CN114772560B - 室温铁磁二硒化钒纳米颗粒及其制备方法和作为析氧反应电催化剂的应用 - Google Patents
室温铁磁二硒化钒纳米颗粒及其制备方法和作为析氧反应电催化剂的应用 Download PDFInfo
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- WCQOLGZNMNEYDX-UHFFFAOYSA-N bis(selanylidene)vanadium Chemical compound [Se]=[V]=[Se] WCQOLGZNMNEYDX-UHFFFAOYSA-N 0.000 title claims abstract description 66
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Abstract
本发明提供了一种室温铁磁二硒化钒纳米颗粒及其制备方法和作为析氧反应电催化剂的应用。所述制备方法具体为:提供衬底和靶材,所述靶材为二硒化钒靶和碳靶的混合靶材;在真空环境中,使所述衬底和靶材沿相反方向旋转,并利用准分子激光轰击所述靶材,使得所述靶材中的二硒化钒和碳交替沉积到所述衬底上;在惰性气体氛围中,将沉积了二硒化钒和碳的所述衬底进行退火处理,得到所述室温铁磁二硒化钒纳米颗粒。这种新颖的室温铁磁二硒化钒纳米颗粒在充分暴露边缘催化活性位点的同时保证了较好的导电性,且在外磁场作用下析氧反应性能可以得到大幅提升;其在电解水析氧反应中表现出优异的催化活性、良好的稳定性以及显著的磁场增强析氧反应。
Description
技术领域
本发明属于电催化技术领域,具体涉及室温铁磁二硒化钒纳米颗粒及其制备方法和应用。
背景技术
析氧反应(Oxygen evolution reaction,OER)是水裂解、CO2还原和金属空气电池等众多电化学储能和转换技术中的关键过程。但OER的四电子过程动力学缓慢,从根本上限制了其反应效率。近年来,理论和实验研究表明室温铁磁(Ferromagnetic,FM)电催化剂利用自旋相关动力学可降低OER动力学势垒(即从自旋平行排列的氧原子到具有三重基态的氧分子的过程),从而提高反应效率。然而,大多数成本效益好的电催化剂在室温下是非室温铁磁性的。2018年,Manuel Bonilla等人报道了单层二硒化钒(VSe2)的室温铁磁性(《自然纳米技术》第13卷第289-293页),这得益于V 3d和Se 4p轨道杂化以及VSe2与范德华衬底之间的相互作用。然而单层VSe2在空气中极易氧化退化导致磁性消失,这对于实际应用来说是非常不理想的。因此,设计合成空气稳定的室温铁磁VSe2催化剂是研究者面临的一大挑战。
另一方面,VSe2具有优异的催化活性、结构稳定性和丰富的地球储量,被认为是可替代铂族贵金属的理想析氧反应电催化剂。VSe2的催化活性主要来源于晶体的活性边缘,而大面积的基面是惰性的。为提高VSe2析氧反应性能,一个很好的途径是增加其边缘活性位点数。其中,通过合成纳米颗粒等VSe2纳米催化剂可极大限度地提高活性边缘的暴露,是增加边缘活性位点数的最有效的方法之一。然而,在设计新型高效催化剂时,除了增加活性位点数外,如何提高催化剂的导电性也是研究者需要考虑的一个主要问题。
发明内容
有鉴于此,本发明的目的是提供一种室温铁磁二硒化钒纳米颗粒及其制备方法,以及作为析氧反应电催化剂的应用。
本发明提供的一种室温铁磁二硒化钒纳米颗粒的制备方法,包括以下步骤:
(1)提供衬底和靶材,所述靶材为二硒化钒靶和碳靶的混合靶材;
(2)在真空环境中,使所述衬底和靶材沿相反方向旋转,并利用准分子激光轰击所述靶材,使得所述靶材中的二硒化钒和碳交替沉积到所述衬底上;
(3)在惰性气体氛围中,将沉积了二硒化钒和碳的所述衬底进行退火处理,得到所述室温铁磁二硒化钒纳米颗粒。
优选地,所述靶材为通过银胶粘合的二硒化钒靶和碳靶混合靶材。更优选地,所述二硒化钒靶为高纯二硒化钒材料,其纯度大于等于99.99%;所述碳靶为高纯碳材料,其纯度大于等于99.99%。
优选地,所述真空环境是指气体压力小于等于1.0×10-8托(Torr)的环境。
优选地,所述旋转的速度为20转每分钟。
优选地,所述准分子激光为248纳米的氟化氪(KrF)准分子激光,激光能量为300毫焦(mJ),激光频率为5赫兹(Hz)。
优选地,所述惰性气体为氩气。
优选地,所述退火处理的温度为600℃,时间为5分钟。
上述方法得到的室温铁磁二硒化钒纳米颗粒在电解水析氧反应中表现出优异的催化活性、良好的稳定性以及显著的磁场增强析氧反应,可以作为析氧反应电催化剂。
本发明采用脉冲激光沉积技术结合快速退火方法制备获得了室温铁磁二硒化钒纳米颗粒,其在充分暴露边缘催化活性位点的同时保证了较好的导电性,且在外磁场作用下(磁化后)析氧反应性能可以得到大幅提升,可以作为电催化剂并应用于析氧反应。
附图说明
图1是本发明实施例中室温铁磁VSe2纳米颗粒的透射电子显微镜图。
图2是本发明实施例中室温铁磁VSe2纳米颗粒的X射线光电子能谱图。
图3是本发明实施例中室温铁磁VSe2纳米颗粒的拉曼光谱图。
图4是本发明实施例中室温铁磁VSe2纳米颗粒300 K下的磁滞曲线图。
图5是本发明实施例中在有无外磁场作用下,室温铁磁VSe2纳米颗粒的极化曲线图。
图6是本发明实施例中室温铁磁VSe2纳米颗粒的析氧性能稳定性测试结果图。
具体实施方式
下面对本发明实施例中的技术方案进行清楚、完整地描述,显然,所介绍的发明实施例仅是本发明一部分实施例,而非全部实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护范畴。
其次,本发明结合附图进行详细描述,在详述本发明实施例时,为便于说明,所述附图只是示例,其在此不应限制本发明保护的范围。
下述实施例中所述实验表征方法,如无特殊说明,均为常规方法;所述试剂、材料和仪器设备,如无特殊说明,均可从商业途径获得。
示例性实施例:
室温铁磁二硒化钒纳米颗粒析氧反应电催化剂采用脉冲激光沉积技术结合快速退火方法制备获得,具体包括以下步骤:
(1)分别将衬底和靶材放置在脉冲激光沉积系统的样品托和靶托上,两者间距为60毫米,靶材为通过银胶粘合的高纯(99.99%)二硒化钒靶和高纯(99.99%)碳靶混合靶材;
(2)将生长腔室真空抽至1.0×10-8托(Torr),样品托和靶托沿相反方向旋转,转速均为20转每分钟;并利用248纳米的氟化氪(KrF)准分子激光轰击混合靶材25分钟,激光能量为300毫焦(mJ),激光频率为5赫兹(Hz);
(3)设置氩气流速为30标况毫升每分钟(sccm),快速退火炉600℃退火5分钟,即可得到所述室温铁磁二硒化钒纳米颗粒。
图1示出了脉冲激光沉积技术结合快速退火方法制备获得的室温铁磁VSe2纳米颗粒的透射电子显微镜图,高密度单晶VSe2纳米颗粒均匀埋嵌在无定形碳基体中,平均颗粒尺寸约为4纳米。高分辨透射电子显微镜图显示纳米颗粒晶格间距为0.260纳米,与VSe2(011)晶面匹配。
图2示出了室温铁磁VSe2纳米颗粒的X射线光电子能谱图,确认了合成的VSe2纳米颗粒的元素组成和价态。
图3示出了室温铁磁VSe2纳米颗粒的拉曼光谱图,进一步证实合成的VSe2纳米颗粒具有很高的结晶质量。
图4示出了室温铁磁VSe2纳米颗粒在300 K(开尔文温度)下的磁滞回线,证实合成的VSe2纳米颗粒具有室温铁磁性。
在1 mol/L KOH溶液中开展三电极电化学测试,探究室温铁磁VSe2纳米颗粒析氧反应性能。其中,室温铁磁VSe2纳米颗粒作为工作电极,饱和Hg/HgO和石墨分别作为参比电极和对电极。
图5示出了在有无外磁场作用下,室温铁磁VSe2纳米颗粒的极化曲线。在外磁场作用下,室温铁磁VSe2纳米颗粒析氧反应性能得到显著提升。
图6示出了室温铁磁VSe2纳米颗粒的析氧性能稳定性测试,在10 mA/cm2恒定电流密度下进行催化析氧稳定性测试,在长达10小时的测试中,室温铁磁VSe2纳米颗粒展现出良好的催化稳定性。
以上所述仅为本发明的优选实施例而已,并不用于限制本发明,对于本领域的技术人员来说,本发明可以有各种更改和变化。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种室温铁磁二硒化钒纳米颗粒的制备方法,包括以下步骤:
(1)提供衬底和靶材,所述靶材为二硒化钒靶和碳靶的混合靶材;
(2)在真空环境中,使所述衬底和靶材沿相反方向旋转,并利用准分子激光轰击所述靶材,使得所述靶材中的二硒化钒和碳交替沉积到所述衬底上;
(3)在惰性气体氛围中,将沉积了二硒化钒和碳的所述衬底进行退火处理,得到所述室温铁磁二硒化钒纳米颗粒。
2.根据权利要求1所述的方法,其特征在于:所述靶材为通过银胶粘合的二硒化钒靶和碳靶混合靶材。
3.根据权利要求2所述的方法,其特征在于:所述二硒化钒靶为高纯二硒化钒材料,其纯度大于等于99.99%;所述碳靶为高纯碳材料,其纯度大于等于99.99%。
4.根据权利要求1所述的方法,其特征在于:所述真空环境是指气体压力小于等于1.0×10-8托(Torr)的环境。
5.根据权利要求1所述的方法,其特征在于:所述旋转的速度为20转每分钟。
6.根据权利要求1所述的方法,其特征在于:所述准分子激光为248纳米的氟化氪(KrF)准分子激光,激光能量为300毫焦(mJ),激光频率为5赫兹(Hz)。
7.根据权利要求1所述的方法,其特征在于:所述惰性气体为氩气。
8.根据权利要求1所述的方法,其特征在于:所述退火处理的温度为600℃,时间为5分钟。
9.根据权利要求1~8任一权利要求所述的方法得到的室温铁磁二硒化钒纳米颗粒。
10.根据权利要求9所述的室温铁磁二硒化钒纳米颗粒在电解水析氧反应中的应用。
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