CN112695335A - Preparation method of acid steam assisted nickel-iron hydrotalcite nanosheet-foamed nickel - Google Patents
Preparation method of acid steam assisted nickel-iron hydrotalcite nanosheet-foamed nickel Download PDFInfo
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- CN112695335A CN112695335A CN202110065678.8A CN202110065678A CN112695335A CN 112695335 A CN112695335 A CN 112695335A CN 202110065678 A CN202110065678 A CN 202110065678A CN 112695335 A CN112695335 A CN 112695335A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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 an acid-steam-assisted preparation method of nickel-iron hydrotalcite nanosheet-foamed nickel, and belongs to the field of preparation of oxygen evolution electrodes under an electrocatalytic alkaline condition. The method comprises the following steps: after acetone deoiling treatment is carried out on a nickel-based current collector, the nickel-based current collector is soaked in ferric chloride solution fully and is subjected to ultrasonic treatment for about 5 min, then the nickel-based current collector is taken out and is placed in an acid-resistant container capable of being sealed, vacuum pumping is carried out, then mixed gas of specific gas and acid steam is filled into the sealed container, sealing is kept, a certain temperature is kept, the nickel-based current collector is placed for 8-16h, finally the nickel-based current collector is taken out, and the nickel-iron hydrotalcite nanosheet array-nickel electrode is obtained after repeated cleaning by using distilled water and is used as a working electrode in an alkaline electro. The surface of the prepared nickel catalytic electrode is uniformly covered with a vertically distributed nickel-iron hydrotalcite nanosheet array, and the electrode has excellent alkaline electrocatalytic oxygen evolution activity and good stability under alkaline conditions.
Description
Technical Field
The invention relates to the technical field of catalytic electrode preparation, in particular to a preparation method of acid steam assisted nickel-iron hydrotalcite nanosheet-foamed nickel.
Background
In the rapid development of the modern society, the traditional fossil energy is a power pillar of the modern society, the storage amount of the fossil energy is reduced day by day, but the demand of the energy is increased continuously under the development demand, and the energy crisis is deepened continuously. Meanwhile, fossil resources also bring about increasingly serious environmental pollution problems in the process of energy conversion, for example, a large amount of SO is also generated in the process of converting fossil energy into energy such as power, heat, electricity and the like2、NOx、PM2.5And the like contaminating substances. The efficient and clean sustainable energy conversion technology is the most important way to solve the energy crisis and environmental problems. Among them, advanced energy conversion technologies such as fuel cells, water decomposition catalysis, metal air cells, and carbon dioxide reduction have been widely paid attention. The technologies can convert intermittent and clean low-voltage electric energy which is difficult to be combined into a grid and can be obtained by renewable energy sources (such as wind energy, light energy and the like) into chemical energy to be stored in products such as ethanol, hydrogen and the like. The oxygen evolution process of the above technology is an anodic half-reaction of many electrocatalytic reactions, and is a kinetic retardation step of the reaction as a four-electron reaction. Reducing the oxygen evolution overpotential is one of the key issues to improve the energy conversion efficiency of the above process.
The development of cheap, efficient and stable catalytic electrode materials is the key for improving the energy conversion efficiency in the oxygen evolution process. Many researches show that the nickel-iron bimetallic hydrotalcite is a stable catalytic material with high energy conversion efficiency. The nickel-iron hydrotalcite nanosheet array can be grown on a current collector with good electron transport capacity in a hydrothermal mode, an electrodeposition mode and the like, so that a catalytic electrode with high oxygen evolution performance is obtained. However, all the existing methods for preparing the nickel-iron hydrotalcite electrode are solution synthesis, can generate a large amount of waste liquid and simultaneously have high energy consumption. In addition, both hydrothermal and electrodeposition are limited by reaction conditions, making it difficult to produce large-sized catalytic electrodes.
The invention content is as follows:
the invention aims to solve the problems of high energy consumption, high pollution, high cost and inconvenience for large-scale production in the preparation of the high-performance nickel-iron hydrotalcite catalytic electrode. The preparation method of the nickel-iron hydrotalcite-foamed nickel electrode with high oxygen evolution performance is provided, and the obtained foamed nickel electrode which is assembled by nano sheets and grows in a nickel-iron hydrotalcite array is provided. The catalytic electrode prepared by the method has higher oxygen evolution activity, and has the characteristics of simple preparation, easy large-scale production and the like.
The invention relates to an acid steam assisted preparation method of nickel iron hydrotalcite nanosheet-foamed nickel, which comprises the following steps:
a. dissolving ferric chloride in deionized water to prepare ferric chloride solution, soaking deoiled foam nickel in the ferric chloride solution, immersing and performing ultrasonic treatment for 5 min, taking out the foam nickel, and drying the foam nickel for 30 min at normal temperature;
b. b, placing the foamed nickel treated in the step a into a closed acid-resistant container, and placing an open bottle of concentrated acid solution into the same closed container to ensure an acidic steam atmosphere in the closed container;
c. and (c) sealing the container in the step (b) and vacuumizing, then introducing gas until the pressure is equal to the external atmospheric pressure (the first two steps can be omitted in the reaction under the air), then sealing the system again, keeping the constant temperature for reaction for a period of time, taking out, opening the sealed container, taking out the foamed nickel, and repeatedly washing the foamed nickel by using distilled water to obtain the nickel-iron hydrotalcite nanosheet-foamed nickel.
As a further improvement of the invention, in the step a, the concentration of the ferric chloride solution is 10mmol/L-50mmol/L, wherein the ratio of the area of the nickel foam to the volume of the ferric chloride solution is 0.4cm2/ml-1.2cm2/ml。
As a further improvement of the invention, in the step b, the concentrated acid solution is concentrated sulfuric acid, concentrated nitric acid or a mixed solution of the concentrated sulfuric acid and the concentrated nitric acid in any proportion.
As a further improvement of the invention, in the step b, the introduced gas is oxygen, carbon dioxide or a mixed gas of the oxygen and the carbon dioxide in any proportion.
As a further improvement of the invention, in the step c, the temperature of the closed container is kept between 30 and 80 ℃, and the reaction time is between 10 and 14 hours.
Compared with the prior art, the invention has the following beneficial effects:
1. the acid steam auxiliary preparation method adopted by the invention is simple, low in cost and low in waste liquid amount;
2. the preparation method adopted by the invention requires simple and easily available experimental instruments, so that the production scale is easily enlarged;
3. the nickel-iron hydrotalcite nano-sheet double-nickel-iron metal prepared by the method is not uniformly distributed, and iron is locally concentrated on the surface, so that the electro-catalytic oxygen evolution activity of the material is improved;
4. the nickel-iron hydrotalcite-foamed nickel electrode prepared by the invention has stable performance, excellent water energy decomposition by electro-catalysis, and wide application prospect in the field of energy conversion.
Description of the drawings:
FIG. 1 is an X-ray diffraction pattern of nickel iron hydrotalcite (named A-NiFe/NF, O-NiFe/NF and C-NiFe/NF, respectively) in different atmospheres (air, nitrogen, oxygen) prepared by the present invention;
FIG. 2 is the scanning electron microscope and scanning transmission electron microscope photographs of nickel iron hydrotalcite prepared by the present invention under different atmospheres (air, nitrogen, oxygen), (A-C) is A-NiFe/NF, (D-F) is O-NiFe/NF and (G-I) is C-NiFe/NF;
fig. 3 is an electrochemical performance characterization of nickel iron hydrotalcite-foamed nickel electrode prepared in different atmospheres (air, nitrogen and oxygen) according to the invention, (a) a polarization curve, (B) a tafel curve, (C) an electrochemical activity specific surface area test and (D) a constant current curve, and the inset is the polarization curve before and after 75 hours of constant current.
The specific implementation mode is as follows:
example 1
The preparation method of the acid vapor assisted nickel-iron hydrotalcite nanosheet-foamed nickel of the embodiment is carried out according to the following steps:
a. dissolving ferric chloride in deionized water to prepare 25mmol/L ferric chloride solution, soaking deoiled foam nickel in the ferric chloride solution, performing ultrasonic treatment for 5 min, taking out the foam nickel, and drying for 30 min at normal temperature; wherein the ratio of the area of the foamed nickel to the volume of the ferric chloride solution is 0.4cm2/ml；
b. B, placing the foamed nickel treated in the step a into an acid-resistant container, and placing an open bottle containing 5ml of concentrated nitric acid solution in the container to ensure an acidic steam atmosphere in the closed container;
c. and c, sealing the container in the step b, then sealing the system again, keeping the temperature of the system at 50 ℃ for reaction for 12 hours, cooling, opening the sealed container, taking out the foamed nickel, repeatedly washing the foamed nickel by using distilled water, and airing to obtain the nickel-iron hydrotalcite nanosheet-foamed nickel.
Example 2
The present embodiment is different from embodiment 1 only in that: the concentration of the ferric chloride solution in the step a is 15 mmol/L.
Example 3
The present embodiment is different from embodiment 1 only in that: in step b, 5ml of concentrated sulfuric acid is placed in an open container.
Example 4
The present embodiment is different from embodiment 1 only in that: and c, sealing the container, vacuumizing, and introducing oxygen or carbon dioxide until the pressure is equal to the external atmospheric pressure.
Example 5
The present embodiment is different from embodiment 1 only in that: in step c, the reaction was carried out for 12h while maintaining the temperature in the closed vessel at 60 ℃.
Example 6
The present embodiment is different from embodiment 1 only in that: in the step a, the concentration of the ferric chloride solution is 10mmol/L, wherein the ratio of the area of the nickel foam to the volume of the ferric chloride solution is 1.0cm2Per ml; in the step b, the concentrated sulfuric acid and the concentrated nitric acid are mixed and dissolved, and the mixing volume ratio is 1: 2; in the step c, the temperature of the closed container is kept between 30 ℃, and the reaction time is 10 hours.
Example 7
The present embodiment is different from embodiment 1 only in that: in the step a, the concentration of the ferric chloride solution is 50mmol/L, wherein the ratio of the area of the nickel foam to the volume of the ferric chloride solution is 1.2cm2Per ml; in the step b, the concentrated sulfuric acid and the concentrated nitric acid are mixed and dissolved, and the mixing volume ratio is 5: 3; in the step c, the temperature of the closed container is kept between 80 ℃, and the reaction time is 14 h.
The physical properties and catalytic performance of the nickel-iron hydrotalcite nanosheet-foamed nickel prepared by the method of example 1 were verified as follows:
firstly, the samples are subjected to physical property characterization by an X-ray diffraction and scanning electron microscope under the conditions of air, oxygen and carbon dioxide. The X-ray diffraction pattern is shown in FIG. 1, and the test samples are all powder scraped from the surface of the foamed nickel electrode, except the diffraction peak of the elemental nickel (card number 04-0850) from the foamed nickel, the diffraction peak can be assigned to the NiFe LDH (card number 40-0215). The scanning electron microscope and projection scanning electron microscope photographs are shown in FIG. 2, and FIG. 2(A-C) is A-NiFe/NF, FIG. 2(D-F) is O-NiFe/NF and FIG. 2(G-I) is C-NiFe/NF photographs, and the results show that the surface of the foamed nickel obtained in the three atmospheres is covered by the nano-sheet, wherein the nano-sheet of the sample obtained in the atmosphere of air and carbon dioxide can completely cover the foamed nickel, and part of the foamed nickel is exposed in the atmosphere of oxygen.
And secondly, verifying the electrocatalytic oxygen evolution activity of the nickel-iron hydrotalcite composite material under a three-electrode system, wherein nickel-iron hydrotalcite foam nickel is used as a working electrode, a carbon rod is used as a counter electrode, a calomel electrode is used as a reference electrode, and the electrolyte is 1mol/L KOH. And the electrocatalytic activity is verified by a polarization curve, a Tafel curve and the specific surface area of electrochemical activity, and the current density is 100 mA/cm2The stability was verified by keeping the temperature for 75 hours at constant current. Test results show that the catalytic electrode has excellent oxygen evolution activity, wherein the A-NiFe/NF prepared under the air condition has the most activity and has the current density of 100 mA/cm2The time potential is only 1.496VvsRHE. At the same time, the constant current is 100 mA/cm2The potential can be kept stable for a long time and before constant current testingThe stability of the rear polarization curve can be further proved by ensuring the basic coincidence.
Claims (5)
1. An acid steam assisted preparation method of nickel iron hydrotalcite nanosheet-foamed nickel comprises the following steps:
a. dissolving ferric chloride in deionized water to prepare ferric chloride solution, soaking deoiled foam nickel in the ferric chloride solution, immersing and performing ultrasonic treatment for 5 min, taking out the foam nickel, and drying the foam nickel for 30 min at normal temperature;
b. b, placing the foamed nickel treated in the step a into a closed acid-resistant container, and placing an open bottle of concentrated acid solution into the same closed container to ensure an acidic steam atmosphere in the closed container;
c. and c, sealing the container in the step b, vacuumizing, introducing gas until the pressure is equal to the external atmospheric pressure, sealing the system again, keeping the constant temperature, reacting for a period of time, taking out, opening the sealed container, taking out the foamed nickel, and repeatedly washing with distilled water to obtain the nickel-iron hydrotalcite nanosheet-foamed nickel.
2. The method for preparing acid vapor assisted nickel iron hydrotalcite nano-sheet-nickel foam according to claim 1, wherein in step a, the concentration of the ferric chloride solution is 10mmol/L-50mmol/L, and the ratio of the area of the nickel foam to the volume of the ferric chloride solution is 0.4cm2 /ml-1.2 cm2 /ml。
3. The method for preparing acid vapor assisted nickel iron hydrotalcite nano-sheet-nickel foam according to claim 1, wherein in step b, the concentrated acid solution is concentrated sulfuric acid, concentrated nitric acid or a mixture of the two at any ratio.
4. The method for preparing acid vapor assisted nickel-iron hydrotalcite nanosheet-foamed nickel according to claim 1, wherein in step b, the gas introduced is oxygen, carbon dioxide or a mixture of the oxygen and the carbon dioxide in any proportion.
5. The method for preparing acid vapor assisted nickel iron hydrotalcite nano-sheet-nickel foam according to claim 1, wherein in step c, the temperature of the closed container is kept between 30 ℃ and 80 ℃, and the reaction time is 10h to 14 h.
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