CN112481633B - Carbon-coated CoS2-FeS2Preparation method of heterojunction nanosheet - Google Patents

Carbon-coated CoS2-FeS2Preparation method of heterojunction nanosheet Download PDF

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CN112481633B
CN112481633B CN202010868515.9A CN202010868515A CN112481633B CN 112481633 B CN112481633 B CN 112481633B CN 202010868515 A CN202010868515 A CN 202010868515A CN 112481633 B CN112481633 B CN 112481633B
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CN112481633A (en
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李忠成
王文嫔
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Qingdao University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Abstract

The invention relates to a carbon-coated CoS2‑FeS2Preparation method of heterojunction nanosheet, specifically CoCl2·6H2O、FeCl3·6H2O, copper reagent C5H10NS2Na·3H2O is used as a precursor, and carbon-coated CoS is synthesized by hydrothermal synthesis2‑FeS2Heterojunction nanoplatelets, the carbon-coated CoS2‑FeS2The heterojunction nanosheet can be used for efficiently and electrically catalyzing and decomposing water at room temperature.

Description

Carbon-coated CoS2-FeS2Preparation method of heterojunction nanosheet
Technical Field
The invention relates to carbon-coated CoS2-FeS2A preparation method of a heterojunction nanosheet belongs to the field of preparation of materials.
Background
Transition metal sulfides are of great interest because of their specific physicochemical properties. FeS2The soil crust is rich in content, has excellent optical, magnetic, electrical and catalytic properties, and becomes a hotspot of recent research. But FeS2The defects of low conductivity, poor cycling stability and the like limit further application of the conductive material. Thus modulating FeS2Surface composition or nanosized FeS2The method has important practical significance for changing the performance of the product.
Modified FeS2The FeS is modulated due to its simple process and low cost2Important methods of materials. For example: zhang et al convert FeS2Deposited on TiO2Synthesis of FeS on nanotubes2/TiO2Nanotubes exhibiting excellent properties in photoelectrocatalytic decomposition of water (ACS Sustainable Chemistry)&Engineering,2016,4, 6659-6667). Kang et al used FeSO4·7H2O、 CoSO4·7H2O, S powder as precursor, and synthesizing Co-doped FeS by hydrothermal method at 180 ℃ for 12h2Nanospheres (Angewandte Chemie-International Edition,2016,55, 12822-. Using FeCl for Li or the like3·6H2O and C5H10NS2Na·3H2O hydrothermal synthesis of pyrite FeS2Nanoparticles; mixing it with C, effectively achieving catalytic water decomposition (Dalton Transactions,2018,47, 14917-. Therefore, the new path synthesis modulation FeS is used2It is important that the material and the catalyst are highly active to effect the catalytic reaction.
Mainly by CH in industry4And H2The disadvantages of high-temperature reaction of O to prepare hydrogen, use of fossil fuel, environmental pollution and the like cause resource crisis and harm to human living environment. The hydrogen is prepared by electrocatalysis water decomposition, and has wide application prospect due to the advantages of mild condition, no pollution and the like. Modulation of FeS2The material has important scientific value for the high-efficiency catalytic decomposition of water.
The invention content is as follows:
the present invention aims to provideCarbon-coated CoS2-FeS2A preparation method of the heterojunction nanosheet and application of the heterojunction nanosheet in preparing hydrogen by electrocatalytic decomposition of water.
Based on the above purpose, the technical scheme of the invention is as follows:
1) carbon coated CoS2-FeS2Heterojunction nanosheet: adding 50-240 mg CoCl into a beaker2·6H2O，0.4～0.6g FeCl3·6H2O, 0.4-0.6 g of copper reagent (C)5H10NS2Na·3H2O) and 40-80mL of water are stirred until the solution is dissolved, the obtained liquid is transferred into a stainless steel reaction kettle with a polytetrafluoroethylene lining for hydrothermal treatment at the temperature of 220-260 ℃ for 6-24 h, then the solution is naturally cooled to room temperature, and the product is centrifugally washed and dried to obtain carbon-coated CoS2-FeS2A heterojunction nanosheet.
2) Coating carbon with CoS2-FeS2The heterojunction nanosheet is used for preparing hydrogen through electrocatalysis water decomposition at room temperature. The current density is 20mA/cm at a voltage of 1.73V2At a voltage of 1.9V, the current density was 100mA/cm2。
The invention has the following advantages:
1) using CoCl2·6H2O，FeCl3·6H2O, copper reagent (C)5H10NS2Na·3H2O) is taken as a precursor, and carbon-coated CoS is hydrothermally synthesized2-FeS2The heterojunction nano-sheet effectively expands the carbon-coated CoS2-FeS2A preparation method of heterojunction nanometer material.
2) The method has the characteristics of simplicity, high efficiency and low cost.
Description of the drawings:
FIG. 1 is carbon-coated CoS2-FeS2Characterization results of the heterojunction nanoplatelets, (a-b) electron microscopy pictures and (c) XRD.
Detailed Description
The following examples are intended to further illustrate the invention but are not intended to limit the invention thereto.
Example 1
Carbon coated CoS2-FeS2The specific preparation process of the heterojunction nanosheet is as follows: 170mg CoCl was added to the beaker2·6H2O、 0.54g FeCl3·6H2O, 0.45g of copper reagent (C)5H10NS2Na·3H2O) and 60mL of water are stirred until the mixture is dissolved, the obtained liquid is transferred into a stainless steel reaction kettle with a polytetrafluoroethylene lining for hydrothermal treatment at 240 ℃ for 12 hours, then the mixture is naturally cooled to room temperature, and the product is centrifugally washed and dried.
Example 2
50mg CoCl was added to the beaker2·6H2O、0.54g FeCl3·6H2O, 0.45g of copper reagent (C)5H10NS2Na·3H2O) and 60mL of water are stirred until the mixture is dissolved, the obtained liquid is transferred into a stainless steel reaction kettle with a polytetrafluoroethylene lining for hydrothermal treatment at 240 ℃ for 12 hours, then the mixture is naturally cooled to room temperature, and the product is centrifugally washed and dried.
Example 3
240mg CoCl was added to the beaker2·6H2O、0.54g FeCl3·6H2O, 0.45g of copper reagent (C)5H10NS2Na·3H2O) and 60mL of water are stirred until the mixture is dissolved, the obtained liquid is transferred into a stainless steel reaction kettle with a polytetrafluoroethylene lining for hydrothermal treatment at 240 ℃ for 12 hours, then the mixture is naturally cooled to room temperature, and the product is centrifugally washed and dried.
Example 4
170mg CoCl was added to the beaker2·6H2O、0.54g FeCl3·6H2O, 0.45g of copper reagent (C)5H10NS2Na·3H2O) and 40mL of water are stirred until the mixture is dissolved, the obtained liquid is transferred into a stainless steel reaction kettle with a polytetrafluoroethylene lining for hydrothermal treatment at 240 ℃ for 12 hours, then the mixture is naturally cooled to room temperature, and the product is centrifugally washed and dried.
Example 5
170mg CoCl was added to the beaker2·6H2O、0.54g FeCl3·6H2O, 0.45g of copper reagent (C)5H10NS2Na·3H2O) and 80mL of water are stirred until the mixture is dissolved, the obtained liquid is transferred into a stainless steel reaction kettle with a polytetrafluoroethylene lining for hydrothermal treatment at 240 ℃ for 12 hours, then the mixture is naturally cooled to room temperature, and the product is centrifugally washed and dried.
Example 6
80 μ L of the homogeneous slurry from example 1 was applied dropwise to a thickness of 1X 1cm2On a Nickel Foam (NF) electrode, dried and used as an anode, 80. mu.L of the uniform slurry of example 1 was applied dropwise to a thickness of 1X 1cm2And (3) drying a foamed Nickel (NF) electrode to be used as a cathode, and measuring the full-hydrolytic performance of the electrode on a CHI760E electrochemical workstation at a sweep speed of 5mV/s by using the two electrode bodies as an electrolyte of 1.0mol/L KOH solution. The current density is 20mA/cm at a voltage of 1.73V2At a voltage of 1.9V, the current density was 100mA/cm2。

Claims (2)

1. Carbon-coated CoS2-FeS2Preparation method of heterojunction nanosheet, specifically CoCl2·6H2O、FeCl3·6H2O, copper reagent C5H10NS2Na·3H2O is used as a precursor, and carbon-coated CoS is synthesized by hydrothermal synthesis2-FeS2Heterojunction nanoplatelets, the carbon-coated CoS2-FeS2The heterojunction nanosheet can be used for efficiently and electrically catalyzing and decomposing water at room temperature; carbon coated CoS2-FeS2The heterojunction nanosheet is prepared by the following steps: adding 50-240 mg CoCl into a beaker2·6H2O，0.4～0.6g FeCl3·6H2O, 0.4-0.6 g of copper reagent C5H10NS2Na·3H2Stirring O and 40-80mL of water until the O and the water are dissolved, transferring the obtained liquid into a stainless steel reaction kettle with a polytetrafluoroethylene lining for hydrothermal treatment at the temperature of 220-260 ℃ for 6-24 h, then naturally cooling to room temperature, centrifugally washing the product, and drying to obtain carbon-coated CoS2-FeS2A heterojunction nanosheet.
2. The method of claim 1, wherein:
coating carbon with CoS2-FeS2Heterojunction nanosheet for room temperature electricityThe hydrogen is prepared by catalyzing and decomposing water, and the current density is 20mA/cm when the voltage is 1.73V2At a voltage of 1.9V, the current density was 100mA/cm2。
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CN113912132B (en) * 2021-09-26 2022-09-30 青岛科技大学 Defect heterojunction FeS 2 -Fe 7 S 8 Preparation method of (1)
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