CN113470983A - 一种硒化镍—二硒化三镍纳米棒复合材料及其制备方法和应用 - Google Patents
一种硒化镍—二硒化三镍纳米棒复合材料及其制备方法和应用 Download PDFInfo
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- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 239000002073 nanorod Substances 0.000 title claims abstract description 23
- XIMIGUBYDJDCKI-UHFFFAOYSA-N diselenium Chemical compound [Se]=[Se] XIMIGUBYDJDCKI-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- QHASIAZYSXZCGO-UHFFFAOYSA-N selanylidenenickel Chemical compound [Se]=[Ni] QHASIAZYSXZCGO-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 13
- -1 transition metal selenide Chemical class 0.000 claims abstract description 10
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- 238000006243 chemical reaction Methods 0.000 claims description 22
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- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 12
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000011065 in-situ storage Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 239000007774 positive electrode material Substances 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
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- YGHCWPXPAHSSNA-UHFFFAOYSA-N nickel subsulfide Chemical compound [Ni].[Ni]=S.[Ni]=S YGHCWPXPAHSSNA-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
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- 238000006479 redox reaction Methods 0.000 description 2
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- 238000004729 solvothermal method Methods 0.000 description 2
- 229910005809 NiMoO4 Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
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- 239000002135 nanosheet Substances 0.000 description 1
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Abstract
本发明公开一种硒化镍—二硒化三镍纳米棒复合材料及其制备方法和应用,以泡沫镍为镍源,Se粉为硒源,采用一步溶剂热法在泡沫镍表面原位生成Ni3Se2/NiSe纳米棒复合结构电极材料,具有优异的电化学性能,其最大比容量为1068.0μAhcm‑2。本发明制备的过渡金属硒化物相较于普通所得具有更多的活性位点,在作为电极材料的应用中具有更好的电化学性能,原料廉价易得,工艺流程简单,有望实现工业化制备过渡金属硒化物。
Description
技术领域
本发明属于复合新材料技术领域,更加具体地说,涉及一种Ni3Se2/NiSe纳米棒复合正极材料及其制备方法,主要应用于超级电容器的正极材料。
技术背景
超级电容器是指介于传统电容器和充电电池之间的一种新型储能装置,它既具有电容器快速充放电的特性,同时又具有电池的储能特性。相较于其他储能器件,突出优点是功率密度高、充放电时间短、循环寿命长、工作温度范围宽,是世界上已投入量产的电容器中容量最大的一种。因此它在移动通讯,电动交通工具,航空航天等电化学储能领域具有很大的潜在应用价值。作为超级电容器的核心,电极材料的电化学性能对其储能性能起决定性的影响。金属基硫化物电极材料凭借材料来源丰富、低成本、高理论比容量和高导电性等优点成为有潜力的超级电容器电极材料。而其复合电极材料更是达成两种电极材料之间性能的互补,复合材料结构单元可有不同的组分组合而成,材料间由于多种界面的引入和存在,更有利于实现1+1>2的优化效果。近年来随着对镍基电极材料的深入研究,其与过渡金属化合物结合形成的复合材料也倍受关注,大多数研究为Ni3S2/CoS、NiS/Ni3S2、NiS/NiMoO4等复合电极材料,但对Ni3Se2/NiSe纳米棒复合结构却鲜有涉及。
发明内容
本发明的目的在于克服现有技术的不足,提供一种硒化镍—二硒化三镍纳米棒复合材料及其制备方法和应用,将其应用于超级电容器的正极材料。
本发明的技术目的通过下述技术方案予以实现。
一种硒化镍—二硒化三镍纳米棒复合材料及其制备方法,以泡沫镍为镍源,硒粉为硒源,采用一步溶剂热法在泡沫镍表面原位生成Ni3Se2/NiSe复合材料。
将硒粉均匀分散在无水乙二胺中,再加入无水乙醇,分散均匀以形成反应溶液;将泡沫镍置于所述反应溶液中进行反应,以在泡沫镍表面原位生成Ni3Se2/NiSe复合材料。
而且,采用聚四氟乙烯反应釜为水热反应容器,体积为100—200mL。
而且,无水乙二胺和无水乙醇的体积比为2:1。
而且,在使用之前,对泡沫镍进行处理,以去除油污,促进反应,泡沫镍的大小为3cm×2cm×1.5mm。
而且,反应的气氛为空气、温度为160—190摄氏度,反应时间为8—12小时。
而且,反应的气氛为空气、温度为160—180摄氏度,反应时间为10—12小时。
而且,Se粉和无水乙二胺的质量比为1:(100—500),优选1:(300—400)。
与现有技术相比,本发明的高性能Ni3Se2/NiSe复合超级电容器正极材料,属于新能源储存领域,以泡沫镍为镍源,Se粉为硒源,采用一步溶剂热法在泡沫镍表面原位生成Ni3Se2/NiSe纳米棒复合结构电极材料。基于Ni3Se2/NiSe的超级电容器材料组装的混合超级电容器具有优异的电化学性能,其最大比容量为1068.0μAh cm-2。本发明制备的过渡金属硒化物相较于普通所得具有更多的活性位点,在作为电极材料的应用中具有更好的电化学性能,原料廉价易得,工艺流程简单,有望实现工业化制备过渡金属硒化物。
附图说明
图1为本发明制备的Ni3Se2/NiSe电极材料的SEM照片。
图2为本发明制备的Ni3Se2/NiSe电极材料的XRD图。
图3为本发明制备的Ni3Se2/NiSe电极材料的TEM照片。
图4为本发明制备的Ni3Se2/NiSe电极材料应用于超级电容器的循环伏安性能测试和倍率性能测试结果曲线图。
具体实施方式
下面结合具体实施例进一步说明本发明的技术方案。
实施例1
将0.8mmoL Se粉溶解至20mL无水乙二胺中,形成均匀的溶液A,然后将10mL无水乙醇的混合均匀溶液加到溶液A中后,用磁力搅拌充分搅拌形成均匀的溶液B。最后将均匀的溶液B转移至100mL聚四氟乙烯反应釜中并加入已处理好的泡沫镍(3cm×2cm×1.5mm),在鼓风干燥箱中180℃反应10h制得复合材料Ni3Se2/NiSe。
实施例2
在实施例1的基础之上,调整反应温度为160摄氏度,时间为12小时。
实施例3
在实施例1的基础之上,调整反应温度为190摄氏度,时间为8小时。
下面以复合结构Ni3Se2/NiSe电极材料为例,对本发明制备的Ni3Se2/NiSe纳米棒复合结构电极材料(实施例1)进行表征。SEM图如图1所示,可以明显看出泡沫镍表面原位生长纳米棒,且在泡沫镍上生长的非常均匀,并具有坚固的结构。图2是电极材料的X射线粉末衍射(XRD)图。数据中在29.6°、29.9°、37.2°、47.7°和52.7°对应的是Ni3Se2(JCPDS No.85-0754)的特征峰,其对应的峰的晶面分别为(110)、(012)、(003)、(211)和(122)晶面;而在31.0°、34.0°、38.7°、48.0°、50.4°和55.1°对应的是NiSe(JCPDS No.18-0887)的特征峰其对应的峰的晶面分别为(300)、(021)、(211)、(410)、(401)和(300)晶面。而且数据中除了Ni、NiSe和Ni3Se2的特征峰外,没有发现其他的衍射峰,这表明在本实验中,在泡沫镍上直接生长Ni3Se2和NiSe复合结构。图3为复合材料的TEM图,可以看出复合材料是在纳米棒和纳米片复合形成的纳米棒。
以Ni3Se2/NiSe复合电极材料为工作电极(1cm×1cm×1.5mm),Hg/HgO(1M KOH)为参比电极,活性炭(AC)为对电极构成三电极系统,在3M KOH电解液中,控制扫描速度为2~20mV s-1,测得循环伏安曲线如图4中a所示,可以看出Ni3Se2/NiSe电极材料在充放电过程中存在明显的氧化还原反应,电流密度随着扫速的增加而增加,且氧化峰向右偏移,还原峰向左偏移。不同扫速下循环伏安曲线非常相似,表明电极发生氧化还原反应过程速度控制步骤受动力学控制;控制电流密度为2~50mA cm-2,测得恒电流充放电曲线如图4中b和c所示,当电流密度为2mA cm-2时,电极材料的质量比容量高达1068.0μAh cm-2,当电流密度为15mA cm-2时,电极材料的质量比容量高达792.0μAh cm-2,其容量保持率高达74.2%。
根据本发明内容进行工艺参数的调整,均可实现复合材料Ni3Se2/NiSe的制备,经测试表现出与本发明基本一致的性能。以上对本发明做了示例性的描述,应该说明的是,在不脱离本发明的核心的情况下,任何简单的变形、修改或者其他本领域技术人员能够不花费创造性劳动的等同替换均落入本发明的保护范围。
Claims (9)
1.一种硒化镍—二硒化三镍纳米棒复合材料,其特征在于,以泡沫镍为镍源,硒粉为硒源,将硒粉均匀分散在无水乙二胺中,再加入无水乙醇,分散均匀以形成反应溶液;将泡沫镍置于所述反应溶液中进行反应,以在泡沫镍表面原位生成Ni3Se2/NiSe复合材料;硒粉和无水乙二胺的质量比为1:(100—500),无水乙二胺和无水乙醇的体积比为2:1;反应的气氛为空气、温度为160—190摄氏度,反应时间为8—12小时。
2.根据权利要求1所述的一种硒化镍—二硒化三镍纳米棒复合材料,其特征在于,反应的气氛为空气、温度为160—180摄氏度,反应时间为10—12小时。
3.根据权利要求1所述的一种硒化镍—二硒化三镍纳米棒复合材料,其特征在于,硒粉和无水乙二胺的质量比为1:(300—400)。
4.根据权利要求1所述的一种硒化镍—二硒化三镍纳米棒复合材料,其特征在于,采用聚四氟乙烯反应釜为水热反应容器,体积为100—200mL;泡沫镍的大小为3cm×2cm×1.5mm。
5.一种硒化镍—二硒化三镍纳米棒复合材料的制备方法,其特征在于,以泡沫镍为镍源,硒粉为硒源,将硒粉均匀分散在无水乙二胺中,再加入无水乙醇,分散均匀以形成反应溶液;将泡沫镍置于所述反应溶液中进行反应,以在泡沫镍表面原位生成Ni3Se2/NiSe复合材料;硒粉和无水乙二胺的质量比为1:(100—500),无水乙二胺和无水乙醇的体积比为2:1;反应的气氛为空气、温度为160—190摄氏度,反应时间为8—12小时。
6.根据权利要求5所述的一种硒化镍—二硒化三镍纳米棒复合材料的制备方法,其特征在于,反应的气氛为空气、温度为160—180摄氏度,反应时间为10—12小时。
7.根据权利要求5所述的一种硒化镍—二硒化三镍纳米棒复合材料的制备方法,其特征在于,硒粉和无水乙二胺的质量比为1:(300—400)。
8.根据权利要求5所述的一种硒化镍—二硒化三镍纳米棒复合材料的制备方法,其特征在于,采用聚四氟乙烯反应釜为水热反应容器,体积为100—200mL;泡沫镍的大小为3cm×2cm×1.5mm。
9.如权利要求1—4之一所述的一种硒化镍—二硒化三镍纳米棒复合材料在超级电容器的正极材料中的应用。
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Cited By (3)
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CN113789535A (zh) * | 2021-10-09 | 2021-12-14 | 华中科技大学 | 一种棒状钌颗粒/硒化物复合催化剂及其制备方法与应用 |
CN114724866A (zh) * | 2022-03-11 | 2022-07-08 | 上海健康医学院 | 一种无粘接剂的钒掺杂硒化镍纳米阵列材料及其制备方法和应用 |
CN115458336A (zh) * | 2022-09-20 | 2022-12-09 | 青岛科技大学 | 一种超级电容器正极材料的制备方法 |
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