CN102714265A - 作为水分子的扩散屏障的浇铸组合物 - Google Patents
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Abstract
本发明涉及基于透明环氧或有机硅树脂(1),特别用于优选发射白光的电致发光组件(3)中的浇铸组合物。该浇铸组合物通过玻璃和/或二氧化硅颗粒(2)的使用而用作湿气或水分子的扩散屏障。
Description
本发明涉及一种基于透明环氧树脂或有机硅树脂的浇铸组合物,其特别用于优选发射白光的电致发光组件中,和制备这类浇铸组合物的方法。这里,浇铸组合物通过玻璃或二氧化硅片的使用而用作水分子的扩散屏障。
商业白光pc-LED由发射蓝光光谱区的芯片和由聚硅氧烷或环氧树脂组成的涂层组成,一种或多种无机发光材料位于所述涂层中。
无机发光材料通常基于硅酸盐、硫化、氮化或氮氧化材料。这些材料具有在极痕量湿气的存在下分解的性能。
在原硅酸盐无机发光材料的情况下,这特别适用于包含高浓度钡的绿色无机发光材料。空气中存在的湿气通过聚硅氧烷或环氧树脂基体扩散至无机发光材料颗粒中。这样的结果是由于无机发光材料的分解,其亮度降低并随时间劣化。这与白光pc-LED的性能下降有关:首先,LED的色点改变。此外,存在于芯片的LED中的反射器和电连接被硫化或氮(氧)化无机发光材料的水解产物腐蚀性破坏。
由于需要置换LED导致的成本上升妨碍了白光LED快速取代效率低且具有短寿命的白炽灯泡、卤素灯和荧光灯。
EP862794公开了一种由环氧树脂组成且包含无机发光材料颜料的波长转换浇铸组合物。为减少聚集体形成,无机发光材料颜料可具有聚硅氧烷涂层。
因此,本发明的目的是提供不具有一个或多个上述缺点的浇铸组合物。
令人惊讶的是,现在已发现包含聚硅氧烷或环氧树脂基体的浇铸组合物中由痕量扩散水导致的无机发光材料的分解可通过将片形无机颗粒引入基体中而防止。由玻璃或二氧化硅组成的片形颗粒充当水分子的有效扩散屏障。此外,片形颗粒可分散于聚硅氧烷或环氧树脂中并可作为单独扩散阻挡层直接施涂于LED的无机发光材料涂层上。(图1A或1B)
因此,本发明涉及一种基于至少一种透明聚硅氧烷或环氧树脂的浇铸组合物,其包含无机发光材料颗粒和优选片形式的玻璃和/或二氧化硅颗粒,和UV或蓝色发光二极管。
在优选实施方案中,玻璃或二氧化硅颗粒和无机发光材料颗粒均匀分布于浇铸组合物中(参见图1A)。
在另一优选实施方案中,片形玻璃或二氧化硅颗粒以平行平面方式分散并排列于浇铸组合物中且作为单独扩散阻挡层直接排列于仅包含无机发光材料颗粒的另一浇铸组合物上(参见图1B)。
玻璃和二氧化硅颗粒优选具有5-20μm的直径和0.1-5μm的厚度。
无机发光材料颗粒的平均粒径d50优选为<20μm。
片形玻璃和二氧化硅颗粒的作用基于这一事实:水分子的扩散路径在包含聚硅氧烷或环氧树脂基体的浇铸组合物中被阻断。这通过颗粒在特定畴中的平行平面排列以及通过片在垂直方向上的偏斜排列进行(参见图2)。
由于玻璃或二氧化硅颗粒具有n=1.4-1.5范围内的聚硅氧烷或环氧树脂基体折射指数这一事实,白光LED的光学性能不会受到不利影响。由于片形颗粒的轻微散射性能(颗粒边缘的作用),亮度和颜色温度经白光LED的角范围改善。
为改善环氧或聚硅氧烷树脂内片形玻璃和/或二氧化硅颗粒的分散性,可将颗粒表面涂覆。然后通过湿化学方法或通过气相沉积将片形颗粒用聚硅氧烷/硅烷涂覆。这些有机硅化合物与片形颗粒的表面OH基团反应。所需颗粒的疏水性、低聚物/聚合物链的结构和在树脂上的偶联(物理和/或化学)通过硅化合物的有机链的改性控制。
无机发光材料颗粒优选由至少一种如下无机发光材料组成:(Y,Gd,Lu,Sc,Sm,Tb)3(Al,Ga)5O12:Ce(具有或不具有Pr)、(Ca,Sr,Ba)2SiO4:Eu、YSiO2N:Ce、Y2Si3O3N4:Ce、Gd2Si3O3N4:Ce、(Y,Gd,Tb,Lu)3Al5-xSixO12-xNx:Ce、BaMgAl10O17:Eu、SrAl2O4:Eu、Sr4Al14O25:Eu、(Ca,Sr,Ba)Si2N2O2:Eu、SrSiAl2O3N2:Eu、(Ca,Sr,Ba)2Si5N8:Eu、CaAlSiN3:Eu、锌碱土金属原硅酸盐、铜碱土金属原硅酸盐、铁碱土金属原硅酸盐、钼酸盐、钨酸盐、钒酸盐、III族氮化物、氧化物,在每种情况下单独或为其与一种或多种活化剂离子如Ce、Eu、Mn、Cr和/或Bi的混合物。
特别优选用于生产白光光电组件的无机发光材料颗粒为原硅酸盐。
用于生产无机发光材料颗粒的原料由基材(例如钇、铝、钆等的盐溶液)和至少一种掺杂剂(例如铈)组成。合适的原料为无机和/或有机物质,例如金属、半金属、过渡金属和/或稀土元素的硝酸盐、卤化物、碳酸盐、碳酸氢盐、磷酸盐、羧酸盐、醇化物、乙酸盐、草酸盐、硫酸盐、有机金属化合物、氢氧化物和/或氧化物,其溶于和/或悬浮液无机和/或有机液体中。优选使用包含必须化学计量比的相应元素的混合硝酸盐溶液、氯化物或氢氧化物溶液。
此外,本发明的目的通过一种制备基于至少一种透明聚硅氧烷或环氧树脂的浇铸组合物的方法实现,所述浇铸组合物包含无机发光材料颗粒和玻璃和/或二氧化硅颗粒和UV或蓝色发光二极管,所述方法的特征在于具有如下步骤:
a)将无机发光材料颗粒与粉状玻璃和/或二氧化硅颗粒均匀混合,
b)将无机发光材料和玻璃或二氧化硅颗粒的混合物用透明聚硅氧烷或环氧树脂分散,
c)将蓝色发光二极管用包含无机发光材料和玻璃和/或二氧化硅颗粒的聚硅氧烷或环氧树脂涂覆,
d)将涂层固化。
涂层的固化在120-180℃的温度下,优选在150℃下进行。
玻璃和二氧化硅颗粒的生产通过常规方法借助带方法由相应的碱金属盐(例如由用于二氧化硅的钾或钠水玻璃溶液)进行。生产方法详细描述于EP763573、EP608388和DE19618564中。
此外,本发明涉及一种制备基于至少一种透明聚硅氧烷或环氧树脂的浇铸组合物的方法,所述浇铸组合物包含无机发光材料颗粒和玻璃和/或二氧化硅颗粒和UV或蓝色发光二极管,所述方法的特征在于具有如下步骤:
a)将无机发光材料颗粒用聚硅氧烷或环氧树脂分散,
b)将发光二极管用无机发光材料颗粒和聚硅氧烷或环氧树脂的混合物涂覆,
c)将涂层固化,
d)将玻璃和/或二氧化硅颗粒分散于聚硅氧烷或环氧树脂中,
e)通过涂覆固化的无机发光材料涂层而产生扩散阻挡层,
f)将扩散阻挡层固化。
此外,优选通过湿化学方法或通过气相沉积将片形玻璃或二氧化硅颗粒用有机硅化合物(例如聚硅氧烷或硅烷)表面涂覆。如已提到的,在环氧或有机硅树脂上的偶联通过该涂层改善。
另外可将光散射颗粒,所谓的扩散剂(例如CaF2)加入浇铸组合物中。这有利地能使半导体组件的颜色印象(colour impression)和发射特征最佳化。
另外,浇铸组合物还可包含附着力促进剂、疏水剂、加工助剂和/或触变剂。可使用的触变剂例如为热解硅酸。触变剂用于环氧树脂的增稠以防止无机发光材料颗粒沉降。合适的加工助剂例如为乙二醇醚。
可使用的附着力促进剂例如为官能烷氧基硅氧烷,其改进无机发光材料颗粒与树脂之间的附着力。
可使用的疏水剂例如为液体有机硅蜡,其同样用于无机发光材料颗粒表面的改性。
本发明UV或蓝色发光二极管为包含特别是式InjGajAlkN的发光氮化铟铝镓的光源,其中0≤i,0≤j,0≤k,且i+j+k=1。
这类光源的可能形式是本领域技术人员已知的。这些可以为具有各种结构的发光LED芯片。
以下实施例意欲阐明本发明。然而,它们应决不被认为是限制性的。可用于制备的所有化合物或组分是已知且市售的或可通过已知方法合成。实施例中所述温度总是以℃表示。此外,不言而喻,在说明书和实施例中,组合物中组分的加入量总是合计为100%的总量。给出的百分数数据总是在给定上下文中考虑。然而,它们通常总是涉及所述部分重量或总重量。
实施例
实施例1:具有官能团的片形玻璃或二氧化硅颗粒的涂层
1.A)环氧聚合物的硅烷化
将100g二氧化硅或玻璃颗粒悬浮于1350ml去离子水中,同时强力搅拌。使用5重量%H2SO4将悬浮液的pH调整至pH=6.5,并将悬浮液加热至75℃。随后将4.0g Silquest A-186[β-(3,4-环氧基环己基)乙基三甲氧基硅烷]和Silquest A-1310[γ-异氰酸酯基丙基三乙氧基硅烷]的1:1混合物经60分钟计量加入悬浮液中,同时温和搅拌。当加入完成时,随后将混合物搅拌15分钟以完成硅烷在表面上的偶联。借助5重量%H2SO4将pH校正至6.5。随后将悬浮液过滤,并将滤饼用去离子水洗涤直至不含盐。干燥在130℃下进行20小时。然后将这样得到的粉末通过40μm筛筛分。
1.B)用于聚硅氧烷树脂偶联的硅烷化
将100g二氧化硅或玻璃颗粒悬浮于1350ml去离子水中,同时强力搅拌。使用5重量%H2SO4将悬浮液的pH调整至pH=6.5,并将悬浮液加热至75℃。随后将6.0g Silquest A-1110[γ-氨基丙基三甲氧基硅烷]和SilquestA-1524[γ-脲丙基三甲氧基硅烷]的1:2混合物经75分钟计量加入悬浮液中,同时温和搅拌。当加入完成时,随后将混合物搅拌15分钟以完成硅烷在表面上的偶联。借助5重量%H2SO4将pH校正至6.5。随后将悬浮液过滤,并将滤饼用去离子水洗涤直至不含盐。干燥在140℃下进行20小时。然后将这样得到的粉末通过40μm筛筛分。
1.C)对于聚硅氧烷树脂偶联,用乙烯基硅烷硅烷化
将100g二氧化硅或玻璃颗粒悬浮于1350ml去离子水中,同时强力搅拌。使用5重量%H2SO4将悬浮液的pH调整至pH=6.8,并将悬浮液加热至75℃。随后将6.0g Silquest A-174[γ-甲基丙烯酰氧基丙基三甲氧基硅烷]和Silquest A-151[乙烯基三乙氧基硅烷]的1:2混合物经90分钟计量加入悬浮液中,同时温和搅拌。当加入完成时,随后将混合物搅拌15分钟以完成硅烷在表面上的偶联。借助5重量%H2SO4将pH校正至6.5。随后将悬浮液过滤,并将滤饼用去离子水洗涤直至不含盐。干燥在140℃下进行20小时。然后将这样得到的粉末通过40μm筛筛分。
实施例2:LED的生产
A)无机发光材料与片形颗粒的混合物
将50ml两种树脂组分JCR 6122a和b中每一种与4重量%一种绿色原硅酸盐无机发光材料和2%未涂覆玻璃或二氧化硅颗粒或已根据实施例1A、B或C相容的片形颗粒混合。片形颗粒具有5-20μm的平均直径和0.1-5μm的厚度分布。将两种树脂混合物结合,搅拌并除气。然后将10ml引入喷射分配器或螺旋计量阀分配器的储存容器中。将粘合COB(板上芯片)粗LED包放在分配阀之下。然后使用分配器将树脂混合物的圆顶封装体(glob tops)逐滴置于粗LED包的芯片上。将这些涂覆的LED在干燥箱中在150℃下调节1小时,在此期间树脂(=浇铸组合物)固化。
B)单独扩散阻挡层
将50ml两种树脂组分JCR 6122a和b中每一种与4重量%一种绿色原硅酸盐无机发光材料混合。将两种树脂混合物结合,搅拌并除气。然后将10ml引入喷射分配器或螺旋计量阀分配器的储存容器中。将粘合COB(板上芯片)粗LED包放在分配阀之下。然后使用分配器将树脂混合物的圆顶封装体逐滴置于粗LED包的芯片上。将这些涂覆的LED在干燥箱中在150℃下调节1小时,在此期间树脂(=浇铸组合物)固化。
随后再次将50ml两种树脂组分JCR 6122a和b与4%未涂覆玻璃或二氧化硅颗粒或已根据实施例1A、B或C相容的片形颗粒混合。将两种树脂混合物结合,搅拌并除气。然后将10ml引入喷射分配器或螺旋计量阀分配器的储存容器中。将涂覆的LED包放在分配阀之下。然后使用分配器将由树脂混合物和片形颗粒组成的扩散阻挡层施涂于涂覆的LED上。然后将这些涂覆的LED在干燥箱中在150℃下调节1小时,在此期间扩散阻挡层的树脂固化。
图
下面参考大量说明性实施方案更详细地解释本发明。
图1显示玻璃或二氧化硅片在聚硅氧烷或环氧树脂基体中的均匀分布。1:聚硅氧烷/环氧树脂,2:玻璃或二氧化硅片,3:LED芯片;4:无机发光材料颗粒;B)单独扩散阻挡层;5:由仅包含片形颗粒的聚硅氧烷/环氧树脂基体组成的扩散阻挡层;6:扩散进的水。
图2:1:玻璃或二氧化硅颗粒。片形颗粒以垂直方向平行重叠排列,有效地防止水的扩散。
图3:1:50个具有单独水扩散阻挡层的LED的光通量测量的平均值。
2:50个具有水扩散屏障的LED的光通量测量的平均值。此处绿色原硅酸盐无机发光材料与片形颗粒混合。
3:50个不具有水扩散屏障的LED的光通量测量的平均值。
Claims (10)
1.基于至少一种透明聚硅氧烷或环氧树脂的浇铸组合物,其包含无机发光材料颗粒和玻璃和/或二氧化硅颗粒和UV或蓝色发光二极管。
2.根据权利要求1的浇铸组合物,其特征在于玻璃和/或二氧化硅颗粒和无机发光材料颗粒均匀分布于浇铸组合物中。
3.根据权利要求1的浇铸组合物,其特征在于玻璃和/或二氧化硅颗粒以平行平面方式分散并排列于浇铸组合物中,且作为单独扩散阻挡层直接排列于仅包含无机发光材料颗粒的另一浇铸组合物上。
4.根据权利要求1-3中一项或多项的浇铸组合物,其特征在于玻璃和/或二氧化硅颗粒具有5-20μm的直径和0.1-5μm的厚度。
5.根据权利要求1-4中一项或多项的浇铸组合物,其特征在于无机发光材料颗粒的平均粒径d50为<20μm。
6.根据权利要求1-5中一项或多项的浇铸组合物,其特征在于无机发光材料颗粒选自:
(Y,Gd,Lu,Sc,Sm,Tb)3(Al,Ga)5O12:Ce(具有或不具有Pr)、(Ca,Sr,Ba)2SiO4:Eu、YSiO2N:Ce、Y2Si3O3N4:Ce、Gd2Si3O3N4:Ce、(Y,Gd,Tb,Lu)3Al5-xSixO12-xNx:Ce、BaMgAl10O17:Eu、SrAl2O4:Eu、Sr4Al14O25:Eu、(Ca,Sr,Ba)Si2N2O2:Eu、SrSiAl2O3N2:Eu、(Ca,Sr,Ba)2Si5N8:Eu、CaAlSiN3:Eu、锌碱土金属原硅酸盐、铜碱土金属原硅酸盐、铁碱土金属原硅酸盐、钼酸盐、钨酸盐、钒酸盐、III族氮化物、氧化物,在每种情况下单独或为其与一种或多种活化剂离子如Ce、Eu、Mn、Cr和/或Bi的混合物。
7.根据权利要求6的浇铸组合物,其特征在于无机发光材料颗粒为原硅酸盐。
8.制备基于至少一种透明聚硅氧烷或环氧树脂的浇铸组合物的方法,所述浇铸组合物包含无机发光材料颗粒和玻璃和/或二氧化硅颗粒和UV或蓝色发光二极管,所述方法的特征在于具有如下步骤:
a)将无机发光材料颗粒与粉状玻璃和/或二氧化硅颗粒均匀混合,
b)将无机发光材料和玻璃和/或二氧化硅颗粒的混合物用透明聚硅氧烷或环氧树脂分散,
c)将蓝色发光二极管用包含无机发光材料和玻璃和/或二氧化硅颗粒的聚硅氧烷或环氧树脂涂覆,
d)将涂层固化。
9.制备基于至少一种透明聚硅氧烷或环氧树脂的浇铸组合物的方法,所述浇铸组合物包含无机发光材料颗粒和玻璃和/或二氧化硅颗粒和UV或蓝色发光二极管,所述方法的特征在于具有如下步骤:
a)将无机发光材料颗粒用聚硅氧烷或环氧树脂分散,
b)将发光二极管用无机发光材料颗粒和聚硅氧烷或环氧树脂的混合物涂覆,
c)将涂层固化,
d)将玻璃或二氧化硅颗粒分散于聚硅氧烷或环氧树脂中,
e)通过涂覆固化的无机发光材料涂层而产生扩散阻挡层,
f)将扩散阻挡层固化。
10.根据权利要求8和/或9的方法,其特征在于将玻璃和/或二氧化硅颗粒用有机硅化合物表面涂覆。
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- 2010-12-01 CN CN2010800595375A patent/CN102714265A/zh active Pending
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Also Published As
Publication number | Publication date |
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EP2519986A1 (de) | 2012-11-07 |
SG181935A1 (en) | 2012-08-30 |
US20120329184A1 (en) | 2012-12-27 |
EP2519986B1 (de) | 2018-09-12 |
US9093623B2 (en) | 2015-07-28 |
KR20120107127A (ko) | 2012-09-28 |
TW201136998A (en) | 2011-11-01 |
JP5767245B2 (ja) | 2015-08-19 |
JP2013516747A (ja) | 2013-05-13 |
WO2011079900A1 (de) | 2011-07-07 |
TWI527847B (zh) | 2016-04-01 |
KR101795091B1 (ko) | 2017-11-07 |
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