CN105969024B - 一种含有物理剥离石墨烯的导热涂层材料及其制备方法 - Google Patents
一种含有物理剥离石墨烯的导热涂层材料及其制备方法 Download PDFInfo
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Abstract
本发明提供一种含有物理剥离石墨烯的导热涂层材料及其制备方法,一种含有物理剥离石墨烯的导热涂层材料,所述涂层材料包括聚合物、导热粉体、溶剂、助剂,所述聚合物占涂层材料的5‑30wt%;所述导热粉体占涂层材料的5‑30wt%;所述溶剂占涂层材料的40%‑90wt%;所述助剂占涂层材料的0.1‑10wt%,本发明所述涂层材料分为水性涂层材料和溶剂型涂层材料两种,可根据不同需求灵活调整。所述涂层材料具备高导热性、耐高温性、防腐蚀性、自流平的优异性能。该涂层材料使用方便,适用于各种涂敷方式。
Description
技术领域
本发明属于导热材料领域,具体涉及一种含有物理剥离石墨烯的导热涂层材料及其制备方法。
背景技术
石墨烯的导热系数高达5300W/(m·K),是良好的导热体。石墨烯改性散热涂层材料一方面由于石墨烯具有高的热导率而散热能力强,另一方面由于石墨烯比表面积高,能充分填充在涂层中,增大了涂层散热表面积,因而能同时降低物体表面和内部温度。石墨烯改性散热涂层材料能够长期在高温下工作,耐磨性、抗冲击性强,具有很好的耐候性、耐盐雾性、耐酸碱性、耐光照老化性等性能,在各种极端环境下均可使用。可以应用于各类需要散热的物件,如笔记本电脑、智能手机、LED、可穿戴设备、工业设备、汽车零部件等各行业。
物理剥离的石墨烯拥有良好的导热性能,但其在溶剂中的分散性不好,容易沉降结块,影响涂层材料的施工和涂敷后的性能,限制了其在涂层材料工业中的实际应用。氧化石墨烯与物理剥离的石墨烯相比,在溶剂中有良好的分散性,但氧化石墨烯中有大量有机官能团,而物理剥离石墨烯中没有,因此导热性能降低。本发明制备了一种即具有导热性能,又具有良好的分散稳定性的石墨烯基导热涂层材料。
发明内容
为了解决上述问题,本发明提供一种含有物理剥离石墨烯的导热涂层材料及其制备方法,一种含有物理剥离石墨烯的导热涂层材料,所述涂层材料包括聚合物、导热粉体、溶剂、助剂,所述聚合物占涂层材料的5-30wt%;所述导热粉体占涂层材料的5-30wt%;所述溶剂占涂层材料的40%-90wt%;所述助剂占涂层材料的0.1-10wt%;
进一步地,所述聚合物为聚乙烯吡咯烷酮、聚乙烯醇、聚乙二醇、聚马来酸酐、聚丙烯酰胺、聚季铵盐、聚醋酸乙烯酯、醇酸树脂、脲醛树脂、酚醛树脂或环氧树脂;
进一步地,所述导热粉体为物理剥离石墨烯,所述导热粉体为物理剥离石墨烯,所述物理剥离石墨烯的碳含量为85-99.8%,层数为2-50层,粉体颗粒的粒度为50-5000目;
进一步地,所述溶剂为N-甲基吡咯烷酮、N,N-二甲基甲酰胺、二氧六环、水、丙酮、丁酮、环己酮、醋酸丁酯、醋酸乙酯、乙醇、乙二醇、正丙醇、异丙醇、正丁醇、1,4-丁二醇、异辛醇、二甘醇、纯苯、甲苯或二甲苯;
进一步地,所述助剂包括分散剂、消泡剂和流平剂,所述流平剂为有机硅流平剂、丙烯酸流平剂或氟碳化合物流平剂;所述消泡剂为水性消泡剂、聚合物消泡剂或有机硅消泡剂;所述分散剂为离子型分散剂或高分子型分散剂;
进一步地,所述助剂还包括偶联剂,所述偶联剂为硅烷偶联剂或钛酸酯偶联剂;
进一步地,所述涂层材料的涂敷厚度为10-200μm;
进一步地,一种含有物理剥离石墨烯的导热涂层材料的制备方法,所述制备方法包括:
S1:将5-30份的聚合物溶解在20-45份的溶剂中,得到聚合溶液;
S2:将5-30份的石墨烯加入到20-45份的溶剂中,超声分散1-3h,得到石墨烯浆料;
S3:将0.1-10份的助剂加入S1中所述聚合溶液中;
S4:将S3所获得的混合物加入S2中所述石墨烯浆料混合均匀;所述混合方式包括高速搅拌与超声分散;
进一步地,S1和S2中所述的溶剂为N-甲基吡咯烷酮、N,N-二甲基甲酰胺、二氧六环、水、丙酮、丁酮、环己酮、醋酸丁酯、醋酸乙酯、乙醇、乙二醇、正丙醇、异丙醇、正丁醇、1,4-丁二醇、异辛醇、二甘醇、纯苯、甲苯或二甲苯;
S1中所述聚合物为聚合物为聚乙烯吡咯烷酮、聚乙烯醇、聚乙二醇、聚马来酸酐、聚丙烯酰胺、聚季铵盐、聚醋酸乙烯酯、醇酸树脂、脲醛树脂、酚醛树脂、环氧树脂;
S2中所述石墨烯为物理剥离石墨烯粉体,所述石墨烯的碳含量85-99.8%,层数为2-50层,粉体颗粒的粒度为50-5000目;
进一步地,S3中所述助剂包括分散剂、流平剂、消泡剂和偶联剂,所述分散剂为离子型分散剂或高分子型分散剂;所述流平剂为有机硅流平剂、丙烯酸流平剂或氟碳化合物流平剂;所述消泡剂为水性消泡剂、聚合物消泡剂或有机硅消泡剂;所述偶联剂为硅烷偶联剂或钛酸酯偶联剂;
本发明的有益效果如下:
1)本发明所述涂层材料分为水性涂层材料和溶剂型涂层材料两种,可根据不同需求灵活调整;
2)通过加入聚合物、导热粉体、溶剂、助剂,使得物理剥离石墨烯有大量有机官能团,在溶剂中有良好的分散性,提高导热性能,不容易沉降结块,对施工和涂敷后的性能没有影响,在涂层材料工业中的实际应用更加广泛;
3)本发明所述涂层材料具备高导热性、耐高温性、防腐蚀性、自流平的优异性能;
4)本发明所述涂层材料使用方便,适用于各种涂敷方式。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细描述。应当理解,此处所描述的具体实施例仅仅用于解释本发明,并不用于限定本发明。相反,本发明涵盖任何由权利要求定义的在本发明的精髓和范围上做的替代、修改、等效方法以及方案。进一步,为了使公众对本发明有更好的了解,在下文对本发明的细节描述中,详尽描述了一些特定的细节部分。对本领域技术人员来说没有这些细节部分的描述也可以完全理解本发明。
下面结合具体实施例对本发明作进一步说明,但不作为对本发明的限定,下面为本发明的举出最佳实施例:
本发明提供一种含有物理剥离石墨烯的导热涂层材料,所述涂层材料包括聚合物、导热粉体、溶剂、助剂,所述聚合物占涂层材料的5-30wt%;所述导热粉体占涂层材料的5-30wt%;所述溶剂占涂层材料的40-90wt%;所述助剂占涂层材料的0.1-10wt%,所述聚合物包括聚乙烯吡咯烷酮、聚乙烯醇、聚乙二醇、聚马来酸酐、聚丙烯酰胺、聚季铵盐、聚醋酸乙烯酯、醇酸树脂、脲醛树脂、酚醛树脂、环氧树脂,所述导热粉体为物理剥离石墨烯,所述物理剥离石墨烯的碳含量为85-99.8%,层数为2-50层,粉体颗粒的粒度为50-5000目,所述溶剂包括N-甲基吡咯烷酮、N,N-二甲基甲酰胺、二氧六环、水、丙酮、丁酮、环己酮、醋酸丁酯、醋酸乙酯、乙醇、乙二醇、正丙醇、异丙醇、正丁醇、1,4-丁二醇、异辛醇、二甘醇、纯苯、甲苯、二甲苯,所述助剂包括分散剂、消泡剂、流平剂,所述流平剂包括有机硅流平剂、丙烯酸流平剂、氟碳化合物流平剂;所述消泡剂包括水性消泡剂、聚合物消泡剂、有机硅消泡剂;所述分散剂包括离子型分散剂和高分子型分散剂,所述助剂还包括偶联剂,所述偶联剂包括硅烷偶联剂和钛酸酯偶联剂,所述涂层材料的涂敷厚度为10-200μm。
一种含有物理剥离石墨烯的导热涂层材料的制备方法,所述制备方法包括:
S1:将5-30份的聚合物溶解在20-45份的溶剂中,得到聚合溶液;
S2:将5-30份的石墨烯加入到20-45份的溶剂中,超声分散1-3h,得到石墨烯浆料;
S3:将0.1-10份的助剂加入S1中所述聚合溶液中;
S4:将S3所获得的混合物加入S2中所述石墨烯浆料混合均匀,所述混合方式包括高速搅拌与超声分散。
S1和S2中所述的溶剂为N-甲基吡咯烷酮、N,N-二甲基甲酰胺、二氧六环、水、丙酮、丁酮、环己酮、醋酸丁酯、醋酸乙酯、乙醇、乙二醇、正丙醇、异丙醇、正丁醇、1,4-丁二醇、异辛醇、二甘醇、纯苯、甲苯、二甲苯;
S1中所述聚合物为聚合物为聚乙烯吡咯烷酮、聚乙烯醇、聚乙二醇、聚马来酸酐、聚丙烯酰胺、聚季铵盐、聚醋酸乙烯酯、醇酸树脂、脲醛树脂、酚醛树脂、环氧树脂;
S2中所述石墨烯为物理剥离石墨烯粉体,所述石墨烯的碳含量85-99.8%,层数为2-50层,粉体颗粒的粒度为50-5000目。
S3中所述助剂包括分散剂、流平剂、消泡剂和偶联剂,所述分散剂包括离子型分散剂、高分子型分散剂;所述流平剂又包括有机硅流平剂、丙烯酸流平剂、氟碳化合物流平剂;所述消泡剂有包括水性消泡剂、聚合物消泡剂、有机硅消泡剂;所述偶联剂包括硅烷偶联剂、钛酸酯偶联剂。
本发明中所述聚合物和粉体的比例是聚合物占5-30wt%,石墨烯粉体占5-30wt%;助剂占整体的0.1-10wt%,其余为溶剂。所述涂层材料分为水性涂层材料和溶剂型涂层材料两种,可根据不同需求灵活调整。所述涂层材料具备高导热性、耐高温性、防腐蚀性、自流平的优异性能。所述涂层材料使用方便,适用于各种涂敷方式。
实施例1
称取9份聚乙烯吡咯烷酮用于30份的N-甲基吡咯烷酮中。取9份400目的高品质物理剥离石墨烯粉体加入40份N-甲基吡咯烷酮超声2h,超声功率500W超声温度30℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入3份BYK161、3份BYK361、3份BYK88、3份kh570高速分散机分散,分散速度2000r/min,分散时间30min。
实施例2
称取5份聚乙烯吡咯烷酮用于30份的N-甲基吡咯烷酮中。取15份400目的高品质物理剥离石墨烯粉体加入40份N-甲基吡咯烷酮超声2h,超声功率500W超声温度30℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入4份BYK161、4份BYK361、4份BYK88、4份kh560高速分散机分散,分散速度2000r/min,分散时间30min。
实施例3
称取14份聚乙烯吡咯烷酮用于30份的水中。取5份400目的高品质物理剥离石墨烯粉体加入40份N-甲基吡咯烷酮超声2h,超声功率500W超声温度30℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入3份BYK161、3份BYK361、3份BYK88、三份钛酸酯高速分散机分散,分散速度2000r/min,分散时间30min。
实施例4
称取9份聚乙烯吡咯烷酮用于30份的水中。取9份400目的高品质物理剥离石墨烯粉体加入10:30份N-甲基吡咯烷酮与水的混合溶液超声2h,超声功率500W超声温度30℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入4份BYK161、4份BYK361、4份BYK88、3份钛酸酯高速分散机分散,分散速度2000r/min,分散时间30min。
实施例5
称取9份聚乙烯醇用于30份的水中。取9份400目的高品质石墨烯物理剥离粉体加入40份N-甲基吡咯烷酮超声2h,超声功率500W超声温度30℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入3份BYK161、3份BYK361、3份BYK88、3份kh550高速分散机分散,分散速度2000r/min,分散时间30min。
实施例6
称取9份乙二醇用于30份的水中。取9份400目的高品质物理剥离石墨烯粉体加入40份水超声2h,超声功率500W超声温度60℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入3份BYK161、3份BYK361、3份BYK88、3份kh550高速分散机分散,分散速度2000r/min,分散时间30min。
实施例7
称取9份聚乙烯吡咯烷酮用于30份的N-甲基吡咯烷酮中。取9份5000目的高品质物理剥离石墨烯粉体加入40份N-甲基吡咯烷酮超声2h,超声功率500W超声温度30℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入5份BYK161、5份BYK361、5份BYK88、3份kh550高速分散机分散,分散速度2000r/min,分散时间30min。
实施例8
称取9份聚乙烯吡咯烷酮用于30份的N-甲基吡咯烷酮中。取9份50目的高品质物理剥离石墨烯粉体加入40份N-甲基吡咯烷酮超声2h,超声功率500W超声温度30℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入4份BYK161、4份BYK361、4份BYK88、3份钛酸酯高速分散机分散,分散速度2000r/min,分散时间30min。
实施例9
称取9份聚马来酸酐用于30份的N-甲基吡咯烷酮中。取9份400目的高品质物理剥离石墨烯粉体加入40份N-甲基吡咯烷酮超声2h,超声功率500W超声温度30℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入3份BYK161、3份BYK361、5份BYK88、4份钛酸酯高速分散机分散,分散速度2000r/min,分散时间30min。
实施例10
称取9份聚丙烯酰胺用于30份的乙二醇中。取9份400目的高品质物理剥离石墨烯粉体加入40份乙二醇超声2h,超声功率500W超声温度30℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入4份BYK161、3份BYK361、4份BYK88、3份钛酸酯高速分散机分散,分散速度2000r/min,分散时间30min。
实施例11
称取9份聚季铵盐用于30份的N-甲基吡咯烷酮中。取9份400目的高品质物理剥离石墨烯粉体加入40份N-甲基吡咯烷酮超声2h,超声功率500W超声温度30℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入3份BYK161、3份BYK361、4份BYK88、kh550高速分散机分散,分散速度2000r/min,分散时间30min。
实施例12
称取9份聚醋酸乙烯酯用于30份的N-甲基吡咯烷酮中。取9份400目的高品质物理剥离石墨烯粉体加入40份N-甲基吡咯烷酮超声2h,超声功率500W超声温度30℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入3份BYK161、3份BYK3550、4份BYK88、5份kh570高速分散机分散,分散速度2000r/min,分散时间30min。
实施例13
称取9份醇酸树脂用于30份的N-甲基吡咯烷酮中。取9份400目的高品质物理剥离石墨烯粉体加入40份N-甲基吡咯烷酮超声2h,超声功率500W超声温度30℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入3份BYK2164、3份BYK361、4份BYK57、kh570高速分散机分散,分散速度2000r/min,分散时间30min。
实施例14
称取9份脲醛树脂用于30份的N-甲基吡咯烷酮中。取9份400目的高品质物理剥离石墨烯粉体加入40份N-甲基吡咯烷酮超声2h,超声功率500W超声温度30℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入3份BYK161、3份BYK360、4份BYK88、kh570高速分散机分散,分散速度2000r/min,分散时间30min。
实施例15
称取9份酚醛树脂用于30份的N-甲基吡咯烷酮中。取9份400目的高品质物理剥离石墨烯粉体加入40份N-甲基吡咯烷酮超声2h,超声功率500W超声温度30℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入3份BYK2164、3份BYK399、4份BYK885份钛酸酯、高速分散机分散,分散速度2000r/min,分散时间30min。
实施例16
称取9份环氧树脂用于30份的N-甲基吡咯烷酮中。取9份400目的高品质物理剥离石墨烯粉体加入40份N-甲基吡咯烷酮超声2h,超声功率500W超声温度30℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入3份BYK110、3份BYK356、4份BYK72、5份钛酸酯高速分散机分散,分散速度2000r/min,分散时间30min。
实施例17
称取9份酚醛树脂用于30份的二甲苯。取9份400目的高品质物理剥离石墨烯粉体加入40份二甲苯超声2h,超声功率500W超声温度30℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入3份BYK110、3份BYK356、4份BYK72、5份钛酸酯高速分散机分散,分散速度2000r/min,分散时间30min。
实施例18
称取9份环氧树脂用于30份的丁酮。取9份400目的高品质物理剥离石墨烯粉体加入40份丁酮超声2h,超声功率500W超声温度30℃。将聚乙烯吡咯烷酮溶液与超声后的石墨烯浆料混合在一起加入3份BYK110、3份BYK356、5份BYK72、4钛酸酯高速分散机分散,分散速度2000r/min,分散时间30min。
将上述实施例1-16的涂层材料涂敷在PET膜上,60℃烘干30min。热导率使用C-THERM TCI仪器采用ASTM D7984标准测试薄膜水平热导率
本发明通过加入聚合物、导热粉体、溶剂、助剂,使得物理剥离石墨烯有大量有机官能团,在溶剂中有良好的分散性,提高导热性能,不容易沉降结块,对施工和涂敷后的性能没有影响,在涂层材料工业中的实际应用更加广泛。
表1为各实施例最终产品的热导率数据
以上所述的实施例,只是本发明较优选的具体实施方式的一种,本领域的技术人员在本发明技术方案范围内进行的通常变化和替换都应包含在本发明的保护范围内。
Claims (4)
1.物理剥离石墨烯作为导热粉体在导热涂层材料中的应用,其特征在于,所述涂层材料包括聚合物、导热粉体、溶剂、助剂,所述聚合物占涂层材料的5-30wt%;所述导热粉体占涂层材料的5-30wt%;所述溶剂占涂层材料的40-90wt%;所述助剂占涂层材料的0.1-10wt%;
所述物理剥离石墨烯的碳含量为85-99.8%,层数为2-50层,粉体颗粒的粒度为50-5000目;
所述助剂包括分散剂、消泡剂、流平剂和偶联剂,所述偶联剂为硅烷偶联剂或钛酸酯偶联剂;
所述涂层材料的制备方法包括:
S1:将5-30份的聚合物溶解在20-45份的溶剂中,得到聚合溶液;
S2:将5-30份的物理剥离石墨烯加入到20-45份的溶剂中,超声分散1-3h,得到石墨烯浆料;
S3:将0.1-10份的助剂加入S1中所述聚合溶液中;
S4:将S3所获得的混合物加入S2中所述石墨烯浆料混合均匀;所述混合方式包括高速搅拌与超声分散。
2.根据权利要求1所述的应用,其特征在于,所述聚合物为聚乙烯吡咯烷酮、聚乙烯醇、聚乙二醇、聚马来酸酐、聚丙烯酰胺、聚季铵盐、聚醋酸乙烯酯、醇酸树脂、脲醛树脂、酚醛树脂或环氧树脂。
3.根据权利要求1所述的应用,其特征在于,所述溶剂为N-甲基吡咯烷酮、N,N-二甲基甲酰胺、二氧六环、水、丙酮、丁酮、环己酮、醋酸丁酯、醋酸乙酯、乙醇、乙二醇、正丙醇、异丙醇、正丁醇、1,4-丁二醇、异辛醇、二甘醇、纯苯、甲苯或二甲苯。
4.根据权利要求1所述的应用,其特征在于,所述流平剂为有机硅流平剂、丙烯酸流平剂或氟碳化合物流平剂;所述消泡剂为水性消泡剂、聚合物消泡剂或有机硅消泡剂;所述分散剂为离子型分散剂或高分子型分散剂。
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