CN112624103B - 一种基于壳聚糖的碳电极材料的制备方法 - Google Patents
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Abstract
本发明提供了一种基于壳聚糖的碳电极材料的制备方法,是将壳聚糖,抗坏血酸,FeCl3加入二次水中,在80~90℃下搅拌直至形成均匀的低粘性红棕色溶胶,干燥,即得到碳前驱体材料;将前驱体材料在氮气气氛中进行两步退火处理,即可得到碳电极材料。本发明以壳聚糖作为碳源,FeCl3作为制孔剂,抗坏血酸作为还原剂,Fe3+与壳聚糖和抗坏血酸之间能够形成稳定的化学键,有利于形成丰富的孔结构,从而有利于高比电容的形成。本发明制备方法简单,易于操作,原料来源广泛、价格低廉、绿色环保且利用率高,制备的碳电极材料石墨化程度高,且显示出较高的比电容和良好的倍率性能,可应用于超级电容器、电池等柔性能量转化和存储器件。
Description
技术领域
本发明涉及一种碳电极材料的制备方法,尤其涉及一种基于壳聚糖的碳电极材料的制备方法,属于生物质材料和电化学材料制备领域。
背景技术
随着全球经济和人口激增等问题的出现,能源短缺和环境污染问题一直是人类面临的挑。这些问题的加剧使得电能代替石油是一种必然的趋势。近年来,超级电容器(SCs)作为一种很有前景的储能设备受到了人们的关注,与锂离子电池相比,它具有更快的充放电周期、更高的功率密度,既具备传统电池的高储能能力又有传统电容器的高供电能力,弥补了传统电容器与电池之间的差距,被视为理想的电化学储能设备。
对于SCs而言,电极材料对其性能起着关键性的作用。根据不同的储能机理可将超级电容器的电极材料分为两类:(1)以碳材料为主的双电层电极材料(2)以过渡金属(氢)氧化物和导电聚合物为主的赝电容电极材料。常见的碳基电极材料主要有:活性炭、碳纳米管、石墨烯、碳纤维、模板碳、多孔碳等。其中多孔碳材料以孔隙结构丰富、比表面积大、稳定性好、原料来源广泛、价格低廉、制备工艺简单且绿色环保等优点,受到研究者的广泛关注。然而,多孔碳材料属于双电层储能机理,大多数使用生物质衍生碳材料的研究具有低的比电容或较差的倍率性能,同时得到的电极材料石墨化程度低。
发明内容
针对上述技术问题,本发明的目的是提供一种具有高比电容、良好倍率性能和较高石墨化程度的基于壳聚糖的碳电极材料的制备方法。
一、碳电极材料的制备
(1)将壳聚糖、抗坏血酸、FeCl3加入二次水中,在80~90℃下搅拌直至形成均匀的低粘性红棕色溶胶,在50~70℃下干燥10~12h,即得到碳前驱体材料。其中,所述抗坏血酸、壳聚糖、FeCl3的质量比为1:1:1~1:2:4;所述壳聚糖、抗坏血酸、FeCl3在二次水中的浓度为0.02~0.12g/mL。
(2)将前驱体材料在氮气气氛中进行两步退火处理,首先以3~5℃/min的速率升温至300~500℃,保持30~100min,然后再升温至700~900℃,保持100~180min,用HCl和二次水洗涤,50~70℃下干燥,即可得到碳电极材料。
二、碳电极材料的结构表征
1、场发射扫描电镜(FE-SEM)分析
图1a,b为本发明制备的碳电极材料在不同放大倍数下的场发射扫描电镜(FE-SEM)图片。从图中可以观察到碳电极材料是相互交联的类石墨烯纳米片层结构,且具有开放的孔道结构。
2、X衍射谱图(XRD)分析
图2为本发明制备的碳电极材料的X衍射(XRD)谱图。从图谱中可以看到,该材料在24.1°和43.3°处有两个衍射峰,分别对应于无序微晶面(002)和石墨型碳(100)晶面,表明该材料以无定形结构的形式存在。
3、拉曼(Raman)分析
图3为本发明制备的碳电极材料的拉曼(Raman)谱图。从图谱中可以看到,该材料在1327cm-1(D带)和1598cm-1(G带)有两个尖峰,分别代表石墨化碳和石墨层的缺陷和紊乱程度。D峰和G峰的强度比为0.95,表明虽然该材料具有较高的石墨化程度,但仍然以无定形结构的形式存在。
三、电化学性能测试
电化学性能测试是在室温下利用电化学工作站CHI660E(辰华,上海,中国)在三电极体系中完成的。下面通过电化学工作站CHI660E对本发明制备的碳电极材料的电化学性能进行详细说明。
1、工作电极的制备
在三电极体系下,使用玻碳电极(直径5mm)作为集流体。将4mg碳电极材料和0.7mg乙炔黑的混合固体粉充分研磨,加入到0.4mL质量分数为0.25wt%的Nafion溶液中超声分散形成悬浮液,然后用移液枪量取6μL上述悬浮液滴于玻碳电极表面,室温下干燥。
2、电化学性能测试
以上述制备的电极作为工作电极,饱和甘汞和碳棒分别作为参比电极和对电极组成三电极体系,1mol/LNaSO4溶液作为电解质溶液进行电化学性能测试。如图4所示为本发明制备的碳电极材料在不同扫速下的循环伏安(CV)曲线。从图中的可以看出:当扫速从5mV/s增加到50mV/s时,可观察到曲线呈矩形形状基本保持不变,这是由于碳电极材料典型的双电层储能机理。
图5为本发明制备的碳电极材料在不同电流密度下的恒电流充放电(GCD)曲线。从图中的可以看出:随着电流密度由1A/g增大到10A/g时,比电容分别为262,244,240,230,226,222F/g且所有曲线仍保持对称的等腰三角形形状,表明该电极材料具有良好的电化学可逆性,同时从数据中也可看出该碳电极材料具有较高的比电容和良好的倍率性能。
图6为本发明制备的碳电极材料在频率范围为0.1Hz~100kHz,偏置电压为0.9V下测得的交流阻抗图。曲线由两部分组成包括高频区的半圆和低频区的直线,半圆与实部的第一个交点表示等效串联电阻(Rs),它代表电解液中的离子电阻,电解液与电极材料之间的界面电阻,电极材料自身的电阻以及电极材料与导电集流体之间接触电阻的总和,高频区半圆的直径表示电荷转移电阻(Rct),低频区直线的斜率表示电解液的扩散电阻。从图中可看出:本发明制备的碳电极材料具有较低的等效串联电阻和电荷转移电阻,电解液的扩散阻力较低,离子传输速度较快;低频区的直线与虚轴接近平行也表明该电极材料具有良好的电容性质。
综上所述,本发明和现有技术相比具有以下优点:
1、本发明以富含多氨基和多羟基的生物质材料壳聚糖天然高分子作为碳源,FeCl3作为制孔剂,抗坏血酸作为还原剂制备碳电极材料,Fe3+与壳聚糖和抗坏血酸之间能够形成稳定的化学键,有利于形成丰富的孔结构,从而有利于高比电容的形成。
2、本发明解决了使用生物质衍生碳材料制备碳电极材料石墨化程度低,以及具有低比电容或低倍率性能的问题,制备的碳电极材料石墨化程度高,并显示出较高的比电容和良好的倍率性能,可应用于超级电容器、电池等柔性能量转化和存储器件。
3、本发明制备方法简单,易于操作,原料来源广泛、价格低廉、绿色环保且利用率高。
附图说明
图1为为本发明制备的碳电极材料在不同放大倍数下的场发射扫描电镜(FE-SEM)图片。
图2为本发明制备的碳电极材料的X衍射(XRD)谱图。
图3为本发明制备的碳电极材料的拉曼(Raman)谱图。
图4为本发明制备的碳电极材料在不同扫速下的循环伏安(CV)曲线。
图5为本发明制备的碳电极材料在不同电流密度下的恒电流充放电(GCD)曲线。
图6为本发明制备的碳电极材料在频率范围为0.1Hz~100kHz,偏置电压为0.9V下测得的交流阻抗图。
具体实施方式
下面通过具体实施例对本发明碳电极材料的制备及电化学性能作进一步详细的说明。
使用的仪器和试剂:电子天平(北京赛多利斯仪器有限公司)用于称量药品;恒温磁力搅拌器(90-1上海沪西分析仪器厂);CHI660E电化学工作站(上海辰华仪器公司)用于电化学性能测试;FE-SEM(Ultra Plus,CarlZeiss,Germany)场发射扫描电子显微镜用于材料的形貌表征;由粉末X-射线衍射仪(XRD;D/Max-2400,Cu靶:
λ=0.15418nm,扫描速率为5℃/min,管电压为40kV,管电流为60mA)对材料的晶体结构进行分析;拉曼光谱采用inVia拉曼光谱仪(Renishawλ=514nm)完成。壳聚糖(山东荣宜达纤维有限公司);抗坏血酸(上海中秦化学试剂有限公司);FeCl3(西陇化工股份有限公司)。实验过程中使用的水均为二次水,实验所用的试剂均为分析纯。
实施例1
(1)碳电极材料的制备:将2g壳聚糖,1g抗坏血酸和3gFeCl3加入35mL二次水中,在85℃下搅拌直至形成均匀的低粘性红棕色溶胶,在60℃下干燥10h,即可得碳前驱体材料;将前驱体材料在氮气气氛中进行两步退火处理,首先以3℃/min的速率升温至300℃,保持60min,然后再升温至800℃,保持120min,最后用1mol/L的HCl和二次水多次洗涤,最后在60℃下干燥,即可得碳电极材料。
(2)工作电极的制备:在三电极体系下,使用玻碳电极(直径5mm)作为集流体。将4mg碳电极材料和0.7mg乙炔黑的混合固体粉充分研磨,加入到0.4mL质量分数为0.25wt%的Nafion溶液中超声分散形成悬浮液,然后用移液枪量取6μL上述悬浮液滴于玻碳电极表面,室温下干燥。
(3)电化学性能测试:以上述制备的电极作为工作电极,饱和甘汞和碳棒分别作为参比电极和对电极组成三电极体系,1mol/LNaSO4溶液作为电解质溶液进行电化学性能测试。测试结果表明,当电流密度为1A/g时,碳电极材料的比电容可以达262F/g。
实施例2
(1)碳电极材料的制备:将2g壳聚糖,2g抗坏血酸和2gFeCl3加入35mL二次水中,在85℃下搅拌直至形成均匀的低粘性红棕色溶胶,在60℃下干燥10h,即可得碳前驱体材料;将前驱体材料在氮气气氛中进行两步退火处理,首先以3℃/min的速率升温至400℃,保持60min,然后再升温至800℃,保持120min,最后用1mol/L的HCl和二次水多次洗涤,最后在60℃下干燥,即可得碳电极材料。
(2)工作电极的制备及电化学性能测试过程同实施例1,当电流密度为1A/g时,碳电极材料的比电容为243F/g。
实施例3
(1)碳电极材料的制备:将2g壳聚糖,1g抗坏血酸和4gFeCl3加入35mL二次水中,在85℃下搅拌直至形成均匀的低粘性红棕色溶胶,在60℃下干燥10h,即可得碳前驱体材料;将前驱体材料在氮气气氛中进行两步退火处理,首先以3℃/min的速率升温至500℃,保持60min,然后再升温至700℃,保持120min,最后用1mol/L的HCl和二次水多次洗涤,最后在60℃下干燥,即可得碳电极材料。
(2)工作电极的制备及电化学性能测试过程同实施例1,当电流密度为1A/g时,碳电极材料的比电容为250F/g。
Claims (5)
1.一种基于壳聚糖的碳电极材料的制备方法,包括以下步骤:
(1)将壳聚糖、抗坏血酸、FeCl3加入二次水中,在80~90℃下搅拌直至形成均匀的低粘性红棕色溶胶,干燥,即得到碳前驱体材料;
(2)将前驱体材料在氮气气氛中进行两步退火处理,首先以3~5℃/min的速率升温至300~500℃,保持30~100min,然后再升温至700~900℃,保持100~180min,用HCl和二次水洗涤,干燥,即可得到碳电极材料。
2.如权利要求1所述一种基于壳聚糖的碳电极材料的制备方法,其特征在于:步骤(1)中,所述抗坏血酸、壳聚糖、FeCl3的质量比为1:1:1~1:2:4。
3.如权利要求1所述一种基于壳聚糖的碳电极材料的制备方法,其特征在于:步骤(1)中,所述壳聚糖、抗坏血酸、FeCl3在二次水中的浓度为0.02~0.12g/mL。
4.如权利要求1所述一种基于壳聚糖的碳电极材料的制备方法,其特征在于:步骤(1)中,所述干燥是在50~70℃下干燥10~12h。
5.如权利要求1所述一种基于壳聚糖的碳电极材料的制备方法,其特征在于:步骤(2)中,干燥温度为50~70℃。
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