CN113583193B - 一种光热离子凝胶薄膜及其制备方法和应用 - Google Patents
一种光热离子凝胶薄膜及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种光热离子凝胶薄膜及其制备和应用,属于柔性电子和光热、热电功能材料领域。这种光热发电离子凝胶薄膜包含两个部分,一半为由丙烯酸酯单体、交联剂、离子导电填充物和光引发剂通过光交联反应制备的离子凝胶薄膜;另一半为在上述离子凝胶膜中添加光热转化材料的离子凝胶薄膜。这两种离子凝胶薄膜都是通过将各种前驱体加入到模具中,在紫外灯照射下发生共聚反应获得。在光照条件下,该离子凝胶薄膜能形成内部温度差,进而形成内部电势差,从而实现发电。本发明所提出的光热离子凝胶薄膜具有制备简单,原料易得,便于大规模生产等优点。
Description
技术领域
本发明属于柔性电子和光热、热电功能材料领域。更具体而言,属于光热离子凝胶薄膜及其制备方法和应用。
背景技术
随着人类对能源需求的日益增长,传统的化石能源由于其高排放、高污染、不可再生等缺点,需要人类寻求新的能源获取方式。由此产生了例如太阳能发电、地热能发电、风能发电等一系列清洁型能源获取方式,并且在全球能源供给比例中这些新能源的占比也越来越高。其中太阳能发电越来越得到人们的认可,并成为人类获取能源的主要途径之一。当前利用太阳能发电的器件主要有染料敏化太阳能电池、硅基太阳能电池、聚合物太阳能电池和钙钛矿太阳能电池等,这些太阳能电池各有优劣。如硅基太阳能电池的稳定性好、效率高,但存在制备流程复杂和难以柔性发电的缺点;钙钛矿太阳能电池效率高、能实现柔性性能,但稳定性还需要提高等。因此,发展新型的光伏发电技术,是太阳能发电领域人们孜孜以求的目标。
当今世界能源的消耗,根据不同的行业,所产生的余热占到能源总消耗的15%-60%。因此利用热电技术收集余热也获得了人们的关注。目前所使用的热电技术主要还是基于无机半导体材料,但无机材料制备复杂、难以溶液加工和刚性结构的特点,限制了其在柔性电子领域的应用。而有机材料由于其易于加工和柔性结构的特点,能很好的解决这个问题。
有机热电技术发展已经有较成熟的研究,其中基于离子聚合物的热电技术是发展的重点之一。当前基于离子型聚合物材料的热电技术已经开展了一些工作,但是其热源的获取仍为简单的直接与冷热两端相接触获得温度差从而达到发电的效果。此外,对于光伏发电技术而言,由于光照强度易于受到天气的影响,如果能发展结合光热和热电技术来进行发电,对于实现全天候发电具有重要意义。基于以上现状,本发明提出一种光热离子薄膜的制备方法,并探究其在光照条件下的发电情况,实现了光热效应和热电效应一体化的设计。
发明内容
本发明公开了一种光热离子凝胶薄膜、制备方法及其应用,提出一种基于离子凝胶的全新概念光伏发电技术。该光热离子凝胶薄膜集光热效应、热电效应为一体,拓展了能源获取途径。
为了实现利用离子凝胶发电,本发明通过选取合适的丙烯酸酯单体、交联剂、离子导电填充物和引发剂配制前驱体溶液,在前驱体溶液中加入光热转化材料,就可使得聚合后的凝胶在光照条件下达到升温的效果。这种光热发光离子凝胶薄膜包含两个部分,一半为由丙烯酸酯单体、交联剂、离子导电填充物和光引发剂通过光交联反应制备的离子凝胶薄膜;另一半为在上述离子凝胶膜中添加光热转化材料的离子凝胶薄膜。在光照条件下,含光热转化材料的一侧凝胶可升温,而另一侧几乎不升温,从而在凝胶内部产生温度差,温度差进一步产生电势差达到发电的效果。
本发明通过巧妙的结构设计制备一种一侧在光照条件下产生稳定的升温效果而另一侧不发生明显升温的离子凝胶,这种升温效果的不同会在凝胶两侧产生温度差,由于温度差的存在可产生电势差达到发电的效果。
离子凝胶薄膜的制备过程如下:通过物理共混配制前驱体溶液,搅拌均匀后倒入聚四氟乙烯模具中用紫外灯照射引发聚合反应,通过两次聚合实现薄膜整体的制备。
一种光热离子凝胶薄膜,所述的光热离子凝胶薄膜包含两个部分:一半为前驱体,包括丙烯酸酯单体、交联剂、离子导电填充物和光引发剂,通过光交联反应制备的离子凝胶薄膜;另一半为添加了光热转化材料的前驱体;然后将两个部分通过光聚合制备含有光热转化材料的离子凝胶薄膜。
其中选取的丙烯酸酯单体包括丙烯酸乙酯、丙烯酸丁酯、丙烯酸羟乙酯、丙烯酸羟丙酯、丙烯酸羟丁酯、丙烯酸乙氧基乙氧基乙酯中的一种或几种。
交联剂包括聚乙二醇二丙烯酸脂、乙氧基化三羟甲基丙烷三丙烯酸酯、乙氧基化季戊四醇四丙烯酸酯中的一种或几种。
离子导电填充物包括双三氟甲烷磺酰亚胺锂、1-乙基-3-甲基咪唑双三氟甲烷磺酰亚胺盐、1-乙基-3-甲基咪唑醋酸盐中的一种或几种。
光引发剂选择的是1-羟基环己基苯基甲酮。
光热转化材料选择的是聚吡咯、聚多巴胺、四氧化三铁纳米颗粒、MXene、纳米硫化铜、碳黑、黑色墨水中的一种或几种。
优选,前驱体和光热转化材料质量比为:丙烯酸酯单体:80%-90%;交联剂:0.01%-0.1%;离子导电填充物:10%-20%;引发剂:0.5%-2.5%;光热转化材料:0.001%-1%。
优选,前驱体为丙烯酸丁酯,聚乙二醇二丙烯酸脂,双三氟甲烷磺酰亚胺;1-羟基环己基苯基甲酮,光热转换材料MXene;
或者所述前驱体为丙烯酸乙氧基乙氧基乙酯,丙烯酸羟丁酯,乙氧基化三羟甲基丙烷三丙烯酸酯,双三氟甲烷磺酰亚胺锂, 1-羟基环己基苯基甲酮,光热转换材料为四氧化三铁纳米颗粒;
或者所述前驱体为丙烯酸丁酯,丙烯酸羟丙酯,聚乙二醇二丙烯酸脂, 1-乙基-3-甲基咪唑双三氟甲烷磺酰亚胺盐, 1-羟基环己基苯基甲酮,光热转换材料为黑色墨水;
或者所述前驱体为丙烯酸乙氧基乙氧基乙酯,丙烯酸羟丙酯,聚乙二醇二丙烯酸脂,双三氟甲烷磺酰亚胺锂, 1-羟基环己基苯基甲酮,光热转换材料为聚吡咯。
一种光热离子凝胶薄膜的制备方法,包括以下步骤:
(1)按照上述任意一种光热离子凝胶薄膜配置前驱体和添加光热转化材料的前驱体,均超声;
(2)将步骤(2)中的前驱体加入到聚四氟乙烯模具中聚合,再将添加光热转化材料的前驱体设置在聚四氟乙烯模具中聚合形成完整的薄膜,所述的前驱体和添加光热转化材料的前驱体设置聚四氟乙烯模具中反应后是化学相连状态。
本发明的光热离子凝胶薄膜应用于LED灯泡、发电、自供能传感器、人机交互。
光热离子凝胶薄膜的制备方法如下所示:
(1)上述原料按质量百分数称取:丙烯酸酯单体80%-90%,交联剂0.01%-0.1%,离子导电填充物10%-20%,引发剂0.5%-2.5%,在需要加入光热转化材料的前驱体中加入光热转换材料0.001%-1%。将称取的前驱体倒入到玻璃瓶中密封后超声分散10-30分钟确保均匀分散。
(2)在聚四氟乙烯模具上贴上离型膜,在中间贴上一层隔膜使得模具分为两个部分。在其中一侧加入一定量的前驱体溶液(优先选择不含光热转化材料的溶液),调整紫外灯照射功率10-80瓦中间对模具中的溶液进行照射引发自由基聚合,3-30分钟即可完成聚合此时撤去中间的隔膜,加入含有光热转化材料的前驱体溶液,后加入溶液的量为略高于前一次合成的膜的表面。再次用相同的方法聚合3-30分钟,即可完成光热离子凝胶薄膜的制备。
将配制的两种前驱体溶液,任选其一吸取适量,加入到聚四氟乙烯模具中同时用隔膜阻挡在模具中间,先在模具一半的位置用紫外灯照射引发3-30分钟的聚合反应。成膜后撤去中间隔膜,吸取另一份前驱体溶液加入到模具的另一半,用紫外灯照射3-30分钟,此时即可得到一张完整膜,其中一半为可光热部分,另一半为不可光热部分。
将该种薄膜置于一定波长的光线下进行照射,含有光热转化材料的一部分吸收所照射光线的能量,产生热量造成局部升温,而另一部分由于是透明状态,几乎不会吸收光线,因此不发生升温现象。此时即可在薄膜两端产生一个稳定的温度差,在温度差存在的条件下,由于塞贝克效应和索雷特尔效应可以在薄膜两端产生电势差达到发电的效果。
所制备的光热离子凝胶薄膜具有优异的光热转换能力,在光照条件下凝胶的两侧形成稳定的温度差。尤其是在激光照射条件下升温迅速可快速升温至90℃左右。由于温度差的存在,根据索雷特效应会在离子凝胶内部产生离子迁移造成离子浓度分布不均,从而产生塞贝克效应产生电势差,在11℃温度差的存在下可获得接近20毫伏的电压整体发电功率达30纳瓦。所产生的电势可以发电、驱动超低功耗器件例如微型LED灯泡、自供能传感器、人机交互等。
附图说明
图1为MXene掺杂的光热离子凝胶薄膜。
图2为四氧化三铁纳米颗粒掺杂的光热离子凝胶薄膜。
图3为黑色墨水掺杂的光热离子凝胶薄膜。
图4为聚吡咯掺杂的光热离子凝胶薄膜。
图5为MXene掺杂的光热离子凝胶薄膜在激光照射后的红外图像。
图6为MXene掺杂的光热离子凝胶薄膜的升温温度-时间图。
图7为四氧化三铁纳米颗粒掺杂的光热离子凝胶薄膜在红外灯照射下的红外图像。
图8为四氧化三铁纳米颗粒掺杂的光热离子凝胶薄膜的电压-时间和电流-时间图。
图9为演示发电效果的外部工作电路实物图和等效电路图。
图10为聚吡咯掺杂的光热离子凝胶薄膜在激光照射时发电点亮微型LED灯泡的实物演示图。
具体实施方式
下面结合实例,结合附图对本发明及应用作进一步的详细说明
实施例1
取10mL的丙烯酸丁酯,25μL的聚乙二醇二丙烯酸脂,1.4g的双三氟甲烷磺酰亚胺锂,0.14g的1-羟基环己基苯基甲酮,同时配一组相同比例,但另加入了10mg光热转换材料MXene的前驱体溶液,超声15分钟分散均匀。
聚四氟乙烯模具整体呈现一个“凹”字型,在聚四氟乙烯模具的底部处贴上离型膜。同时在该离型膜中间贴上隔膜,将隔膜弯成“L”型,隔膜的高度大于聚四氟乙烯模具的高度,隔膜将聚四氟乙烯模具的凹槽处分成两个部分,同时在隔膜底部涂覆薄层硅油使“L”型隔膜贴合在离型膜中间部位。
先取未加入光热转换材料的前驱体溶液,用移液枪取1mL加入到聚四氟乙烯模具的一侧,调整紫外灯功率为50瓦照射10分钟,使该溶液聚合成膜。用移液枪吸取1mL含有光热转换材料的前驱体,撤去聚四氟乙烯模具中间的隔膜后在另一侧加入该前驱体,随后用相同功率紫外灯照射5分钟即可得到光热离子凝胶薄膜(如图1所示)。
实施例2
取8mL的丙烯酸乙氧基乙氧基乙酯,2mL的丙烯酸羟丁酯,50μL的乙氧基化三羟甲基丙烷三丙烯酸酯,1.45g的双三氟甲烷磺酰亚胺锂,0.1g的1-羟基环己基苯基甲酮,同时配制一组相同比例的溶液加入10mg四氧化三铁纳米颗粒,超声分散20分钟确保分散均匀。
聚四氟乙烯模具整体呈现一个“凹”字型,在聚四氟乙烯模具的底部处贴上离型膜。同时在该离型膜中间贴上隔膜,将隔膜弯成“L”型,隔膜的高度大于聚四氟乙烯模具的高度,隔膜将聚四氟乙烯模具的凹槽处分成两个部分,同时在隔膜底部涂覆薄层硅油使“L”型隔膜贴合在离型膜中间部位。
用移液枪吸取1mL不含光热转化材料的前驱体溶液,加入到聚四氟乙烯模具的一侧,调整紫外灯功率为10瓦照射5分钟,随后撤去中间隔膜在另一侧加入1mL含有四氧化三铁纳米颗粒的前驱体溶液,反应5分钟后即可得到光热离子凝胶薄膜(如图2所示)。
实施例3
取9mL的丙烯酸丁酯,1mL的丙烯酸羟丙酯,20μL的聚乙二醇二丙烯酸脂,1g的1-乙基-3-甲基咪唑双三氟甲烷磺酰亚胺盐,0.1g的1-羟基环己基苯基甲酮,同时配制一组相同比例的溶液加入50μL的黑色墨水,超声15分钟分散均匀。
聚四氟乙烯模具整体呈现一个“凹”字型,在聚四氟乙烯模具的底部处贴上离型膜。同时在该离型膜中间贴上隔膜,将隔膜弯成“L”型,隔膜的高度大于聚四氟乙烯模具的高度,隔膜将聚四氟乙烯模具的凹槽处分成两个部分,同时在隔膜底部涂覆薄层硅油使“L”型隔膜贴合在离型膜中间部位。
取1mL不含黑色墨水的前驱体溶液用15瓦的紫外光照射10分钟,随后撤去中间隔膜加入含有黑色墨水的前驱体用相同功率反应5分钟,即可得到光热离子凝胶薄膜(如图3所示)。
实施例4
取8ml的丙烯酸乙氧基乙氧基乙酯,2mL的丙烯酸羟丙酯,25μL的聚乙二醇二丙烯酸脂,1.5g的双三氟甲烷磺酰亚胺锂,0.12g的1-羟基环己基苯基甲酮,同时配制一组相同比例的溶液加入5mg的聚吡咯。超声分散30分钟
聚四氟乙烯模具整体呈现一个“凹”字型,在聚四氟乙烯模具的底部处贴上离型膜。同时在该离型膜中间贴上隔膜,将隔膜弯成“L”型,隔膜的高度大于聚四氟乙烯模具的高度,隔膜将聚四氟乙烯模具的凹槽处分成两个部分,同时在隔膜底部涂覆薄层硅油使“L”型隔膜贴合在离型膜中间部位。
用移液枪吸取1mL不含聚吡咯的前驱体溶液,调节紫外灯功率为10瓦照射5分钟,随后撤去隔膜,加入含有聚吡咯的前驱体溶液以相同的方式聚合5分钟,即可得到光热离子凝胶薄膜(如图4所示)。
实施例5
选取实施例1中的光热离子凝胶薄膜对其光热性能进行测试,将该薄膜切割成0.5×1cm的长方形,贴在玻璃瓶上用5瓦的发射波长为850nm的激光灯在距离薄膜5cm处照射薄膜可光热部分。如图5所示经过激光照射从室温可以稳定升温到88℃左右。图6为升温曲线图。
实施例6
选取实施例2中的光热离子凝胶薄膜对其发电性能进行准确测量。将该薄膜切割成1×2cm的长方形,测试时选择吉时利半导体参数分析系统对其光热发电进行表征。用导线平口夹从探针台上引出接线夹在光热离子凝胶薄膜两端,用30瓦的红外灯在距离薄膜30cm处进行照射在经过4分钟的照射后薄膜两端温度趋于稳定如图7所示。通过分析仪对离子凝胶薄膜的输出电压和稳定后短路电流的进行测量,如图8所示,该薄膜两端的电势差在11℃的温差条件下可以缓慢上升到大约17mV,此时的短路电流为0.2μA,综合输出功率大约为30纳瓦。
实施例7
选取实施例4中的光热离子凝胶薄膜进行实际应用演示,将其切割成1×2cm的长方形,将其贴在玻璃瓶上,同时搭建如图9所示的电路,用平口夹导线连接凝胶和工作电路,用5瓦的发射波长为850nm的激光照射贴在玻璃瓶上的光热薄膜的可光热一侧,进过照射升温后所产生的电势差可以驱动微型LED灯泡产生微弱亮光如图10所示。
Claims (9)
1.一种光热离子凝胶薄膜,其特征在于:所述的光热离子凝胶薄膜包含两个部分:一半为前驱体,包括丙烯酸酯单体、交联剂、离子导电填充物和光引发剂,通过光交联反应制备的离子凝胶薄膜;另一半为添加了光热转化材料的前驱体;然后将两个部分通过光聚合制备含有光热转化材料的离子凝胶薄膜;所述的光热转化材料为聚吡咯、聚多巴胺、四氧化三铁纳米颗粒、MXene、纳米硫化铜、碳黑、黑色墨水中的一种或几种;其添加量为原料总量的0.001%-1%。
2.根据权利要求1所述的一种光热离子凝胶薄膜,其特征在于:所述的丙烯酸酯单体为:丙烯酸乙酯、丙烯酸丁酯、丙烯酸羟乙酯、丙烯酸羟丙酯、丙烯酸羟丁酯、丙烯酸乙氧基乙氧基乙酯中的一种或几种。
3.根据权利要求1所述的一种光热离子凝胶薄膜,其特征在于:所述的交联剂为:聚乙二醇二丙烯酸脂、乙氧基化三羟甲基丙烷三丙烯酸酯、乙氧基化季戊四醇四丙烯酸酯中的一种或几种。
4.根据权利要求1所述的一种光热离子凝胶薄膜,其特征在于:所述的离子导电填充物为:双三氟甲烷磺酰亚胺锂、1-乙基-3-甲基咪唑双三氟甲烷磺酰亚胺盐、1-乙基-3-甲基咪唑醋酸盐中的一种或几种。
5.根据权利要求1所述的一种光热离子凝胶薄膜,其特征在于:所述的光聚合反应中光引发剂为:1-羟基环己基苯基甲酮;所述的光热转化材料为聚吡咯、聚多巴胺、纳米四氧化三铁、MXene、纳米硫化铜、碳黑、黑色墨水中的一种或几种。
6.根据权利要求1所述的一种光热离子凝胶薄膜,其特征在于:所述的前驱体和所述的光热转化材料质量比为:丙烯酸酯单体:85.4%;交联剂:0.08%;离子导电填充物:13.5%;引发剂:1%;光热转化材料:0.005%。
7.根据权利要求1所述的一种光热离子凝胶薄膜,其特征在于:所述前驱体为丙烯酸丁酯,聚乙二醇二丙烯酸脂,双三氟甲烷磺酰亚胺锂,1-羟基环己基苯基甲酮,光热转化材料为MXene;
或者所述前驱体为丙烯酸乙氧基乙氧基乙酯,丙烯酸羟丁酯,乙氧基化三羟甲基丙烷三丙烯酸酯,双三氟甲烷磺酰亚胺锂,1-羟基环己基苯基甲酮,光热转化材料为四氧化三铁纳米颗粒;
或者所述前驱体为丙烯酸丁酯,丙烯酸羟丙酯,聚乙二醇二丙烯酸脂,1-乙基-3-甲基咪唑双三氟甲烷磺酰亚胺盐,1-羟基环己基苯基甲酮,光热转化材料为黑色墨水;
或者所述前驱体为丙烯酸乙氧基乙氧基乙酯,丙烯酸羟丙酯,聚乙二醇二丙烯酸脂,双三氟甲烷磺酰亚胺锂,1-羟基环己基苯基甲酮,光热转化材料为聚吡咯。
8.一种光热离子凝胶薄膜的制备方法,其特征在于,包括以下步骤:
(1)按照权利要求1-7任意一种光热离子凝胶薄膜配置前驱体和添加光热转化材料的前驱体,均超声分散;
(2)将步骤(1)中的前驱体加入到聚四氟乙烯模具中聚合,再将添加光热转化材料的前驱体设置在聚四氟乙烯模具中聚合形成完整的薄膜,所述的前驱体发生聚合反应和添加光热转化材料的前驱体发生聚合反应后是化学连接状态。
9.根据权利要求1-7任意一项所述的光热离子凝胶薄膜或根据权利要求8所述的制备方法制得的光热离子凝胶薄膜应用于发电、自供能传感器、人机交互。
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