CN113912132A - 缺陷异质结FeS2-Fe7S8的制备方法 - Google Patents
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- 238000007254 oxidation reaction Methods 0.000 claims abstract description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 9
- 229910052802 copper Inorganic materials 0.000 claims abstract description 9
- 239000010949 copper Substances 0.000 claims abstract description 9
- MQLVWQSVRZVNIP-UHFFFAOYSA-L ferrous ammonium sulfate hexahydrate Chemical compound [NH4+].[NH4+].O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O MQLVWQSVRZVNIP-UHFFFAOYSA-L 0.000 claims abstract description 9
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- 238000001035 drying Methods 0.000 claims description 5
- 238000000354 decomposition reaction Methods 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 19
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052723 transition metal Inorganic materials 0.000 description 4
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- -1 transition metal carbides Chemical class 0.000 description 3
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
- 229910052960 marcasite Inorganic materials 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
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- 229910052683 pyrite Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(IV) oxide Inorganic materials O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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Abstract
本发明涉及缺陷异质结FeS2‑Fe7S8的制备方法，具体的说是将六水合硫酸亚铁铵((NH4)2Fe(SO4)2·6H2O)溶于水，然后加入铜试剂(C5H10NS2Na·3H2O)，水热合成缺陷异质结FeS2‑Fe7S8，该缺陷异质结FeS2‑Fe7S8室温下实现电催化水氧化。
Description
技术领域
本发明涉及缺陷异质结FeS2-Fe7S8的制备方法，属于材料的制备领域。
背景技术
化石能源的大量使用给人们带来了严重的污染，另外作为不可再生资源，其大量消耗造成了能源危机。发展新型能源取代化石能源成为人们研究的前沿方向。其中水氧化制氧反应是现在研究的热点之一。目前，常用的水氧化反应的催化剂是Ru基催化剂。贵金属的稀缺性和高价格限制了其广泛应用。
目前，人们已经实现了过渡金属碳化物、过渡金属磷化物、过渡金属氮化物、过渡金属氧化物质、过渡金属硫化物等材料有效催化水氧化。其中，硫化铁作为地壳中含量较高的材料，研究其催化水氧化，引起了科学家的广大关注。导电性弱限制了硫化铁在催化水氧化领域的应用。人们通过对硫化铁进行掺杂、负载、纳米化等手段，研究了其催化水氧化性能。例如：Kuila等电沉积方法合成了Ni掺杂的FeS2材料，其在电催化水氧化反应中表现出优于RuO2催化剂的性能(ACS Sustainable Chemistry&Engineering 2019,7,1801-18026)。Liu等用硫脲为S源对N-CNTs@Ni3Fe进行硫化，得到了N-CNTs@NiS2/Fe7S8，其在电催化水氧化反应中，保持24h的稳定性(Chemical Communications,2020,56,1489)。Xi等利用甲酰胺通过剥离技术合成了丝状界面FeS2/NiS2复合纳米材料，其在催化水氧化反应中，过电势为233mV时达到10mA/cm2(Chinese Journal of Catalysis,2019,40,43-51)。目前，人们并没有实现将FeS2和Fe7S8合成为异质结结构。因此，合成缺陷异质结FeS2-Fe7S8对催化水氧化具有重要的意义。
发明内容：
本发明旨在提供缺陷异质结FeS2-Fe7S8的制备方法和其在电催化水氧化领域的应用。
基于上述目的，本发明所涉及的技术方案如下：
1)缺陷异质结FeS2-Fe7S8的制备方法：将0.5-1.2g六水合硫酸亚铁铵((NH4)2Fe(SO4)2·6H2O)溶于30-90mL水，然后加入0.4-0.8g铜试剂(C5H10NS2Na·3H2O)，200-260℃水热反应6-18h，经离心洗涤后，干燥得到缺陷异质结FeS2-Fe7S8。
2)当电压为1.53V时，缺陷异质结FeS2-Fe7S8电催化水氧化反应电流密度达到10mA/cm2。
本发明具有如下优点：
1)将六水合硫酸亚铁铵((NH4)2Fe(SO4)2·6H2O)溶于水，然后加铜试剂(C5H10NS2Na·3H2O)，水热合成了缺陷异质结FeS2-Fe7S8，开发了缺陷异质结FeS2-Fe7S8制备的新原料。
2)本发明简单易操作的特点。
附图说明：
图1是缺陷异质结FeS2-Fe7S8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
缺陷异质结FeS2-Fe7S8具体制备过程如下：将0.78g六水合硫酸亚铁铵((NH4)2Fe(SO4)2·6H2O)溶于60mL水，然后加入0.45g铜试剂(C5H10NS2Na·3H2O)，240℃水热反应12h，经离心洗涤后，干燥得到产物。
实施例2
将0.5g六水合硫酸亚铁铵((NH4)2Fe(SO4)2·6H2O)溶于30mL水，然后加入0.4g铜试剂(C5H10NS2Na·3H2O)，200℃水热反应6h，经离心洗涤后，干燥得到产物。
实施例3
将1.2g六水合硫酸亚铁铵((NH4)2Fe(SO4)2·6H2O)溶于90mL水，然后加入0.8g铜试剂(C5H10NS2Na·3H2O)，260℃水热反应18h，经离心洗涤后，干燥得到产物。
实施例4
将0.5g六水合硫酸亚铁铵((NH4)2Fe(SO4)2·6H2O)溶于90mL水，然后加入0.8g铜试剂(C5H10NS2Na·3H2O)，260℃水热反应18h，经离心洗涤后，干燥得到产物。
实施例5
将实施例1制成浆液，涂于镍电极上，利用CHI760E工作站，三电极体系催化水氧化，在1.0mol/L KOH电解液中，当电压为1.53V时，电流密度达到10mA/cm2。
Claims (2)
1.缺陷异质结FeS2-Fe7S8的制备方法，具体的说是将六水合硫酸亚铁铵((NH4)2Fe(SO4)2·6H2O)溶于水，然后加入铜试剂(C5H10NS2Na·3H2O)，水热合成缺陷异质结FeS2-Fe7S8，该缺陷异质结FeS2-Fe7S8室温下实现电催化水氧化；缺陷异质结FeS2-Fe7S8由如下步骤制得：将0.5-1.2g六水合硫酸亚铁铵((NH4)2Fe(SO4)2·6H2O)溶于30-90mL水，然后加入0.4-0.8g铜试剂(C5H10NS2Na·3H2O)，200-260℃水热反应6-18h，经离心洗涤后，干燥得到缺陷异质结FeS2-Fe7S8。
2.按照权利要求1所述的方法，其特征在于：
将缺陷异质结FeS2-Fe7S8电催化水分解。当电压为1.53V时，缺陷异质结FeS2-Fe7S8电催化水氧化反应电流密度达到10mA/cm2。
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| CN114808015A (zh) * | 2022-05-06 | 2022-07-29 | 青岛科技大学 | 一种Fe7S8-CoS-Co3S4异质结的制备方法 |
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