CN112575336B - Method for obtaining super-strong industrial alkaline water oxygen evolution electrode by regulating and controlling anode surface magnetic field - Google Patents
Method for obtaining super-strong industrial alkaline water oxygen evolution electrode by regulating and controlling anode surface magnetic field Download PDFInfo
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Abstract
The invention discloses a method for obtaining an ultra-strong industrial alkaline water oxygen evolution electrode by regulating and controlling a magnetic field on the surface of an anode, which comprises the steps of sequentially using dilute hydrochloric acid, absolute ethyl alcohol and deionized water to ultrasonically clean foam iron, and then soaking the foam iron in NiSO with different concentrations 4 And finally, taking out the foamed iron nickel, washing the surface solution with absolute ethyl alcohol, and air-drying the washed surface solution to be used as an oxygen evolution electrode. The electrochemical testing medium is alkaline solution, the testing temperature is room temperature, and the magnet is close to the oxygen evolution electrode in the testing process. The method has the advantages of cheap and easily-obtained used materials, simple and easy operation and no pollution to the environment, and is an efficient, simple and convenient method.
Description
Technical Field
The invention belongs to the field of electrocatalysis of electrolyzed water oxygen evolution, and mainly relates to a preparation method of a high-activity electrolyzed water oxygen evolution self-supporting anode, namely a method for obtaining an ultra-strong industrial alkaline water oxygen evolution electrode by regulating and controlling a magnetic field on the surface of an anode.
Background
Electrochemical water splitting has long been considered as a promising method for producing clean hydrogen fuel using renewable energy sources. Oxygen dissociation reactions (OERs) and hydrogen dissociation reactions (HER) are the main half-reactions that occur in a reactor. OER consumes more energy in the water splitting reaction than HER, because the half-reaction is inherently more complex with multiple proton/electron coupling steps. Therefore, effective OER electrocatalysis is important for the overall efficiency of water splitting reactions and there is a strong need for an oxygen evolution electrode with high catalytic activity. However, two main problems exist at present, namely: the oxygen evolution electrode used commercially at the present stage has the defect of higher overpotential; secondly, the following steps: the Ru/Ir-based compounds that have been found, while the most effective catalysts for OER, the scarcity and high cost of these materials greatly discourage their large-scale use in commercial electrolyzers. In recent years, as a bifunctional catalyst of OER or HER, fe/Ni mixed compounds, especially hydroxides, have attracted much attention. The advantages of such materials, including high activity, high stability and non-toxicity, have been demonstrated by a number of basic research efforts.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a method for obtaining the super-strong industrial alkaline water oxygen evolution electrode by regulating and controlling the surface magnetic field of the anode, and has the advantages of simple and easy operation, no environmental pollution, low equipment requirement and good effect.
The technical purpose of the invention is realized by the following technical scheme.
The method for obtaining the alkaline water oxygen evolution electrode for the super-strong industry by regulating and controlling the surface magnetic field of the anode comprises the steps of placing foam iron in a nickel sulfate aqueous solution for treatment, forming a nickel-iron bimetal hydroxide nanosheet array film on the foam iron, and forming a large number of gaps among the nanosheets; the foamed iron treated with nickel sulfate was used as an oxygen evolution electrode, and a magnet was placed in an alkaline solution and disposed on one side of the oxygen evolution electrode.
Further, the alkaline solution is a 1mol/L KOH or NaOH aqueous solution.
And, the reference electrode uses saturated calomel electrode, and the auxiliary electrode is platinum net.
Furthermore, the magnet is placed in the alkaline solution and close to the oxygen evolution electrode.
And ultrasonically cleaning the foamed iron by dilute hydrochloric acid, absolute ethyl alcohol and deionized water, and then carrying out nickel sulfate treatment.
And, the concentration of nickel sulfate was 10 -1 —10 -3 mol/L, the treatment temperature is 20-25 ℃ and the treatment time is 9-24 hours.
Further, the nickel sulfate-treated foam iron was washed with an anhydrous ethanol to remove the surface solution and air-dried.
The invention also discloses application of the magnet in improving the performance of the alkaline water oxygen evolution electrode.
In the technical scheme of the invention, the text is generallyThe super-strong alkaline water oxygen evolution electrode for industrial use is obtained by adjusting and controlling the magnetic field on the surface of the anode. Firstly, the foamed iron is ultrasonically cleaned by using dilute hydrochloric acid, absolute ethyl alcohol and deionized water in sequence, and then is soaked in NiSO with different concentrations 4 And finally, taking out the foamed iron nickel, washing the surface solution with absolute ethyl alcohol, and air-drying the washed surface solution to be used as an oxygen evolution electrode. The electrochemical testing medium is alkaline solution, the testing temperature is room temperature, and the magnet is close to the oxygen evolution electrode in the testing process. The method has the advantages of cheap and easily-obtained materials, simple and easy operation, no environmental pollution, low equipment requirement and good effect.
Drawings
FIG. 1 is a diagram of a sample oxygen evolution process under magnetic field regulation in the technical scheme of the invention.
FIG. 2 shows a schematic view of a solution 10 according to the invention -3 mol/L NiSO 4 CV curve diagram of the soaked sample under the regulation and control of no magnetic field.
FIG. 3 shows a schematic view of a solution 10 according to the invention -2 mol/L NiSO 4 The CV curve of the soaked sample is regulated and controlled in the presence of a magnetic field.
FIG. 4 shows a schematic view of a solution 10 according to the invention -1 mol/L NiSO 4 The CV curve diagram of the soaked sample is regulated and controlled in the presence of a non-magnetic field.
FIG. 5 shows a schematic view of a solution 10 according to the invention -3 mol/L NiSO 4 The slope curve of the immersed sample in the presence of a magnetic field to regulate Tafel is shown.
FIG. 6 shows a schematic view of a solution 10 according to the invention -2 mol/L NiSO 4 The slope curve of the Tafel is regulated and controlled in the presence of a magnetic field when a sample is soaked.
FIG. 7 shows a schematic view of a solution 10 according to the invention -1 mol/L NiSO 4 The slope curve of the Tafel is regulated and controlled in the presence of a magnetic field when a sample is soaked.
FIG. 8 shows a schematic view of a solution 10 according to the invention -3 mol/L NiSO 4 The EIS picture of the soaked sample is regulated and controlled in the presence of a magnetic field.
FIG. 9 shows a schematic view of a solution 10 according to the invention -2 mol/L NiSO 4 The soaked sample is subjected to EIS (electronic impedance spectroscopy) graph regulation and control without a magnetic field.
FIG. 10 shows a schematic view of a solution 10 according to the invention -1 mol/L NiSO 4 SoakingThe EIS picture of the sample is regulated and controlled in the presence of a magnetic field.
FIG. 11 is a graph showing the stability of the corrosion-treated foam iron under the control of a magnetic field according to the present invention.
Figure 12 is an XRD spectrum plot of samples treated at different concentrations in the present invention.
FIG. 13 is SEM pictures at 300, 10K, 60K magnification of samples treated with different concentrations in the present invention.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
Example 1: the method for regulating and controlling the surface magnetic field of the anode to obtain the ultra-strong industrial alkaline water oxygen evolution electrode utilizes the magnetic field to regulate and control the high-activity oxygen evolution electrode, and further enhances the oxygen evolution activity of the electrode.
The technological parameters are as follows: size of the foamed iron: 10mm × 5mm × 1mm; niSO 4 Concentration of aqueous solution: 10 -3 mol/L; soaking time: 24h; the soaking temperature is as follows: 25 deg.C
The preparation method comprises the following steps:
(1) The foam iron pieces were cut to a size of 10mm × 5mm × 1mm.
(2) And ultrasonically cleaning the cut foam iron sheet for 10min by using dilute hydrochloric acid, absolute ethyl alcohol and deionized water in sequence.
(3) Putting the cleaned foam iron sheet into the container 10 -3 mol/L of NiSO 4 Soaking and corroding for 24h.
(4) Taking out the foam iron sheet, washing off the surface solution by using absolute ethyl alcohol, and air-drying to be used as an oxygen evolution electrode.
(5) The OER test adopts a three-electrode system, a saturated calomel electrode is used as a reference electrode, and a platinum mesh is used as an auxiliary electrode. The electrolyte is 1mol/L KOH aqueous solution, the temperature is room temperature (25 ℃), in the test process, a magnet is immersed in the potassium hydroxide aqueous solution and is arranged on one side of an oxygen evolution electrode, as shown in a sample oxygen evolution process real object diagram under the regulation and control of a magnetic field shown in figure 1, the magnet is tightly close to one side of the oxygen evolution electrode, and an oxygen evolution phenomenon is generated on one side of the oxygen evolution electrode, namely oxygen is generated.
Example 2: the method for obtaining the super-strong industrial alkaline water oxygen evolution electrode by regulating and controlling the surface magnetic field of the anode utilizes the magnetic field to regulate and control the high-activity oxygen evolution electrode, and further enhances the oxygen evolution activity of the electrode.
The technological parameters are as follows: size of the foamed iron: 10mm × 5mm × 1mm; niSO 4 Concentration of aqueous solution: 10 -2 mol/L; soaking time: 9h; the soaking temperature is as follows: 25 deg.C
The preparation method comprises the following steps:
(1) The foam iron pieces were cut to a size of 10mm × 5mm × 1mm.
(2) And ultrasonically cleaning the cut foam iron sheet for 10min by using dilute hydrochloric acid, absolute ethyl alcohol and deionized water in sequence.
(3) Putting the cleaned foam iron sheet into the container 10 -2 mol/L of NiSO 4 Soaking and corroding for 9h.
(4) Taking out the foam iron sheet, washing the surface solution with absolute ethyl alcohol, and air-drying to obtain the final product for use as oxygen evolution electrode.
(5) The OER test adopts a three-electrode system, a saturated calomel electrode is used as a reference electrode, and a platinum mesh is used as an auxiliary electrode. The electrolyte was a 1mol/L KOH aqueous solution at room temperature (25 deg.C) and during the test the magnet was immersed in an aqueous potassium hydroxide solution and brought into proximity with the oxygen evolving electrode.
Example 3: the method for regulating and controlling the surface magnetic field of the anode to obtain the ultra-strong industrial alkaline water oxygen evolution electrode utilizes the magnetic field to regulate and control the high-activity oxygen evolution electrode, and further enhances the oxygen evolution activity of the electrode.
The technological parameters are as follows: size of the foamed iron: 10mm × 5mm × 1mm; niSO 4 Concentration of aqueous solution: 10 -1 mol/L; soaking time: 9h; the soaking temperature is as follows: 25 deg.C
The preparation method comprises the following steps:
(1) The foam iron pieces were cut to a size of 10mm × 5mm × 1mm.
(2) And ultrasonically cleaning the cut foam iron sheet for 10min by using dilute hydrochloric acid, absolute ethyl alcohol and deionized water in sequence.
(3) Putting the cleaned foam iron sheet into the container 10 -1 mol/L of NiSO 4 Soaking and corroding for 9 hours.
(4) Taking out the foam iron sheet, washing off the surface solution by using absolute ethyl alcohol, and air-drying to be used as an oxygen evolution electrode.
(5) The OER test adopts a three-electrode system, a saturated calomel electrode is used as a reference electrode, and a platinum mesh is used as an auxiliary electrode. The electrolyte was a 1mol/L KOH aqueous solution at room temperature (25 deg.C) and the magnet was immersed in an aqueous potassium hydroxide solution and brought into proximity to the oxygen evolving electrode during the test.
As can be seen from the OER CV curves of fig. 2, fig. 3, and fig. 4, when the potential is lower, the adjustment of the magnetic field does not significantly improve the OER activity of the sample soaked in the three concentrations. However, as the potential is increased, it is obvious that under the action of the magnetic field, the current density of the three samples is gradually increased compared with the condition without the magnetic field, and the slope of Tafel is significantly reduced, as shown in fig. 5, 6 and 7. The smaller the Tafel slope is, the faster the current density is increased, the smaller the overpotential change is, and the better the electrocatalytic performance of the material is. The concrete explanation is as follows: the OER reaction is a slow four-electron process requiring energy, the formation of O-O bonds must generate paramagnetic triplet ground state oxygen molecules through spin conservation, and the regulation and control of a magnetic field can limit spin, so that oxygen radicals can be favorably arranged in parallel on the surface of an electrode in the process of forming the O-O bonds, and the electrocatalytic performance of the material can be improved. On the other hand, at 10 -3 mol/L NiSO 4 The foamed iron sheet soaked in the solution for 24 hours is corroded to reach 200mA cm -2 The overpotential of the current density is 490mV, and the overpotential is reduced to 430mV after being regulated and controlled by a magnetic field; at 10 -2 mol/L NiSO 4 The foamed iron sheet is soaked in the solution for corrosion for 9 hours until the thickness reaches 200 mA-cm -2 The overpotential of the current density is 460mV, and the overpotential is reduced to 420mV after being regulated and controlled by a magnetic field; at 10 -1 mol/L NiSO 4 The foamed iron sheet is soaked in the solution for corrosion for 9 hours until the thickness reaches 200 mA-cm -2 The overpotential of the current density is 480mV, and the overpotential is reduced to 440mV after being regulated and controlled by a magnetic field. The above data indicate the use of NiSO 4 The soaked and corroded foam iron not only has high OER activity, but also can reduce the oxygen evolution overpotential to a great extent through the regulation and control of a magnetic field. Tafel slope and 200mA cm for the different samples described above -2 The overpotential of (2) is shown in the following table.
In addition, it can be seen from the EIS diagrams of the three samples that the EIS curves of the three samples are shifted forward compared with the EIS diagram of the sample without magnetic field regulation after the magnetic field regulation is added, as shown in fig. 8, 9 and 10. This indicates that the adjustment and control of the magnetic field can reduce the solution resistance and the internal resistance of the electrode, so that the OER activity of the material is improved. FIG. 11 is a graph of the stability of corrosion treated foam iron under magnetic field control, which was tested at 10mA cm -2 The potential of the sample has no obvious change after 100 hours, which shows that the sample has good stability.
FIG. 12 shows three different concentrations of NiSO 4 XRD pattern of solution-soaked treated foam iron. The XRD results show that besides XRD peaks of metallic iron and iron oxide, a group of XRD peaks with structural characteristics of LDHs (namely nickel-iron double metal hydroxide is formed on the foamed iron after nickel sulfate treatment) can be identified, but the intensity of the peaks gradually weakens with the increase of the solution concentration, probably because the solution concentration influences the crystallinity of the material.
FIG. 13 shows three different concentrations of NiSO 4 SEM images of solution-soaked foamed iron at 300, 10K and 60K magnifications. A1-A4 are foamed iron at 10 -3 mol/L of NiSO 4 SEM image of 24h of soaking corrosion; B1-B4 are foamed iron 10 - 2 mol/L of NiSO 4 SEM image of medium immersion corrosion for 9h; C1-C4 is foamed iron at 10 -1 mol/L NiSO 4 SEM image of medium immersion etching for 9h. A3, B3, C3 showed uniform LDH (i.e. nickel sulfate treated to form nickel-iron double metal hydroxide on foamed iron) nanosheet array films grown vertically across the entire iron plate surface with a large number of voids between the nanosheets.
The self-supporting anode can be prepared by adjusting the process parameters according to the content of the invention, and the self-supporting anode shows the performance basically consistent with the invention through tests. The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (2)
1. A method for obtaining an ultra-strong industrial alkaline water oxygen evolution electrode by regulating and controlling a magnetic field on the surface of an anode is characterized in that foamed iron is placed in a nickel sulfate aqueous solution for treatment, a nickel-iron bimetal hydroxide nanosheet array film formed on the foamed iron vertically grows on the surface of the whole iron plate, and a large number of gaps are formed among the nanosheets; the foamed iron treated by the nickel sulfate is used as an oxygen evolution electrode, and the magnet is placed in an alkaline solution and is arranged on one side of the oxygen evolution electrode;
the alkaline solution is 1mol/LKOH or NaOH aqueous solution;
the magnet is arranged in the alkaline solution and close to the oxygen evolution electrode;
the concentration of nickel sulfate is 10 -1 -10 -3 mol/L, the treatment temperature is 20-25 ℃, and the treatment time is 9-24 hours.
2. The method for obtaining the ultra-strong industrial alkaline water oxygen evolution electrode by regulating and controlling the surface magnetic field of the anode according to claim 1, wherein a saturated calomel electrode is used as a reference electrode, and a platinum mesh is used as an auxiliary electrode.
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