CN113445073A - Preparation and electrocatalysis application of carbon cloth-loaded polyacid-derived cobalt molybdenum sulfide - Google Patents

Preparation and electrocatalysis application of carbon cloth-loaded polyacid-derived cobalt molybdenum sulfide Download PDF

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CN113445073A
CN113445073A CN202110652278.7A CN202110652278A CN113445073A CN 113445073 A CN113445073 A CN 113445073A CN 202110652278 A CN202110652278 A CN 202110652278A CN 113445073 A CN113445073 A CN 113445073A
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carbon cloth
polyacid
cobalt molybdenum
molybdenum sulfide
loaded
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CN113445073B (en
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庞海军
胡素敏
杨若茹
马慧媛
张春晶
于晓晶
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Harbin 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
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/054—Electrodes comprising electrocatalysts supported on a carrier
    • 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
    • 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
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
    • C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
    • C25B11/065—Carbon
    • 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
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
    • C25B11/077—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound the compound being a non-noble metal oxide
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention relates to preparation and application of carbon cloth loaded cobalt molybdenum sulfide in the field of electrocatalysis hydrogen evolution. The invention aims to solve the problems of rare raw material storage, high overpotential of hydrogen evolution reaction and high cost of the prior art for synthesizing the high-performance electrocatalyst. The patent designs and develops a carbon cloth loaded cobalt molybdenum sulfide material CoS2‑MoS2. The adopted method comprises the following steps: the Keggin type polyacid cobalt molybdenum dodecasulfide, thiourea and carbon cloth are used as raw materials, and a one-step hydrothermal synthesis method is adopted, so that the prepared polyacid derived cobalt molybdenum sulfide loaded on the carbon cloth can be suitable for electrocatalytic hydrogen evolution reaction in alkaline electrolyte and has low hydrogen evolution overpotential and high catalytic activity.

Description

Preparation and electrocatalysis application of carbon cloth-loaded polyacid-derived cobalt molybdenum sulfide
Technical Field
The invention relates to the field of electrocatalytic hydrogen evolution, in particular to preparation of carbon cloth-loaded polyacid-derived cobalt molybdenum sulfide
Background
With the urgent need of the development of society for energy demand and the gradual exhaustion of fossil fuels, the ecological-friendly and sustainable hydrogen energy has attracted great attention. The electrochemical hydrogen evolution reaction is a clean, simple and reproducible way which can effectively relieve the energy demand. At present, the most traditional and most different electrocatalysts are based on noble metal materials, the noble metal Pt has strong catalytic activity and is paid much attention in the field of electrocatalysis hydrogen evolution, but the application market of the electrocatalysis is limited by the rarity and the expensive price of the electrocatalysis. The polyacid has good redox ability and can reversibly accept and release one or more electrons. This makes it possible to act as a HER catalyst, since the electrochemical reaction takes place via electron transfer. The polyacid is a polyacid inorganic-organic hybrid compound which can be combined with an organic system through covalent bonds and can also replace/dope other elements to form a heteropoly acid nanocluster, so that the properties of the polyacid, such as electrochemistry and the like, can be adjusted to a certain extent. Furthermore, combining the polyacid with other substances by some means into a composite material is also a means to adjust the properties of the polyacid itself. Previous studies have shown that the electrocatalytic properties of bimetallic-based composites are superior. Therefore, the preparation of high activity, high stability and conductivity bimetallic-based composites from polyacids as precursors is a promising and meaningful work.
Disclosure of Invention
In order to overcome the defects of low specific surface area, high price, poor stability and poor conductivity of polyacid used as a raw material and the like of the existing electrocatalytic hydrogen evolution catalyst, the invention provides a method with simple preparation and low price, and the prepared carbon cloth-loaded polyacid-derived cobalt molybdenum sulfide used as an electrocatalytic hydrogen evolution catalyst material has the advantages of higher specific surface area, higher electrocatalytic performance, good stability and the like.
The purpose of the invention is realized as follows:
the preparation method of the carbon cloth-supported polyacid-derived cobalt molybdenum sulfide comprises the following steps:
(1) cutting the carbon cloth to about 1x1.5cm2Rectangular square block ofAnd carrying out ultrasonic treatment on the carbon cloth for 30min by using acetone, ethanol and deionized water, then soaking the carbon cloth in concentrated nitric acid, transferring the carbon cloth into a hydrothermal reaction kettle, keeping the temperature of 100 ℃ for 1-2 h, cooling to room temperature, recovering the nitric acid for next reuse, repeatedly washing the carbon cloth by using the deionized water, and drying in an oven at 80 ℃ overnight for later use.
(2) Dissolving 0.0345g of cobalt molybdenum dodecanedioic acid and 0.06g of thiourea in 10ml of deionized water, putting a piece of carbon cloth pretreated in the step (1), stirring on a magnetic stirrer for 1-2 hours, placing the mixed solution in a hydrothermal reaction kettle, reacting in an oven at 200 ℃ for 24 hours, and naturally cooling to room temperature.
(3) Taking out the carbon cloth after the reaction, repeatedly washing the carbon cloth by deionized water, and drying the carbon cloth in a 60 ℃ oven overnight to obtain the cobalt molybdenum sulfide material CoS loaded on the carbon cloth2-MoS2And the surface of the carbon cloth is uniformly covered.
The application of the carbon cloth-loaded polyacid-derived cobalt molybdenum sulfide is mainly in the aspect of electrocatalytic decomposition of water for hydrogen evolution.
The application method comprises the following steps: taking 1.0 mol/L potassium hydroxide aqueous solution as electrolyte solution, and the carbon cloth loaded cobalt molybdenum sulfide material CoS2-MoS2And (3) as a working electrode, taking a saturated calomel electrode as a reference electrode and taking a carbon rod electrode as a counter electrode, and thus constructing a three-electrode system. In an alkaline electrolyte solution, the current density was 10mA cm at an overpotential of 69mV-2And can be kept in a stable working state for 24 hours.
Compared with the prior art, the invention has the following characteristics:
the invention provides a stable bimetallic source by adopting Keggin polyacid as a precursor, which not only effectively breaks through the technical bottlenecks of uneven mixing of reaction raw materials, mutual separation, asynchronous reaction, inconsistent product appearance, easy agglomeration and the like in the traditional technical line for preparing the bimetallic sulfide by taking simple sodium molybdate and metal salt as main raw materials, but also effectively overcomes the defect that free metal salt has different nucleation rates in the hydrothermal process. And realizes the directional preparation of the high-dispersion bimetallic sulfideThe purpose of (1). And the two transition metal sulfides exert a synergistic effect between the two to promote the electrocatalytic performance. When the material is used as an electrocatalytic hydrogen evolution catalyst, the result shows that the material has good hydrogen evolution performance and lower overpotential, and the current density is 10mA cm in alkaline electrolyte solution when the overpotential is 69mV-2And can be kept in a stable working state for 24 hours. The polyacid precursor, thiourea, is used as a sulfur source to be compounded with the carbon cloth by a simple one-step hydrothermal method, so that the agglomeration of materials is avoided, and the stability of the electrode in a wide pH range is enhanced; under the condition of no additional binder, the charge transfer is enhanced, and the covering of the active center by the use of the binder is avoided, so that the electrode is endowed with high catalytic activity, the composite material and the conductive material are tightly combined, the stability of the catalyst is improved while the electron transfer capacity is improved, and the carbon cloth-loaded polyacid-derived cobalt molybdenum sulfide material is prepared.
Drawings
Fig. 1 is a hydrogen evolution polarization curve of a carbon cloth-supported polyacid-derived cobalt molybdenum sulfide in an alkaline electrolyte solution at different temperatures, prepared in example 1 of the present invention.
Fig. 2 is an XRD spectrum of a carbon cloth supported polyacid-derived cobalt molybdenum sulfide prepared in example 1 of the present invention.
FIG. 3 is an infrared spectrum of cobalt molybdenum dodecanoic acid prepared in example 1 of the present invention.
FIG. 4 is a plot of cyclic voltammograms of carbon cloth supported polyacid-derived cobalt molybdenum sulfide prepared in example 1 of the present invention at different sweep rates (10, 20, 30, 40, 50, 60, 70, 80, 90, 100mV/s) with a potential window of-0.70V to-0.50V.
Fig. 5 is a transmission electron microscope image of a carbon cloth-supported polyacid-derived cobalt molybdenum sulfide prepared in example 1 of the present invention.
Fig. 6 is scanning electron micrographs of carbon cloth-supported polyacid-derived cobalt molybdenum sulfide prepared in example 1 of the present invention at different sizes.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and examples.
Example 1, a carbon cloth supported polyacid-derived cobalt molybdenum sulfide, comprising the following preparation steps:
(1) cutting the carbon cloth to about 1x1.5cm2And carrying out ultrasonic treatment on the rectangular square blocks by using acetone, ethanol and deionized water for 30min, then soaking the carbon cloth in concentrated nitric acid, transferring the carbon cloth into a hydrothermal reaction kettle, keeping the temperature at 100 ℃ for 1-2 h, cooling to room temperature, recovering the nitric acid for next repeated use, repeatedly washing the carbon cloth by using the deionized water, and drying in an oven at 80 ℃ overnight for later use. Acetone is used to remove surface impurities and insoluble materials, ethanol is used to remove organic impurities, and water is used to remove residual acetone and ethanol.
(2) Dispersing 0.0345g of cobalt molybdenum dodecanedioic acid and 0.06g of thiourea in 10ml of deionized water, putting a piece of carbon cloth pretreated in the step (1), stirring on a magnetic stirrer for 1-2 hours, then putting the mixed solution in a hydrothermal reaction kettle, putting the reaction kettle in an oven to react for 24 hours at 200 ℃, and naturally cooling to room temperature.
(3) Taking out the carbon cloth after reaction, repeatedly washing the carbon cloth with deionized water, and drying the carbon cloth in a 60 ℃ oven overnight to obtain the cobalt molybdenum sulfide CoS loaded on the carbon cloth2-MoS2And the flower-like clusters formed by the nano particles are uniformly covered on the surface of the foamed nickel. The invention is further described with reference to the following drawings and examples:
fig. 1 shows the hydrogen evolution polarization curve of a carbon cloth supported polyacid-derived cobalt molybdenum sulfide in an alkaline electrolyte solution. It can be observed that when the current density is 10mA cm-2The overpotential of the electrode material was 69 mV.
As shown in FIG. 2, the XRD spectrum of a carbon cloth supported polyacid-derived cobalt molybdenum sulfide shows that different characteristic peaks appear in the target material, and the characteristic peaks are different from those of CoS2And MoS2Comparing the standard color comparison card to see MoS2And CoS2The diffraction peak of (a) appears on the PXRD pattern of the target material. In particular, it relates toDiffraction peaks appearing at 14.1 °, 32.6 °, 35.3 ° and 58.5 ° are assigned to MoS2(JCPDS, No.37-1492) crystal planes of (002), (101), (102) and (110). The positions of diffraction peaks appearing at 32.3 °, 36.2 ° and 54.9 ° at the same time are attributed to CoS2(JCPDS, No.65-3322) crystal planes (200), (210) and (311).
FIG. 3 shows an infrared test spectrum of a cobalt molybdenum dodecanedioic acid precursor, which can be seen at 963cm-1、874cm-1、 795cm-1、620cm-1The characteristic peak of cobalt molybdenum dodecanedioic acid appears, which is consistent with the literature.
FIG. 4 is a cyclic voltammogram graph of a carbon cloth supported polyacid-derived cobalt molybdenum sulfide with a potential window of-0.70V to-0.50V at different sweep rates (10, 20, 30, 40, 50, 60, 70, 80, 90, 100 mV/s).
FIG. 5 shows the Tafel slope of a carbon cloth supported polyacid-derived cobalt molybdenum sulfide at various temperatures, the Tafel slope of the electrode material in 1.0M KOH electrolyte is about 137mV dec-1。
FIG. 6 is a scanning electron micrograph of a carbon cloth-supported polyacid-derived cobalt molybdenum sulfide under different sizes, which shows that the surface of the carbon cloth is covered with uniform MoS2And CoS2The nanosheet structure of (a).

Claims (4)

1. A preparation method and electrocatalysis application of carbon cloth-loaded polyacid derived cobalt molybdenum sulfide comprises the following steps:
(1) cutting the carbon cloth to about 1X1.5cm2And carrying out ultrasonic treatment on the rectangular square blocks by using acetone, ethanol and deionized water in sequence for 30min, then soaking the carbon cloth in concentrated nitric acid, transferring the carbon cloth into a hydrothermal reaction kettle, keeping the temperature of 100 ℃ for 1-2 h, cooling to room temperature, recovering the nitric acid for next repeated use, repeatedly washing the carbon cloth by using the deionized water, and drying in an oven at 80 ℃ overnight for later use.
(2) Dissolving 0.0345g of cobalt molybdenum dodecanedioic acid and 0.06g of thiourea in 10ml of deionized water, stirring for 1-2 hours on a magnetic stirrer, then placing the mixture in a hydrothermal reaction kettle, simultaneously placing a piece of carbon cloth pretreated in the step (1), placing the reaction kettle in an oven to react for 24 hours at 200 ℃, and naturally cooling to room temperature.
(3) Taking out the carbon cloth after reaction, repeatedly washing the carbon cloth with deionized water, and drying the carbon cloth in a drying oven at 60 ℃ to obtain the cobalt molybdenum sulfide CoS loaded on the carbon cloth2-MoS2And the surface of the carbon cloth is uniformly covered.
2. The use of the carbon cloth supported polyacid-derived cobalt molybdenum sulfide of claim 1, wherein a carbon cloth supported polyacid-derived cobalt molybdenum sulfide is used in the field of electrocatalytic decomposition of water to produce hydrogen.
3. The application according to claim 1, characterized in that the application method is as follows: taking 1.0 mol/L potassium hydroxide aqueous solution as electrolyte solution, the carbon cloth-loaded polyacid-derived cobalt molybdenum sulfide as a working electrode, a saturated calomel electrode as a reference electrode, a carbon rod electrode as a counter electrode, and in alkaline electrolyte solution, when the overpotential is 69mV, the current density is 10mA cm-2And remains stable after 24 hours of operation.
4. The preparation and electrocatalysis application of the carbon cloth-loaded polyacid-derived cobalt molybdenum sulfide are characterized by being different from technical bottlenecks such as uneven mixing of reaction raw materials, mutual separation, asynchronous reaction, inconsistent product morphology, easy agglomeration and the like in the traditional technical line for preparing the bimetallic sulfide by using simple sodium molybdate and metal salt as main raw materials in the past for most of the materials, and the defects that free metal salt has different nucleation rates in the hydrothermal process, so that the electrocatalysis hydrogen evolution material has poor hydrogen evolution performance and high hydrogen evolution overpotential. The carbon cloth-loaded polyacid-derived cobalt molybdenum sulfide material provided by the invention starts from a simple Keggin type polyacid cobalt molybdenum twelve basic building unit, provides a stable bimetallic source, and compounds polyacid and carbon cloth to obtain a high-efficiency electrocatalytic catalyst. A polyacid precursor and thiourea are compounded with the carbon cloth substrate by a one-step hydrothermal method, so that the agglomeration of materials is avoided and the stability of the electrode in a wide pH range is enhanced; under the condition of no additional binder, the charge transfer is enhanced, and the covering of the active center by the use of the binder is avoided, so that the electrode is endowed with high catalytic activity, the composite material and the conductive material are tightly combined, the electron transfer capability is improved, the stability of the catalyst is improved, and the required composite electrode material is prepared.
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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN113846350A (en) * 2021-10-09 2021-12-28 黑龙江大学 Transition metal phosphide composite material for acidic electrolyzed water oxygen evolution and preparation method thereof
CN114774973A (en) * 2022-04-22 2022-07-22 河北师范大学 Nanometer flower-like cobalt molybdenum sulfide supported catalyst and preparation method and application thereof
CN114959777A (en) * 2022-03-09 2022-08-30 哈尔滨理工大学 Carbon cloth-loaded polyacid-derived trimetal CoS 2 -MoS 2 -VS 2 Electrode material and electrocatalytic application
CN116926957A (en) * 2023-07-17 2023-10-24 广西师范大学 Preparation method and application of dysprosium-doped nickel-metal organic frame composite material

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113846350A (en) * 2021-10-09 2021-12-28 黑龙江大学 Transition metal phosphide composite material for acidic electrolyzed water oxygen evolution and preparation method thereof
CN114959777A (en) * 2022-03-09 2022-08-30 哈尔滨理工大学 Carbon cloth-loaded polyacid-derived trimetal CoS 2 -MoS 2 -VS 2 Electrode material and electrocatalytic application
CN114959777B (en) * 2022-03-09 2024-02-02 哈尔滨理工大学 Polyacid-derived trimetallic CoS loaded by carbon cloth 2 -MoS 2 -VS 2 Electrode material and electrocatalytic application
CN114774973A (en) * 2022-04-22 2022-07-22 河北师范大学 Nanometer flower-like cobalt molybdenum sulfide supported catalyst and preparation method and application thereof
CN114774973B (en) * 2022-04-22 2024-03-08 河北师范大学 Nanometer flower-like cobalt-molybdenum sulfide supported catalyst and preparation method and application thereof
CN116926957A (en) * 2023-07-17 2023-10-24 广西师范大学 Preparation method and application of dysprosium-doped nickel-metal organic frame composite material

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