CN113584671A - 导热聚合物、导热聚合物复合材料及其制备方法和应用 - Google Patents

导热聚合物、导热聚合物复合材料及其制备方法和应用 Download PDF

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CN113584671A
CN113584671A CN202110870142.3A CN202110870142A CN113584671A CN 113584671 A CN113584671 A CN 113584671A CN 202110870142 A CN202110870142 A CN 202110870142A CN 113584671 A CN113584671 A CN 113584671A
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fiber
heat
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吴凯
陈馨
傅强
陈枫
张琴
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Sichuan University
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Abstract

本发明涉及一种导热聚合物、导热聚合物复合材料及其制备和应用,属于功能高分子复合材料领域。本发明提供一种导热聚合物材料的制备方法,所述制备方法为:先将高分子纤维加捻、定捻得到高分子纤维束,再将高分子纤维束加工成纤维布并定型得导热聚合物材料。本发明提供了一种能同时实现水平和垂直方向高导热的聚合物材料的制备方法,利用该方法制得的导热聚合物材料具有优异的导热性能(能够同时实现水平和垂直方向的高导热性能),良好的绝缘性与力学性能,该导热材料可用作PCB电路板基板材料,导热封装或外壳材料。

Description

导热聚合物、导热聚合物复合材料及其制备方法和应用
技术领域
本发明涉及一种导热聚合物、导热聚合物复合材料及其制备方法和应用,属于功能高分子复合材料领域。
背景技术
近年来,随着电子产品集成化、小型化和高功率化程度的提高,电子设备的热管理问题也越来越突出,高热流密度及温度的不均匀分布等问题严重影响了电子设备的寿命和可靠性。数据显示,在电子设备中,百分之五十五的性能问题源自于温度,由此可以说明电子器件中热管理问题的重要性。印刷电路板(PCB)是电子元器件连接的重要载体,也是电子器件热管理材料中的重要组成部分,它主要由电子玻纤布或其他增强材料浸入聚合物树脂,单面或两面覆以铜箔并经热压制得,但现有印刷电路板很难同时满足高导热性能和力学性能,更难根据需求调控导热方向、同时实现水平和垂直多个方向的导热。除此之外,电子器件的热管理也常用到一些相变材料,通过依靠相变材料在特定温度的巨大热焓,可以使电子器件的温度保持在较低的工作温度,然而相变材料的高导热和高热焓也是一个巨大的挑战。
高分子聚合物密度比较低,一般具有良好的绝缘性能,介电常数也小于金属等材料,为其在小型、高集成化电子设备的应用提供了保障,因为纯聚合物的导热系数通常很小,研究人员会通过向聚合物中添加具有高导热性能的填料提高材料的导热性能。但常见的填料型导热聚合物材料有很多局限性,例如这类材料通常只能在填料的取向方向上实现单一方向的高导热,而在其他方向上导热性能很差,而对于少部分能够同时实现水平和垂直方向导热性能的填料型复合材料,他们在两个方向上的导热系数都很低,通常在2-4W/mK范围内。
发明内容
针对上述问题,本发明的目的在于提供一种能同时实现水平和垂直方向高导热的聚合物材料的制备方法,利用该方法制得的导热聚合物材料具有优异的导热性能(能够同时实现水平和垂直方向的高导热性能),良好的绝缘性与力学性能,该导热材料可用作PCB电路板基板材料,导热封装或外壳材料。
本发明的技术方案:
本发明要解决的第一个技术问题是提供一种导热聚合物材料的制备方法,所述制备方法为:先将高分子纤维加捻、定捻得到高分子纤维束,再将高分子纤维束加工成纤维布并定型即得导热聚合物材料。
进一步,将高分子纤维加捻、定捻得到高分子纤维束的捻系数为10~120。
进一步,所述高分子纤维选自:超高分子量聚乙烯纤维、聚对苯撑苯并二噁唑纤维、尼龙纤维、聚对苯二甲酰对苯二胺纤维、聚酯纤维、聚对苯二甲酸丁二酯纤维、聚2,5-二羟基-1,4-苯撑并二咪唑纤维或芳纶纤维中的至少一种。
进一步,所述将高分子纤维束加工成纤维布采用编制或纺织的方法。
进一步,所述定捻采用包浆工艺,其中,所采用的包浆材料选自:聚乙烯醇(PVA)聚氨酯(PU)或酚醛树脂等。
本发明要解决的第二个技术问题是提供一种导热聚合物材料,其采用上述方法制得。
进一步,所述导热聚合物材料的水平和垂直方向均高导热:水平方向导热系数≥5W/m K,垂直方向导热系数≥8W/m K。
本发明要解决的第三个技术问题是提供一种能够同时提高高分子纤维材料水平方向和垂直方向导热性能的方法,所述方法为:先将高分子纤维材料加捻、定捻得到高分子纤维束,再将高分子纤维束加工成纤维布并将其定型。
进一步,将高分子纤维材料加捻、定捻得到的高分子纤维束的捻系数在10~120。
进一步,所述定捻采用包浆工艺,其中,所采用的包浆材料选自:聚乙烯醇(PVA)聚氨酯(PU)或酚醛树脂等。
本发明要解决的第四个技术问题是提供一种导热聚合物复合材料的制备方法,所述复合材料的制备方法为:先将高分子纤维材料加捻、定捻得到高分子纤维束,再将高分子纤维束加工成结构整齐的纤维布;最后将纤维布与可固化材料或相变材料复合得到导热聚合物复合材料。
进一步,将高分子纤维材料加捻、定捻得到的高分子纤维束的捻系数在10~120。
进一步,所述导热聚合物复合材料中,所述纤维布的体积分数为20%~45%,所述可固化材料或相变材料的加入量占导热聚合物复合材料体积的55%~80%。即纤维布占复合材料总体积的20%~45%。
进一步,所述可固化材料为可固化的高分子聚合物或其单体、预聚物;相变材料为金属类、盐类或有机物类。
进一步,所述可固化材料中的可固化高分子聚合物选自:热固性聚合物、光固化性聚合物或相变储能聚合物等可塑性聚合物。
更进一步,所述可塑性的热固性聚合物选自:聚二甲基硅氧烷、酚醛树脂、聚酰亚胺、或环氧树脂等;所述可相变的有机材料选自:石蜡、脂肪酸及其衍生物等。
本发明要解决的第五个技术问题是提供一种导热聚合物复合材料,其采用上述方法制得。
本发明要解决的第六个技术问题是提供上述导热聚合物复合材料的应用:可用PCB电路板材料,导热封装或外壳材料,热能输送、热电、热能存储等领域。
本发明的有益效果:
本发明导热聚合物复合材料的制备方法具有以下显著优点:(1)选用的高分子纤维具有很好的导热性能;(2)选用高分子纤维为原料制备高导热复合材料,价格低廉易于商业化;(3)通过将高分子纤维材料利用编织或纺织等方法得到纤维布制备的导热复合材料的导热性能优异,质轻绝缘且韧性好;(3)能够调控其导热性能,同时实现水平和垂直方向导热;(4)制备方法简便易行,易于产业化。
具体实施方式
本发明选择经过高度拉伸的高分子纤维如超高分子量聚乙烯纤维、聚对苯撑苯并二噁唑纤维和芳纶纤维等,他们的分子链中没有多余的侧基,且经过高强度拉伸之后,分子链取向十分整齐,降低了分子链之间的声子散射,具有很高的机械强度和热导率,相比于常规的导热填料有着巨大优势。同时在这些高分子纤维中,热量几乎完全沿纤维传输,可以通过调节纤维束的组合形状控制热量传输通道,进而可以实现水平和垂直方向上的高导热传输。
本发明通过对高分子纤维束加捻,再利用编织或纺织等方式得到高分子纤维布结构,然后将纤维布中填充入热固性聚合物或相变材料,经过高温或光照或调节温度定型,再去除表面多余可固化或相变物质得到在水平和垂直方向上具有高导热性的导热聚合物复合材料。
本发明的机理为:声子散射是造成高分子复合材料导热性能降低的主要原因,高度拉伸的高分子纤维材料的分子链上没有多余的侧基,同时高强度拉伸之后,分子链取向十分整齐,降低了分子链之间的声子散射,具有很高的机械强度和热导率;本发明通过将高分子纤维制备成规整的纤维布复合材料的形式,提供了沿水平方向和垂直方向的热传导路径,将整个复合材料的声子散射集中在微观的高分子链之间,最大程度的降低了在热传输方向的声子散射,从而提高了复合材料的导热能力,增加了复合材料的力学性能。
实施例1
将聚对苯撑苯并二噁唑纤维加捻得到捻系数为40的纤维束,用PVA对纤维束包浆定捻,将定捻好的纤维束编织得到具有平纹结构的纤维布,将已编织好的纤维布放于去离子水中高温浸泡10h除去PVA,再烘干得到纯净纤维布,取4.2cm*5cm的纤维布放于模具,向模具中加入1.5g环氧树脂,将模具转移到真空烘箱,在常温抽真空8小时排出空气,在80℃条件下固化。最后,将固化结束的聚对苯撑苯并二噁唑纤维布从模具中取出,将表面多余的可固化物质先用磨砂机打磨,再用砂纸细磨,得到表面平整且不破坏编织结构的导热复合材料。本发明高分子聚合物导热复合材料具有优良水平和垂直方向导热性能,密度较低,绝缘且韧性强,面内导热系数可达8.1W/m K,面外导热系数可达7.4W/m K。
对比例1
将1.5g六方氮化硼与2.0g环氧树脂直接共混,放入模具中,再将模具转移到真空烘箱,在常温抽真空8小时排出空气,在80℃条件下固化。最后,将固化结束的共混聚合物从模具中取出,将表面多余的可固化物质先用磨砂机打磨,再用砂纸细磨,得到表面平整且不破坏内部结构的导热复合材料。经过测试,其面内导热系数在8.8W/m K,但面外导热系数仅为0.23W/m K.
实施例2
将超分子量聚乙烯纤维加捻得到捻系数为80的纤维束,用PVA对纤维束包浆定捻,将定捻好的纤维束编织成具有平纹结构的纤维布,将已编织好的纤维布放于去离子水中高温浸泡10h除去PVA,再烘干得到纯净纤维布,取4.2cm*5cm单位的纤维布放于模具,向模具中加入1.5g PDMS橡胶,将模具转移到真空烘箱,抽真空8小时排出空气。然后,将装有纤维布和PDMS的模具转移到60℃烘箱中,加热8小时固化。最后,将固化结束的超分子量聚乙烯纤维布从模具中取出,将表面多余的可固化物质先用小型磨砂机打磨,再用砂纸细磨,得到表面平整且不破坏编织结构的导热复合材料。本发明高分子聚合物导热复合材料具有优良水平和垂直方向导热性能,密度较低,约为1300kg/m3,并且介电系数低,导热性能优异,面内导热系数可达9.4W/m K,面外导热系数可达12.5W/m K。
对比例2未进行加捻定捻
将超分子量聚乙烯纤维束沿纵向整齐排列得到4.2cm*5cm的纤维束布,放置于模具中,向模具中加入1.5g PDMS橡胶,将模具转移到真空烘箱,抽真空8小时排出空气。然后,将装有纤维布和PDMS的模具转移到60℃烘箱中,加热8小时固化。最后,将固化结束的超分子量聚乙烯纤维布从模具中取出,将表面多余的可固化物质先用小型磨砂机打磨,再用砂纸细磨,得到表面平整且不破坏编织结构,具有优良导热性能的导热复合材料。测试得到材料的面内导热系数为5.31W/m K,面外导热系数仅为0.56W/m K。
实施例3
将聚对苯撑苯并二噁唑纤维加捻得到捻系数为60的纤维束,用PVA对纤维束包浆定捻,干燥后将纤维束编织得到具有平纹结构的纤维布,将已编织好的纤维布放于去离子水中高温浸泡10h除去PVA,再烘干得到纯净纤维布,取4.2cm*5cm的纤维布浸入1.5g环氧树脂,将浸满环氧树脂的纤维布转移到真空烘箱,抽真空8小时排出空气。然后,将装有带有环氧树脂的纤维布转移到80℃烘箱中,加热8小时固化。最后,将固化结束的纤维布从模具中取出,将表面多余的可固化物质先用小型磨砂机打磨,再用砂纸细磨,得到表面平整且不破坏编织结构的导热复合材料。本发明高分子聚合物纤维基体的导热复合材料具有优良的性能,密度较低约为1100kg/m3,导热性能优异,面内导热系数可达9.6W/m K,面外导热系数可达11.2W/m K。
对比例3
将1.5氮化硼纳米片与2.0g环氧树脂直接共混,放入模具中,再将模具转移到真空烘箱,在常温抽真空8小时排出空气,在80℃条件下固化。最后,将固化结束的共混聚合物从模具中取出,将表面多余的可固化物质先用磨砂机打磨,再用砂纸细磨,得到表面平整且不破坏内部结构的样品,测试得到面内导热系数仅为2.8W/m K,面外导热系数仅为2.4W/m K.
实施例4
将尼龙纤维加捻得到捻系数为40的纤维束,用PVA对纤维束包浆定捻,干燥后将纤维束编织得到具有平纹结构的纤维布,将已编织好的纤维布放于去离子水中高温浸泡10h除去PVA,再烘干得到纯净纤维布,取4.2cm*5cm的纤维布放于模具,向模具中加入1.5g环氧树脂,将模具转移到真空烘箱,抽真空8小时排出空气。然后,将装有纤维束和环氧树脂的模具转移到80℃烘箱中,加热8小时固化。最后,将固化结束的尼龙纤维束从模具中取出,将表面多余的可固化物质先用小型磨砂机打磨,再用砂纸细磨,得到表面平整且不破坏编织结构,具有优良导热性能的导热复合材料。本发明高分子聚合物纤维基体的导热复合材料具有优良的性能,密度较低约为1000kg/m3,导热性能优异,面内导热系数可达8.2W/m K,面外导热系数可达6.3W/m K。
对比例4
将尼龙纤维束沿横向整齐排列得到4.2cm*5cm的纤维布放于模具,向模具中加入1.5g环氧树脂,将模具转移到真空烘箱,抽真空8小时排出空气。然后,将装有纤维束和环氧树脂的模具转移到80℃烘箱中,加热8小时固化。最后,将固化结束的尼龙纤维束从模具中取出,将表面多余的可固化物质先用小型磨砂机打磨,再用砂纸细磨,得到表面平整且不破坏内部结构的导热复合材料,测试得到面内导热系数为6.32W/m K,面外导热系数仅为0.56W/m K。
实施例5
将芳纶纤维加捻得到捻系数为80的纤维束,用PVA对纤维束包浆定捻,干燥后将纤维束编织得到具有平纹结构的纤维布,然后将已编织好的纤维布放于去离子水中高温浸泡10h除去PVA,再烘干得到纯净的纤维布,取4.2cm*5cm的纤维布放于模具,向模具中加入1.5g光敏固化树脂,将模具转移到真空烘箱,抽真空8小时排出空气。然后,将装有纤维布和光敏固化树脂的模具转移到紫外灯下中,照射30分钟固化。最后,将固化结束的芳纶纤维布从模具中取出,将表面多余的可固化物质先用小型磨砂机打磨,再用砂纸细磨,得到表面平整且不破坏编织结构的导热复合材料。本发明高分子聚合物纤维基体的导热复合材料具有优良的性能,密度较低约为1000kg/m3,导热性能优异,面内导热系数可达7.5W/m K,面外导热系数可达9.8W/m K。
实施例6
将聚对苯撑苯并二噁唑纤维加捻得到捻系数为40的纤维束,用PVA对纤维束包浆定捻,干燥后将纤维束编织得到具有缎纹结构的纤维布,将已编织好的纤维布放于去离子水中高温浸泡10h除去PVA,再烘干得到纯净纤维布,取4.2cm*5cm的纤维布浸入1.5g石蜡,将浸满石蜡的纤维布转移到真空烘箱,抽真空8小时排出空气。然后,将装有带有石蜡的纤维布在室温下冷却定型。最后,将定型好的纤维布复合材料从模具中取出,将表面多余的可固化物质先用小型磨砂机打磨,再用砂纸细磨,得到表面平整且不破坏编织结构的导热相变复合材料。本发明高分子聚合物纤维基体的导热相变复合材料具有优良的性能,密度较低约为1100kg/m3,导热性能优异,面内导热系数可达8.3W/m K,面外导热系数可达9.3W/mK。

Claims (10)

1.一种导热聚合物材料的制备方法,其特征在于,所述制备方法为:先将高分子纤维加捻、定捻得到高分子纤维束,再将高分子纤维束加工成纤维布并定型得导热聚合物材料。
2.根据权利要求1所述的一种导热聚合物材料的制备方法,其特征在于,将高分子纤维加捻、定捻得到高分子纤维束的捻系数为10~120;
进一步,所述高分子纤维选自:超高分子量聚乙烯纤维、聚对苯撑苯并二噁唑纤维、尼龙纤维、聚对苯二甲酰对苯二胺纤维、聚酯纤维、聚对苯二甲酸丁二酯纤维、聚2,5-二羟基-1,4-苯撑并二咪唑纤维或芳纶纤维中的至少一种。
3.根据权利要求1或2所述的一种导热聚合物材料的制备方法,其特征在于,所述定捻采用包浆工艺,其中,所采用的包浆材料选自聚乙烯醇、聚氨酯或酚醛树脂。
4.一种导热聚合物材料,其特征在于,所述导热聚合物材料采用权利要求1~3任一项所述的方法制得。
5.根据权利要求4所述的导热聚合物材料,其特征在于,所述导热聚合物材料的水平方向导热系数≥5W/m K,垂直方向导热系数≥8W/m K。
6.一种同时提高高分子纤维材料水平方向和垂直方向导热性能的方法,其特征在于,所述方法为:先将高分子纤维材料加捻、定捻得到高分子纤维束,再将高分子纤维束加工成纤维布并将其定型。
7.根据权利要求6所述的同时提高高分子纤维材料水平方向和垂直方向导热性能的方法,其特征在于,将高分子纤维材料加捻、定捻得到的高分子纤维束的捻系数为10~120。
进一步,所述定捻采用包浆工艺,其中,所采用的包浆材料选自聚乙烯醇、聚氨酯或酚醛树脂。
8.一种导热聚合物复合材料的制备方法,其特征在于,所述复合材料的制备方法为:先将高分子纤维材料加捻、定捻得到高分子纤维束;再将高分子纤维束加工成结构整齐的纤维布;最后将纤维布与可固化材料或相变材料复合得到导热聚合物复合材料;
进一步,将高分子纤维材料加捻、定捻得到的高分子纤维束的捻系数为10~120;
进一步,所述导热聚合物复合材料中,所述纤维布的体积分数为20%~45%,所述可固化材料或相变材料的加入量占导热聚合物复合材料体积的55%~80%;
进一步,所述可固化材料为可固化的高分子聚合物或其单体、预聚物;相变材料为金属类、盐类或有机物类;
更进一步,所述可固化材料中的可固化高分子聚合物选自:热固性聚合物、光固化性聚合物或相变储能聚合物;
更进一步,所述热固性聚合物选自:聚二甲基硅氧烷、酚醛树脂、聚酰亚胺或环氧树脂;所述相变材料选自:石蜡、脂肪酸及其衍生物。
9.一种导热聚合物复合材料,其特征在于,所述导热聚合物复合材料采用权利要求8所述得方法制得。
10.导热聚合物复合材料的应用,其特征在于,所述导热聚合物复合材料用作PCB电路板材料、导热封装或外壳材料。
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