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CN113264770A - 一种抗弯折MXene/碳复合材料散热膜制备方法 - Google Patents

一种抗弯折MXene/碳复合材料散热膜制备方法 Download PDF

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CN113264770A
CN113264770A CN202110583225.4A CN202110583225A CN113264770A CN 113264770 A CN113264770 A CN 113264770A CN 202110583225 A CN202110583225 A CN 202110583225A CN 113264770 A CN113264770 A CN 113264770A
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mxene
heat dissipation
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张鑫
路馨语
牛永安
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Shenyang University of Chemical Technology
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Abstract

本发明公开了一种抗弯折MXene/碳复合材料散热膜制备方法，涉及一种复合材料散热膜制备方法，首先采用聚酰亚胺（polyimide）作为基体，刻蚀MAX相得到的MXene颗粒作为增强材料，易成碳聚合物作为中间层，经过充分混合、反应、涂膜、固化形成MXene/成碳聚合物/聚酰亚胺复合膜。其次将制备的MXene/成碳聚合物/聚酰亚胺复合膜装入高温碳化炉中，保护气氛下进行高温热解与碳化形成MXene/碳复合材料。最后用水与乙醇反复清洗其表面，获得抗弯折MXene/碳复合材料散热膜。该方法制备的MXene/碳复合材料散热膜不仅具备优异的耐热性以及散热性，且其质轻强度高，具有突出的抗弯折性能，可用于大功率电子设备、LED背底、微电子与传感器件等散热。

Description

一种抗弯折MXene/碳复合材料散热膜制备方法
技术领域
本发明涉及一种散热膜制备方法，特别是涉及一种抗弯折MXene/碳复合材料散热膜制备方法。
背景技术
5G、6G网络高速发展阶段，智能手机、笔记本电脑等智能设备离不开CPU等芯片，芯片与散热器之间存在很多沟壑或空隙，充斥着大量空气，然而空气的热阻值很高，因此通常采用其他介质降低热阻。特别是，智能机及电脑等电子设备终究归向便携式、多功能化的方向发展，在方便生活的同时，由于散热问题，同时也成为威胁人类安全的隐患。因此，芯片散热问题也是电子领域的研究热点。
常用的导热硅胶、硅脂由于其黏着性很强，残留物很难清除；而碳化的聚酰亚胺（polyimide）膜，由于其具有低密度、高散热性、能有效反射电磁波和较高的导热系数等优点，具有广阔的应用前景。现在大部分电子设备的散热膜是石墨膜及复合石墨膜、碳化的聚酰亚胺膜等材料，其中石墨膜制备复杂、密度较大、难以成型，制备出的膜厚度为0.1mm左右，其结构缺陷多、散热性较差；碳化的聚酰亚胺膜的厚度通常只有几微米(μm)，其密度较小、散热较好，但柔韧性差、不易存储运输，在装备使用过程中消耗过大，所以仅使用纯的碳化聚酰亚胺膜的成本造价过高。
MXene材料柔韧度强、密度低，且导热性好。MXene材料一般是由M层和X层组成，M可以是Ti，X可以是C，因此具有很好的稳定性。MXene可以在聚合物中自由运动获得均匀分布，在很大程度上保留了MXene的二维层片状结构特性而不被破坏，为制备具有优异机械柔韧性的MXene复合材料提供了可能性。由于MXene是二维层状结构，原子和原子之间存在较大空隙，所以在与聚合物进行复合时，一些聚合物分子可分布在双层结构之间，形成了良好的导热通路，实现力学与导热性能协同增强。因此，将MXene材料和碳化的聚酰亚胺复合制备散热膜，不仅制备方法简单、可行性强，且成本低，能够较好地弥补单一碳化聚酰亚胺膜的性能不足。
发明内容
本发明的目的在于提供一种抗弯折MXene/碳复合材料散热膜制备方法，该方法将MXene材料分散在DMAc等有机溶剂中，使MXene能够与聚酰亚胺前驱体均匀地混合，方法简单，易于操作；所加入层状MXene材料，有效地弥补纯聚酰亚胺碳化后柔韧性的不足，制备的MXene/碳复合材料具有较高的导热性、柔韧性和综合性能，解决了现有散热膜不抗弯折的问题。
本发明的目的是通过以下技术方案实现的：
一种抗弯折MXene/碳复合材料散热膜制备方法，所述方法包括如下制备步骤：
（1）将易成碳聚合物和MXene颗粒溶于极性溶剂中，超声、搅拌形成均匀、稳定的混合溶液；
（2）将上述混合溶液按比例加入到聚酰亚胺前驱体溶液中，搅拌、共混形成MXene/易成聚合物/聚酰亚胺复合前驱体；
（3）采用涂膜工艺涂覆于平板形成前驱体膜，放入固化炉中，经过热固化形成具有三层结构的MXene/易成聚合物/聚酰亚胺复合膜；
（4）将MXene/易成聚合物/聚酰亚胺复合膜放入碳化炉，在惰性气体保护氛围下进行高温碳化，降温冷却后再用溶剂清洗其表面，制得抗弯折MXene/碳复合材料散热膜。
所述的一种抗弯折MXene/碳复合材料散热膜制备方法，所述步骤（1）中易成碳聚合物为碳含量大于50%的聚醚醚酮、聚酰亚胺、环氧树脂、酚醛树脂、双马来酰亚胺、聚芳炔中的任意一个或任意组合。
所述的一种抗弯折MXene/碳复合材料散热膜制备方法，所述步骤（1）中MXene颗粒是二维层状结构Ti2C、Ti3C2、Ti2N、Ti3N2、Ti4N3、Ti3(CN)、Zr2C、Zr3C2、Zr2N、Zr3N2、Zr3N3、Hf2C、Hf2C3、Hf2N、Hf3N2、Hf3N3、V2C、V4C3、V2N、V2N2、V2N3、Cr2C、Cr2C2、Cr2N、Mo2C、Mo2C2、Mo2N、Nb2C、Nb4C3、Nb2N、Ta2C、Ta4C3、Ta2N、Sc2C中的任意一个或任意组合，平均厚度为0.1~10nm，平均粒径为10~10000nm，使用前需经过1~50wt%的氢氟酸刻蚀0.5~12h。
所述的一种抗弯折MXene/碳复合材料散热膜制备方法，所述步骤（1）中极性溶剂为水、甲醇、乙醇、甲苯、甲酰胺、三氟乙酸、二甲基亚砜、乙腈、N，N-二甲基甲酰胺（DMF）、N，N-二甲基乙酰胺（DMAc）、六甲基磷酰胺、乙酸、异丙醇、吡啶、四甲基乙二胺、丙酮、三乙胺、正丁醇、二氧六环、四氢呋喃、甲酸甲酯、三丁胺、甲乙酮、乙酸乙酯、氯仿、三辛胺、碳酸二甲酯、乙醚、异丙醚、正丁醚、三氯乙烯、二苯醚、二氯甲烷、二氯乙烷、环己烷、N-甲基吡咯烷酮中的一种或以任意比例组合。
所述的一种抗弯折MXene/碳复合材料散热膜制备方法，所述步骤（1）中易成碳聚合物为极性溶剂用量的0.01~20wt%，MXene颗粒为极性溶剂用量的0.01~40wt%，搅拌时间为0.1~5小时，形成均匀稳定的混合溶液为胶体溶液。
所述一种抗弯折MXene/碳复合材料散热膜制备方法，所述步骤（2）中聚酰亚胺前驱体为聚酰亚胺、聚酰胺酸或其衍生物的溶液，浓度为0.1~50wt%，溶剂为上述权利要求4所指的极性溶剂，前驱体的用量为MXene颗粒用量的0.1~500倍，搅拌时间为0.1~5小时。
所述的一种抗弯折MXene/碳复合材料散热膜制备方法，所述步骤（3）中涂膜工艺包括旋涂、刮涂、喷涂、蘸涂、滴涂、模具法、半烘干法。
所述的一种抗弯折MXene/碳复合材料散热膜制备方法，所述步骤（3）中混合溶液涂覆成膜，在涂覆过程中控制膜的厚度在0.1~1000μm之间；固化过程温度为100~500℃，保温时间为0.1~24小时。
所述的一种抗弯折MXene/碳复合材料散热膜制备方法，所述步骤（4）中碳化膜的清洗采用水或乙醇反复清洗1~5次。
所述的一种抗弯折MXene/碳复合材料散热膜制备方法，所述步骤（4）中惰性气体为氮气、氩气、氦气中的任意一种或任意组合；碳化温度为500~2000℃，保温时间为0.1~24小时。
本发明的优点与效果是：
（1）本发明通过加热、再混合的方法将MXene材料分散在DMAc等有机溶剂中，使MXene能够与聚酰亚胺前驱体均匀地混合，方法简单，易于操作；
（2）本发明所加入了层状MXene材料，呈双层结构，同层原子紧密排列，显示出良好的柔韧性，将其与聚酰亚胺复合碳化，可以有效地弥补纯聚酰亚胺碳化后柔韧性的不足。
（3）MXene和聚酰亚胺为主要原料制备的MXene/碳复合材料具有较高的导热性、柔韧性和综合性能，能解决现有散热膜不抗弯折的问题。
附图说明
图1是MXene/碳复合材料的微观形貌图；
图2是MXene/碳复合材料散热效果模拟图；
图3是不同温度下制备的MXene/碳复合材料的XRD图谱。
具体实施方式
下面结合附图所示实施例对本发明进行详细说明。
实施例1
首先，将0.5g洗涤、干燥后的Ti3C2的MXene颗粒加入0.1g的易成碳聚酰亚胺和20mL的N，N-二甲基乙酰胺超声分散，搅拌1小时后形成包覆易成碳聚酰亚胺包覆的Ti3C2胶体溶液。其次，将5g的聚酰胺酸前驱体溶液加入胶体溶液，搅拌溶液1小时使其混合、摇匀，制得MXene/易成碳聚酰亚胺/聚酰胺酸混合前驱体溶液；然后，将上述混合前驱体溶液喷涂于基板上，放入固化炉中在100℃，200℃分别处理2小时，再升温到300℃固化3小时，制备的MXene/易成碳聚酰亚胺/聚酰亚胺复合膜。最后，将上述复合膜放入高温碳化炉中，在氮气保护下升温到1500℃，保温2h，待冷却后取出，用水与乙醇分别清洗3次，得到的抗弯折MXene/碳复合材料散热膜。经测试，散热膜的导热系数为217W/mK，面密度为84.76g/m2，失重率为40.64%。
实施例2
首先，将0.6g洗涤、干燥后的Ti2N的MXene颗粒加入0.06g的易成碳双马来酰亚胺和15mL的N，N-二甲基乙酰胺超声分散，搅拌2小时后形成包覆易成碳聚酰亚胺包覆的Ti2N胶体溶液。其次，将10g的聚酰亚胺前驱体溶液加入胶体溶液，搅拌溶液1.5小时使其混合、摇匀，制得MXene/易成碳双马来酰亚胺/聚酰亚胺混合前驱体溶液；然后，将上述混合前驱体溶液刮涂于基板上，放入固化炉在100℃，200℃，300℃分别处理2小时，再升温到350℃固化1小时，制备的产物MXene/易成碳双马来酰亚胺/聚酰亚胺复合膜。最后，将上述复合膜放入高温碳化炉中，在氩气保护下升温到1400℃，保温3h，待冷却后取出，得到的抗弯折MXene/碳复合材料散热膜。经测试，散热膜的导热系数为201W/mK，面密度为85.56g/m2，失重率为40.33%。
以上实施例并不是全部实施方式的列举。在本发明基础上的步骤替换、变换、改进等实现制备抗弯折MXene/碳复合材料散热膜的技术方案，也在本发明的权利要求范围之内。

Claims (10)

1.一种抗弯折MXene/碳复合材料散热膜制备方法，其特征在于，所述方法包括如下制备步骤：
（1）将易成碳聚合物和MXene颗粒溶于极性溶剂中，超声、搅拌形成均匀、稳定的混合溶液；
（2）将上述混合溶液按比例加入到聚酰亚胺前驱体溶液中，搅拌、共混形成MXene/易成聚合物/聚酰亚胺复合前驱体；
（3）采用涂膜工艺涂覆于平板形成前驱体膜，放入固化炉中，经过热固化形成具有三层结构的MXene/易成聚合物/聚酰亚胺复合膜；
（4）将MXene/易成聚合物/聚酰亚胺复合膜放入碳化炉，在惰性气体保护氛围下进行高温碳化，降温冷却后再用溶剂清洗其表面，制得抗弯折MXene/碳复合材料散热膜。
2.根据权利要求1所述的一种抗弯折MXene/碳复合材料散热膜制备方法，其特征在于，所述步骤（1）中易成碳聚合物为碳含量大于50%的聚醚醚酮、聚酰亚胺、环氧树脂、酚醛树脂、双马来酰亚胺、聚芳炔中的任意一个或任意组合。
3.根据权利要求1所述的一种抗弯折MXene/碳复合材料散热膜制备方法，其特征在于，所述步骤（1）中MXene颗粒是二维层状结构Ti2C、Ti3C2、Ti2N、Ti3N2、Ti4N3、Ti3(CN)、Zr2C、Zr3C2、Zr2N、Zr3N2、Zr3N3、Hf2C、Hf2C3、Hf2N、Hf3N2、Hf3N3、V2C、V4C3、V2N、V2N2、V2N3、Cr2C、Cr2C2、Cr2N、Mo2C、Mo2C2、Mo2N、Nb2C、Nb4C3、Nb2N、Ta2C、Ta4C3、Ta2N、Sc2C中的任意一个或任意组合，平均厚度为0.1~10nm，平均粒径为10~10000nm，使用前需经过1~50wt%的氢氟酸刻蚀0.5~12h。
4.根据权利要求1所述的一种抗弯折MXene/碳复合材料散热膜制备方法，其特征在于，所述步骤（1）中极性溶剂为水、甲醇、乙醇、甲苯、甲酰胺、三氟乙酸、二甲基亚砜、乙腈、N，N-二甲基甲酰胺（DMF）、N，N-二甲基乙酰胺（DMAc）、六甲基磷酰胺、乙酸、异丙醇、吡啶、四甲基乙二胺、丙酮、三乙胺、正丁醇、二氧六环、四氢呋喃、甲酸甲酯、三丁胺、甲乙酮、乙酸乙酯、氯仿、三辛胺、碳酸二甲酯、乙醚、异丙醚、正丁醚、三氯乙烯、二苯醚、二氯甲烷、二氯乙烷、环己烷、N-甲基吡咯烷酮中的一种或以任意比例组合。
5.根据权利要求1所述的一种抗弯折MXene/碳复合材料散热膜制备方法，其特征在于，所述步骤（1）中易成碳聚合物为极性溶剂用量的0.01~20wt%，MXene颗粒为极性溶剂用量的0.01~40wt%，搅拌时间为0.1~5小时，形成均匀稳定的混合溶液为胶体溶液。
6.根据权利要求1所述一种抗弯折MXene/碳复合材料散热膜制备方法，其特征在于，所述步骤（2）中聚酰亚胺前驱体为聚酰亚胺、聚酰胺酸或其衍生物的溶液，浓度为0.1~50wt%，溶剂为上述权利要求4所指的极性溶剂，前驱体的用量为MXene颗粒用量的0.1~500倍，搅拌时间为0.1~5小时。
7.根据权利要求1所述的一种抗弯折MXene/碳复合材料散热膜制备方法，其特征在于，所述步骤（3）中涂膜工艺包括旋涂、刮涂、喷涂、蘸涂、滴涂、模具法、半烘干法。
8.根据权利要求1所述的一种抗弯折MXene/碳复合材料散热膜制备方法，其特征在于，所述步骤（3）中混合溶液涂覆成膜，在涂覆过程中控制膜的厚度在0.1~1000μm之间；固化过程温度为100~500℃，保温时间为0.1~24小时。
9.根据权利要求1所述的一种抗弯折MXene/碳复合材料散热膜制备方法，其特征在于，所述步骤（4）中碳化膜的清洗采用水或乙醇反复清洗1~5次。
10.根据权利要求1所述的一种抗弯折MXene/碳复合材料散热膜制备方法，其特征在于，所述步骤（4）中惰性气体为氮气、氩气、氦气中的任意一种或任意组合；碳化温度为500~2000℃，保温时间为0.1~24小时。
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