CN113929146A - 一种核壳结构MnO/Mn3O4电极材料的制备及应用 - Google Patents
一种核壳结构MnO/Mn3O4电极材料的制备及应用 Download PDFInfo
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Abstract
一种核壳结构MnO/Mn3O4电极材料的制备及应用，属于材料制备领域。MnO为核，Mn3O4为壳，包括以下合成步骤：在室温下，将Mn(NO3)2溶解于蒸馏水中形成溶液，配制过氧化氢水溶液和四甲基氢氧化铵溶液，搅拌均匀，将过氧化氢溶液和四甲基氢氧化铵溶液倒入硝酸锰溶液中，搅拌过夜，过滤，得到锰氧化物前驱体；置于管式炉中煅烧，获得核壳结构MnO/Mn3O4。本发明通过异质结的作用，从而提高了锰氧化物电极材料的电化学性能和稳定性，该方法制备安全，简单，易于操作。
Description
技术领域
本发明属于电极材料制备领域，主要涉及超级电容器电极材料的制备方法。
背景技术
随着工业的迅猛发展，传统的不可再生能源如煤炭、石油等化石燃料日益枯竭，全球将面临能源危机。同时，使用化石燃料会排放大量的有害气体，导致出现全球变暖等一系列环境问题。因此，实现能源的安全和可持续发展是人类面临的严峻挑战。目前各国都在积极研究和开发绿色可再生的新能源，如太阳能、风能以及热能等。但是直接使用这些能源会受到一些制约，需要储能系统先将能量储存起来，从而实现能量的稳定供给。当今三大主要的储能系统包括电容器、电池和超级电容器。超级电容器的性能介于电池和传统电容器之间，具有高于电池的功率密度和传统电容器的能量密度，综合了电池和传统电容器的优点。因此，近年来超级电容器引起了人们极大的研究兴趣。目前，在油电混合车和电动汽车以及一些便携式电子设备领域中，超级电容器都发挥着不可或缺的作用。
在目前常见的电极材料中，过渡金属氧化物由于其低成本和高理论电容而受到广泛关注。四氧化三锰、二氧化锰是常见的作为电极材料的过渡金属氧化物。不过近几年来人们发现Mn3O4是制备锂离子电池正极材料锂锰氧的优质原料，其效果优于MnO2。而Mn3O4用于超级电容器的报道较少，其中，林等人通过溶胶凝胶法制备了Mn2O3和Mn3O4纳米复合膜，该锰的氧化物膜的比电容最高可达230.5F·g-1。陈等人研究了Mn3O4和碳纳米管复合电极的超级电容器。显然纯Mn3O4电极的比电容值还比较低，可以通过改进Mn3O4的制备方法，如制备Mn3O4的纳米材料，增大其比表面积来提高比电容。Mn3O4的制备方法很多，如高价锰氧化物以甲烷为还原气体在250～500℃温度下还原生成Mn3O4，另外水热法，溶剂热法，微波辐射法等都可以制备Mn3O4材料。然而，低电导率、大体积变化和在反应过程中易团聚限制了其实际应用。
我们提出了一种异质结策略，可以促进电荷转移，提高电极材料的电导率和氧化还原活性。通过简单的化学沉淀法和煅烧处理，成功合成了核壳结构MnO/Mn3O4。得到核壳结构MnO/Mn3O4具有离域电子构型，显著加速了电子转移。界面处的电场可以有效地降低离子扩散能垒，促进Na+输运动力学。结果表明，在1A g-1条件下，Ov-Mn3O4的Na+存储容量为331.2F g-1，在20A g-1条件下，其Na+存储容量为192F g-1。基于Ov-Mn3O4阴极的非对称超级电容器(ASC)在功率密度为1000W kg-1时，能提供40.56Wh kg-1的能量密度。
发明内容
本发明的首要目的是制备一种核壳结构MnO/Mn3O4电极材料，提高锰氧化物的稳定性和电化学性能。
为实现上述技术目的，本发明采用的技术方案如下：
本发明所述的核壳结构MnO/Mn3O4电极材料的制备方法，其中MnO为核，Mn3O4为壳，包括以下合成步骤：
步骤1：在室温下，将Mn(NO3)2溶解于蒸馏水中形成溶液，配制过氧化氢水溶液和四甲基氢氧化铵溶液，搅拌均匀，将过氧化氢溶液和四甲基氢氧化铵溶液倒入硝酸锰溶液中，搅拌过夜，过滤，得到锰氧化物前驱体；
优选每0.811gMn(NO3)2对应过氧化氢0.009mmol-0.027mmol、四甲基氢氧化铵0.022mmol-0.088mmol。
步骤2：将步骤1的固体粉末置于管式炉中煅烧，获得核壳结构MnO/Mn3O4。
其中步骤2的煅烧为氩气氛围下450℃-650℃/1-3h，管式炉的升温速率为3℃/min。
本发明所得材料用于超级电容器。
采用本发明的方法制备的电极材料，具有较大的电容和较小的电阻。在MnO和Mn3O4之间形成异质的结界面，两种不同带隙的纳米晶体偶极子可以激发纳米晶体内嵌的电场效应，从而实现快速的电荷传输和令人满意的反应动力学，提高了电化学性能。
附图说明
图1为得到核壳结构MnO/Mn3O4材料和Mn3O4材料的SEM对比
图2为得到核壳结构MnO/Mn3O4材料和Mn3O4材料的TEM和HRTEM对比
图3核壳结构MnO/Mn3O4材料和Mn3O4材料的XRD对比。
图4核壳结构MnO/Mn3O4材料和Mn3O4材料XPS的Mn 3s对比。
图5核壳结构MnO/Mn3O4材料和Mn3O4材料循环伏安测试结果(扫描速率为5mV s-1)和恒电流充放电测试结果(电流密度为1A g–1)。
具体实施方式
下面结合实施例对本发明做进一步说明，但本发明并不限于以下实施例。
实施例1
在室温下，将0.811gMn(NO3)2溶解于蒸馏水中形成10ml溶液，配制过氧化氢水溶液(浓度为30％的过氧化氢水0.625mL溶于7ml去离子水)和四甲基氢氧化铵溶液(浓度为25％的TMA·OH水4.3ml溶于7ml水中)，搅拌均匀，将过氧化氢溶液和四甲基氢氧化铵溶液倒入硝酸锰溶液中，搅拌过夜，过滤，得到锰氧化物前驱体。将得到的固体粉末置于管式炉氩气氛围中煅烧(500℃，2h)，获得核壳结构MnO/Mn3O4。
实施例2(对比例)
在室温下，将0.811gMn(NO3)2溶解于蒸馏水中形成10ml溶液，配制过氧化氢水溶液(0.625mL溶于7mL去离子水)和四甲基氢氧化铵溶液(4.3mL TMA·OH溶于7mL水中)，搅拌均匀，将过氧化氢溶液和四甲基氢氧化铵溶液倒入硝酸锰溶液中，搅拌过夜，过滤。将得到的固体粉末置于管式炉氩气氛围中煅烧(280℃，2h)，获得Mn3O4。
图1为得到核壳结构MnO/Mn3O4材料(a)和Mn3O4材料(b)的SEM图；
图2为得到核壳结构MnO/Mn3O4材料和Mn3O4材料的TEM图和HRTEM图。
其中(a)为MnO/Mn3O4的TEM图，(b)为Mn3O4的TEM图。(c)为MnO/Mn3O4的HRTEM图，(d)为Mn3O4的HRTEM图。晶格间距被归属于氧化锰的距离为
对应于其(200)晶面，晶格间距被归属于四氧化三锰的距离为
对应于(112)晶面；晶格间距被归属于四氧化三锰的距离
分别对应于(101)、(112)晶面。
图3为得到核壳结构MnO/Mn3O4材料和Mn3O4材料的XRD对比图。从图3可以看出MnO/Mn3O4与Mn3O4材料的晶型都与标准卡片对应，证明材料的合成成功。
图4核壳结构MnO/Mn3O4材料和Mn3O4材料XPS的Mn 3s对比。从Mn 3s图可知，MnO/Mn3O4的两峰间距相较于MnO2更宽，表明Mn的价态变低了，证明材料的合成成功。
图5为核壳结构MnO/Mn3O4材料和Mn3O4材料循环伏安测试结果和恒电流充放电测试结果。电化学测量是在1M Na2SO4水溶液中，以Ag/AgCl和铂箔分别作为参比电极和对电极的三电极配置进行的。循环伏安法(CV)和恒电流充放电(GCD)测试在0到1V的电位窗口内进行。图5(a)(b)为在5mV/s扫描速率下核壳结构MnO/Mn3O4和Mn3O4电极相对于Hg/HgO参考电极的典型CV曲线和在1A·g-1电流密度下的GCD曲线。结果显示Mn3O4具有比较差的电化学性能，其比电容为191F·g-1在1A·g-1电流密度下，而MnO/Mn3O4的比电容高达331.2F·g-1。对实施例1与实施例2所得到的电极材料进行电化学性能的对比，说明了异质结对锰氧化物的性能起到了促进作用，核壳结构MnO/Mn3O4具备更优异的电化学性能。
Claims (5)
1.一种核壳结构MnO/Mn3O4电极材料的制备方法，其特征在于，其中MnO为核，Mn3O4为壳，包括以下合成步骤：
步骤1：在室温下，将Mn(NO3)2溶解于蒸馏水中形成溶液，配制过氧化氢水溶液和四甲基氢氧化铵溶液，搅拌均匀，将过氧化氢溶液和四甲基氢氧化铵溶液倒入硝酸锰溶液中，搅拌过夜，过滤，得到锰氧化物前驱体；
步骤2：将步骤1的固体粉末置于管式炉中煅烧，获得核壳结构MnO/Mn3O4。
2.按照权利要求1所述的一种核壳结构MnO/Mn3O4电极材料的制备方法，其特征在于，每0.811gMn(NO3)2对应过氧化氢0.009mmol-0.027mmol、四甲基氢氧化铵0.022mmol-0.088mmol。
3.按照权利要求1所述的一种核壳结构MnO/Mn3O4电极材料的制备方法，其特征在于，步骤2的煅烧为氩气氛围下450℃-650℃煅烧1-3h，管式炉的升温速率为3℃/min。
4.按照权利要求1-3任一项所述的方法制备得到的核壳结构MnO/Mn3O4电极材料。
5.按照权利要求1-3任一项所述的方法制备得到的核壳结构MnO/Mn3O4电极材料的应用，用于超级电容器。
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