CN114516207B - 一种夹层结构高导热复合薄膜热界面材料及其制备方法 - Google Patents

一种夹层结构高导热复合薄膜热界面材料及其制备方法 Download PDF

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CN114516207B
CN114516207B CN202210146578.2A CN202210146578A CN114516207B CN 114516207 B CN114516207 B CN 114516207B CN 202210146578 A CN202210146578 A CN 202210146578A CN 114516207 B CN114516207 B CN 114516207B
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fiber film
filler
heat conducting
heat conduction
elastic fiber
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马传国
宋沐原
迟洪涛
陆绍宁
张平
戴培邦
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Guilin University of Electronic Technology
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Abstract

本发明公开了一种夹层结构高导热复合薄膜热界面材料，该复合薄膜具有3层结构，由上下表面的弹性纤维薄膜层和中间的非弹性纤维薄膜层热压延复合而成，其中弹性纤维薄膜层和非弹性纤维薄膜层中均含有零维、一维导热填料、二维导热填料和异形导热填料中的至少两种。该复合薄膜解决了常规填充方法制备条件下热界面材料中导热网络构筑困难，填料间界面热阻以及热界面的接触热阻较大等问题，具有导热性能提升高效、制备工艺简单、易于实现规模化生产等优点。

Description

一种夹层结构高导热复合薄膜热界面材料及其制备方法
技术领域
本发明涉及导热复合薄膜技术领域，具体是一种夹层结构高导热复合薄膜热界面材料及其制备方法。
背景技术
随着电子器件集成度越来越高，功率逐渐增加，其发热问题也日益严重，对具有高导热性能的热界面材料的需求也越来越迫切。聚合物基复合材料因其性能优秀，易于制备，成本低等优点而被广泛应用于热界面管理领域。由于聚合物基体本征导热率较低，故需要添加导热率较高的导热填料以提高复合材料整体导热率，但是，为了保证复合材料的力学性能以及其他性能，同时控制成本，导热填料的填充率不宜过高。目前，使导热填料搭建三维导热网络，构建声子传输路径，是在低填充率下提高复合材料导热性能的最佳方法。
对于导热复合材料而言，热阻是影响导热性能的一个关键因素，包括复合材料与热界面间的接触热阻，复合材料中填料与基体以及填料与填料间的界面热阻。热界面凹凸不平而形成的空气层会产生接触热阻，大大降低热界面材料与热源表面的接触面积，导致散热效果不理想。而复合材料中填料间不良的相互接触或填料与基体间的界面缺陷会导致导热网络的不完整，从而引起导热性能下降。所以，提高复合材料导热性能的关键在于构建完整的导热网络，降低界面热阻，同时，也要降低接触热阻。通过在纤维膜的纤维表面吸附不同导热填料并多层热压的方式制备夹层结构高导热复合薄膜，可以在较低填充率下有效构建三维导热网络，降低界面热阻，提高导热性能的同时保证力学性能。在复合薄膜两侧使用弹性纤维膜作为基体，使其在接触面能够发生较大形变，提高与器件的接触面积，进一步降低接触热阻，从而提升导热散热性能。
发明内容
本发明的目的在于针对现有热界面材料界面接触热阻大，难以同时提升面内和垂直方向导热系数的不足，而提供一种夹层结构高导热复合薄膜热界面材料及其制备方法，该薄膜能够降低内部填料间的界面热阻，同时具有较低的接触热阻，且具有导热性能提升高效、制备工艺简单、易于实现规模化生产等优点。
实现本发明目的的技术方案是：
一种夹层结构高导热复合薄膜，该复合薄膜具有3层结构，由上下表面的弹性纤维薄膜层和中间的非弹性纤维薄膜层热压延复合而成，其中所述弹性纤维薄膜层和非弹性纤维薄膜层中均含有零维、一维导热填料、二维导热填料和异形导热填料中的至少两种。
所述的弹性纤维薄膜层，是由TPUPU、聚烯烃POE、聚苯乙烯-丁二烯嵌段共聚物SBS、聚酯酰胺PEA等典型热塑性弹性体材料制备的纤维薄膜或无纺布中的一种，纤维直径为50nm-50μm，面密度为10g-30g/m2；
所述的非弹性纤维薄膜层，为聚四氟乙烯PVDF、聚酰胺PA、聚乳酸PLA、聚丙烯PP、聚丙烯腈PAN、聚对苯二甲酸乙二醇酯PET、芳纶、聚酰亚胺PI纤维薄膜或无纺布中的一种，纤维直径为50nm-50μm，面密度为10g-30g/m2。所述的零维导热填料，为球形氧化铝Al2O3、球形氮化铝AlN中的至少一种，其粒径为500nm-100μm；
所述的一维导热填料，为羧基化碳纳米管CNTs、氮化碳纳米管CNNTs、碳化硅纳米线SiCNWs、银纳米线AgNWs中的至少一种，其长度为10μm-200μm；
所述的二维导热填料，为氮化硼纳米片BNNS、石墨烯纳米片GNPs、MXene中的至少一种，其粒径为100nm-5μm，厚度为5nm-100nm；
所述的异形导热填料，为四针状氧化锌ZnO、膨胀石墨EG中的至少一种，其粒径为500nm-100μm。
一种夹层结构高导热复合薄膜热界面材料的制备方法，包括如下步骤：
1）分别将零维导热填料、一维导热填料、二维导热填料和异形导热填料中分别加入去离子水中分散均匀，得到3种导热填料分散液；
2）将表面改性剂加入去离子水和无水乙醇的混合溶液中分散均匀，得到表面改性剂溶液；
3）分别将弹性纤维薄膜和非弹性纤维薄膜完全浸入步骤2）制得的表面改性剂溶液中浸渍10-30s，得到表面改性的弹性纤维薄膜和非弹性纤维薄膜；
4）将步骤3）得到的表面改性的弹性纤维薄膜和非弹性纤维薄膜分别先后浸入步骤1）制得的3种导热填料分散液中的至少两种中浸渍10-30s，且每浸渍完1种导热填料分散液后，将弹性纤维薄膜和非弹性纤维薄膜置于50-80℃下烘干，再浸入一种导热填料分散液中并烘干，如此重复进行表面改性和吸附过程2-10次，分别制得均匀吸附有零维导热填料、一维导热填料、二维导热填料和异形导热填料中至少两种的弹性纤维薄膜和非弹性纤维薄膜；
5）将步骤4）制得非弹性纤维薄膜进行第一次热压延，再将步骤4）制得的弹性纤维薄膜分别置于热压延后的非弹性纤维薄膜上下表面再进行第二次热压延后，制得夹层结构的高导热复合材料。
所述的第一次热压延，热压延工艺为：温度为100-300℃，压力为1-30MPa，压延速度为0.01-10m/min。
所述的第二次热压延，热压延工艺为：温度为50-200℃，压力为1-50MPa，压延速度为0.01-10m/min。
有益效果
本发明提供的一种夹层结构高导热复合薄膜热界面材料及其制备方法，与现有技术相比，有如下优点：
（1）该复合薄膜的中间层使用非弹性纤维膜为基体，上下表面层使用弹性纤维薄膜为基体，既保证了薄膜整体的包括拉伸性能在内的力学性能，又提高了与热界面的接触面积，增强了界面作用，降低接触热阻，提高了导热散热性能。
（2）中间层与上下表面层均经表面改性后通过超声辅助循环浸渍的方法吸附两种或两种以上的零维/一维/二维/异形导热填料，协同构建导热通路，同时中间层纤维膜经过热压延使纤维在剪切力与压力的共同作用下相互接触并熔融，负载在其表面的导热填料得以发生接触从而构建三维导热网络。
（3）上下表面层经二次热压延在构建导热网络的同时与中间层紧密结合，在降低了填料-基体与填料-填料界面热阻的同时，两侧的弹性层能够发生形变，提高薄膜与热源的接触面积，降低接触热阻，提高导热性能，中间层能够使热量沿垂直方向传递，提高散热效果。
（4）该复合薄膜具有制备简单，成本低，导热性能好的优点，适合作为热界面材料应用于电子封装领域。
附图说明
图1为实施例1中制备复合薄膜的模型示意图；
图2为实施例1制得的夹层结构复合薄膜的示意图。
具体实施方式
下面结合附图和实施例对本发明内容做进一步阐述，但不是对本发明的限定。
实施例1：
一种TPU电纺纤维膜/聚酰胺无纺布夹层结构高导热复合薄膜的制备方法，包括如下步骤：
（1）将TPU粉末溶于体积比为1：3的N，N-二甲基甲酰胺和四氢呋喃混合溶液中，室温下搅拌3h，配制质量分数为10%的静电纺丝溶液。
（2）取步骤（1）中的电纺溶液10ml通过静电纺丝设备进行静电纺丝，使用辊筒式接收器进行接收，得到弹性TPU电纺纤维膜。电纺参数：电压为12-15KV、喷头到接收器的距离为15-18cm，喷丝速度为80mm/min、温度为40℃，接收器转速为400rpm。
（3）配制羧基化碳纳米管、纳米氧化铝分散液、聚乙烯亚胺溶液：
分别取2g羧基化碳纳米管和2g纳米氧化铝，分别加入两份100ml去离子水中，搅拌均匀后分别使用超声清洗机进行超声分散2h，得到浓度为20mg/ml的羧基化碳纳米管分散液和纳米氧化铝分散液；
取1g聚乙烯亚胺溶于100ml去离子水中，搅拌至均一溶液，得到浓度为10mg/ml的聚乙烯亚胺溶液。
（4）将步骤（2）中得到的TPU电纺纤维膜裁剪成若干30cm×30cm的正方形薄膜，浸入步骤（3）得到的聚乙烯亚胺溶液中，10s后取出，得到表面改性后的电纺纤维膜。
（5）将步骤（3）制得的羧基化碳纳米管分散液置于超声清洗机中进行超声分散，同时将步骤（4）中得到的表面改性后的TPU电纺纤维膜浸入超声处理中的羧基化碳纳米管分散液中，10s取出，并在60℃下烘干30min，得到吸附一次碳纳米管的TPU电纺纤维膜。
（6）将步骤（3）制得的纳米氧化铝分散液置于超声清洗机中进行超声分散，将步骤（5）得到的吸附一次碳纳米管的TPU电纺纤维膜浸入超声处理中的纳米氧化铝分散液中，10s取出，并在60℃下烘干30min，得到循环吸附一次碳纳米管、氧化铝的TPU电纺纤维膜。
（7）将步骤（6）中得到的循环吸附一次碳纳米管、氧化铝的TPU电纺纤维膜重复（4）-（6）的过程5次，得到循环吸附五次碳纳米管、纳米氧化铝的TPU电纺纤维膜。
（8）按照步骤（4）-（6）的过程制备循环吸附五次碳纳米管、纳米氧化铝的聚酰胺无纺布。
（9）将步骤（8）得到的循环吸附五次碳纳米管、纳米氧化铝的聚酰胺无纺布经双辊压延机进行第一次压延得到中间层薄膜。压延工艺参数为：温度280℃，压力15MPa，速度0.6m/min。
（10）将步骤（9）得到的中间层薄膜两侧附上步骤（7）得到的循环吸附五次碳纳米管、纳米氧化铝的TPU电纺纤维膜，经双辊压延机进行第二次热压延，得到夹层结构导热复合薄膜。压延工艺参数为：温度150℃，压力30MPa，速度0.8m/min。
经过上述步骤，制得一种夹层结构高导热复合薄膜，如图1和图2所示。
制得的导热复合薄膜使用激光闪光法进行导热性能测试，该薄膜的面内导热系数为8.32W/mK，垂直导热系数为1.98W/mK。
实施例2：
一种氨纶/PET无纺布夹层结构高导热复合薄膜的制备方法，包括如下步骤：
（1）配制银纳米线、氮化硼纳米片分散液，以及聚乙烯亚胺溶液：
分别取2g银纳米线与2g氮化硼纳米片，分别加入两份100ml去离子水中，搅拌均匀后分别使用超声清洗机进行超声分散2h，得到浓度为20mg/ml的银纳米线分散液和氮化硼纳米片分散液。
取1g聚乙烯亚胺溶于100ml去离子水中，搅拌至均一溶液，得到浓度为10mg/ml的聚乙烯亚胺溶液。
（2）将PET无纺布裁剪成若干30cm×30cm的正方形薄膜，浸入步骤（1）得到的聚乙烯亚胺溶液中，10s后取出，得到表面改性后的PET无纺布。
（3）将步骤（1）制得的银纳米线分散液置于超声清洗机中进行超声分散，同时将步骤（2）中得到的表面改性后的PET无纺布浸入超声处理中的银纳米线分散液中，10s取出，并在60℃下烘干30min，得到吸附一次银纳米线的PET无纺布。
（4）将步骤（1）制得的氮化硼纳米片分散液置于超声清洗机中进行超声分散，将步骤（3）得到的吸附一次银纳米线的PET无纺布浸入超声处理中的氮化硼纳米片分散液中，10s取出，并在60℃下烘干30min，得到循环吸附一次银纳米线、氮化硼纳米片的PET无纺布。
（5）将步骤（4）中得到的循环吸附一次银纳米线、氮化硼纳米片的PET无纺布重复（2）-（4）的过程5次，得到循环吸附五次银纳米线、氮化硼纳米片的PET无纺布。
（6）按照步骤（2）-（5）的过程制备循环吸附五次银纳米线、氮化硼纳米片的氨纶无纺布。
（7）将步骤（5）得到的循环吸附五次银纳米线、氮化硼纳米片的PET无纺布经双辊压延机进行第一次压延得到中间层薄膜。压延工艺参数为：温度270℃，压力15MPa，速度0.6m/min。
（8）将步骤（7）得到的中间层薄膜两侧附上步骤（6）得到的循环吸附五次银纳米线、氮化硼纳米片的氨纶无纺布，经双辊压延机进行第二次热压延，得到夹层结构导热复合薄膜。压延工艺参数为：温度150℃，压力30MPa，速度0.8m/min。
经过上述步骤，制得一种夹层结构导热复合薄膜。
制得的导热复合薄膜使用激光闪光法进行导热性能测试，该薄膜的面内导热系数为8.57W/mK，垂直导热系数为2.12W/mK。
实施例3：
一种TPU/PVDF电纺纤维膜夹层结构高导热复合薄膜的制备方法，包括如下步骤：
（1）将聚氨酯粉末溶于体积比为1：3的N，N-二甲基甲酰胺和四氢呋喃的混合溶液中，室温下搅拌3h，配制质量分数为10%的TPU静电纺丝溶液；将PVDF粉末溶于N,N-二甲基甲酰胺中和丙酮2:1混合溶液中，室温下搅拌3h，配制质量分数为16%的PVDF静电纺丝溶液。
（2）分别取步骤（1）中的电纺溶液10ml通过静电纺丝设备进行静电纺丝，使用辊筒式接收器进行接收，分别得到弹性TPU电纺纤维膜和PVDF电纺纤维膜。TPU电纺参数：电压为12-15KV、喷头到接收器的距离为15-18cm，喷丝速度为80mm/min、温度为40℃，接收器转速为400rpm；PVDF电纺参数：电压为12-15KV、喷头到接收器的距离为17-18cm，喷丝速度为80mm/min、温度为40℃，接收器转速为400rpm。
（3）配制碳化硅纳米线、氮化硼纳米片分散液，以及聚乙烯亚胺溶液：
分别取2g碳化硅纳米线与2g氮化硼纳米片，分别加入两份100ml去离子水中，搅拌均匀后分别使用超声清洗机进行超声分散2h，得到浓度为20mg/ml的碳化硅纳米线分散液和氮化硼纳米片分散液。
取1g聚乙烯亚胺溶于100ml去离子水中，搅拌至均一溶液，得到浓度为10mg/ml的聚乙烯亚胺溶液。
（4）将步骤（2）中得到的TPU电纺纤维膜裁剪成若干30cm×30cm的正方形薄膜，浸入步骤（3）得到的聚乙烯亚胺溶液中，10s后取出，得到表面改性后的电纺纤维膜。
（5）将步骤（3）制得的碳化硅纳米线分散液置于超声清洗机中进行超声分散，同时将步骤（4）中得到的表面改性后的TPU电纺纤维膜浸入超声处理中的碳化硅纳米线分散液中，10s取出，并在60℃下烘干30min，得到吸附一次碳化硅纳米线的TPU电纺纤维膜。
（6）将步骤（3）制得的氮化硼纳米片分散液置于超声清洗机中进行超声分散，将步骤（5）得到的吸附一次碳化硅纳米线的TPU电纺纤维膜浸入超声处理中的氮化硼纳米片分散液中，10s取出，并在60℃下烘干30min，得到循环吸附一次碳化硅纳米线、氮化硼纳米片的TPU电纺纤维膜。
（7）将步骤（6）中得到的循环吸附一次碳化硅纳米线、氮化硼纳米片的TPU电纺纤维膜重复（4）-（6）的过程5次，得到循环吸附五次碳化硅纳米线、氮化硼纳米片的TPU电纺纤维膜。
（8）按照步骤（4）-（6）的过程制备循环吸附五次碳化硅纳米线、氮化硼纳米片的PVDF电纺纤维膜。
（9）将步骤（8）得到的循环吸附五次碳化硅纳米线、氮化硼纳米片的PVDF电纺纤维膜无纺布经双辊压延机进行第一次压延得到中间层薄膜。压延工艺参数为：温度150℃，压力15MPa，速度0.6m/min。
（10）将步骤（9）得到的中间层薄膜两侧附上步骤（7）得到的循环吸附五次碳化硅纳米线、氮化硼纳米片的TPU电纺纤维膜，经双辊压延机进行第二次热压延，得到夹层结构导热复合薄膜。压延工艺参数为：温度150℃，压力30MPa，速度0.8m/min。
经过上述步骤，制得一种夹层结构导热复合薄膜。
制得的导热复合薄膜使用激光闪光法进行导热性能测试，该薄膜的面内导热系数为9.68W/mK，垂直导热系数为1.83W/mK。
实施例4
一种氨纶无纺布/PVDF电纺纤维膜夹层结构高导热复合薄膜的制备方法，包括如下步骤：
（1）将PVDF粉末溶于体积比为2:1的N,N-二甲基甲酰胺和丙酮混合溶液中，室温下搅拌3h，配制质量分数为16%的PVDF电纺丝溶液。
（2）取步骤（1）中的电纺溶液10ml通过静电纺丝设备进行静电纺丝，使用辊筒式接收器进行接收，得到PVDF电纺纤维膜。PVDF电纺参数：电压为12-15KV、喷头到接收器的距离为17-18cm，喷丝速度为80mm/min、温度为40℃，接收器转速为400rpm。
（3）配制羧基化碳纳米管、四针状氧化锌分散液，以及聚乙烯亚胺溶液：
分别取2g羧基化碳纳米管与2g四针状氧化锌，分别加入两份100ml去离子水中，搅拌均匀后分别使用超声清洗机进行超声分散2h，得到浓度为20mg/ml的羧基化碳纳米管分散液和四针状氧化锌分散液。
取1g聚乙烯亚胺溶于100ml去离子水中，搅拌至均一溶液，得到浓度为10mg/ml的聚乙烯亚胺溶液。
（4）将步骤（2）中得到的PVDF电纺纤维膜裁剪成若干30cm×30cm的正方形薄膜，浸入步骤（3）得到的聚乙烯亚胺溶液中，10s后取出，得到表面改性后的电纺纤维膜。
（5）将步骤（3）制得的羧基化碳纳米管分散液置于超声清洗机中进行超声分散，同时将步骤（4）中得到的表面改性后的PVDF电纺纤维膜浸入超声处理中的羧基化碳纳米管分散液中，10s取出，并在60℃下烘干30min，得到吸附一次碳纳米管的PVDF电纺纤维膜。
（6）将步骤（3）制得的四针状氧化锌分散液置于超声清洗机中进行超声分散，将步骤（5）得到的吸附一次碳纳米管的PVDF电纺纤维膜浸入超声处理中的四针状氧化锌分散液中，10s取出，并在60℃下烘干30min，得到循环吸附一次碳纳米管、四针状氧化锌的PVDF电纺纤维膜。
（7）将步骤（6）中得到的循环吸附一次碳纳米管、四针状氧化锌的PVDF电纺纤维膜重复（4）-（6）的过程5次，得到循环吸附五次碳纳米管、四针状氧化锌的PVDF电纺纤维膜。
（8）按照步骤（4）-（6）的过程制备循环吸附五次碳纳米管、四针状氧化锌的氨纶无纺布。
（9）将步骤（8）得到的循环吸附五次碳纳米管、四针状氧化锌的PVDF电纺纤维膜无纺布经双辊压延机进行第一次压延得到中间层薄膜。压延工艺参数为：温度150℃，压力15MPa，速度0.6m/min。
（10）将步骤（9）得到的中间层薄膜两侧附上步骤（7）得到的循环吸附五次碳纳米管、氮化硼纳米片的氨纶无纺布，经双辊压延机进行第二次热压延，得到夹层结构导热复合薄膜。压延工艺参数为：温度150℃，压力30MPa，速度0.8m/min。
经过上述步骤，制得一种夹层结构导热复合薄膜。
制得的导热复合薄膜使用激光闪光法进行导热性能测试，该薄膜的面内导热系数为7.53W/mK，垂直导热系数为1.77W/mK。

Claims (4)

1.一种夹层结构高导热复合薄膜，其特征在于，该复合薄膜具有3层结构，由上下表面的弹性纤维薄膜层和中间的非弹性纤维薄膜层热压延复合而成，其中所述弹性纤维薄膜层和非弹性纤维薄膜层中均含有零维、一维导热填料、二维导热填料和异形导热填料中的至少两种；该复合薄膜的制备方法包括如下步骤：
1）分别将不同导热填料加入去离子水和表面改性剂中分散均匀，得到不同导热填料分散液；
2）将表面改性剂加入去离子水和无水乙醇的混合溶液中分散均匀，得到表面改性剂溶液；
3）分别将弹性纤维薄膜和非弹性纤维薄膜完全浸入步骤2）制得的表面改性剂溶液中浸渍10-30s，得到表面改性的弹性纤维薄膜和非弹性纤维薄膜；
4）将步骤3）得到的表面改性的弹性纤维薄膜和非弹性纤维薄膜分别先后浸入步骤1）制得的不同导热填料分散液中的一种中浸渍10-30s，每浸渍完1种导热填料分散液后，于50-80℃下烘干，再浸入一种导热填料分散液中并烘干，如此重复进行表面改性和吸附过程2-10次，分别制得均匀吸附有零维导热填料、一维导热填料、二维导热填料和异形导热填料中至少两种的弹性纤维薄膜和非弹性纤维薄膜；
5）将步骤4）制得吸附填料的非弹性纤维薄膜进行第一次热压延，再将步骤4）制得的吸附填料的弹性纤维薄膜分别置于热压延后的非弹性纤维薄膜上下表面再进行第二次热压延后，制得夹层结构的高导热复合薄膜；
所述的表面改性剂为聚乙烯亚胺；
所述的异形导热填料，为四针状氧化锌ZnO、膨胀石墨EG中的至少一种，其粒径为500nm-100μm。
2.根据权利要求1所述的一种夹层结构高导热复合薄膜，其特征在于，所述的弹性纤维薄膜层，是PU、聚烯烃、聚苯乙烯-丁二烯嵌段共聚物、聚酯酰胺热塑性弹性体材料制备的纤维薄膜或无纺布中的一种，纤维直径为50nm-50μm，面密度为10g-30g/m2；
所述的非弹性纤维薄膜层，为聚四氟乙烯、聚酰胺、聚乳酸、聚丙烯、聚丙烯腈、聚对苯二甲酸乙二醇酯、芳纶、聚酰亚胺纤维薄膜或无纺布中的一种，纤维直径为50nm-50μm，面密度为10g-30g/m2。
3.根据权利要求1所述的一种夹层结构高导热复合薄膜，其特征在于，所述的零维导热填料，为球形氧化铝Al2O3、球形氮化铝AlN中的至少一种，其粒径为500nm-100μm；
所述的一维导热填料，为羧基化碳纳米管CNTs、氮化碳纳米管CNNTs、碳化硅纳米线SiCNWs、银纳米线AgNWs中的至少一种，其长度为10μm-200μm；
所述的二维导热填料，为氮化硼纳米片BNNS、石墨烯纳米片GNPs、MXene中的至少一种，其粒径为100nm-5μm，厚度为5nm-100nm。
4.根据权利要求1所述的一种夹层结构高导热复合薄膜，其特征在于，所述的第一次热压延，热压延工艺为：温度为100-300℃，压力为1-30MPa，压延速度为0.01-10m/min；
所述的第二次热压延，热压延工艺为：温度为50-200℃，压力为1-50MPa，压延速度为0.01-10m/min。
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