CN110563981A - 一种取向氮化硼复合膜的制备方法 - Google Patents
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Abstract
本发明涉及一种取向氮化硼复合膜的制备方法,具体为氮化硼接枝四氧化三铁以改善氮化硼在磁场中的响应性。通过氮化硼磁性体在磁场中的响应行为,使其在复合材料中形成定向的取向结构,以制备氮化硼的各向异性复合材料。本发明主要强调取向结构对介电性能的提高。本发明利用多巴胺的包覆作用以及它与四氧化三铁的耦合作用,实现了氮化硼与四氧化三铁结合,从而实现了氮化硼在磁场中取向,取向结构的形成提高了氮化硼复合材料的介电性能。本发明涉及的多巴胺对粒子包覆后与四氧化三铁耦合技术不仅可应用于氮化硼一种粒子,对于大多数粒子都可实现磁性改性和取向。
Description
【技术领域】
本发明涉及电器电子材料技术领域,特别涉及一种电容储能元件电子领域。
【背景技术】
各向异性复合材料因其性能在各个方向上有所不同,而且在某一方向上性能得到了很大的提升,因此得到了很广泛的使用,这类材料由于特有的各向异性结构和性能而应用于一些特殊的领域,例如用于电子封装材料的导电胶膜、柔性电极的取向碳纳米管等领域。制备各向异性复合材料成为当前研究热点,但是大多数粒子不具有简单制备各项异性材料的方式方法,于是提出改性,使其具有磁响应,从而制备各向异性的复合材料。
电子电力器件的小型化、集成化的发展与材料发展息息相关。电容作为电力电子元件的重要的部件,其小体积电容的实现需要高介电材料。保持大电容的情况下减小电容体积比较实际的做法是提高介电常数,通过制备各向异性复合材料来提高材料的介电常数。
氮化硼是一种片层材料,由硼元素和氮元素构成,有多种晶体,其中包括六方氮化硼和立方氮化硼等晶体。六方氮化硼为片层结构,导热性好,耐腐蚀,介电常数也比较高,填充到基体中能有效提高材料的导热性和介电常数,因此引起了人们的广泛关注和研究。
聚二甲基硅氧烷(PDMS)是一种主链由交替排列的硅原子和氧原子构成的高分子化合物,侧基和端基以主要是以烃基为主。PDMS总体上有导热性、表面张力小、耐寒性和耐热性等性质特点。其存在形式分固态和液态两种,液态的PDMS无色无味无毒呈现粘稠状,粘度随温度变化小。
利用电磁场作为动力介质能够诱导粒子发生取向排列的技术早在二十世纪八十年代就被人们发现,这是因为在外加磁场环境中,由于物质具有铁磁性,在施加磁场后会产生对液体介质中的粒子起主要影响的磁化作用。在这种环境下,粒子的热运动与磁场作用抗争,当磁场作用大于热运动时,粒子沿着磁场的方向的取向排列。
因此,本发明将通过对氮化硼磁性体/聚二甲基硅氧烷的复合材料在外加磁场的情况下进行加热固化,制备出一种高介电柔性膜。
【发明内容】
本发明意在提供一种利用氮化硼磁性体和PDMS制备高介电柔性膜的方法,以增加背景技术中提到物质的应用范围。为实现上述目的,提出了如下技术方案:
一种高介电柔性膜其制备包括如下步骤:
(1)氮化硼磁性体制备:将30ml PH=9.90的缓冲溶液与10ml无水乙醇混合起来,然后将0.2g六方氮化硼加入到该混合溶液中,超声30min。然后加入80mg的盐酸多巴胺,常温反应9小时,得到BN@PDA。
把0.2g三氯化铁加入到80ml乙二醇中,然后加入2.0g聚乙二醇和0.2g BN@PDA。超声5min,然后加入6.0g醋酸钠,在60℃下搅拌反应2h.然后转入反应釜中,在180℃反应9h,反应完后,用乙醇反复洗涤三次(离心转速7200转,离心时间30min),除去小分子。在60℃烘干干燥,得到BN-Fe3O4。
(2)制备氮化硼磁性体/聚二甲基硅氧烷复合材料:根据所需浓度比例取PDMS与BN-Fe3O4在非介质匀质机中混合均匀,按照固化剂和PDMS为1:10的比例加入固化剂并再用匀质机再真空状态下搅拌脱泡,脱泡后的混合液即液体形式的BN-Fe3O4/PDMS的复合材料。
(3)制备高介电柔性膜:利用玻璃制作所需模具,将制备BN-Fe3O4/PDMS的复合材料的液体倒入模具内部后在上层表面压上玻璃,上下两面覆盖加热片。利用电磁铁装置,产生外加磁场,对样品施加磁场作用力,其中磁场的强度为1020mT,,让样品在常温下取向两小时,然后再在100℃下取向十分钟,同时受热固化。
本发明不仅能对氮化硼进行磁场改性,使之在复合材料中进行取向提高材料的介电常数,而且对于大多数材料都能进行磁改性,使之在磁场下取向,增强某一项性能。
【附图说明】
图1是高介电柔性膜的制备方法流程图
图2是多巴胺材料在粒子表面接枝四氧化三铁
图3和图4是本发明实施例和对比例提供的氮化硼磁性体/PDMS复合膜的介电常数数据图
【具体实施方式】
下面将结合本次发明实施例对本发明中的技术方案进行详尽、清晰的描述。但本发明的保护范围不仅限于此,本领域技术人员依据本发明中的实施例在没有创造性劳动前提下所获得的其他所有其他实施例都应为本发明的保护范围。
实施例1.
将30ml PH=9.90的缓冲溶液与10ml无水乙醇混合起来,然后将0.2g六方氮化硼加入到该混合溶液中,超声30min。然后加入80mg的盐酸多巴胺,常温反应9小时,得到BN@PDA;把0.2g三氯化铁加入到80ml乙二醇中,然后加入2.0g聚乙二醇和0.2g BN@PDA。超声5min,然后加入6.0g醋酸钠,在60℃下搅拌反应2h.然后转入反应釜中,在180℃反应9h,反应完后,用乙醇反复洗涤三次(离心转速7200转,离心时间30min),除去小分子。在60℃烘干干燥,得到BN-Fe3O4;称取9g PDMS与0.1g BN-Fe3O4在非介质匀质机中混合均匀,按照固化剂和PDMS为1:10的比例加入固化剂并再用匀质机再真空状态下搅拌脱泡,脱泡后的混合液即液体形式的BN-Fe3O4/PDMS的复合材料;利用玻璃制作5.5mm×5.5mm×1mm所需模具,将制备BN-Fe3O4/PDMS的复合材料的液体倒入模具内部后在上层表面压上玻璃,上下两面覆盖加热片.利用电磁铁装置,产生外加磁场,对样品施加磁场作用力,磁场的强度为1020mT,让样品在常温下取向两小时,然后再在100℃取向十分钟,同时受热固化。
实施例2.
所用材料种类和工艺流程同实施例1,不同的是加入PDMS 8.7g、BN-Fe3O4 0.4g
对比例1.
所用材料种类和用量同实施例1,不同的是利用玻璃制作5.5mm×5.5mm×1mm所需模具,将制备BN-Fe3O4/PDMS的复合材料的液体倒入模具内部后在上层表面压上玻璃,上下两面覆盖加热片.在100℃加热固化十分钟。
对比例2.
所用材料种类同实施例1,不同的是加入PDMS 8.7g、BN-Fe3O40.4g,利用玻璃制作5.5mm×5.5mm×1mm所需模具,将制备BN-Fe3O4/PDMS的复合材料的液体倒入模具内部后在上层表面压上玻璃,上下两面覆盖加热片.在100℃加热固化十分钟。
图3和图4表示在PDMS与Fe3O4不同比例介电常数随频率变化。
以上所述仅为本发明较佳的实施例,并不用以限制本发明,凡在本发明精神和原则之内,所做的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (5)
1.一种改变物质磁场响应性的方法,其特征在于,对于大多数物质,通过多巴胺的包覆作用以及它与四氧化三铁的耦合作用,从而实现了物质与四氧化三铁结合,进而可以使物质在磁场中取向,提高复合材料的某种性能。
2.根据权利要求1所述改变物质磁场响应性的方法,通过多巴胺实现氮化硼与与四氧化三铁结合在一起。
3.根据权利要求1所述改变物质磁场响应性的方法,氮化硼表面接四氧化三铁,四氧化三铁使氮化硼具有了磁性。
4.根据权利要求1所述改变物质磁场响应性的方法,所采用物质是氮化硼。使之具有磁性的具体步骤为:
1)氮化硼磁性体制备:将30ml PH=9.90的缓冲溶液与10ml无水乙醇混合起来,然后将0.2g六方氮化硼加入到该混合溶液中,超声30min。然后加入80mg的盐酸多巴胺,常温反应9小时,得到BN@PDA。
2)把0.2g三氯化铁加入到80ml乙二醇中,然后加入2.0g聚乙二醇和0.2g BN@PDA。超声5min,然后加入6.0g醋酸钠,在60℃下搅拌反应2h.然后转入反应釜中,在180℃反应9h,反应完后,用乙醇反复洗涤三次(离心转速7200转,离心时间30min),除去小分子。在60℃烘干干燥,得到BN-Fe3O4。
5.根据权利要求1所述提高的某种性能,所提高性能为复合材料的介电性能。复合材料的制备步骤为:
1)一种高介电柔性膜,其特征在于,所述膜是一种氮化硼磁性体/PDMS复合材料,并可以制出任意厚度的膜,且具有光滑的表面结构,所述氮化硼磁性体/PDMS复合材料包括PDMS基体以及氮化硼磁性体粉体,所述氮化硼磁性体粉体分散在所述PDMS基体中。
2)制备高介电柔性膜:将制备BN-Fe3O4/PDMS的复合材料的液体倒入模具内,上下两面覆盖加热片。利用电磁铁装置,产生外加磁场,让样品在常温下取向两小时,然后再在100℃取向十分钟,同时受热固化。
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