CN115260575A - 一种具有垂直取向的导热骨架及其制备方法和应用 - Google Patents
一种具有垂直取向的导热骨架及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及一种具有垂直取向结构的导热骨架及其制备方法和应用。本发明制备的具有垂直取向结构的导热骨架材料中,导热填料在骨架中垂直取向分布,形成连续的导热通路,与聚合物复合后赋予薄膜垂直方向上优异的导热性能。本发明包括的步骤有:选取合适溶剂,配制含导热填料和聚合物A的混合液,并将其以一定厚度刮涂到平整基材上。将湿膜浸入与该溶剂互溶性更强、且为聚合物A的不良溶剂凝固浴中进行非溶剂致相分离过程,得到具有垂直取向结构的聚合物A/导热填料多孔骨架材料。本发明制成的导热骨架材料与聚合物B填充孔隙复合后,所得薄膜材料具有优异的垂直方向导热性能和机械性能,能有效填充电子器件中热源与热沉之间的界面,增强界面传热,提高散热性能,具有重要的科学研究意义与实用价值。
Description
技术领域
本发明涉及一种具有垂直取向结构的导热骨架及其制备方法和应用,属于导热复合材料技术领域。
背景技术
近年来,在聚合物基体中添加具有高导热特性的填料如氮化硼、石墨烯是提高复合材料导热性能的有效手段。然而,由于填料与基体之间的声子谱不匹配,界面结合弱等因素,填料与基体之间存在较大的界面热阻,使得复合材料即使在高填料含量情况下,热导率提升非常有限。且高含量导热填料的加入严重影响复合材料的可加工性及机械性能等。因此,为了减少填料与基体之间的界面,在较少填料添加量的情况下在基体中构建连续的导热路径,尤其是垂直方向取向排列的导热骨架,成为聚合物基导热复合材料研究的热点。
发明内容
本发明的目的在于提供了一种具有垂直取向结构的导热骨架及其薄膜材料制备方法。本发明中,采用非溶剂致相分离法构建填料在垂直方向上取向排列的多孔导热骨架,进一步通过柔性聚合物的真空灌注或溶液填充,可获得填料垂直取向的致密复合薄膜。由非溶剂致相分离法获得的导热骨架与聚合物复合后,在垂直方向上获得优异的导热性能的同时,还具有良好的柔性性能,为其在电子元件散热上的实际应用奠定了基础。该复合材料还具有良好的形状稳定性,高温下极低的膨胀系数,其制备方法具有较高的理论研究和实际应用价值。
本发明提出的一种具有垂直取向结构的导热骨架,所述导热骨架中导热填料主要呈垂直排列;通过聚合物A的非溶剂致相分离,诱导导热填料随聚合物A相分离,获得垂直取向排列的聚合物A/导热填料多孔骨架,即为导热骨架,所述导热骨架采用真空灌注或溶液填充与聚合物B复合后,能在聚合物B基体中形成良好的导热路径,在垂直方向上表现出高导热性能。
本发明提出的具有垂直取向结构的导热骨架的制备方法,具体步骤如下:
(1)、量取10mL溶剂,加入0.5~1.5g聚合物A材料,相应溶解条件下充分溶解后,加入0.1~3g导热填料,充分搅拌后,得到混合浆料;
(2)、将步骤(1)得到的混合浆料以一定厚度刮涂到平整基材上,然后将湿膜浸入到凝固浴中,进行非溶剂致相分离过程,即可获得具有垂直取向排列的聚合物A/导热填料多孔骨架。
本发明中,步骤(1)中溶剂为N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、二甲亚砜、水或乙醇中的至少一种。
本发明中,步骤(1)中聚合物A材料为聚丙烯腈、聚偏氟乙烯、热塑性聚氨酯、聚酰亚胺或芳纶的至少一种。
本发明中,步骤(1)中导热填料为氮化硼、砷化硼、石墨烯、碳纳米管、碳纤维、碳化硅、氮化铝、Mxene或氧化铝的至少一种。
本发明中,步骤(2)中所述凝固浴为与步骤(1)溶剂互溶性更好的、步骤(1)中聚合物A的不良溶剂。
本发明所述的具有垂直取向结构的导热骨架在薄膜材料中的应用,以聚合物B溶液作为凝固浴,可在非溶剂致相分离过程中进行聚合物B的填充,得到致密的具有垂直取向骨架的薄膜材料。
本发明中,所述聚合物B溶液为聚氨酯、聚丙烯酸酯、聚乙烯醇、环氧树脂、甲基纤维素、乙基纤维素、羟乙基纤维素或硅橡胶中的至少一种。
本发明中制备的导热骨架材料的有益效果在于:
(1)、本发明中,由于聚合物A/导热填料形成的骨架中,导热填料合理取向排列,可在垂直方向上形成导热通路,经聚合物B复合并填充孔隙后导热性能十分优异;
(2)、本发明中,运用的非溶剂致相分离法解决了导热填料难以在柔性聚合物薄膜中垂直取向的难题,且制备工艺简单;
(3)、本发明中,本方法获得的氮化硼骨架复合柔性聚合物而成的导热材料,在微型计算机中央处理器(CPU)满载运行时表现出优越的散热效果。
附图说明
图1为实施例1中具有垂直取向结构的多孔聚合物/氮化硼骨架材料外观照片和扫描电镜照片。其中(a)为具有垂直取向结构的多孔聚合物A/氮化硼骨架材料的宏观照片,(b)为具有垂直取向结构的多孔聚合物A/氮化硼骨架材料的扫描电镜照片;
图2为实施例2中,柔性聚合物B填充多孔导热骨架后,保持垂直取向结构氮化硼骨架的聚合物复合材料的外观照片和扫描电镜照片。其中(a)为具有垂直取向结构氮化硼骨架的聚合物复合材料宏观照片,(b)为具有垂直取向结构氮化硼骨架的聚合物复合材料扫描电镜照片;
图3为实施例2中为具有垂直取向结构氮化硼骨架的聚合物复合材料垂直方向导热系数;
图4为实施例2中为具有垂直取向结构氮化硼骨架的聚合物复合材料受热膨胀曲线;
图5为实施例2中具有垂直取向结构氮化硼骨架的聚合物复合材料的电阻率;
图6为实施例2中具有垂直取向结构氮化硼骨架的聚合物复合材料用于微型计算机散热时CPU核心温度变化。
具体实施方式
下面结合具体实施例与附图对本发明做进一步阐述,但本发明并不限于以下实施例。所述方法如无特别说明均为常规方法。所述原材料如无特别说明均能从公开商业途径获得。
实施例1:
首先将0.8g聚丙烯腈粉末(PAN,Mw=250000)与10mL二甲亚砜中搅拌并充分溶解后,加入2g商业六方氮化硼(BN)粉末继续搅拌2h以上充分混合;
其次将获得的混合液以200μm厚度刮涂于平整基材上,将其浸入室温水浴中产生相分离。10min后将湿膜从基材上剥离并转移至60℃烘箱中干燥,得到具有垂直取向结构的多孔PAN/BN骨架;
如图1所示,所制备的PAN/BN骨架材料具有白色的外观,横截面的SEM照片表明该骨架具有垂直取向结构。
实施例2:
首先将1gPAN粉末(Mw=250000)与10mL二甲亚砜中搅拌并充分溶解后,加入5g商业BN粉末继续搅拌2h以上充分混合;
其次将获得的混合溶液以25μm厚度刮涂于平整基材上,将其浸入水性聚氨酯溶液中产生相分离。10min后将湿膜从基材上剥离并转移至60℃烘箱中干燥,得到具有垂直取向导热骨架的聚合物/BN复合材料;
如图2所示,聚合物/BN复合薄膜可任意裁剪成各种形状,承受多次折叠后而无明显破坏,且横截面扫描电镜照片显示,聚合物能完全填充骨架缝隙,获得致密的复合材料;
图3展示了纯聚合物薄膜和聚合物/BN复合薄膜的垂直方向导热系数,聚合物中BN骨架的引入能有效提高其导热系数;
如图4所示,相较于纯聚合物薄膜,聚合物/BN复合薄膜受热膨胀小,形状稳定性好;
图5展示了聚合物/BN复合薄膜的电阻率,远远超过109Ωcm,具有优异的电绝缘性能;
图6展示了聚合物/BN复合薄膜作为计算机的热界面材料时CPU的核心温度曲线,可以看出使用聚合物/BN复合薄膜后,满载运行的CPU核心温度较不使用热界面材料时可降低45℃。
Claims (8)
1.一种具有垂直取向结构的导热骨架,其特征在于,所述导热骨架中导热填料主要呈垂直排列;通过聚合物A的非溶剂致相分离,诱导导热填料随聚合物A相分离,获得垂直取向排列的聚合物A/导热填料多孔骨架,即为导热骨架,所述导热骨架采用真空灌注或溶液填充与聚合物B复合后,能在聚合物B基体中形成良好的导热路径,在垂直方向上表现出高导热性能。
2.一种如权利要求1所述的具有垂直取向结构的导热骨架的制备方法,其特征在于,具体步骤如下:
(1)、量取10mL溶剂,加入0.5~1.5g聚合物A材料,相应溶解条件下充分溶解后,加入0.1~3g导热填料,充分搅拌后,得到混合浆料;
(2)、将步骤(1)得到的混合浆料以一定厚度刮涂到平整基材上,然后将湿膜浸入到凝固浴中,进行非溶剂致相分离过程,即可获得具有垂直取向排列的聚合物A/导热填料多孔骨架。
3.根据权利要求2所述的制备方法,其特征在于,步骤(1)所述溶剂为N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、二甲亚砜、水或乙醇中至少一种。
4.根据权利要求2所述的制备方法,其特征在于,步骤(1)中所述聚合物A材料为聚丙烯腈、聚偏氟乙烯、热塑性聚氨酯、聚酰亚胺或芳纶中的至少一种。
5.根据权利要求2所述的制备方法,其特征在于,步骤(1)中所述导热填料为氮化硼、砷化硼、石墨烯、碳纳米管、碳纤维、碳化硅、氮化铝、Mxene或氧化铝中至少一种。
6.根据权利要求2所述的制备方法,其特征在于,步骤(2)中所述凝固浴为与步骤(1)溶剂互溶性更好的、步骤(1)中聚合物A的不良溶剂。
7.一种如权利要求1所述的具有垂直取向结构的导热骨架在薄膜材料中的应用,其特征在于:以聚合物B溶液作为凝固浴,可在非溶剂致相分离过程中进行聚合物B的填充,得到致密的具有垂直取向骨架的薄膜材料。
8.根据权利要求7所述的应用,其特征在于,所述聚合物B溶液为聚氨酯、聚丙烯酸酯、聚乙烯醇、环氧树脂、甲基纤维素、乙基纤维素、羟乙基纤维素或硅橡胶中至少一种。
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