CN110128992A - 一种能有效提高导热效率的聚氨酯灌封胶及制备方法 - Google Patents

一种能有效提高导热效率的聚氨酯灌封胶及制备方法 Download PDF

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CN110128992A
CN110128992A CN201910412783.7A CN201910412783A CN110128992A CN 110128992 A CN110128992 A CN 110128992A CN 201910412783 A CN201910412783 A CN 201910412783A CN 110128992 A CN110128992 A CN 110128992A
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Abstract

本发明涉及聚氨酯灌封胶制备技术领域，且公开了一种能有效提高导热效率的聚氨酯灌封胶及制备方法，通过在聚氨酯树脂的原料组分中添加导热系数高的微米级氮化铝陶瓷颗粒，同时添加具有胶凝作用的微米级MgO颗粒，各组分在硅烷偶联剂、钛酸酯偶联剂、气相二氧化硅防沉剂与异佛尔酮二异氰酸酯固化剂的共同作用下，发生交联固化反应，制备出聚氨酯灌封胶。本发明解决了现有技术中的聚氨酯灌封胶，在具有优异电绝缘性能的同时，无法实现对灌封的电子元器件有效散热的技术问题。

Description

一种能有效提高导热效率的聚氨酯灌封胶及制备方法
技术领域
本发明涉及聚氨酯灌封胶制备技术领域，具体为一种能有效提高导热效率的聚氨酯灌封胶及制备方法。
背景技术
在集成电路的制造过程中，对集成电路进行封装是非常必要的步骤，封装就是使用灌浆材料把构成电子设备的各个零部件按照要求进行组装，将电子元器件密封起来，使电子器件与外界环境隔离。然而电子元器件的散热问题，对电子灌封胶提出了更高的要求，要求电子灌封胶不但要具有较好的电绝缘性能，而且还要具有较高的导热率。
聚氨酯灌封胶是一类以多异氰酸酯与低聚物多元醇反应制得的由聚合物多元醇与氨基甲酸酯重复单元组成的嵌段共聚物。聚氨酯灌封胶具有硬度范围较宽，有着优良的耐磨性，具有良好的弹性、耐化学腐蚀性和粘结性，气体透过率低，具有较优异的吸振性能。然而，聚氨酯是热的不良导体，导热系数仅为0.18～0.20W/mK，一般地，导热绝缘材料的导热系数大于1W/mK左右，才可以应用于电子器件的散热，所以，聚氨酯灌封胶远远达不到导热的要求。
本发明提供一种能有效提高导热效率的聚氨酯灌封胶及制备方法，旨在解决现有技术中的聚氨酯灌封胶，在具有优异电绝缘性能的同时，无法实现对灌封的电子元器件有效散热的技术问题。
发明内容
(一)解决的技术问题
针对现有技术的不足，本发明提供了一种能有效提高导热效率的聚氨酯灌封胶及制备方法，解决了现有技术中的聚氨酯灌封胶，在具有优异电绝缘性能的同时，无法实现对灌封的电子元器件有效散热的技术问题。
(二)技术方案
为实现上述目的，本发明提供如下技术方案：
一种能有效提高导热效率的聚氨酯灌封胶，包括以下重量份数配比的原料：100份聚环氧丙烷二元醇、15份质量分数0.1％的二月桂酸二丁基锡、5份质量分数0.2％的有机硅消泡剂、8份由乙二醇、1,4-丁二醇、乙二胺及三羟甲基丙烷按照等质量组成的扩链交联剂、19份硅烷偶联剂、16份钛酸酯偶联剂、45份异佛尔酮二异氰酸酯固化剂、20份微米级氮化铝陶瓷颗粒、5份MgO胶凝剂；
通过在聚氨酯灌封胶的原料组分中添加导热系数高的微米级氮化铝陶瓷颗粒，同时添加具有胶凝作用的MgO，各组分在硅烷偶联剂、钛酸酯偶联剂与异佛尔酮二异氰酸酯固化剂的共同作用下，发生交联固化反应，制备出聚氨酯灌封胶。
优选的，所述微米级氮化铝陶瓷颗粒包括：13份平均粒径≤25um的氮化铝陶瓷和7份平均粒径≤10um的氮化铝陶瓷。
优选的，所述MgO胶凝剂的平均粒径≤25um。
一种能有效提高导热效率的聚氨酯灌封胶的制备方法，包括以下步骤：
(1)称取19份乙烯基三乙氧基硅烷偶联剂，加入由5份蒸馏水和15份无水乙醇组成的溶剂中，在室温下水解30min，配制得到偶联剂A；
(2)将8份钛酸四异丙酯加热到份g液体石蜡中，充分溶解后，配制得到偶联剂B；
(3)称取20份微米级氮化铝陶瓷颗粒、5份MgO胶凝剂，配制得到填料组分；
(4)将上述填料组分加入到装有搅拌装置和加热装置的反应器中，加入8份气相二氧化硅防沉剂，在80～100℃下搅拌，转速为300～500rpm，加入偶联剂A与偶联剂B后搅拌均匀；制备得到导热填料；
(5)将100份减压脱水处理的聚环氧丙烷二元醇、15份质量分数0.1％的二月桂酸二丁基锡、5份质量分数0.2％的有机硅消泡剂及8份由乙二醇、1,4-丁二醇、乙二胺及三羟甲基丙烷按照等质量组成的扩链交联剂，在500～600rpm下剪切2h，加入导热填料，搅拌均匀，制备得到基体组分；
(6)称取45份异佛尔酮二异氰酸酯固化剂加入基体组分中，排气泡后将灌封胶转移至聚四氟乙烯模具中，流平，在80～100℃下固化处理，制备得到聚氨酯灌封胶。
(三)有益的技术效果
与现有技术相比，本发明具备以下有益的技术效果：
通过在聚氨酯树脂的原料组分中添加导热系数较高的两种不同粒径的微米级氮化铝陶瓷(AlN)，同时添加具有胶凝作用的微米级MgO颗粒，各组分在硅烷偶联剂、钛酸酯偶联剂、气相二氧化硅防沉剂与异佛尔酮二异氰酸酯固化剂的共同作用下，发生交联固化反应，制备出聚氨酯灌封胶；
且制备出的聚氨酯灌封胶的导热系数为1.46～1.62W/mK，体积电阻率为3.1×1012～3.9×1012Ω·cm，从而取得了在具有优异电绝缘性能的同时，实现对灌封的电子元器件有效散热的技术效果。
具体实施方式
实施例一：
(1)称取19g乙烯基三乙氧基硅烷偶联剂，加入由5g蒸馏水和15g无水乙醇组成的溶剂中，在室温下水解30min，配制得到偶联剂A；
(2)将8g钛酸四异丙酯加热到8g液体石蜡中，充分溶解后，配制得到偶联剂B；
(3)称取13g平均粒径≤25um的氮化铝陶瓷(AlN)、7g平均粒径≤10um的氮化铝陶瓷(AlN)、5g平均粒径≤25um的MgO，配制得到填料组分；
(4)将上述填料组分加入到装有搅拌装置和加热装置的反应器中，加入8g气相二氧化硅防沉剂，在80℃下搅拌，转速为300rpm，缓慢加入偶联剂A后，转为600rpm下搅拌10min；
转为300rpm下搅拌，缓慢加入偶联剂B后，转为600rpm下搅拌10min；冷却后出料，将填料置于120℃的干燥箱内，干燥6h，制备得到导热填料；
(5)将100g聚环氧丙烷二元醇加热至120℃减压脱水处理3h；
(6)将减压脱水处理的聚环氧丙烷二元醇、15g质量分数0.1％的二月桂酸二丁基锡、5g质量分数0.2％的有机硅消泡剂及8g由乙二醇、1,4-丁二醇、乙二胺及三羟甲基丙烷按照等质量组成的扩链交联剂，在转速为120rpm下混合均匀，转为500rpm下剪切2h，缓慢加入导热填料，转为600rpm下搅拌1h，制备得到基体组分；
(7)称取45g异佛尔酮二异氰酸酯固化剂加入基体组分中，在转速300rpm下混合均匀，之后以抽真空放气的方式对灌封胶进行排气泡处理，排气泡后将灌封胶转移至聚四氟乙烯模具中，流平，至灌封胶表面平整，之后在80℃下固化处理2h，制备得到聚氨酯灌封胶；
(8)上述制备出的聚氨酯灌封胶的导热系数为1.62W/mK，体积电阻率为3.9×1012Ω·cm。
实施例二：
(1)称取19g乙烯基三乙氧基硅烷偶联剂，加入由5g蒸馏水和15g无水乙醇组成的溶剂中，在室温下水解30min，配制得到偶联剂A；
(2)将8g钛酸四异丙酯加热到8g液体石蜡中，充分溶解后，配制得到偶联剂B；
(3)称取20g平均粒径≤25um的氮化铝陶瓷(AlN)、5g平均粒径≤25um的MgO，配制得到填料组分；
(4)将上述填料组分加入到装有搅拌装置和加热装置的反应器中，加入8g气相二氧化硅防沉剂，在100℃下搅拌，转速为500rpm，缓慢加入偶联剂A后，转为800rpm下搅拌10min；
转为500rpm下搅拌，缓慢加入偶联剂B后，转为800rpm下搅拌10min；冷却后出料，将填料置于120℃的干燥箱内，干燥6h，制备得到导热填料；
(5)将100g聚环氧丙烷二元醇加热至120℃减压脱水处理3h；
(6)将减压脱水处理的聚环氧丙烷二元醇、15g质量分数0.1％的二月桂酸二丁基锡、5g质量分数0.2％的有机硅消泡剂及8g由乙二醇、1,4-丁二醇、乙二胺及三羟甲基丙烷按照等质量组成的扩链交联剂，在转速为180rpm下混合均匀，转为600rpm下剪切2h，缓慢加入导热填料，转为800rpm下搅拌1h，制备得到基体组分；
(7)称取45g异佛尔酮二异氰酸酯固化剂加入基体组分中，在转速500rpm下混合均匀，之后以抽真空放气的方式对灌封胶进行排气泡处理，排气泡后将灌封胶转移至聚四氟乙烯模具中，流平，至灌封胶表面平整，之后在100℃下固化处理2h，制备得到聚氨酯灌封胶；
(8)上述制备出的聚氨酯灌封胶的导热系数为1.47W/mK，体积电阻率为3.1×1012Ω·cm。
实施例三：
(1)称取19g乙烯基三乙氧基硅烷偶联剂，加入由5g蒸馏水和15g无水乙醇组成的溶剂中，在室温下水解30min，配制得到偶联剂A；
(2)将8g钛酸四异丙酯加热到8g液体石蜡中，充分溶解后，配制得到偶联剂B；
(3)称取20g平均粒径≤10um的氮化铝陶瓷(AlN)、5g平均粒径≤25um的MgO，配制得到填料组分；
(4)将上述填料组分加入到装有搅拌装置和加热装置的反应器中，加入8g气相二氧化硅防沉剂，在90℃下搅拌，转速为400rpm，缓慢加入偶联剂A后，转为400rpm下搅拌10min；
转为400rpm下搅拌，缓慢加入偶联剂B后，转为700rpm下搅拌10min；冷却后出料，将填料置于120℃的干燥箱内，干燥6h，制备得到导热填料；
(5)将100g聚环氧丙烷二元醇加热至120℃减压脱水处理3h；
(6)将减压脱水处理的聚环氧丙烷二元醇、15g质量分数0.1％的二月桂酸二丁基锡、5g质量分数0.2％的有机硅消泡剂及8g由乙二醇、1,4-丁二醇、乙二胺及三羟甲基丙烷按照等质量组成的扩链交联剂，在转速为150rpm下混合均匀，转为550rpm下剪切2h，缓慢加入导热填料，转为700rpm下搅拌1h，制备得到基体组分；
(7)称取45g异佛尔酮二异氰酸酯固化剂加入基体组分中，在转速400rpm下混合均匀，之后以抽真空放气的方式对灌封胶进行排气泡处理，排气泡后将灌封胶转移至聚四氟乙烯模具中，流平，至灌封胶表面平整，之后在90℃下固化处理2h，制备得到聚氨酯灌封胶；
(8)上述制备出的聚氨酯灌封胶的导热系数为1.46W/mK，体积电阻率为3.5×1012Ω·cm。

Claims (4)

1.一种能有效提高导热效率的聚氨酯灌封胶，其特征在于，包括以下重量份数配比的原料：100份聚环氧丙烷二元醇、15份质量分数0.1％的二月桂酸二丁基锡、5份质量分数0.2％的有机硅消泡剂、8份由乙二醇、1,4-丁二醇、乙二胺及三羟甲基丙烷按照等质量组成的扩链交联剂、19份硅烷偶联剂、16份钛酸酯偶联剂、8份气相二氧化硅防沉剂、45份异佛尔酮二异氰酸酯固化剂、20份微米级氮化铝陶瓷颗粒、5份微米级MgO胶凝剂；
通过在聚氨酯树脂的原料组分中添加导热系数高的微米级氮化铝陶瓷颗粒，同时添加具有胶凝作用的微米级MgO颗粒，各组分在硅烷偶联剂、钛酸酯偶联剂、气相二氧化硅防沉剂与异佛尔酮二异氰酸酯固化剂的共同作用下，发生交联固化反应，制备出聚氨酯灌封胶。
2.根据权利要求1所述的聚氨酯灌封胶，其特征在于，所述微米级氮化铝陶瓷颗粒包括：13份平均粒径≤25um的氮化铝陶瓷和7份平均粒径≤10um的氮化铝陶瓷。
3.根据权利要求1所述的聚氨酯灌封胶，其特征在于，所述MgO胶凝剂的平均粒径≤25um。
4.一种能有效提高导热效率的聚氨酯灌封胶的制备方法，其特征在于，包括以下步骤：
(1)称取19份乙烯基三乙氧基硅烷偶联剂，加入由5份蒸馏水和15份无水乙醇组成的溶剂中，在室温下水解30min，配制得到偶联剂A；
(2)将8份钛酸四异丙酯加热到份g液体石蜡中，充分溶解后，配制得到偶联剂B；
(3)称取20份微米级氮化铝陶瓷颗粒、5份微米级MgO胶凝剂，配制得到填料组分；
(4)将上述填料组分加入到装有搅拌装置和加热装置的反应器中，加入8份气相二氧化硅防沉剂，在80～100℃下搅拌，转速为300～500rpm，加入偶联剂A与偶联剂B后搅拌均匀；制备得到导热填料；
(5)将100份减压脱水处理的聚环氧丙烷二元醇、15份质量分数0.1％的二月桂酸二丁基锡、5份质量分数0.2％的有机硅消泡剂及8份由乙二醇、1,4-丁二醇、乙二胺及三羟甲基丙烷按照等质量组成的扩链交联剂，在500～600rpm下剪切2h，加入导热填料，搅拌均匀，制备得到基体组分；
(6)称取45份异佛尔酮二异氰酸酯固化剂加入基体组分中，排气泡后将灌封胶转移至聚四氟乙烯模具中，流平，在80～100℃下固化处理，制备得到聚氨酯灌封胶。
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