CN113690064B - 一种具有可调n-tm-c异质结界面的超级电容器电极材料及其制备方法 - Google Patents
一种具有可调n-tm-c异质结界面的超级电容器电极材料及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种具有可调N‑TM‑C异质结界面的超级电容器电极材料及其制备方法，属于超级电容器电极材料领域。本发明的电极材料包含一种过渡金属的碳化物和氮化物，构成N‑TM‑C异质结界面，过渡金属碳化物的质量含量为1‑99％，所述过渡金属氮化物的质量含量为1‑99％。所述的制备方法包括的原材料有：提供过渡金属源材料、碳源、氮源、调节异质结界面比例的材料和形成二维带孔片层结构的材料。且通过调控调节异质结界面比例而不改变材料形貌的材料的添加量，实现对二维非层状形貌的调控。本发明通过调节N‑TM‑C异质界面，调节异质结面内在电场，从而改善电解液离子扩散和吸附行为，提高超级电容器性能。
Description
技术领域
本发明涉及一种具有可调N-TM-C异质结界面的超级电容器电极材料的制备方法，属于超级电容器电极材料领域。
背景技术
近年来，随着能源危机和环境污染等问题的日益严重，开发利用新型储能设备势在必行。由于具有高的功率密度，快速充放电，以及循环寿命长等特性，超级电容器已成为混合动力汽车，便携式电子设备以及智能电网中最有前途的储能设备之一。然而，目前所报道的大多数超级电容器的较低能量密度仍未满足实际应用的需要。一般来说，由于离子储存主要发生在电极/电解质界面，电极材料作为超级电容器的核心部件，在决定其性能方面起着至关重要的作用。
在工业应用中，双电层电容器和赝电容器的电极材料仍分别是活性炭和金属氧化物。活性炭通常表现出不规则的形态、较差的石墨化框架和较宽的孔径分布。金属氧化物在赝电容器中的应用受到它们相对较低的电子电导率的严重阻碍，无法在更高速率的环境中跟上能量储存的需求。含过渡金属(Transition Metal，TM)碳/氮化物是近些年快速发展起来的一种类石墨烯二维材料，具有金属级导电性、良好的亲水性及丰富的表面化学，与目前广泛研究的碳基电极材料相比，堆积密度高且具有赝电容特征，有望降低器件体积，被认为在储能电极材料中有巨大的应用潜力。与传统三维多孔材料相比，二维(2D)多孔材料可以暴露出更多的活性位点和更短的离子传输路径，缩小尺度后的量子特性也广受研究者青睐。但二维材料由于维度上的限制，其合成一直是研究难点。而在二维异质结材料中，N-TM-C异质结界面由于存在更多的活性位点，可以促进电子转移，费米能级的差距能够重新分配电子，优化电子结构从而促进材料内在电场的构建。在超级电容器电极中，这样的性质有助于电解液离子的扩散行为，有望作为高性能超级电容器材料。异质界面的调整可以调控材料异质结面的内在电场，从而调控电解液离子的扩散行为，改善电极材料的电化学性能。因此，开发出方便的可调节N-TM-C异质结界面，且具有二维片层结构的异质结材料的制备方法非常有意义。
发明内容
本发明的目的在于提供一种具有可调N-TM-C异质结界面的超级电容器电极材料的制备方法。本发明的电极材料包含一种过渡金属的碳化物和氮化物，构成N-TM-C异质结界面，过渡金属碳化物的质量含量为1-99％，所述过渡金属氮化物的质量含量为1-99％。所述的制备方法包括的原材料有：提供过渡金属源材料、碳源、氮源、调节异质结界面比例的材料和形成二维带孔片层结构的材料。
一种具有可调N-TM-C异质结界面的超级电容器电极材料的制备方法，包括如下步骤：
步骤一、将含过渡金属源材料溶于去离子水中，超声分散后，加入碳源，常温搅拌；
步骤二、持续搅拌，加入造孔材料和调节异质结界面比例而不改变材料形貌的材料；
步骤三、加入一定量形成二维片层结构的材料，干燥后在一定温度下煅烧；待冷却后酸洗、离心分离和干燥，得到电极材料。
步骤一所述含过渡金属源材料为：四水合钼酸铵((NH4)6Mo7O24·4H2O)
步骤一所述碳源为：二-甲基咪唑(2-mlm)
步骤二所述造孔材料为：六水合硝酸锌(Zn(NO3)2·6(H2O))
步骤二所述调节异质结界面比例而不改变材料形貌的材料为：NH4Cl、(NH4)2CO3、(NH4)2SO4
步骤三所述形成二维片层结构的材料为：NaCl、KCl
步骤三所述煅烧温度为：600℃-900℃
物质添加量：1-5g四水合钼酸铵，1-3g 2-mlm，10-50g NaCl，0.5-3g Zn(NO3)2·6H2O和0.5-3g NH4Cl。
制备异质结材料时，原材料中加入AHM(四水合钼酸铵)和(2-甲基咪唑)，钼酸铵作用是提供钼源和N源，2-甲基咪唑提供碳源。在反应过程中，首先钼酸铵加热后生成NH3与Mo生成Mo2N，然后2-甲基咪唑提供碳源生成Mo2C，在不改变Mo含量的情况下，加入NH4Cl可以调节Mo2N的生成量，由此调整异质结界面。如果只是改变钼酸铵的比例，可导致Mo含量也同时增多；如果不改变钼酸铵的量，只改变2-甲基咪唑的加入量，由于先生成Mo2N，所以改变2-甲基咪唑的加入量对异质结界面比例的改变影响不大。
本发明还提供一种按照如上所述方法制备得到的异质结电极材料。
通过调控调节异质结界面比例而不改变材料形貌的材料的添加量，实现对二维非层状形貌的调控，具体方法为：高温渗碳/氮，共生成碳化物/氮化物异质结颗粒，沿着NaCl盐模板组装成2D层状结构。
有益效果
1、本发明的一种具有可调N-TM-C异质结界面的超级电容器电极材料的制备方法，具有可调N-TM-C异质界面的电极材料制备方法，以及利用相应制备方法所制备的电极材料。这种材料通过调节N-TM-C异质界面，调节异质结面内在电场，从而改善电解液离子扩散和吸附行为，提高超级电容器性能。
2、本发明通过加入NH4Cl，方便和有效的实现异质结界面的调整。
附图说明
图1为所制备材料β-Mo2C/γ-Mo2N异质结的选区电子衍射(SAED)图片，证明具有N-Mo-C界面；
图2为所制备材料β-Mo2C/γ-Mo2N异质结的2D非层状结构示意图；
图3为所制备材料β-Mo2C/γ-Mo2N异质结在不同电流密度下的比电容图；
图4为所制备β-Mo2C/γ-Mo2N异质结材料的电化学阻抗图(EIS)；
图5为不同NH4Cl用量下样品的SEM图；
图6为不同Zn(NO3)2用量下样品的SEM图。
具体实施方式
下面结合实施例与附图对本发明做进一说明。
实施例1：
一种具有可调N-TM-C异质结界面的超级电容器电极材料的制备方法，包括如步骤：
第一步：1-5g AHM(四水合钼酸铵)溶于50ml去离子水中，超声分散10min，加入1-3g 2-mlm(2-甲基咪唑)，常温搅拌2h；
第二步：0.5-3g Zn(NO3)2 6H2O(六水合硝酸锌)和0.5-3g NH4Cl溶于50ml去离子水中，完全溶解后倒入上述溶液，继续常温搅拌2h；
第三步：加入10-50g NaCl，搅拌蒸发，待完全干燥后在Ar(氩气)气氛下600-900℃煅烧2h；
第四步：煅烧后的样品，待完全冷却后用HCl酸洗，搅拌2h后离心分离，洗至中性，50℃真空干燥，得到含有N-Mo-C界面(如图1所示)，且具有带孔片层的电极材料，其片层结构的电镜照片如图2所示；电流密度为1A/g时，比电容为2050F/g，10A/g时电容保持率为85.6％，如图3所示；EIS图中阻抗弧不存在，Rs值为0.6Ω，如图4所示。
实施例2：
本实施例和实施例1基本相同，所不同的是NH4Cl的用量，样品其他比例相同，其结构的电镜照片如图5所示，10A/g时电容保持率为73.5％；EIS图中Rs值为1.4Ω。不同NH4Cl比例对应材料的形貌如图2和图5所示，片层形貌以及片层上孔的大小和数量可以通过NH4Cl进行调控：随着NH4Cl的增加，片层逐渐变薄，且孔隙更加丰富，孔隙尺寸更大，这是造孔剂Zn(NO3)2·6H2O和NH4Cl共同作用的结果；在一定用量范围内能够保持片层的完整性。据分析，NH4Cl的作用相当于气源，加入的NH4Cl越多，煅烧过程中产生的NH3越多，气体的存在克服了层间的作用力，将片层分离，同时气体在层间穿梭，扩大原有孔隙的尺寸。
实施例3：
本实施例和实施例1基本相同，所不同的是Zn(NO3)2的用量，样品其他比例相同，其结构的电镜照片如图6所示，10A/g时电容保持率为81.2％；EIS图中Rs值为0.8Ω。
以上所述的具体描述，对发明的目的、技术方案和有益效果进行了进一步详细说明，所应理解的是，以上所述仅为本发明的具体实施例而已，并不用于限定本发明的保护范围，凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (1)
1.一种具有可调N-TM-C异质结界面的超级电容器电极材料，其特征在于：材料是一种包含过渡金属的碳化物和氮化物，构成N-TM-C异质结界面，过渡金属碳化物的质量含量为1-99％，所述过渡金属氮化物的质量含量为1-99％；通过调节N-TM-C异质界面，调节异质结面内建电场，从而改善电解液离子扩散和吸附行为，提高超级电容器性能；
所述具有可调N-TM-C异质结界面的超级电容器电极材料的制备方法为：通过调控调节异质结界面比例而不改变材料形貌的材料的添加量，实现对二维非层状形貌的调控，具体方法为：高温渗碳/氮，共生成碳化物/氮化物异质结颗粒，沿着NaCl盐模板组装成2D层状结构；
所述方法包括如下步骤：
步骤一、将含过渡金属源材料溶于去离子水中，超声分散后，加入碳源，常温搅拌；
步骤二、持续搅拌，加入造孔材料和调节异质结界面比例而不改变材料形貌的材料；
步骤三、加入一定量模板形成二维片层结构的材料，干燥后在一定温度下煅烧；待冷却后酸洗、离心分离和干燥，得到电极材料；
步骤一所述含过渡金属源材料为：四水合钼酸铵(NH4)6Mo7O24·4H2O；
步骤一所述碳源为：二-甲基咪唑2-mlm；
步骤二所述造孔材料为：六水合硝酸锌Zn(NO3)2·6(H2O)；
步骤二所述调节异质结界面比例而不改变材料形貌的材料为：NH4Cl、(NH4)2CO3、(NH4)2SO4；
步骤三所述形成二维片层结构的材料为：NaCl、KCl；
步骤三所述煅烧温度为：600℃-900℃；
物质添加量：1-5 g四水合钼酸铵，1-3 g 2-mlm，10-50 g NaCl，0.5-3 g Zn(NO3)2·6H2O和0.5-3 g NH4Cl。
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