CN115368758A - 一种非离子表面活性剂非共价改性氮化硼导热填料及基于其的导热复合材料 - Google Patents
一种非离子表面活性剂非共价改性氮化硼导热填料及基于其的导热复合材料 Download PDFInfo
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 16
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
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Abstract
本发明公开了一种非离子表面活性剂非共价改性氮化硼导热填料及基于其的导热复合材料,是将壬基酚聚氧乙烯醚接枝在BN上获得导热填料NP@BN,然后将聚偏氟乙烯与NP@BN通过热压的方法获得导热复合材料。本发明的方法可以通过非离子表面活性剂壬基酚聚氧乙烯醚与BN之间形成的非共价作用,改善填料与基体间的相容性及分散性,使填料在基体中均匀分散以降低界面热阻,从而提高复合材料的导热性能。
Description
技术领域
本发明涉及导热复合材料技术领域,具体涉及一种非离子表面活性剂非共价改性BN导热填料及基于其的导热复合材料。
背景技术
如今,高度集成的电子设备将不可避免地遇到散热问题,优异的散热能力意味着累积的热量可以迅速消散,从而可提高器件的可靠性和寿命。高分子材料中界面热阻的调控和热传递路径的构筑是提升聚合物基复合材料导热性能的有效途径。而提高高分子材料导热性能较为经济实用的方法是掺入高导热填料。
对导热填料进行改性可以有效调控填料间界面热阻,改性方法包括共价改性和非共价改性。其中,共价改性虽然能通过化学键在填料间构筑热传导路径,但其会破坏填料固有结构,影响复合材料的导热性能。而非共价改性在保证填料本身导热性能的基础上,通过诸如氢键相互作用、静电相互作用等方式降低填料间界面热阻,故非共价改性成为当前填料改性的主流方式。六方氮化硼是一种高导热、耐高温的高绝缘材料。目前,通过强酸、强碱、高分子化合物等对BN改性,不仅工艺复杂,而且会破坏BN的结构,以致影响复合材料的热性能。
发明内容
基于上述现有技术所存在的问题,本发明提供一种非离子表面活性剂非共价改性BN导热填料及基于其的导热复合材料,通过将壬基酚聚氧乙烯醚与BN进行非共价连接,改善填料与基体间的相容性及分散性,使填料在基体中均匀分散以降低界面热阻,从而提高复合材料的导热性能。
为了实现上述目的,本发明采用以下技术方案:
本发明首先公开了一种非离子表面活性剂非共价改性氮化硼导热填料的制备方法,其特点在于:首先将六方氮化硼与壬基酚聚氧乙烯醚研磨混合均匀,得到混合液;然后将所述混合液分散在丙酮中,磁力搅拌均匀后,再超声处理2-3h,获得非共价改性氮化硼导热填料,记为NP@BN。具体包括如下步骤:
将0.04-0.2gh-BN和0.2-1mL壬基酚聚氧乙烯醚混合,在玛瑙碗中手动研磨15-30分钟,得到混合液;将所得混合液分散在5-10mL丙酮中,先磁力搅拌10-30分钟,再在30℃以下超声处理2-3小时,然后以4000rpm离心5-10分钟,去除上清液,即获得非共价改性氮化硼导热填料NP@BN。
本发明还公开了基于所述NP@BN导热填料的导热复合材料,其特点在于:将聚偏氟乙烯PVDF与NP@BN通过热压法复合,即获得聚偏氟乙烯基非共价改性氮化硼导热复合材料,记为NP@BN/PVDF。其中,所述NP@BN的加入量占导热复合材料总质量的1%~15%。
本发明所述导热复合材料的制备方法为:在10mLN,N-二甲基甲酰胺DMF中加入1~3gPVDF,在60℃油浴下搅拌至PVDF完全溶解,然后加入所述NP@BN导热填料,超声混合均匀,获得涂覆液;将所述涂覆液均匀涂覆在玻璃板上,干燥去除DMF,然后再热压,即获得NP@BN/PVDF。
进一步地,所述干燥是在烘箱中120℃干燥1h。
进一步地,所述热压是在180℃、10Mpa热压5分钟。
本发明的有益效果体现在:
本发明选用壬基酚聚氧乙烯醚对BN进行改性,其是一种非离子表面活性剂,在水溶液中不会离子化,稳定性高,并且与填料有良好的相容性。本发明的方法可以通过非离子表面活性剂壬基酚聚氧乙烯醚与BN之间形成的非共价作用,改善填料与基体间的相容性及分散性,使填料在基体中均匀分散以降低界面热阻,从而提高复合材料的导热性能。
附图说明
图1为本发明实施例1所得NP@BN的SEM图,其中(a)、(b)对应不同放大倍数;
图2为本发明实施例1所得NP@BN/PVDF的SEM图,其中(a)、(b)对应不同放大倍数;
图3为本发明实施例1和对比例1所得各样品的导热性能图。
具体实施方式
下面对本发明的实施例作详细说明,本实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。
实施例1
本实施例按如下步骤制备NP@BN/PVDF导热复合材料:
步骤1、NP@BN的制备
将0.1g六方氮化硼和0.25mL壬基酚聚氧乙烯醚(NP-10)混合,在玛瑙碗中手动研磨20分钟,得到混合液;将所得混合液分散在10mL丙酮中,先磁力搅拌20分钟,再在25℃超声处理2小时,然后以4000rpm离心5-10分钟,去除上清液,即获得非共价改性氮化硼导热填料NP@BN。
步骤2、NP@BN/PVDF的制备
在10mLN,N-二甲基甲酰胺DMF中加入1gPVDF,在60℃油浴下搅拌至PVDF完全溶解,然后加入步骤1制备的NP@BN,超声混合均匀,获得涂覆液;
将涂覆液均匀涂覆在玻璃板上,烘箱中120℃干燥1h去除DMF,然后再在180℃、10Mpa热压5分钟,即获得NP@BN/PVDF。控制NP@BN的加入量分别占复合材料质量的0%、1%、5%、10%、15%。
对比例1
本对比例按如下步骤制备BN/PVDF导热复合材料:
在10mLN,N-二甲基甲酰胺DMF中加入1gPVDF,在60℃油浴下搅拌至PVDF完全溶解,然后加入h-BN,超声混合均匀,获得涂覆液;
将涂覆液均匀涂覆在玻璃板上,烘箱中120℃干燥1h去除DMF,然后再在180℃、10Mpa热压5分钟,即获得BN/PVDF。控制h-BN的加入量分别占复合材料质量的0%、1%、5%、10%、15%。
图1为实施例1所得NP@BN的SEM图,从图中可以看出,改性后的h-BN被剥离成层数较少的片层,利于热量的传递。
图2为实施例1所得NP@BN/PVDF的SEM图,可以看出填料与基体相容性较好,使导热性能得到提升。
图3为各样品的导热性能测试结果,相比于纯PVDF,NP@BN/PVDF的导热性能有明显提高,且在15wt%填充量下热导率达到2.07W/(mK),相对于纯PVDF的0.230W/(mK)提高了800%。
本发明通过非离子表面活性剂壬基酚聚氧乙烯醚与BN之间形成的非共价作用,改善填料与基体间的相容性及分散性,使填料在基体中均匀分散以降低界面热阻,从而提高了复合材料的导热性能。
以上仅为本发明的示例性实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所做的任何修改,等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (8)
1.一种非离子表面活性剂非共价改性氮化硼导热填料的制备方法,其特征在于:首先将六方氮化硼与壬基酚聚氧乙烯醚研磨混合均匀,得到混合液;然后将所述混合液分散在丙酮中,磁力搅拌均匀后,再超声处理2-3h,获得非共价改性氮化硼导热填料,记为NP@BN。
2.根据权利要求1所述的制备方法,其特征在于,包括如下步骤:
将0.04-0.2gh-BN和0.2-1mL壬基酚聚氧乙烯醚混合,在玛瑙碗中手动研磨15-30分钟,得到混合液;将所得混合液分散在5-10mL丙酮中,先磁力搅拌10-30分钟,再在30℃以下超声处理2-3小时,然后以4000rpm离心5-10分钟,去除上清液,即获得非共价改性氮化硼导热填料NP@BN。
3.一种权利要求1~2中任意一项所述制备方法所获得的NP@BN导热填料。
4.一种基于权利要求3所述NP@BN导热填料的导热复合材料,其特征在于:将聚偏氟乙烯PVDF与NP@BN通过热压法复合,即获得聚偏氟乙烯基非共价改性氮化硼导热复合材料,记为NP@BN/PVDF。
5.根据权利要求4所述的导热复合材料,其特征在于:所述NP@BN的加入量占导热复合材料总质量的1%~15%。
6.一种权利要求4或5所述导热复合材料的制备方法,其特征在于:在10mLN,N-二甲基甲酰胺DMF中加入1~3g PVDF,在60℃油浴下搅拌至PVDF完全溶解,然后加入所述NP@BN导热填料,超声混合均匀,获得涂覆液;
将所述涂覆液均匀涂覆在玻璃板上,干燥去除DMF,然后再热压,即获得NP@BN/PVDF。
7.根据权利要求6所述的制备方法,其特征在于:所述干燥是在烘箱中120℃干燥1h。
8.根据权利要求6所述的制备方法,其特征在于:所述热压是在180℃、10Mpa热压5分钟。
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