CN110444412A - 一种等级蜂窝状Ni3S2薄膜电极的制备方法 - Google Patents
一种等级蜂窝状Ni3S2薄膜电极的制备方法 Download PDFInfo
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- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 14
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- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 7
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
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Abstract
本发明公开了一种等级蜂窝状Ni3S2薄膜电极及其制备方法，首先以泡沫镍为基底，硝酸镍为镍源，六次甲基四胺（HMTA）为成核剂，采用水热法，得到由纳米片构成的Ni(OH)2蜂窝状薄膜；再以Ni(OH)2为基底，乙二醇作为溶剂，硫脲作为成核剂和硫化剂，一方面对Ni(OH)2进行硫化，使其转化成Ni3S2蜂窝，同时在Ni3S2上生成二次纳米片结构，即可得到等级蜂窝状Ni3S2薄膜电极。一方面，Ni3S2的导电性比Ni(OH)2更高，能加速电化学过程中电子传输；同时本发明制备的Ni3S2薄膜呈等级蜂窝结构，即组成蜂窝结构的纳米片表面又布满小纳米片团簇，该结构比单一蜂窝结构具有更大的比表面积，能提供更多的电化学反应活性位点，同时有利于电解液浸润和电解液离子传输，从而具有优异的电化学性能。
Description
技术领域
本发明超级电容器领域，具体涉及一种等级蜂窝状Ni3S2薄膜电极及其制备方法。
背景技术
采用具有高理论容量的赝电容材料作为电极材料，是提高超级电容器能量密度的有效途径之一。Ni(OH)2作为一种典型的赝电容材料，具有理论容量高、原料丰富、制备方法简单、成本低廉等优势，已成功应用于商用超级电容器。然而，目前商用超级电容器中Ni(OH)2受微观形貌和结构的限制，比容量通常远低于理论容量。研究表明，将Ni(OH)2制备成纳米结构，能增加比表面积，从而获得更高的容量，但目前研究中报道的Ni(OH)2仍然低于其理论容量。同时，由于导电性较差，Ni(OH)2作为超级电容器电极材料时倍率性能和循环稳定性能通常不够理想。相比于金属氢氧化物，金属硫化物的电导率普遍较高，特别是Ni2S3，甚至可归为导体一类，作为超级电容器电极材料时，显示出更优异的倍率特性和循环稳定性。
尽管目前文献中报道了多种制备方法，得到了不同微观结构的Ni2S3，但未见具有等级蜂窝状结构的Ni2S3。
发明内容
本发明的目的是针对Ni(OH)2电极材料比容量低，倍率性能和循环稳定性不佳的问题，对其微观结构和导电性进行双重优化的研究，通过简单的硫化处理即对Ni(OH)2薄膜电极进行硫化，获得导电性能更好的Ni3S2，同时在其表面构造二次纳米片团簇结构，增加电化学活性位点，从而得到具有优异电化学性能的等级蜂窝状Ni3S2薄膜。本方法具有简单易操作、性能优异、无污染等特点，适合制备各种金属硫化物材料。
本发明的技术方案：以泡沫镍为基底，利用两步水热方法，通过第一步获得蜂窝状Ni(OH)2薄膜，紧接着对Ni(OH)2薄膜进行硫化，获得等级蜂窝状Ni3S2薄膜，既提高了导电性，同时也增加了电化学活性位点。
本发明的技术方法包括以下步骤：
（1）将硝酸镍加入去离子水中，搅拌至充分溶解后加入六次甲基四胺（HMTA），再次搅拌，然后将所配溶液倒入反应釜内，将干净的泡沫镍放入反应釜中，在70-100℃，恒温反应8-12h，用去离子水冲洗干净并自然凉干；
（2）将硫脲加入乙二醇中，搅拌至充分溶解，然后将所配溶液倒入反应釜内，将上一步所制得的样品放入反应釜中，在一定温度下恒温加热一定时间后取出，先用去离子水冲洗，再用无水乙醇冲洗干净并自然凉干。其中硫脲的浓度为5~40mM，优选为20mM，加热温度为90-200℃，优选为150℃，加热时间为1-10h，优选为5h。
采用本发明的技术方案得到的材料呈等级蜂窝结构，均匀生长在泡沫镍基底表面，蜂窝孔洞大小为3-5μm，组成蜂窝的纳米片厚度约为100nm，纳米片表面又均匀生长了大小为100~200nm的纳米片团簇。
附图说明
图1为实施例1中等级蜂窝状结构的Ni3S2的扫描电镜照片。
图2为实施例1中等级蜂窝状的Ni3S2的XRD图。
图3为实施例1中等级蜂窝状的Ni3S2的循环伏安曲线。
图4为实施例1中等级蜂窝状的Ni3S2的比容量与电流密度关系图。
具体实施方式：
实施例1
称取1mmol硝酸镍溶解于40mL去离子水中，在超声作用下获得透明溶液，然后在磁力搅拌下，慢慢加入5mmol HMTA，待完全溶解后，将溶液倒入50mL反应釜内胆中，并放入一块3cm×5cm的泡沫镍，用不锈钢外套密封，放入80℃的恒温干燥箱内，保温10h，待反应釜降至室温后，取出泡沫镍，用去离子水反复冲洗泡沫镍表面，在自然条件下晾干即可得到Ni(OH)2薄膜。
称取1mmol硫脲溶解于50 mL乙二醇，磁力搅拌下充分溶解。将溶液倒入50mL反应釜内胆中，放入上述制得的Ni(OH)2薄膜，并用不锈钢外套密封，放入150℃的恒温干燥箱内，保温5h，待反应釜降至室温后，取出泡沫镍，先用去离子水反复冲洗镍网表面，再用无水乙醇反复冲洗泡沫镍，在自然条件下晾干，即可得到Ni3S2薄膜电极。
对所得的Ni3S2薄膜进行SEM和XRD分析，如图1所示：
图1中a,b为较低倍数下的SEM图，表明所得Ni3S2薄膜为蜂窝结构，均匀生长在泡沫镍基底上，蜂窝孔洞大小为3~5µm，构成蜂窝的纳米片厚度约为100nm，同时纳米片表面上均匀分布了大量白点。进一步放大得到c,d图，可以看出，纳米片表面的白点实际上是由更小的纳米片组成的团簇，大小约为100~200nm。正是由于这些均匀分布的纳米片团簇，增加了电极材料的比表面积和表面的活性位点，从而可以获得更高的容量。
图2为所得样品的XRD图，可以看出除了来自泡沫镍基底的峰，其余的峰都来自Ni3S2(JCPDS卡片号：44-1418)，表明该方案最终得到的材料为Ni3S2。
图3为所得样品的循环伏安曲线，每条曲线上成对的氧化还原峰表明具有很好的电化学可逆性，图4为不同电流密度下的比电容，当电流密度为2mA/cm2时，最大比电容可达到1800F/g，表明样品具有很好的储能性能。
Claims (3)
1.一种等级蜂窝状Ni3S2薄膜电极的制备方法，其特征在于，包括以下步骤：
（1）将硝酸镍水溶液中加入六次甲基四胺，搅拌均匀后倒入反应釜内胆，放入干净的泡沫镍，不锈钢外套密封后，恒温加热一定时间后取出，反应完成后用去离子水冲洗干净并自然凉干，得到Ni(OH)2薄膜；
（2）将步骤（1）所制得的Ni(OH)2薄膜放入内胆中，加入硫脲的乙二醇溶液，恒温加热一定时间后取出，依次用去离子水、无水乙醇冲洗，凉干，即可得到等级蜂窝状Ni3S2薄膜电极。
2.根据权利要求1所述的等级蜂窝状 Ni3S2薄膜电极的制备方法，其特征在于，步骤（1）中硝酸镍与六次甲基四胺的摩尔比为1:3-6，恒温反应温度为70-100℃，反应时间为8-12h。
3.根据权利要求1所述的等级蜂窝状 Ni3S2薄膜电极的制备方法，其特征在于，步骤（2）中硫脲的浓度为5~40mM，恒温反应温度为140-200℃，反应时间为1-10h。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111282582A (zh) * | 2020-03-19 | 2020-06-16 | 苏州楚捷新材料科技有限公司 | 一种泡沫镍基电解水制氢催化剂的制备方法 |
| WO2020230530A1 (ja) * | 2019-05-13 | 2020-11-19 | 国立大学法人新潟大学 | 触媒、電極、水電解方法および触媒の製造方法 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020230530A1 (ja) * | 2019-05-13 | 2020-11-19 | 国立大学法人新潟大学 | 触媒、電極、水電解方法および触媒の製造方法 |
| CN111282582A (zh) * | 2020-03-19 | 2020-06-16 | 苏州楚捷新材料科技有限公司 | 一种泡沫镍基电解水制氢催化剂的制备方法 |
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Application publication date: 20191112 |