CN110054999B - 防残胶导热双面胶带的制备方法 - Google Patents

防残胶导热双面胶带的制备方法 Download PDF

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CN110054999B
CN110054999B CN201910109602.3A CN201910109602A CN110054999B CN 110054999 B CN110054999 B CN 110054999B CN 201910109602 A CN201910109602 A CN 201910109602A CN 110054999 B CN110054999 B CN 110054999B
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金闯
张庆杰
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Sidike New Materials Jiangsu Co Ltd
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Abstract

本发明公开了一种防残胶导热双面胶带的制备方法，包括以下步骤：S1.将端羟基聚硅氧烷、环氧树脂、MQ树脂、四乙氧基硅烷、异丁基三乙氧基硅烷、乙烯基甲苯和有机溶剂加入反应釜中，升温加入钛酸异丙酯和有机锡类催化剂，反应得有机硅压敏胶液；S2.将石墨烯粉末、纳米氮化硼、3‑巯丙基三乙氧基硅烷、乙氧基炔二醇和有机溶剂加入到搅拌釜中，再将有机硅压敏胶液加入搅拌釜中，搅拌制得导热胶粘剂；S3.将导热胶粘剂涂布于玻纤布基材层两面，烘干固化，形成导热胶层；S4.将离型膜层贴覆于导热胶层表面，收卷分切；本发明制得的防残胶导热双面胶带导热系数高，可用于电子元器件的散热和粘结。

Description

防残胶导热双面胶带的制备方法
技术领域
本发明涉及胶带领域，尤其涉及一种防残胶导热双面胶带的制备方法。
背景技术
随着电子行业的快速发展，电子产品趋于轻便，体积越来越小，因而电子元件的集成度就越来越高，所以对电子元器件的导散热性能的要求就越来越高。导热胶带因具有导热和粘接为一体的功能而被广泛的使用，且其具有柔软性、压缩性、服帖性和适应温度范围大等特性而占据着较大的导热材料市场。
目前制备导热胶带的方法是在胶体中加入导热填料，达到导热的目的，但是目前的导热双面胶的导热系数普遍比较小，且胶体在长期在高温环境下工作后揭除时容易发生残胶的情况。因此，如何提供一种导热性能好，且经湿热老化后无明显残胶的防残胶导热双面胶带，成为本领域技术人员努力的方向。
发明内容
本发明目的在于提供一种防残胶导热双面胶带的制备方法，该方法制备得到的胶带导热性能好，且经湿热老化后无明显残胶，可移除性好。
为达到上述目的，本发明采用的技术方案是：一种防残胶导热双面胶带的制备方法，所述防残胶导热双面胶带包括玻纤布基材层、涂布于玻纤布基材层两面的导热胶层、以及贴覆于导热胶层相背于玻纤布基材层的一面的离型膜层；
所述防残胶导热双面胶带的制备方法包括以下步骤：
S1. 将端羟基聚硅氧烷30~45份、环氧树脂10~18份、MQ树脂30~40份、四乙氧基硅烷2~5份、异丁基三乙氧基硅烷1~3份、乙烯基甲苯2~6份和有机溶剂30~40份加入反应釜中，升温至130~135℃后加入钛酸异丙酯0.1~1份和有机锡类催化剂0.1~3份，在140~150℃下反应2~3小时，冷却后制得有机硅压敏胶液；
S2. 将石墨烯粉末25~40份、纳米氮化硼5~10份、3-巯丙基三乙氧基硅烷5~10份、乙氧基炔二醇0.1~1份和剩余的有机溶剂加入到搅拌釜中，高速分散40~60分钟，再将S1中制得的有机硅压敏胶液缓慢加入搅拌釜中，搅拌30~40分，制得导热胶粘剂；
S3. 将S2中制得的导热胶粘剂涂布于玻纤布基材层两面，烘干、固化，形成导热胶层；
S4. 将离型膜层贴覆于导热胶层相背于玻纤布基材层的一面，收卷分切，即制得所述防残胶导热双面胶带；
所述份数均为重量份，S1和S2中使用溶剂的总量为55~70重量份。
上述技术方案中进一步改进的技术方案如下：
1. 上述方案中，所述端羟基聚硅氧烷的分子量为20~30万，所述端羟基聚硅氧烷的羟基含量为0.3~1.5%。
2. 上述方案中，所述有机锡类催化剂选自二月桂酸二丁基锡、二月桂酸二辛基锡、二月桂酸二丁基锡或者辛酸亚锡中的至少一种。
3. 上述方案中，所述有机溶剂为乙酸乙酯。
4. 上述方案中，所述玻纤布基材层的厚度为20~50μm。
5. 上述方案中，所述导热胶层的厚度为5~20μm。
由于上述技术方案的运用，本发明与现有技术相比具有下列优点：
1. 本发明防残胶导热双面胶带的制备方法，其导热胶层采用石墨烯粉末25~40份和纳米氮化硼5~10份形成复合导热体系，并添加了乙氧基炔二醇0.1~1份和3-巯丙基三乙氧基硅烷5~10份与导热填料共同分散，以进一步改善其导热性能，起到尽量少的导热填料添加量达到较高导热系数的效果，制得胶层的导热系数达到3W/(m.K)以上，避免了导热填料添加过多影响胶体力学性能和绝缘性能的问题。
2. 本发明防残胶导热双面胶带的制备方法，其导热胶层配方以端羟基聚硅氧烷30~45份为基础树脂并引入了环氧树脂10~18份，在此基础上，还添加了四乙氧基硅烷2~5份、异丁基三乙氧基硅烷1~3份和乙烯基甲苯2~6份，并采用钛酸异丙酯0.1~1份和有机锡类催化剂0.1~3份的混合催化体系，制得的胶层交联密度大，具有较高的内聚力，因此本发明制备的的防残胶导热双面胶带经湿热老化后无明显残胶，可移除性好。
附图说明
附图1为本发明残胶导热双面胶带示意图。
具体实施方式
下面结合实施例对本发明作进一步描述：
实施例1~4：一种防残胶导热双面胶带的制备方法，所述防残胶导热双面胶带包括玻纤布基材层、涂布于玻纤布基材层两面的导热胶层、以及贴覆于导热胶层相背于玻纤布基材层的一面的离型膜层；
上述玻纤布基材层的厚度为30μm，上述导热胶层的厚度为15μm；
上述防残胶导热双面胶带的制备方法包括以下步骤：
S1. 将端羟基聚硅氧烷30~45份、环氧树脂10~18份、MQ树脂30~40份、四乙氧基硅烷2~5份、异丁基三乙氧基硅烷1~3份、乙烯基甲苯2~6份和有机溶剂30~40份加入反应釜中，升温至130~135℃后加入钛酸异丙酯0.1~1份和有机锡类催化剂0.1~3份，在140~150℃下反应2~3小时，冷却后制得有机硅压敏胶液；
S2. 将石墨烯粉末25~40份、纳米氮化硼5~10份、3-巯丙基三乙氧基硅烷5~10份、乙氧基炔二醇0.1~1份和剩余的有机溶剂加入到搅拌釜中，高速分散40~60分钟，再将S1中制得的有机硅压敏胶液缓慢加入搅拌釜中，搅拌30~40分，制得导热胶粘剂；
S3. 将S2中制得的导热胶粘剂涂布于玻纤布基材层两面，烘干、固化，形成导热胶层；
S4. 将离型膜层贴覆于导热胶层相背于玻纤布基材层的一面，收卷分切，即制得所述防残胶导热双面胶带；
各实施例中的导热胶层具体由以下重量份组分组成：
表1
Figure 927975DEST_PATH_IMAGE002
上述端羟基聚硅氧烷的分子量为20~30万，上述端羟基聚硅氧烷的羟基含量为0.3~1.5%。
上述实施例1的有机锡类催化剂为二月桂酸二丁基锡，实施例2的有机锡类催化剂为二月桂酸二辛基锡，实施例3的有机锡类催化剂为二月桂酸二丁基锡，实施例4的有机锡类催化剂为辛酸亚锡。
上述有机溶剂为乙酸乙酯。
对比例1~3，一种导热双面胶带的制备方法，所述导热双面胶带包括玻纤布基材层、涂布于玻纤布基材层两面的导热胶层、以及贴覆于导热胶层相背于玻纤布基材层的一面的离型膜层；
上述玻纤布基材层的厚度为30μm，上述导热胶层的厚度为15μm；
上述导热双面胶带的制备方法包括以下步骤：
S1. 将端羟基聚硅氧烷、环氧树脂、MQ树脂、四乙氧基硅烷、异丁基三乙氧基硅烷、乙烯基甲苯和部分有机溶剂加入反应釜中，升温至130~135℃后加入钛酸异丙酯和有机锡类催化剂，在140~150℃下反应2~3小时，冷却后制得有机硅压敏胶液；
S2. 将石墨烯粉末、纳米氮化硼、3-巯丙基三乙氧基硅烷、乙氧基炔二醇和剩余的有机溶剂加入到搅拌釜中，高速分散40~60分钟，再将S1中制得的有机硅压敏胶液缓慢加入搅拌釜中，搅拌30~40分，制得导热胶粘剂；
S3. 将S2中制得的导热胶粘剂涂布于玻纤布基材层两面，烘干、固化，形成导热胶层；
S4. 将离型膜层贴覆于导热胶层相背于玻纤布基材层的一面，收卷分切，即制得所述导热双面胶带；
各对比例的导热胶层具体由以下重量份组分组成：
表2
Figure 641853DEST_PATH_IMAGE004
上述端羟基聚硅氧烷的分子量为20~30万，上述端羟基聚硅氧烷的羟基含量为0.3~1.5%。
上述对比例1的有机锡类催化剂为二月桂酸二丁基锡，对比例2的有机锡类催化剂为二月桂酸二丁基锡，对比例3的有机锡类催化剂为辛酸亚锡。
上述有机溶剂为乙酸乙酯。
上述实施例1~4和对比例1~3制得的导热双面胶带的导热胶层性能如表3所示：
表3
Figure 952749DEST_PATH_IMAGE006
表3中，“×”表示明显残胶，“△”表示轻微残胶，“○”表示无残胶。
如表3的评价结果所示，本发明各实施例制备的防残胶导热双面胶带的导热胶层的导热系数均高于各对比例，且经湿热老化后亦无明显残胶，制得的胶带可移除性好。
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。

Claims (6)

1.一种防残胶导热双面胶带的制备方法，其特征在于：所述防残胶导热双面胶带包括玻纤布基材层、涂布于玻纤布基材层两面的导热胶层、以及贴覆于导热胶层相背于玻纤布基材层的一面的离型膜层；
所述防残胶导热双面胶带的制备方法包括以下步骤：
S1. 将端羟基聚硅氧烷30~45份、环氧树脂10~18份、MQ树脂30~40份、四乙氧基硅烷2~5份、异丁基三乙氧基硅烷1~3份、乙烯基甲苯2~6份和有机溶剂30~40份加入反应釜中，升温至130~135℃后加入钛酸异丙酯0.1~1份和有机锡类催化剂0.1~3份，在140~150℃下反应2~3小时，冷却后制得有机硅压敏胶液；
S2. 将石墨烯粉末25~40份、纳米氮化硼5~10份、3-巯丙基三乙氧基硅烷5~10份、乙氧基炔二醇0.1~1份和剩余的有机溶剂加入到搅拌釜中，高速分散40~60分钟，再将S1中制得的有机硅压敏胶液缓慢加入搅拌釜中，搅拌30~40分，制得导热胶粘剂；
S3. 将S2中制得的导热胶粘剂涂布于玻纤布基材层两面，烘干、固化，形成导热胶层；
S4. 将离型膜层贴覆于导热胶层相背于玻纤布基材层的一面，收卷分切，即制得所述防残胶导热双面胶带；
所述份数均为重量份，S1和S2中使用溶剂的总量为55~70重量份。
2.根据权利要求1所述的防残胶导热双面胶带的制备方法，其特征在于：所述端羟基聚硅氧烷的分子量为20~30万，所述端羟基聚硅氧烷的羟基含量为0.3~1.5%。
3.根据权利要求1所述的防残胶导热双面胶带的制备方法，其特征在于：所述有机锡类催化剂选自二月桂酸二丁基锡、二月桂酸二辛基锡、二月桂酸二丁基锡或者辛酸亚锡中的至少一种。
4.根据权利要求1所述的防残胶导热双面胶带的制备方法，其特征在于：所述有机溶剂为乙酸乙酯。
5.根据权利要求1所述的防残胶导热双面胶带的制备方法，其特征在于：所述玻纤布基材层的厚度为20~50μm。
6.根据权利要求1所述的防残胶导热双面胶带的制备方法，其特征在于：所述导热胶层的厚度为5~20μm。
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