CN110354872B - 一种具有优异电解水析氧性能的碳包覆Fe掺杂NiSe纳米材料及其制备方法 - Google Patents
一种具有优异电解水析氧性能的碳包覆Fe掺杂NiSe纳米材料及其制备方法 Download PDFInfo
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Abstract
一种具有优异电解水析氧性能的碳包覆Fe掺杂NiSe纳米材料及其制备方法。所述方法包括:将滤纸裁剪成1×2厘米的长方形纸条,乙醇中重复清洗三次后去取出后干燥;将干净滤纸浸泡在适量硝酸铁(Fe(NO3)3·9H2O)和硝酸镍(Ni(NO3)2·6H2O)的混合溶液中;将吸附饱和后的滤纸从混合溶液中取出,然后用卫生纸将滤纸表面多余的溶液吸干并干燥;把干燥后的饱和滤纸与硒粉一并放入管式炉中,在氮气保护下高温退火处理,得到Fe‑NiSe。本发明获得的Fe‑NiSe具有制备速度快、产率高,在碱性条件下电解水析氧方面具有重要的应用价值。
Description
技术领域
本发明涉及一种具有优异电解水析氧性能的碳包覆Fe掺杂NiSe纳米催化剂及其制备方法, 属于无机纳米材料技术领域。
背景技术
对现代社会来说,随着化石能源枯竭和环境污染问题日益严峻,可再生能源和清洁能源的发展研究显得越来越重要。氢气因具有较高的能量密度、环境友好和可再生等特点,是一种化石燃料的理想替代品。电化学催化水分解是一种高效的生产清洁氢能源的方法,但它的析氧反应(OER)需要一个超高的过电势来完成一个四电子转移过程,因此阻碍了水分解反应的速率。研究表明,贵金属氧化物(如IrO2和RuO2)对OER具有很高的催化活性,但是高昂的成本和地球资源的稀缺限制了他们的大规模实际应用。因此,制备出一个高效、经济的电化学催化剂来催化析氧反应是当务之急。
过渡金属储量丰富,价格低廉,其硒化物、硫化物、氧化物和磷化物的催化活性可与贵金属氧化物相媲美,成为最有潜力的电解水催化剂。但受到其暴露的活性位点少、在电解质溶液中易溶解、导电性差等问题的限制,寻找有效且经济的方法提高过渡金属基催化剂的析氧反应催化活性仍然是现在的一个研究难点。根据最近的文献报道,将过渡金属包裹在碳材料中,如碳纳米管、石墨烯等,形成金属@碳结构,不仅能有效解决过渡金属在电解液中稳定性差的问题,还能够防止相邻的金属纳米颗粒之间发生聚合,从而提高催化剂的析氧活性。因此我们选择过渡金属中的镍元素,将其负载到滤纸上,经高温硒化退火后滤纸的纤维形成多孔碳包覆在硒化镍上面,从而起到保护作用,可以有效提高催化剂的稳定性,而且掺杂铁元素可以有效的改变其电子结构,进一步提高导电性和催化活性。
发明内容
本发明要解决的技术问题为克服现有过渡金属硒化物的制备技术中的不足之处,发展一种具有优异电解水析氧性能的碳包覆Fe掺杂NiSe纳米材料(Fe-NiSe)的制备方法。
本发明中Fe-NiSe纳米材料的典型合成过程是将干净的滤纸浸泡在含有硝酸铁(Fe(NO3)3 .9H2O)和硝酸镍(Ni(NO3)2 .6H2O)的混合溶液中;待滤纸吸附饱和后,取出滤纸并将其表面多余的溶液用卫生纸吸收;最后,将干燥后的饱和滤纸与硒粉一并放入管式炉中,高温退火,得到Fe-NiSe纳米材料。
本发明中所述的一种具有优异电解水析氧性能的Fe-NiSe纳米材料的制备方法,包括以下具体步骤:
(1)将滤纸裁剪成1 × 2 厘米的长方形纸条,并浸泡在乙醇溶液中超声30分钟,重复清洗三次后去取出,在60摄氏度烘箱中晾干;
(2)将适量硝酸铁(Fe(NO3)3·9H2O)和硝酸镍(Ni(NO3)2·6H2O)加入到10毫升水中,溶解为均匀的混合溶液,再将步骤(1)中所得的干净滤纸在混合溶液中浸泡2小时,其中硝酸铁(Fe(NO3)3·9H2O)和硝酸镍(Ni(NO3)2·6H2O)的质量分别为0.5和1.0克;
(3)将吸附饱和后的滤纸从混合溶液中取出,然后用卫生纸将滤纸表面多余的溶液吸干,并在50摄氏度烘箱中烘干处理;
(4)把步骤(3)所得滤纸与0.5克硒粉一并放入管式炉中,并通入氮气进行保护,随后进行高温退火处理,先加热到450摄氏度保温2小时,再加热到750摄氏度保温两小时,升温速率为3摄氏度/分钟;
与现有技术相比,本发明所提供的一种具有优异电解水析氧性能的碳包覆Fe掺杂NiSe纳米材料(Fe-NiSe)的制备方法至少具有以下有益效果:
(1)本发明实施例所提供一种具有优异电解水析氧性能的碳包覆Fe掺杂NiSe纳米材料(Fe-NiSe)的制备方法最大优点在于原料价格便宜、来源广、反应过程简单;
(2)本发明实施例所提供的Fe-NiSe产量高、单分散性好,能够在室温、环境气氛条件下长时间保存;
(3)本发明实施例所提供的Fe-NiSe具有活性位点多、易吸附反应物等优点;
(4)本发明实施例所提供一种具有电解水析氧性能的Fe-NiSe纳米材料的制备方法仅需烧杯、石英舟、管式炉、烘箱等一些普通设备,工艺过程简单且易于操作;
(5)本发明实施例所提供的Fe-NiSe,对碱性环境中电解水析氧具有优异的催化活性,同时具有良好的稳定性。
附图说明
图1a为Fe-NiSe纳米材料的X-射线衍射花样,通过与标准卡片的比对可以证实Fe-NiSe的组分,其中由于铁离子的掺杂,铁镍的峰值相对于NiSe有轻微的变化;图1b为采用Sirion 200场发射扫描电子显微镜拍摄得到的低倍和高倍照片,可以看到约在200纳米左右的Fe-NiSe颗粒均匀的附着在滤纸的碳纤维上;图1c为Fe-NiSe纳米材料的铁(Fe)、镍(Ni)、硒(Se)和碳(C)元素的面分布图(EDX mapping),由图可以看出铁镍和硒均匀分布在碳层中;图1d为Fe-NiSe纳米材料的高分辨透射电子显微镜(HRTEM)照片, 由图可以清晰地观察到Fe-NiSe颗粒被包覆在碳层中,0.19纳米的晶格间距来自于Fe-NiSe的(110)晶面;图1e中的拉曼光谱显示了1350 cm-1和1590 cm-1的两个特征峰,其中1590 cm-1的g带是石墨烯的特征峰这表明Fe-NiSe纳米材料存在着一定程度的石墨化多孔碳。
图2a对制得的Fe-NiSe纳米材料进行表征得到的X-射线光电子能谱图,图2b-2d分别是Ni、Fe和Se的X-射线光电子能谱的高分辨图,由图可知制备的Fe-NiSe纳米材料确实含有铁、镍、硒和碳元素。
图3是将制备的Fe-NiSe纳米材料涂在泡沫镍(NF)上,在辰华760e电化学测试系统中测试得到的电化学图谱:图3a分别是Fe-NiSe、NiSe、RuO2和泡沫镍(Ni foam)的极化曲线,扫描速率为2毫伏/秒(mV/s),图3b是由图3a转化而来的塔菲尔曲线,图3c为Fe-NiSe和NiSe的阻抗谱图,图3d为Fe-NiSe和NiSe的双电层电容图;图3e和3f为Fe-NiSe的稳定性测试图谱,图3a的横坐标为Potential/V vs.RHE(即电极电势,单位为V),纵坐标为Currentdensenty(即电流密度,单位为mA cm-2);图3b的横坐标为电流密度的Log值即Log(j /mAcm-2),Potential/V vs.RHE(即电极电势,单位为V);图3c的横坐标为Z'/ohm (即欧姆(实部),单位为ohm),横坐标为-Z〞/ohm(即欧姆(虚部),单位为ohm);图3d的横坐标为测试扫描速度(单位为mV s-1),纵坐标为Current densenty(即电流密度,单位为mA cm-2)图3e的横坐标Time(即时间,单位为h),纵坐标为Current densenty(即电流密度,单位为mA cm-2),图3f的横坐标Potential/V vs.RHE(即电极电势,单位为V),纵坐标为Current densenty(即电流密度,单位为mA cm-2),图3说明相比于NiSe、RuO2和泡沫镍(Ni foam),所制备的Fe-NiSe具有最优异的催化活性、最高的反应速率、最小的电阻以及连续20小时或循环1000圈之后仍然具有较好的稳定性。
具体实施方式
首先准备本发明用到的滤纸、硝酸铁(Fe(NO3)3·9H2O)和硝酸镍(Ni(NO3)2·6H2O),随后将滤纸浸泡在硝酸铁(Fe(NO3)3·9H2O)和硝酸镍(Ni(NO3)2·6H2O)的混合溶液中,待吸附饱和后干燥,最后经高温退火硒化过程得到Fe-NiSe。
下面结合具体实施实例对本发明的内容作进一步详细说明,显然所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明的实施例,本领域普通技术人员在没有付出创造性劳动前提下所获得的所有其他实施例,都属于本发明的保护范围。
实施例1
将0.5克硝酸铁(Fe(NO3)3·9H2O)和1.0克硝酸镍(Ni(NO3)2·6H2O)加入到10毫升水中,溶解为均匀的混合溶液,再将处理干净的滤纸在混合溶液中浸泡2小时,吸附饱和后取出滤纸用卫生纸将表面多余的溶液吸干,烘干处理后与0.5克硒粉一并放入管式炉中,氮气气氛下,先加热到450摄氏度保温2小时,再加热到750摄氏度保温2小时后自然降温至室温,即得到Fe-NiSe复合电解水析氧催化剂。
实施例2
将1.0克硝酸铁(Fe(NO3)3·9H2O)和2.0克硝酸镍(Ni(NO3)2·6H2O)加入到20毫升水中,溶解为均匀的混合溶液,再将处理干净的滤纸在混合溶液中浸泡2小时,吸附饱和后取出滤纸用卫生纸将表面多余的溶液吸干,烘干处理后与0.5克硒粉一并放入管式炉中,氮气气氛下,先加热到450摄氏度保温2小时,再加热到750摄氏度保温2小时后自然降温至室温,即得到Fe-NiSe复合电解水析氧催化剂。
实施例3
将0.5克硝酸铁(Fe(NO3)3·9H2O)和1.0克硝酸镍(Ni(NO3)2·6H2O)加入到10毫升水中,溶解为均匀的混合溶液,再将处理干净的滤纸在混合溶液中浸泡1小时,吸附饱和后取出滤纸用卫生纸将表面多余的溶液吸干,烘干处理后与0.5克硒粉一并放入管式炉中,氮气气氛下,先加热到450摄氏度保温2小时,再加热到750摄氏度保温2小时后自然降温至室温,即得到Fe-NiSe复合电解水析氧催化剂。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到的变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应该以权利要求书的保护范围为准。
Claims (2)
1.一种具有优异电解水析氧性能的碳包覆Fe掺杂NiSe纳米材料Fe-NiSe的制备方法,其特征在于:
(1)将普通滤纸浸泡在九水合硝酸铁和六水合硝酸镍的混合溶液中,吸附饱和后经干燥处理,再进行一步硒化退火处理即可得到Fe-NiSe;所述的混合溶液为九水合硝酸铁和六水合硝酸镍以质量比1:2的比例配制而成
(2)Fe-NiSe为碳包覆Fe掺杂的NiSe纳米结构,滤纸的碳纤维在高温退火后形成部分石墨化的多孔碳;
所述Fe-NiSe在室温环境中具有很好的稳定性;
所述Fe-NiSe在碱性条件下具有优异的电解水析氧的催化活性。
2.一种权利要求1所述的制备方法,其特征在于:
(1)将滤纸裁剪成1 × 2 厘米的长方形纸条,并浸泡在乙醇溶液中超声30分钟,重复清洗三次后取出,在60摄氏度烘箱中晾干;
(2)将0.5克九水合硝酸铁和1.0克六水合硝酸镍加入到10毫升水中,溶解为均匀的混合溶液,再将步骤(1)中所得的干净滤纸在混合溶液中浸泡2小时;
(3)将吸附饱和后的滤纸从混合溶液中取出,然后用卫生纸将滤纸表面多余的溶液吸干,并在50摄氏度烘箱中烘干处理;
(4)把步骤(3)所得滤纸与0.5克硒粉一并放入管式炉中,并通入氮气进行保护,随后进行高温退火处理,先升温至450摄氏度保温2小时再升温至750摄氏度保温2小时,其中升温速率为3摄氏度/分钟。
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