CN109638169A - 有机阻隔膜、有机阻隔膜的制备方法以及量子点器件 - Google Patents

有机阻隔膜、有机阻隔膜的制备方法以及量子点器件 Download PDF

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CN109638169A
CN109638169A CN201811267839.6A CN201811267839A CN109638169A CN 109638169 A CN109638169 A CN 109638169A CN 201811267839 A CN201811267839 A CN 201811267839A CN 109638169 A CN109638169 A CN 109638169A
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layer
barrier film
organic barrier
oxidation prevention
quantum dot
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CN109638169B (zh
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王海琳
胡奇乐
康永印
叶佳敏
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Najing Technology Corp Ltd
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Najing Technology Corp Ltd
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Priority to CN201811267839.6A priority Critical patent/CN109638169B/zh
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Priority to PCT/CN2019/113738 priority patent/WO2020088418A1/zh
Priority to US17/285,920 priority patent/US20210347957A1/en
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Abstract

本发明公开了有机阻隔膜、有机阻隔膜的制备方法以及量子点器件。其中，有机阻隔膜包括由外到内依次设置基材层、粘结层以及阻氧层，阻氧层包括聚乙烯醇，粘结层与阻氧层之间形成化学交联。本发明的有益效果在于：粘结层与阻氧层之间形成化学交联，提高了阻氧层在基材层表面的附着力。

Description

有机阻隔膜、有机阻隔膜的制备方法以及量子点器件
技术领域
本发明涉及量子点材料领域，尤其涉及有机阻隔膜、有机阻隔膜的制备方法以及量子点器件。
背景技术
目前，量子点合成技术已经相对成熟，量子点的效率和稳定性均到达了产业化水平，但是量子点独特的表面效应也决定了其对水汽和氧气的敏感性，水汽和氧气会破坏量子点表面的配体，降低量子点的效率。因此，量子点需要在隔水隔氧的条件下才能发挥其高发光效率和稳定性。目前量子点主流的使用方法包括量子点管和量子点膜，量子点管是将量子点材料封装在玻璃管中，而量子点膜是利用阻隔膜将量子点材料包覆在中间形成三明治结构。由于量子点膜材料的生产工艺简单、可弯折、且能显著提高液晶显示的色域和颜色饱和度，量子点膜逐渐成为量子点电视的热点材料。
然而，量子点膜材料中除了极为重要的量子点材料以外，阻隔膜也至关重要。目前主流的阻隔膜的制备方法一般为：先在聚酯膜的基材上通过蒸镀、磁控溅射或真空化学沉积等方法铺设无机氧化物层，再在无机氧化物层上涂覆有机物层。同时包括有机物层和无机氧化物层的阻隔膜具有较好的阻隔性能。这种阻隔膜的工艺较为复杂，成本较高，而且阻隔膜在卷曲过程中易导致无机氧化物层破裂进而失去阻隔性能。
发明内容
为了克服现有技术的不足，本发明的目的在于提供一种有机阻隔膜及其制备方法，制得的有机阻隔膜具有良好的阻氧阻水性能。
根据本发明的一个方面，本发明提供一种有机阻隔膜，包括由外到内依次设置的基材层、粘结层以及阻氧层，所述阻氧层包括聚乙烯醇，所述粘结层与所述阻氧层之间形成化学交联。
进一步地，所述基材层的外侧设置有疏水层或磨砂层，所述疏水层包括以下一种或多种疏水聚合物：聚偏二氯乙烯、聚偏氟乙烯、聚四氟乙烯、聚三氟氯乙烯，所述磨砂层包括载体以及透明颗粒。
进一步地，制备所述粘结层的原料包括：高分子粘结剂、交联剂和螯合剂，所述高分子粘结剂选自聚酯、聚氨酯或聚丙烯酸酯中的一种或多种，所述高分子粘结剂包括以下基团中的至少一种：羟基、羧基、氨基，所述螯合剂与所述聚乙烯醇形成化学键交联。
进一步地，所述螯合剂选自以下一种或多种：硼酸、硼酸钠、丙烯酸钠、钛酸酯。
进一步地，所述交联剂选自以下一种或多种：聚碳二亚胺、氮丙啶、甲醚化六羟甲基三聚氰胺。
进一步地，所述高分子粘结剂的玻璃化转变温度小于50℃。
根据本发明的另一方面，本发明提供一种有机阻隔膜的制备方法，包括以下步骤：
提供基材层；
在所述基材层的第二侧设置粘结层，在所述粘结层上设置阻氧层，所述阻氧层包括聚乙烯醇，所述粘结层与所述阻氧层之间形成化学交联。
进一步地，所述粘结层的制备方法包括：将包括高分子粘结剂、交联剂和螯合剂的混合物设置于所述基材层的第二侧，所述高分子粘结剂选自聚酯、聚氨酯、聚丙烯酸酯中的一种或多种，所述高分子粘结剂包括以下基团中的至少一种：羟基、羧基、氨基，所述螯合剂与所述聚乙烯醇形成化学键交联。
进一步地，所述螯合剂选自以下一种或多种：硼酸、硼酸钠、丙烯酸钠、钛酸酯；优选地，所述螯合剂在所述混合物中的质量百分数为1％～10％。
进一步地，所述交联剂选自以下一种或多种：聚碳二亚胺、氮丙啶、甲醚化六羟甲基三聚氰胺。
进一步地，在所述基材层的第一侧设置疏水层或磨砂层。
进一步地，所述阻氧层的制备方法包括：将包括聚乙烯醇、水、消泡剂和流平剂的混合物，设置于所述粘结层。
根据本发明的另一方面，本发明提供一种量子点器件，包括量子点层以及设置在所述量子点层一侧或两侧的本发明的所述有机阻隔膜，所述有机阻隔膜的所述阻氧层设置在靠近所述量子点层的内侧。
相比现有技术，本发明的有益效果在于：
(1)聚乙烯醇很难在大部分聚酯膜片的表面有效附着，本发明通过粘结层将包括聚乙烯醇的阻氧层与基材层粘结，粘结层与阻氧层之间形成化学交联，提高了阻氧层在基材层表面的附着力；
(2)聚乙烯醇之所以具有优良的气体阻隔性，一方面聚乙烯醇规整的分子链使得其结晶度很高，另一方面是由于大量的羟基氢键使得分子之间形成致密的交联网络，因此其对大多数气体有超强的阻隔性能，但是，其交联的氢键容易受到水汽的破坏，从而影响阻氧层的阻隔性，因此本发明在基材层的外侧设置了疏水层，疏水层可以有效防止水汽在有机阻隔膜表面的吸附和溶解，降低了体系的水汽渗透，此外，基材层也具有一定的阻水功能，通过疏水层与基材层的组合，可以大幅降低渗透到阻氧层的水汽，使阻氧层的聚乙烯醇保持良好的阻隔性。
附图说明
图1为本发明的有机阻隔膜的一个实施例的示意图；
图2为本发明的有机阻隔膜的另一个实施例的示意图；
图3为本发明的有机阻隔膜的再一个实施例的示意图；
图中：1、疏水层；2、基材层；3、粘结层；4、阻氧层；5、磨砂层。
具体实施方式
下面，结合具体实施方式，对本发明做进一步描述，需要说明的是，在不相冲突的前提下，以下描述的各实施例之间或各技术特征之间可以任意组合形成新的实施例。
如图1所示，本发明提供一种有机阻隔膜，其包括由外到内依次设置的基材层2、粘结层3以及阻氧层4，阻氧层4包括聚乙烯醇，粘结层3与阻氧层4之间形成化学交联。
基材层2的主要作用是保护阻氧层4。粘结层3用于提高基材层2与阻氧层4之间的粘结性，由于阻氧层4的聚乙烯醇与一般的粘结剂粘结性较差，因此本发明使粘结层3与阻氧层4之间形成化学交联，以提高阻氧层4与粘结层3的粘结性。
在一些实施例中，如图2所示，有机阻隔膜还包括疏水层1，疏水层1设置在基材层2的外侧，疏水层1包括以下一种或多种疏水聚合物：聚偏二氯乙烯、聚偏氟乙烯、聚四氟乙烯、聚三氟氯乙烯。疏水层1可以有效防止水汽在有机阻隔膜表面的吸附和溶解，降低了水汽向内渗透。
在另一些实施例中，如图3所示，有机阻隔膜还包括磨砂层5，磨砂层5设置在基材层2的外侧，磨砂层5包括载体和透明颗粒，载体选自环氧树脂、丙烯酸酯树脂、有机硅树脂与聚氨酯树脂中的一种或多种，透明颗粒的材料选自聚丙烯酸酯、聚苯乙烯、聚丙烯、聚碳酸酯、甲基丙烯酸甲酯-丁二烯-苯乙烯三元共聚物与苯乙烯-丙烯腈共聚物中的一种或多种。磨砂层5有利于提高有机阻隔膜的进光率。
在一些实施例中，基材层2的材料为聚对苯二甲酸乙二醇酯(PET)。
在一些实施例中，粘结层3的原料包括：高分子粘结剂、交联剂和螯合剂，其中高分子粘结剂选自聚酯、聚氨酯或聚丙烯酸酯中的一种或多种，高分子粘结剂包括以下基团中的至少一种：羟基、羧基、氨基，上述螯合剂与聚乙烯醇形成化学键交联。
在一些实施例中，为了提高高分子粘结剂与聚乙烯醇的粘结力，高分子粘结剂中的羟基、羧基、氨基等极性基团的数量要多一些，另外，这些极性基团能帮助液态高分子粘结剂在聚乙烯醇层上的铺展，实现更大面积的粘结。当高分子粘结剂极性基团多至表现出一定的亲水性时，螯合剂和交联剂需要能较均匀地分散在液态高分子粘结剂中，优选螯合剂和交联剂能溶解在液态的高分子粘结剂中，从而实现均匀的粘结和可靠的粘结。
螯合剂的主要作用是在粘结层3与阻氧层4之间形成桥梁，从而提高了粘结层3与阻氧层4之间的粘结力。
在一些实施例中，螯合剂选自以下一种或多种：硼酸、硼酸钠、丙烯酸钠、钛酸酯。一方面，螯合剂与高分子粘结剂之间产生一定的相互作用，使得螯合剂不易与高分子粘结剂分离，螯合剂与高分子粘结剂之间的相互作用可以是结晶嵌入，还可以是螯合剂与高分子粘结剂之间发生化学交联，也可以是其他的形式；另一方面螯合剂与聚乙烯醇形成化学键交联，从而使粘结层3与阻氧层4之间形成化学交联，提高了粘结层3与阻氧层4之间的粘结力。
以螯合剂为硼酸为例，螯合剂与聚乙烯醇之间适于形成如下所示的化学结构：
螯合剂在粘结层3中的质量百分数为1％～10％，且随着螯合剂添加量的增加，基材层2与阻氧层4之间的剥离力大幅增加。
交联剂的主要作用是提高粘结层3的内聚力，从而提高粘结层3的耐水性和耐溶剂性。交联剂选自以下一种或多种：聚碳二亚胺、氮丙啶、甲醚化六羟甲基三聚氰胺。
在一些实施例中，高分子粘结剂选自含羟基的聚酯、含羟基的聚氨酯、聚丙烯酸酯中的一种或多种，且高分子粘结剂的玻璃化转变温度小于50℃。高分子粘结剂选用玻璃化转变温度低、损耗模量较大的乳液，有助于提高其与PET基材层2的初粘力。
本发明还提供一种有机阻隔膜的制备方法，包括以下步骤：
提供基材层2；
在基材层2的第二侧设置粘结层3，在粘结层3上设置阻氧层4，阻氧层4包括聚乙烯醇，粘结层3与阻氧层4之间形成化学交联。
在一些实施例中，粘结层3的制备方法包括：将包括高分子粘结剂、交联剂、螯合剂的混合物设置于基材层2的第二侧。
在一些实施例中，上述高分子粘结剂选自聚酯、聚氨酯、聚丙烯酸酯中的一种或多种，上述高分子粘结剂包括以下基团中的至少一种：羟基、羧基、氨基，螯合剂与聚乙烯醇形成化学键交联。
在一些实施例中，上述制备粘结层3时，混合物中还包括流平剂与消泡剂。
螯合剂选自以下一种或多种：硼酸、硼酸钠、丙烯酸钠、钛酸酯，螯合剂在上述混合物中的质量百分数为1％～10％。交联剂选自以下一种或多种：聚碳二亚胺、氮丙啶、甲醚化六羟甲基三聚氰胺。
在一些实施例中，在基材层2的第一侧设置疏水层1或磨砂层5。
疏水层1的制备方法包括：将包括疏水聚合物、散射粒子、流平剂、消泡剂的混合物设置于基材层2的第一侧。磨砂层5的制备方法为现有技术，本发明不再详述。
本发明还提供一种量子点器件，其包括量子点层以及设置在量子点层一侧或两侧的上述有机阻隔膜，有机阻隔膜的阻氧层4设置在靠近量子点层的内侧。在一些实施例中，疏水层1或磨砂层5设置在远离量子点层的外侧。
在一些实施例中，量子点层与阻氧层4之间还设置用于提高粘结性的第二粘结层。
阻氧层原料通过以下步骤制备：取10g聚合度1700的完全水解型聚乙烯醇加入90g去离子水中，于95℃下加热1h，冷却后加入适量流平剂及消泡剂，配制成固含量10％的PVA涂布液。
疏水层原料通过以下步骤制备：将PVDC乳液(苏威193D)稀释至30％固含量，加入10％粒径5μm左右的PMMA扩散粒子以及适量润湿分散剂、消泡剂、流平剂，防沉剂，超声搅拌30min，得阻水乳液涂布液。
【实施例1】
将丙烯酸、丙烯酸丁酯、丙烯酸羟乙酯和定量的去离子水加入带搅拌和冷凝回流管的三口烧瓶中，通氮气10min，搅拌并升温至75℃，加入定量的过硫酸钾水溶液，保温8h，降温至30℃出料，测定固含量，然后加入质量百分数为0.2％流平剂、0.1％的消泡剂、0.5％的聚碳二亚胺和3％的硼酸，得丙烯酸酯粘结乳液。
将上述丙烯酸酯粘结乳液涂布于厚度为100μm的PET基材一侧，于120℃烘烤固化3min，形成厚度为1μm的粘结层，再在粘结层上涂布一层前述阻氧层原料，120℃烘烤固化3min，形成厚度为5μm的阻氧层。得有机阻隔膜，测得其氧气透过率为0.323cm3/m2·24h·0.1MPa，水蒸气透过率为0.548g/m2·24h，百格法测试涂层附着力为1级。
将上述有机阻隔膜的阻氧层上涂布自制的红绿量子点UV胶水，准备另一片相同的有机阻隔膜，并两片相对贴合成三明治结构，UV固化后即得量子点膜。
【实施例2】
将脱水处理过的聚已二酸乙二醇酯、二环己基甲烷二异氰酸酯加入带搅拌和冷凝回流管的三口烧瓶中，通氮气10min，搅拌并升温至65℃，加入二月桂酸二丁基锡催化剂，保温15min，再升温至85℃，保温1h，加入二羟甲基丙酸，保温1h，降温至50℃，向体系内加入三乙胺，反应30min，再取适量去离子水在室温下3000rpm搅拌乳化1h，得均一的蓝白色乳液，然后添加质量百分数为0.1％的消泡剂、0.3％的氮丙啶和1％的硼酸，得聚氨酯粘结乳液。
将上述聚氨酯粘结乳液涂布于厚度为100μm的PET基材一侧，于120℃烘烤固化3min，形成厚度为1μm的粘结层，再在粘结层上涂布一层前述阻氧层原料，120℃烘烤固化3min，形成厚度为5μm的阻氧层。得有机阻隔膜，测得其氧气透过率为0.284cm3/m2·24h·0.1MPa，水蒸气透过率为0.641g/m2·24h，百格法测试涂层附着力为1级。
将有机阻隔膜的阻氧层上涂布如实施例1的红绿量子点UV胶水，准备另一片相同的有机阻隔膜，并两片相对贴合成三明治结构，UV固化后即得量子点膜。
【实施例3】
将新戊二醇、邻苯二甲酸酐、己二酸、间苯二甲酸-5-磺酸钠、三羟甲基丙烷以及催化剂氧化二丁基锡加入带搅拌和冷凝回流管的三口烧瓶中，通氮气10min，搅拌并升温至150℃保温1h，再升至180℃保温1h，最后升至200℃，真空抽去体系内小分子产物水，反应完全后，降温至80℃，加入去离子水，然后再加入质量百分数为0.2％的流平剂、0.1％的消泡剂、3％甲醚化六羟甲基三聚氰胺和10％的硼酸钠，得聚酯粘结乳液。
将上述聚酯粘结乳液涂布于厚度为100μm的PET基材一侧，于120℃烘烤固化3min，形成厚度为1μm的粘结层，再在粘结层上涂布一层前述阻氧层原料，140℃烘烤固化3min，形成厚度为5μm的阻氧层。得有机阻隔膜，测得其氧气透过率为0.351cm3/m2·24h·0.1MPa，水蒸气透过率为0.488g/m2·24h，百格法测试涂层附着力为0级。
将有机阻隔膜的阻氧层上涂布如实施例1的红绿量子点UV胶水，准备另一片相同的有机阻隔膜，并两片相对贴合成三明治结构，UV固化后即得量子点膜。
【实施例4】
将丙烯酸、丙烯酸丁酯、丙烯腈和定量的去离子水加入带搅拌和冷凝回流管的三口烧瓶中，通氮气10min，搅拌并升温至75℃，加入定量的过硫酸钾水溶液，保温8h，降温至30℃出料，测定固含量，加入质量百分数为0.2％的流平剂、0.1％的消泡剂、0.5％的聚碳二亚胺和3％的丙烯酸钠，得丙烯酸酯粘结乳液。
将上述丙烯酸酯粘结乳液涂布于厚度为100μm的PET基材一侧，120℃烘烤固化3min，形成厚度为1μm的粘结层，再在粘结层上涂布一层前述阻氧层原料，120℃烘烤固化3min，形成厚度为5μm的阻氧层。在PET基材的另一侧涂布前述疏水层原料，同样120℃烘烤固化3min，得到厚度为5μm的疏水层。最后得有机阻隔膜，测得其氧气透过率为0.302cm3/m2·24h·0.1MPa，水蒸气透过率为0.224g/m2·24h，百格法测试涂层附着力为1级。
将有机阻隔膜的阻氧层上涂布如实施例1的红绿量子点UV胶水，准备另一片相同的有机阻隔膜，并两片相对贴合成三明治结构，UV固化后即得量子点膜。
【实施例5】
将丙烯酸、丙烯酸丁酯、丙烯酸羟乙酯和定量的去离子水加入带搅拌和冷凝回流管的三口烧瓶中，通氮气10min，搅拌并升温至75℃，加入定量的过硫酸钾水溶液，保温8h，降温至30℃出料，测定固含量，加入质量百分数为0.2％的流平剂、0.1％的消泡剂、0.5％的聚碳二亚胺和3％的水溶性钛酸酯螯合剂，得丙烯酸酯粘结乳液。
将上述丙烯酸酯粘结乳液涂布于厚度为100μm的PET基材一侧，120℃烘烤固化3min，形成厚度为1μm的粘结层，再在粘结层上涂布一层前述阻氧层原料，120℃烘烤固化3min，形成厚度为5μm的阻氧层。在PET基材的另一侧涂布前述疏水层原料，同样120℃烘烤固化3min，得到厚度为5μm的疏水层。最后得有机阻隔膜，测得其氧气透过率为0.410cm3/m2·24h·0.1MPa，水蒸气透过率为0.198g/m2·24h，百格法测试涂层附着力为0级。
将有机阻隔膜的阻氧层上涂布如实施例1的红绿量子点UV胶水，准备另一片相同的有机阻隔膜，UV固化后即得量子点膜。
【对比例1】
将丙烯酸甲酯、丙烯酸丁酯、苯乙烯和定量的去离子水加入带搅拌和冷凝回流管的三口烧瓶中，通氮气10min，搅拌并升温至75℃，加入定量的过硫酸钾水溶液，保温8h，降温至30℃出料，测定固含量，加入质量百分数为0.2％的流平剂、0.1％的消泡剂、0.5％的聚碳二亚胺和3％的水溶性钛酸酯螯合剂，得丙烯酸酯粘结乳液。
将丙烯酸酯粘结乳液涂布于厚度为100μm的PET基材一侧，120℃烘烤固化3min，形成厚度为1μm的粘结层，再在粘结层上涂布一层前述阻氧层原料，120℃烘烤固化3min，形成厚度为5μm的阻氧层。在PET基材的另一侧涂布前述疏水层原料，同样120℃烘烤固化3min，得到厚度为5μm的疏水层。最后得有机阻隔膜，测得其氧气透过率为0.422cm3/m2·24h·0.1MPa，水蒸气透过率为0.178g/m2·24h，百格法测试涂层附着力为3级。
将有机阻隔膜的阻氧层上涂布如实施例1的红绿量子点UV胶水，准备另一片相同的有机阻隔膜，并两片相对贴合成三明治结构，UV固化后即得量子点膜。
【对比例2】
将丙烯酸、丙烯酸丁酯、丙烯酸羟乙酯和定量的去离子水加入带搅拌和冷凝回流管的三口烧瓶中，通氮气10min，搅拌并升温至75℃，加入定量的过硫酸钾水溶液，保温8h，降温至30℃出料，测定固含量，加入适量流平剂、消泡剂，得丙烯酸酯粘结乳液。
将丙烯酸酯粘结乳液涂布于厚度为100μm的PET基材一侧，120℃烘烤固化3min，形成厚度为1μm粘结层，再在粘结层上涂布一层前述阻氧层原料，120℃烘烤固化3min，形成厚度为5μm的阻氧层。在PET基材的另一侧涂布前述疏水层原料，同样120℃烘烤固化3min，得到厚度为5μm的疏水层。最后得有机阻隔膜，测得其氧气透过率为0.387cm3/m2·24h·0.1MPa，水蒸气透过率为0.256g/m2·24h，百格法测试涂层附着力为3级。
将有机阻隔膜的阻氧层上涂布如实施例1的红绿量子点UV胶水，准备另一片相同的有机阻隔膜，并两片相对贴合成三明治结构，UV固化后即得量子点膜。
【对比例3】
将丙烯酸、丙烯酸丁酯、丙烯酸羟乙酯和定量的去离子水加入带搅拌和冷凝回流管的三口烧瓶中，通氮气10min，搅拌并升温至75℃，加入定量的过硫酸钾水溶液，保温8h，降温至30℃出料，测定固含量，然后加入质量百分数为0.2％流平剂、0.1％的消泡剂，得丙烯酸酯粘结乳液。
将丙烯酸酯粘结乳液涂布于厚度为100μm的PET基材一侧，120℃烘烤固化3min，形成厚度为1μm粘结层，再在粘结剂上涂布一层前述阻氧层原料，120℃烘烤固化3min，形成厚度为5μm的阻氧层。得有机阻隔膜，测得其氧气透过率为0.588cm3/m2·24h·0.1MPa，水蒸气透过率为1.207g/m2·24h，百格法测试涂层附着力为4级。
将有机阻隔膜的阻氧层上涂布本公司的红绿量子点UV胶水，准备另一片相同的有机阻隔膜，并两片相对贴合成三明治结构，UV固化后即得量子点膜。
【对比例4】
将丙烯酸、丙烯酸丁酯、丙烯酸羟乙酯和定量的去离子水加入带搅拌和冷凝回流管的三口烧瓶中，通氮气10min，搅拌并升温至75℃，加入定量的过硫酸钾水溶液，保温8h，降温至30℃出料，测定固含量，然后加入质量百分数为0.2％流平剂、0.1％的消泡剂、0.5％的聚碳二亚胺和3％的水溶性钛酸酯螯合剂，得丙烯酸酯粘结乳液。
将丙烯酸酯粘结乳液涂布于厚度为100μm的PET基材一侧，120℃烘烤固化3min，形成厚度为1μm粘结层，再在粘结剂上涂布一层前述阻氧层原料，120℃烘烤固化3min，形成厚度为5μm的阻氧层。再在该阻氧层上涂布前述疏水层原料，同样120℃烘烤固化3min，得到厚度为5μm的疏水层。得有机阻隔膜，测得其氧气透过率为0.305cm3/m2·24h·0.1MPa，水蒸气透过率为0.427g/m2·24h，百格法测试涂层附着力为2级。
将有机阻隔膜的疏水层上涂布本公司的如实施例1的红绿量子点UV胶水，准备另一片相同的有机阻隔膜，并两片相对贴合成三明治结构，UV固化后即得量子点膜。
氧气透过率按GB/T 1038-2000测试，条件为38℃/0％RH；水蒸气透过率按GB/T21529标准测试，条件为38℃/90％RH。对以上各实施例以及对比例制作的量子点膜进行发光效率以及稳定性测试，测试结果见表1。其中，量子点发光效率的检测方法是：以450nm蓝色LED作为背光源，利用积分球分别测试蓝色背光光谱和透过量子点膜的光谱，利用谱图的积分面积计算量子点发光效率。量子点发光效率＝(红色量子点吸收峰面积+绿色量子点吸收峰面积)/(蓝色背光峰面积-透过量子点膜未被吸收的蓝色峰面积)*100％。老化稳定性的检测方法是：老化稳定性的检测方法主要包括在高温蓝光光照(70℃，0.5W/cm2)，高温高湿(65℃/95％RH)和高温储存(85℃)等老化条件下，检测量子点膜的发光效率变化。由于量子点对湿气和氧气非常敏感，因此重点检测了高温高湿(65℃/95％RH)老化和高温老化后量子点发光效率衰减。RH指的是相对湿度。
表1各量子点膜发光性能
实施例5与对比例1的区别在于高分子粘结剂的不同，实施例5中的高分子粘结剂包括羟基，而对比例1的高分子粘结剂不含羟基，通过实验数据可以看出，对比例1的有机阻隔膜的附着力(3级)比实施例5的有机阻隔膜的附着力(0级)差，而且对比例1的量子点膜的剥离力更小，可见高分子粘结剂中含有羟基或者与羟基活性类似的官能团，对提高粘结层的粘结性能具有重要的作用。此外，实施例5的量子点膜的量子点稳定性也较对比例1更好，可见高分子粘结剂中含有羟基或者与羟基活性类似的官能团，对提高有机阻隔膜的水氧阻隔性能具有重要的作用。
实施例5与对比例2的区别在于：对比例2的粘结层中不添加交联剂以及螯合剂，通过实验数据可以看出，对比例2的有机阻隔膜的附着力较差，由其制备的量子点膜的剥离力很小，且量子点稳定性差。可见交联剂以及螯合剂对提高有机阻隔膜的附着力以及水氧阻隔性具有重要的作用。
实施例5与对比例3的区别在于：对比例3的粘结层中不添加交联剂以及螯合剂，且有机阻隔膜不包括疏水层，实验测得实施例5的有机阻隔膜的氧气透过率为0.410cm3/m2·24h·0.1MPa，水蒸气透过率为0.198g/m2·24h，对比例3的有机阻隔膜的氧气透过率为0.588cm3/m2·24h·0.1MPa、水蒸气透过率为1.207g/m2·24h，可见在没有疏水层的情况下，不添加交联剂和螯合剂会导致有机阻隔膜的阻氧性，特别是导致阻水性急剧下降。通过表1的数据，也可以看出，对比例3的量子点膜的稳定性及剥离力比实施例5更差，而且在湿度较高的环境下，对比例3的量子点膜的稳定性更差，原因是在没有阻水层的情况下，水汽渗透通过膜片到达没有螯合剂及交联剂的粘结层，导致粘结层胶体溶胀完全失去和阻氧层的粘结性，加速水汽及氧气从侧面渗透到三明治结构量子点胶层中导致量子点快速失效。
实施例5与对比例4的区别在于：对比例4的量子点膜的疏水层在靠近量子点胶水的一侧，而阻氧层则在疏水层的外侧。通过实验数据可以看出，对比例4的量子点膜的剥离力差，且量子点的稳定性也差，说明将疏水层设置在阻氧层的外侧有利于提高有机阻隔膜的阻隔性；另一方面，量子点胶水与阻氧层的粘结性更好，因此实施例5的量子点膜的剥离力更高。
上述实施方式仅为本发明的优选实施方式，不能以此来限定本发明保护的范围，本领域的技术人员在本发明的基础上所做的任何非实质性的变化及替换均属于本发明所要求保护的范围。

Claims (13)

1.一种有机阻隔膜，其特征在于，包括由外到内依次设置的基材层、粘结层以及阻氧层，所述阻氧层包括聚乙烯醇，所述粘结层与所述阻氧层之间形成化学交联。
2.根据权利要求1所述的有机阻隔膜，其特征在于，所述基材层的外侧设置有疏水层或磨砂层，所述疏水层包括以下一种或多种疏水聚合物：聚偏二氯乙烯、聚偏氟乙烯、聚四氟乙烯、聚三氟氯乙烯，所述磨砂层包括载体以及透明颗粒。
3.根据权利要求1所述的有机阻隔膜，其特征在于，制备所述粘结层的原料包括：高分子粘结剂、交联剂和螯合剂；优选地，所述高分子粘结剂选自聚酯、聚氨酯或聚丙烯酸酯中的一种或多种，所述高分子粘结剂包括以下基团中的至少一种：羟基、羧基、氨基，所述螯合剂与所述聚乙烯醇形成化学键交联。
4.根据权利要求3所述的有机阻隔膜，其特征在于，所述螯合剂选自以下一种或多种：硼酸、硼酸钠、丙烯酸钠、钛酸酯。
5.根据权利要求3所述的有机阻隔膜，其特征在于，所述交联剂选自以下一种或多种：聚碳二亚胺、氮丙啶、甲醚化六羟甲基三聚氰胺。
6.根据权利要求3所述的有机阻隔膜，其特征在于，所述高分子粘结剂的玻璃化转变温度小于50℃。
7.一种有机阻隔膜的制备方法，其特征在于，包括以下步骤：
提供基材层；
在所述基材层的第二侧设置粘结层，在所述粘结层上设置阻氧层，所述阻氧层包括聚乙烯醇，所述粘结层与所述阻氧层之间形成化学交联。
8.根据权利要求7所述的制备方法，其特征在于，所述粘结层的制备方法包括：
将包括高分子粘结剂、交联剂和螯合剂的混合物设置于所述基材层的第二侧，所述高分子粘结剂选自聚酯、聚氨酯、聚丙烯酸酯中的一种或多种；优选地，所述高分子粘结剂包括以下基团中的至少一种：羟基、羧基、氨基，所述螯合剂与所述聚乙烯醇形成化学键交联。
9.根据权利要求8所述的制备方法，其特征在于，所述螯合剂选自以下一种或多种：硼酸、硼酸钠、丙烯酸钠、钛酸酯；优选地，所述螯合剂在所述混合物中的质量百分数为1％～10％。
10.根据权利要求8所述的制备方法，其特征在于，所述交联剂选自以下一种或多种：聚碳二亚胺、氮丙啶、甲醚化六羟甲基三聚氰胺。
11.根据权利要求7-10任一所述的制备方法，其特征在于，在所述基材层的第一侧设置疏水层或磨砂层。
12.根据权利要求7-10任一所述的制备方法，其特征在于，所述阻氧层的制备方法包括：将包括聚乙烯醇、水、消泡剂和流平剂的混合物，设置于所述粘结层。
13.一种量子点器件，其特征在于，包括量子点层以及设置在所述量子点层一侧或两侧的如权利要求1-6任一所述的有机阻隔膜，所述有机阻隔膜的所述阻氧层设置在靠近所述量子点层的内侧。
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