CN116005192A - Ferronickel oxyhydroxide oxygen evolution electrode and preparation method thereof - Google Patents
Ferronickel oxyhydroxide oxygen evolution electrode and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a ferronickel oxyhydroxide oxygen evolution electrode and a preparation method thereof, and relates to the field of water electrolysis hydrogen production. The electrode consists of a conductive substrate and ferronickel oxyhydroxide from which high-valence metals are removed. According to the method, a nickel-iron M composite oxide grows in situ on a conductive substrate through hydrothermal reaction of nickel salt, ferric salt and high-valence metal M salt (M=chromium, molybdenum and tungsten), then high-valence metal M element in the nickel-iron M composite oxide is removed through an electrochemical method in a positive potential anodic oxidation process, and further crystal phase and valence state change of the nickel-iron composite oxide are realized, and a nickel-iron oxyhydroxide oxygen evolution electrode is formed. In the invention, the ferronickel M composite oxide generated by hydrothermal reaction provides a ferronickel element library for forming ferronickel oxyhydroxide, and a large number of oxygen-evolving active sites are exposed after high-valence metal elements are removed, so that the oxygen-evolving electrode of the ferronickel oxyhydroxide with rich defects and high activity is formed, and the ferronickel composite oxide can be used in the field of hydrogen production by water electrolysis.
Description
Technical Field
The invention belongs to the field of hydrogen production by water electrolysis, and particularly relates to a ferronickel oxyhydroxide oxygen evolution electrode and a preparation method thereof.
Background
In recent years, the problems of energy exhaustion and environmental pollution caused by the large-scale use of fossil energy are increasingly serious, and the demand of human beings for renewable clean energy is more urgent. Hydrogen energy is widely known as a highly efficient clean energy source. The hydrogen energy is a green energy source with zero carbon emission, has the characteristics of maximum specific heat capacity and reproducibility, and can be used for a hydrogen fuel cell so as to convert the hydrogen energy into heat energy for utilization. The hydrogen production by water electrolysis has continuity and environmental protection, is a late-onset elegance of the hydrogen energy industry, and has unlimited potential. High purity hydrogen and oxygen can be produced to replace fossil fuels to provide energy. The electrolyzed water reaction consists of two half reactions, namely a Hydrogen Evolution Reaction (HER) and an Oxygen Evolution Reaction (OER), wherein in the oxygen evolution reaction, the four electron transfer process required for the cleavage of the O-H bond and the formation of the O-O bond is kinetically slow, so that a catalyst for the reaction is required to reduce the reaction energy barrier and the cost.
OER reaction catalyst uses noble metal catalyst RuO 2 、IrO 2 As a representative, excellent electrocatalytic activity and stability are exhibited. However, the high cost and low reserves of Ru and Ir limit the wide application of the Ru and Ir in the field of hydrogen production by water electrolysis. For this reason, a large number of researchers have focused on the study of non-noble metals, particularly nickel and nickel-based composite metals. In the nickel-based OER catalyst, nickel-iron composite hydroxide (NiFe-LDH), nickel-molybdenum composite oxide and the like show better OER activity. The invention patent CN202210500972.1 discloses a preparation method and application of a transition metal sulfide composite hydroxide electrode, wherein non-metal sulfur doping is carried out on NiFe-LDH to form sulfides and hydroxides, and regulation and control are carried outThe oxygen evolution activity is high. However, the sulfide is unstable in the OER reaction process, and the sulfide is easy to deactivate the cathode electrode catalyst, so that the electrolytic water performance is attenuated. Patent CN201911249955.X discloses a preparation method and application of a 3D nano-sheet-nano-rod mixed structure nickel-molybdenum oxide, wherein a mixed structure is constructed by using high-valence metal molybdenum element to form the nickel-molybdenum oxide, and the nickel-molybdenum oxide has good performance. But such nickel molybdenum-based oxides have general catalytic properties compared to nickel iron catalysts.
In summary, no nickel iron oxyhydroxide electrode with rich defects and high activity is reported to be formed after removing high-valence M metal elements in NiFeM composite oxides.
Disclosure of Invention
In order to overcome the defects and drawbacks mentioned in the background art, one of the purposes of the present invention is to provide a ferronickel oxyhydroxide oxygen evolution electrode.
In order to achieve the above purpose, the invention adopts the following technical scheme: and growing the ferronickel M composite oxide on the conductive substrate in situ by a hydrothermal method, and removing high-valence metal elements by an electrochemical method to form the ferronickel oxyhydroxide oxygen evolution electrode.
The second purpose of the invention is to provide a preparation method of the ferronickel oxyhydroxide oxygen evolution electrode, which comprises the following specific operation methods:
(1) Pre-treating the conductive substrate by acid washing, water washing and ethanol washing, and then drying in an oven for later use;
(2) Preparing a nickel-iron M metal salt solution. The nickel salt comprises at least one of nickel nitrate, nickel chloride and nickel sulfate; the ferric salt comprises at least one of ferric nitrate, ferric chloride and ferric sulfate; the high-valence metal salt comprises at least one of sodium chromate, sodium molybdate, ammonium molybdate and sodium tungstate; the molar concentration ratio of nickel to iron to M is (1-20): (0.1-5): (0.2-50), and the pH value is regulated to be below 3.5 by using acid;
(3) Transferring the solution into a polytetrafluoroethylene reaction kettle, adding a treated conductive substrate, performing hydrothermal reaction for 3-24 hours at 80-200 ℃, repeatedly washing the substrate with ultrapure water after the substrate is naturally cooled to room temperature, and drying the substrate in a vacuum oven at 40-100 ℃ for 2-24 hours to obtain a ferronickel M composite oxide electrode grown in situ on the conductive substrate;
(4) And (3) taking the in-situ grown ferronickel M composite oxide electrode on the obtained conductive substrate as a working electrode, taking a Ni net and titanium ruthenium commercial electrode which are stable in alkaline solution as an auxiliary electrode, removing high-valence metal in alkaline solution (0.1-10M KOH+0.01-0.5M NaCl) with chloride ions through a periodic double-current step method, performing electrochemical reaction for 0.1-2h, repeatedly cleaning by using ultrapure water, and drying for 2-24 h at 40-100 ℃ in a vacuum oven to obtain the ferronickel oxyhydroxide oxygen evolution electrode.
Preferably, the conductive substrate of step (1) is selected from nickel foam (surface density 380-420 g m -2 Porosity 98%).
Preferably, in the step (2), the nickel salt is nickel nitrate, the iron salt is ferric chloride, the high-valence metal salt is sodium molybdate, and the acid used is nitric acid.
Preferably, the reaction temperature of the hydrothermal reaction in the step (3) is 150 ℃, the reaction time is 6 hours, the drying temperature is 70-80 ℃, and the drying time is 6-9 hours.
Preferably, the alkali solution with chloride ions in the step (4) is 6M KOH+0.01M NaCl, the temperature is 60 ℃, and the current density in the first stage of the periodic double current step method is 0.5A/cm 2 The current density in the second stage is 0A/cm 2 Each stage lasted 1min with a cycle number of 10.
Preferably, the drying temperature in the step (4) is 70-80 ℃, and the drying time is 4-6 h.
The invention provides a ferronickel oxyhydroxide oxygen evolution electrode which can be applied to hydrogen production by alkaline water electrolysis. Compared with the prior art, the invention has the following technical advantages:
(1) The medicine used by the nickel-iron oxyhydroxide electrode does not contain noble metal-based medicine, has large medicine storage capacity and is convenient to purchase;
(2) The nickel iron oxyhydroxide electrode has excellent durability at 50 ℃ and 6 DEG CIn a mol/L KOH electrolyte at 100mA cm -2 The constant current test is carried out for 100 hours, and the long-term stability is good, so that the constant current test has great application potential in water electrolysis;
(3) The OER activity of the nickel-iron oxyhydroxide electrode is obviously better than that of noble metal and non-noble metal catalysts reported in the current research, and the activity is better than that of commercial IrO 2 Is a catalyst activity of (a). 10mA cm at 1M KOH at 27 ℃ -2 The time overpotential is less than 200mV;
(4) The preparation method of the ferronickel oxyhydroxide electrode is simple, easy to operate and convenient for large-scale production.
Drawings
FIG. 1 is an X-ray diffraction pattern (XRD) of a nickel iron oxyhydroxide oxygen evolution electrode obtained in example 1 before and after removal of high-valence metals.
FIG. 2 is an X-ray photoelectron spectroscopy analysis (XPS) of the Mo3d orbitals before and after removal of high valence metals by a nickel iron oxyhydroxide oxygen evolution electrode obtained in example 1.
FIG. 3 is a Scanning Electron Microscope (SEM) image of the nickel iron oxyhydroxide oxygen evolution electrode of example 1 after removal of the higher metals.
FIG. 4 is a linear sweep voltammogram of one of the nickel iron oxyhydroxide electrodes obtained in example 1 at 27℃with 1M KOH.
Detailed Description
The present invention will be described more fully hereinafter with reference to the accompanying drawings, in which preferred embodiments are shown, for the purpose of illustrating the invention, but the scope of the invention is not limited to the specific embodiments shown.
The technical scheme of the invention will be further described with reference to specific examples.
Example 1:
cutting a foam nickel substrate into pieces with the specification of 3.8cm multiplied by 4cm, putting the cut foam nickel substrate into absolute ethyl alcohol, carrying out ultrasonic treatment for 20 minutes, then putting the cut foam nickel substrate into 1mol/L hydrochloric acid for ultrasonic treatment for 10 minutes, then putting the cut foam nickel substrate into ultrapure water for ultrasonic treatment for 20 minutes, and repeatedly flushing the cut foam nickel substrate with the ultrapure water three times after each stage of ultrasonic treatment. Then placing the mixture into absolute ethyl alcohol, carrying out ultrasonic treatment for 5 minutes, taking out and drying at normal temperature for later use;
ni (NO) with the molar concentration ratio of nickel, iron and molybdenum of 1:0.33:3 is prepared 3 ) 2 ·6H 2 O、FeCl 3 And Na (Na) 2 MoO 4 Adjusting the pH of the system to below 3.5 by using nitric acid; transferring the solution into a 100mL polytetrafluoroethylene reaction kettle, adding a piece of treated foam nickel, carrying out hydrothermal reaction for 6 hours at 150 ℃, naturally cooling to room temperature, repeatedly washing with ultrapure water, putting into a baking oven, drying at 70 ℃ for 9 hours to obtain a nickel-iron-molybdenum oxide electrode growing on the foam nickel in situ, and marking as NiFeMoO 4 /NF。
The obtained NiFeMoO 4 The NF is subjected to a periodic double-current step method at 60 ℃ and 6M KOH+0.01M NaCl to remove the high-valence metal. By NiFeMoO 4 The NF is a working electrode, a Ni net and a titanium ruthenium commercial electrode which are stable in alkaline solution are used as auxiliary electrodes, and the current density in the first stage is 0.5A/cm 2 The current density in the second stage is 0A/cm 2 Each stage lasts for 1min, after 10 cycles of circulation, ultrapure water is used for repeated cleaning, and the mixture is put into a vacuum oven for drying at 70 ℃ for 6 hours, so that the ferronickel oxyhydroxide oxygen evolution electrode which is recorded as NiFeOOH/NF is obtained.
The NiFeOOH/NF prepared by the method is used for electrocatalytic oxygen evolution reaction, and comprises the following specific steps: constructing a three-electrode system, wherein the working electrode is a NiFeOOH/NF electrode, the reference electrode is a mercury/mercuric chloride electrode, and the counter electrode is a titanium ruthenium electrode. OER Performance in an oxygen-saturated 1mol/L Potassium hydroxide solution, 10mA cm -2 The time overpotential was only 145mV (data were not resistance compensated).
Structural analysis
FIG. 1 shows X-ray diffraction patterns (XRD) of a nickel iron oxyhydroxide oxygen evolution electrode obtained in example 1 before and after removal of high-valence metals. As shown in FIG. 1, after electrochemical removal of the higher metals, niMoO 4 And Fe (Fe) 2 (MoO 4 ) 3 The characteristic peaks of (2) basically disappear, and new characteristic peaks of NiOOH and FeOOH appear.
FIG. 2 shows the X-ray photoelectron spectroscopy (XPS) of the Mo3d orbitals before and after removal of the high valence metal by the ferronickel oxyhydroxide oxygen evolution electrode obtained in example 1, wherein the characteristic peak of the high valence metal molybdenum is basically disappeared.
FIG. 3 shows a Scanning Electron Micrograph (SEM) of a nickel iron oxyhydroxide oxygen evolution electrode obtained in example 1, the NiFeOOH/NF electrode consisted of micropillars and the surface of the micropillars was roughened by removal of high valence metal. The structure increases the electrochemical activity specific surface area of the catalyst, increases the number of active sites, and effectively improves the electrocatalytic performance of the catalyst.
FIG. 4 is a linear voltammetric image of an OER scan taken in 1M potassium hydroxide electrolyte at a scan rate of 5mV/s for a nickel iron oxyhydroxide oxygen evolution electrode obtained in example 1, 10mA cm -2 The time overpotential was only 145mV (data were not resistance compensated).
Example 2:
cutting a foam nickel substrate into pieces with the specification of 10cm multiplied by 10cm, putting the cut foam nickel substrate into absolute ethyl alcohol, carrying out ultrasonic treatment for 20 minutes, then putting the cut foam nickel substrate into 1mol/L hydrochloric acid for ultrasonic treatment for 10 minutes, then putting the cut foam nickel substrate into ultrapure water for ultrasonic treatment for 20 minutes, and repeatedly flushing the cut foam nickel substrate with the ultrapure water three times after each stage of ultrasonic treatment. Then placing the mixture into absolute ethyl alcohol, carrying out ultrasonic treatment for 5 minutes, taking out and drying at normal temperature for later use;
ni (NO) was formulated at a molar concentration ratio of nickel, iron, molybdenum of 1:0.33:0.5 3 ) 2 ·6H 2 O、FeCl 3 And (NH) 4 ) 6 Mo 7 O 24 ·4H 2 A mixed solution of O; transferring the solution into a 500mL polytetrafluoroethylene reaction kettle, adding a piece of treated foam nickel with the specification of 10cm multiplied by 10cm, performing hydrothermal reaction for 6 hours at 150 ℃, naturally cooling to room temperature, repeatedly washing with ultrapure water, putting into a baking oven, drying at 70 ℃ for 9 hours to obtain a nickel-iron-molybdenum oxide electrode growing on the foam nickel in situ, and marking as NiFeMoO 4 /NF。
The obtained NiFeMoO 4 The NF is subjected to a periodic double-current step method at 60 ℃ and 6M KOH+0.01M NaCl to remove the high-valence metal. To be used forNiFeMoO 4 The NF is a working electrode, a Ni net and a titanium ruthenium commercial electrode which are stable in alkaline solution are used as auxiliary electrodes, and the current density in the first stage is 0.1A/cm 2 The current density in the second stage is 0A/cm 2 Each stage lasts for 0.5min, after 20 cycles, ultrapure water is used for repeatedly cleaning, and the mixture is put into a vacuum oven for drying at 70 ℃ for 6 hours, so that the ferronickel oxyhydroxide oxygen evolution electrode is obtained and is marked as NiFeOOH/NF.
The NiFeOOH/NF prepared by the method is used for electrocatalytic oxygen evolution reaction, and comprises the following specific steps: constructing a three-electrode system, wherein the working electrode is a NiFeOOH/NF electrode, the reference electrode is a mercury/mercuric chloride electrode, and the counter electrode is a titanium ruthenium electrode. OER Performance in an oxygen-saturated 1mol/L Potassium hydroxide solution, 10mA cm -2 The time overpotential was 180mV (data were not resistance compensated).
Example 3:
the same procedure as in example 1 was followed except that Ni (NO) was used in a molar concentration ratio of 1:0.25:10 for hydrothermal reaction 3 ) 2 ·6H 2 O、Fe(NO 3 ) 3 And Na (Na) 2 WO 4 Is a mixed solution of (a) and (b). OER Performance in an oxygen-saturated 1mol/L Potassium hydroxide solution, 10mA cm -2 The time overpotential was 240mV (data was not resistance compensated).
Example 4:
the same procedure as in example 1 was followed except that Ni (NO) was used in a molar concentration ratio of 1:0.5:1.25 for hydrothermal reaction 3 ) 2 ·6H 2 O、Fe(NO 3 ) 3 And Na (Na) 2 CrO 4 Is a mixed solution of (a) and (b). OER Performance in an oxygen-saturated 1mol/L Potassium hydroxide solution, 10mA cm -2 The time overpotential was 250mV (data were not resistance compensated).
The above is only a preferred embodiment of the present invention, and the scope of the present invention is not limited to the above examples, but various process schemes without substantial differences from the inventive concept are within the scope of the present invention.
Claims (5)
1. The ferronickel oxyhydroxide oxygen-evolving electrode is characterized in that high-valence metal M elements in ferronickel M (M=chromium, molybdenum and tungsten) composite oxides grown in situ on a conductive substrate are removed, so that the ferronickel oxyhydroxide oxygen-evolving electrode with rich defects and high activity is formed. The preparation method of the ferronickel oxyhydroxide oxygen evolution electrode comprises the following steps:
(1) Pre-treating the conductive substrate by acid washing, water washing and ethanol washing, and then drying in an oven for later use;
(2) Preparing nickel, iron and M metal salt solution to a molar concentration ratio of (1-20) (0.1-5) (0.2-50), and regulating pH to below 3.5 with acid;
(3) Transferring the solution into a polytetrafluoroethylene reaction kettle, adding a treated conductive substrate, carrying out hydrothermal reaction in an oven at 80-200 ℃ for 3-24 hours, naturally cooling, cleaning, and then drying in a vacuum oven at 40-100 ℃ for 2-24 hours to obtain a nickel-iron M composite oxide electrode growing in situ on a metal substrate;
(4) And (3) removing high-valence metal from the obtained ferronickel M composite oxide electrode in alkali liquor with chloride ions by using an electrochemical method, repeatedly cleaning by using ultrapure water after electrochemical reaction for 0.1-2 hours, and drying for 2-24 hours at 40-100 ℃ in a vacuum oven to obtain the ferronickel oxyhydroxide oxygen evolution electrode.
2. The ferronickel oxyhydroxide oxygen evolution electrode of claim 1, wherein: the conductive substrate comprises foam metal, braided metal and carbon-based material; the nickel salt comprises at least one of nickel nitrate, nickel chloride and nickel sulfate; the ferric salt comprises at least one of ferric nitrate, ferric chloride and ferric sulfate; the M salt comprises at least one of sodium chromate, ammonium molybdate, sodium molybdate and sodium tungstate.
3. The ferronickel oxyhydroxide oxygen evolution electrode of claim 1, wherein: when the electrochemical removal of high-valence metals, the in-situ grown nickel-iron-M composite oxide electrode is used as a working electrode, a Ni net and titanium-ruthenium commercial electrode which are stable in alkaline solution are used as auxiliary electrodes, and the electrochemical removal of the high-valence metals is carried out by a periodic double-current step method in the electrolyte with the temperature of 27-90 ℃ and the concentration of 0.1-10M KOH+0.01-0.5M NaCl.
4. The ferronickel oxyhydroxide oxygen evolution electrode of claim 1, wherein: in the periodic double-current step method for electrochemically removing M element, the current density in the first stage is 0.01-0.5A/cm 2 The current density in the second stage is 0A/cm 2 Each stage lasts for 0.1-5min, and the period number is 5-40.
5. A ferronickel oxyhydroxide oxygen evolution electrode according to claim 1, characterized by the use of the ferronickel oxyhydroxide oxygen evolution electrode in the field of hydrogen production by electrolysis of water.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116334673A (en) * | 2023-05-30 | 2023-06-27 | 中石油深圳新能源研究院有限公司 | Nickel-based catalyst and preparation method and application thereof |
| CN117845257A (en) * | 2024-03-07 | 2024-04-09 | 汕头大学 | NiFeMO-containing material x Ni-based self-supporting electrode of electrocatalyst and preparation and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116334673A (en) * | 2023-05-30 | 2023-06-27 | 中石油深圳新能源研究院有限公司 | Nickel-based catalyst and preparation method and application thereof |
| CN116334673B (en) * | 2023-05-30 | 2023-09-05 | 中石油深圳新能源研究院有限公司 | Nickel-based catalyst and preparation method and application thereof |
| CN117845257A (en) * | 2024-03-07 | 2024-04-09 | 汕头大学 | NiFeMO-containing material x Ni-based self-supporting electrode of electrocatalyst and preparation and application thereof |
| CN117845257B (en) * | 2024-03-07 | 2024-05-07 | 汕头大学 | Ni-based self-supporting electrode containing NiFeMOx electrocatalyst and preparation and application thereof |
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