CN109545561B - 一种光引发不可逆凝胶电解质及其制备方法和应用 - Google Patents
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Abstract
本发明公开了一种光引发不可逆凝胶电解质及其制备方法。本发明的电解质是利用光引发聚合物单体发生聚合反应,形成具有稳定三维网络结构的不可逆凝胶,然后吸附液态电解质形成,其中:所述聚合物单体为肉桂酸酯类化合物;所述吸附的液态电解质为含有I‑/I3 ‑氧化还原电对的染料敏化太阳电池电解液。本发明制得的电解质热稳定性好,且具有优良的柔韧性。另外,本发明制备方法简单、成本低廉,有利于产业化。将本发明制得的电解质应用于染料敏化太阳电池及其它电池器件领域,所得器件光电性能优异。
Description
技术领域
本发明属于化学、材料及物理技术的交叉领域,具体地说,本发明涉及一种光引发不可逆凝胶电解质、其制备方法和在染料敏化太阳电池及其它电池器件中的应用。
背景技术
染料敏化太阳电池因其成本低廉、制备工艺简单、转换效率高等特点,得到了广泛的关注并迅速发展起来。
DSSC的经典结构是“三明治”夹心结构,主要由导电基底、半导体纳米多孔薄膜(多为TiO2、ZnO等)、染料敏化剂(N719、C101等)、含有氧化还原电对(I-/I3 -,或Br-/Br3 -,SeCN-/(SeCN)2,SCN-/(SCN)2等)的电解质,和对电极(如涂有Pt的导电玻璃)几个主要部分组成,其中电解质作为其重要的组成部分之一,对电池的效率及其稳定性具有重要影响。液态电解质具有扩散速率快、良好的浸润性、光电转换效率高等特点而被广泛应用。
然而随着光电效率超过14%的液态电解质DSSC的诞生,虽然液态电解质DSSC的光电效率虽然较高,但同时存在电解质溶剂易挥发泄露、电池封装困难等问题,固态电解质和准固态电解质可有效改善上述问题,其中固态电解质由于离子导电性能差,且不能有效浸润TiO2多孔薄膜,导致其组装的固态DSSC光电转换效率较低,而准固态电解质因其良好导电性,在提高DSSC的长期稳定性的同时,能够保证DSSC的光电性能因而受到研究学者的广泛关注。
基于上述理由,特提出本申请。
发明内容
本发明的目的在于提供一种光引发不可逆凝胶电解质及其制备方法和应用。本发明的不可逆凝胶是一类重要的准固态材料,具有热稳定性好、制备简单、成本低廉等特点。此外,本发明的凝胶电解质具备非常优异的柔韧性,能够应用于柔性器件。
本发明第一目的是通过以下技术方案实现的:
一种光引发不可逆凝胶电解质,是利用光引发聚合物单体发生聚合反应,形成具有稳定三维网络结构的不可逆凝胶,然后吸附液态电解质形成准固态电解质。
进一步地,上述技术方案,所述聚合物单体为肉桂酸酯类化合物,优选为聚乙烯醇肉桂酸酯,所述聚乙烯醇肉桂酸酯的结构式如下式一所示:
进一步地,上述技术方案,所述光引发采用的光源为紫外光。
进一步地,上述技术方案,所述吸附的液态电解质为含有I-/I3 -氧化还原电对的染料敏化太阳电池电解液。
本发明第二个目的在于提供上述所述的光引发不可逆凝胶电解质的制备方法,所述方法包括如下步骤:
(1)将聚合物单体溶解在有机溶剂中,然后加入光引发剂,超声分散均匀,获得混合液体;
(2)将步骤(1)所得混合液体置于紫外光下照射,使聚合物单体发生聚合反应,形成具有稳定三维网络结构的不可逆凝胶;
(3)将步骤(2)制得的凝胶去吸附含有I-/I3 -氧化还原电对的液态电解液,形成所述光引发不可逆凝胶电解质。
进一步,上述技术方案,步骤(1)所述有机溶剂可以为乙腈、N-甲基-2-吡咯烷酮、二甲基甲酰胺、乙醇、3-甲氧基丙腈等中的一种或多种混合。
进一步,上述技术方案,步骤(1)所述聚合物单体在有机溶剂中的含量为1~50wt%,所述光引发剂在有机溶剂中的含量为0.1~50wt%。
进一步,上述技术方案,步骤(2)所述紫外光照射液体表面的功率密度为1mW/cm2~200mW/cm2,紫外光照射的时间为1s~24h。
进一步,上述技术方案,步骤(3)所述凝胶吸附电解液的时间为0.01~50h。
进一步,上述技术方案,步骤(3)所述液态电解质的配方通式可以为:
aA+bB+cC+dD+eE;
通式中:
A表示卤素氟、氯、溴、碘或拟卤素氰根、硫氰根,如I2、(SeCN)2、(SCN)2等;
B表示卤素氟、氯、溴、碘或拟卤素氰根、硫氰根、高氯酸根的一价、二价或三价金属阳离子或非金属阳离子盐类;如碘化锂、碘化钠、碘化钾、氯化钠、氯化钾等;
C表示卤素(氟、氯、溴、碘)、拟卤素(氰根、硫氰根)、硒氰根的咪唑类阳离子盐类,如1,3-二甲基-3-咪唑碘;
D表示一种有机溶剂或者几种有机溶剂的混合物,离子液体或者几种离子液体的混合物,离子液体与有机溶剂的混合物,水或者水与有机溶剂或离子液体的混合物,如水、腈类、酰胺类溶剂、醇类、1-甲基-3-丙基咪唑碘等;
E表示N-甲基苯并咪唑、苯并咪唑等暗电流抑制剂或者添加剂的一种或多种;
a,b,c,d,e分别表示A、B、C、D、E的质量分数,并且其范围为:0≤a≤70%,0≤b≤70%,0≤c≤70%,0.01%≤d≤99.99%,0≤e≤70%。
本发明的第三个目的在于提供上述所述方法制得的光引发不可逆凝胶电解质,可应用于染料敏化太阳电池和其它电池器件。
一种染料敏化太阳电池,包括光阳极、对电极和设置在光阳极、对电极之间的准固态电解质,所述电解质为本发明上述所述的光引发不可逆凝胶电解质。
与现有技术相比,本发明具有如下有益效果:
本发明采用光引发方法制备不可逆凝胶电解质,具有制备简单、成本廉价、热稳定性优异等特点。将本发明的电解质应用在染料敏化太阳电池中,制得的电池具有较高效的光电性能(有效面积为0.25cm2,效率可达5%以上),且可保障器件的长期稳定性。同时,本发明涉及的光引发不可逆凝胶电解质具有优良的柔韧性,适用于柔性器件。
附图说明
图1为本发明的光引发不可逆凝胶电解质的实物照片;
图2为本发明应用实施例1中制得的基于光引发不可逆凝胶电解质的染料敏化太阳电池的J-V曲线。
具体实施方式
下面结合具体实施案例和附图对本发明作进一步详细说明。本实施案例在以本发明技术为前提下进行实施,现给出详细的实施方式和具体的操作过程来说明本发明具有创造性,但本发明的保护范围不限于以下的实施案例。
根据本申请包含的信息,对于本领域技术人员来说可以轻而易举地对本发明的精确描述进行各种改变,而不会偏离所附权利要求的精神和范围。应该理解,本发明的范围不局限于所限定的过程、性质或组分,因为这些实施方案以及其他的描述仅仅是为了示意性说明本发明的特定方面。实际上,本领域或相关领域的技术人员明显能够对本发明实施方式做出的各种改变都涵盖在所附权利要求的范围内。
为了更好地理解本发明而不是限制本发明的范围,在本申请中所用的表示用量、百分比的所有数字、以及其他数值,在所有情况下都应理解为以词语“大约”所修饰。因此,除非特别说明,否则在说明书和所附权利要求书中所列出的数字参数都是近似值,其可能会根据试图获得的理想性质的不同而加以改变。各个数字参数至少应被看作是根据所报告的有效数字和通过常规的四舍五入方法而获得的。
实施例1
本实施例的一种光引发不可逆凝胶电解质的制备方法,所述方法包括如下步骤:
分别称取160mg聚乙烯醇肉桂酸酯(聚合物单体)、60mg 2-羟基-2-甲基-1-苯基-1-丙酮(光引发剂)和1g二甲基甲酰胺(有机溶剂)于样品瓶中,超声20min使其分散,然后将混合液体置于100μm厚的膜具中紫外光照射1min使其形成具有稳定三维网络结构的不可逆凝胶,所述液体表面处紫外光功率密度为100mw/cm2;随后将所述凝胶置于0.5ml的液态电解质中,吸附10min后取出,此时光引发不可逆凝胶电解质制备完成。所述液态电解质包括:1mol/L 1,3-二甲基-3-咪唑碘(DMII),0.1mol/L碘化锂,0.13mol/L硫氰酸胍,0.11mol/L碘,0.7mol/L 4-叔丁基吡啶,溶剂为体积比为85:15的乙腈和戊腈的混合溶液。
实施例2
本实施例的一种光引发不可逆凝胶电解质的制备方法,所述方法包括如下步骤:
分别称取50mg聚乙烯醇肉桂酸酯)、15mg 2-羟基-2-甲基-1-苯基-1-丙酮和1g3-甲氧基丙腈于样品瓶中,超声20min使其分散;然后将混合液体置于100μm厚的膜具中紫外光照射12h使其形成具有稳定三维网络结构的不可逆凝胶,所述液体表面处紫外光功率密度为10mw/cm2;随后将所述凝胶置于0.5ml的液态电解质中,吸附1h后取出,此时光引发不可逆凝胶电解质制备完成。所述液态电解质包括:1mol/L 1,3-二甲基-3-咪唑碘(DMII),0.12mol/L氯化钠,0.13mol/L硫氰酸胍,0.11mol/L碘,0.7mol/L4-叔丁基吡啶,溶剂为体积比为85:15的乙腈和乙醇的混合溶液。
实施例3
本实施例的一种光引发不可逆凝胶电解质的制备方法,所述方法包括如下步骤:
分别称取500mg聚乙烯醇肉桂酸酯、200mg 2-羟基-2-甲基-1-苯基-1-丙酮和1g乙腈于样品瓶中,超声30min使其分散,然后将混合液体置于100μm厚的膜具中紫外光照射0.5min使其形成具有稳定三维网络结构的不可逆凝胶,所述液体表面处紫外光功率密度为200mw/cm2;随后将所述凝胶置于10ml的液态电解质中,吸附50h后取出,此时光引发不可逆凝胶电解质制备完成。所述液态电解质包括:1mol/L 1,3-二甲基-3-咪唑碘(DMII),0.1mol/L碘化钾,0.15mol/L硒氰酸胍,0.11mol/L碘,0.6mol/L 4-叔丁基吡啶,溶剂为体积比为75:25的乙腈和水的混合溶液。
实施例4
本实施例的一种光引发不可逆凝胶电解质的制备方法,所述方法包括如下步骤:
分别称取10mg聚乙烯醇肉桂酸酯、1mg 2-羟基-2-甲基-1-苯基-1-丙酮和1g N-甲基-2-吡咯烷酮于样品瓶中,超声15min使其分散;然后将混合液体置于100μm厚的膜具中紫外光照射1s使其形成具有稳定三维网络结构的不可逆凝胶,所述液体表面处紫外光功率密度为200mw/cm2;随后将所述凝胶置于0.5ml的液态电解质中,吸附36s后取出,此时光引发不可逆凝胶电解质制备完成。所述液态电解质包括:1mol/L 1,3-二甲基-3-咪唑碘(DMII),0.13mol/L氯化钾,0.11mol/L硫氰酸胍,0.15mol/L碘,0.5mol/L 4-叔丁基吡啶,溶剂为体积比为75:25的乙醇和水的混合溶液。
应用实施例1
将本发明上述实施例1制得的光引发不可逆凝胶电解质应用于制备准固态染料敏化太阳能电池,所述电池采用如下方法制得:
利用丝网印刷技术将TiO2纳米颗粒印刷在洗净的FTO导电玻璃上,控制其厚度11μm左右,在程序控温马弗炉中510℃热处理30min,待冷却至室温后,于70℃下浸泡于30mMTiCl4的水溶液中20min,然后510℃高温烧结30min,冷却到120℃时,将其浸泡于N719染料中16h,取出即可得到吸附N719染料的光阳极。用含氯铂酸的异丙醇溶液涂在另一块洗净的FTO导电玻璃上,在410℃高温煅烧30min,冷却到室温得到含Pt的对电极。最后利用三明治的方法将所述光引发不可逆凝胶电解质置于光阳极和对电极之间,组装成电池。
图2为本应用实施例1中制得的基于光引发不可逆凝胶电解质的染料敏化太阳电池的J-V曲线。
表1为图2所示J-V曲线所对应的染料敏化太阳的光伏性能参数。由表1可以得到,基于发明中所涉及的光引发不可逆凝胶电解质所组装的染料敏化太阳电池,在AM1.5(100mW/cm2)测试条件下,可获得开路电压为648mV,短路电流密度为13.26mA·cm-2,填充因子为65,光电转换效率为5.19%的光伏性能。
表1
Claims (8)
2.权利要求1所述的光引发不可逆凝胶电解质的制备方法,其特征在于:所述方法包括如下步骤:
(1)将聚合物单体溶解在有机溶剂中,然后加入光引发剂,超声分散均匀,获得混合液体;
(2)将步骤(1)所得混合液体置于紫外光下照射,使聚合物单体发生聚合反应,形成具有稳定三维网络结构的不可逆凝胶;
(3)将步骤(2)制得的凝胶去吸附含有I-/I3 -氧化还原电对的液态电解液,形成所述光引发不可逆凝胶电解质。
3.根据权利要求2所述的光引发不可逆凝胶电解质的制备方法,其特征在于:步骤(1)所述有机溶剂为乙腈、N-甲基-2-吡咯烷酮、二甲基甲酰胺、乙醇、3-甲氧基丙腈中的一种或多种混合。
4.根据权利要求2所述的光引发不可逆凝胶电解质的制备方法,其特征在于:步骤(1)所述聚合物单体在有机溶剂中的含量为1~50 wt%,所述光引发剂在有机溶剂中的含量为0.1~50 wt%。
5.根据权利要求2所述的光引发不可逆凝胶电解质的制备方法,其特征在于:步骤(2)所述紫外光照射液体表面的功率密度为1 mW/cm2~200 mW/cm2,紫外光照射的时间为1 s~24 h。
6.根据权利要求2所述的光引发不可逆凝胶电解质的制备方法,其特征在于:步骤(3)所述凝胶吸附电解液的时间为0.01~50 h。
7.根据权利要求2所述的光引发不可逆凝胶电解质的制备方法,其特征在于:步骤(3)所述液态电解质的配方通式为:
aA+bB+cC+dD+eE;
通式中:
A表示卤素氟、氯、溴、碘或拟卤素氰根、硫氰根;
B表示卤素氟、氯、溴、碘或拟卤素氰根、硫氰根、高氯酸根的一价、二价或三价金属阳离子或非金属阳离子盐类;
C表示卤素、拟卤素、硒氰根的咪唑类阳离子盐类;
D表示一种有机溶剂或者几种有机溶剂的混合物,离子液体或者几种离子液体的混合物,离子液体与有机溶剂的混合物,水或者水与有机溶剂或离子液体的混合物;
E表示N-甲基苯并咪唑、苯并咪唑暗电流抑制剂或者添加剂的一种或多种;
a,b,c,d,e分别表示A、B、C、D、E的质量分数,并且其范围为:0≤a≤70%,0≤b≤70%,0≤c≤70%,0.01%≤d≤99.99%,0≤e≤70%。
8.权利要求1所述的光引发不可逆凝胶电解质在制备染料敏化太阳电池中的应用。
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