CN111009422A - 一种镍基核壳结构NiCo2O4/聚苯胺纳米材料的制备方法 - Google Patents
一种镍基核壳结构NiCo2O4/聚苯胺纳米材料的制备方法 Download PDFInfo
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- 229910005949 NiCo2O4 Inorganic materials 0.000 claims abstract description 21
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Abstract
本发明公开了一种镍基核壳结构NiCo2O4/聚苯胺纳米材料的制备方法，进一步提高NiCo2O4/聚苯胺复合材料在超级电容器电极材料领域的比电容值。本发明方法采用泡沫镍为基底，通过水热法在基底上制备NiCo2O4纳米材料，接着通过原位聚合法，低温下在该材料表面直接聚合苯胺，然后取出材料，洗涤并干燥即得到了本发明所述的镍基核壳结构NiCo2O4/聚苯胺纳米材料。该复合纳米材料制备简单、成本低廉，在超级电容器电极材料应用中性能优异，比电容值在扫描速率为5mA/cm2时，可达14F/cm2。
Description
技术领域
本发明涉及电极材料制备技术领域，具体是一种镍基核壳结构NiCo2O4/聚苯胺纳米材料的制备方法，进一步提高NiCo2O4/聚苯胺复合材料在超级电容器电极材料领域的比电容值。
背景技术
超级电容器具有比能高、循环能力强、充放电速率快等优点，作为一种极具发展前景的储能元件引起了广泛的关注。电极材料是提高超级电容器性能的关键因素。NiCo2O4得益于其独特的双离子结构，具有更高的导电性和电化学活性，在过渡金属氧化物中表现出较好的性能。同时，聚苯胺因其独特的质子化机理、固有电导率和易于合成的优点，在现有的导电聚合物中脱颖而出。然而聚苯胺的机械稳定性和循环稳定性较差，再去掺杂态时电导率较低。
基于二者协同效应，NiCo2O4与聚苯胺复合之后，一方面NiCo2O4提供快速的离子传输路径，可以减弱PANI的极化，另一方面，聚苯胺聚合过程中掺杂了Ni2+/Ni3+，Co2+/Co3+金属离子，可以促进电荷沿聚合物链的局部转移，进一步提升材料的电容性能。但基于这两种材料在超级电容器电极的研究还很少，且比电容值还有很大提升空间。
发明内容
本发明目的是为了进一步提高NiCo2O4/聚苯胺电极材料的比电容，提供一种镍基核壳结构NiCo2O4/聚苯胺纳米材料的制备方法。在该制备方法中，NiCo2O4/聚苯胺纳米材料是直接生长在泡沫镍基底上的，同时也解决了活性材料在电极组装过程中的性能弱化的问题。
本发明是采用如下技术方案实现的：
一种镍基核壳结构NiCo2O4/聚苯胺纳米材料的制备方法，包括如下步骤：
1）、取CoCl2·6H2O，NiCl2·6H2O，CO(NH2)2，NH4F摩尔量比为2:1:3:3~9，并加去离子水搅拌溶解，之后将泡沫镍同上述溶液共同加入到聚四氟乙烯内衬的反应釜中，100℃~150℃水热6~10h，之后将泡沫镍取出冲洗并干燥，然后将泡沫镍在300℃~500℃退火2h，得到产物镍基NiCo2O4纳米材料；
2）、配置100ml HCl溶液，加入氧化剂(NH4)2S2O8，低温下磁力搅拌10~30min之后，取1ml苯胺逐滴加入上述溶液，并继续低温搅拌2h；HCl、(NH4)2S2O8和苯胺物质的量比为1~10:1:1；
3）、取步骤1）中产物镍基NiCo2O4纳米材料加入到步骤2）所得溶液中，在常温下反应4~8h；
4）、反应完毕后，将泡沫镍取出，用去离子水洗涤，然后在60℃真空干燥24h，即得到了镍基核壳结构NiCo2O4/聚苯胺纳米材料。
进一步优选的，步骤1）中，CoCl2·6H2O、NiCl2·6H2O、CO(NH2)2、NH4F摩尔量比为2:1:3:9，150℃水热6h，泡沫镍在400℃退火2h。
进一步优选的，步骤2）中，HCl、(NH4)2S2O8和苯胺物质的量比为10:1:1。
本发明方法采用泡沫镍为基底，通过水热法在基底上制备NiCo2O4纳米材料，接着通过原位聚合法，低温下在该材料表面直接聚合苯胺，然后取出材料，洗涤并干燥即得到了本发明所述的镍基核壳结构NiCo2O4/聚苯胺纳米材料。该复合纳米材料制备简单、成本低廉，在超级电容器电极材料应用中性能优异，比电容值在扫描速率为5mA/cm2时，可达14F/cm2。
附图说明
图1表示本发明方法实施例2制备过程中的NiCo2O4纳米材料的SEM图。
图2表示本发明方法实施例2制备过程中的NiCo2O4纳米材料的XRD图。
图3表示本发明方法实施例2制备过程中的NiCo2O4/聚苯胺纳米复合材料的SEM图。
图4表示本发明方法实施例2制备过程中的NiCo2O4/聚苯胺复合纳米材料的XPS测试图。
图5表示本发明方法实施例2制备过程中的NiCo2O4/聚苯胺复合纳米材料的充放电图。
图6表示不同实施示例在5mA/cm2电流密度下的充放电对比图。
具体实施方式
下面结合附图对本发明的具体实施例进行详细说明。
实施例1
一种镍基核壳结构NiCo2O4/聚苯胺纳米材料的制备方法，包括如下步骤：
1）、取CoCl2·6H2O，NiCl2·6H2O，CO(NH2)2，NH4F摩尔量比为2:1:3:3，并加去离子水搅拌溶解，之后将泡沫镍同上述溶液共同加入到聚四氟乙烯内衬的反应釜中，100℃水热10h，之后将泡沫镍取出冲洗并干燥，然后将泡沫镍在300℃退火2h，得到产物镍基NiCo2O4纳米材料；
2）、配置100ml HCl溶液，加入氧化剂(NH4)2S2O8，0℃下磁力搅拌10min之后，取1ml苯胺逐滴加入上述溶液，并继续于0℃下磁力搅拌2h；HCl、(NH4)2S2O8和苯胺物质的量比为1:1:1；
3）、取步骤1）中产物镍基NiCo2O4纳米材料加入到步骤2）所得溶液中，在常温下反应4h；
4）、反应完毕后，将泡沫镍取出，用去离子水洗涤，然后在60℃真空干燥24h，即得到了镍基核壳结构NiCo2O4/聚苯胺纳米材料。
实施例2
一种镍基核壳结构NiCo2O4/聚苯胺纳米材料的制备方法，包括如下步骤：
1）、取CoCl2·6H2O，NiCl2·6H2O，CO(NH2)2，NH4F摩尔量比为2:1:3:9，并加去离子水搅拌溶解，之后将泡沫镍同上述溶液共同加入到聚四氟乙烯内衬的反应釜中，150℃水热6h，之后将泡沫镍取出冲洗并干燥，然后将泡沫镍在400℃退火2h，得到产物镍基NiCo2O4纳米材料；
2）、配置100ml HCl溶液，加入氧化剂(NH4)2S2O8，0℃下磁力搅拌30min之后，取1ml苯胺逐滴加入上述溶液，并继续在0℃下磁力搅拌2h；HCl、(NH4)2S2O8和苯胺物质的量比为10:1:1；
3）、取步骤1）中产物镍基NiCo2O4纳米材料加入到步骤2）所得溶液中，在常温下反应6h；
4）、反应完毕后，将泡沫镍取出，用去离子水洗涤，然后在60℃真空干燥24h，即得到了镍基核壳结构NiCo2O4/聚苯胺纳米材料。
实施例3
一种镍基核壳结构NiCo2O4/聚苯胺纳米材料的制备方法，包括如下步骤：
1）、取CoCl2·6H2O，NiCl2·6H2O，CO(NH2)2，NH4F摩尔量比为2:1:3:6，并加去离子水搅拌溶解，之后将泡沫镍同上述溶液共同加入到聚四氟乙烯内衬的反应釜中，130℃水热8h，之后将泡沫镍取出冲洗并干燥，然后将泡沫镍在500℃退火2h，得到产物镍基NiCo2O4纳米材料；
2）、配置100ml HCl溶液，加入氧化剂(NH4)2S2O8，0℃下磁力搅拌30min之后，取1ml苯胺逐滴加入上述溶液，并继续0℃下磁力搅拌2h；HCl、(NH4)2S2O8和苯胺物质的量比为5:1:1；
3）、取步骤1）中产物镍基NiCo2O4纳米材料加入到步骤2）所得溶液中，在常温下反应8h；
4）反应完毕后，将泡沫镍取出，用去离子水洗涤，然后在60℃真空干燥24h，即得到了镍基核壳结构NiCo2O4/聚苯胺纳米材料。
本发明实施例2采用泡沫镍为基底，通过水热法在基底上制备NiCo2O4纳米材料，得到的NiCo2O4纳米材料以自生长的方式依附在泡沫镍基底上，其SEM图如图1所示，从图1可以看出，NiCo2O4纳米材料整体呈球状，纳米球表面呈鳞片状，可进一步扩大活性物质的比表面。为了表征NiCo2O4纳米材料的成分，NiCo2O4纳米材料的XRD图如图2，由图2可知，本发明实施例制备出成分单一，无杂质，稳定性高的NiCo2O4纳米材料。
本发明实施例2制备的镍基核壳结构NiCo2O4/聚苯胺纳米材料的SEM图如图3所示，与图1相比可以看出，NiCo2O4纳米材料表面包覆了一层致密的聚苯胺。本发明制得的NiCo2O4/聚苯胺复合纳米材料的XPS测试图谱如图4，从图4中可以看出，所制得的纳米材料无其他杂质。通过恒流充放电对材料的性能进行了测试，其充放电图谱如图5，通过公式（1）可得，材料的面积比电容在电流密度为5mA/cm2条件下可达14F/cm2，展现出良好的电容性能。
图6为三个实施例在电流密度为5mA/cm2条件下的充放电对比图，由图6可得，虽然实施例2的电压降相对较小，但是其比电容值（14F/cm2）要远远大于实施例1（1.7F/cm2）和实施例3（3F/cm2），展现出了最优异的电容性能，说明在本实验环境下，苯胺聚合过程中H+的掺杂浓度以及聚合时间对所制备电极性能有很大影响。
总之，本发明方法成本低廉，制备工艺简单，原料来源容易，且制得的材料比容量高，基底依附的自生长方式也规避了纳米材料电极组装过程中的活性降低等因素。
最后应说明的是，以上实施例仅用以说明本发明的技术方案而非限制，尽管参照本发明实施例进行了详细说明，本领域的普通技术人员应当理解，对本发明的技术方案进行修改或者等同替换，都不脱离本发明的技术方案的精神和范围，其均应涵盖本发明的权利要求保护范围中。
Claims (6)
1.一种镍基核壳结构NiCo2O4/聚苯胺纳米材料的制备方法，其特征在于：包括如下步骤：
（1）、取CoCl2·6H2O、NiCl2·6H2O、CO(NH2)2、NH4F，并加去离子水搅拌溶解，之后将泡沫镍同上述溶液共同加入到聚四氟乙烯内衬的反应釜中，100℃~150℃水热6~10h，之后将泡沫镍取出冲洗并干燥，然后将泡沫镍在300℃~500℃退火2h，得到产物镍基NiCo2O4纳米材料；
（2）、配置HCl溶液，加入氧化剂(NH4)2S2O8，低温下磁力搅拌， 10~30min之后，取苯胺加入上述溶液，并继续低温下搅拌2h；
（3）、取步骤（1）中产物镍基NiCo2O4纳米材料加入到步骤（2）所得溶液中，在常温下反应4~8h；
（4）、反应完毕后，将泡沫镍取出，用去离子水洗涤，然后在60℃真空干燥24h，即得到了镍基核壳结构NiCo2O4/聚苯胺纳米材料。
2.根据权利要求1所述的一种镍基核壳结构NiCo2O4/聚苯胺纳米材料的制备方法，其特征在于：步骤（1）中，CoCl2·6H2O、NiCl2·6H2O、CO(NH2)2、NH4F摩尔量比为2:1:3:3~9。
3.根据权利要求2所述的一种镍基核壳结构NiCo2O4/聚苯胺纳米材料的制备方法，其特征在于：步骤（1）中，CoCl2·6H2O、NiCl2·6H2O、CO(NH2)2、NH4F摩尔量比为2:1:3:9；150℃水热6h；泡沫镍在400℃退火2h。
4.根据权利要求1所述的一种镍基核壳结构NiCo2O4/聚苯胺纳米材料的制备方法，其特征在于：步骤（2）中，HCl、(NH4)2S2O8和苯胺物质的量比为1~10:1:1。
5.根据权利要求4所述的一种镍基核壳结构NiCo2O4/聚苯胺纳米材料的制备方法，其特征在于：步骤（2）中，HCl、(NH4)2S2O8和苯胺物质的量比为10:1:1；0℃下磁力搅拌。
6.根据权利要求1所述的一种镍基核壳结构NiCo2O4/聚苯胺纳米材料的制备方法，其特征在于：步骤（3）中，在常温下反应6h。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113782346A (zh) * | 2021-09-09 | 2021-12-10 | 福州大学 | 一种聚3,4-乙撑二氧噻吩/钴酸镍/碳布柔性电极 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106449175A (zh) * | 2016-11-14 | 2017-02-22 | 江苏大学 | 泡沫镍为基底的钨酸镍/聚苯胺超级电容器电极材料的制备方法 |
| CN107170589A (zh) * | 2017-04-14 | 2017-09-15 | 江苏大学 | 一种MnO2系三元复合超级电容器电极材料的制备方法 |
| CN107180704A (zh) * | 2017-05-16 | 2017-09-19 | 江苏大学 | 一种钴酸镍/钨酸镍/聚苯胺三元复合纳米线阵列电极的制备方法 |
| US20190173079A1 (en) * | 2017-12-05 | 2019-06-06 | Nanotek Instruments, Inc. | Method of Producing Participate Electrode Materials for Alkali Metal Batteries |
-
2019
- 2019-12-10 CN CN201911255198.7A patent/CN111009422B/zh active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106449175A (zh) * | 2016-11-14 | 2017-02-22 | 江苏大学 | 泡沫镍为基底的钨酸镍/聚苯胺超级电容器电极材料的制备方法 |
| CN107170589A (zh) * | 2017-04-14 | 2017-09-15 | 江苏大学 | 一种MnO2系三元复合超级电容器电极材料的制备方法 |
| CN107180704A (zh) * | 2017-05-16 | 2017-09-19 | 江苏大学 | 一种钴酸镍/钨酸镍/聚苯胺三元复合纳米线阵列电极的制备方法 |
| US20190173079A1 (en) * | 2017-12-05 | 2019-06-06 | Nanotek Instruments, Inc. | Method of Producing Participate Electrode Materials for Alkali Metal Batteries |
Non-Patent Citations (1)
| Title |
|---|
| ZHIYUAN YU: "《Facile synthesis of NiCo2O4@Polyaniline core–shell nanocompositefor sensitive determination of glucose》", 《BIOSENSORS AND BIOELECTRONICS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113782346A (zh) * | 2021-09-09 | 2021-12-10 | 福州大学 | 一种聚3,4-乙撑二氧噻吩/钴酸镍/碳布柔性电极 |
| CN113782346B (zh) * | 2021-09-09 | 2022-06-14 | 福州大学 | 一种聚3,4-乙撑二氧噻吩/钴酸镍/碳布柔性电极 |
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