CN114808016B - 一种Fe7S8/CoS缺陷异质结微米片的制备方法 - Google Patents

一种Fe7S8/CoS缺陷异质结微米片的制备方法 Download PDF

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CN114808016B
CN114808016B CN202210488633.6A CN202210488633A CN114808016B CN 114808016 B CN114808016 B CN 114808016B CN 202210488633 A CN202210488633 A CN 202210488633A CN 114808016 B CN114808016 B CN 114808016B
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CN114808016A (zh
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李忠成
王文嫔
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Qingdao University of Science and Technology
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Abstract

本发明涉及一种Fe7S8/CoS缺陷异质结微米片的制备方法，具体的说是FeCl3·6H2O、CoCl2·6H2O、KSCN为前驱体，水热制备Fe7S8/CoS缺陷异质结微米片，该Fe7S8/CoS缺陷异质结微米片可高效电催化水氧化。

Description

一种Fe7S8/CoS缺陷异质结微米片的制备方法
技术领域
本发明涉及一种Fe7S8/CoS缺陷异质结微米片的制备方法，属于材料的制备领域。
背景技术
铁基硫化物因为在地壳中储量丰富、价格低廉等优点，而在水分解领域被广泛关注。其中磁黄铁矿Fe7S8是一类混合价态的硫化铁，研究表明磁黄铁矿Fe7S8对水分解具有一定的催化活性，但目前研究的较少，且活性较低。因此调变磁黄铁矿Fe7S8表面组成，改进催化反应动力学，高效催化水分解是十分必要的。
合成微纳米尺度的材料，构建异质材料和设计缺陷是主要的改进方法。例如：Javaid等将Au纳米粒子、CoCl2·6H2O、NiCl2·6H2O、Fe7S8、十六胺混合，焙烧后得到Ni2+/Co2 +掺杂的doped Au-Fe7S8纳米片,其催化水氧化反应，在过电势243mV时，电流密度为10mA/cm2(Nano Energy89(2021)106463)。Le等利用NaH2PO2·H2O磷化硫铁化合物得到P掺杂的Fe7S8@C纳米线，其催化水氧化，在过电势210mV时，电流密度为20mA/cm2(J.Mater.Sci.Technol.74(2021)168-175)。Jiang等将Fe7S8纳米粒子包覆入N,S共掺杂的C，其催化水氧化，在过电势450mV时，电流密度为10mA/cm2(Micro Nano Lett.15(2020)495-498)。因此，调变磁黄铁矿高效催化水氧化，具有重要的意义。
随着人类对于清洁能源的需求日益增加，寻求可持续的绿色、清洁能源显得更为重要。电催化水氧化反应是电解水反应的半反应，调变磁黄铁矿Fe7S8表面结构，使其高效催化水氧化，具有重要的科学价值。
发明内容：
本发明旨在提供一种Fe7S8/CoS缺陷异质结微米片的制备方法和其在电催化水氧化反应中的应用。
基于上述目的，本发明所涉及的技术方案如下：
1)一种Fe7S8/CoS缺陷异质结微米片：将0.5～0.6g FeCl3·6H2O、0.2～0.3gCoCl2·6H2O、0.3～0.4g KSCN加入到55～65mL水，混合均匀，在反应釜中于230～250℃处理10～18h，产物经离心、干燥得到Fe7S8/CoS缺陷异质结微米片。
2)将Fe7S8/CoS缺陷异质结微米片用于催化水氧化，电压为1.47V时，电流密度为10mA/cm2。
本发明具有如下优点：
1)将FeCl3·6H2O、CoCl2·6H2O、KSCN为前驱体，构建了Fe7S8/CoS缺陷异质结微米片，拓展了Fe7S8/CoS缺陷异质结微米片的合成路径。
2)本发明具有操作简单的特点。
附图说明：
图1是Fe7S8/CoS缺陷异质结微米片的XRD表征结果。
具体实施方式
下列实施例用来进一步说明本发明，但不因此而限制本发明。
实施例1
Fe7S8/CoS缺陷异质结微米片制备过程如下：将0.5g FeCl3·6H2O、0.2g CoCl2·6H2O、0.3g KSCN加入到55mL水，混合均匀，在反应釜中于230℃处理10h，产物经离心、干燥得到Fe7S8/CoS缺陷异质结微米片。
实施例2
将0.6g FeCl3·6H2O、0.3g CoCl2·6H2O、0.4g KSCN加入到65mL水，混合均匀，在反应釜中于250℃处理18h，产物经离心、干燥得到。
实施例3
将0.55g FeCl3·6H2O、0.25g CoCl2·6H2O、0.35g KSCN加入到60mL水，混合均匀，在反应釜中于240℃处理12h，产物经离心、干燥得到。
实施例4
取实施例1浆液滴涂于1×1cm2泡沫镍电极上，干燥后在三电极体系下测其催化水氧化，电压为1.47V时，电流密度为10mA/cm2。

Claims (2)

1.一种Fe7S8/CoS缺陷异质结微米片的制备方法，具体的说是FeCl3·6H2O、CoCl2·6H2O、KSCN为前驱体，水热制备Fe7S8/CoS缺陷异质结微米片，该Fe7S8/CoS缺陷异质结微米片可高效电催化水氧化；Fe7S8/CoS缺陷异质结微米片由如下步骤制得：将0.5～0.6g FeCl3·6H2O、0.2～0.3g CoCl2·6H2O、0.3～0.4g KSCN加入到55～65mL水，混合均匀，在反应釜中于230～250℃处理10～18h，产物经离心、干燥得到Fe7S8/CoS缺陷异质结微米片。
2.按照权利要求1所述的方法，其特征在于：
将Fe7S8/CoS缺陷异质结微米片用于催化水氧化，电压为1.47V时，电流密度为10mA/cm2。
CN202210488633.6A 2022-05-06 2022-05-06 一种Fe7S8/CoS缺陷异质结微米片的制备方法 Active CN114808016B (zh)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108682563A (zh) * 2018-04-17 2018-10-19 江苏大学 一种Fe7S8@Fe5Ni4S8复合电极材料及其制备方法和应用
CN113937281A (zh) * 2021-09-24 2022-01-14 中国科学院深圳先进技术研究院 负极材料及其制备方法和钠离子电池

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US20210162392A1 (en) * 2019-12-03 2021-06-03 The Governing Council Of The University Of Toronto Electrocatalysts comprising transition metals and chalcogen for oxygen evolution reactions (oer) and manufacturing thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108682563A (zh) * 2018-04-17 2018-10-19 江苏大学 一种Fe7S8@Fe5Ni4S8复合电极材料及其制备方法和应用
CN113937281A (zh) * 2021-09-24 2022-01-14 中国科学院深圳先进技术研究院 负极材料及其制备方法和钠离子电池

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Co8FeS8/Fe7S8@N-doped porous carbons as highly efficient and stable electrocatalysts for oxygen evolution reaction;Hai Yu et al.;Journal of Solid State Chemistry;第310卷;第123033页 *
Constructing bifunctional Fe7S8/CoS heterostructures for efficient water electrolysis;Yue Xu et al.;international journal of hydrogen energy;第48卷;第113-122页 *
Enhanced oxygen and hydrogen evolution performance by carbon-coated CoS2–FeS2 nanosheets;Wenpin Wang et al.;Dalton Transactions;第49卷;第13352-13358页 *
Fe/Co and Ni/Co‐pentlandite type electrocatalysts for the hydrogen evolution reaction;Mathias Smialkowski et al.;Chinese Journal of Catalysis;第42卷;第1360–1369页 *
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