CN107227142A - 一种led封装用有机硅灌封胶的制备方法 - Google Patents
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Abstract
本发明公开了一种LED封装用有机硅灌封胶的制备方法,属于电子灌封材料制备技术领域。本发明将硅微粉、球形氧化铝等混合加热制得基料,并将羟基硅油、四甲基四乙烯基环四硅氧烷等混合加热制得增粘剂后,将基料与增粘剂、铂催化剂等混磨制得A组份,随后以基料、乙烯基硅油、含氢硅油、甲基丁炔醇为原料,混磨分散得B组份,将A、B组份按等质量比混匀排泡后灌在粘接基材上固化,即可得LED封装用有机硅灌封胶,本发明所得有机硅灌封胶兼具良好的流动性和粘接性能,同时灌封胶导热性能优良,在LED封装领域具有广阔的应用前景。
Description
技术领域
本发明公开了一种LED封装用有机硅灌封胶的制备方法,属于电子灌封材料制备技术领域。
背景技术
随着LED照明技术的发展,功率型LED制造技术在不断提升和完善,其发光效率、亮度和功率都有了大幅提高。在制造功率型LED器件的过程中,除了芯片、荧光粉和散热技术外,LED封装材料对LED器件的性能存在着重要的影响。
随着LED封装材料的性能要求的不断提高,LED封装材料已逐步从环氧树脂、有机硅改性环氧树脂,发展到现在的有机硅灌封胶。有机硅灌封胶具有耐冷热冲击、耐紫外线辐射、无色透明等优点,是功率型LED的理想封装材料。从交联机理角度可把有机硅封装材料分为缩合型和加成型两种。缩合型有机硅灌封胶是通过分子间发生缩合反应而实现交联反应,固化过程中常有水、甲醇、乙醇等小分子化合物放出,容易产生气泡和孔隙,往往达不到高标准的封装性能要求。加成型有机硅灌封胶目前主要通过硅氢加成反应实现,以铂化合物为催化剂,在固化过程中无小分子产生,收缩率小,工艺适应性好,生产效率高。因此,在LED封装材料市场上,硅氢加成型有机硅灌封胶发展较快,已逐步取代缩合型有机硅灌封胶。
由于灌封胶要在固化后才能发挥它的使用价值,因而要求固化前的液体状灌封胶具有粘度小、流动性好的特点,以便于使用过程中方便排泡,同时要求其具有良好的防水性,使LED电子器件在潮湿、雨水、灰尘或辐射等环境条件下正常运行,此外,作为灌封胶,还必须保证其与灌封元器件或灌封腔体具有很好的粘接性,以更好的发挥防水防潮、防尘、绝缘、保密、防腐蚀和防震等作用。
专利号CN104513644A公开了一种透明灌封胶及其用途,透明灌封胶由A剂和B剂组成,A剂包括端乙烯基聚硅氧烷、支链型乙烯基聚硅氧烷和铂金催化剂;B剂包括:35~40wt%的端乙烯基聚硅氧烷、40~50wt%的支链型乙烯基聚硅氧烷、15~20wt%的含氢聚硅氧烷,以及0~0.5wt%的抑制剂。其使用方法为将透明灌封胶的A剂和B剂按质量比1:1混合搅拌均匀,在真空下排完泡后使用。虽然这种透明灌装胶具有较低的粘度、良好的透明度及较好的柔韧性,但是其粘接性能没有得到改善和提升,不能满足实际使用需求。
专利号CN102675882A公开了一种加成型导热防沉降硅橡胶及其制备方法,采用的硅橡胶原料包括A组份和B组份,其中A组份含有基料、含氢硅油、抑制剂、稀释剂和防沉降剂;B组份含有基料、铂催化剂、稀释剂和防沉降剂,其中基料为乙烯基硅油与导热填料。取A组份原料,搅拌获得A组份,取B组份原料,搅拌获得B组份,再取A组份和B组份共混均匀,脱泡,得到加成型导热防沉降硅橡胶。虽然制得的硅橡胶具有较高的导热系数,可广泛用于电子电器领域中需要散热和传热的部件,但是其粘接性能仍不理想。因此,亟待开发一种兼具固化前有良好的流动性和固化后具有优良粘接性的灌封胶产品。
发明内容
本发明主要解决的技术问题,针对现有的有机硅灌封胶不能兼具固化前良好流动性和固化后优良粘接性的缺陷,提供了一种LED封装用有机硅灌封胶的制备方法。
为了解决上述技术问题,本发明所采用的技术方案是:
(1)取乙烯基硅油、硅微粉、球形氧化铝和硅烷偶联剂A-171装入捏合机内,加热至120~160℃混合1~2h,再加热至160~180℃处理1~2h,出料得基料;(2)取羟基硅油、硅烷偶联剂KH-560、四甲基四乙烯基环四硅氧烷装入反应釜中混合均匀后再加入二月桂酸二丁基锡,加热至60~65℃搅拌并抽真空至100~1000Pa,反应1~8h后出料,得增粘剂;
(3)取基料、乙烯基硅油、增粘剂、铂催化剂装入捏合机中混合均匀,再用三辊研磨机研磨分散20~30min,得A组份;
(4)取基料、乙烯基硅油、含氢硅油、甲基丁炔醇,装入捏合机中混合均匀,再用三辊研磨机研磨分散20~30min,得B组份;
(5)将A、B组份按质量比1:1混合均匀后,在真空下减压排泡,然后在室温下灌在粘接基材上,室温下固化1~2h后再加热至60~80℃固化1~2h,得LED封装用有机硅灌封胶。
步骤(1)中各原料的重量份为100~120份乙烯基硅油,350~420份硅微粉,10~50份球形氧化铝,5~6份硅烷偶联剂A-171。
步骤(2)中各原料的重量份为360~400份羟基硅油,200~240份硅烷偶联剂KH-560,70~80份四甲基四乙烯基环四硅氧烷,0.15~0.20份二月桂酸二丁基锡。
步骤(3)中各原料的重量份为200~250份基料,50~60份乙烯基硅油,20~30份增粘剂,0.1~0.3份铂催化剂。
步骤(4)中各原料的重量份为200~250份基料,20~30份乙烯基硅油,20~30份含氢硅油,0.01~0.03份甲基丁炔醇。
本发明的有益效果是:
(1)本发明采用球形氧化铝作为导热补强填料,因表面的活性基团较少,与聚硅氧烷分子链之间存在物理吸附和化学键合作用小,灌封胶流动时受到的阻力较小,形成具有良好流动性的有机硅灌封胶;
(2)本发明通过硅烷偶联剂A-171改性硅微粉,在粉体表面形成含乙烯基的单分子层,该单分子层与基胶乙烯基硅油相容性好,且降低了粉体表面极性,减弱了与增粘剂分子间作用力,大大降低了增粘剂迁移阻力,使增粘剂更容易迁移到基材表面,形成良好粘接效果,同时增粘剂分子结构外围还含有大量烷氧基等极性基团,可显著改善加成型硅胶体系低表面能,从而提高其粘接效果。
具体实施方式
取100~120g乙烯基硅油,350~420g硅微粉,10~50g球形氧化铝和5~6g硅烷偶联剂A-171装入捏合机内,加热至120~160℃混合1~2h,再加热至160~180℃处理1~2h,冷却至室温后出料,得基料,取360~400g羟基硅油,200~240g硅烷偶联剂KH-560,70~80g四甲基四乙烯基环四硅氧烷装入反应釜中,加热至50~55℃,并以200~300r/min搅拌20~30min,再加入0.15~0.20g二月桂酸二丁基锡,继续搅拌加热至60~65℃,保温反应3~4h后抽真空至100~1000Pa,持续30~40min,再保温反应1~2h,冷却至室温后出料,得增粘剂,按重量份数计,取200~250份基料,50~60份乙烯基硅油,20~30份增粘剂,0.1~0.3份铂催化剂装入捏合机中混合均匀,再用三辊研磨机研磨分散20~30min,得A组份,再按重量份数计,取200~250份基料,20~30份乙烯基硅油,20~30份含氢硅油,0.01~0.03份甲基丁炔醇,装入捏合机中混合均匀,再用三辊研磨机研磨分散20~30min,得B组份,将A、B组份按质量比1:1混合均匀后,在真空下减压排泡,然后在室温下灌在粘接基材上,室温下固化1~2h后再加热至60~80℃固化1~2h,得LED封装用有机硅灌封胶。
实例1
取100g乙烯基硅油,350g硅微粉,10g球形氧化铝和5g硅烷偶联剂A-171装入捏合机内,加热至120℃混合1h,再加热至160℃处理1h,冷却至室温后出料,得基料,取360g羟基硅油,200g硅烷偶联剂KH-560,70g四甲基四乙烯基环四硅氧烷装入反应釜中,加热至50℃,并以200r/min搅拌20min,再加入0.15g二月桂酸二丁基锡,继续搅拌加热至60℃,保温反应3h后抽真空至100Pa,持续30min,再保温反应1h,冷却至室温后出料,得增粘剂,按重量份数计,取200份基料,50份乙烯基硅油,20份增粘剂,0.1份铂催化剂装入捏合机中混合均匀,再用三辊研磨机研磨分散20min,得A组份,再按重量份数计,取200份基料,20份乙烯基硅油,20份含氢硅油,0.01份甲基丁炔醇,装入捏合机中混合均匀,再用三辊研磨机研磨分散20min,得B组份,将A、B组份按质量比1:1混合均匀后,在真空下减压排泡,然后在室温下灌在粘接基材上,室温下固化1h后再加热至60℃固化1h,得LED封装用有机硅灌封胶。
实例2
取110g乙烯基硅油,385g硅微粉,30g球形氧化铝和5g硅烷偶联剂A-171装入捏合机内,加热至140℃混合1h,再加热至170℃处理1h,冷却至室温后出料,得基料,取380g羟基硅油,220g硅烷偶联剂KH-560,75g四甲基四乙烯基环四硅氧烷装入反应釜中,加热至53℃,并以250r/min搅拌25min,再加入0.18g二月桂酸二丁基锡,继续搅拌加热至63℃,保温反应3h后抽真空至550Pa,持续35min,再保温反应1h,冷却至室温后出料,得增粘剂,按重量份数计,取225份基料,55份乙烯基硅油,25份增粘剂,0.2份铂催化剂装入捏合机中混合均匀,再用三辊研磨机研磨分散25min,得A组份,再按重量份数计,取225份基料,25份乙烯基硅油,25份含氢硅油,0.02份甲基丁炔醇,装入捏合机中混合均匀,再用三辊研磨机研磨分散25min,得B组份,将A、B组份按质量比1:1混合均匀后,在真空下减压排泡,然后在室温下灌在粘接基材上,室温下固化1h后再加热至70℃固化1h,得LED封装用有机硅灌封胶。
实例3
取120g乙烯基硅油,420g硅微粉,50g球形氧化铝和6g硅烷偶联剂A-171装入捏合机内,加热至160℃混合2h,再加热至180℃处理2h,冷却至室温后出料,得基料,取400g羟基硅油,240g硅烷偶联剂KH-560,80g四甲基四乙烯基环四硅氧烷装入反应釜中,加热至55℃,并以300r/min搅拌30min,再加入0.20g二月桂酸二丁基锡,继续搅拌加热至65℃,保温反应4h后抽真空至1000Pa,持续40min,再保温反应2h,冷却至室温后出料,得增粘剂,按重量份数计,取250份基料,60份乙烯基硅油,30份增粘剂,0.3份铂催化剂装入捏合机中混合均匀,再用三辊研磨机研磨分散30min,得A组份,再按重量份数计,取250份基料,30份乙烯基硅油,30份含氢硅油,0.03份甲基丁炔醇,装入捏合机中混合均匀,再用三辊研磨机研磨分散30min,得B组份,将A、B组份按质量比1:1混合均匀后,在真空下减压排泡,然后在室温下灌在粘接基材上,室温下固化2h后再加热至80℃固化2h,得LED封装用有机硅灌封胶。
对比例:北京某生产的双组份橡胶型LED封装用有机硅灌封胶。
表1各LED封装用有机硅灌封胶的性能对比表
从上表可以看出,本发明制得的LED封装用有机硅灌封胶兼具良好的流动性、粘接性及导热性能,其流动性和粘结性均优于市售LED封装用有机硅灌封胶产品,在LED封装领域具有广阔的应用前景。
Claims (5)
1.一种LED封装用有机硅灌封胶的制备方法,其特征在于,具体制备步骤为:
(1)取乙烯基硅油、硅微粉、球形氧化铝和硅烷偶联剂A-171装入捏合机内,加热至120~160℃混合1~2h,再加热至160~180℃处理1~2h,出料得基料;
(2)取羟基硅油、硅烷偶联剂KH-560、四甲基四乙烯基环四硅氧烷装入反应釜中混合均匀后再加入二月桂酸二丁基锡,加热至60~65℃搅拌并抽真空至100~1000Pa,反应1~8h后出料,得增粘剂;
(3)取基料、乙烯基硅油、增粘剂、铂催化剂装入捏合机中混合均匀,再用三辊研磨机研磨分散20~30min,得A组份;
(4)取基料、乙烯基硅油、含氢硅油、甲基丁炔醇,装入捏合机中混合均匀,再用三辊研磨机研磨分散20~30min,得B组份;
(5)将A、B组份按质量比1:1混合均匀后,在真空下减压排泡,然后在室温下灌在粘接基材上,室温下固化1~2h后再加热至60~80℃固化1~2h,得LED封装用有机硅灌封胶。
2.如权利要求1所述的一种LED封装用有机硅灌封胶的制备方法,其特征在于,步骤(1)中各原料的重量份为100~120份乙烯基硅油,350~420份硅微粉,10~50份球形氧化铝,5~6份硅烷偶联剂A-171。
3.如权利要求1所述的一种LED封装用有机硅灌封胶的制备方法,其特征在于,步骤(2)中各原料的重量份为360~400份羟基硅油,200~240份硅烷偶联剂KH-560,70~80份四甲基四乙烯基环四硅氧烷,0.15~0.20份二月桂酸二丁基锡。
4.如权利要求1所述的一种LED封装用有机硅灌封胶的制备方法,其特征在于,步骤(3)中各原料的重量份为200~250份基料,50~60份乙烯基硅油,20~30份增粘剂,0.1~0.3份铂催化剂。
5.如权利要求1所述的一种LED封装用有机硅灌封胶的制备方法,其特征在于,步骤(4)中各原料的重量份为200~250份基料,20~30份乙烯基硅油,20~30份含氢硅油,0.01~0.03份甲基丁炔醇。
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