CN114540833A - CeO (CeO)2@Co3S4Heterogeneous multi-level nano-structure catalytic material and preparation method and application thereof - Google Patents
CeO (CeO)2@Co3S4Heterogeneous multi-level nano-structure catalytic material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses CeO2@Co3S4A heterogeneous multi-level nano-structure catalytic material, a preparation method and application thereof belong to the technical field of inorganic nano-catalytic material preparation. The invention is realized by adding Ce (NH)4)2(NO3)6，CH3CSNH2And CO (NH)2)2Dissolving in dilute nitric acid (pH value is 2-6) to form a solution, then placing in foam cobalt and transferring to a hydrothermal reaction kettle together, and reacting for 6-10h at the temperature of 160-; naturally cooling after the reaction is finished, taking out the foamed cobalt sample, and then washing and drying to obtain the foamed cobalt loadCeO (B) of2@Co3S4Heterogeneous multi-level nano-structure catalytic material. The material preparation method provided by the invention is simple to operate, is suitable for large-scale production, and the prepared product has the characteristics of stability and high catalytic activity of electrolyzed water, can be widely applied to electrochemical energy storage and conversion technology, and has a high application value.
Description
Technical Field
The invention belongs to the technical field of preparation of inorganic nano catalytic materials, and relates to CeO2@Co3S4A preparation method of heterogeneous multi-layer nano-structure catalytic material, in particular to a one-step method for synthesizing CeO2@Co3S4A preparation method of a heterogeneous multilevel nano-structure electrolytic water catalyst.
Background
Environmental issues arising from increasing fossil fuel consumption are receiving increasing attention and it is therefore necessary to establish a clean and sustainable energy system on a global scale. The hydrogen production by water electrolysis is a promising method, and the obtained hydrogen has high purity and can be directly used as a fuel cell. However, the relatively high cost of water electrolysis for preparing hydrogen still limits the large-scale commercial application of the catalyst, and particularly in an alkaline electrolysis water environment, the catalyst used in the current commercial water electrolysis hydrogen production catalyst faces the problems of high cost, low stability and the like. Therefore, a catalyst for producing hydrogen by electrolyzing water with high efficiency and low cost is developed.
In recent years, cobalt sulfide catalysts have been receiving increasing attention in the field of electrolysis of water because of their excellent electrical characteristics. How to further improve the catalytic performance of the cobalt sulfide electrocatalyst is a research hotspot. Researches find that the catalytic property of the cobalt sulfide catalyst material can be effectively improved by adding other components into the cobalt sulfide catalyst material based on the heterogeneous effect and the synergistic effect, and meanwhile, the multi-layer nano structure can greatly improve the exposure of active sites of the catalyst, so that the catalytic performance of the catalyst is further improved. Creped copper supported CoS prepared by Zhouzen et al using hydrothermal methodxThe water catalyst was electrolyzed, but the cobalt sulfide was not effectively doped. Von et al also produced Ni with heterostructures using a two-step hydrothermal process3Se2/Co9S, however, such methods, while producing heterostructures, also do not effectively dope cobalt sulfide.
Cerium (Ce) is a rare earth element with different valence states3+And Ce4+) Can form synergistic effect with transition metal to promote the catalytic performance of transition metal-based catalysis. Wear et al prepared a Co3O4/CeO2Nano hybrid catalyst for greatly increasing Co3O4Oxygen evolution catalysis performance in alkaline environments. Ledu et al electro-deposition of CeO2Doping to Co4In N, the catalytic performance of the electrolytic water is greatly improved (adv. Funct. Mater.2020, 1910596). However, CeO was prepared by hydrothermal method2The research of doping into cobalt sulfide is not reported.
Disclosure of Invention
In view of the above, the present invention is directed to providing a CeO solution for solving the problems of the prior art2@Co3S4Heterogeneous multi-level nano-structure catalytic material and preparation method and application thereof.
In order to achieve the purpose, the technical scheme of the invention is as follows:
CeO (CeO)2@Co3S4The preparation method of the heterogeneous multi-layer nano-structure catalytic material specifically comprises the following steps:
(1) adding Ce (NH)4)2(NO3)6，CH3CSNH2And CO (NH)2)2Dissolving in dilute nitric acid to form a solution, then adding foamed cobalt into the solution, and stirring to obtain a reaction system;
(2) transferring the reaction system to a hydrothermal reaction kettle for reaction, naturally cooling after the reaction is finished, taking out the foamed cobalt, and washing and drying to obtain the foamed cobalt loaded CeO2@Co3S4Heterogeneous multi-level nano-structure catalytic material.
Preferably, in the step (1), Ce (NH)4)2(NO3)6，CH3CSNH2And CO (NH)2)2The ratio of the amounts of substances of (a) to (b) is 1: 5: 10, and said Ce (NH)4)2(NO3)6，CH3CSNH2And CO (NH)2)2The total concentration is 0.15-0.17 mol/L.
And the pH value of the dilute nitric acid is 2-6.
Further preferably, C ise(NH4)2(NO3)6，CH3CSNH2And CO (NH)2)2The total concentration is 0.16 mol/L; and the pH value of the dilute nitric acid is 4 so as to ensure the regularity of the heterogeneous multilayer nano structure.
Preferably, the reaction temperature in the step (2) is 160-200 ℃, and the reaction time is 6-10 h.
Further, the temperature of the hydrothermal reaction is 180 ℃, and the reaction time is 8 h.
In addition, the invention also claims CeO prepared by the method2@Co3S4A heterogeneous multi-layer nano-structured catalytic material comprises CeO with nano-rod-shaped structures with vertical three-dimensional growth and close arrangement on the surface2@Co3S4And the said CeO2@Co3S4Growing on the surface of the foamed cobalt.
And, it is yet another object of the present invention to provide CeO2@Co3S4Application of heterogeneous multi-level nano-structure catalytic material in the field of water electrolysis.
It should be noted that doping cerium oxide in cobalt sulfide can improve the electronic structure of cobalt sulfide, and enhance the electrocatalytic performance thereof through a synergistic effect, specifically, CeO2Can be added with Co3S4The heterojunction is formed, the electronic structure of cobalt sulfide is improved, active sites are fully exposed, and the layered structure and the high-conductivity foam cobalt carrier are benefited, so that the electrocatalytic performance of the electrocatalyst is obviously improved.
According to the technical scheme, compared with the prior art, the CeO is provided2@Co3S4The heterogeneous multi-level nano-structure catalytic material, the preparation method and the application thereof have the following excellent effects:
in the method provided by the invention, the foam cobalt which is pretreated to remove the oxide layer and the diluted nitric acid are used for dissolving Ce (NH)4)2(NO3)6，CH3CSNH2And CO (NH)2)2Under certain conditionsMixing, then putting into a reaction kettle, washing and drying under the reaction condition of 180 ℃ for 8 hours to obtain the heterogeneous multi-layer nano-structure electrocatalyst;
according to the invention, the heterogeneous multi-layer nano-structure electrocatalyst is prepared by a one-step hydrothermal method, and the catalyst prepared by the method can obtain a nano array with a high specific surface area, and has good catalytic results on hydrogen evolution reaction and oxygen evolution reaction. Compared with the modern technology, the method finally realizes the purpose of preparing the heterogeneous multi-level nano-structure electrocatalyst with better bifunctional catalytic activity by in-situ growing the nano-array on the metallic cobalt foam under certain conditions.
In addition, the present invention provides CeO2@Co3S4The preparation method of the heterogeneous multilevel nano-structure electrolytic water catalyst is simple, the reaction condition is mild, and the method is suitable for large-scale production; the prepared product has the characteristics of stability and high catalytic activity of electrolyzed water, can be widely applied to electrochemical energy storage and conversion technology, and has high application value.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 shows the results of X-ray diffraction analysis of samples prepared under different pH conditions.
FIG. 2 shows the results of SEM measurements of samples prepared at different pH conditions.
FIG. 3 shows the results of the catalytic performance tests of the catalysts prepared under different pH conditions on Hydrogen Evolution Reaction (HER) and Oxygen Evolution Reaction (OER).
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention discloses a one-step method for synthesizing CeO2@Co3S4A preparation method of a heterogeneous multi-level nano-structure electrolytic water catalytic material.
The present invention will be further specifically illustrated by the following examples for better understanding, but the present invention is not to be construed as being limited thereto, and certain insubstantial modifications and adaptations of the invention by those skilled in the art based on the foregoing disclosure are intended to be included within the scope of the invention.
The technical solution of the present invention will be further described with reference to the following specific examples.
Example 1
With Ce (NH)4)2(NO3)6，CH3CSNH2And CO (NH)2)2The method is characterized in that a three-dimensional foam cobalt skeleton is used as a carrier, and a dilute nitric acid solution is used as a reaction solution.
CeO (CeO)2@Co3S4The preparation method of the heterogeneous multi-level nano-structure catalytic material comprises the following steps:
(a) 0.22g of Ce (NH)4)2(NO3)6，0.15g CH3CSNH2And 0.24g CO (NH)2)2Sequentially putting into a dilute nitric acid solution with the pH value of 4, and stirring for 30 minutes;
(b) and simultaneously transferring the mixed solution and the foamed cobalt into a polytetrafluoroethylene reaction kettle, and putting the polytetrafluoroethylene reaction kettle into an oven for hydrothermal reaction under the reaction conditions of 180 ℃ and 8 hours.
(c) After the reaction is finished, taking out the reacted foam cobalt, respectively ultrasonically washing the foam cobalt for three times by using deionized water and absolute ethyl alcohol, and drying to obtain CeO2@Co3S4-CF-4 heterogeneous multi-layered nanostructured electrocatalyst.
Example 2:
controlling the pH value of the dilute nitric acid in the embodiment 1 to be 2, controlling the pH value to be 2, carrying out the same other steps, taking out the foamed cobalt after the reaction is finished, respectively carrying out ultrasonic washing for three times by using deionized water and absolute ethyl alcohol, and drying to obtain CeO2@Co3S4-CF-2 heterogeneous multi-layered nanostructure electrocatalyst
Example 3:
controlling the pH value of the dilute nitric acid in the embodiment 1 to be 6, controlling the pH value to be 6, carrying out the same other steps, taking out the foamed cobalt after the reaction is finished, respectively carrying out ultrasonic washing for three times by using deionized water and absolute ethyl alcohol, and drying to obtain CeO2@Co3S4-CF-6 heterogeneous multi-layered nanostructured electrocatalyst.
Example 4:
with Ce (NH)4)2(NO3)6，CH3CSNH2And CO (NH)2)2The method is characterized in that a three-dimensional foam cobalt skeleton is used as a carrier, and a dilute nitric acid solution is used as a reaction solution. Respectively adding 0.11g of Ce (NH)4)2(NO3)6，0.15gCH3CSNH2And 0.24g CO (NH)2)2Sequentially putting into a dilute nitric acid solution with the pH value of 4, and stirring for 30 minutes; simultaneously transferring the mixed solution and the foamed cobalt into a polytetrafluoroethylene reaction kettle, and putting the polytetrafluoroethylene reaction kettle into a drying oven for hydrothermal reaction under the reaction conditions of 180 ℃ and 8 hours; and after the reaction is finished, taking out the reacted foam cobalt, and respectively ultrasonically washing the foam cobalt for three times by using deionized water and absolute ethyl alcohol.
Example 5:
with Ce (NH)4)2(NO3)6，CH3CSNH2And CO (NH)2)2The method is characterized in that a three-dimensional foam cobalt skeleton is used as a carrier, and a dilute nitric acid solution is used as a reaction solution. Respectively adding 0.44g of Ce (NH)4)2(NO3)6，0.15gCH3CSNH2And 0.24g CO (NH)2)2Sequentially putting into a dilute nitric acid solution with the pH value of 4, and stirring for 30 minutes; simultaneously transferring the mixed solution and the foamed cobalt into a polytetrafluoroethylene reaction kettle, and putting the polytetrafluoroethylene reaction kettle into an oven for hydrothermal reactionThe reaction condition is 180 ℃ and 8 hours; and after the reaction is finished, taking out the reacted foam cobalt, and respectively ultrasonically washing the foam cobalt for three times by using deionized water and absolute ethyl alcohol.
Example 6:
with Ce (NH)4)2(NO3)6，CH3CSNH2And CO (NH)2)2The method is characterized in that a three-dimensional foam cobalt skeleton is used as a carrier, and a dilute nitric acid solution is used as a reaction solution. Respectively adding 0.22g of Ce (NH)4)2(NO3)6，0.15gCH3CSNH2And 0.24g CO (NH)2)2Sequentially putting into a dilute nitric acid solution with the pH value of 4, and stirring for 30 minutes; simultaneously transferring the mixed solution and the foamed cobalt into a polytetrafluoroethylene reaction kettle, and putting the polytetrafluoroethylene reaction kettle into a drying oven for hydrothermal reaction under the reaction conditions of 160 ℃ and 8 hours; and after the reaction is finished, taking out the reacted foam cobalt, and respectively ultrasonically washing the foam cobalt for three times by using deionized water and absolute ethyl alcohol.
Example 7:
with Ce (NH)4)2(NO3)6，CH3CSNH2And CO (NH)2)2The method is characterized in that a three-dimensional foam cobalt skeleton is used as a carrier, and a dilute nitric acid solution is used as a reaction solution. 0.22g of Ce (NH)4)2(NO3)6，0.15gCH3CSNH2And 0.24g CO (NH)2)2Sequentially putting into a dilute nitric acid solution with the pH value of 4, and stirring for 30 minutes; simultaneously transferring the mixed solution and the foamed cobalt into a polytetrafluoroethylene reaction kettle, and putting the polytetrafluoroethylene reaction kettle into a drying oven for hydrothermal reaction under the reaction conditions of 200 ℃ and 8 hours; and after the reaction is finished, taking out the reacted foam cobalt, and respectively ultrasonically washing the foam cobalt for three times by using deionized water and absolute ethyl alcohol.
Example 8:
with Ce (NH)4)2(NO3)6，CH3CSNH2And CO (NH)2)2The method is characterized in that a three-dimensional foam cobalt skeleton is used as a carrier, and a dilute nitric acid solution is used as a reaction solution. Respectively adding 0.22g of Ce (NH)4)2(NO3)6，0.15gCH3CSNH2And 0.24g CO (NH)2)2Sequentially putting into a dilute nitric acid solution with the pH value of 4, and stirring for 30 minutes; simultaneously transferring the mixed solution and the foamed cobalt into a polytetrafluoroethylene reaction kettle, and putting the polytetrafluoroethylene reaction kettle into a drying oven for hydrothermal reaction under the reaction conditions of 180 ℃ and 6 hours; and after the reaction is finished, taking out the reacted foam cobalt, and respectively ultrasonically washing the foam cobalt for three times by using deionized water and absolute ethyl alcohol.
Example 9:
with Ce (NH)4)2(NO3)6，CH3CSNH2And CO (NH)2)2The method is characterized in that a three-dimensional foam cobalt skeleton is used as a carrier, and a dilute nitric acid solution is used as a reaction solution. 0.22g of Ce (NH)4)2(NO3)6，0.15gCH3CSNH2And 0.24g CO (NH)2)2Sequentially putting into a dilute nitric acid solution with the pH value of 4, and stirring for 30 minutes; simultaneously transferring the mixed solution and the foamed cobalt into a polytetrafluoroethylene reaction kettle, and putting the polytetrafluoroethylene reaction kettle into a drying oven for hydrothermal reaction under the reaction conditions of 180 ℃ and 10 hours; and after the reaction is finished, taking out the reacted foam cobalt, and respectively ultrasonically washing the foam cobalt for three times by using deionized water and absolute ethyl alcohol.
Test example 1: structural composition analysis
The samples prepared in examples 1, 2 and 3 were subjected to X-ray diffraction analysis, and the results are shown in fig. 1, which indicates that the samples prepared in examples 1, 2 and 3 were foam cobalt-supported CeO2And Co3S4。
Test example 2: surface topography observation
Scanning Electron Microscopy (SEM) was used to determine the CeO obtained in examples 1, 2 and 32@Co3S4The surface topography and structure of the heterogeneous multi-layer nano-structure electrocatalyst are observed, and the results are shown in figure 2(a-c pH 2; d-fpH 4; g-IpH 6): flake Co at pH43S4The nano sheets are regularly distributed in the rod-shaped CeO2Surface, and forming CeO2@Co3S4A heterogeneous multi-layered nanostructure.
Test example 3: testing of catalyst Performance
FIG. 3 shows the results of the catalytic performance tests of the catalysts prepared in examples 1, 2 and 3 on Hydrogen Evolution Reaction (HER) and Oxygen Evolution Reaction (OER).
As can be seen from the figure: in the hydrogen evolution reaction, when the pH value is 4, the heterogeneous multi-layer nano-structure electrocatalyst CeO2@Co3S4Compared with other catalysts, the catalyst has lower overpotential when the current density is 10mA/cm2When the overpotential is as low as 74.9mV, the Tafel slope is only 40mV dec-1This shows that the heterogeneous multi-layer nano-structure electrocatalyst prepared by the method has better electrocatalytic performance. And in the electrocatalytic oxygen evolution curve, when the current density is 10mA/cm2When the overpotential is as low as 213mV, the Tafel slope is only 97.3mV dec-1. Moreover, the preparation method of the electrocatalyst enables CeO to be prepared2@Co3S4Can grow uniformly and improve CeO2@Co3S4The yield of the catalyst is high, the rod-shaped nano array loaded with the nano sheets is obtained, the catalyst has a multi-layer nano structure of a heterojunction, the specific surface area of the catalyst can be effectively improved, more active sites are exposed, the electron transfer is facilitated, the catalytic activity of the catalyst is improved, the catalyst has the advantages of low overpotential, good stability and high current density, the preparation method is simple to operate, the reaction condition is mild, and the catalyst is suitable for large-scale production.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. CeO (CeO)2@Co3S4A preparation method of heterogeneous multi-layer nano-structure catalytic material,the method is characterized by comprising the following steps:
(1) adding Ce (NH)4)2(NO3)6，CH3CSNH2And CO (NH)2)2Dissolving in dilute nitric acid to form a solution, then adding foamed cobalt into the solution, and stirring to obtain a reaction system;
(2) transferring the reaction system to a hydrothermal reaction kettle for reaction, naturally cooling after the reaction is finished, taking out the foamed cobalt, and washing and drying to obtain the foamed cobalt loaded CeO2@Co3S4Heterogeneous multi-level nano-structure catalytic material.
2. CeO according to claim 12@Co3S4The preparation method of the heterogeneous multi-layer nano-structure catalytic material is characterized in that in the step (1), Ce (NH)4)2(NO3)6，CH3CSNH2And CO (NH)2)2The ratio of the amounts of substances (a) to (b) is 0.5: 5: 10. 1: 5: 10 and 2: 5: 10, and said Ce (NH)4)2(NO3)6，CH3CSNH2And CO (NH)2)2The total concentration is 0.15-0.17 mol/L.
3. CeO according to claim 22@Co3S4The preparation method of the heterogeneous multi-layer nano-structure catalytic material is characterized in that the pH value of the dilute nitric acid is 2-6.
4. CeO according to claim 12@Co3S4The preparation method of the heterogeneous multi-layer nano-structure catalytic material is characterized in that the reaction temperature in the step (2) is 160-200 ℃, and the reaction time is 6-10 h.
5. CeO prepared by the method of claim 12@Co3S4Heterogeneous multi-level nanostructured catalytic material, characterized in that said catalytic materialComprises CeO with a nano rod-shaped structure with a vertical three-dimensional growing and compact arrangement surface2@Co3S4And the said CeO2@Co3S4Growing on the surface of the foamed cobalt.
6. CeO prepared by the method of claim 12@Co3S4The heterogeneous multi-level nano-structure catalytic material can be applied to the field of water electrolysis.
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