CN113299869B - 一种用于抑制锌离子电池/电容器中锌枝晶生长的方法 - Google Patents
一种用于抑制锌离子电池/电容器中锌枝晶生长的方法 Download PDFInfo
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Abstract
本发明公开了一种用于抑制锌离子电池/电容器中锌枝晶生长的方法,属于电化学镀锌和锌离子电池/电容器技术领域。本发明通过以导电柔性基底为工作电极,锌片用作对电极和参比电极,配置硫酸锌和柠檬酸钠的混合溶液作为电沉积液,在‑1.8V的电压下沉积锌晶种,使导电柔性基底表面沉积一层锌晶种,随后在‑0.8V的电压下继续沉积,得到柔性的锌阳极;以硫酸锌和柠檬酸钠的混合溶液与聚乙烯醇混匀并搅拌至凝胶呈无色透明状,得到固态凝胶电解质;将锌阳极、阴极材料和固态凝胶电解质组装成无枝晶生长的柔性锌离子电池/电容器。本发明电解液中的柠檬酸钠可有效减少锌离子周围的水分子,并减小去锌离子溶剂化能,从而可达到抑制锌枝晶生长的目的。
Description
技术领域
本发明涉及电化学镀锌和锌离子电池/电容器技术领域,具体涉及一种含有抑制锌枝晶生长电解液的一维柔性锌离子电池的制备方法。
背景技术
随着可穿戴电子设备的快速发展,开发一种柔性的且无锌枝晶生长的锌离子电池/电容器已经成为了一个重要的研究方向。在重复充放电过程中,锌枝晶的生长会破坏器件的电化学稳定性能。通常,通过使用高导电性或亲锌基底制备锌电极、对锌电极表面进行修饰和使用高浓度电极液或在电解液中加入添加剂等方法都可有效抑制锌枝晶的生长。例如,通过使用三维碳纳米框架、金属铜或锡等基底制备锌阳极,在锌阳极表面涂覆碳酸钙等绝缘层或石墨烯和碳纳米管等高导电层,以及使用水包油式的高浓度电解液或在电解液中加入尿素等添加剂等方法都可有效抑制锌枝晶的生长。(Nat.Commun.,2015,6,8058;Angew.Chem.Int.Ed.2019,58,15841-15847.;Adv.Mater.Interfaces 2018,5,1800848;ACS Appl.Mater.Interfaces 2018,10,25446-25453;Adv.Energy Mater.2019,9,1901469;Nat.Mater.2018,17,543-549;ACS Appl.Mater.Interfaces 2017,9,9681-9687.)。在上述抑制锌枝晶生长的方法中,在电解液中加入添加剂更加适用于一维柔性锌离子电池/电容器的制备,且操作更为简单,因此,通过对锌离子电池/电容器的电解液进行调控成为抑制锌枝晶生长的一个研究热点。
发明内容
本发明的目的在于解决锌离子电池/电容器中锌枝晶生长的问题,提供一种工艺简单,成本低,更适用于抑制一维锌离子电池/电容器中锌枝晶生长的方法。
为了达到上述目的,本发明采用了下列技术方案:
一种用于抑制锌离子电池/电容器中锌枝晶生长的方法,包括以下步骤:
步骤1,以导电柔性基底为工作电极,锌片用作对电极和参比电极,配置硫酸锌和柠檬酸钠的混合溶液作为电沉积液,在-1.8V的电压下沉积锌晶种,使导电柔性基底表面沉积一层锌晶种,随后在-0.8V的电压下继续沉积,得到柔性的锌阳极;
步骤2,以硫酸锌和柠檬酸钠的混合溶液与聚乙烯醇混匀并搅拌至凝胶呈无色透明状,得到固态凝胶电解质;
步骤3,将锌阳极、阴极材料和固态凝胶电解质组装成无枝晶生长的柔性锌离子电池/电容器。
进一步,所述步骤1中导电柔性基底为碳纤维、碳布、钢丝或碳纤维布中的任意一种。
进一步,所述步骤1)中在-1.8V的电压下沉积锌晶种的时间为20-200s。
进一步,所述步骤1)中在-0.8V的电压下沉积金属锌的时间为100s-1800s。
进一步,所述步骤1)中硫酸锌的浓度为1-3mol/L,柠檬酸钠的浓度为0.05-0.2mol/L。
进一步,所述步骤2)中硫酸锌的浓度为1-3mol/L,柠檬酸钠的浓度为0.05-0.2mol/L。
进一步,所述步骤2)中搅拌温度为80℃。
进一步,所述硫酸锌和柠檬酸钠的混合溶液与聚乙烯醇的用量比为10mL:1g。
进一步,所述步骤3)中阴极材料为用作锌离子电池/电容器的阴极材料。
进一步,所述步骤3)中阴极材料为聚吡咯、聚苯胺、石墨烯、活性炭中的任意一种。
与现有技术相比本发明具有以下优点:
1、本发明中,电解液中的柠檬酸钠可有效减少锌离子周围的水分子,并减小去锌离子溶剂化能,从而可达到抑制锌枝晶生长的目的。
2、本发明中在制备锌阳极时,沉积液中加入柠檬酸钠可促进锌阳极形成由颗粒状组成的岩石状结构,使得锌阳极的表面分布更加均匀。
3、本发明中在制备锌阳极时,现在-1.8V点位下使柔性基底表面生成锌晶种,再在-0.8V的电位下沉积金属锌,可使得锌金属沉积更加均匀。
附图说明
图1为本发明实施例1中制备的柔性锌阳极在不同放大倍数的扫描电子显微镜图。
图2为本发明实施例1中制备的固态柔性锌离子电池在扫描速率为5mV/s的循环伏安曲线。该器件的循环伏安曲线呈现出明显的氧化还原峰。
图3为本发明实施例1中制备的固态柔性锌离子电池在电流密度为0.16A/g的放电曲线。质量电容达到116mAh/g,表现出良好的电容性能。
图4为本发明实施例2中制备的柔性锌阳极组装成对称电池的稳定性测试,其中电流密度为2mA/cm,容量为0.5mAh/cm,对称电池表现出平稳的充放电平台,表现出良好的电化学稳定性。
图5为本发明实施例3中制备的柔性锌离子电容器经过1000次循环后的扫描电子显微镜图,观察不到锌枝晶的生成。
图6为本发明实施例4中制备的柔性锌离子电容器循环前和经过1000次循环后的X射线衍射谱图,反应前后锌阳极的X射线衍射谱图几乎相同,观察不到副产物生成。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
一种用于抑制锌离子电池中锌枝晶生长的方法,包括如下步骤:
1)以碳纤维为工作电极,锌片用作对电极和参比电极,配置1mol/L的硫酸锌和0.05mol/L柠檬酸钠的混合溶液作为电沉积液,先在-1.8V的电压下沉积30s,使导电柔性基底表面沉积一层锌晶种,随后在-0.8V的电压下沉积170s,得到柔性的锌阳极;
2)以10mL 1mol/L的硫酸锌和0.05mol/L柠檬酸钠的混合溶液与0.1g/mL聚乙烯醇均匀混合并在80℃下搅拌至凝胶呈无色透明状,得到固态凝胶电解质。
3)将锌阳极、聚吡咯和凝胶电解质组装成无枝晶生长的柔性锌离子电池。
图1为本发明实施例1中制备的柔性锌阳极在不同放大倍数的扫描电子显微镜图。
图2为本发明实施例1中制备的固态柔性锌离子电池在扫描速率为5mV/s的循环伏安曲线。该器件的循环伏安曲线呈现出明显的氧化还原峰。
图3为本发明实施例1中制备的固态柔性锌离子电池在电流密度为0.16A/g的放电曲线。质量电容达到116mAh/g,表现出良好的电容性能。
实施例2
一种用于抑制锌离子电池中锌枝晶生长的方法,包括如下步骤:
1)以碳布为工作电极,锌片用作对电极和参比电极,配置1.5mol/L的硫酸锌和0.1mol/L柠檬酸钠的混合溶液作为电沉积液,先在-1.8V的电压下沉积100s,使导电柔性基底表面沉积一层锌晶种,随后在-0.8V的电压下沉积900s,得到柔性的锌阳极;
2)以10mL 1.5mol/L的硫酸锌和0.1mol/L柠檬酸钠的混合溶液与0.1g/mL聚乙烯醇均匀混合并在80℃下搅拌至凝胶呈无色透明状,得到固态凝胶电解质。
3)将锌阳极、聚苯胺和凝胶电解质组装成无枝晶生长的柔性锌离子电池。
图4为本发明实施例2中制备的柔性锌阳极组装成对称电池的稳定性测试,其中电流密度为0.02mA/cm,容量为0.5mAh/cm为5mV/s,对称电池表现出平稳的充放电平台,表现出良好的电化学稳定性。
实施例3
一种用于抑制锌离子电容器中锌枝晶生长的方法,包括如下步骤:
1)以钢丝为工作电极,锌片用作对电极和参比电极,配置2mol/L的硫酸锌和0.15mol/L柠檬酸钠的混合溶液作为电沉积液,先在-1.8V的电压下沉积50s,使导电柔性基底表面沉积一层锌晶种,随后在-0.8V的电压下沉积350s,得到柔性的锌阳极;
2)以10mL 2mol/L的硫酸锌和0.15mol/L柠檬酸钠的混合溶液与0.1g/mL聚乙烯醇均匀混合并在80℃下搅拌至凝胶呈无色透明状,得到固态凝胶电解质。
3)将锌阳极、石墨烯和凝胶电解质组装成无枝晶生长的柔性锌离子电容器。
图5为本发明实施例3中制备的柔性锌离子电容器经过1000次循环后的扫描电子显微镜图,观察不到锌枝晶的生成。
实施例4
一种用于抑制锌离子电容器中锌枝晶生长的方法,包括如下步骤:
1)以碳纤维布为工作电极,锌片用作对电极和参比电极,配置2.5mol/L的硫酸锌和0.2mol/L柠檬酸钠的混合溶液作为电沉积液,先在-1.8V的电压下沉积150s,使导电柔性基底表面沉积一层锌晶种,随后在-0.8V的电压下沉积750s,得到柔性的锌阳极;
2)以10mL 2.5mol/L的硫酸锌和0.2mol/L柠檬酸钠的混合溶液与0.1g/mL聚乙烯醇均匀混合并在80℃下搅拌至凝胶呈无色透明状,得到固态凝胶电解质。
3)将锌阳极、活性炭和凝胶电解质组装成无枝晶生长的柔性锌离子电容器。
图6为本发明实施例4中制备的柔性锌离子电容器循环前和经过1000次循环后的X射线衍射谱图,反应前后锌阳极的X射线衍射谱图几乎相同,观察不到副产物生成。
本发明说明书中未作详细描述的内容属于本领域专业技术人员公知的现有技术。尽管上面对本发明说明性的具体实施方式进行了描述,以便于本技术领的技术人员理解本发明,但应该清楚,本发明不限于具体实施方式的范围,对本技术领域的普通技术人员来讲,只要各种变化在所附的权利要求限定和确定的本发明的精神和范围内,这些变化是显而易见的,一切利用本发明构思的发明创造均在保护之列。
Claims (8)
1.一种用于抑制锌离子电池/电容器中锌枝晶生长的方法,其特征在于:包括以下步骤:
步骤1,以导电柔性基底为工作电极,锌片用作对电极和参比电极,配置硫酸锌和柠檬酸钠的混合溶液作为电沉积液,在-1.8 V的电压下沉积锌晶种,使导电柔性基底表面沉积一层锌晶种,随后在-0.8 V的电压下继续沉积,得到柔性的锌阳极;
步骤2,以硫酸锌和柠檬酸钠的混合溶液与聚乙烯醇混匀并搅拌至凝胶呈无色透明状,得到固态凝胶电解质;
步骤3,将锌阳极、阴极材料和固态凝胶电解质组装成无枝晶生长的柔性锌离子电池/电容器;
所述步骤1)中在-1.8 V的电压下沉积锌晶种的时间为20-200 s;
所述步骤1)中硫酸锌的浓度为1-3 mol/L,柠檬酸钠的浓度为0.05-0.2 mol/L;
在沉积液中加入柠檬酸钠促进锌阳极形成由颗粒状组成的岩石状结构。
2.根据权利要求1所述的一种用于抑制锌离子电池/电容器中锌枝晶生长的方法,其特征在于:所述步骤1中导电柔性基底为碳纤维、碳布、钢丝中的任意一种。
3.根据权利要求2所述的一种用于抑制锌离子电池/电容器中锌枝晶生长的方法,其特征在于:所述步骤1)中在-0.8V的电压下沉积金属锌的时间为100 s-1800 s。
4.根据权利要求3所述的一种用于抑制锌离子电池/电容器中锌枝晶生长的方法,其特征在于:所述步骤2)中硫酸锌的浓度为1-3 mol/L,柠檬酸钠的浓度为0.05-0.2 mol/L。
5.根据权利要求4所述的一种用于抑制锌离子电池/电容器中锌枝晶生长的方法,其特征在于:所述步骤2)中搅拌温度为80℃。
6.根据权利要求5所述的一种用于抑制锌离子电池/电容器中锌枝晶生长的方法,其特征在于:所述硫酸锌和柠檬酸钠的混合溶液与聚乙烯醇的用量比为10 mL : 1 g。
7.根据权利要求6所述的一种用于抑制锌离子电池/电容器中锌枝晶生长的方法,其特征在于:所述步骤3)中阴极材料为用作锌离子电池/电容器的阴极材料。
8.根据权利要求7所述的一种用于抑制锌离子电池/电容器中锌枝晶生长的方法,其特征在于:所述步骤3)中阴极材料为聚吡咯、聚苯胺、石墨烯、活性炭中的任意一种。
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