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
molybdenum sulfide
cobalt molybdenum
electrode
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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
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    • 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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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)

1.一种碳布负载的多酸衍生钴钼硫化物的制备及电催化应用，其制备方法包括以下步骤：1. the preparation and electrocatalytic application of the polyacid-derived cobalt-molybdenum sulfide of a carbon cloth load, its preparation method may further comprise the steps: (1)将碳布裁剪成约1x1.5cm2的长方形方块，依次用丙酮、乙醇和去离子水对其进行超声处理30min，然后再将碳布浸泡在浓硝酸中，转移到水热反应釜中，100℃恒温1～2h，降至室温后，回收硝酸待下次重复使用，再用去离子水反复冲洗碳布，放入烘箱中80℃烘干过夜备用。(1) Cut the carbon cloth into a rectangular square of about 1 ×1.5cm , and then use acetone, ethanol and deionized water to ultrasonically treat it for 30min, then soak the carbon cloth in concentrated nitric acid and transfer it to the hydrothermal reactor 1 to 2 hours at a constant temperature of 100 °C for 1 to 2 hours, and after dropping to room temperature, recover the nitric acid for reuse next time, then rinse the carbon cloth with deionized water repeatedly, and put it in an oven to dry at 80 °C overnight for use. (2)将0.0345g的钴钼十二多酸，0.06g的硫脲，溶解于10ml的去离子水中，在磁力搅拌器上搅拌1～2个小时，然后置于水热反应釜中，同时放入一片步骤(1)中预处理过的碳布，将反应釜放入烘箱中在200℃条件下反应24个小时，自然冷却至室温。(2) 0.0345g of cobalt molybdenum dodecanoic acid and 0.06g of thiourea were dissolved in 10ml of deionized water, stirred on a magnetic stirrer for 1 to 2 hours, then placed in a hydrothermal reactor, while Put a piece of carbon cloth pretreated in step (1), put the reaction kettle into an oven to react for 24 hours at 200°C, and naturally cool to room temperature. (3)取出反应过后的碳布，用去离子水反复冲洗并置于60℃烘箱中烘干，即得到碳布负载的钴钼硫化物CoS2-MoS2，在碳布表面均匀覆盖。(3) Take out the reacted carbon cloth, repeatedly rinse with deionized water and place it in an oven at 60°C for drying to obtain the cobalt-molybdenum sulfide CoS 2 -MoS 2 supported by the carbon cloth, which is evenly covered on the surface of the carbon cloth. 2.权利要求1所述的一种碳布负载的多酸衍生钴钼硫化物的应用，其特征在于，一种碳布负载的多酸衍生钴钼硫化物应用于电催化分解水制氢领域。2. the application of the polyacid-derived cobalt-molybdenum sulfide of a kind of carbon cloth load of claim 1, is characterized in that, a kind of carbon cloth-supported polyacid-derived cobalt-molybdenum sulfide is applied to the field of electrocatalytic water splitting for hydrogen production . 3.根据权利要求1所述的应用，其特征在于，应用方法如下：以1.0摩尔每升氢氧化钾水溶液为电解液溶液，所述碳布负载的多酸衍生钴钼硫化物作为工作电极，以饱和甘汞电极为参比电极，碳棒电极作为对电极，在碱性电解质溶液中，当过电位为69mV时，电流密度为10mA cm-2，并在工作状态24个小时之后仍然保持稳定。3. application according to claim 1, is characterized in that, application method is as follows: take 1.0 moles of every liter of potassium hydroxide aqueous solution as electrolyte solution, the polyacid-derived cobalt molybdenum sulfide of described carbon cloth load is as working electrode, Taking saturated calomel electrode as reference electrode and carbon rod electrode as counter electrode, in alkaline electrolyte solution, when the overpotential is 69mV, the current density is 10mA cm -2 , and it remains stable after 24 hours of operation . 4.一种碳布负载的多酸衍生钴钼硫化物的制备及电催化应用，其特征在于区别于以往多数此类材料以往以简单钼酸钠和金属盐为主要原料的传统制备双金属硫化物技术线路中反应原料混合不均匀、彼此分离、反应不同步、产物形貌不一、容易团聚等技术瓶颈以及在水热过程中游离金属盐具有不同成核速率的缺点，导致此类电催化析氢材料析氢性能较差，析氢过电位较高。而本发明所制备的一种碳布负载的多酸衍生钴钼硫化物材料从简单的Keggin型多酸钴钼十二基本建筑单元出发，提供稳定的双金属源，将多酸与碳布复合以获得高效的电催化催化剂。采用通过一步水热法将多酸前驱体，硫脲为硫源与碳布基底复合在一起，避免材料的团聚并增强了电极在宽pH范围内的稳定性；在无附加粘结剂的情况下，不仅增强了电荷转移，而且避免了粘结剂的使用对活性中心的掩盖，从而赋予电极的高催化活性从而实现复合材料和导电材料的紧密结合，提高电子传输能力的同时提高催化剂的稳定性，制备出所需的复合电极材料。4. the preparation and electrocatalytic application of the polyacid-derived cobalt-molybdenum sulfide of a carbon cloth load, it is characterized in that being different from the traditional preparation bimetallic sulfide that used simple sodium molybdate and metal salt as main raw materials in the past for most of these materials in the past The technical bottlenecks such as uneven mixing of reaction raw materials, separation of each other, asynchronous reaction, different product morphologies, and easy agglomeration in the biotechnology circuit, as well as the disadvantages of different nucleation rates of free metal salts in the hydrothermal process, lead to this type of electrocatalysis. The hydrogen evolution material has poor hydrogen evolution performance and high hydrogen evolution overpotential. And a carbon cloth-supported polyacid-derived cobalt-molybdenum sulfide material prepared by the present invention starts from a simple Keggin-type polyacid-cobalt-molybdenum twelve basic building unit, provides a stable bimetal source, and composites the polyacid and carbon cloth to obtain efficient electrocatalytic catalysts. The polyacid precursor, thiourea as the sulfur source, and the carbon cloth substrate are compounded together by a one-step hydrothermal method, which avoids material agglomeration and enhances the stability of the electrode in a wide pH range; in the case of no additional binder It not only enhances the charge transfer, but also avoids the masking of the active center by the use of the binder, thus endows the electrode with high catalytic activity, thereby realizing the close combination of the composite material and the conductive material, improving the electron transport ability and improving the stability of the catalyst. properties to prepare the desired composite electrode materials.
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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 A carbon cloth-supported polyacid-derived three-metallic CoS2-MoS2-VS2 electrode material and its 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 framework composite material

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