CN114874644A - 一种包覆型球形硅微粉的制备方法 - Google Patents

一种包覆型球形硅微粉的制备方法 Download PDF

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CN114874644A
CN114874644A CN202210427487.6A CN202210427487A CN114874644A CN 114874644 A CN114874644 A CN 114874644A CN 202210427487 A CN202210427487 A CN 202210427487A CN 114874644 A CN114874644 A CN 114874644A
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周蔚
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Abstract

本发明开发了一种包覆型球形硅微粉的制备方法，通过在硅微粉研磨过程中，添加水玻璃包覆液，使研磨得到的硅微粉的流动性得到增强，其在环氧树脂体系中的储存稳定性也有明显改善；水玻璃溶液中添加硅油混合液，可进一步提升硅微粉的流动性，而且在环氧树脂体系中具有自分散效果，储存稳定性进一步增强。

Description

一种包覆型球形硅微粉的制备方法
技术领域
本发明涉及硅微粉的生产工艺，尤其涉及一种包覆型球形硅微粉的制备方法。
背景技术
硅微粉是一种用途极为广泛的无机材料，具有导热系数小、介电性能优、热膨胀系数小、耐腐蚀等特点。集成电路封装是指把电路管脚用导线接引到外部接头处时，用集成电路封装进行安装、固定、密封、保护集成电路。集成电路封装还能为集成电路起到保护作用，保证其正常工作。
目前，集成电路封装主要使用环氧树脂体系，这是由于环氧树脂体系热固化的效率极高，而且工艺简单、成本低廉。环氧树脂体系在制备和使用时需对分散的硅微粉进行长时间的研磨或砂磨，以使其分散均匀。在研磨的过程中需添加润湿分散剂，但润湿分散剂在较长时间储存后，由于双电层效应减弱而使硅微粉凝聚，使环氧树脂体系的储存稳定性不佳。
本发明开发了一种包覆型球形硅微粉的制备方法，所制得的包覆型球形硅微粉在环氧树脂体系中具有自分散效果，同时具有良好的储存稳定性，有利于提高后续封装效率。
发明内容
本发明开发了一种包覆型球形硅微粉的制备方法，通过在硅微粉研磨过程中，添加水玻璃包覆液，使研磨得到的硅微粉的流动性得到增强，其在环氧树脂体系中的储存稳定性也有明显改善。
一种包覆型球形硅微粉的制备方法，所述制备方法具体如下：
(1)选择高纯石英砂，经多级球磨机破碎为中位粒径10.0～12.0μm的原级硅微粉；
(2)将水玻璃溶解于水中，溶解制得1.15-1.20g/mL的水玻璃溶液；
(3)将上述原级硅微粉继续球磨，球磨的过程中喷淋原级硅微粉质量2％-4％的水玻璃溶液；
(4)球磨的过程中持续通入50℃-60℃的热空气，通气速率控制为30-50L/min*kg原级硅微粉；
(5)持续球磨至中位粒径1.2～3.0μm，制得包覆型球形硅微粉。
进一步的，所述水玻璃的模数为2.2-2.6。
进一步的，第(2)步制得的水玻璃溶液中继续添加溶液质量1％-3％的乙烯基羟基硅油:阳离子羟基硅油体积比为3-5:1的硅油混合液，均质乳化而成。
进一步的，所述乙烯基羟基硅油牌号为GP-203。
进一步的，所述阳离子羟基硅油牌号为SM-5017。
进一步的，第(3)步喷淋水玻璃溶液之前在原级硅微粉中加入原级硅微粉质量1％-2％的含519酰胺增电剂质量分数2％-3％的无水乙醇溶液。
本发明的优点：
1、本发明通过在硅微粉研磨过程中，添加水玻璃包覆液，使研磨得到的硅微粉的流动性得到增强，其在环氧树脂体系中的储存稳定性也有明显改善；
2、通过在水玻璃溶液中添加硅油混合液，可进一步提升硅微粉的流动性，而且在环氧树脂体系中具有自分散效果，储存稳定性进一步增强；
3、在水玻璃溶液包覆之前加入酰胺增电剂，能提升包覆层与硅微粉的结合力，使包覆型球形硅微粉的分散效果和储存稳定性进一步增强。
具体实施方式
实施例1
一种包覆型球形硅微粉的制备方法，制备方法具体如下：
(1)选择高纯石英砂，经多级球磨机破碎为中位粒径12.0μm的原级硅微粉；
(2)将模数为2.6的水玻璃溶解于水中，溶解制得1.15g/mL的水玻璃溶液；然后在水玻璃溶液中继续添加溶液质量1％的乙烯基羟基硅油GP-203:阳离子羟基硅油SM-5017体积比为5:1的硅油混合液，均质乳化而成；
(3)将上述原级硅微粉继续球磨，球磨的过程中在原级硅微粉中加入原级硅微粉质量1％的含519酰胺增电剂质量分数3％的无水乙醇溶液；然后喷淋原级硅微粉质量2％的水玻璃溶液；
(4)球磨的过程中持续通入50℃的热空气，通气速率控制为50L/min*kg原级硅微粉；
(5)持续球磨至中位粒径2.0μm，制得包覆型球形硅微粉。
实施例2
一种包覆型球形硅微粉的制备方法，制备方法具体如下：
(1)选择高纯石英砂，经多级球磨机破碎为中位粒径10.0μm的原级硅微粉；
(2)将模数为2.3的水玻璃溶解于水中，溶解制得1.17g/mL的水玻璃溶液；然后在水玻璃溶液中继续添加溶液质量2％的乙烯基羟基硅油GP-203:阳离子羟基硅油SM-5017体积比为4:1的硅油混合液，均质乳化而成；
(3)将上述原级硅微粉继续球磨，球磨的过程中在原级硅微粉中加入原级硅微粉质量2％的含519酰胺增电剂质量分数2％的无水乙醇溶液；然后喷淋原级硅微粉质量3％的水玻璃溶液；
(4)球磨的过程中持续通入60℃的热空气，通气速率控制为45L/min*kg原级硅微粉；
(5)持续球磨至中位粒径2.0μm，制得包覆型球形硅微粉。
实施例3
一种包覆型球形硅微粉的制备方法，制备方法具体如下：
(1)选择高纯石英砂，经多级球磨机破碎为中位粒径10.0μm的原级硅微粉；
(2)将模数为2.2的水玻璃溶解于水中，溶解制得1.20g/mL的水玻璃溶液；然后在水玻璃溶液中继续添加溶液质量3％的乙烯基羟基硅油GP-203:阳离子羟基硅油SM-5017体积比为3:1的硅油混合液，均质乳化而成；
(3)将上述原级硅微粉继续球磨，球磨的过程中在原级硅微粉中加入原级硅微粉质量2％的含519酰胺增电剂质量分数2％的无水乙醇溶液；然后喷淋原级硅微粉质量4％的水玻璃溶液；
(4)球磨的过程中持续通入60℃的热空气，通气速率控制为30L/min*kg原级硅微粉；
(5)持续球磨至中位粒径2.0μm，制得包覆型球形硅微粉。
实施例4
一种包覆型球形硅微粉的制备方法，其第(3)步未添加酰胺增电剂，其余工艺同实施例2。
实施例5
一种包覆型球形硅微粉的制备方法，制备方法具体如下：
(1)选择高纯石英砂，经多级球磨机破碎为中位粒径10.0μm的原级硅微粉；
(2)将模数为2.3的水玻璃溶解于水中，溶解制得1.17g/mL的水玻璃溶液；
(3)将上述原级硅微粉继续球磨，球磨的过程中喷淋原级硅微粉质量3％的水玻璃溶液；
(4)球磨的过程中持续通入60℃的热空气，通气速率控制为45L/min*kg原级硅微粉；
(5)持续球磨至中位粒径2.0μm，制得包覆型球形硅微粉。
对比例1
一种硅微粉的制备方法，其直接球磨至中位粒径2.0μm。
对比例2
用对比例1制得的硅微粉，吸附与实施例2等量的硅油混合液。
对比例3
一种硅微粉的制备方法，其中第(2)步硅油混合液仅含乙烯基羟基硅油GP-203，其余工艺同实施例2。
对比例4
一种硅微粉的制备方法，其中第(2)步硅油混合液仅含阳离子羟基硅油SM-5017，其余工艺同实施例2。
对比例5
一种硅微粉的制备方法，用等量的分散剂ASD201替代第(2)步硅油混合液，其余工艺同实施例2。
检测分析：
1、取上述各实施例和对比例制得的硅微粉，根据休止角法用漏斗测试硅微粉的休止角θ，θ＝arctan(粉体堆积高度/半径)；
2、以HE200环氧树脂作为环氧树脂体系进行测试，加入质量20％的上述实施例与对比例制得的硅微粉，并以相同的搅拌速度搅拌分散1h，然后保存在透明容器中；然后放置于60℃的烘箱中，观察上述制得的环氧树脂体系发生明显沉降所需时间(D)；明显沉降的判断以在冷白荧光灯为背景光源，肉眼观察，当环氧树脂体系有明显不均匀时，判定为已发生沉降。
样品 休止角θ 沉降时间(D)
实施例1 30.3° 31
实施例2 28.9° 35
实施例3 29.0° 37
实施例4 30.1° 26
实施例5 35.7° 13
对比例1 42.2° 6
对比例2 40.3° 20
对比例3 31.8° 15
对比例4 35.5° 17
对比例5 35.1° 23
最后：以上所述仅为本发明的优选实施例而已，并不用于限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (6)

1.一种包覆型球形硅微粉的制备方法，其特征在于：所述制备方法具体如下：
(1)选择高纯石英砂，经多级球磨机破碎为中位粒径10.0～12.0μm的原级硅微粉；
(2)将水玻璃溶解于水中，溶解制得1.15-1.20g/mL的水玻璃溶液；
(3)将上述原级硅微粉继续球磨，球磨的过程中喷淋原级硅微粉质量2％-4％的水玻璃溶液；
(4)球磨的过程中持续通入50℃-60℃的热空气，通气速率控制为30-50L/min*kg原级硅微粉；
(5)持续球磨至中位粒径1.2～3.0μm，制得包覆型球形硅微粉。
2.根据权利要求1所述的包覆型球形硅微粉的制备方法，其特征在于：所述水玻璃的模数为2.2-2.6。
3.根据权利要求1所述的包覆型球形硅微粉的制备方法，其特征在于：第(2)步制得的水玻璃溶液中继续添加溶液质量1％-3％的乙烯基羟基硅油:阳离子羟基硅油体积比为3-5:1的硅油混合液，均质乳化而成。
4.根据权利要求3所述的包覆型球形硅微粉的制备方法，其特征在于：所述乙烯基羟基硅油牌号为GP-203。
5.根据权利要求3所述的包覆型球形硅微粉的制备方法，其特征在于：所述阳离子羟基硅油牌号为SM-5017。
6.根据权利要求1所述的包覆型球形硅微粉的制备方法，其特征在于：第(3)步喷淋水玻璃溶液之前在原级硅微粉中加入原级硅微粉质量1％-2％的含519酰胺增电剂质量分数2％-3％的无水乙醇溶液。
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