CN112140677A - 钙钛矿量子点膜 - Google Patents

钙钛矿量子点膜 Download PDF

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CN112140677A
CN112140677A CN202011030122.7A CN202011030122A CN112140677A CN 112140677 A CN112140677 A CN 112140677A CN 202011030122 A CN202011030122 A CN 202011030122A CN 112140677 A CN112140677 A CN 112140677A
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quantum dot
perovskite quantum
dot film
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喻四海
童建宇
施法宽
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Kunshan Bye Polymer Material Co ltd
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Abstract

本发明公开了钙钛矿量子点膜，包括依次设置的第一阻水层、第一阻氧层、量子点层、第二阻氧层、第二阻水层；所述量子点层由0.5～10重量份的钙钛矿量子点，75～95重量份的热塑性弹性体、2～25重量份的扩散粒子与0.02～10重量份的抗氧化剂构成，所述阻水层由PP构成，所述阻氧层由EVOH构成。本发明钙钛矿量子点膜总厚度可以低至40um，满足手机、平板等超薄液晶显示屏对量子点膜厚度的要求。具有较高的荧光量子产率，极窄的半峰宽。具有超高的光稳定性、高温高湿稳定性。作为液晶显示器背光模组的下转换荧光材料，NTSC色域最高可达105％，可应用于广色域、高亮度、高稳定性液晶显示器。

Description

钙钛矿量子点膜
技术领域
本发明属于钙钛矿量子点膜技术领域，具体涉及钙钛矿量子点膜。
背景技术
钙钛矿量子点膜由于其出色的荧光性能，可作为广色域液晶显示器(LCD)背光模组的光学转换膜，具有巨大的市场潜力。由于钙钛矿量子点对水氧敏感，为了保护钙钛矿量子点免受周围环境中水和氧的影响，通常将钙钛矿量子点分散在聚合物材料中，并且用高阻隔性的光学薄膜保护起来。通常，制备钙钛矿量子点薄膜需要先通过热注射法在有机溶剂中合成钙钛矿量子点，然后通过离心、分离纯化，再将纯化后的量子点均匀地混合到UV胶水或高分子树脂中，然后将含有量子点的胶水或高分子树脂材料涂覆在水氧阻隔膜上，并用另一张水氧阻隔膜覆盖，采用UV或热固化的方法固化树脂材料，得到三明治结构的钙钛矿量子点膜。然而，由于在分离和纯化过程中过量去除钙钛矿量子点的表面配体，造成钙钛矿量子点表面配体钝化不充分，常常导致所得钙钛矿量子点膜的荧光效率(PL QY)较低且光稳定性较差。此外，这类钙钛矿量子点膜要求使用阻隔性较高的水氧阻隔膜才能保证量子点膜的老化稳定性，大大增加了量子点膜的生产成本。并且，采用涂布的方式制备量子点膜对设备及工艺的要求较高，尤其是在制备低厚度量子点膜时无法满足要求，而当前手机、平板等液晶显示屏等对光学薄膜厚度有上限要求，部分产品要求厚度小于55um，因此，有必要探索一种简便而高效的方法制备钙钛矿量子点膜，既能有效制备超薄产品，同时确保其在恶劣的老化条件下，特别是在光照老化及高温高湿老化条件下，具有高效率的发光和良好的稳定性。
发明内容
为解决上述背景技术中提出的问题。本发明提供了钙钛矿量子点膜。
为实现上述目的，本发明提供如下技术方案：钙钛矿量子点膜，包括依次设置的第一阻水层、第一阻氧层、量子点层、第二阻氧层、第二阻水层；所述量子点层由0.5～10重量份的钙钛矿量子点，75～95重量份的热塑性弹性体、2～25重量份的扩散粒子与0.02～10重量份的抗氧化剂构成，所述阻水层由PP构成，所述阻氧层由EVOH构成。
优选的，所述量子点膜的厚度为40～200um。
优选的，所述量子点层的厚度所占层比为10％～40％。
优选的，所述第一阻水层及第二阻水层的厚度占层比为20％～80％。
优选的，所述第一阻氧层及第二阻氧层厚度占层比为10％～40％。
与现有技术相比，本发明的有益效果是：
钙钛矿量子点膜总厚度可以低至40um，满足手机、平板等超薄液晶显示屏对量子点膜厚度的要求。钙钛矿量子点膜具有较高的荧光量子产率，极窄的半峰宽。钙钛矿量子点膜具有超高的光稳定性、高温高湿稳定性。钙钛矿量子点膜作为液晶显示器背光模组的下转换荧光材料，NTSC色域最高可达105％，可应用于广色域、高亮度、高稳定性液晶显示器。
附图说明
图1为钙钛矿量子点膜的结构示意图。
图2为钙钛矿量子点膜的性能测试结果图。
图中：1、第一阻水层，2、第一阻氧层，3、量子点层，4、第二阻氧层，5、第二阻水层。
具体实施方式
以下结合附图和具体实施例对本发明作具体的介绍，为了方便说明，将荧光发射峰表示为PL，荧光量子效率表示为PLQY，半峰宽表示为FWHM。
实施例1：一种钙钛矿量子点膜
1)钙钛矿量子点聚合物粒子的制备
将4.0mmol的PbBr2、油酸(32mmol)、油胺(32mmol)装入10L搅拌槽中，在120℃下真空干燥30min以除去原料中的水分。在氮气保护下将所得混合物加热至150℃直至PbBr2完全溶解。然后将温度升至180℃加入4kg热塑性弹性体SEBS G1657M，待完全熔融后，注入0.16mmol油酸铯前驱体。随后分别0.1kg二氧化钛扩散粒子与0.01kg抗氧化剂1010，充分搅拌后，将均匀混合后的产物经过真空脱泡后加入到双螺杆挤出机，挤出产物经冷却、造粒，即得到所需的钙钛矿量子点聚合物粒子；
2)钙钛矿量子点膜的制备
将PP粒子、EVOH粒子及步骤1)所制备的钙钛矿量子点聚合物粒子、EVOH粒子以及PP粒子分别通过真空进料系统，加入到A挤出机、B挤出机和C挤出机，D挤出机，E挤出机，分别得到第一阻水PP层1、第一阻氧层2、量子点层3、第二阻氧层4、第二阻水PP层5，设定层比25％:15％:20％:15％:25％，通过流延机的挤出机挤出，并通过流延机的模头分配器合并在一起。即可得到钙钛矿量子点膜，钙钛矿量子点膜的总厚度在50um。
实施例2：一种钙钛矿量子点膜
1)钙钛矿量子点聚合物粒子的制备
将4.0mmol的PbBr2、油酸(32mmol)、油胺(32mmol)装入10L搅拌槽中，在120℃下真空干燥30min以除去原料中的水分。在氮气保护下将所得混合物加热至150℃直至PbBr2完全溶解。然后将温度升至180℃加入4kg亚克力系嵌段共聚物LA2330，待完全熔融后，注入0.16mmol油酸铯前驱体。随后分别加入0.1kg二氧化钛扩散粒子与0.01kg抗氧化剂1010，充分搅拌后，将均匀混合后的产物经过真空脱泡后加入到双螺杆挤出机，挤出产物经冷却、造粒，即得到所需的钙钛矿量子点聚合物粒子；
2)钙钛矿量子点膜的制备
将PP粒子、EVOH粒子及步骤1)所制备的钙钛矿量子点聚合物粒子、EVOH粒子以及PP粒子分别通过真空进料系统，加入到A挤出机、B挤出机和C挤出机，D挤出机，E挤出机，设定层比30％:10％:20％:10％:30％，通过流延机的挤出机挤出，并通过流延机的模头分配器合并在一起，即可得到钙钛矿量子点膜，钙钛矿量子点膜的总厚度在50um。
实施例3：一种钙钛矿量子点膜
重复实施例1，不同之处仅在步骤1)钙钛矿量子点聚合物粒子的制备中，热塑性弹性体为EVA，牌号为Levamelt@686。
实施例4：一种钙钛矿量子点膜
重复实施例1，不同之处仅在步骤1)钙钛矿量子点聚合物粒子的制备中，抗氧化剂1010的加入量为0.02Kg。
实施例5：一种钙钛矿量子点膜
重复实施例2，不同之处仅在步骤1)钙钛矿量子点聚合物粒子的制备中，亚克力系嵌段共聚物LA2330的加入量为8Kg。步骤2)钙钛矿量子点膜的制备中，钙钛矿量子点膜的总厚度为100um。
实施例6：一种钙钛矿量子点膜
重复实施例1，不同之处仅在步骤1)钙钛矿量子点聚合物粒子的制备中，SEBSG1657M加入量为3.2Kg。步骤2)钙钛矿量子点膜的制备中，钙钛矿量子点膜的总厚度为40um；
实施例7：一种钙钛矿量子点膜
重复实施例2，不同之处仅在步骤1)钙钛矿量子点聚合物粒子的制备中，亚克力系嵌段共聚物LA2330的加入量为3.2Kg。步骤2)钙钛矿量子点膜的制备中，钙钛矿量子点膜的总厚度为40um；
可见光透过率及雾度测试：
对实施例1、2、3、4、5、6、7中所制得的钙钛矿量子点膜的可见光透过率及雾度进行测试。每个实施例平行测试6个样品后，对测试结果求平均值得到可见光透过率及雾度。各实施例样品的可见光透过率及雾度测试结果具体见图2。
荧光性能测试：
在450nm的激发波长下，对实施例1、2、3、4、5、6、7中所制得的钙钛矿量子点膜的PL、FWHM、PLQY进行测试。每个实施例平行测试6个样品后，对测试结果求平均值得到最终结果。各实施例样品的PL、FWHM、PLQY测试结果具体见图2。
高温高湿老化测试：
将各钙钛矿量子点膜样品在60℃、90％相对湿度老化箱中老化1000小时后，在450nm的特定波长下，测定各样品的PLQY。每个实施例平行测试6个样品后，对测试结果求平均值得到薄膜高温高湿老化后的荧光效率。各实施例样品的高温高湿老化测试结果具体见图2。
光老化测试:
将各钙钛矿量子点膜样品在45℃蓝光老化箱中老化1000小时后，在450nm的特定波长下，测定各样品的PLQY。每个实施例平行测试6个样品后，对测试结果求平均值得到薄膜光照老化后的荧光效率。各实施例样品的光照老化测试结果具体见图2。
NTSC色域测试：
使用显示器颜色分析仪(型号：CA 310)测量含有钙钛矿量子点膜的LCD原型机的NTSC色域，工作温度为室温。每个实施例平行测试6个样品后，对测试结果求平均值得到NTSC色域。各实施例样品的NTSC色域测试结果具体见图2。
实验结果显示，本发明钙钛矿量子点膜总厚度可以低至40um，满足手机、平板等超薄液晶显示屏对量子点膜厚度的要求。钙钛矿量子点膜具有较高的荧光量子产率，极窄的半峰宽。钙钛矿量子点膜具有超高的光稳定性、高温高湿稳定性。钙钛矿量子点膜作为液晶显示器背光模组的下转换荧光材料，NTSC色域最高可达105％，可应用于广色域、高亮度、高稳定性液晶显示器。
以上显示和描述了本发明的基本原理、主要特征和优点。本行业的技术人员应该了解，上述实施例不以任何形式限制本发明，凡采用等同替换或等效变换的方式所获得的技术方案，均落在本发明的保护范围内。

Claims (5)

1.钙钛矿量子点膜，其特征在于：包括依次设置的第一阻水层、第一阻氧层、量子点层、第二阻氧层、第二阻水层；所述量子点层由0.5～10重量份的钙钛矿量子点，75～95重量份的热塑性弹性体、2～25重量份的扩散粒子与0.02～10重量份的抗氧化剂构成，所述阻水层由PP构成，所述阻氧层由EVOH构成。
2.根据权利要求1所述的钙钛矿量子点膜，其特征在于，所述量子点膜的厚度为40～200um。
3.根据权利要求1所述的钙钛矿量子点膜，其特征在于，所述量子点层的厚度所占层比为10％～40％。
4.根据权利要求1所述的钙钛矿量子点膜，其特征在于，所述第一阻水层及第二阻水层的厚度占层比为20％～80％。
5.根据权利要求1所述的钙钛矿量子点膜，其特征在于，所述第一阻氧层及第二阻氧层厚度占层比为10％～40％。
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CN115284697A (zh) * 2022-08-09 2022-11-04 烟台布莱特光电材料有限公司 一种防潮耐热的量子点荧光薄膜及其应用

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