CN113956517A - 一种多功能被动辐射冷却薄膜的制备方法 - Google Patents
一种多功能被动辐射冷却薄膜的制备方法 Download PDFInfo
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Abstract
本发明公开了一种多功能被动辐射冷却薄膜的制备方法,属于冷却薄膜技术领域,本发明首先通过涂布和退火工艺在基底上制备聚苯乙烯小球光子晶体结构;然后,在聚苯乙烯小球光子晶体结构上涂布氧化锌胶体并在真空中干燥;接着,在箱式炉通过退火化工艺移除聚苯乙烯小球;接下来,在二氧化钛骨架上旋涂或滴涂量子点溶液;最后,继续涂布聚二甲基硅氧烷前聚体并固化脱模得到多功能辐射冷却薄膜;该方法制备的多功能被动辐射冷却薄膜同时具备三项功能:被动辐射冷却、激发发光和防伪,具有较好的应用价值。
Description
技术领域
本发明属于冷却薄膜技术领域,具体涉及一种多功能被动辐射冷却薄膜的制备方法。
背景技术
随着人类社会的快速发展,人类对能源的消耗大幅上升,特别是对空间制冷的需求也是在不断增长,制冷用电已经占全球总耗电量的10%,而且占比还逐年增加。而近年来被动辐射冷却技术因为其零耗能,零污染而不断受到人们关注。被动辐射冷却的基本原理是:尽可能多地反射或散射掉太阳光谱波段的能量;同时,通过“大气窗口”(8-13μm)向温度接近绝对零度的宇宙空间发射足够多的红外辐射能量来释放热量,从而达到制冷的目的。被动辐射冷却不仅可以作为一种无耗能的建筑温度调控手段,还可应用于冷凝水、电子产品散热、冷链运输等多个领域。
为了实现对太阳光谱的反射,目前被动辐射冷却制冷材料一般采用金属反射薄膜(如银膜、铝膜等),或微纳米散射微粒以及光子晶体结构。因此,被动辐射冷却制冷材料往往要么对太阳光进行镜面反射造成光污染,要么呈现白色,不仅很难和建筑外观相匹配,而且也限制了在电子产品散热等领域的实际应用。此外,目前,被动辐射冷却材料功能单一,一般仅仅只能实现被动辐射冷却效果,缺少其他附加功能,如彩色、防伪等等。
CN111996679A的发明专利“一种彩色辐射制冷柔性复合薄膜及其制备方法”,采用掺入颜料的方法制备了一种彩色被动辐射冷却薄膜,在被动辐射辐射冷却的同时还实现彩色的附加功能。
CN112500595A的发明专利“空气孔光子晶体结构被动辐射薄膜及其制备方法”公布了由空气孔光子晶体结构组成的柔性被动辐射冷却薄膜制备方法,该薄膜仅具有被动辐射冷却功能。
发明内容
发明目的:本发明的目的是针对上述现有技术不足,提出一种具有制作简单,成本低廉的多功能被动辐射冷却薄膜制备方法。
技术方案:为实现上述发明目的,本发明提出的一种多功能被动辐射冷却薄膜的制备方法,包括步骤:
S1)在基底上通过涂布和退火工艺制备聚苯乙烯小球光子晶体结构;
S2)在聚苯乙烯小球光子晶体结构上涂布氧化锌胶体并在真空中干燥;
S3)在箱式炉通过退火化工艺移除聚苯乙烯小球;
S4)在二氧化钛骨架上旋涂或滴涂量子点溶液并干燥;
S5)继续涂布聚二甲基硅氧烷前聚体并固化脱模得到多功能辐射冷却薄膜,其中,聚苯乙烯小球直径为900nm~5μm,薄膜厚度大于80μm。
进一步的,所述的步骤S1)中基底材质是硅、石英、FTO玻璃和ITO玻璃中的一种。
进一步的,所述的步骤S2)中氧化锌胶体颗粒大小为5nm~15nm,干燥的退火温度为120~150℃,时间为1~3分钟。
进一步的,所述的步骤S3)的箱式炉通过退火工艺是指退火温度保持在400℃~450℃,时间为7~9h。
进一步的,所述的步骤S4)的滴涂量子点溶液是硫化锌/硒化铬量子点(CdSe/ZnSQDs)、硫化锌/磷化铟量子点(InP/ZnS QDs)、碳量子点(C QDs)、硫化铅量子点(PbS QDs)、和钙钛矿量子点(CsPbX3 QDs)中的一种。
进一步的,所述的步骤S4)的量子点溶液的溶剂是去离子水、乙醇、油胺、十二烷基硫醇和油酸中的一种。
进一步的,所述的步骤S5)涂布的聚二甲基硅氧烷是由聚二甲基硅氧烷基本组分与固化剂(道康宁DC 184)按照9~10:1重量比混合得到的液体,温度为40℃~70℃,时间为1~4小时。
本发明与现有技术相比所具有的有益效果是:提供了多功能被动辐射冷却薄膜制备方法,不仅具备反射太阳光和“大气窗口”波段的高发射率的特性,还具备激发发光和防伪的功能,即:当不用特定的激发光照射该薄膜时,薄膜呈现白色,当用激发光照射薄膜时,薄膜能根据实际采用的量子点发出特定波长的光,可以用于既需要被动辐射冷却、又需要装饰或防伪的领域,如电子产品辐射冷却降温等;该方法制备的多功能被动辐射冷却薄膜同时具备三项功能:被动辐射冷却、激发发光和防伪,具有较好的应用价值。
附图说明
图1是多功能被动辐射冷却薄膜工作原理示意图;
图2是多功能被动辐射冷却薄膜制备方法流程图;
图3是实施例的去除聚苯乙烯小球后的氧化锌骨架SEM图;
图4是实施例的被动辐射冷却薄膜的激发发光谱图;
图5是实施例的被动辐射冷却薄膜的可见光区域的反射率测试图;
图6是实施例的被动辐射冷却薄膜的降温测试图。
具体实施方式
下面结合附图及具体实施方式对本发明进行详细介绍。但这些实施方式并不限制本发明,本领域的技术人员在不付出创造性劳动的情况下根据这些具体实施方式所做出的结构、方法或功能上的变换均应包含在本发明的保护范围内。
一种多功能被动辐射冷却薄膜的制备方法,包括步骤:
S1)在基底上通过涂布和退火工艺制备聚苯乙烯小球光子晶体结构;
S2)在聚苯乙烯小球光子晶体结构上涂布氧化锌胶体并在真空中干燥;
S3)在箱式炉通过退火化工艺移除聚苯乙烯小球;
S4)在二氧化钛骨架上旋涂或滴涂量子点溶液并干燥;
S5)继续涂布聚二甲基硅氧烷前聚体并固化脱模得到多功能辐射冷却薄膜,其中,聚苯乙烯小球直径为900nm~5μm,薄膜厚度大于80μm。
步骤S1)中基底材质是硅、石英、FTO玻璃和ITO玻璃中的一种。
步骤S2)中氧化锌胶体颗粒大小为5nm~15nm,干燥的退火温度为120~150℃,时间为1~3分钟。
步骤S3)的箱式炉通过退火工艺是指退火温度保持在400℃~450℃,时间为7~9h。
步骤S4)的滴涂量子点溶液是硫化锌/硒化铬量子点(CdSe/ZnS QDs)、硫化锌/磷化铟量子点(InP/ZnS QDs)、碳量子点(C QDs)、硫化铅量子点(PbS QDs)、和钙钛矿量子点(CsPbX3 QDs)中的一种。
步骤S4)的量子点溶液的溶剂是去离子水、乙醇、油胺、十二烷基硫醇和油酸中的一种。
步骤S5)涂布的聚二甲基硅氧烷是由聚二甲基硅氧烷基本组分与固化剂按照9~10:1重量比混合得到的液体,温度为40℃~70℃,时间为1~4小时。
实施例
参见图1所示,图1是多功能被动辐射冷却薄膜工作原理示意图。该多功能被动辐射冷却薄膜由材质为聚二甲基硅氧烷1构成,在聚二甲基硅氧烷薄膜内设置蜂窝状排列的氧化锌骨架结构2,在蜂窝状排列的氧化锌骨架结构2内设置量子点发光材料。
参见图1至图5,多功能光子晶体结构被动辐射冷却薄膜制备方法包括步骤:
S1)在基底上通过涂布和退火工艺制备聚苯乙烯小球光子晶体结构;
在该步骤中,在一种实施方式中,采用本领域公知的分散聚合法制备直径为900nm的水溶性聚苯乙烯单分散小球,并将聚苯乙烯微球按质量比20%溶于去离子水中,然后均匀涂布在石英基底上,在40℃下退火1.5小时,经过自然冷却降温后在石英基底上得到直径为900nm聚苯乙烯小球光子晶体结构。
在其他实施方式中,在保持分散聚合法的前提下,通过改变分散聚合法中采用的聚苯乙烯聚合单体的用量,可以得到直径范围为900nm-5μm的聚苯乙烯小球。该基底也可以采用硅、FTO玻璃或者ITO玻璃。
S2)在聚苯乙烯小球光子晶体结构上涂布氧化锌胶体并在真空中干燥;
在该步骤中,在一种实施方式中,氧化锌胶体配制方法如下:将220mg的二水乙酸锌、2ml的甲氧基乙醇和61μl的乙醇胺溶液混合放置于配液瓶中,并放入磁力搅拌子在室温下搅拌4小时,获得颗粒尺寸在5nm~15nm的氧化锌胶体溶液。然后,将氧化锌胶体溶液均匀涂布在聚苯乙烯小球光子晶体结构表面,并放置到真空干燥箱,在真空度130Pa下,保持退火温度为120℃,时间为3分钟。经过真空干燥,胶体溶液溶液填充到聚苯乙烯小球的空隙中,并固化。
在其他实施方式中,退火温度为可设置为120~150℃,时间为1~3分钟。
S3)在箱式炉通过退火工艺移除聚苯乙烯小球;
将步骤S2)中得到的样品放置到箱式炉中,保持退火温度为400℃,时间为7h,经过退火后,聚苯乙烯小球在高温下完全气化消失,仅留下材质为氧化锌的蜂窝状的空气孔结构(如附图3所示)。
在其他实施方式中,退火温度可选择在400℃~450℃范围内,时间可选择在7~9h范围内。
S4)在二氧化钛骨架上旋涂或滴涂量子点溶液并干燥;
在一种实施方式中,将溶剂为乙醇的硫化锌/硒化铬量子点(CdSe/ZnS QDs)溶液滴涂在步骤S3)中得到的氧化锌的蜂窝状的空气孔结构(即:二氧化钛骨架)上,该量子点溶液均匀渗透到蜂窝状的空气孔中,并置于干燥箱中,在40℃下干燥2小时,经干燥后,量子点均匀分布在蜂窝状的空气孔的侧壁上。
在其他实施方式中,量子点溶液可以采用硫化锌/磷化铟量子点(InP/ZnS QDs)、碳量子点(C QDs)、硫化铅量子点(PbS QDs)、或者钙钛矿量子点(CsPbX3QDs);量子点溶液的溶剂可以采用去离子水、油胺、十二烷基硫醇或者油酸,而且干燥的温度和时间可灵活设置。
S5)继续涂布聚二甲基硅氧烷前聚体并固化脱模得到多功能辐射冷却薄膜。
将聚二甲基硅氧烷基本组分和固化剂按照9:1体积比混合得到的聚二甲基硅氧烷前聚体溶液,将得到的前聚体溶液均匀涂布到步骤S4)中得到的样品表面,此时聚二甲基硅氧烷前聚体溶液在重力作用下会自动填充到蜂窝状的空气孔中,将样品放置到干燥箱中,在温度40℃下,干燥固化4小时后,聚二甲基硅氧烷前聚体溶液固化成膜,直接从石英基底上剥离后,即得到多功能被动辐射冷却薄膜。
在其他实施方式中,聚二甲基硅氧烷基本组分与固化剂的体积比选择范围在9~10:1,固化温度可选择在40℃~70℃范围内,固化时间可选择为1~4小时。
用波长为375nm的紫外光照射按上述制备方法得到的被动辐射冷却薄膜,测得的归一化激发光谱如图4所示,此时薄膜发出波长峰值为525nm的绿光,表现出发光薄膜特性。
经紫外可见分光光度计测试,如图5所示,该多功能被动辐射冷却薄膜在太阳光谱的0.38μm-1.2μm范围内的平均反射率为90.5%,从而反射了大部分太阳光辐射,说明样品在无激发的情况下,呈现自然白色。这种呈现自然白色、受激发后发光的特性可以用于防伪装饰领域。
进一步测试该被动辐射冷却薄膜的被动辐射冷却效果,将样品置于四周密封隔热、顶部采用低密度聚乙烯薄膜密封并作为窗口的测试箱内进行试验测试。测试结果如图6所示,从图中可以看出:从上午10:00时到下午15:00时,薄膜样品温度比环境周围温度明显偏低,平均降低约4.7℃,说明该薄膜不仅具有激发发光和防伪的附加功能,还具有良好的被动辐射冷却作用。
Claims (7)
1.一种多功能被动辐射冷却薄膜的制备方法,其特征在于,包括以下步骤:
S1)在基底上通过涂布和退火工艺制备聚苯乙烯小球光子晶体结构;
S2)在聚苯乙烯小球光子晶体结构上涂布氧化锌胶体并在真空中干燥;
S3)通过退火工艺移除聚苯乙烯小球;
S4)在二氧化钛骨架上旋涂或滴涂量子点溶液并干燥;
S5)继续涂布聚二甲基硅氧烷前聚体并固化脱模得到多功能辐射冷却薄膜,其中,聚苯乙烯小球直径为900nm~5μm,多功能辐射冷却薄膜的厚度大于80μm。
2.根据权利1所述的一种多功能被动辐射冷却薄膜的制备方法,其特征在于:所述的步骤S1)中,基底材质是硅、石英、FTO玻璃和ITO玻璃中的一种。
3.根据权利1所述的一种多功能被动辐射冷却薄膜的制备方法,其特征在于:所述的步骤S2)中氧化锌胶体颗粒大小为5nm~15nm,干燥的退火温度为120~150℃,时间为1~3分钟。
4.根据权利1所述的一种多功能被动辐射冷却薄膜的制备方法,其特征在于:所述的步骤S3)中,通过退火工艺是指退火温度保持在400℃~450℃,时间为7~9h。
5.根据权利1所述的一种多功能被动辐射冷却薄膜的制备方法,其特征在于:所述的步骤S4)中,滴涂量子点溶液是硫化锌/硒化铬量子点、硫化锌/磷化铟量子点、碳量子点、硫化铅量子点和钙钛矿量子点中的一种。
6.根据权利1所述的一种多功能被动辐射冷却薄膜的制备方法,其特征在于:所述的步骤S4)中,量子点溶液的溶剂是去离子水、乙醇、油胺、十二烷基硫醇和油酸中的一种。
7.根据权利1所述的一种多功能被动辐射冷却薄膜的制备方法,其特征在于:所述的步骤S5)中,涂布的聚二甲基硅氧烷是由聚二甲基硅氧烷前聚体与固化剂按照9~10:1重量比混合得到的液体,温度为40℃-70℃,时间为1-4小时。
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