CN116426287A - 一种改性防蓝光量子点和量子点扩散板及制备方法 - Google Patents
一种改性防蓝光量子点和量子点扩散板及制备方法 Download PDFInfo
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- CN116426287A CN116426287A CN202310097107.1A CN202310097107A CN116426287A CN 116426287 A CN116426287 A CN 116426287A CN 202310097107 A CN202310097107 A CN 202310097107A CN 116426287 A CN116426287 A CN 116426287A
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Abstract
本专利提供了一种改性防蓝光量子点和量子点扩散板及制备方法。这种可吸收和转化短波蓝光的改性量子点和扩散板可以有效降低通过扩散板出射的短波蓝光，以达到防蓝光护眼的效果。改性量子点为表面包覆蓝光转化剂分子，可吸收短波蓝光并转化为450nm以上蓝光或与量子点本身发光波长相近的红光或绿光；另一方面，扩散板中加入可吸收短波蓝光的吸收或转化剂，进一步提升了量子点扩散板的防蓝光能力，可以有效降低短波蓝光出射，并且减少防蓝光膜的产线成本。
Description
技术领域
本发明属于显示技术领域。具体涉及一种应用于液晶显示技术领域的防蓝光量子点和量子点扩散板。
背景技术
量子点作为一种新型纳米材料，具有良好的光致发光和电致发光性能。相对于传统荧光材料，由于量子尺寸效应和量子限域效应，使得量子点的发光峰窄，且覆盖整个可见光范围，具有色彩丰富，色纯度高等优势。将量子点与传统液晶结构结合可以提升色彩显示效果。量子点扩散板是将量子点与传统扩散板结合，所获得增强显示的新产品。
目前，量子点扩散板应用于蓝光激发的背光结构中。蓝光光源通过激发扩散板中的红色和绿色量子点产生所需的红光和绿光，与蓝光激发光源共同产生白光效果。量子点对于不同波长的激发蓝光具有不同的吸收效果。
短波蓝光波长处于400～450nm之间，具有较高能量。另一方面，短波蓝光对于人眼具有较大危害。研究表明，人眼晶状体无法阻挡短波蓝光到达视网膜，而该波长范围内的蓝光长时间照射会使得眼内黄斑区毒素增多，诱发眼部疾病。因此，在保证显示效果的情况下，需要采用合适的方式减少短波蓝光的出射。
在扩散板中，为了减少短波蓝光的出射，通常在扩散板表面添加额外的防蓝光层。这种防蓝光层主要通过表面微结构吸收蓝光或者是添加蓝光吸收材料，实现减少有害蓝光的效果。一方面，添加的防蓝光层会增加生产过程中的产线成本，增加了扩散板的厚度；另一方面，这种防蓝光层是通过吸收或者散射蓝光的方式降低蓝光出射，减少蓝光的同时降低了扩散板亮度和量子点的转换效率。因此，在减少有害蓝光出射的同时，降低对量子点效率的影响是亟待解决的问题。
发明内容
本发明的目的是提供一种降低短波蓝光出射的量子点和量子点扩散板，通过吸收和转化有害蓝光，保护人眼健康。
为解决上述问题，本发明通过两种方式共同减少量子点扩散板的短波蓝光出射：第一个方面是通过可转化短波蓝光有机分子对量子点进行包覆改性；第二个方面是在量子点扩散板中引入适量的短波蓝光吸收剂或转化剂。此方法不仅可以将对人眼有害的短波蓝光转化为其他波长的可见光，提高量子点的转换效率；而且减少了生产防蓝光膜的产线成本。
进一步的，所述改性量子点为表面包覆有可转化短波蓝光的转化剂分子。其一，包覆的有机分子具有在不影响450nm以上蓝光波段的转化和透过的基础上，可吸收400～440nm范围内的短波蓝光；其二，根据所选用的短波蓝光转化剂不同，将其转化为与量子点发光波段相近的绿光或红光、或者对人眼伤害较小的波长在450nm以上的蓝光。
进一步的，扩散板中掺杂有适量的短波蓝光吸收或转化剂。吸收或转化剂的选择应当具备以下特点：其一，短波蓝光吸收或转化剂需要和扩散板中的其他材料有较好的兼容性，特别是量子点材料；其二，短波蓝光吸收或转化剂应当不影响整体扩散板的光线输出；其三，短波蓝光吸收或转化剂添加的量应当遵循整体扩散板的出光白平衡。
进一步的，所述改性量子点的制备过程包括：将量子点和转化剂溶于有机溶剂中；将量子点溶液和转化剂溶液分别注入反应器中，使转化剂与量子点充分反应，转化剂分子包覆在量子点表面；将反应完成的混合溶液干燥，去除有机溶剂，得到表面包覆有机蓝光转化剂的改性量子点。
进一步的，量子点扩散板的制作方法如下：将制备好的改性防蓝光量子点与塑料颗粒混合，经熔融共混制备量子点母粒；将蓝光吸收或转化剂、光散射粒子、抗氧化剂分别与塑料颗粒混合，按照蓝光吸收或转化剂：光散射粒子：抗氧剂：塑料颗粒＝(0.5～5)：(0.5～20)：(0.5～5)：100的质量比例，经过熔融混合制备添加剂母粒；将所制备的红色和绿色量子点母粒、添加剂母粒、塑料颗粒按照(1～10):(1～10)：100的比例通过挤塑成型的方法制备量子点扩散板。
进一步的，所述的转化剂为有机蓝光转化剂，为香豆素类、喹啉类、吡唑啉酮类、联苯类、萘酚类、芳胺类有机染料或稀土配合物中的一种或多种；所述量子点为Cd、Zn、S、Se、Sn、In、P、Cu中的两种或多种元素组成的量子点材料或者钙钛矿量子点；量子点和蓝光转化剂质量比为1:(0.2～10)；所述量子点表面包覆有机分子的方法包括但不限于交联法或配体交换法；
进一步的，蓝光吸收或转化剂包括硅量子点、碳量子点、银纳米材料、钛酸锶、氧化锌、氧化镉、氧化铬中的一种或几种的组合。在总的塑料含量中占比为0.05％～5％；所述改性量子点占总的塑料颗粒的质量比例为：0.01％～2％；所述光散射粒子为纳米氧化硅、氧化钛、有机硅、硫酸钡、交联聚苯乙烯、碳酸钙、丙烯酸塑料中的一种或几种。光散射粒子占总的扩散板质量比为：0.05％～3％。
进一步的，所述可吸收和转化的短波蓝光范围为400～440nm。
进一步的，所述改性量子点的制备过程包括以下过程：
S1、在反应气氛中，将量子点均匀分散在有机溶剂中配成溶液A，将蓝光转化剂分散于有机溶剂中配成溶液B；
S2、将量子点溶液A和蓝光转化剂溶液B分别注入反应有机溶剂中，再加入交联剂，密闭反应器，保持反应气氛，搅拌1～12h，使蓝光转化剂和量子点充分反应，转化剂分子包覆在量子点表面；
S3、将反应完成的混合溶液通过醇类溶剂洗涤后干燥，去除有机溶剂，得到表面包覆有短波蓝光转化剂的改性量子点。
进一步的，所述改性量子点的制备原料包括：蓝光转化剂和量子点。转化剂为有机蓝光转化剂。所述有机蓝光转化剂选自香豆素类、喹啉类、吡唑啉酮类、联苯类、萘酚类、芳胺类有机染料和稀土配合物，发光波长与量子点发光波长相近。并且，有机蓝光转化剂中包含有吡啶、巯基、胺、膦、羧基、氨基等基团，可连接在量子点表面。量子点与蓝光转化剂质量比例为1:0.2～10；
进一步地，所述反应气氛为空气气氛、氮气气氛或惰性气体气氛，优选地，所述反应气氛为惰性气体气氛。
进一步的，所述量子点为Cd、Zn、S、Se、Sn、In、P、Cu中的两种或多种元素组成的量子点或者钙钛矿量子点。
进一步的，所述量子点表面包覆有机分子的方法包括但不限于交联法或配体交换法。所述有机分子交联法是将表面具有巯基或羧基或氨基配体的量子点溶解分散，并加入交联剂将有机蓝光转化剂包覆在量子点表面。所述配体交换法是将量子点与有机蓝光转化剂在溶液中进行反应，通过配体交换作用，将量子点表面配体部分交换为转化剂分子。所述包覆过程的反应温度为10℃～160℃，反应时间为1～12h。
进一步的，所述有机溶剂为常见有机溶剂。优选的，溶液A中有机溶剂为芳香烃类，反应有机溶剂为醇类。溶液B中有机溶剂根据蓝光转化剂的不同选择。溶液A中量子点与有机溶剂的质量比为1:1～10；溶液B中蓝光转化剂与有机溶剂的质量比为1:2～20。
进一步的，所述交联剂选自戊二醛、二异氰酸化合物、N，N′-二环己基碳二亚胺(DCC)、1-乙基-3-(3-二甲基氨基丙基)碳二亚胺(EDC)、N-羟基琥珀酰亚胺(NHS)、二卤化二硝基苯。交联剂与量子点的质量比例为1:0.01～0.2。
进一步的，所述量子点扩散板的制备方法如下：
S1、制备改性防蓝光量子点；
S2、将改性防蓝光量子点与塑料颗粒混合，经熔融混合制备量子点母粒；
S3、将蓝光吸收或转化剂、光散射粒子、抗氧化剂分别与塑料颗粒混合，按照(0.5～5)：(0.5～20)：(0.5～5)：100的质量比例，经过熔融混合制备添加剂母粒；
S4、将所制备的红色和绿色量子点母粒、添加剂母粒、塑料颗粒按照(1～10):(1～10)：100的质量比例通过挤塑成型的方式制备量子点扩散板。
进一步的，所述改性防蓝光量子点占扩散板总的质量比例为：0.01％～2％。
进一步的，所述光散射粒子为纳米氧化硅、氧化钛、有机硅、硫酸钡、交联聚苯乙烯、碳酸钙、丙烯酸塑料中的一种或几种。光散射粒子占总的扩散板质量比为0.05％～3％。
进一步的，所述抗氧化剂为N，N’-六次甲基双一3(3,5二叔丁基-4羟基苯基)丙酰胺、1，3，5-三(3，5叔丁基-4-羟基苄基)三甲基苯、2、6二叔丁基对甲酚、β-(3，5二叔丁基-4一羟基苯基)丙酸十八醇酯、1，1，3三(2一甲基一4羟基一5叔丁基苯基)丁烷、1，3，5三甲基2，4，6三(3，5二叔丁基-4羟基苄基)苯、2,2’-甲撑双(4-乙基一6叔丁基苯酚)、1，3，5一三(3，5二叔丁基-4-羟基苯基)异氰酸酯、4-羟基十二烷酸酰替苯胺、4-羟基十八烷酸酰替苯胺、4，4’-硫代双(3-甲基-6-叔丁基苯酚)、2,2’-甲撑双(4-甲基-6-叔丁基苯酚)、4，4’-二叔辛基二苯胺、1，6六次甲基双(3，5二叔丁基-4-羟基苯基)丙酸酯、三(壬基代苯基)亚磷酸酯、三(2，4-二叔丁基苯基)亚磷酸酯、季戊四醇二亚磷酸双十八酯、四(2，4-二叔丁基苯基)4，4’-联苯撑二磷酸酯、硫代二丙酸二月桂酸酯中的一种或几种。抗氧剂占总的扩散板质量比例为0.05％～3％。
进一步的，所述熔融共混温度在100℃～300℃范围内。
进一步的，所述无机蓝光吸收或转化剂包括硅量子点、碳量子点、银纳米材料、钛酸锶、氧化锌、氧化镉、氧化铬中的一种或几种或组合。蓝光吸收或转化剂占扩散板总的质量比例为：0.05％～5％。
进一步的，所述蓝光吸收或转化剂位于量子点层中，减少了量子点扩散板的厚度，并且降低防蓝光膜的产线成本。
本方法相对现有技术具有以下有益效果：
1.本方法制备的防蓝光量子点和扩散板，可以有效解决量子点液晶显示中存在的有害短波蓝光发射问题。通过在量子点表面包覆有机蓝光转化剂，减少短波蓝光的同时，提升了量子点扩散板的器件效率。
2.本方法同样采用了蓝光吸收和转化剂，可有效防止短波蓝光通过扩散板，降低蓝光对人眼的伤害。
附图说明
图1是本发明所述防蓝光量子点扩散板制备流程图。
图2是本发明所述的量子点扩散板结构图。其中1为改性量子点，2为短波蓝光吸收或转化剂，3为光散射粒子和其他添加剂粒子。
图3是本发明所述的防蓝光量子点结构示意图。其中11为蓝光转化剂包覆层；12为量子点。
图4是实施例1所采用的一种香豆素衍生物分子结构(DOI：10.13451/j.sxu.ns.2019057)。对于420nm左右的蓝光具有强的吸收作用，产生520nm的绿光发射。
图5是实施例1中改性量子点扩散板和未改性量子点制备的扩散板的PL光谱对比。
图6是实施例2所采用的一种咔唑类分子结构(学位论文：基于咔唑及二苯胺衍生物的共振型热活化延迟荧光材料的合成及性质研究)。对于430nm左右的蓝光具有强的吸收作用，产生470nm左右的蓝光发射。
图7是实施例3所采用的一种喹啉类衍生物分子结构(学位论文：8-羟基喹啉类锌配合物/共价三嗪骨架材料的制备与性质研究)。对于400nm左右的蓝光具有强的吸收作用，产生620nm的红光发射。
具体实施方式
一种改性防蓝光量子点和量子点扩散板及制备方法包括两个部分，第一部分，改性量子点的制备过程包括以下过程：
S1、在反应气氛中，将量子点均匀分散在有机溶剂配成溶液A，将蓝光转化剂分散于有机溶剂中配成溶液B；
S2、将量子点溶液A和蓝光转化剂溶液B分别注入反应有机溶剂中，再加入交联剂，密闭反应器，保持反应气氛，搅拌1～12h，使蓝光转化剂和量子点充分反应，转化剂分子包覆在量子点表面；
S3、将反应完成的混合溶液通过醇类溶剂洗涤后干燥，去除有机溶剂，得到表面包覆有短波蓝光转化剂的改性量子点。
第二部分，量子点扩散板的制备方法如下：
S1、制备改性防蓝光量子点；
S2、将改性防蓝光量子点与塑料颗粒混合，经熔融混合制备红色和绿色量子点母粒；
S3、将蓝光吸收或转化剂、光散射粒子、抗氧化剂分别与塑料颗粒混合，按照(0.5～5)：(0.5～20)：(0.5～5：100)的质量比例，经过熔融混合制备添加剂母粒；
S4、将所制备的红色和绿色量子点母粒、添加剂母粒、塑料颗粒按照(1～10):(1～10)：100的质量比例通过挤塑成型的方式制备量子点扩散板。
下面结合具体实施例，进一步阐述本专利。
实施例1
(1)改性量子点的制备：在氮气环境下，分别称量0.15g CdSe/ZnS红色量子点溶于2mL甲苯中、0.1g香豆素衍生物固体粉末溶于2mL四氢呋喃中，并充分搅拌使溶质分散，制成红色量子点溶液和蓝光转化剂溶液；保持氮气气氛，将量子点溶液和蓝光转化剂溶液加入30mL乙醇中，并降温至10℃，充分搅拌3h，避光反应，使香豆素衍生物与量子点表面配体产生交换；将反应后的溶液用乙醇洗涤3次，保留沉淀，60℃真空干燥6h，获得红色改性量子点粉末。
(2)量子点扩散板的制作：将制备好的改性0.2g红色量子点和同样方法按比例放大制备的1.8g CdZnSeS/ZnS改性绿色量子点分别与1kg聚甲基丙烯酸甲酯(PMMA)塑料颗粒混合造粒，获得量子点母粒；造粒设置温度为200～270℃，8个温区的温度梯度为10℃；将5gTiO2光散射粒子和5g抗氧剂季戊四醇二亚磷酸双十八酯、5g硅量子点加入到1kg PMMA塑料颗粒中，混合造粒，制备添加剂母粒，温度设置为200～270℃，8个温区的温度梯度为10℃；分别取2g红色改性量子点母粒和20g绿色改性量子点母粒、50g添加剂母粒、1kg PMMA塑料颗粒，经挤出成型制备防蓝光量子点扩散板。
附图5展示了通过实施例1制备的改性量子点扩散板和未改性量子点制备的扩散板的光致发光图谱的对比。从图中可以看出，在添加同样的无机蓝光吸收或转化剂的情况下，改性后的量子点扩散板显著减少了有害蓝光发射的同时，增加了绿光的占比，并且增强了红光部分。这是因为有机蓝光吸收剂的包覆增加了量子点的蓝光吸收率(增加约35％)，尤其是420nm左右的有害蓝光，并且将其转化成了与绿色量子点波长相近的光。说明改性量子点有效降低了有害蓝光的发射，并且提升了量子点的转化效率(增加约20％)。
实施例2
(1)改性量子点的制备：分别称量0.18g CdSe/CdS红色量子点溶于2mL甲苯中、0.1g咔唑和二苯胺衍生物溶于1mL甲苯中，并充分搅拌使溶质分散；将量子点溶液和转化剂溶液加入25mL甲苯中，并加入0.05g交联剂1-乙基-3-(3-二甲基氨基丙基)碳二亚胺(EDC)粉末，避光反应3h，使转化剂充分与量子点表面配体偶联；将反应溶液用二氯甲烷洗涤纯化，保留下层沉淀，获得改性红色量子点胶状物。
(2)量子点扩散板的制作：将制备好的改性0.2g红色量子点和同样方法制备的2gCdZnSeS/ZnS改性绿色量子点分别与1kg聚苯乙烯(PS)塑料颗粒混合造粒，获得量子点母粒；造粒设置温度为190～260℃,8个温区的温度梯度为10℃；将5g TiO2光散射粒子和5g抗氧剂β-(3，5二叔丁基-4一羟基苯基)丙酸十八醇酯、5g氧化铬加入到1kg PS塑料颗粒中，混合造粒，制备添加剂母粒，温度设置为190～260℃，8个温区的温度梯度为10℃；分别取2g红色改性量子点母粒和20g绿色改性量子点母粒、50g添加剂母粒、1kg PS塑料颗粒，经挤出成型制备防蓝光量子点扩散板。
实施例3
(1)改性量子点的制备：分别称量1g CdZnSeS绿色合金化量子点溶于5m甲苯中、0.4g喹啉类衍生物(2-[2-(4-氰基苯基)乙烯基]-8-羟基-喹啉)溶于20mL二氯甲烷中，并充分搅拌使溶质分散均匀；将量子点溶液和喹啉类衍生物溶液加入100mL去离子水中，避光密封反应瓶，搅拌反应3h，使配体交换反应完全；用二氯甲烷和水的混合溶液三次洗涤，经高速离心获得产物；将产物在60℃真空干燥箱中干燥8h，获得改性量子点粉体。
(2)量子点扩散板的制作：取制备好的改性1.2g绿色改性量子点和同样方法制备的0.15g改性CdSe/CdS红色量子点分别与1kg聚碳酸酯(PC)塑料颗粒混合造粒，获得量子点母粒；造粒设置温度为240～310℃，8个温区的温度梯度为10℃；将5g TiO2光散射粒子和5g抗氧化剂季戊四醇二亚磷酸双十八酯、5g钛酸锶加入到1kg PC塑料颗粒中，混合造粒，制备添加剂母粒，温度设置为240～310℃，；分别取2g红色改性量子点母粒和20g绿色改性量子点母粒、50g添加剂母粒、1kg PC塑料颗粒，经挤出成型制备防蓝光量子点扩散板。
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。
Claims (10)
1.一种改性防蓝光量子点的制备方法，其特征在于，包括以下步骤：
S1、在反应气氛中，将量子点均匀分散在有机溶剂中配成溶液A，将蓝光转化剂分散于有机溶剂中配成溶液B；
S2、将量子点溶液A和蓝光转化剂溶液B分别注入反应有机溶剂中，再加入交联剂，密闭反应器，保持反应气氛，搅拌1～12h，使蓝光转化剂和量子点充分反应，转化剂分子包覆在量子点表面；
S3、将反应完成的混合溶液通过醇类溶剂洗涤后干燥，去除有机溶剂，得到表面包覆有短波蓝光转化剂的改性量子点。
2.根据权利要求1所述的制备方法，其特征在于，所述蓝光转化剂选自香豆素类、喹啉类、吡唑啉酮类、联苯类、萘酚类、芳胺类有机染料和稀土配合物，发光波长与量子点发光波长相近，同时蓝光转化剂中包含有吡啶、巯基、胺、膦、羧基或氨基基团；量子点与蓝光转化剂质量比例为1:0.2～10。
3.根据权利要求1所述的制备方法，其特征在于，所述反应气氛为空气气氛、氮气气氛或惰性气体气氛；所述量子点为Cd、Zn、S、Se、Sn、In、P、Cu中的两种或多种元素组成的量子点或者钙钛矿量子点；步骤S2中包覆过程的反应温度为10℃～160℃。
4.根据权利要求1所述的制备方法，其特征在于，溶液A中有机溶剂为芳香烃类，反应有机溶剂为醇类；溶液A中量子点与有机溶剂的质量比为1:1～10；溶液B中蓝光转化剂与有机溶剂的质量比为1:2～20。
5.根据权利要求1所述的制备方法，其特征在于，所述交联剂选自戊二醛、二异氰酸化合物、N,N′-二环己基碳二亚胺、1-乙基-3-（3-二甲基氨基丙基）碳二亚胺、N-羟基琥珀酰亚胺、二卤化二硝基苯中的一种；交联剂与量子点的质量比例为1:0.01～0.2。
6.一种利用权利要求1中所述的改性防蓝光量子点制备量子点扩散板的方法，其特征在于，包括以下步骤：
（1）将改性防蓝光量子点与塑料颗粒混合，经熔融混合制备量子点母粒；
（2）将蓝光吸收或转化剂、光散射粒子、抗氧化剂与塑料颗粒混合，按照（0.5～5）：（0.5～20）：（0.5～5）：100的质量比例，经过熔融混合制备添加剂母粒；
（3）将制备的量子点母粒、添加剂母粒、塑料颗粒按照（1～10）:（1～10）：100的质量比例通过挤塑成型的方式制备量子点扩散板。
7.根据权利要求6所述的制备方法，其特征在于，所述改性防蓝光量子点占扩散板总的质量比例为：0.01%～2%；所述光散射粒子为纳米氧化硅、氧化钛、有机硅、硫酸钡、交联聚苯乙烯、碳酸钙、丙烯酸塑料中的一种或几种，光散射粒子占扩散板总的质量比例为：0.05%～3%。
8.根据权利要求6所述的制备方法，所述抗氧化剂为N，N‘-六次甲基双一3(3,5二叔丁基-4羟基苯基)丙酰胺、1，3，5-三(3，5叔丁基-4-羟基苄基)三甲基苯、2、6二叔丁基对甲酚、β-(3，5二叔丁基-4一羟基苯基)丙酸十八醇酯、1，1，3三(2一甲基一4羟基一5叔丁基苯基)丁烷、1，3，5三甲基2，4，6三(3，5二叔丁基-4羟基苄基)苯、2,2’-甲撑双(4-乙基一6叔丁基苯酚)、1，3，5一三(3，5二叔丁基-4-羟基苯基)异氰酸酯、4-羟基十二烷酸酰替苯胺、4-羟基十八烷酸酰替苯胺、4，4’-硫代双(3-甲基-6-叔丁基苯酚)、2,2’-甲撑双(4-甲基-6-叔丁基苯酚)、 4，4’-二叔辛基二苯胺、1，6六次甲基双(3，5二叔丁基-4-羟基苯基)丙酸酯、三(壬基代苯基)亚磷酸酯、三(2，4-二叔丁基苯基)亚磷酸酯、季戊四醇二亚磷酸双十八酯、四(2，4-二叔丁基苯基)4，4’-联苯撑二磷酸酯、硫代二丙酸二月桂酸酯中的一种或几种；抗氧剂占扩散板总的质量比例为：0.05%～3%。
9.根据权利要求6所述的制备方法，所述熔融共混温度在100℃～300℃范围内。
10.根据权利要求6所述的制备方法，所述蓝光吸收或转化剂包括硅量子点、碳量子点、银纳米材料、钛酸锶、氧化锌、氧化镉、氧化铬中的一种或几种组合；蓝光吸收或转化剂占扩散板总的质量比例为：0.05%～5%；所述蓝光吸收或转化剂位于量子点层中。
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