CN114808016A - 一种Fe7S8/CoS缺陷异质结微米片的制备方法 - Google Patents
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- 230000007547 defect Effects 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 12
- 230000003647 oxidation Effects 0.000 claims abstract description 10
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 claims abstract description 8
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- 238000002156 mixing Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 19
- 239000000203 mixture Substances 0.000 description 5
- 229910052952 pyrrhotite Inorganic materials 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 description 1
- 229910017390 Au—Fe Inorganic materials 0.000 description 1
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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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
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。
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Citations (3)
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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 |
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 |
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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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 |
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 |
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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Title |
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LIYUAN WU ET AL.: "The synergy of sulfur vacancies and heterostructure on CoS@FeS nanosheets for boosting the peroxymonosulfate activation", CHEMICAL ENGINEERING JOURNAL, vol. 446, pages 136759 * |
MATHIAS SMIALKOWSKI ET AL.: "Fe/Co and Ni/Co‐pentlandite type electrocatalysts for the hydrogen evolution reaction", CHINESE JOURNAL OF CATALYSIS, vol. 42, pages 1360 * |
WENPIN WANG ET AL.: "Enhanced oxygen and hydrogen evolution performance by carbon-coated CoS2–FeS2 nanosheets", DALTON TRANSACTIONS, vol. 49, pages 13352 - 13358 * |
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徐跃: "铁基硫化物纳米材料的制备及其电催化水分解性能研究", 中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑, no. 01, pages 014 - 945 * |
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