CN109206808A - 一种导热高分子液晶分散膜的制备方法 - Google Patents
一种导热高分子液晶分散膜的制备方法 Download PDFInfo
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Abstract
本发明公开了一种导热高分子液晶分散膜的制备方法,包括:将聚合物基材研磨,与水或溶剂混合,浸泡,得到聚合物基底溶液,室温静置得到均相澄清的溶液;将侧链液晶聚硅氧烷的晶状体研磨;将侧链液晶聚硅氧烷分散到聚合物基底溶液中,得到微黄乳状溶液;乳状溶液缓慢平铺在玻璃器皿中,加热蒸干成膜,即得导热高分子液晶分散膜。本发明制备的导热高分子液晶分散膜,兼具高热导率、优异的力学性能和易成型加工等特性。
Description
技术领域
本发明涉及电子封装导热材料,具体是一种导热高分子液晶分散膜的制备方法。
背景技术
在工业需求和科学技术的发展过程中,对各类工程导热材料提出了更新、更高的要求。如电子元器件所需的高绝缘导热柔性界面、封装材料,化工换热器和废水处理所需的卓越耐高温和耐化学腐蚀的轻质导热材料等。理想的导热材料要兼具高热导率、优异力学性能及易成型加工等性能。相比无机和金属等传统导热材料,高分子导热材料以其良好的冲击韧性、力学强度,低成本和易加工等优异特性得到了广泛应用。
LCP(高分子液晶)在高分子制膜领域是一种新的材料,它独一无二的物理和化学性质使其在制膜材料上炙手可热。而热导率的提高则取决于在基体内形成的导热输运通路的完整性、稳定性及界面热阻。只有当导热粒子用量增大到某一临界值时,粒子间开始相互接触和作用,局部导热链或导热网才会相互连接和贯穿形成通路,热导率才会显著提高;但这是以牺牲聚合物优良韧性等力学性能为前提的,且热导率的提高也有限,此外还会降低聚合物的电阻,而且因导热粒子种类、粒径、分散性和电性能差异还会降低聚合物的击穿强度。
由于导热粒子和聚合物因界面性能的不匹配所造成的严重声子散射,以及聚合物基体的巨大热阻,导致体系热导率提高有限。而且导热粒子和聚合物的热导率差异为10-104倍,当差异超过102倍之后,导热粒子的添加对聚合物热导率的提高作用甚微。
因此,提供一种兼具高热导率以及优异力学性能的易成型加工的本征型导热材料成为目前本领域亟待解决的技术问题。
发明内容
为解决现有技术中存在的上述缺陷,本发明的目的在于提供一种导热高分子液晶分散膜,本发明通过改善聚合物连续相基体的热导率来提高体系的热导率,该方式远比提高导热粒子的更有效,并能够解决聚合物韧性等力学性能劣化、制备工艺复杂的的技术问题。
本发明是通过下述技术方案来实现的。
根据本发明实施例提供的一种导热高分子液晶分散膜的制备方法,包括以下步骤:
步骤1,聚合物基底溶液的制备
将聚合物基材研磨,研磨后的固体按质量比1∶(4-6)比例与水或溶剂混合,并浸泡,然后在搅拌的状态下加热使其溶解,得到聚合物基底溶液,室温静置至溶液中的气泡自然溶出,最终得到均相澄清的溶液;
步骤2,侧链液晶聚硅氧烷的预处理
将侧链液晶聚硅氧烷的晶状体研磨,使其便于在聚合物基底溶液中分散;
步骤3,按照质量比为1:5的比例在搅拌加热条件下,将侧链液晶聚硅氧烷分散到聚合物基底溶液中,直至溶液从均相澄清的状态变为微黄乳状溶液;
步骤4,导热高分子液晶分散膜的制备
将步骤3制备的乳状溶液缓慢平铺在平整的玻璃器皿中,避免产生气泡,加热蒸干,成膜,即得导热高分子液晶分散膜。
优选的,所述聚合物基材为聚乙烯醇、聚氯乙烯、聚丙烯或聚丙烯腈。
优选的,所述溶剂为丙酮、四氢呋喃、对二甲苯或二甲基甲酰胺。
优选的,所述步骤1中,对聚合物基材研磨200-600目,用溶剂将其浸泡5-20个小时;在温度为25-150℃加热0.5-2个小时。
优选的,所述步骤1中,聚合物基底溶液静置2-6个小时。
优选的,所述步骤2中,将侧链液晶聚硅氧烷的晶状体进行研磨至60-120目。
优选的,所述步骤2中,所述侧链液晶聚硅氧烷为聚硅氧烷分别与反式-4-乙烯基-反式-4’-丙基双环己烷、反式-4-丙烯基-反式-4’-丙基双环己烷、4-烯丙氧基苯甲酸-4’-羟基苯氰酯和4-烯丙氧基苯甲酸-4’-羟基苯甲氧基酯聚合得到的。
优选的,所述步骤3中,加热温度为50-120℃。
优选的,所述步骤4中,成膜厚度为100-200μm。
优选的,所述步骤4中,在55-160℃下加热16-24个小时。
本发明由于采取以上技术方案,其具有以下有益效果:
本发明通过将侧链液晶聚硅氧烷分散到聚合物基底溶液中,制备的乳状溶液蒸干制膜,得到导热高分子液晶分散膜,其兼具高热导率、优异力学性能和易成型加工等特性。本发明通过改善聚合物连续相基体的热导率来提高体系的热导率。
本发明明确了导热高分子液晶分散膜的制备方法的适用性,并提高了导热高分子液晶分散膜的成膜性、高热导率和优异力学性能。在LCP膜材料的应用领域上,为高分子液晶导热膜材料的制备和应用提供了一定的理论基础和技术支持,进而拓宽高分子液晶膜材料在导热领域的应用。
附图说明
此处所说明的附图用来提供对本发明的进一步理解,构成本申请的一部分,并不构成对本发明的不当限定,在附图中:
图1为本发明工艺流程图。
具体实施方式
下面将结合附图以及具体实施例来详细说明本发明,在此本发明的示意性实施例以及说明用来解释本发明,但并不作为对本发明的限定。
如图1所示,本发明的导热高分子液晶分散膜的制备方法,包括以下步骤:
导热高分子液晶分散膜的制备可分为以下4个部分,分别是聚合物基底溶液的制备、侧链液晶聚硅氧烷的预处理、侧链液晶聚硅氧烷在聚合物基底溶液中的分散、导热高分子液晶分散膜的制备。
步骤1,聚合物基底溶液的制备
将聚合物基材研磨200-600目,在搅拌的状态下用蒸馏水或溶剂将其浸泡5-20个小时,然后在25-150℃温度下加热0.5-2h使其溶解,在溶解过程中应不停搅拌,得到聚合物基底溶液,室温下将其静置2-6个小时,让溶液中的气泡自然溶出,最终得均相澄清的溶液。
其中,聚合物基材为聚乙烯醇、聚氯乙烯、聚丙烯或聚丙烯腈。溶剂为丙酮、四氢呋喃、对二甲苯或二甲基甲酰胺。
步骤2,侧链液晶聚硅氧烷的预处理
将侧链液晶聚硅氧烷的晶状体进行研磨至60-120目,使其便于在聚合物基底溶液中分散;其中,侧链液晶聚硅氧烷通过聚硅氧烷和液晶单体接枝聚合而得,其中聚硅氧烷与反式-4-乙烯基-反式-4’-丙基双环己烷聚合得到的侧链液晶聚硅氧烷为P1、聚硅氧烷和反式-4-丙烯基-反式-4’-丙基双环己烷聚合得到的侧链液晶聚硅氧烷为P2、聚硅氧烷和4-烯丙氧基苯甲酸-4’-羟基苯氰酯聚合得到的侧链液晶聚硅氧烷为P3、聚硅氧烷和4-烯丙氧基苯甲酸-4’-羟基苯甲氧基酯聚合得到的侧链液晶聚硅氧烷为P4。其结构见表1所示。
表1侧链液晶聚硅氧烷分子结构式
上述侧链液晶聚硅氧烷的合成方法见(P1:Ying Li,Guangcheng Zhang,YingJiang,Zhenzhong Hou,Longgui Peng,Synthesis and Characterization of Side-ChainLiquid-Crystalline Polysiloxanes exhibiting Spherulite Texture of PolymericSmectic A Phase,Journal of Chemical Research,2011,35(35):715-719.P2:李颖,胆甾相小板块织构聚硅氧烷侧链液晶的合成和性能,功能高分子学报,2016,29(01):80-84.P3:李颖,张广成,胡灵峰,史爱华,近晶型聚硅氧烷侧链液晶的合成与表征,功能高分子学报,2011,24(02):211-216.P4:蒋莹,李颖,杨建业,张亮,陈晶,新型含苯甲醚基团的向列型聚硅氧烷侧链液晶的合成与表征,合成化学,2013,21(4):420-423)。
步骤3,按照质量比1:5的比例在搅拌加热50-120℃条件下,将侧链液晶聚硅氧烷分散到聚合物基底溶液,直到溶液从均相澄清的状态变为微黄乳状溶液。
步骤4,导热高分子液晶分散膜的制备
将制好的溶液平铺在平整的玻璃器皿中,避免产生气泡,根据所选溶剂选择合适的温度55-160℃加热16-24个小时,制备导热高分子液晶分散膜,成膜厚度为100-200μm。
下面给出不同的具体实施例来进一步说明本发明。
实施例1
步骤1,将聚合物基材聚乙烯醇研磨200目,在搅拌的状态下用蒸馏水或丙酮将其浸泡20个小时,然后在25℃温度下加热2h使其溶解,在溶解过程中应不停搅拌,得到聚合物基底溶液,室温下将其静置4个小时,让溶液中的气泡自然溶出,最终得均相澄清的溶液;
步骤2,将侧链液晶聚硅氧烷的晶状体进行研磨至60目,使其便于在聚合物基底溶液中分散;
其中,侧链液晶聚硅氧烷为聚硅氧烷和反式-4-乙烯基-反式-4’-丙基双环己烷聚合得到的P1;
步骤3,按照质量比1:5的比例在搅拌加热50℃条件下,将侧链液晶聚硅氧烷分散到聚合物基底溶液,直到溶液从均相澄清的状态变为微黄乳状溶液;
步骤4,将制好的溶液平铺在平整的玻璃器皿中,避免产生气泡,根据所选溶剂选择合适的温度55℃加热24个小时,制备导热高分子液晶分散膜,成膜厚度为120μm。
实施例2
步骤1,将聚合物基材聚氯乙烯研磨300目,在搅拌的状态下用四氢呋喃将其浸泡15个小时,然后在100℃温度下加热时间1h使其溶解,在溶解过程中应不停搅拌,得到聚合物基底溶液,室温下将其静置6时,让溶液中的气泡自然溶出,最终得均相澄清的溶液;
步骤2,侧链液晶聚硅氧烷的预处理
将侧链液晶聚硅氧烷的晶状体进行研磨至100目,使其便于在聚合物基底溶液中分散;
其中,侧链液晶聚硅氧烷为聚硅氧烷和反式-4-丙烯基-反式-4’-丙基双环己烷聚合得到的P2;
步骤3,按照质量比1:5的比例在搅拌加热80℃条件下,将侧链液晶聚硅氧烷分散到聚合物基底溶液,直到溶液从均相澄清的状态变为微黄乳状溶液;
步骤4,将制好的溶液平铺在平整的玻璃器皿中,避免产生气泡,根据所选溶剂选择合适的温度90℃加热20个小时,制备导热高分子液晶分散膜,成膜厚度为150μm。
实施例3
步骤1,将聚合物基材聚丙烯研磨600目,在搅拌的状态下用对二甲苯将其浸泡5个小时,然后在50℃温度下加热时间1.5h使其溶解,在溶解过程中应不停搅拌,得到聚合物基底溶液,室温下将其静置3个小时,让溶液中的气泡自然溶出,最终得均相澄清的溶液;
步骤2,侧链液晶聚硅氧烷的预处理
将侧链液晶聚硅氧烷的晶状体进行研磨至80目,使其便于在聚合物基底溶液中分散;
其中,侧链液晶聚硅氧烷为聚硅氧烷和4-丙氧基苯甲酸-4’-羟基苯氰酯聚合而得的P3;
步骤3,按照质量比1:5的比例在搅拌加热120℃条件下,将侧链液晶聚硅氧烷分散到聚合物基底溶液,直到溶液从均相澄清的状态变为微黄乳状溶液;
步骤4,将制好的溶液平铺在平整的玻璃器皿中,避免产生气泡,根据所选溶剂选择合适的温度160℃加热16个小时,制备导热高分子液晶分散膜,成膜厚度为100μm。
实施例4
步骤1,将聚合物基材聚丙烯腈研磨500目,在搅拌的状态下用二甲基甲酰胺将其浸泡10个小时,然后在150℃温度下加热时间0.5h使其溶解,在溶解过程中应不停搅拌,得到聚合物基底溶液,室温下将其静置2个小时,让溶液中的气泡自然溶出,最终得均相澄清的溶液;
步骤2,侧链液晶聚硅氧烷的预处理
将侧链液晶聚硅氧烷的晶状体进行研磨至120目,使其便于在聚合物基底溶液中分散;
其中,侧链液晶聚硅氧烷为聚硅氧烷和4-丙氧基苯甲酸-4’-羟基苯甲氧基酯聚合得到的P4;
步骤3,按照质量比1:5的比例在搅拌加热100℃条件下,将侧链液晶聚硅氧烷分散到聚合物基底溶液,直到溶液从均相澄清的状态变为微黄乳状溶液;
步骤4,将制好的溶液平铺在平整的玻璃器皿中,避免产生气泡,根据所选溶剂选择合适的温度120℃加热20个小时,制备导热高分子液晶分散膜,成膜厚度为200μm。
将本发明实施例所得检测并讨论导热高分子液晶分散膜的性能
本发明将100-200μm厚度的导热高分子液晶分散膜,放在Hot Disk导热仪中,测量样品的热扩散系数和热导率,表征并分析样品的导热性能。试验中测试了本发明所制备的四种导热高分子液晶分散膜样品的导热性能,见表2所示。
表2导热高分子液晶分散膜的性能测试
由表2可以得到,本发明制备的导热高分子液晶分散膜具有优良的导热性能,其导热率达0.4781W/mK,且导热率不小于0.4002W/mK,远高于一般高分子材料(大约为0.2W/mK);其拉伸强度可达3.74Mpa,且拉伸强度不小于2.79Mpa;断裂伸长率达338.57%,且断裂伸长率不小于288.19%。因此,本发明方法制备的导热高分子液晶分散膜是一种具有良好导热性能和优异力学性能的高分子液晶膜。
本发明并不局限于上述实施例,在本发明公开的技术方案的基础上,本领域的技术人员根据所公开的技术内容,不需要创造性的劳动就可以对其中的一些技术特征作出一些替换和变形,这些替换和变形均在本发明的保护范围内。
Claims (10)
1.一种导热高分子液晶分散膜的制备方法,其特征在于,包括以下步骤:
步骤1,聚合物基底溶液的制备
将聚合物基材研磨,研磨后的固体按质量比1∶(4-6)比例与水或溶剂混合,并浸泡,然后在搅拌的状态下加热使其溶解,得到聚合物基底溶液,室温静置至溶液中的气泡自然溶出,最终得到均相澄清的溶液;
步骤2,侧链液晶聚硅氧烷的预处理
将侧链液晶聚硅氧烷的晶状体研磨,使其便于在聚合物基底溶液中分散;
步骤3,按照质量比为1:5的比例在搅拌加热条件下,将侧链液晶聚硅氧烷分散到聚合物基底溶液中,直至溶液从均相澄清的状态变为微黄乳状溶液;
步骤4,导热高分子液晶分散膜的制备
将步骤3制备的乳状溶液缓慢平铺在平整的玻璃器皿中,避免产生气泡,加热蒸干,成膜,即得导热高分子液晶分散膜。
2.根据权利要求1所述的导热高分子液晶分散膜的制备方法,其特征在于,所述聚合物基材为聚乙烯醇、聚氯乙烯、聚丙烯或聚丙烯腈。
3.根据权利要求1所述的导热高分子液晶分散膜的制备方法,其特征在于,所述溶剂为丙酮、四氢呋喃、对二甲苯或二甲基甲酰胺。
4.根据权利要求1所述的导热高分子液晶分散膜的制备方法,其特征在于,所述步骤1中,对聚合物基材研磨200-600目,用溶剂将其浸泡5-20个小时;在温度为25-150℃加热0.5-2个小时。
5.根据权利要求1所述的导热高分子液晶分散膜的制备方法,其特征在于,所述步骤1中,聚合物基底溶液静置2-6个小时。
6.根据权利要求1所述的导热高分子液晶分散膜的制备方法,其特征在于,所述步骤2中,将侧链液晶聚硅氧烷的晶状体进行研磨至60-120目。
7.根据权利要求1所述的导热高分子液晶分散膜的制备方法,其特征在于,所述步骤2中,所述侧链液晶聚硅氧烷为聚硅氧烷分别与反式-4-乙烯基-反式-4’-丙基双环己烷、反式-4-丙烯基-反式-4’-丙基双环己烷、4-烯丙氧基苯甲酸-4’-羟基苯氰酯和4-烯丙氧基苯甲酸-4’-羟基苯甲氧基酯聚合得到的。
8.根据权利要求1所述的导热高分子液晶分散膜的制备方法,其特征在于,所述步骤3中,加热温度为50-120℃。
9.根据权利要求1所述的导热高分子液晶分散膜的制备方法,其特征在于,所述步骤4中,成膜厚度为100-200μm。
10.根据权利要求1所述的导热高分子液晶分散膜的制备方法,其特征在于,所述步骤4中,在55-160℃下加热16-24个小时。
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