CN105906955B - 一种透明环氧化聚异丁烯灌封料 - Google Patents
一种透明环氧化聚异丁烯灌封料 Download PDFInfo
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Abstract
本发明公开了一种透明环氧化聚异丁烯灌封料。该材料由环氧化低分子量聚异丁烯树脂、纳米二氧化硅‑环氧杂化树脂、酸酐固化剂、固化促进剂和添加剂经搅拌混合、超声分散、加热固化制备得到。制得的透明环氧化聚异丁烯灌封料同时具有材料离子杂质含量低、水汽渗透系数小、抗紫外老化能力强、粘合密封性好的优点,有效解决包括现有照明LED在内的光电器件灌封料的不足。
Description
技术领域
本发明属于高分子材料和光电器件封装,具体涉及到一种透明环氧化聚异丁烯灌封料。
背景技术
用于太阳能电池、照明LED灯具等光电器件的透明密封材料,不但要提供光伏芯片、LED芯片、电气连接、荧光粉等的密封保护,还需采集太阳辐射或抽取芯片发射的光子,赋予产品的光电转换或者照明功能。太阳能电池和LED芯片封装是这些光电器件生产中的重要环节。它们的外量子效率及使用寿命与封装设计和封装密封材料密切相关。为取得高的外量子效率和低的光衰速度,所用塑封材料必须:1)透光率高,减少光能损失;2)离子含量低,减缓金属部件的腐蚀,提高电气连接的可靠性;3)抗热氧、紫外老化性好,延长器件的使用寿命;4)水汽渗透系数低,防止电气连接和荧光粉界面的快速衰退。
照明LED塑封材料经历了从双酚-A环氧树脂、脂环族环氧树脂到聚硅氧烷橡胶的变化历程。双酚-A环氧树脂在蓝光LED或紫外辐射照射下,因苯环双键的光化学氧化而变黄,使材料透光率下降。脂环族环氧树脂不含双键,具有优异的抗紫外老化性能;但一般脂环族环氧树脂分子交联点密,材料模量高,热应力大,吸湿性强,加快封装LED的湿热老化。聚硅氧烷塑胶主链键能高,具有优异的抗热氧和紫外老化性能,可在很宽范围内通过组成调节材料的模量,同时提高封装LED的抗紫外和热疲劳的能力;但聚硅氧烷水汽渗透系数大、力学强度低、粘合密封性差,以聚硅氧烷封装的照明LED产品可靠性并不理想。一些国际著名有机硅生产厂家推出多芳基聚硅氧烷新产品,以降低聚硅氧烷塑封材料的水汽渗透系数和包埋荧光粉的表面退化速度。但高芳基聚硅氧烷的抗紫外、抗光衰能力下降。而且,有机硅材料以氯硅烷工艺为基础,可水解氯含量高,一般产品不符合电子封装的要求,提纯除杂成本高。本发明专利针对现有透明灌封材料的问题,公开一种高纯度、低透汽、抗紫外的透明灌封料。
发明内容
本发明的目的在于解决包括现有照明LED在内的光电器件灌封料的不足,提供一种透明环氧化聚异丁烯灌封料。
环氧化低分子量聚异丁烯树脂离子含量低、透明度高,由低分子量聚异丁烯环氧化合成。环氧化低分子量聚异丁烯的主链为饱和碳链,每隔一个次甲基连有两个侧甲基,材料疏水性大、吸水率低,耐紫外老化性能好,水汽渗透系数小,符合优质光电器件灌封材料的基本要求。但环氧化低分子量聚异丁烯分子只有一个末端环氧基团,树脂官能度小于1,不易形成交联网络。环氧化低分子量聚异丁烯树脂与其它环氧树脂的内聚能密度差别大,共混时容易出现相分离,材料透光度下降,雾度增加。
纳米二氧化硅-环氧杂化树脂是以气相白炭黑与环氧硅氧烷为原料合成的接枝共聚物,基本粒子直径低于50纳米,粒子表面环氧基团数目达103量级,为多官能度环氧树脂。将纳米二氧化硅-环氧杂化树脂与环氧化低分子量聚异丁烯树脂共混,能得到官能度大于1的共混环氧树脂。纳米二氧化硅-环氧杂化树脂的粒径小,分散到环氧化低分子量聚异丁烯树脂能形成透明的环氧树脂共混物。纳米二氧化硅-环氧杂化树脂的摩尔质量大,在环氧化低分子量聚异丁烯树脂中运动的阻力大,分子动能和重力场不足以克服运动阻力,实现动力学上的有效变化,树脂共混体系的宏观稳定性好,储存期长。纳米二氧化硅-环氧杂化树脂的环氧官能团与环氧化低分子量聚异丁烯树脂的环氧官能团结构相似,反应活性相近,能与酸酐固化剂同步反应,形成分子水平的共混杂化材料,提供优质的光电器件灌封料。
一种透明环氧化聚异丁烯灌封料,由环氧化低分子量聚异丁烯树脂、纳米二氧化硅-环氧杂化树脂、酸酐固化剂、固化促进剂和添加剂经搅拌混合、超声分散、在120~150oC分段加热固化制备得到。制得的透明环氧化聚异丁烯灌封料为高透明、低透汽、抗紫外的光电器件密封材料。
进一步地,所述环氧化低分子量聚异丁烯树脂的环氧值为0.07-0.25 mol/100g;所述环氧化低分子量聚异丁烯树脂的平均分子量低于1000 g/mol。
进一步地,所述纳米二氧化硅-环氧杂化树脂中的环氧基团为3,4-环氧环己基或缩水甘油醚,优选3,4-环氧环己基。
进一步地,所述纳米二氧化硅-环氧杂化树脂的环氧值为0.010-0.025 mol/100g,优选0.012-0.025mol/100g。
进一步地,所述纳米二氧化硅-环氧杂化树脂的用量为环氧化低分子量聚异丁烯树脂质量的3-25%,满足封装器件对灌封料不同硬度的要求。
进一步地,所述酸酐固化剂为甲基六氢邻苯二甲酸酐和十二烷基琥珀酸酐中的一种以上。酸酐是环氧树脂的常用固化剂,甲基六氢邻苯二甲酸酐饱和度高,以甲基六氢邻苯二甲酸酐固化的环氧树脂透明度好,抗紫外老化能强。十二烷基琥珀酸酐的饱和度也高,而且与环氧化低分子量聚异丁烯的相容性好,也用作共混树脂的固化剂。环氧基团与酸加成产生的羟基可参与环氧基团的开环加成反应,为减少固化材料中残存的酸基或环氧基,优化固化材料的光学性能和抗老化性能。所述酸酐固化剂的用量为体系中环氧化低分子量聚异丁烯树脂和纳米二氧化硅-环氧杂化树脂的环氧基团总摩尔量的0.8倍。
进一步地,所述固化促进剂包括三苯基膦和磷晴化合物中的一种以上。固化促进剂可提高环氧树脂与酸酐的反应速度,降低固化温度。三苯基膦和磷睛化合物固化促进剂效率高,固化物光学性能好,且固化促进剂并用可减少溶解混合的时间。
进一步地,所述固化促进剂总用量低于环氧化低分子量聚异丁烯树脂质量的2.0%,优选0.5-1.0%。
进一步地,所述添加剂包含稳定剂、抗静电剂和荧光粉中的一种以上,所述稳定剂为抗氧化剂和光稳定剂,以实现满足不同封装结构的要求。
更进一步地,所述抗氧剂的用量低于环氧化低分子量聚异丁烯树脂质量的1.0%。常用抗氧剂有抗氧剂1010、抗氧剂168、抗氧剂412S、抗氧剂445、抗氧剂1098、抗氧剂1790、抗氧剂DLTDP、抗氧剂DSTP。抗氧剂主要防止灌封料在加工过程中的热氧老化。
更进一步地,所述光稳定剂的添加量低于环氧化低分子量聚异丁烯树脂质量的1.0%。环氧化低分子量聚异丁烯树脂抗紫外老化性能好,添加紫外光吸收光稳定剂可进一步增加灌封料抵抗紫外辐射的能力,纳米二氧化硅-环氧杂化树脂本身是一种紫外吸收光稳定剂。
更进一步地,所述荧光粉的用量为环氧化低分子量聚异丁烯树脂质量的8-25%。荧光粉是实现白光LED的添加剂,在采用远程荧光粉或玻璃预封荧光粉的封装结构时,灌封料中省出荧光粉。
进一步地,所述加热固化为120 到150 oC分段固化,且在120 oC固化时间不少于90min,在150 oC固化60min以下。
与现有灌封料比较,本发明具有如下的优点与技术效果:
本发明与现有光电器件灌封料相比,同时具有材料离子杂质含量低、水汽渗透系数小、抗紫外老化能力强、粘合密封性好的优点。
具体实施方式
以下结合实施例对本发明作进一步说明,但本发明不仅限于如下实施例。
实施例:
表1 透明灌封料化学组成(质量份)
按表1所列质量份数值将Hybrid-186与EPIB450搅拌混合,超声分散,得到混合树脂;将抗氧剂1010和光稳定剂UV531加入混合树脂中;将三苯基膦溶入MHHPA,再加入混合树脂中,搅拌均匀,得无色透明灌封料。用1mm刮涂棒将灌封料涂于洁净的载玻片,于烘箱中加热固化。固化工艺为120℃加热4h,再130℃加热2 h,最后150℃加热45 min,随炉冷却,得到样品。
用紫外-可见分光光度计测定样品的透射光谱,取550纳米的值为样品的透光率。以动态粘弹谱仪测量样品的动态力学性能。按GB/T1034-2008B将样品浸入水中,测量样品的吸水率。将样品在0.83W/m2的334nm 氙灯紫外老化箱中于50℃照射老化168小时,用紫外-可见分光光度计测定样品的透射光谱,求样品的透光率和黄变指数。测得实施例1~4得到的样品的性能如表2所示。
表2 实施例1~4得到的透明环氧化低分子聚异丁烯灌封料的性能
从表2可以看出,各样品具有高的透光率,随纳米二氧化硅-环氧杂化树脂含量增加,透光率有所下降,实施例1所得样品的透光率达99.8%;实施例3纳米二氧化硅-环氧杂化树脂含量为8phr,但样品透光率仍为90%。
随纳米二氧化硅-环氧杂化树脂用量增多,玻璃化温度上升,弹性模量增加。
随着纳米二氧化硅-环氧杂化树脂用量增加,样品吸水率增加,实施例1样品的平衡吸水率仅有0.1%;实施例3纳米二氧化硅-环氧杂化树脂用量为8phr,但样品平衡吸水率仍低至0.25%。
实施例得到的样品有优良的抗紫外老化性能,经紫外辐射照射168h,样品透光率略有下降。实施例1样品的透光率仍高达97.5%,实施例3样品的透光率接近90%;实施例1样品的黄变因子为0.80%,随纳米二氧化硅-环氧杂化树脂含量增加,实施例样品的黄变因子减小,实施例3样品的黄变因子为0.60%,优于大多数环氧灌封胶。
表3透明灌封料化学组成(质量份)
按表3所列质量份数值,在40oC将EPIB1000与Hybrid-186h或 EPIB1000与Hybrid1872搅拌混合,超声分散,得到混合树脂;将抗氧剂1010和光稳定剂UV531加入混合树脂中;将三苯基膦溶入MHHPA,再加入混合树脂中,搅拌均匀,真空脱泡,得无色透明灌封料。用1mm刮涂棒将灌封料涂于洁净的载玻片,于烘箱中加热固化。固化工艺为120℃加热2h,再135℃加热3h,最后150℃加热1h,随炉冷却,得到样品。
用紫外-可见分光光度计测定样品的透射光谱,取550纳米的值为样品的透光率。以动态粘弹谱仪测量样品的动态力学性能。按GB/T1034-2008B将样品浸入水中,测量样品的吸水率。将样品在0.83W/m2的334nm 氙灯紫外老化箱中于50℃照射老化168小时,用紫外-可见分光光度计测定样品的透射光谱,求样品的透光率和黄变指数。测得实施例5~8得到的样品的性能如表4所示。
表4 实施例5~8得到的透明环氧化低分子聚异丁烯灌封料的性能
从表4可以看出,各实施例样品的吸水率随纳米二氧化硅-环氧杂化树脂用量增加而上升,但在Hybrid186用量为25质量份时,固化样品的吸水率才1.5%,远低于一般环氧灌封料的吸水率。随纳米二氧化硅-环氧杂化树脂用量增多,玻璃化温度上升,弹性模量增加。实施例5和实施例6的透光率分别为92% 和88%,而黄变因子分别为0.53 %和0.25%。实施例7和实施例8的透光率分别为95% 和90%,而黄变因子分别为0.63 %和0.40%。透明环氧化聚异丁烯灌封料有优异的抗紫外老化性能。
比较表2和表4可见,环氧化低分子聚异丁烯分子量增加,固化灌封料玻璃化温度下降,有效交联网络增加,弹性模量增加。
Claims (8)
1.一种透明环氧化聚异丁烯灌封料,其特征在于由环氧化低分子量聚异丁烯树脂、纳米二氧化硅-环氧杂化树脂、酸酐固化剂、固化促进剂和添加剂经搅拌混合、超声分散、加热固化制备得到;
所述环氧化低分子量聚异丁烯树脂的环氧值为0.07-0.25 mol/100g;所述环氧化低分子量聚异丁烯树脂的平均分子量低于1000 g/mol;
所述纳米二氧化硅-环氧杂化树脂的环氧值为0.01-0.025 mol/100g;所述纳米二氧化硅-环氧杂化树脂的用量为环氧化低分子量聚异丁烯树脂质量的3-25%;
所述酸酐固化剂的用量为环氧化低分子量聚异丁烯树脂和纳米二氧化硅-环氧杂化树脂的环氧基团总摩尔量的0.8倍;所述固化促进剂的用量低于环氧化低分子量聚异丁烯树脂质量的2.0%。
2.根据权利要求1所述的一种透明环氧化聚异丁烯灌封料,其特征在于所述纳米二氧化硅-环氧杂化树脂为气相白炭黑与环氧硅氧烷的接枝共聚物;所述纳米二氧化硅-环氧杂化树脂中的环氧基团为3,4-环氧环己基或缩水甘油醚。
3.根据权利要求1所述的一种透明环氧化聚异丁烯灌封料,其特征在于所述酸酐固化剂为甲基六氢邻苯二甲酸酐和十二烷基琥珀酸酐中的一种以上。
4.根据权利要求1所述的一种透明环氧化聚异丁烯灌封料,其特征在于所述固化促进剂包括三苯基膦和磷腈化合物中的一种以上。
5.根据权利要求1所述的一种透明环氧化聚异丁烯灌封料,其特征在于所述添加剂包含稳定剂和荧光粉中的一种以上。
6.根据权利要求5所述的一种透明环氧化聚异丁烯灌封料,其特征在于所述稳定剂为抗氧剂和光稳定剂,所述抗氧剂的用量低于环氧化低分子量聚异丁烯树脂质量的1.0%;所述光稳定剂为紫外光吸收剂,所述光稳定剂的用量低于环氧化低分子量聚异丁烯树脂质量1.0%。
7.根据权利要求5所述的一种透明环氧化聚异丁烯灌封料,其特征在于所述荧光粉的用量为环氧化低分子量聚异丁烯树脂质量的8-25%;所述荧光粉是实现白光LED的添加剂,在采用远程荧光粉或玻璃预封荧光粉的封装结构时,灌封料中省出荧光粉。
8.根据权利要求1所述的一种透明环氧化聚异丁烯灌封料,其特征在于所述加热固化为120~150 oC分段固化,且在120℃ 固化时间不少于90min,在150 oC固化60min以下。
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