CN116239855B - 一种透明聚合物网络骨架复合凝胶电解质薄膜及其制备方法和应用 - Google Patents
一种透明聚合物网络骨架复合凝胶电解质薄膜及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种透明聚合物网络骨架复合凝胶电解质薄膜及其制备方法和应用,属于电致变色器件领域,该复合凝胶电解质薄膜包括聚合物网络骨架以及均匀分布于所述聚合物网络骨架中的强极性塑性晶体、混合增塑剂和金属锂盐,聚合物网络骨架由聚合物单体原位热触发交联形成,聚合物单体、强极性塑性晶体、混合增塑剂和金属锂盐的质量比为13~24:8~32:15~33:1。本发明的透明聚合物网络骨架复合凝胶电解质薄膜的制备方法简单、原料易得、易于大规模生产,且具有可见光透明度高、离子电导率高、机械强度良好的特点。
Description
技术领域
本发明涉及电致变色器件领域,具体涉及一种透明聚合物网络骨架复合凝胶电解质薄膜及其制备方法和应用。
背景技术
聚合物电解质由于其良好的机械性能,易实现的高透明度,可作为电致变色器件离子存储层材料应用,但常温下聚合物电解质的离子电导率低,界面阻抗较大,仍需进一步改进来满足实际使用的需求。研究工作发现,向聚合物基体中加入增塑剂可以有效改善离子电导率低、界面阻抗较大的问题,常用的碳酸乙烯酯、碳酸丙烯酯等液体增塑剂本身粘度低而极性不够强,虽然一定程度上改善了界面阻抗和离子电导率,但削减了聚合物电解质机械性能,不利于成膜。因此,仅仅通过添加适量增塑剂较难将聚合物电解质的离子电导率提升至理想水平,从而满足电致变色器件所需响应速度。
无机填料丁二腈(SN)是一种强极性小分子塑晶,室温下呈蜡状,相同体积下较液态增塑剂能更进一步改善机械性能。目前主要研究集中在将包含SN的电解液混合液贮存于韧性高的聚合物基底微孔中,协同搭建三维导锂离子通道,如公开号为CN115051028A的中国专利文献公开了一种纳米纤维基复合固态电解质,以具有三维互通网络结构的导电聚合物纳米纤维膜为基底,将电解质溶液(丁二腈、锂盐和离子液体的混合物)涂覆于纳米纤维膜表面并渗透至三维互通网络的纳米纤维膜的介微孔中,得到。然而上述方法中,SN无法完全渗透到膜整体,且不同相之间的界面传输阻抗对离子电导率有抑制作用,另外,产品薄膜不透明,难以应用于电致变色器件中。
公开号为CN110527229A的中国专利文献公开了一种全固态塑性晶体柔性电解质薄膜,该发明以聚乙烯醇、聚乙烯醇缩丁醛等高分子化合物为基体,锂盐为碱金属盐,无机纳米粒子(纳米ZrO2或纳米Ta2O5)为电解质添加剂,采用浇铸法或熔融挤出法两种制备方法得到产品电解质薄膜,但是可能存在溶剂挥发过程较长、进而导致电解液不能均匀分散的问题。
发明内容
为了解决现有技术中相分离所导致的离子迁移率低及透明度低的问题,本发明提供了一种透明聚合物网络骨架复合凝胶电解质薄膜,具备三维交联骨架内“锁”有电解液的结构,可自愈、粘弹性高,塑性晶体分布均匀,且可见光透明度高、离子电导率高、机械强度良好。
具体采用的技术方案如下:
一种透明聚合物网络骨架复合凝胶电解质薄膜,包括聚合物网络骨架以及均匀分布于所述聚合物网络骨架中的强极性塑性晶体、混合增塑剂和金属锂盐,聚合物网络骨架由聚合物单体原位热触发交联形成,聚合物单体、强极性塑性晶体、混合增塑剂和金属锂盐的质量比为13~24:8~32:15~33:1。
所述的强极性塑性晶体包括丁二腈;
所述的混合增塑剂包括碳酸丙烯酯、碳酸乙烯酯、碳酸二乙酯、碳酸甲乙酯、二甲基甲酰胺、r-丁内酯、PEG400(聚乙二醇)、PPG1000(聚丙二醇)、甲酸甲酯、乙酸甲酯、四氢呋喃、1,2-二甲氧基乙烷中的至少两种;
所述的聚合物单体包括但不限于甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯、甲基丙烯酸丁酯等;
所述的金属锂盐包括高氯酸锂、六氟磷酸锂、二氟草酸硼酸锂、双三氟甲基磺酰亚胺锂、六氟砷酸锂、四氟硼酸锂、二草酸硼酸锂、三氟甲基磺酸锂中的至少一种。
本发明还提供了所述的透明聚合物网络骨架复合凝胶电解质薄膜的制备方法,包括以下步骤:
(1)以聚合物单体、引发剂、交联剂、强极性塑性晶体、混合增塑剂和金属锂盐为原料制备前驱体溶液;
(2)将前驱体溶液热交联,得到所述的透明聚合物网络骨架复合凝胶电解质薄膜。
本发明利用强极性塑性晶体与混合增塑剂、聚合物单元之间的相互作用,通过原位热触发聚合,制备结构均匀的聚合物交联网络,使塑性晶体在交联网络中均匀分布,形成有效离子传输通道。
优选的,以聚合物单体重量为100%计,引发剂的加入量为0.1wt%~0.5wt%,交联剂的加入量为1wt%~5wt%;引发剂包括偶氮二异丁腈、过氧化苯甲酰、二苯甲酮中的至少一种,交联剂选用有机硅交联剂。
步骤(2)中,可以采用一步热交联制备得到所述的透明聚合物网络骨架复合凝胶电解质薄膜,也可以采用两步热交联制备,当采用一步热交联方法时,热交联的参数为:50~70℃,2-6h,当采用两步热交联方法时,第一步交联的参数为:50~60℃,0.5~2h,第二步交联的参数为:60~70℃,2~4h。
本发明还提供了一种电致变色器件,结构包含所述的透明聚合物网络骨架复合凝胶电解质薄膜。优选的,所述的电致变色器件的结构包括依序叠置的如下部件:基底层、集流层、电致变色层、所述的透明聚合物网络骨架复合凝胶电解质薄膜、离子存储层、集流层、基底层。
该复合凝胶电解质薄膜制得的电致变色器件界面阻抗低,循环性能好,同时,由于该复合凝胶电解质薄膜自身优良的弹性、韧性和热固性,增强了电致变色器件的机械性能和耐热性能。
该透明聚合物网络骨架复合凝胶电解质薄膜离子电导率高,主要用于在正负极之间传输锂离子,且其可见光透明度高、不会影响电致变色层的变化。
所述的电致变色器件的制备方法为:
(1)以聚合物单体、引发剂、交联剂、强极性塑性晶体、混合增塑剂和金属锂盐为原料制备前驱体溶液;
(2)将前驱体溶液在50~60℃下进行第一步交联0.5~2h,制备得到预交联凝胶电解质薄膜;
(3)将步骤(2)得到的预交联凝胶电解质薄膜与基底层、集流层、电致变色层和离子存储层依序组装完毕后,加固并抽真空封装得到电致变色原件,将电致变色原件在60~70℃下进行第二步交联2~4h,得到电致变色器件。
在制备电致变色器件的过程中,所述的透明聚合物网络骨架复合凝胶电解质薄膜两步热交联成型,分两步进行热交联,第一步得到有一定交联度的预交联凝胶电解质薄膜,第二步再组装成器件后进一步固化,既有效避免热凝胶效应的影响,又使电解质膜与电极有良好接触。如果将未交联溶液直接注入器件中加热固化,可能由于热凝胶效应导致聚合物电解质分布不均,与电极接触不均匀,影响变色效果和循环稳定性;而如果将完全交联的凝胶电解质薄膜与器件组装,存在接触不良的问题,并且由于交联网络结构特殊的热固化性能,无法像一般聚合物电解质在组装完成后再次受热融化后冷却成膜而与电极有良好接触。
优选的,电致变色器件的组装过程中,真空度范围小于133MPa。
与现有技术相比,本发明的有益效果在于:
(1)本发明利用聚合物单体溶液原位热触发自由基聚合形成三维交联网络结构,强极性塑性晶体均匀分布于所述聚合物网络骨架中,共同搭建三维导锂离子通道,同时利用三维交联网络的凝胶溶胀特性,封锁锂离子活性导电液体。三维交联网络结构提高了透明聚合物网络骨架复合凝胶电解质薄膜的机械强度,实现柔性可自愈高粘弹性。另外,本发明的透明聚合物网络骨架复合凝胶电解质薄膜的制备方法简单、原料易得、易于大规模生产,且具有可见光透明度高、离子电导率高、机械强度良好的特点。
(2)本发明制备方法与采用强极性溶剂溶解聚合物基体颗粒的传统流延法相比,无需溶剂挥发,一方面简化工序,另一方面避免溶剂挥发过程所导致的高浓度塑性晶体及电解液不能均匀分散的问题,从而改进其制得的电致变色器件的性能,避免电致变色器件工作过程出现的空间选择性电致变色成像缺陷。
(3)本发明利用预交联凝胶电解质薄膜初步组装成电致变色原件,再进行第二步交联处理得到电致变色器件,取代直接在电致变色器件中灌注溶液热引发成膜,改善了凝胶效应带来的反应不均,以及电解质层两侧接触不良问题。
附图说明
图1为实施例1和对比例1中产品薄膜的交流阻抗谱图,其中,A为实施例1(PMMA/PC/SN),B为对比例1(PMMA/PC)。
图2为实施例1和对比例1中产品薄膜的电流-时间曲线。
图3为实施例1中透明聚合物网络骨架复合凝胶电解质薄膜的伏安曲线。
图4为实施例5中电致变色器件的透射光谱图。
图5为实施例5中电致变色器件在不同电化学状态下变色前后的光学图片,其中A为变色前,B为变色后。
具体实施方式
下面结合实施例与附图,进一步阐明本发明。应理解,这些实施例仅用于说明本发明,而不用于限制本发明的范围。
实施例1透明聚合物网络骨架复合凝胶电解质薄膜的制备
S1.将MMA(甲基丙烯酸甲酯)、AIBN(偶氮二异丁腈)和EDGMA(二甲基丙烯酸乙二醇酯)按质量比1:0.03:0.3(6g MMA单体溶液、0.018g AIBN和0.18g EDGMA)加入至三颈烧瓶中,采用智能数显磁力搅拌器搅拌直至三颈烧瓶内形成澄清透明溶液,搅拌温度30℃,搅拌速度600rpm;进一步向该澄清透明溶液中加入3.5g PC(碳酸丙烯酯),4.0g EC(碳酸乙烯酯),2.5g SN(丁二腈),继续保持上述条件搅拌均匀;再加入0.3g LiClO4,氮气拂扫5min,继续保持上述条件搅拌6h,使活性锂盐在溶液中充分溶解并电离,制备得到前驱体溶液;
S2.透明聚合物网络骨架复合凝胶电解质薄膜制备:将前驱体溶液自然流延至模具中,放入烘箱中60℃交联2h,使SN和PC、EC、LiClO4有序均匀分散于由MMA单体交联而成的聚合物构建的三维导离子网络中,得到透明聚合物网络骨架复合凝胶电解质薄膜。
实施例2透明聚合物网络骨架复合凝胶电解质薄膜的制备
本实施例中透明聚合物网络骨架复合凝胶电解质薄膜的制备方法与实施例1中的区别仅在于,步骤S1中,丁二腈添加量为3.5g。
实施例3透明聚合物网络骨架复合凝胶电解质薄膜的制备
本实施例中透明聚合物网络骨架复合凝胶电解质薄膜的制备方法与实施例1中的区别仅在于,步骤S1中,丁二腈添加量为6.5g。
实施例4透明聚合物网络骨架复合凝胶电解质薄膜的制备
本实施例中透明聚合物网络骨架复合凝胶电解质薄膜的制备方法与实施例1中的区别仅在于,步骤S1中,聚合物单体选用丙烯酸丁酯,金属锂盐选用氟磷酸锂,添加量为0.25g,步骤S2中,放入烘箱中先50℃交联0.5h,再70℃交联2h。
对比例1
本对比例中的凝胶聚合物电解质薄膜与实施例1中的透明聚合物网络骨架复合凝胶电解质薄膜的制备方法区别仅在于,步骤S1中,不添加丁二腈。
对比例2
本对比例中的凝胶聚合物电解质薄膜与实施例1中的透明聚合物网络骨架复合凝胶电解质薄膜的制备方法区别在于,步骤S1中,不添加6gMMA单体溶液、0.018g AIBN和0.18g EDGMA,而是添加6.18gPMMA聚合物,由25g丙酮溶解,进一步按照实施例1中的方法加入极性塑性晶体、混合增塑剂和金属锂盐制备得到前驱体溶液;步骤S2中,将该前驱体溶液在真空烘箱内60℃下烘24h得到凝胶聚合物电解质薄膜。
实施例5电致变色器件的制备
本实施例中,电致变色器件的制备方法包括以下步骤:
S1.将MMA(甲基丙烯酸甲酯)、AIBN(偶氮二异丁腈)和EDGMA(二甲基丙烯酸乙二醇酯)按质量比1:0.03:0.3(6g MMA单体溶液、0.018g AIBN和0.18g EDGMA)加入至三颈烧瓶中,采用智能数显磁力搅拌器搅拌直至三颈烧瓶内形成澄清透明溶液,搅拌温度30℃,搅拌速度600rpm;进一步向该澄清透明溶液中加入3.5g PC(碳酸丙烯酯),4.0g EC(碳酸乙烯酯),6.5g SN(丁二腈),继续保持上述条件搅拌均匀;再加入0.3g LiClO4,氮气拂扫5min,继续保持上述条件搅拌6h,使活性锂盐在溶液中充分溶解并电离,制备得到前驱体溶液;
S2.透明聚合物网络骨架复合凝胶电解质薄膜制备:将前驱体溶液自然流延至模具中,放入烘箱中60℃预交联1h,使SN和PC、EC、LiClO4有序均匀分散于由MMA单体交联而成的聚合物构建的三维导离子网络中,得到透明聚合物网络骨架复合凝胶电解质薄膜。
S3.电致变色器件的制备:用切片机剪裁S2制得的透明聚合物网络骨架复合凝胶电解质薄膜为10cm×10cm的方形薄片,采用10cm×10cm的正负极组装成结构为:玻璃/ITO/WO3/S2制得的复合凝胶电解质薄膜/NiO/ITO/玻璃的器件原型,将器件真空密封后放入真空烘箱内,60℃下4h完成固化交联,即得到结合紧密的电致变色器件。
对比例3电致变色器件的制备
本实施例中电致变色器件的制备方法与实施例5中的区别仅在于,采用对比例2所制备凝胶聚合物电解质薄膜组装电致变色器件,将器件真空密封后放入真空烘箱内,140℃下加热0.5h,即得到结合紧密的电致变色器件。
样品分析
1、离子电导率
交流阻抗谱测试是将待测产品电解质薄膜夹在阻塞电极之间,使用荷兰IVIUM电化学工作站,将实施例1~4制备的复合凝胶电解质薄膜和对比例1~2制备的凝胶聚合物电解质薄膜进行离子电导率测试,实施例1~3的变量为加入SN与碳酸酯类增塑剂的体积比,经测试可知,实施例中复合凝胶电解质薄膜的离子电导率都高于对比例1,实施例1和对比例1中产品薄膜的交流阻抗谱图分别如图1中的A和B所示,当SN添加量为6.5g时,室温下离子电导率可达到1.2×10-2S/cm,明显高于对比例1、2。
2、锂离子迁移率测试
锂离子迁移率测试将待测产品电解质薄膜夹在阻塞电极之间,使用上海辰华CHI604B电化学工作站,将实施例1~4和对比例1-2制备的产品电解质薄膜进行恒压下电流随时间变化曲线测试。实施例1和对比例1中产品薄膜的电流-时间曲线如图2所示,由图可见,实施例1中复合凝胶电解质薄膜的锂离子迁移率在0.35左右,对比例1中凝胶聚合物电解质薄膜的锂离子迁移率在0.2左右,说明添加丁二腈可有效提高锂离子传输效率。
3、电化学窗口测试
电化学窗口测试将待测产品电解质薄膜夹在阻塞电极之间,使用上海辰华CHI604B电化学工作站,实施例1中透明聚合物网络骨架复合凝胶电解质薄膜的伏安曲线如图3所示。由图可见,该复合凝胶电解质薄膜在±4V内均处于稳定状态,具有良好电化学稳定性。
4、电致变色器件测试
电致变色器件性能测试采用紫外分光光度计和电化学工作站,测试实施例5中的电致变色器件的透射光谱,如图4所示,实施例5中电致变色器件的电化学稳定性较高,器件在-3.5V处呈褪色态,在3.5V处呈深蓝色着色态,695nm处调制幅度为50%;图5为该电致变色器件在不同电化学状态下变色前后的光学图片,其中A为变色前,B为变色后,表明该电致变色器件具有良好的变色性能。对比例3中直接利用PMMA制得的薄膜组装得到的器件由于接触不良,产生变色不均现象,同时循环稳定性差,难以实现实际应用。
以上所述的实施例对本发明的技术方案进行了详细说明,应理解的是以上所述的仅为本发明的具体实施例,并不用于限制本发明,凡在本发明的原则范围内所做的任何修改、补充或类似方式替代等,均应包含在本发明的保护范围之内。
Claims (4)
1.一种电致变色器件,其特征在于,所述的电致变色器件的结构包括依序叠置的如下部件:基底层、集流层、电致变色层、透明聚合物网络骨架复合凝胶电解质薄膜、离子存储层、集流层、基底层;
所述的透明聚合物网络骨架复合凝胶电解质薄膜包括聚合物网络骨架以及均匀分布于所述聚合物网络骨架中的强极性塑性晶体、混合增塑剂和金属锂盐,聚合物网络骨架由聚合物单体原位热触发交联形成,聚合物单体、强极性塑性晶体、混合增塑剂和金属锂盐的质量比为13~24:8~32:15~33:1;
所述的电致变色器件的制备方法为:
(1)以聚合物单体、引发剂、交联剂、强极性塑性晶体、混合增塑剂和金属锂盐为原料制备前驱体溶液;
(2)将前驱体溶液在50~60℃下进行第一步交联0.5~2h,制备得到预交联凝胶电解质薄膜;
(3)将步骤(2)得到的预交联凝胶电解质薄膜与基底层、集流层、电致变色层和离子存储层依序组装完毕后,加固并抽真空封装得到电致变色原件,将电致变色原件在60~70℃下进行第二步交联2~4h,得到电致变色器件。
2.根据权利要求1所述的电致变色器件,其特征在于,所述的强极性塑性晶体包括丁二腈;所述的混合增塑剂包括碳酸丙烯酯、碳酸乙烯酯、碳酸二乙酯、碳酸甲乙酯、二甲基甲酰胺、r-丁内酯、聚乙二醇、聚丙二醇、甲酸甲酯、乙酸甲酯、四氢呋喃、1,2-二甲氧基乙烷中的至少两种。
3.根据权利要求1所述的电致变色器件,其特征在于,所述的聚合物单体包括甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯或甲基丙烯酸丁酯;所述的金属锂盐包括高氯酸锂、六氟磷酸锂、二氟草酸硼酸锂、双三氟甲基磺酰亚胺锂、六氟砷酸锂、四氟硼酸锂、二草酸硼酸锂、三氟甲基磺酸锂中的至少一种。
4.根据权利要求1所述的电致变色器件,其特征在于,以聚合物单体重量为100%计,引发剂的加入量为0.1wt%~0.5wt%,交联剂的加入量为1wt%~5wt%;引发剂包括偶氮二异丁腈、过氧化苯甲酰、二苯甲酮中的至少一种,交联剂选用有机硅交联剂。
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