CN115139579A - 一种高导热石墨烯/硅胶泡棉多层复合材料及其制备方法与应用 - Google Patents
一种高导热石墨烯/硅胶泡棉多层复合材料及其制备方法与应用 Download PDFInfo
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- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical compound CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 claims description 6
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Abstract
本发明涉及一种高导热石墨烯/硅胶泡棉多层复合材料及其制备方法与应用,所述高导热石墨烯/硅胶泡棉多层复合材料由石墨烯层与硅胶导热泡棉层交替层叠复合得到。本发明提供的高导热石墨烯/硅胶泡棉多层复合材料为多重层状结构,具有优良的导热性能和缓冲减震性能,实现了导热和缓冲功能的集成,作为热界面材料使用具有极大的市场应用前景。
Description
技术领域
本发明属于层状产品技术领域,具体涉及一种高导热石墨烯/硅胶泡棉多层复合材料及其制备方法与应用。
背景技术
传感器、雷达、绝缘栅双极型晶体管(IGBT)等都是高发热部件,设备的工作性能和可靠性取决于热量能否快速导出。由于元件表面粗糙造成热源和散热器件之间的界面是有限的点接触,散热面积极小,而空气又是热的不良导体,因此需要热界面材料来有效地弥合界面空隙,形成良好的导热通路。另一方面,一些产品如汽车总是在震动较大的情况下工作,震动可能导致电子元件失效,因此需要热界面材料具有优异的减震缓冲效果。
当前常见的泡棉缓冲材料导热系数一般为0.1W/mK左右,不能满足热界面导热需求,而导热垫片等热界面材料虽然导热系数能够满足散热需求,但不具备力学缓冲功能,因此,需要开发具有高导热性能及减震缓冲性能的热界面材料。
发明内容
本发明所要解决的技术问题是针对现有技术中存在的上述不足,提供一种高导热石墨烯/硅胶泡棉多层复合材料及其制备方法与应用,所述高导热石墨烯/硅胶泡棉多层复合材料具有优异的导热性能,并且缓冲减震效果好。
为解决上述技术问题,本发明提供的技术方案是:
提供一种高导热石墨烯/硅胶泡棉多层复合材料,所述高导热石墨烯/硅胶泡棉多层复合材料由石墨烯层与硅胶导热泡棉层交替层叠复合得到。
按上述方案,所述石墨烯层为市售石墨膜或石墨烯膜,导热系数为600~2000W/mK,石墨烯层厚度为2-100μm。
按上述方案,所述硅胶导热泡棉层由硅胶泡棉与导热填料复合得到,其中导热填料的质量百分含量为5~90%,厚度为10-1000μm。
按上述方案,所述导热填料为氧化铝,氮化铝,氮化硼,碳化硅,氮化硼,石墨烯,碳纤维,铝粉,铜粉,金刚石颗粒中的一种或几种,粒径为0.5-200μm。
按上述方案,所述高导热石墨烯/硅胶泡棉多层复合材料中石墨烯层的层数为10-100层。
按上述方案,所述高导热石墨烯/硅胶泡棉多层复合材料厚度为0.5-5mm。
本发明还包括上述高导热石墨烯/硅胶泡棉多层复合材料的制备方法,具体步骤如下:
3)制备硅胶涂层原料:
S1、将发泡硅胶A组分与导热填料混合均匀,得到导热填料填充A组分硅胶;
S2、将发泡硅胶B组分与导热填料混合均匀,得到导热填料填充B组分硅胶;
S3、将S1所得导热填料填充A组分硅胶与S2所得导热填料填充B组分硅胶在低于发泡温度下充分混合均匀,得到硅胶涂层原料;
4)制备高导热石墨烯/硅胶泡棉多层复合材料:将步骤1)所得硅胶涂层原料取出部分涂覆于石墨烯层表面形成硅胶涂层,在硅胶涂层上覆盖一层石墨烯层,重复上述步骤,形成石墨烯层与硅胶涂层交替层叠的复合层状结构;
5)将步骤2)所得复合层状结构在施加压力条件下发泡,最后切割、包装得到高导热石墨烯/硅胶泡棉多层复合材料。
按上述方案,S1所述发泡硅胶A组分由乙烯基硅油、卡斯特催化剂和发泡剂组成,所述乙烯基硅油粘度为10~500Pa·s,所述发泡剂为偶氮二甲酸二异丙酯,偶氮二甲酸钡,偶氮二异丁睛,对甲苯磺酰肼,碳酸氢铵中的一种或几种的混合物。
按上述方案,所述乙烯基硅油、卡斯特催化剂与发泡剂的质量比为100:0.001~0.005:5~15。
按上述方案,S1所述导热填料填充A组分硅胶中导热填料的质量百分含量为5~90%。
按上述方案,S2所述发泡硅胶B组分由含氢硅油、抑制剂和发泡剂组成,所述含氢硅油含氢量为0.3~0.5wt%,粘度为20~500Pa·s,含氢硅油中苯基含氢硅油质量百分含量>50%,所述抑制剂为1-乙炔基环己醇,所述发泡剂为偶氮二甲酸二异丙酯,偶氮二甲酸钡,偶氮二异丁睛,对甲苯磺酰肼,碳酸氢铵中的一种或几种的混合物。
按上述方案,所述含氢硅油、抑制剂与发泡剂的质量比为100:0.001~0.005:5~15。
按上述方案,S2所述导热填料填充B组分硅胶中导热填料的质量百分含量与S1所述导热填料填充A组分硅胶中导热填料的质量百分含量相同。
按上述方案,S3所述导热填料填充A组分硅胶与导热填料填充B组分硅胶质量比为0.66~3:1。
按上述方案,步骤2)所述硅胶涂层厚度为0.1-5mm。
按上述方案,步骤3)施加压力为100-500千帕,所述发泡温度为25-150℃,发泡时间为5-200分钟。
本发明还包括上述高导热石墨烯/硅胶泡棉多层复合材料作为热界面材料的应用,使用过程中,所述高导热石墨烯/硅胶泡棉多层复合材料中的石墨烯层垂直于热源设置。
本发明将氧化铝、氮化铝、铝粉、铜粉等导热颗粒填充制备导热硅胶泡棉,同时将导热硅胶泡棉与石墨烯膜复合,形成石墨烯-导热泡棉复合层状结构,作为热界面材料使用过程中使石墨烯膜与热源垂直设置,在导热硅胶泡棉中导热颗粒在压力下互相搭接构筑成连续导热通路,而垂直排列的多层石墨烯膜构成高效导热通路,这种多重导热路径使得复合材料具有优异的导热性能,同时,导热硅胶泡棉自身的孔洞结构保障了复合材料具有优异的缓冲减震性能。在泡棉制备过程中添加苯基含氢硅油,通过苯基含氢硅油所含苯环与石墨烯产生较强π-π相互作用,增加石墨烯层与硅胶泡棉的结合性,避免分层。
本发明的有益效果在于:1、本发明提供的高导热石墨烯/硅胶泡棉多层复合材料为多重层状结构,具有优良的导热性能和缓冲减震性能(导热系数1.5~3W/mK),实现了导热和缓冲功能的集成,作为热界面材料使用具有极大的市场应用前景。2、本发明的制备方法工艺简单,成本较低,适合工业化生产。
附图说明
图1为本发明实施例1所述的高导热石墨烯/硅胶泡棉多层复合材料的结构示意图;
图2为实施例1所制备的高导热石墨烯/硅胶泡棉多层复合材料中硅胶导热泡棉层的截面照片;
图3为实施例2所制备的高导热石墨烯/硅胶泡棉多层复合材料中硅胶导热泡棉层的扫描电子显微镜图;
图4为实施例3所制备的高导热石墨烯/硅胶泡棉多层复合材料中硅胶导热泡棉层的扫描电子显微镜图。
具体实施方式
为使本领域技术人员更好地理解本发明的技术方案,下面结合附图对本发明作进一步详细描述。
本发明实施例所用石墨烯膜购自武汉汉烯科技有限公司,导热系数为1300W/mK。
实施例1
一种高导热石墨烯/硅胶泡棉多层复合材料,由石墨烯层与硅胶导热泡棉层交替层叠复合得到,其中硅胶导热泡棉层分布有大量孔洞,还含有大量导热颗粒铝粉,其结构示意图如图1所示,具体制备步骤如下:
1)制备硅胶涂层原料:
S1、将50克A组分硅胶(粘度为50Pa·s的乙烯基硅油45.4克、偶氮二甲酸二异丙酯4.5克、卡斯特催化剂0.1毫克)与50克铝粉(10μm)混合,电磁搅拌5分钟,得到铝粉填充A组分硅胶;
S2、将50克B组分硅胶(含氢量为0.3wt%、粘度为50Pa·s、苯基含氢硅油含量60wt%的含氢硅油45.4克、偶氮二甲酸二异丙酯4.5克、抑制剂1-乙炔基环己醇0.1毫克)与50克铝粉(10μm)混合,电磁搅拌5分钟,得到铝粉填充B组分硅胶;
S3、将步骤S1所得铝粉填充A组分硅胶与步骤S2所得铝粉填充B组分硅胶混合,在烧杯中电磁搅拌2分钟充分混合,控制混合温度小于20℃,得到50%铝粉填充A+B组分硅胶;
2)制备高导热石墨烯/硅胶泡棉多层复合材料:将步骤1)所得A+B组分硅胶用涂膜机涂覆于石墨烯膜(厚度为50μm)表面形成硅胶涂层,控制硅胶涂层厚度为0.2毫米,在硅胶涂层之上覆盖一层石墨烯膜,然后重复之前步骤20次,最上层为石墨烯膜,形成21层石墨烯膜中间夹20层硅胶涂层的石墨烯膜-硅胶复合层状结构,总厚度为5厘米左右;
3)在步骤2)所得石墨烯膜-硅胶复合层状结构上用石英板压实(控制压强为350千帕),再放入烘箱中发泡,于30-35℃下发泡2小时,发泡后石墨烯膜-硅胶复合层状结构的厚度为15厘米左右,之后采用切刀垂直进行切割,控制切割厚度为5毫米,铺平后形成石墨烯膜垂直排列的石墨烯/硅胶泡棉多层复合材料。
用刀模将本实施例制备的石墨烯/硅胶泡棉多层复合材料切割成直径为3厘米的圆形垫片,在热流法导热系数测试仪上测试出其导热系数为2.2W/mK。将该圆形垫片置于夹具中在力学性能测试机上测试其压缩应变性能,参照《GB/T18942.1-2003-高聚物多孔弹性材料压缩应力应变特性的测定》,测得50%形变下应力为91KPa,样品反复压缩1000次后仍能恢复98%以上,展现了良好的力学性能。
图2为本实施例制备的高导热石墨烯/硅胶泡棉多层复合材料中硅胶导热泡棉层的截面光学照片,显示硅胶导热泡棉层内部存在大量的孔洞,并且硅胶导热泡棉层内均匀分布有大量导热颗粒铝粉。
实施例2
一种高导热石墨烯/硅胶泡棉多层复合材料,其制备方法步骤如下:
1)制备硅胶涂层原料:
S1、将50克A组分硅胶(粘度为50Pa·s的乙烯基硅油45克、碳酸氢铵5克、卡斯特催化剂0.1毫克)与60克氮化铝粉(5μm)混合,在双行星混胶机中混合10分钟,得到氮化铝粉填充A组分硅胶;
S2、将50克B组分硅胶(含氢量为0.5wt%、粘度为50Pa·s、苯基含氢硅油含量60wt%的含氢硅油45克、碳酸氢铵5克、抑制剂1-乙炔基环己醇0.1毫克)与60克氮化铝粉(5μm)混合,双行星混胶机中混合10分钟,得到铝粉填充B组分硅胶;
S3、将步骤S1所得氮化铝粉填充A组分硅胶与步骤S2所得氮化铝粉填充B组分硅胶混合,在烧杯中电磁搅拌2分钟充分混合,得到54.5%氮化铝粉填充A+B组分硅胶;
2)制备高导热石墨烯/硅胶泡棉多层复合材料:将步骤1)所得A+B组分硅胶用涂膜机涂覆于石墨烯膜(厚度为100μm)表面形成硅胶涂层,控制硅胶涂层厚度为0.5毫米,在硅胶涂层之上覆盖一层石墨烯膜,然后重复之前步骤15次,最上层为石墨烯膜,形成16层石墨烯膜中间夹15层硅胶涂层的石墨烯膜-硅胶复合层状结构,总厚度为9厘米左右;
3)在步骤2)所得石墨烯膜-硅胶复合层状结构上用石英板压实(控制压强为350千帕),再放入烘箱中发泡,于60℃下发泡1小时,发泡后石墨烯膜-硅胶复合层状结构的厚度为20厘米左右,之后采用切刀垂直进行切割,控制切割厚度为3毫米,铺平后形成石墨烯膜垂直排列的石墨烯/硅胶泡棉多层复合材料。
用刀模将本实施例制备的石墨烯/硅胶泡棉多层复合材料切割成直径为3厘米的圆形垫片,在热流法导热系数测试仪上测试出其导热系数为2.5W/mK。将该圆形垫片置于夹具中在力学性能测试机上测试其压缩应变性能,测得50%形变下应力为80KPa,样品反复压缩1000次后仍能恢复97%以上,展现了良好的力学性能。
图3为本实施例制备的高导热石墨烯/硅胶泡棉多层复合材料中硅胶导热泡棉层的内部扫描电子显微镜图,显示硅胶导热泡棉层内部存在许多微孔,并且硅胶导热泡棉层内均匀分布有大量导热颗粒氮化铝粉。
实施例3
一种高导热石墨烯/硅胶泡棉多层复合材料,其制备方法步骤如下:
1)制备硅胶涂层原料:
S1、将50克A组分硅胶(粘度为50Pa·s的乙烯基硅油45克、偶氮胺基苯5克、卡斯特催化剂0.1毫克)与30克长度为200μm的碳纤维微粉混合,在双行星混胶机中混合20分钟,得到碳纤维填充A组分硅胶;
S2、将50克B组分硅胶(含氢量为0.5wt%、粘度为50Pa·s、苯基含氢硅油含量60wt%的含氢硅油45克、偶氮胺基苯5克、抑制剂1-乙炔基环己醇0.1毫克)与30克长度为200μm的碳纤维微粉混合,双行星混胶机中混合20分钟,得到碳纤维填充B组分硅胶;
S3、将步骤S1所得碳纤维填充A组分硅胶与步骤S2所得碳纤维填充B组分硅胶混合,在烧杯中电磁搅拌2分钟充分混合,得到37.5%碳纤维填充A+B组分硅胶;
2)制备高导热石墨烯/硅胶泡棉多层复合材料:将步骤1)所得A+B组分硅胶用涂膜机涂覆于石墨烯膜(厚度为100μm)表面形成硅胶涂层,控制硅胶涂层厚度为0.3毫米,在硅胶涂层之上覆盖一层石墨烯膜,然后重复之前步骤50次,最上层为石墨烯膜,形成51层石墨烯膜中间夹50层硅胶涂层的石墨烯膜-硅胶复合层状结构,总厚度为7厘米左右;
3)在步骤2)所得石墨烯膜-硅胶复合层状结构上用石英板压实(控制压强为500千帕),再放入烘箱中发泡,于110℃下发泡1小时,发泡后石墨烯膜-硅胶复合层状结构的厚度为20厘米左右,之后采用切刀垂直进行切割,控制切割厚度为3毫米,铺平后形成石墨烯膜垂直排列的石墨烯/硅胶泡棉多层复合材料。
用刀模将本实施例制备的石墨烯/硅胶泡棉多层复合材料切割成直径为3厘米的圆形垫片,在热流法导热系数测试仪上测试出其导热系数为3W/mK。将该圆形垫片置于夹具中在力学性能测试机上测试其压缩应变性能,测得50%形变下应力为95KPa,样品反复压缩1000次后仍能恢复98%以上,展现了良好的力学性能。
图4为本实施例制备的高导热石墨烯/硅胶泡棉多层复合材料中硅胶导热泡棉层的内部的扫描电子显微镜照片,可以清晰地显示硅胶导热泡棉层内部存在许多微孔,并且硅胶导热泡棉层内均匀分布有大量碳纤维。
Claims (10)
1.一种高导热石墨烯/硅胶泡棉多层复合材料,其特征在于,所述高导热石墨烯/硅胶泡棉多层复合材料由石墨烯层与硅胶导热泡棉层交替层叠复合得到。
2.根据权利要求1所述的高导热石墨烯/硅胶泡棉多层复合材料,其特征在于,所述石墨烯层为市售石墨膜或石墨烯膜,导热系数为600~2000W/mK,石墨烯层厚度为2-100μm;所述高导热石墨烯/硅胶泡棉多层复合材料中石墨烯层的层数为10-100层。
3.根据权利要求1所述的高导热石墨烯/硅胶泡棉多层复合材料,其特征在于,所述硅胶导热泡棉层由硅胶泡棉与导热填料复合得到,其中导热填料的质量百分含量为5~90%,厚度为10-1000μm;所述导热填料为氧化铝,氮化铝,氮化硼,碳化硅,氮化硼,石墨烯,碳纤维,铝粉,铜粉,金刚石颗粒中的一种或几种,粒径为0.5-200μm。
4.一种权利要求1-3任一项所述的高导热石墨烯/硅胶泡棉多层复合材料的制备方法,其特征在于,具体步骤如下:
1)制备硅胶涂层原料:
S1、将发泡硅胶A组分与导热填料混合均匀,得到导热填料填充A组分硅胶;
S2、将发泡硅胶B组分与导热填料混合均匀,得到导热填料填充B组分硅胶;
S3、将S1所得导热填料填充A组分硅胶与S2所得导热填料填充B组分硅胶在低于发泡温度下充分混合均匀,得到硅胶涂层原料;
2)制备高导热石墨烯/硅胶泡棉多层复合材料:将步骤1)所得硅胶涂层原料取出部分涂覆于石墨烯层表面形成硅胶涂层,在硅胶涂层上覆盖一层石墨烯层,重复上述步骤,形成石墨烯层与硅胶涂层交替层叠的复合层状结构;
3)将步骤2)所得复合层状结构在施加压力条件下发泡,最后切割、包装得到高导热石墨烯/硅胶泡棉多层复合材料。
5.根据权利要求4所述的高导热石墨烯/硅胶泡棉多层复合材料的制备方法,其特征在于,S1所述发泡硅胶A组分由乙烯基硅油、卡斯特催化剂和发泡剂组成,所述乙烯基硅油粘度为10~500Pa·s,所述发泡剂为偶氮二甲酸二异丙酯,偶氮二甲酸钡,偶氮二异丁睛,对甲苯磺酰肼,碳酸氢铵中的一种或几种的混合物。
6.根据权利要求4所述的高导热石墨烯/硅胶泡棉多层复合材料的制备方法,其特征在于,S1所述导热填料填充A组分硅胶中导热填料的质量百分含量为5~90%。
7.根据权利要求4所述的高导热石墨烯/硅胶泡棉多层复合材料的制备方法,其特征在于,S2所述发泡硅胶B组分由含氢硅油、抑制剂和发泡剂组成,所述含氢硅油含氢量为0.3~0.5wt%,粘度为20~500Pa·s,含氢硅油中苯基含氢硅油质量百分含量>50%,所述抑制剂为1-乙炔基环己醇,所述发泡剂为偶氮二甲酸二异丙酯,偶氮二甲酸钡,偶氮二异丁睛,对甲苯磺酰肼,碳酸氢铵中的一种或几种的混合物。
8.根据权利要求4所述的高导热石墨烯/硅胶泡棉多层复合材料的制备方法,其特征在于,S3所述导热填料填充A组分硅胶与导热填料填充B组分硅胶质量比为0.66~3:1。
9.根据权利要求4所述的高导热石墨烯/硅胶泡棉多层复合材料的制备方法,其特征在于,步骤3)施加压力为100-500千帕,所述发泡温度为25-150℃,发泡时间为5-200分钟。
10.一种权利要求1-3任一项所述的高导热石墨烯/硅胶泡棉多层复合材料作为热界面材料的应用,其特征在于,使用过程中,所述高导热石墨烯/硅胶泡棉多层复合材料中的石墨烯层垂直于热源设置。
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