CN106893260A - 光学固态预聚物与模塑组合物 - Google Patents
光学固态预聚物与模塑组合物 Download PDFInfo
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Abstract
本发明提供的光学固态预聚物包括:100重量份的(a)环氧树脂与0.1至30重量份的(b)低聚倍半硅氧烷硅醇反应而成的产物,其中(a)环氧树脂包括(a1)线性硅氧烷环氧树脂与(a2)环状硅氧烷环氧树脂,且(a1)线性硅氧烷环氧树脂与(a2)环状硅氧烷环氧树脂的重量比介于1:1至5:1之间。
Description
【技术领域】
本发明涉及模塑组合物,更特别涉及其包含的光学固态预聚物的组成。
【背景技术】
发光二极管(LED)具有节能省电、体积小、寿命长、应答速度快、污染低、高可靠度、模组弹性大等众多优点,因此应用范畴非常广泛。近年来技术不断的进步,LED的效率及亮度不断的提升,使得其应用范围逐渐延伸至显示器背光模组、车用光源、与一般照明。目前已逐渐取代现有的荧光灯而成为新一代的照明光源。高功率及高亮度LED也已成为现在发展的主流,其需求也将日益增加。而现有热固型环氧树脂模塑组合物(EMC)材料主要应用于半导体IC封装,将先前制程所加工的晶片电路、导线引脚及相关材料加以封装保护包覆,以避免外力破坏及环境影响。EMC所用的环氧树脂及硬化剂几乎都是多官能基固态材料,经由粉碎与干式混合,再经由混练设备(如双螺杆混练机)将导入的高含量无机粉体加热混练进行分散,制备出均匀分散、加工流动性可调整、及可快速固化成型的热硬化型转注成型树脂组合物EMC。然而此类树脂与硬化剂材料不具有光学透明性,故仅局限在半导体IC封装,而无法延伸到需光学透明特性的LED白色反射EMC材料。
目前LED背光模组与一般照明应用的高效能LED封装元件存在朝向高亮度与高功率趋势的需求。传统应用在PLCC LED元件的热塑型树脂PPA(polyphthalamide)反射杯材料具有不耐光热及易黄变等问题,而无法应用到高功率PLCC LED元件。近年来,热塑型材料亦包含新型射出材料PCT(聚酯(polyester)系列),但仍无法有效改善热塑型材料不耐光热易黄变的性质。
综上所述,为符合高功率LED元件耐光热稳定性反射材料的需求,需开发出更高耐光与耐热的热固型EMC白色反射材料,以提升LED封装元件的可靠度。
【发明内容】
本发明一实施例提供的光学固态预聚物,包括:100重量份的(a)环氧树脂与0.1至30重量份的(b)低聚倍半硅氧烷硅醇反应而成的产物,其中(a)环氧树脂包括(a1)线性硅氧烷环氧树脂与(a2)环状硅氧烷环氧树脂,且(a1)线性硅氧烷环氧树脂与(a2)环状硅氧烷环氧树脂的重量比介于1:1至5:1之间。
本发明一实施例提供的模塑组合物,包括:10至50重量份的上述光学固态预聚物;3至15重量份的固态非芳香族酸酐;以及30至85重量份的白色颜料与无机填充剂,其中白色颜料与无机填充剂的重量比介于1:2至1:10之间。
【具体实施方式】
在一实施方式中,光学固态预聚物包括:100重量份的(a)环氧树脂与0.1至30重量份的(b)低聚倍半硅氧烷硅醇反应而成的产物。(b)低聚倍半硅氧烷硅醇比例较高时对组合物的反应性具有提升的效果,同时对(a)环氧树脂的反应速率较快。若(b)低聚倍半硅氧烷硅醇的比例过低,则经由150℃高温加热反应仍无法形成固态预聚物。若(b)低聚倍半硅氧烷硅醇的比例过高,则硬化反应在接近室温下即快速进行,造成后续光学预聚物的制程加工性及后续组合物配方的加工性及反应性的反效果。相较于传统透明环氧树脂系统所用的酸酐硬化剂,上述(b)低聚倍半硅氧烷硅醇对(a)环氧树脂具有较低的反应温度。
上述(a)环氧树脂包括(a1)线性硅氧烷环氧树脂与(a2)环状硅氧烷环氧树脂,且(a1)线性硅氧烷环氧树脂与(a2)环状硅氧烷环氧树脂的重量比介于1:1至5:1之间。若(a2)环状硅氧烷环氧树脂的比例过低,则转注模封的固化物机械强度过软,导致无法均匀填充满模或脱模时粘模。若(a2)环状硅氧烷环氧树脂的比例过高,则转注模封固化物的机械强度则过脆。
在一实施方式中,(a1)线性硅氧烷环氧树脂的结构如式1所示:
(式1)
上述(a1)线性硅氧烷环氧树脂具有两个以上的环氧基。另通过分子结构设计,利用硅氢化反应将环氧基导入硅氧烷分子链中,可将(a1)线性硅氧烷环氧树脂的重均分子量控制在500至15000之间。若(a1)线性硅氧烷环氧树脂的重均分子量过低,则会有机械强度及耐热性不足的问题。若(a1)线性硅氧烷环氧树脂的重均分子量过高,则不易加工。在式1中,m与n的比例介于1:10至3:1之间。上述m/n的比例可让预聚物具有适当的交联密度,可改善传统EMC反射材料机械强度不足的问题。在式1中,R1为C1-6烷基或环氧基;R2为C1-6烷基;以及R3为环氧基。
在一实施方式中,(a2)环状硅氧烷环氧树脂的结构如式2所示:
(式2)
上述(a2)环状硅氧烷环氧树脂的分子量介于700至1100之间。若(a2)环状硅氧烷环氧树脂的分子量过低,则刚性不足。若(a2)环状硅氧烷环氧树脂的分子量过高,则易脆裂。在式2中,R4为C1-6烷基;以及R5为环氧基。
由于上述(a)环氧树脂与(b)低聚倍半硅氧烷硅醇含有大量的硅氧烷结构,使组合物整体键能提高,因此具有优良的紫外光及高温稳定性。
在一实施方式中,(b)低聚倍半硅氧烷硅醇的结构为(R6 3SiO1/2)a(R7 2SiO2/2)b(R8SiO3/2)c(SiO4/2)d(HO1/2)e,且重均分子量介于600至6000之间。若(b)低聚倍半硅氧烷硅醇的重均分子量过低,则无法形成室温固态预聚物。若(b)低聚倍半硅氧烷硅醇的重均分子量过高,则在80~120℃下的预聚物熔融加工流动性不足。R6为C1-8烷基或羟基,R7与R8各自独立为C1-8烷基,a介于0至10之间,b介于0至12之间,c介于0至12之间,d介于0至10之间,且e介于3至18之间。
在一实施方式中,(b)低聚倍半硅氧烷硅醇的结构如式3所示:
(式3)
在式3中,R9为烷基。
上述光学固态预聚物具有多硅氧烷结构,可提升其高耐光热特性。上述光学固态预聚物具有加工流动性可调整的特性,当温度小于50℃为不流动固体,而温度范围在80~120℃,其熔融粘度范围介于100~10,000mPa.s,且具有反应性。此外,上述光学固态预聚物仍残留部分未反应的环氧基及氢氧基等反应性官能基,之后可与其他树脂、硬化剂、其他添加剂、与无机粉体等后续混练加工并快速加热固化,也可作为混练加工的主要树脂组成,以制备转注成型用热固性EMC材料。由于EMC材料的主要树脂结构具有多官能基硅氧烷链段,可比现有白色EMC反射材料具有更优异的高光热稳定性,以及高透明的光学特性。另一方面,具有环状硅氧烷结构的环氧树脂可改善目前白色EMC材料的制程加工过程中因反应速率过慢所造成的溢胶毛边现象。上述组成同时改善转注成型快速模封制程加工特性需求、光电元件构装材料所需的高光热稳定性、模封硬化完的材料机械强度、以及材料的耐候性质。
在一实施方式中,光学固态预聚物可还包括0至25重量份的酸酐与0至0.5重量份的催化剂。酸酐可进一步使反应更快速形成固态预聚物。若酸酐的用量过高,则反应过快形成交联固态预聚物,无法提供后段组合物再加工反应性。举例来说酸酐为常温下固态或液态的非芳香族酸酐。固态的非芳香族酸酐可为四氢苯酐、六氢苯酐、丁二酸酐、丁烯二酸酐、或上述的组合。液态的非芳香族酸酐可为甲基四氢苯酐、甲基六氢苯酐、或上述的组合。若酸酐为芳香族酸酐,则会使产品易黄化。催化剂可进一步加速(a)环氧树脂与(b)低聚倍半硅氧烷硅醇的反应速度。若催化剂的用量过高,则使反应过快形成交联固态预聚物,无法提供后段组合物再加工反应性。举例来说,催化剂可为乙酰丙酮锆或乙酰丙酮铝。
上述光学固态预聚物可用于模塑组合物中。举例来说,可取10至50重量份的光学固态预聚物、3至15重量份的固态非芳香族酸酐;以及30至85重量份的白色颜料与无机填充剂混合形成模塑组合物。若光学固态预聚物的比例过低,则后端模封转注制程时无法均匀填充满模或脱模易脆裂。若光学固态预聚物的比例过高,则组合物反射率偏低,导致耐热性不足、长时间易黄化现象。若固态非芳香族酸酐的比例过低,则组合物交联密度不足,导致机械强度不足易脆裂。若固态非芳香族酸酐的比例过高,则未反应酸酐残余量过高,导致耐热性不足、长时间易黄化现象。值得注意的是,若非芳香族酸酐为液态而非固态,则无法形成固态组合物,无法进行模封转注制程。若白色颜料与无机填充剂的比例过低,则组合物反射率偏低。若白色颜料与无机填充剂的比例过高,则组合物在模封制程熔融粘度过高,流动性降低,导致后端模封转注制程时无法均匀填充满模或脱模易脆裂。
上述白色颜料与无机填充剂的重量比介于1:2至1:10之间。若无机填充剂的比例过低,则组合物在模封制程熔融粘度过高,流动性降低,导致后端模封转注制程时无法均匀填充满模。若无机填充剂的比例过高,则组合物反射率偏低不足。举例来说,白色颜料可为氧化铝、氧化钛、氧化镁、氧化锆、氧化锌、或上述的组合,而无机填充剂可为二氧化硅、氢氧化铝、氢氧化镁、碳酸镁、碳酸钡、或上述的组合。
在一实施方式中,模塑组合物还包括0.2至2重量份的偶合剂与脱模剂,以利固化与脱模制程。若偶合剂与脱模剂的比例过低,则与未添加的效果相同。若偶合剂与脱模剂的比例过高,则导致组合物机械强度不足易脆裂,耐热性不足长时间易黄化现象。举例来说,偶合剂可为γ-缩水甘油氧基丙基三甲氧硅烷、γ-缩水甘油氧基丙基甲基二乙氧硅烷或β-(3,4-环氧环己基)乙基三甲氧硅烷。脱模剂可为硬脂酸钙、脂肪酸酯、或脂肪族醚。
为了让本发明的上述和其他目的、特征、和优点能更明显易懂,下文特举数实施例作详细说明如下:
实施例
表1为实施例中所用的起始物其名称、结构、与来源。
表1(主要使用药品表)
合成例1(SEP-1,线性硅氧烷环氧树脂)
将9.93g的4-乙烯-1-环己烯-1,2-环氧化物、10ppm的三硫丁醚三氯化铑、及0.0015g的N,N-双十八烷基甲胺加入250ml的双颈反应瓶中,再加入50mL的甲苯搅拌并加热至100℃。接着于100℃下,逐滴加入19.5g的HMS-301(甲基氢硅氧烷(Methylhydrosiloxane),购自Gelest)。待HMS-301滴毕后,将温度升高至115℃搅拌,并以FT-IR监测反应混合物于2160cm-1处的吸收峰(-SiH)是否消失,以判断反应是否完全。待反应完全后,将温度降至室温。接着将碳黑加入粗产物(crude)中,搅拌进行纯化。最后过滤去除碳黑,并以旋转浓缩仪移除滤液中的甲苯,以得SEP-1。
合成例2(SEP-2,环状硅氧烷环氧树脂)
取59.52g的4-乙烯-1-环己烯-1,2-环氧化物、10ppm的三硫丁醚三氯化铑、及0.0015g的N,N-双十八烷基甲胺加入250mL的双颈反应瓶中,再加入50mL的甲苯搅拌并加热至100℃。接着于100℃下,逐滴加入24g的1,3,5,7-四甲基环四硅氧烷(SIT7530,购自Gelest)。待SIT7530滴毕后,将温度升高至115℃搅拌,并以FT-IR监测反应混合物于2160cm-1处的吸收峰(-SiH)是否消失,以判断反应是否完全。待反应完全后,将温度降至室温。接着将碳黑加入粗产物中,搅拌进行纯化。最后过滤去除碳黑,并以旋转浓缩仪移除滤液中的甲苯,以得SEP-2。
实施例A
将Zr-催化剂、硅醇-1、硅醇-2、与六氢苯酐的组合溶于甲苯中,并于常温下搅拌20分钟。另外将SEP-1与SEP-2混合均匀后加入上述的甲苯溶液中,常温下搅拌20分钟。接着在室温下搅拌上述混合物,同时以真空方式移除混合物中的甲苯以形成树脂材料。接着将树脂材料加热至加工温度后维持一段加工时间,冷却后观察外观(无色固态不流动)。最后将上述预聚物置于25℃下熟化一段时间后观察其外观。上述反应物用量、加工温度与时间、预聚物的性质、熟化温度与时间、与预聚物外观如表2所示。
比较例B1、B2、与B5
将硅醇-1或硅醇-1与硅醇-2的组合溶于甲苯中,并于常温下搅拌20分钟。另外将SEP-1与SEP-2混合均匀后加入上述的甲苯溶液中,常温下搅拌20分钟。接着在室温下搅拌上述混合物,同时以真空方式移除混合物中的甲苯以形成树脂材料。接着将树脂材料加热至加工温度后维持一段加工时间,冷却后观察外观。比较例B1与B5的预聚物固化不流动,而不适于作为EMC。最后将比较例B2的预聚物置于25℃下熟化一段时间后观察其外观。上述反应物用量、加工温度与时间、预聚物的性质、熟化温度与时间、与预聚物外观如表2所示。
比较例B3
将酚醛硬化剂(HRJ1166)加入酚醛环氧树脂(ECN1273)的甲苯溶液中,并于常温下搅拌20分钟。接着以真空方式移除混合物中的甲苯以形成树脂材料。接着将树脂材料在加热至加工温度后维持一段加工时间,冷却后材料外观呈深褐色的不流动状态。最后将预聚物置于25℃进行熟化一段时间。上述反应物用量、加工温度与时间、预聚物的性质、熟化温度与时间、与预聚物外观如表2所示。
比较例B4
将SEP-1加入Zr-QR与六氢苯酐混合的甲苯溶液中,并于常温下搅拌20分钟。接着以真空方式移除混合物中的甲苯以形成树脂材料。接着将树脂材料在加热至加工温度后维持一段加工时间,冷却后观察其外观。最后将比较例B4的预聚物置于25℃下熟化一段时间后观察其外观。上述反应物用量、加工温度与时间、预聚物的性质、熟化温度与时间、与预聚物外观如表2所示。
表2
实施例C
取实施例A的预聚物、固态酸酐如六氢苯酐、四氢苯酐、或上述的组合、无机填充剂、白色颜料、催化剂、偶合剂、以及脂肪酸酯系脱模剂,以混合机充分搅拌与混合均匀后,得到模塑组合物。接着,利用轧轮机、捏合机、或挤出机在80℃下对模塑组合物加以熔融混练15分钟。冷却后,将所得混练产物进行打粉粉碎并进行打锭,得到胶饼。接着,利用所得胶饼进行转注模封制程,得知在制程温度175℃下具流动性(可完全填入预定的模具内),冷却后可在120秒内固化。最后,测量固化产物在波长450nm下的反射率。上述组成的种类与比例与模塑组合物的加工性如表3所示。
比较例D
取比较例B的预聚物(B2、B3、与B4)、六氢苯酐、无机填充剂、白色颜料、催化剂、偶合剂、以及脂肪酸酯系脱模剂,以混合机充分搅拌与混合均匀后,得到模塑组合物。接着利用轧轮机、捏合机、或挤出机在80℃下对模塑组合物加以熔融混练15分钟。冷却后,将所得混练产物进行打粉粉碎并进行打锭,得到胶饼。接着,利用所得胶饼进行转注模封制程,冷却后固化。最后,测量固化产物在波长450nm下的反射率。上述组成的种类与比例与模塑组合物的加工性如表3所示。
表3
*:转注模封加工成型测试的正圆形模具:直径5cm及厚度3mm,◎:可均匀满模及离模,X:可转注但无法均匀满模或离模。
由上述可知,实施例A的预聚物均适于作为模塑组合物。比较例B的预聚物有部分不具流动性(比如B1与B5),而其他预聚物在作为模塑组合物时的加工性不佳(比如B2与B4),或者硬化后的成品的光反射率过低(比如B3)。
虽然本发明已以数个实施例揭露如上,然其并非用以限定本发明,任何本技术领域技术人员在不脱离本发明的精神和范围内,应可作任意的更动与润饰,因此本发明的保护范围应以所附权利要求书所界定的范围为准。
Claims (11)
1.一种光学固态预聚物,包括:
100重量份的(a)环氧树脂与0.1至30重量份的(b)低聚倍半硅氧烷硅醇反应而成的产物,
其中(a)环氧树脂包括(a1)线性硅氧烷环氧树脂与(a2)环状硅氧烷环氧树脂,且(a1)线性硅氧烷环氧树脂与(a2)环状硅氧烷环氧树脂的重量比介于1:1至5:1之间。
2.如权利要求1所述的光学固态预聚物,其中(a1)线性硅氧烷环氧树脂的结构为:
其中(a1)线性硅氧烷环氧树脂具有两个以上的环氧基且重均分子量为500至15000之间,m与n的比例为1:10至3:1;R1为C1-6烷基或环氧基;R2为C1-6烷基;以及R3为环氧基。
3.如权利要求1所述的光学固态预聚物,其中(a2)环状硅氧烷环氧树脂的结构为:
其中(a2)环状硅氧烷环氧树脂的分子量为700至1100;R4为C1-6烷基;以及R5为环氧基。
4.如权利要求1所述的光学固态预聚物,其中(b)低聚倍半硅氧烷硅醇的结构为(R6 3SiO1/2)a(R7 2SiO2/2)b(R8SiO3/2)c(SiO4/2)d(HO1/2)e,其中(b)低聚倍半硅氧烷硅醇的重均分子量介于600至6000之间,R6为C1-8烷基或羟基,R7与R8各自独立为C1-8烷基,a为0至10,b为0至12,c为0至12,d为0至10,且e为3至18。
5.如权利要求1所述的光学固态预聚物,其中(b)低聚倍半硅氧烷硅醇的结构为:
其中R9为烷基。
6.如权利要求1所述的光学固态预聚物,还包括0至25重量份的酸酐与0至0.5重量份的催化剂。
7.如权利要求6所述的光学固态预聚物,其中酸酐为固态或液态的非芳香族酸酐,包括丁二酸酐、丁烯二酸酐、四氢苯酐、六氢苯酐、甲基四氢苯酐、甲基六氢苯酐、或上述的组合。
8.一种模塑组合物,包括:
10至50重量份的权利要求1所述的光学固态预聚物;
3至15重量份的固态非芳香族酸酐;以及
30至85重量份的白色颜料与无机填充剂,
其中白色颜料与无机填充剂的重量比为1:2至1:10。
9.如权利要求8所述的模塑组合物,其中该白色颜料包含氧化铝、二氧化钛、氧化镁、氧化锆、氧化锌、或上述的组合。
10.如权利要求8所述的模塑组合物,其中该无机填充剂包括二氧化硅、氢氧化铝、氢氧化镁、碳酸镁、碳酸钡、或上述的组合。
11.如权利要求8所述的模塑组合物,还包括0.2至2重量份的偶合剂与脱模剂。
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