中国专利CN106564227A公开了一种具有电磁屏蔽性能的聚合物/石墨烯发泡材料及制备方法和应用,该方法主要利用溶液共混和相分离法制备出热塑性聚合物/石墨烯微发泡薄膜,将其与透波材料粘结成具有三明治结构的一体化材料。但是该专利要求聚合物能够在溶剂中溶解,对于一些耐溶剂型的聚合物不能采用这个方法。
发明内容
本发明的目的是提供一种基于三明治结构的聚醚醚酮电磁屏蔽复合材料的制备方法。与已有专利相比,本发明中聚醚醚酮电磁屏蔽复合材料的制备方法简单,而且在导电填料含量较低的情况下,就可以达到较好的电磁屏蔽效果。与上述专利相比,若在同样厚度情况下,电磁屏蔽性能更为优异。
本发明中所述的一种基于三明治结构的聚醚醚酮电磁屏蔽复合材料为(聚醚醚酮薄膜/含有粘结剂的碳纳米管层)n/聚醚醚酮薄膜的三明治结构(n为大于等于1的整数)。在碳纳米管层以聚酰亚胺(PI)、聚醚酰亚胺(PEI)、聚醚砜(PES)等聚合物作为碳纳米管之间的粘结剂,可以较好解决碳纳米管之间因为碳纳米管表面基团较少,分子间作用力较弱容易剥离等问题。采用背景技术中文献所述的制备方法,随着导电填料的大量加入,复合材料的粘度增加,必然会对加工造成困难,而本发明则无需考虑碳纳米管在基体树脂中团聚和粘度增加的问题。在本发明中碳纳米管层过厚也会削弱粘结剂的作用,为了解决这个问题,我们提出采用多层三明治结构,进而控制每层碳纳米管层的厚度。为了进一步解决聚醚醚酮薄膜和含有粘结剂的碳纳米管层之间的界面问题,采用在聚醚醚酮薄膜表面旋涂一层增容剂,可以增强界面粘合力。本发明中聚醚醚酮电磁屏蔽复合材料的制备方法有助于改善现有聚醚醚酮基电磁屏蔽复合材料制备技术上的不足之处。
本发明所述的一种基于三明治结构的聚醚醚酮电磁屏蔽复合材料的制备方法,其步骤为:(1)将干燥后的聚醚醚酮(PEEK)粒料挤出成膜,得到聚醚醚酮薄膜;(2)将粘结剂和碳纳米管混合后,以10000~26000r/min的速度高速搅拌1~5min,得到含有粘结剂的碳纳米管;(3)将步骤(2)得到的含有粘结剂的碳纳米管取出0.4~2g平铺在步骤(1)得到的聚醚醚酮薄膜上(薄膜的面积150mm×150mm),热压得到聚醚醚酮复合膜;(4)将所需数量的步骤(3)得到的聚醚醚酮复合膜及步骤(1)得到的聚醚醚酮薄膜按照三明治结构进行热压,降至室温后得到基于三明治结构的聚醚醚酮电磁屏蔽复合材料。
本发明中所用到的聚醚醚酮粒料熔融指数(MFI)为16~45g/10min(熔融指数测定条件:测试温度为400℃,载荷为5Kg),不选择熔融指数太高的聚醚醚酮粒料是因为在挤出成膜的过程中容易破裂。
本发明中用于制备聚醚醚酮薄膜的设备由双螺杆挤出机、过滤装置、弓形狭缝式口模、三辊压光机和拉伸设备组成(包含双螺杆挤出机、过滤装置、弓形狭缝式口模、三辊压光机的装置图见中国专利CN102337018A)。
本发明中所用的聚醚醚酮薄膜的制备,是将干燥后的PEEK粒料加入到双螺杆挤出机(HaakePTW16/25p,德国Thermo公司)中,并于350~400℃下熔融,熔融的PEEK粒料依靠双螺杆挤出机的旋转推进装置通过过滤装置,而后流入弓形狭缝式口模,口模的模唇厚度和宽度分别为0.03~0.15mm和150mm,进入弓形狭缝式口模的熔融的PEEK在温度为360~380℃的口模中成型为熔融的熔体膜片,再将熔融的熔体膜片导入三辊压光机进行拉伸冷却定型,三辊压光机的辊温为100~200℃,辊速为1~3m/min,牵引比(三辊压光机辊速与口模挤出速度之比)为1~3:1,从而得到本发明中所用的聚醚醚酮薄膜,膜厚度为60~150μm。在聚醚醚酮薄膜的制备中,双螺杆挤出机为四区段式加热熔融结构,第一段的温度范围为340~370℃,加热区段温度逐渐提高,后一加热区段的温度比前一加热区的温度高5~10℃,双螺杆挤出机喂料螺杆转速与挤出机双螺杆转速比为1~3:1,在此范围内制得聚醚醚酮薄膜质量较好。
在本发明中碳纳米管之间因为碳纳米管表面基团较少,分子间力较弱,所以在碳纳米管中需要加入粘结剂,起到粘接碳纳米管的作用,以解决碳纳米管之间容易剥离的问题,粘结剂主要选用热稳定性较好的聚合物,诸如聚酰亚胺、聚醚酰亚胺、聚醚砜等,其用量为碳纳米管质量的20%~50%。
在本发明步骤(3)中制备PEEK复合膜时,碳纳米管层的厚度是通过含有粘结剂的碳纳米管的加入量来控制的,碳纳米管层过厚会削弱粘结剂的作用,故而厚度一般控制在30~60μm为宜。在热压过程中温度控制在350~380℃,压力为5MPa~10MPa,制备的PEEK复合膜具有较好的韧性和强度。
在本发明步骤(4)中将得到的PEEK复合膜按照需要叠合在一起放入模具中热压即可得到基于三明治结构的聚醚醚酮电磁屏蔽复合材料。其中热压温度控制在350~375℃,压力为1MPa~10MPa。步骤(3)和步骤(4)的热压过程中,升温速率为10~30℃/min,降温速率为15~30℃/min。
在本发明中为了进一步提高聚醚醚酮薄膜和碳纳米管层之间的界面粘接问题,在聚醚醚酮薄膜的表面旋涂一层增容剂,可以增强界面粘合力。增容剂采用与聚醚醚酮以及作为粘结剂的聚合物之间具有良好相容性的嵌段聚合物,比如聚醚醚酮齐聚物和聚酰亚胺齐聚物共聚而成的嵌段聚合物(PEEK-g-PI,嵌段聚合物的制备及表征详见中国专利CN201210421487.1)。
在上述条件下得到的聚醚醚酮复合材料随着碳纳米管层的增加,电磁屏蔽性能增强。在三层碳纳米管层时厚度仅为280μm,拉伸强度为70MPa以上(该复合材料的拉伸强度可以通过调节PEEK层的厚度来调控),电磁屏蔽性能在8.2~40GHz频率范围内达到35dB以上,在相同厚度条件下已经达到了一个较高的电磁屏蔽水平,可以满足现实中的使用要求。
附图说明
图1:对比例1样品拉伸测试后断裂处截面的扫描电镜图;
图2:实施例1样品拉伸测试后断裂处截面的扫描电镜图;
图3:实施例1样品拉伸测试后断裂处碳纳米管层截面的扫描电镜图;
图4:实施例2样品拉伸测试后断裂处截面的扫描电镜图;
图5:实施例3样品拉伸测试后断裂处截面的扫描电镜图;
图6:实施例4样品拉伸测试后断裂处截面的扫描电镜图。
具体实施方式
本发明中所用的聚醚醚酮粒料由长春吉大特塑工程研究有限公司提供。
本发明中所用的力学性能测试仪器是日本岛津AG-120KN型电子万能材料实验机,测试过程中拉伸速率为2mm/min。采用Agilent N5244APNA-X网络分析仪进行电磁屏蔽测试,测试电磁波屏蔽范围是8.2~40GHz。扫描电镜测试仪器是HITACHI-SU8020。
聚醚醚酮薄膜的制备:将聚醚醚酮粒料(MFI=16~45g/10min)在180℃高温干燥3小时后,通过带有喂料螺杆的料斗加入到双螺杆挤出机内,双螺杆挤出机料筒各区段温度为355℃/365℃/375℃/380℃,料斗内喂料螺杆转速与挤出机双螺杆转速比为1:1,口模宽度为150mm,弓型狭缝式口模的模唇厚度为0.1mm,口模的温度为380℃,三辊压光机辊速为2m/min,辊温控制在150℃。牵引比(挤出膜时辊速与模口挤出速度的比)为1.5:1,制得的薄膜厚度为0.08mm。
对比例1
将预先裁剪好(150mm×150mm×0.08mm)的PEEK薄膜(MFI=16g/10min)放入模具中,并用纯碳纳米管0.4g铺满整个薄膜(150mm×150mm×0.08mm),铺满后将整个模具放入热压机中在温度为360℃,压力10MPa的条件下热压成型得到PEEK复合膜。然后将该复合膜和PEEK薄膜叠放在一起放入模具中,在温度为360℃,压力10MPa的条件下热压成型即可得到三明治结构的PEEK/MCNTs/PEEK电磁屏蔽复合材料。将制备的样品拉伸测试后做扫描电镜测试(SEM)。
如图1所示,通过拉伸测试后的SEM分析可知该复合材料在拉伸过程中碳纳米管层已经发生严重剥离。复合材料厚度大约为150μm,其中两层PEEK薄膜层的厚度都大约为60μm,纯碳纳米管层的厚度大约为30μm。采用波导法测试样品在8.2~40GHz频率下的电磁屏蔽效率值为20dB,该复合材料的拉伸强度为35MPa,断裂伸长率4.3%。
实施例1
将碳纳米管和聚酰亚胺(PI)按照4:1(质量比)的比例混合后放入高速搅拌机中以26000r/min的速率搅拌1min后取出,得到包含聚酰亚胺粘结剂的碳纳米管。将预先裁剪好(150mm×150mm×0.08mm)的PEEK薄膜(MFI=16g/10min)放入模具中,并用上述包含聚酰亚胺粘结剂的碳纳米管0.4g铺满整个薄膜,铺满后将整个模具放入热压机中在温度为380℃,压力5MPa的条件下热压成型得到PEEK复合膜。然后将该复合膜和PEEK薄膜叠放在一起放入模具中,在温度为360℃,压力5MPa的条件下热压成型即可得到三明治结构的电磁屏蔽复合材料,记为PEEK/(1PI:4MCNTs)/PEEK。将制备的样品拉伸测试后做扫描电镜测试(SEM)。
如图2所示,通过拉伸测试后的SEM分析可知该复合材料在拉伸过程中碳纳米管层并未发生剥离现象。扩大SEM倍率得到图3,从图3可知聚醚酰亚胺的加入在碳纳米管之间起到了较好的粘结作用。复合材料厚度大约为140μm,其中2层PEEK薄膜的厚度都大约为50μm,包含聚酰亚胺粘结剂的碳纳米管层的厚度都大约为40μm。采用波导法测试样品在8.2~40GHz频率下的电磁屏蔽效率值为19dB,该复合材料的拉伸强度为83MPa,断裂伸长率4.5%。
实施例2
将一定量的碳纳米管和聚酰亚胺按照4:1(质量比)的比例放入高速搅拌机中以26000r/min的速率搅拌1min后取出。将预先裁剪好(150mm×150mm×0.08mm)的PEEK薄膜(MFI=16g/10min)放入模具中,并用上述的碳纳米管0.4g铺满整个薄膜,铺满后将整个模具放入热压机中在温度为365℃,压力5MPa的条件下热压成型得到PEEK复合膜。然后将该两张上述复合膜和PEEK薄膜叠放在一起放入模具中,在温度为355℃,压力10MPa的条件下热压成型即可得到三明治结构的复合材料,记为PEEK/2(1PI:4MCNTs)/PEEK。将制备的样品拉伸测试后做扫描电镜测试(SEM)。
如图4所示,通过拉伸测试后的SEM分析可知该复合材料在拉伸过程中碳纳米管层并未发生剥离现象。复合材料厚度为240μm,复合材料中三层PEEK薄膜的厚度都大约为50μm,两层包含聚酰亚胺粘结剂的碳纳米管层的厚度都大约为45μm。采用波导法测试样品在8.2~40GHz频率下的电磁屏蔽效率值为25dB,该复合材料的拉伸强度为76MPa,断裂伸长率4.3%。
实施例3
将一定量的碳纳米管和聚酰亚胺按照4:1(质量比)的比例放入高速搅拌机中以26000r/min的速率搅拌1min后取出。将预先裁剪好(150mm×150mm×0.08mm)的PEEK薄膜(MFI=16g/10min)放入模具中,并用上述的碳纳米管0.4g铺满整个薄膜,铺满后将整个模具放入热压机中在温度为365℃,压力5MPa的条件下热压成型得到PEEK复合膜。然后将该三张上述复合膜和PEEK薄膜叠放在一起放入模具中,在温度为375℃,压力5MPa的条件下热压成型即可得到三明治结构的复合材料,记为PEEK/3(1PI:4MCNTs)/PEEK。将制备的样品拉伸测试后做扫描电镜测试(SEM)。
如图5所示,通过拉伸测试后的SEM分析可知该复合材料在拉伸过程中碳纳米管层并未发生剥离现象。复合材料厚度为280μm,复合材料中四层PEEK薄膜的厚度都大约为40μm,三层包含聚酰亚胺粘结剂的碳纳米管层的厚度都大约为40μm。采用波导法测试样品在8.2~40GHz频率下的电磁屏蔽效率值为35dB,该复合材料的拉伸强度为72MPa,断裂伸长率4.4%。
实施例4
将一定量的碳纳米管和聚酰亚胺按照1:1(质量比)的比例放入高速搅拌机中以26000r/min的速率搅拌1min后取出。将预先裁剪好(150mm×150mm×0.08mm)的PEEK薄膜(MFI=45g/10min)放入模具中,并用上述的碳纳米管0.4g铺满整个薄膜,铺满后将整个模具放入热压机中在温度为375℃,压力5MPa的条件下热压成型得到PEEK复合膜。然后将该复合膜和PEEK薄膜叠放在一起放入模具中,在温度为350℃,压力10MPa的条件下热压成型即可得到三明治结构的复合材料记为PEEK/(1PI:1MCNTs)/PEEK。将制备的样品拉伸测试后做扫描电镜测试(SEM)。
如图6所示,通过拉伸测试后的SEM分析可知该复合材料在拉伸过程中碳纳米管层并未发生剥离现象。复合材料厚度大约为160μm,其中2层PEEK薄膜的厚度都大约为60μm,包含聚酰亚胺粘结剂的碳纳米管层的厚度都大约为40μm。采用波导法测试样品在8.2~40GHz频率下的电磁屏蔽效率值为15dB,该复合材料的拉伸强度为73MPa,断裂伸长率4.8%。
实施例5
将一定量的碳纳米管和聚醚酰亚胺按照4:1(质量比)的比例放入高速搅拌机中以26000r/min的速率搅拌1min后取出。将预先裁剪好(150mm×150mm×0.08mm)的PEEK薄膜(MFI=45g/10min)放入模具中,并用上述的碳纳米管0.4g铺满整个薄膜,铺满后将整个模具放入热压机中在温度为380℃,压力5MPa的条件下热压成型得到PEEK复合膜。然后将该复合膜和PEEK薄膜叠放在一起放入模具中,在温度为360℃,压力5MPa的条件下热压成型即可得到三明治结构的复合材料,记为PEEK/(1PEI:4MCNTs)/PEEK。
该复合材料厚度大约为150μm,其中两层PEEK薄膜层的厚度都大约为50μm,纯碳纳米管层的厚度大约为50μm,采用波导法测试样品在8.2~40GHz频率下的电磁屏蔽效率值为17.5dB,拉伸强度为88MPa,断裂伸长率4.7%。
实施例6
将一定量的碳纳米管和聚醚砜按照4:1(质量比)的比例放入高速搅拌机中以26000r/min的速率搅拌1min后取出。将预先裁剪好(150mm×150mm×0.08mm)的PEEK薄膜(MFI=45g/10min)放入模具中,并用上述的碳纳米管0.4g铺满整个薄膜,铺满后将整个模具放入热压机中在温度为375℃,压力5MPa的条件下热压成型得到PEEK复合膜。然后将该复合膜和PEEK薄膜叠放在一起放入模具中,在温度为370℃,压力5MPa的条件下热压成型即可得到三明治结构的复合材料,记为PEEK/(1PES:4MCNTs)/PEEK。
该复合材料厚度大约为155μm,其中两层PEEK薄膜层的厚度都大约为55μm,纯碳纳米管层的厚度大约为45μm,采用波导法测试样品在8.2~40GHz频率下的电磁屏蔽效率值为18dB,拉伸强度为85MPa,断裂伸长率4.8%(力学性能测试仪器日本岛津AG-120KN型电子万能材料实验机)。
实施例7
将0.5g增容剂PEEK-g-PI溶解在20mL三氟乙酸中,待聚合物完全溶解后,将其涂覆在聚醚醚酮薄膜上。将一定量的碳纳米管和聚酰亚胺按照4:1(质量比)的比例放入高速搅拌机中以26000r/min的速率搅拌1min后取出。将预先裁剪好(150mm×150mm×0.08mm)涂覆增容剂的PEEK薄膜(MFI=16g/10min)放入模具中,并用上述的碳纳米管0.4g铺满整个薄膜,铺满后将整个模具放入热压机中在温度为365℃,压力5MPa的条件下热压成型得到PEEK复合膜。然后将该三张上述复合膜和PEEK薄膜叠放在一起放入模具中,在温度为375℃,压力5MPa的条件下热压成型即可得到三明治结构的复合材料,记为PEEK/3(1PI:4MCNTs)/PEEK。
该复合材料厚度为250μm,复合材料中四层PEEK薄膜的厚度都大约为40μm,三层包含聚酰亚胺粘结剂的碳纳米管层的厚度都大约为30μm。采用波导法测试样品在8.2~40GHz频率下的电磁屏蔽效率值为33dB,该复合材料的拉伸强度为76MPa,断裂伸长率4.9%。
Claims (9)
1.一种基于三明治结构的聚醚醚酮电磁屏蔽复合材料的制备方法,其步骤如下:
(1)将干燥后的聚醚醚酮粒料挤出成膜,得到聚醚醚酮薄膜,裁剪后得到薄膜的尺寸为150mm×150mm;
(2)将粘结剂和碳纳米管混合后,以10000~26000r/min的速度搅拌1~5min,得到含有粘结剂的碳纳米管;
(3)将步骤(2)得到的含有粘结剂的碳纳米管取出0.4~2g平铺在步骤(1)得到的聚醚醚酮薄膜上,热压得到聚醚醚酮复合膜;
(4)将所需数量的步骤(3)得到的聚醚醚酮复合膜及步骤(1)得到的聚醚醚酮薄膜按照三明治结构进行热压,降至室温后得到基于三明治结构的聚醚醚酮电磁屏蔽复合材料,三明治结构为(聚醚醚酮薄膜/含有粘结剂的碳纳米管层)n/聚醚醚酮薄膜,n为大于等于1的整数。
2.如权利要求1所述的一种基于三明治结构的聚醚醚酮电磁屏蔽复合材料的制备方法,其特征在于:步骤(1)中聚醚醚酮粒料的熔融指数为16~45g/10min,测试温度为400℃,载荷为5Kg。
3.如权利要求1所述的一种基于三明治结构的聚醚醚酮电磁屏蔽复合材料的制备方法,其特征在于:步骤(1)是将干燥后的聚醚醚酮粒料加入到双螺杆挤出机中,并于350~400℃下熔融,熔融的聚醚醚酮粒料依靠双螺杆挤出机的旋转推进装置通过过滤装置,而后流入弓形狭缝式口模,口模的模唇厚度和宽度分别为0.03~0.15mm和150mm,进入弓形狭缝式口模的熔融的聚醚醚酮在温度为360~380℃的口模中成型为熔融的熔体膜片,再将熔融的熔体膜片导入三辊压光机进行拉伸冷却定型,三辊压光机的辊温为100~200℃,辊速为1~3m/min,牵引比为1~3:1,从而得到聚醚醚酮薄膜,膜厚度为60~150μm。
4.如权利要求3所述的一种基于三明治结构的聚醚醚酮电磁屏蔽复合材料的制备方法,其特征在于:双螺杆挤出机为四区段式加热熔融结构,第一段的温度范围为340~370℃,加热区段温度逐渐提高,后一加热区段的温度比前一加热区的温度高5~10℃,双螺杆挤出机喂料螺杆转速与挤出机双螺杆转速比为1~3:1。
5.如权利要求1所述的一种基于三明治结构的聚醚醚酮电磁屏蔽复合材料的制备方法,其特征在于:步骤(2)中的粘结剂为聚酰亚胺、聚醚酰亚胺或聚醚砜,其用量为碳纳米管质量的20%~50%。
6.如权利要求1所述的一种基于三明治结构的聚醚醚酮电磁屏蔽复合材料的制备方法,其特征在于:步骤(3)中含有粘结剂的碳纳米管层的厚度为30~60μm;热压温度为350~380℃,压力为5MPa~10MPa,升温速率为10~30℃/min。
7.如权利要求1所述的一种基于三明治结构的聚醚醚酮电磁屏蔽复合材料的制备方法,其特征在于:步骤(4)中热压温度为350~375℃,压力为1MPa~10MPa;升温速率为10~30℃/min,降温速率为15~30℃/min。
8.如权利要求1所述的一种基于三明治结构的聚醚醚酮电磁屏蔽复合材料的制备方法,其特征在于:在聚醚醚酮薄膜的表面旋涂一层增容剂,增容剂为聚醚醚酮齐聚物和聚酰亚胺齐聚物共聚而成的嵌段聚合物PEEK-g-PI。
9.一种基于三明治结构的聚醚醚酮电磁屏蔽复合材料,其特征在于:是由权利要求1~8任何一项所述的方法制备得到。
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