CN112375524A - 一种环氧胶及其制备方法和应用 - Google Patents
一种环氧胶及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及一种环氧胶制备方法和应用,由下列重量百分比的原料组成:环氧树脂60‑100份,增韧剂25‑45份,消泡剂0.5‑1.5份,固化剂20‑45份,触变剂1.5‑5.0份,抗氧化剂0.3‑1.5份,紫外吸收剂0.3‑1.5份。包括以下步骤:(1)将以上各种原料按配方工艺混合搅拌后,制得环氧胶液;(2)将胶液在涂覆机上按涂膜厚度:200‑300μm,线速5m/min,烘箱温度区间为:100℃/110℃/120℃/110℃/100℃,烘箱段长为12.5m等条件进行涂覆;(3)将涂覆后的胶膜经裁切后、密封并在‑5℃下储存。所制得的胶膜可应用于mini LED封装。
Description
技术领域
本发明涉及半导体封装材料,具体涉及一种环氧胶及其制备方法和应用。
背景技术
LED(Light Emitting Diode)是发光二极管的简称,它可以高效地将电能转化成光能,目前LED具有广泛的用途:如照明、显示及医疗器件。为了满足人们对LED产品更好的体验需要,LED封装技术不断发展,由传统的直插式,SMT逐渐往mini LED和micro LED封装转变的趋势,因为micro LED技术还不够成熟加上制造成本较高,近期mini LED发展势头迅猛,各大封装厂积极布局mini LED封装。有机硅胶因其有较好的耐热性常被应用于LED封装,但有机硅胶自身的结构缺陷限制了它的应用范围,比如粘结力不强,防水、防潮性能较弱。面对新型的封装方式(mini LED封装),有机硅胶无法解决它自身透汽透氧性差的缺陷,且在mini LED封装中,一块板中就含有成百上千颗芯片,对外封胶的防水防潮性能有较高的需求,环氧树脂因其含有环氧基、羟基等极性基团能与基板有良好的粘接力,胶固化后交联密度高有着优异的防水防潮性能,能更好地满足mini LED封装对于气密性方面的要求。
中国专利(CN104804694A)公开了一种新型环氧树脂LED封装胶及其制备方法,其由重量比为1:1的A胶和B胶组成,所述A胶的重量份组成包括:环氧树脂95-99份,消泡剂1-2份,增韧剂0-3份;所述B胶的重量份组成包括:固化剂92-96份,促进剂0.5-2份,脱模剂0.1-0.5份,纳米高岭土2-5份,抗氧剂0.5-2份。所述封装胶由A、B胶组成,无法直接使用。
中国专利(CN103289317A)公开了一种LED封装材料及其制备方法和应用,该材料由以下按重量份数计的组分组成:环氧树脂100份,交联剂60份,交联促进剂2份,抗氧剂0.1-5份,紫外光稳定剂0.05-0.25份,紫外光吸收剂0.05-0.50份。本发明采用含硫的苯并三唑类化合物紫外光吸收剂,性能优良,与抗氧剂、紫外光稳定剂有良好的协同作用,可用作LED封装材料的紫外光吸收剂。其中紫外光吸收剂需要自行合成,不易获得,同时该封装材料封装LED组件时需要配套的模具,封装使用的设备要求复杂。
发明内容
针对有机硅胶粘结力不强,防水、防潮性能不佳等缺陷,本发明的一个目的是提供一种以环氧树脂为基础的胶黏剂,即一种环氧胶。
本发明的另一目的是提供一种制备本发明所述环氧胶的制备方法。.
本发明的再一个目的是提供一种本发明所述环氧胶的应用。
提供一种优异粘结力,防水、防潮性能佳,耐热性优良的环氧胶膜,适用于miniLED封装工艺。
本发明的目的是由以下技术方案实现的。
本发明提供一种环氧胶,按重量份数计,由以下成分制成:
环氧树脂60-100份,
增韧剂25-45份,
消泡剂0.5-1.5份,
固化剂20-45份,
触变剂1.5-5.0份,
抗氧化剂0.3-1.5份,
紫外吸收剂0.3-1.5份。
进一步地,所述环氧树脂选自双酚A环氧树脂、双酚F环氧树脂、氢化双酚A环氧树脂和有机硅改性环氧树脂中的至少一种。
进一步地,所述环氧树脂选自双酚A环氧树脂和氢化双酚A环氧树脂中的至少一种。
进一步地,所述增韧剂选自丁苯核壳橡胶、聚己内酯多元醇和有机硅改性环氧树脂中的至少一种。
进一步地,所述增韧剂选自ALBIFLEX 348、KANEKA的MX125、ALBIFLEX 296和Daicel205U中的至少一种。
进一步地,所述消泡剂选自有机硅聚合物消泡剂。
进一步地,所述消泡剂选自BYK-310、BYK-348、BYK-A530、BYK-054、BYK-1794、R-6501、Airex922、Airex944、Airex900中的至少一种。
进一步地,所述消泡剂选自Airex900、Airex922和BYK-A530中的至少一种。
进一步地,所述固化剂选自改性咪唑类和有机酰肼类中的至少一种。
进一步地,所述固化剂选自FXR-1081、VDH-J和UDH-J中的至少一种。
进一步地,所述触变剂选自疏水性气相二氧化硅。
进一步地,所述触变剂选自TH-20、HL-300、TS-720、HB-139、HB-615、T-40、H13L、R-974和TS-530中的至少一种。
进一步地,所述触变剂选自TS-720、R-974和HB-139中的至少一种。
进一步地,所述抗氧化剂选自磷系抗氧化剂、受阻酚类抗氧化剂中的至少一种。
进一步地,所述抗氧化剂选自Chemnox-1135、Chemnox-1520、Chemnox-6、Chinox245、Chinox35、Chinox TP-10H和CN 510中至少一种。
进一步地,所述抗氧化剂选自Chinox TP-10H、Chinox245和Chemnox-1520中的至少一种。
进一步地,所述紫外吸收剂选自Chisorb Suv、Chemsorb-329、Chemsorb-234、Chemsorb-360、Chisorb Epl、Chemsorb BP4、Chemsorb BP6和Chemfos-TPP中至少一种。
进一步地,所述紫外吸收剂选自Chemfos-TPP、Chisorb Epl和Chemsorb BP4中的至少一种。
进一步地,所述环氧胶胶触变指数为3.0-4.5,黏度值为8000-10000mpa.s.。
本发明提供一种环氧胶的制备方法,包括以下步骤:
(1)树脂与增韧剂、消泡剂的混合:将环氧树脂、增韧剂和消泡剂混合,在75-85℃、真空条件下,转速450-550rpm搅拌10-20分钟,使其混合均匀,冷却至室温,得液体A。
(2)固化剂的添加:在80-120rpm情况下,将固化剂加到步骤(1)的液体A中,将转速调到300-500rpm真空条件搅拌10-15分钟,使混合液搅拌均匀,得液体B。
(3)触变剂和抗氧化剂、紫外吸收剂的添加:在80-120rpm的情况,向步骤(2)的液体B中,加入触变剂、抗氧化剂和紫外线吸收剂,加完后真空条件下将转速调整到500-700rpm,搅拌1-2小时,即得环氧胶。
本发明的提供一种所述环氧胶的应用,所述应用为所述环氧胶在miniLED封装胶膜中的应用。
一种使用本发明所述环氧胶制备的miniLED封装胶膜。
进一步地,所述封装胶膜通过以下步骤制备得到,
(1)涂覆:以一面经过离型处理的雾化PET膜为底,使用所述环氧胶对所述PET膜进行涂覆。
(2)包装及储存:将涂覆后的环氧胶膜进行裁切并密封分隔包装,将成品置于-5℃下冷藏储存。
进一步地,所述涂覆条件为:涂膜厚度:200-300μm,线速5m/min,烘箱温度区间为:100℃/110℃/120℃/110℃/100℃,烘箱段长为12.5m.
本发明的优势在于:
1、本发明提供的制备方法在经过认真的研究和大量的实验基础上,制备出具有较好耐热性,较高透明度,便于mini LED封装工艺操作的环氧胶膜。
2、本发明提供的制备方法采用优选的潜伏性固化剂,能使环氧胶膜具有较长的储存期,胶经过涂覆工艺成膜,这一过程可进行连续性生产,保证胶厚度及品质一致性。
具体实施方式
实施例1
将100份氢化双酚A环氧树脂(ADEKA的EP4080E)、25份的有机硅与环氧共聚树脂(赢创德固赛的ALBIFLEX 348)和0.5份消泡剂(Airex900)添加到反应釜内,在80℃、真空条件下,转速500rpm搅拌30分钟,使其混合均匀;之后将混合液冷至室温;
调搅拌速率为100rpm,将30份有机酰肼固化剂(日本味之素的VDH-J)加到反应釜中,之后将转速调到300rpm真空条件搅拌15分钟,使混合液搅拌均匀;
将转速降低到100rmp开始添加触变剂、抗氧化剂和紫外线吸收剂,取1.5份触变剂(卡博特的TS-720)、0.8份抗氧化剂(双键化工的Chinox TP-10H)和1.0份紫外线吸收剂(恒桥股份的Chemfos-TPP)到反应釜中,加完后抽真空条件下将转速调整到500rpm,搅拌1.5小时,完成环氧胶液的制备。
测试环氧胶胶触变指数为3.05,黏度值为8100mpa.s.
触变指数在3.0-4.5范围内,黏度值在8000-10000mpa.s.范围值内,适合用作miniLED封装胶膜制备工作。
将环氧胶液在涂覆线上进行涂覆操作,将涂胶线速设置为:5m/min,烘箱加热段温度分别设置为:100℃/110℃/120℃/110℃/100℃,用一面带离型的PET薄膜为承载膜,在离型面上进行涂胶的操作,涂胶厚度为200μm,涂完胶经过烘箱段烘烤后,胶呈半固化状态,经冲压机冲压后,将胶膜按指定的尺寸进行裁切,然后进行密封分隔包装,放置于-5℃下低温储存,即得miniLED封装胶膜。
实施例2
将60份氢化双酚A环氧树脂(ADEKA的EP4080E)、45份的丁苯核壳橡胶(KANEKA的MX125)和1.5份消泡剂(A530)添加到反应釜内,在80℃、真空条件下,转速500rpm搅拌30分钟,使其混合均匀;之后将混合液冷至室温;
调低搅拌速率为50rpm,将22份含活泼氢的潜伏型固化剂(日本富士化成的FXR-1081)加到反应釜中,之后将转速调到500rpm真空条件搅拌10分钟,使混合液搅拌均匀;
将转速降低到50rmp以下后,开始添加触变剂、抗氧化剂和紫外线吸收剂,取5.0份触变剂(吉必胜科技的HB-139)、1.1份抗氧化剂(双键化工的Chinox TP-10H)和0.3份紫外线吸收剂(恒桥股份的Chemsorb BP4)到反应釜中,加完后抽真空条件下将转速调整到700rpm,搅拌1.5小时,完成环氧胶液的制备。
测试环氧胶胶触变指数为4.1,黏度值为8800mpa.s.
触变指数在3.0-4.5范围内,黏度值在8000-10000mpa.s.范围值内,适合用作miniLED封装胶膜制备工作。
将环氧胶液在涂覆线上进行涂覆操作,将涂胶线速设置为:5m/min,烘箱加热段温度分别设置为:100℃/110℃/120℃/110℃/100℃,用一面带离型的PET薄膜为承载膜,在离型面上进行涂胶的操作,涂胶厚度为200μm,涂完胶经过烘箱段烘烤后,胶呈半固化状态,经冲压机冲压后,将胶膜按指定的尺寸进行裁切,然后进行密封分隔包装,放置于-5℃下低温储存,即得miniLED封装胶膜。
实施例3
将100份无卤双酚A环氧树脂(南亚的NPEL-127E)、28份的有机硅与环氧共聚树脂(赢创德固赛的ALBIFLEX 296)和0.9份消泡剂(Airex900)添加到反应釜内,在80℃、真空条件下,转速500rpm搅拌30分钟,使其混合均匀;之后使混合液冷至室温;
调低搅拌速率为80rpm,将45份有机酰肼固化剂(日本味之素的UDH-J)加到反应釜中,之后将转速调到400rpm真空条件搅拌15分钟,使混合液搅拌均匀;
将转速降低到80rmp以下后,开始添加触变剂、抗氧化剂和紫外线吸收剂,取2.0份触变剂(卡博特的TS-720)、1.5份抗氧化剂(恒桥股份的Chemnox-1520)和0.6份紫外线吸收剂(恒桥股份的Chisorb Epl)到反应釜中,加完后抽真空条件下将转速调整到700rpm,搅拌1.5小时,完成环氧胶液的制备。
测试环氧胶胶触变指数为3.14,黏度值为9600mpa.s.
触变指数在3.0-4.5范围内,黏度值在8000-10000mpa.s.范围值内,适合用作miniLED封装胶膜制备工作。
将环氧胶液在涂覆线上进行涂覆操作,将涂胶线速设置为:5m/min,烘箱加热段温度分别设置为:100℃/110℃/120℃/110℃/100℃,用一面带离型的PET薄膜为承载膜,在离型面上进行涂胶的操作,涂胶厚度为300μm,涂完胶经过烘箱段烘烤后,胶呈半固化状态,经冲压机冲压后,将胶膜按指定的尺寸进行裁切,然后进行密封分隔包装,放置于-5℃下低温储存,即得miniLED封装胶膜。
实施例4
将80份无卤双酚A环氧树脂(南亚的NPEL-127E)、20份聚己内酯多元醇(Daicel的205U)、25份的环氧与橡胶核复合物(KANEKA的MX125)和0.7份消泡剂(Airex922)添加到反应釜内,在80℃、真空条件下,转速500rpm搅拌30分钟,使其混合均匀;之后使混合液冷至室温;
调低搅拌速率,将27份有机酰肼固化剂(日本味之素的VDH-J)加到反应釜中,之后将转速调到500rpm真空条件搅拌15分钟,使混合液搅拌均匀;
将转速降低到100rmp后,开始添加触变剂、抗氧化剂和紫外线吸收剂,取3.0份触变剂(赢创德固赛的R974)、0.3份抗氧化剂(Chinox245)和1.5份紫外线吸收剂(恒桥股份的Chemfos-TPP)到反应釜中,加完后抽真空条件下将转速调整到500rpm,搅拌1.5小时,完成环氧胶液的制备。
测试环氧胶胶触变指数为3.22,黏度值为8400mpa.s.
触变指数在3.0-4.5范围内,黏度值在8000-10000mpa.s.范围值内,适合用作miniLED封装胶膜制备工作。
将环氧胶液在涂覆线上进行涂覆操作,将涂胶线速设置为:5m/min,烘箱加热段温度分别设置为:100℃/110℃/120℃/110℃/100℃,用一面带离型的PET薄膜为承载膜,在离型面上进行涂胶的操作,涂胶厚度为200μm,涂完胶经过烘箱段烘烤后,胶呈半固化状态,经冲压机冲压后,将胶膜按指定的尺寸进行裁切,然后进行密封分隔包装,放置于-5℃下低温储存,即得miniLED封装胶膜。
对比例1-和实施例4相比,使用脂肪族环氧树脂
将80份脂环族环氧树脂(新纳希的S-06E)、20份聚己内酯多元醇(Daicel的205U)、25份的环氧与橡胶核复合物(KANEKA的MX125)和0.7份消泡剂(Airex922)添加到反应釜内,在80℃、真空条件下,转速500rpm搅拌30分钟,使其混合均匀;之后使混合液冷至室温;
调低搅拌速率,将27份有机酰肼固化剂(日本味之素的VDH-J)加到反应釜中,之后将转速调到500rpm真空条件搅拌15分钟,使混合液搅拌均匀;
将转速降低到100rmp后,开始添加触变剂、抗氧化剂和紫外线吸收剂,取3.0份触变剂(赢创德固赛的R974)、0.3份抗氧化剂(Chinox245)和1.5份紫外线吸收剂(恒桥股份的Chemfos-TPP)到反应釜中,加完后抽真空条件下将转速调整到500rpm,搅拌1.5小时,完成环氧胶液的制备。
测试环氧胶胶触变指数为3.31,黏度值为6400mpa.s.
触变指数在3.0-4.5范围内,黏度值不在要求的8000-10000mpa.s.范围值内,不适合用作miniLED封装胶膜制备工作,因此不做制备胶膜处理。
对比例2-和实施例4相比,使用丁腈橡胶类增韧剂
将80份无卤双酚A环氧树脂(南亚的NPEL-127E)、20份羧基聚丁二烯丙烯腈(CTBN)、25份的环氧与橡胶核复合物(KANEKA的MX125)和0.7份消泡剂(Airex922)添加到反应釜内,在80℃、真空条件下,转速500rpm搅拌30分钟,使其混合均匀;之后使混合液冷至室温;
调低搅拌速率,将27份有机酰肼固化剂(日本味之素的VDH-J)加到反应釜中,之后将转速调到500rpm真空条件搅拌15分钟,使混合液搅拌均匀;
将转速降低到100rmp后,开始添加触变剂、抗氧化剂和紫外线吸收剂,取3.0份触变剂(赢创德固赛的R974)、0.3份抗氧化剂(Chinox245)和1.5份紫外线吸收剂(恒桥股份的Chemfos-TPP)到反应釜中,加完后抽真空条件下将转速调整到500rpm,搅拌1.5小时,完成环氧胶液的制备。
测试环氧胶胶触变指数为3.12,黏度值为8750mpa.s.
触变指数在3.0-4.5范围内,黏度值在8000-10000mpa.s.范围值内,适合用作miniLED封装胶膜制备工作。
将环氧胶液在涂覆线上进行涂覆操作,将涂胶线速设置为:5m/min,烘箱加热段温度分别设置为:100℃/110℃/120℃/110℃/100℃,用一面带离型的PET薄膜为承载膜,在离型面上进行涂胶的操作,涂胶厚度为200μm,涂完胶经过烘箱段烘烤后,胶呈半固化状态,经冲压机冲压后,将胶膜按指定的尺寸进行裁切,然后进行密封分隔包装,放置于-5℃下低温储存,即得miniLED封装胶膜。
本发明各实施例和对比例使用的物料如下表1。
表1实施例1-4和对比例1-2投料表。
测试例
黏度及触变指数测试方法:
用校正好的博勒飞黏度测试仪(DV-S)测试胶水黏度,测试温度:25℃。触变指数:选取10倍转速时的黏度比值,低转速黏度除以高转速黏度值。
透明度测试方法:
选取适当长度的环氧胶膜,用可见光分光光度计测试胶膜的透光度,选择波长450nm处的测试数值。
剪切强度测试方法:
剪取1cm2胶膜,上下面用铝基板热压后(150℃*120S*50kgf)+150℃/1小时烘烤制得测试样品,用电子拉力机测试样品的剪切强度,测试速度:50mm/min。
玻璃化转化温度测试方法:
将胶膜样品置于烘箱中150℃/1小时固化,待冷至室温后,称量0.1-0.5g样放置于 DSC中的坩埚中,测试条件:空气气氛,升温速率:10℃/min.玻璃化转化温度取曲线中形变的中间位置。
储存期测试方法:
参考IPC-TM-650《测试方法手册》,以胶膜初始溢胶量为基准,每一周测试一次溢胶量,低于50%或溢胶量低于150μm,判定为超期。
测试结果见表1。
表1实施例和对比例的性能测试结果
可以看出,对比例1使用脂肪族环氧树脂无法得到粘度符合要求的环氧胶,进而无法用于制备miniLED胶膜。而对比例2使用丁腈橡胶类增韧剂,虽然环氧胶触变系数和粘度符合本发明的要求,但是制备得到的环氧胶膜。透明度较低,剪切强度较差。
最后应当说明的是,以上内容仅用以说明本发明的技术方案,而非对本发明保护范围的限制,本领域的普通技术人员对本发明的技术方案进行的简单修改或者等同替换,均不脱离本发明技术方案的实质和范围。
Claims (10)
1.一种环氧胶,按重量份数计,由以下成分制成:
环氧树脂60-100份,
增韧剂25-45份,
消泡剂0.5-1.5份,
固化剂20-45份,
触变剂1.5-5.0份,
抗氧化剂0.3-1.5份,
紫外吸收剂0.3-1.5份。
2.根据权利要求1所述的环氧胶,其特征在于,所述环氧树脂选自双酚A环氧树脂、双酚F环氧树脂、氢化双酚A环氧树脂和有机硅改性环氧树脂中的至少一种,优选为双酚A环氧树脂和氢化双酚A环氧树脂中的至少一种;所述增韧剂选自丁苯核壳橡胶、聚己内酯多元醇和有机硅改性环氧树脂中的至少一种,优选为ALBIFLEX 348、KANEKA的MX125、ALBIFLEX 296和Daicel 205U中的至少一种。
3.根据权利要求1所述的环氧胶,其特征在于,所述消泡剂选自有机硅聚合物消泡剂,优选为BYK-310、BYK-348、BYK-A530、BYK-054、BYK-1794、R-6501、Airex922、Airex944、Airex900中的至少一种;所述固化剂选自改性咪唑类和有机酰肼类中的至少一种,优选为FXR-1081、VDH-J和UDH-J中的至少一种。
4.根据权利要求1所述的环氧胶,其特征在于,触变剂选自疏水性气相二氧化硅,优选为TH-20、HL-300、TS-720、HB-139、HB-615、T-40、H13L、R-974和TS-530中的至少一种,更优选为TS-720、R-974和HB-139中的至少一种。
5.根据权利要求1所述的环氧胶,其特征在于,所述抗氧化剂选自磷系抗氧化剂、受阻酚类抗氧化剂中的至少一种,优选为Chemnox-1135、Chemnox-1520、Chemnox-6、Chinox245、Chinox35、Chinox TP-10H和CN 510中至少一种,更优选为Chinox TP-10H、Chinox245和Chemnox-1520中的至少一种。
6.根据权利要求1所述的环氧胶,其特征在于,所述紫外吸收剂选自Chisorb Suv、Chemsorb-329、Chemsorb-234、Chemsorb-360、Chisorb Epl、Chemsorb BP4、Chemsorb BP6和Chemfos-TPP中至少一种,优选为Chemfos-TPP、Chisorb Epl和Chemsorb BP4中的至少一种。
7.根据权利要求1所述的环氧胶,其特征在于,所述环氧胶触变指数为3.0-4.5,黏度值为8000-10000mpa.s.。
8.一种如权利要求1-7任一项所述的环氧胶的制备方法,包括以下步骤:
(1)树脂与增韧剂、消泡剂的混合:将环氧树脂、增韧剂和消泡剂混合,在75-85℃、真空条件下,转速450-550rpm搅拌10-20分钟,使其混合均匀,冷却至室温,得液体A;
(2)固化剂的添加:在80-120rpm的情况下,将固化剂加到步骤(1)的液体A中,将转速调到300-500rpm真空条件搅拌10-15分钟,使混合液搅拌均匀,得液体B;
(3)触变剂和抗氧化剂、紫外吸收剂的添加:在80-120rpm的情况,向步骤(2)的液体B中,加入触变剂、抗氧化剂和紫外线吸收剂,加完后真空条件下将转速调整到500-700rpm,搅拌1-2小时,即得环氧胶。
9.一种使用权利要求1-7任一项所述环氧胶制备的miniLED封装胶膜。
10.根据权利要求9所述的封装胶膜,其特征在于,所述胶膜通过以下步骤制备得到,
(1)涂覆:以一面经过离型处理的雾化PET膜为底,使用所述环氧胶对所述PET膜进行涂覆;优选涂覆条件为:涂膜厚度:200-300μm,线速4-6m/min,烘箱温度区间为:100℃/110℃/120℃/110℃/100℃,烘箱段长为12-13m.;
(2)包装及储存:将涂覆后的环氧胶膜进行裁切并密封分隔包装,将成品置于-5-0℃下冷藏储存。
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