CN112708904A - Preparation method and application of carbon fiber loaded nano cobalt-molybdenum alloy catalyst - Google Patents
Preparation method and application of carbon fiber loaded nano cobalt-molybdenum alloy catalyst Download PDFInfo
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Abstract
The inventionThe invention discloses a preparation method and application of a carbon fiber loaded nano cobalt-molybdenum alloy catalyst. The preparation method is simple and controllable, has short preparation period, low production cost and good repeatability, and is very likely to realize large-scale production. The obtained cobalt-molybdenum nano alloy material can be used for hydrogen production reaction by electrolysis in an alkaline electrolytic cell, and the optimal overpotential of only 80mV can achieve the current density of 10mA cm‑2. Can carry out the hydrogen production reaction of the high-efficient catalytic electrolysis water in a super-long time, can greatly improve the energy conversion efficiency of converting electric energy into chemical energy, and has potential industrial application.
Description
Technical Field
The invention belongs to the field of inorganic functional materials, relates to a preparation technology of an electrolytic water catalytic material, and particularly relates to a preparation method of a carbon fiber loaded nano cobalt-molybdenum alloy material and application of the carbon fiber loaded nano cobalt-molybdenum alloy material in the aspect of efficient electrocatalytic splitting of water to produce hydrogen.
Background
The continuous increase in global energy demand, the accelerated consumption of traditional coal, petroleum and fossil fuels, and the consequent environmental pollution problems, has raised a strong interest in developing alternative energy sources. Particularly, the aggravation of geopolitical anxiety and climate threats arouses the development of people towards the direction of having a renewable, stable and environment-friendly benign energy source. Because of the advantages of zero emission of combustion, high energy density and the like, hydrogen energy is considered as one of ideal green energy sources capable of replacing the traditional fossil fuel. Hydrogen production by electrolysis of water is an efficient method for producing hydrogen fuel, but requires high performance water electrolysis catalysts to accelerate the Hydrogen Evolution Reaction (HER) and reduce power consumption. Currently, platinum-based materials are considered the most efficient electrocatalysts, but their high cost and non-renewable nature limit their widespread use. Therefore, there is an urgent need to develop a low-cost, efficient and stable platinum-based alternative electrocatalyst.
In principle, if a catalyst has excellent hydrogen evolution catalytic activity, it may come from one or more of the following four aspects: (1) a large number of active centers are present in the catalyst; (2) the reaction intermediate has proper binding capacity with an active site, so that the catalyst has good intrinsic activity; (3) between the catalyst surface and the electrolyte, the reactant (H)+/H2O) and product (H)2/OH-) A rapid mass transfer reaction occurs; (4) the electrode made of the catalyst has excellent conductivity. Over the past few decades, many transition metal-based catalysts have been considered as desirable alternatives to noble metal hydrogen evolution catalysts, including transition metal-based alloys, compounds (e.g., oxides, hydroxides, sulfides, carbides, selenides, and phosphides). Among these materials, a metal alloy having excellent conductivity attracts attention of many researchers, and is considered as an ideal candidate material for a noble metal catalyst. However, the alloy has poor durability in catalytic hydrogen evolution reaction, and particularly, in severe environments such as strongly alkaline electrolyte and high potential. Therefore, there is still a great challenge in developing a basic hydrogen-generating electrocatalyst with low cost, simple preparation process and high efficiency.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a preparation method and application of a carbon fiber-based nano cobalt-molybdenum alloy catalyst, a target product can be obtained in one step by pulse electrodeposition, the operation is simple, the production cost is low, and the large-scale production is easy to realize.
The invention is realized by adopting the following technical scheme:
a preparation method of a carbon fiber loaded nano cobalt-molybdenum alloy catalyst comprises the following steps: performing one-step electrodeposition in a standard three-electrode system by adopting a conventional pulse voltammetry method by taking a carbon-based conductive material as a working electrode, a carbon rod as a counter electrode and a saturated silver chloride electrode (Ag/AgCl) as a reference electrode to obtain a carbon fiber loaded nano cobalt-molybdenum alloy hydrogen evolution electrode; wherein the electrolyte comprises a cobalt source and a molybdenum source.
Further, the carbon-based conductive material is carbon cloth, carbon fiber paper or carbon felt.
Further, the cobalt source is a cobalt salt soluble in water, and the molybdenum source is a molybdenum salt soluble in water.
Further, the cobalt source is cobalt sulfate, cobalt chloride, cobalt acetate or cobalt nitrate, and the molybdenum source is sodium molybdate, ammonium molybdate or potassium molybdate.
Furthermore, the concentration of cobalt ions is 0.1-0.5 mol/L, the concentration of molybdenum ions is 0.03-0.07 mol/L, and the pH value of the electrolyte is 5-6.
Furthermore, the pulse electrodeposition temperature is 20-60 ℃, the pulse electrodeposition time is 300-1800 s, and the electrodeposition voltage interval is-1.2-1.8V.
Further, the carbon-based conductive material is subjected to high-temperature heat treatment in a muffle furnace to improve the hydrophilicity of the carbon fiber paper to electroplating electrolyte, and the pretreatment method of the carbon fiber paper comprises the following steps: and (3) putting the carbon fiber paper into a muffle furnace for heat treatment at 600 ℃ for 3 hours. The pretreatment method of the carbon cloth and the carbon felt comprises the following steps: and respectively ultrasonically cleaning the carbon cloth or the carbon felt in acetone, ethanol and deionized water for 30 min.
Further, the pH of the electrolyte was adjusted using sodium hydroxide and sodium citrate.
The optimal preparation method of the carbon fiber loaded nano cobalt-molybdenum alloy catalyst comprises the following steps:
preparing an electroplating electrolyte: weighing analytically pure cobalt sulfate, sodium molybdate, sodium hydroxide and sodium citrate solids to prepare a mixed solution, wherein the mixed solution comprises 0.3mol/L cobalt sulfate, 0.05mol/L sodium molybdate, 0.03mol/L sodium hydroxide and 0.3mol/L sodium citrate;
preparing by pulse electrodeposition: using an electrochemical workstation of a three-electrode system, taking the carbon fiber paper after heat treatment as a working electrode, a carbon rod as a counter electrode, and a saturated silver chloride electrode (Ag/AgCl) as a reference electrode, and performing electrodeposition in a standard three-electrode system by adopting a conventional pulse voltammetry; the electroplating parameters of the pulse electrodeposition process are as follows: the temperature is 25 ℃, the initial potential is-1.2V, the end potential is-1.6V, the potential increment is 0.02V, and the electrodeposition time is 900 s.
Carbon fiber loaded with nano cobalt prepared under optimal conditionsThe application of the molybdenum alloy cathode hydrogen evolution catalyst in the cathode hydrogen evolution reaction of electrolyzed water is as follows: the reaction temperature is 25 ℃, the electrolyte is 1M KOH (pH = 13.6), and the potential of 80mV is only needed for hydrogen evolution by electrocatalytic water splitting, so that the current density of the formed alkaline electrolytic cell can reach 10mA cm-2The Tafel slope is 45.5mV dec-1And the performance is stable; electrocatalytic stability test conditions: the reaction temperature is 25 ℃, and the current density is 10mA cm-2And may last 79 hours.
The invention has the following advantages:
1. the electrodeposition has the advantages of simple operation, short preparation period, low production cost, good repeatability and easy realization of large scale.
2. The carbon substrate conductive material has the characteristics of good chemical stability, corrosion resistance and excellent conductive capability. The carbon fiber loaded nano cobalt-molybdenum alloy hydrogen evolution electrode can be directly used as a working electrode for electrolyzing water to produce hydrogen, and binders such as perfluorosulfonic acid-polytetrafluoroethylene copolymer (Nafion) and the like are avoided, so that the mechanical stability and the electronic transmission speed of the hydrogen evolution catalyst are improved, and the electric energy loss and the manufacturing cost of the hydrogen evolution electrode are reduced.
3. Compared with the traditional direct current deposition, the cobalt-molybdenum nano alloy prepared by adopting the pulse electrodeposition method can improve the corrosion resistance and the adhesive force of the plating layer, so that the plating layer is more detailed and uniform, and the stability of the catalytic activity of the cobalt-molybdenum alloy catalyst is enhanced.
4. The carbon fiber loaded nano cobalt-molybdenum alloy material has excellent hydrogen evolution catalytic activity under alkaline conditions.
The invention prepares the hydrogen evolution electrode by pulse electrodeposition, obtains the carbon fiber loaded hydrogen evolution catalyst without a binder, has high catalytic activity and large specific surface area, can keep the microstructure of the catalyst and good catalytic activity for a long time under an alkaline condition, and has potential industrial application value in the aspect of electrocatalytic hydrogen production.
The invention has reasonable design, and the method is a simple and convenient preparation method of the non-noble metal alloy, and simultaneously expands the variety of the non-noble metal alloy as the cathode hydrogen evolution catalyst.
Drawings
Fig. 1 shows an XRD spectrum of a carbon fiber-supported nano cobalt molybdenum alloy catalyst sample obtained in example 1.
Fig. 2A shows an SEM photograph (2 μm) of the heat-treated carbon fiber paper obtained in example 1.
Fig. 2B shows an SEM photograph (5 μm) of the heat-treated carbon fiber paper obtained in example 1.
Fig. 2C shows an SEM photograph (20 μm) of the heat-treated carbon fiber paper obtained in example 1.
Fig. 3A shows an SEM photograph (2 μm) of a carbon fiber-supported nano cobalt molybdenum alloy catalyst sample obtained in example 1.
Fig. 3B shows an SEM photograph (5 μm) of a carbon fiber-supported nano cobalt molybdenum alloy catalyst sample obtained in example 1.
Fig. 3C shows an SEM photograph (10 μm) of a carbon fiber-supported nano cobalt molybdenum alloy catalyst sample obtained in example 1.
Fig. 4 shows an EDX mapping chart of a carbon fiber-supported nano cobalt molybdenum alloy catalyst sample obtained in example 1.
Fig. 5 shows an EDX energy spectrum of a carbon fiber-supported nano cobalt molybdenum alloy catalyst sample obtained in example 1.
Fig. 6a shows an XPS spectrum (Co) of a carbon fiber supported nano cobalt molybdenum alloy catalyst sample obtained in example 1.
Fig. 6b shows an XPS spectrum (Mo) of the carbon fiber supported nano cobalt molybdenum alloy catalyst sample obtained in example 1.
Fig. 7 shows polarization curves of Hydrogen Evolution (HER) by water splitting in alkaline (1M KOH) electrolyte of the carbon fiber supported nano cobalt molybdenum alloy catalyst sample obtained in example 1.
Fig. 8 shows a multi-step current stability test curve of the carbon fiber supported nano cobalt molybdenum alloy catalyst sample obtained in example 1 in an alkaline (1M KOH) electrolyte.
Fig. 9 shows a voltage-time stability test curve of the carbon fiber supported nano cobalt molybdenum alloy catalyst sample obtained in example 1 in an alkaline (1M KOH) electrolyte.
Detailed Description
The present invention will be further described with reference to the following examples, but the scope of the present invention is not limited to the following examples.
According to the embodiment of the invention, carbon fiber paper, carbon cloth and carbon felt are used as carbon substrate materials, sodium hydroxide, sodium citrate, a cobalt source and a molybdenum source are used as raw materials, and a multiphase pulse electrodeposition technology is adopted to obtain the target material.
Example 1
A preparation method of a carbon fiber loaded nano cobalt-molybdenum alloy catalyst comprises the following steps:
after the carbon fiber paper (1 cm multiplied by 3 cm) is subjected to heat treatment in a muffle furnace at 600 ℃ for 3 hours, the carbon fiber paper is used as a working electrode, a carbon rod is used as a counter electrode, a saturated silver chloride electrode (Ag/AgCl) is used as a reference electrode, and electrodeposition is carried out in a standard three-electrode system by adopting a conventional pulse voltammetry method. The components of the electrolyte are 0.3mol/L cobalt sulfate, 0.05mol/L sodium molybdate, 0.03mol/L sodium hydroxide and 0.3mol/L sodium citrate, the pH of the electrolyte (plating solution) is 5.8, and the temperature is 25 ℃. The electroplating parameters of the pulse electrodeposition process are as follows: the initial potential is-1.2V, the end potential is-1.6V, the potential increment is 0.02V, and the electrodeposition time is 900 s. Then, the sample was taken out, washed with distilled water, and dried.
The necessary structural and property studies were performed on the materials prepared by the above-described methods. FIG. 1 is an X-ray diffraction (XRD) pattern of CoMo/CFP, indicating that a CoMo alloy was produced on carbon fibers. Fig. 2A, 2B and 2C are SEM photographs of the resulting heat-treated carbon fiber paper base material, and it can be seen that the carbon fibers still maintain the fibrous morphology. Fig. 3A, 3B and 3C are SEM photographs of the obtained carbon fiber-supported nano cobalt molybdenum alloy material, and it can be seen that CoMo nanoparticles are uniformly supported on the carbon fiber paper. Fig. 4 is an EDX mapping diagram of the obtained carbon fiber-supported nano cobalt molybdenum alloy material, and it can be seen that the material composition is Co, Mo, C, O, and the four elements are uniformly distributed in the material. FIG. 5 is an EDX spectrum of the obtained carbon fiber-supported nano cobalt-molybdenum alloy material, and it can be seen that the content of Co in the material is up to 83.3 Wt%. Fig. 6a and 6b are X-ray photoelectron spectroscopy (XPS) spectra of the obtained catalyst, and zero-valent Co and Mo can prove that the obtained catalyst is a CoMo alloy material.
The catalyst material prepared by the method is subjected to electrocatalytic water splitting hydrogen production (HER) property test in a standard three-electrode electrolytic cell; the working electrode in the electrolytic cell is the carbon fiber loaded nano cobalt molybdenum alloy catalyst (1 cm multiplied by 1 cm) prepared by the invention, the reference electrode is a mercury/mercury oxide electrode, the counter electrode is a carbon rod, and the electrolyte is 1M KOH. It should be noted that all potentials obtained by using the mercury/mercury oxide electrode as a reference electrode in the electrocatalytic test are converted into reversible hydrogen electrode potentials in the property diagram.
FIG. 7 is the polarization curve of the product of the present invention in 1M KOH solution of CoMo/CFP at a current density of 10mA cm-2The overpotential is only 80 mV.
FIG. 8 is a multi-step current curve of the catalyst, with current density from 10mA cm-2Increased to 120mA cm-2Increase by 10mA cm per 1000s-2. At a current density of 10mA cm-2The voltage required for the CoMo/CFP was 80mV and was kept constant for 1000 s. At a current density of 120mA cm-2Similar stability results were also obtained, indicating that CoMo/CFP can still maintain electrochemical stability at high current densities.
FIG. 9 shows the catalyst at a current density of 10mA cm-2The stability tests below all last for more than 79 hours.
Example 2
The same as example 1, except that the carbon fiber paper after pretreatment is changed into the carbon fiber paper without any pretreatment, other synthesis conditions are not changed, the CoMo/CFP catalyst can be obtained, and the current density reaches 10mA cm-2The overpotential is required to be 156 mV.
Example 3
The same as example 1, except that the pretreated carbon fiber paper was changed into pretreated carbon cloth and pretreated carbon felt, other synthesis conditions were not changed, and a CoMo alloy catalyst was obtained with a current density of 10mA cm-2The overpotential needs to be 96mV and 124mV respectively. The pretreatment method of the carbon cloth comprises the following steps:ultrasonically cleaning the carbon cloth in acetone, ethanol and deionized water for 30min respectively; the pretreatment method of the carbon felt comprises the following steps: and ultrasonically cleaning the carbon felt in acetone, ethanol and deionized water for 30min respectively.
Example 4
The same as example 1, except that the electrodeposition time is changed into 300s, 600s, 1200s and 1800s, other synthesis conditions are not changed, the CoMo/CFP catalyst can be obtained, and the current density reaches 10mA cm-2Overpotentials of 170mV, 145mV, 143mV and 128mV, respectively, are required.
Example 5
As in example 1, a CoMo/CFP catalyst can be obtained with a current density of 10mA cm, except that the electrodeposition voltage interval is changed to-1.2 to-1.4V, -1.2 to-1.5V, -1.2 to-1.7V, -1.2 to-1.8V, and other synthesis conditions are not changed-2Overpotentials of 163mV, 156mV, 103mV and 111mV, respectively, are required.
Example 6
The same procedure as in example 1 was repeated except that cobalt sulfate was replaced with cobalt chloride, cobalt acetate and cobalt nitrate, respectively, and the current density reached 10mA cm-2Other synthesis conditions are not changed, the CoMo/CFP catalyst can still be obtained, and overpotentials of 113mV, 126mV and 93mV are needed respectively.
Example 7
As in example 1, except that sodium molybdate was replaced by ammonium molybdate and potassium molybdate, and other synthesis conditions were not changed, a CoMo/CFP catalyst was obtained with a current density of 10mA cm-2The overpotential needs to be 114mV and 103mV, respectively.
The preparation method is simple and controllable, has short preparation period, low production cost and good repeatability, and is very likely to realize large-scale production. The obtained cobalt-molybdenum nano alloy material can be used for hydrogen production reaction by electrolysis in an alkaline electrolytic cell, and the optimal overpotential of only 80mV can achieve the current density of 10mA cm-2. Can carry out the hydrogen production reaction of the high-efficiency catalytic electrolysis water in an overlong time, and can greatly improve the energy source of converting electric energy into chemical energyConversion efficiency, with potential industrial applications.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the detailed description is made with reference to the embodiments of the present invention, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which shall be covered by the claims of the present invention.
Claims (10)
1. A preparation method of a carbon fiber loaded nano cobalt-molybdenum alloy catalyst is characterized by comprising the following steps: performing one-step electrodeposition in a standard three-electrode system by adopting a conventional pulse voltammetry method to obtain a carbon fiber loaded nano cobalt-molybdenum alloy hydrogen evolution electrode; wherein the electrolyte comprises a cobalt source and a molybdenum source.
2. The preparation method of the carbon fiber supported nanometer cobalt molybdenum alloy catalyst according to claim 1, characterized in that: the carbon-based conductive material is carbon cloth, carbon fiber paper or carbon felt.
3. The preparation method of the carbon fiber supported nanometer cobalt molybdenum alloy catalyst according to claim 1 or 2, characterized in that: the cobalt source is a cobalt salt soluble in water, and the molybdenum source is a molybdenum salt soluble in water.
4. The preparation method of the carbon fiber supported nanometer cobalt molybdenum alloy catalyst according to claim 3, characterized in that: the cobalt source is cobalt sulfate, cobalt chloride, cobalt acetate or cobalt nitrate, and the molybdenum source is sodium molybdate, ammonium molybdate or potassium molybdate.
5. The preparation method of the carbon fiber-supported nano cobalt molybdenum alloy catalyst according to claim 4, wherein the preparation method comprises the following steps: the concentration of cobalt ions is 0.1-0.5 mol/L, the concentration of molybdenum ions is 0.03-0.07 mol/L, and the pH value of the electrolyte is 5-6.
6. The preparation method of the carbon fiber-supported nano cobalt molybdenum alloy catalyst according to claim 5, wherein the preparation method comprises the following steps: the pulse electrodeposition temperature is 20-60 ℃, the pulse electrodeposition time is 300-1800 s, and the electrodeposition voltage interval is-1.2 to-1.8V.
7. The preparation method of the carbon fiber supported nanometer cobalt molybdenum alloy catalyst according to claim 2, characterized in that: the pretreatment method of the carbon fiber paper comprises the following steps: putting the carbon fiber paper into a muffle furnace for heat treatment at 600 ℃ for 3 hours; the pretreatment method of the carbon cloth and the carbon felt comprises the following steps: and respectively ultrasonically cleaning the carbon cloth or the carbon felt in acetone, ethanol and deionized water for 30 min.
8. The preparation method of the carbon fiber supported nanometer cobalt molybdenum alloy catalyst according to claim 7, characterized in that: the pH of the electrolyte was adjusted with sodium hydroxide and sodium citrate.
9. The preparation method of the carbon fiber supported nanometer cobalt molybdenum alloy catalyst according to claim 8, characterized in that: preparing an electroplating electrolyte: weighing analytically pure cobalt sulfate, sodium molybdate, sodium hydroxide and sodium citrate solids to prepare a mixed solution, wherein the mixed solution comprises 0.3mol/L cobalt sulfate, 0.05mol/L sodium molybdate, 0.03mol/L sodium hydroxide and 0.3mol/L sodium citrate;
preparing by pulse electrodeposition: using an electrochemical workstation of a three-electrode system, taking the carbon fiber paper after heat treatment as a working electrode, a carbon rod as a counter electrode and a saturated silver chloride electrode as a reference electrode, and performing electrodeposition in a standard three-electrode system by adopting a conventional pulse voltammetry; the electroplating parameters of the pulse electrodeposition process are as follows: the temperature is 25 ℃, the initial potential is-1.2V, the end potential is-1.6V, the potential increment is 0.02V, and the electrodeposition time is 900 s.
10. The application of the carbon fiber loaded nano cobalt molybdenum alloy cathode hydrogen evolution catalyst prepared according to any one of claims 1 to 9 in the cathode hydrogen evolution reaction of electrolyzed water.
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CN115011994A (en) * | 2022-04-17 | 2022-09-06 | 中北大学 | Ag 2 MoO 4 Preparation method and application of/CoMo-LDH electrolyzed water oxygen evolution catalyst |
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YU LIN: "Ultralow ruthenium loading Cobalt-molybdenum binary alloy as highly efficient and super-stable electrocatalyst for water splitting", 《APPLIED SURFACE SCIENCE》 * |
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CN115011994A (en) * | 2022-04-17 | 2022-09-06 | 中北大学 | Ag 2 MoO 4 Preparation method and application of/CoMo-LDH electrolyzed water oxygen evolution catalyst |
CN115011994B (en) * | 2022-04-17 | 2023-05-23 | 中北大学 | Ag (silver) alloy 2 MoO 4 Preparation method and application of CoMo-LDH electrolytic water oxygen evolution catalyst |
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