CN112501645B - Nickel hydroxide/nickel screen composite hydrogen and oxygen evolution electrode, preparation method and application thereof - Google Patents
Nickel hydroxide/nickel screen composite hydrogen and oxygen evolution electrode, preparation method and application thereof Download PDFInfo
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- CN112501645B CN112501645B CN202011455092.4A CN202011455092A CN112501645B CN 112501645 B CN112501645 B CN 112501645B CN 202011455092 A CN202011455092 A CN 202011455092A CN 112501645 B CN112501645 B CN 112501645B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a nickel hydroxide/nickel screen composite hydrogen and oxygen evolution electrode, a preparation method and application thereof, belonging to the field of electrocatalytic decomposition water catalyst. The initial overpotential of the electrode in 3 mol/L NaOH electrolyte at 80 ℃ is 1.471V, which is superior to the Raney nickel/nickel mesh electrode widely used in industrial water electrolysis hydrogen production. The stability of the composite hydrogen evolution and oxygen evolution electrode is also obviously superior to that of an industrial Raney nickel/nickel mesh electrode, and meanwhile, the composite hydrogen evolution and oxygen evolution electrode is simple in preparation process, low in cost and easy to realize industrial mass production, and can provide a new idea for the industrial development of hydrogen production by water electrolysis.
Description
Technical Field
The invention relates to the field of electrocatalytic water decomposition catalysts, in particular to a nickel hydroxide/nickel mesh composite hydrogen and oxygen evolution electrode, a preparation method and application thereof.
Background
Nowadays, with the overuse of fossil energy, the environmental deterioration problem becomes more serious and the fossil fuel reserves are reduced, so the development and utilization of new energy sources and renewable energy sources such as nuclear energy, wind energy, solar energy, hydrogen energy and the like are highly regarded by countries all over the world. Among them, hydrogen energy is widely regarded by scientists in all countries in the world due to its advantages of good combustion performance, less consumption, no toxicity, no pollution, etc. In the hydrogen preparation technology, the hydrogen production by water electrolysis becomes one of the fastest and most mature large-scale hydrogen production means due to the advantages of simple principle, high product purity, cleanness, no pollution and the like. The core reaction of hydrogen production by water electrolysis is two semi-reactions which are independent in space: the hydrogen evolution reaction at the cathode and the oxygen evolution reaction at the anode. In order to make the hydrogen production by water electrolysis economical and practical, the consumption of electrolysis energy needs to be reduced to the maximum extent, and an effective method for solving the problem is to reduce overpotential of hydrogen evolution reaction and oxygen evolution reaction. Therefore, the research and design of the catalyst electrode with low overpotential are significant for the industry of water electrolysis for hydrogen production.
The research on the catalyst for hydrogen production by water electrolysis is mainly carried out on noble metals such as platinum, iridium and ruthenium, but the catalyst is rare in storage and expensive, and is difficult to realize large-scale application. Currently, the electrode widely used in industrial water electrolysis hydrogen production is a raney nickel/nickel mesh electrode which is low in price, but the water decomposition performance of the electrode has a great space for improvement. Among a plurality of electrolytic water catalytic electrode materials, non-noble metal oxides/hydroxides are approaching to or even surpassing commercial electrode materials such as noble metals in the aspects of catalytic activity and durability due to lower cost and adjustable electronic structure, and have application potential. Therefore, the development of low-cost, high electrocatalytic activity and stability non-noble metal catalysts has become a very important and popular research area.
Disclosure of Invention
The invention aims to provide a nickel hydroxide/nickel mesh composite hydrogen and oxygen evolution electrode, a preparation method and application thereof, which aim to solve the problems in the prior art. The invention prepares the electrolytic water electrode with high efficiency, high stability and low price by simple, economic and easy-to-realize industrialized preparation conditions or methods, reduces hydrogen evolution and oxygen evolution overpotential of the electrolytic water, improves the efficiency of the electrolytic water, and promotes the industrialized development of hydrogen production by the electrolytic water.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a nickel hydroxide/nickel screen composite hydrogen and oxygen evolution electrode, which comprises nickel hydroxide nanosheets uniformly grown in situ on a nickel screen substrate.
The invention also provides another nickel hydroxide/nickel mesh composite hydrogen and oxygen evolution electrode, wherein iron-cobalt alloy nano particles are uniformly covered on the nickel hydroxide nano sheets to form the iron-cobalt alloy particle/nickel hydroxide/nickel mesh composite electrode.
Further, the nickel hydroxide nanoplates are about 300 nanometers in length; the iron-cobalt alloy nanoparticles have a diameter of about 50 nanometers.
The invention also provides a preparation method of the nickel hydroxide/nickel mesh composite hydrogen and oxygen evolution electrode, which comprises the following steps:
dissolving NaCl in deionized water, and stirring for 10-15 minutes to obtain a NaCl solution; and putting the nickel screen into the NaCl solution, carrying out water bath, taking out and drying to obtain the nickel hydroxide/nickel screen electrode.
The invention also provides a preparation method of the nickel hydroxide/nickel screen composite hydrogen and oxygen evolution electrode, which is characterized by comprising the following steps:
dissolving NaCl in deionized water, and stirring for 10-15 minutes to obtain a NaCl solution; putting the nickel screen into the NaCl solution, carrying out water bath, taking out and drying to obtain a nickel hydroxide/nickel screen electrode;
dissolving a mixture of cobalt nitrate hexahydrate, ferrous sulfate heptahydrate and sodium citrate in deionized water, and stirring for 25-35 minutes to obtain a mixed solution; and putting the nickel hydroxide/nickel screen electrode into the mixed solution, and carrying out water bath to obtain the nickel hydroxide/nickel screen composite hydrogen and oxygen evolution electrode.
Further, the concentration of the NaCl solution was 0.5 mol/l.
Further, in the first step, the temperature of the water bath is 90 ℃ and the time is 8 hours; before use, the nickel screen is subjected to primary ultrasonic cleaning for 15-30 minutes by using 5% HCl, absolute ethyl alcohol and deionized water respectively; and drying the nickel hydroxide/nickel screen electrode for 30 minutes at 80 ℃ under a vacuum condition to obtain the nickel hydroxide/nickel screen electrode.
Further, in the second step, the concentrations of the cobalt nitrate hexahydrate, the ferrous sulfate heptahydrate and the sodium citrate in the mixed solution are 0.1 mol/l, 0.1 mol/l and 37 mmol/l, respectively.
Further, in the second step, the temperature of the water bath is 90 ℃ and the time is 2 hours.
The invention also provides an application of the nickel hydroxide/nickel screen composite electrode or the nickel hydroxide/nickel screen composite electrode prepared by the preparation method in hydrogen production by water electrolysis.
Further, the nickel hydroxide/nickel screen composite hydrogen and oxygen evolution electrode can be used for manufacturing an electrode or a catalyst for hydrogen production by water electrolysis.
The invention discloses the following technical effects:
(1) the nickel hydroxide/nickel screen composite hydrogen and oxygen evolution electrode adopts the nickel screen as the substrate, the nickel hydroxide growing in situ has good contact with the nickel screen, the stability is good, the preparation process is simple, the energy consumption in the preparation process is low, and the industrial production is convenient.
(2) The nickel hydroxide grown in situ can also enhance the binding capacity with iron-cobalt alloy particles, and the nickel hydroxide and iron-cobalt alloy have good stability under alkaline conditions. The reserves of non-noble metal elements such as Ni, Fe and Co are abundant and the price is low.
(3) The Fe-Co alloy particle/nickel hydroxide/nickel screen composite hydrogen and oxygen evolution electrode prepared by the invention is of a porous structure, has a large electrochemical active area, and greatly improves the catalytic activity. Can be widely used as an electrode material of alkaline electrolytic water and has wide application prospect.
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 embodiments will be briefly described below. It is obvious that the drawings in the following description are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
1. FIG. 1 is a scanning electron microscope image of the surface topography of the nickel hydroxide/nickel mesh composite hydrogen and oxygen evolution electrode prepared in example 1 of the present invention and the Raney nickel/nickel mesh electrode of comparative example 1, wherein (a) is the Raney nickel/nickel mesh electrode; (b) is nickel hydroxide/nickel screen electrode, and (c) is iron-cobalt alloy particle/nickel hydroxide/nickel screen electrode.
2. Fig. 2 is a graph of current density versus potential for the electrodes of examples 1 and 2 of the present invention and comparative example 1.
3. FIG. 3 is a graph of current versus time for an electrode of example 2 of the present invention at an applied voltage of 1.78 volts.
4. Fig. 4 is a scanning electron microscope image of the surface topography of the nickel hydroxide/nickel mesh composite hydrogen and oxygen evolution electrode prepared in example 1 of the present invention and the raney nickel/nickel mesh electrode of comparative example 1 after 1 hour of ultrasound, wherein, (a) is the raney nickel/nickel mesh electrode, (b) is the nickel hydroxide/nickel mesh electrode, and (c) is the iron-cobalt alloy particle/nickel hydroxide/nickel mesh electrode.
5. Fig. 5 is a graph of current density versus potential after 1 hour of sonication for the electrodes of examples 1 and 2 of the invention and comparative example 1.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
Example 1
The preparation method of the nickel hydroxide/nickel screen composite hydrogen and oxygen evolution electrode comprises the following steps:
a. pretreatment of electrically conductive substrates
Selecting a cut nickel screen with the size of 1 multiplied by 1 square centimeter, soaking the nickel screen in an ethanol solvent for ultrasonic treatment for 20 minutes, and then, performing ultrasonic treatment for 10 minutes by using a hydrochloric acid solution with the concentration of 20 percent to perform chemical degreasing and surface oxidation; and finally, washing the nickel substrate with deionized water.
b. Growing porous nickel structures on nickel screens
Dissolving NaCl in deionized water to obtain NaCl water solution of 0.5 mol/L concentration; stirring for 13 minutes; and putting the nickel screen into the obtained solution, putting the nickel screen into a water bath kettle, reacting at the temperature of 90 ℃ for 8 hours, washing and drying the product after the reaction is finished, thus obtaining the nickel hydroxide/nickel screen electrode.
Example 2
The preparation method of the iron-cobalt alloy particle/nickel hydroxide/nickel screen composite hydrogen and oxygen evolution electrode comprises the following steps:
c. pretreatment of electrically conductive substrates
Selecting a cut nickel screen with the size of 1 multiplied by 1 square centimeter, soaking the nickel screen in an ethanol solvent for ultrasonic treatment for 20 minutes, and then, performing ultrasonic treatment for 10 minutes by using a hydrochloric acid solution with the concentration of 20 percent to perform chemical degreasing and surface oxidation; and finally, washing the nickel substrate with deionized water.
d. Growing porous nickel structures on nickel screens
Dissolving NaCl in deionized water to obtain NaCl water solution of 0.5 mol/L concentration; stirring for 13 minutes; and putting the nickel screen into the obtained solution, putting the nickel screen into a water bath kettle, reacting at the temperature of 90 ℃ for 8 hours, washing and drying the product after the reaction is finished, thus obtaining the nickel hydroxide/nickel screen electrode.
e. Water bath preparation of iron-cobalt alloy particle/nickel hydroxide/nickel mesh composite electrode
And (b) dissolving a mixture of cobalt nitrate hexahydrate, ferrous sulfate heptahydrate and sodium citrate in deionized water according to a certain concentration, stirring for 30 minutes, wherein the concentrations of the cobalt nitrate hexahydrate, the ferrous sulfate heptahydrate and the sodium citrate are 0.1 mol/L, 0.1 mol/L and 37m mol/L respectively, then putting the nickel hydroxide/nickel mesh electrode obtained in the step b into the obtained solution, putting the solution into a water bath kettle for reaction and synthesis, reacting at the temperature of 90 ℃ for 8 hours, washing and drying a product after the reaction is finished, and obtaining the iron-cobalt alloy particle/nickel hydroxide/nickel mesh composite hydrogen and oxygen evolution electrode.
Comparative example 1
A widely used electrode in industrial water electrolysis hydrogen production is a raney nickel/nickel mesh electrode.
As can be seen from the scanning electron micrograph of fig. 1, the surface of the nickel hydroxide/nickel mesh composite electrode prepared in example 1 shows a porous nano-sheet structure. The surface of the iron-cobalt alloy particle/nickel hydroxide/nickel mesh electrode prepared in the embodiment 2 has a large number of nano particles densely and uniformly attached to the nickel hydroxide nanosheets, so that the surface of the sample is rougher, and the specific surface area is greatly increased. Compared with the raney nickel/nickel mesh electrode of comparative example 1, it shows a larger specific surface area, and thus can expose more active sites for decomposing water.
The nickel hydroxide/nickel mesh and iron-cobalt alloy particle/nickel hydroxide/nickel mesh composite hydrogen and oxygen evolution electrode prepared in the above examples 1 and 2 and the raney nickel/nickel mesh electrode in the comparative example 1 were applied to hydrogen production by electrolysis of water, and a linear sweep voltammetry test was performed: a three-electrode system is adopted, 3 mol/L NaOH at 80 ℃ is used as electrolyte, a platinum wire is used as a counter electrode, Ag/AgCl is used as a reference electrode, and the test result is shown in figure 2.
As can be seen from FIG. 2, the potential of the nickel hydroxide/nickel mesh composite hydrogen and oxygen evolution electrode is about 1.569V when the electrode is driven by 10 mA/cm, and the water decomposition performance is inferior to that of the Raney nickel/nickel mesh electrode (the potential is about 1.51V when the electrode is driven by 10 mA/cm). However, after depositing dense and uniform iron cobalt nanoparticles on a nickel hydroxide/nickel mesh, the potential was only 1.471 volts when the electrode was driven at 10 milliamps/square centimeter. The comparison shows that the Fe-Co alloy particle/nickel hydroxide/nickel screen composite hydrogen evolution oxygen evolution electrode prepared by the method has excellent catalytic performance and is expected to become a substitute material of a noble metal catalyst in the field of hydrogen production by water electrolysis.
The current-time curve of the raney nickel/nickel mesh electrode in comparative example 1 at an applied voltage of 1.91 v is shown in fig. 3 (a). The current-time curves of the nickel hydroxide/nickel mesh and the iron-cobalt alloy particle/nickel hydroxide/nickel mesh composite hydrogen evolution oxygen electrode prepared in examples 1 and 2 at an applied voltage of 2.15 v and 2.43 v, respectively, are shown in fig. 3(b) and (c). The three electrodes can be stored stably for 70 hours or more after continuously decomposing water. Thus, we performed 1 hour ultrasonic destruction at a frequency of 40 kHz for all three electrodes.
As can be seen from fig. 4, after the ultrasonic destruction was performed for 1 hour, the surface of the raney nickel/nickel mesh electrode of comparative example 1 began to peel off, and the surface morphologies of the nickel hydroxide/nickel mesh and iron-cobalt alloy particles/nickel hydroxide/nickel mesh prepared in examples 1 and 2 were substantially consistent with the electrode before the ultrasonic destruction.
The nickel hydroxide/nickel mesh and iron-cobalt alloy particle/nickel hydroxide/nickel mesh composite hydrogen evolution oxygen electrode obtained in examples 1 and 2 and the raney nickel/nickel mesh electrode in comparative example 1 were subjected to ultrasonic destruction treatment with an ultrasonic fixed frequency of 40 khz. The 3 electrodes are applied to hydrogen production by water electrolysis, and a linear sweep voltammetry test is carried out: a three-electrode system is adopted, 3 mol/L NaOH at 80 ℃ is used as electrolyte, a platinum wire is used as a counter electrode, Ag/AgCl is used as a reference electrode, and the test result is shown in figure 5.
As can be seen from fig. 5, after 1 hour of ultrasonic treatment, the potentials of the nickel hydroxide/nickel mesh and the iron-cobalt alloy particle/nickel hydroxide/nickel mesh composite hydrogen and oxygen evolution electrode prepared in examples 1 and 2 were attenuated to 1.593 v and 1.521 v when driven by 10 ma/cm. While the comparative raney nickel/nickel mesh electrode decayed most strongly with a potential of 1.627 volts at 10 milliamps/cm. The dropping of the catalyst is accelerated through an ultrasonic experiment, and compared with a Raney nickel/nickel mesh electrode widely used in industrial water electrolysis hydrogen production, the iron-cobalt alloy particle/nickel hydroxide/nickel mesh electrode has better stability performance.
In conclusion, when the Fe-Co alloy particle/nickel hydroxide/nickel mesh composite hydrogen evolution oxygen evolution electrode is driven by 10 milliamperes per square centimeter, the potential is obviously reduced, the stability is good, and the Fe-Co alloy particle/nickel hydroxide/nickel mesh composite hydrogen evolution oxygen evolution electrode is expected to be a substitute material of a noble metal catalyst in the field of industrial-grade water electrolysis hydrogen production.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (3)
1. A preparation method of an iron-cobalt alloy particle/nickel hydroxide/nickel screen composite hydrogen and oxygen evolution electrode is characterized by comprising the following steps:
dissolving NaCl in deionized water, and stirring for 10-15 minutes to obtain a NaCl solution; putting the nickel screen into the NaCl solution, carrying out water bath, taking out and drying to obtain a nickel hydroxide/nickel screen electrode;
dissolving a mixture of cobalt nitrate hexahydrate, ferrous sulfate heptahydrate and sodium citrate in deionized water, and stirring for 25-35 minutes to obtain a mixed solution; putting the nickel hydroxide/nickel screen electrode into the mixed solution, and carrying out water bath to obtain an iron-cobalt alloy particle/nickel hydroxide/nickel screen composite hydrogen and oxygen evolution electrode;
the concentration of the NaCl solution is 0.5 mol/L;
in the first step, the temperature of the water bath is 90 ℃ and the time is 8 hours;
in the second step, the concentrations of the cobalt nitrate hexahydrate, the ferrous sulfate heptahydrate and the sodium citrate in the mixed solution are respectively 0.1 mol/L, 0.1 mol/L and 37 mmol/L;
in the second step, the temperature of the water bath is 90 ℃ and the time is 2 hours.
2. The method for preparing the Fe-Co alloy particle/nickel hydroxide/nickel screen composite hydrogen and oxygen evolution electrode according to claim 1, wherein in the step one, the nickel screen is ultrasonically cleaned for 15-30 minutes by 5% HCl, absolute ethyl alcohol and deionized water for one time before use; and drying the nickel hydroxide/nickel screen electrode for 30 minutes at 80 ℃ under a vacuum condition to obtain the nickel hydroxide/nickel screen electrode.
3. The application of the Fe-Co alloy particle/nickel hydroxide/nickel screen composite hydrogen evolution oxygen evolution electrode prepared by the preparation method of the Fe-Co alloy particle/nickel hydroxide/nickel screen composite hydrogen evolution electrode in water electrolysis hydrogen production is disclosed in any one of claims 1-2.
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