CN114959791A - Preparation method of Mg-doped NiFe-based (oxy) hydroxide and oxygen evolution electrocatalysis application thereof - Google Patents
Preparation method of Mg-doped NiFe-based (oxy) hydroxide and oxygen evolution electrocatalysis application thereof Download PDFInfo
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- JSPLKZUTYZBBKA-UHFFFAOYSA-N trioxidane Chemical compound OOO JSPLKZUTYZBBKA-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 title claims abstract description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000001301 oxygen Substances 0.000 title claims abstract description 19
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title abstract description 7
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- 229910052742 iron Inorganic materials 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
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- 229910052751 metal Inorganic materials 0.000 claims description 4
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- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 239000010411 electrocatalyst Substances 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
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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
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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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- 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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- 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
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/054—Electrodes comprising electrocatalysts supported on a carrier
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
Abstract
The invention relates to a preparation method of Mg-doped NiFe-based (oxy) hydroxide and oxygen evolution electrocatalysis application thereof. The method comprises the following steps: mixing MgCl 2 、NiCl 2 ·6H 2 Dissolving O in deionized water, and stirring to obtain mixed solution. Immersing the processed foam iron in the mixed solution, stirring, cleaning and drying to obtain Mg-doped NiFe-based (oxy) hydroxide; the method comprises the steps of designing Mg-doped NiFe-based (oxy) hydroxide with a nanosheet structure by using foamed iron as a substrate and a one-step corrosion method; the nano-sheet structure can be increasedThe specific surface area of the catalyst provides more active sites, and enhances electron transfer in the electrocatalytic process. The preparation method is simple and convenient, is easy to operate, and the Mg doping ensures that the catalyst obtains better stability and better inherent electrocatalytic activity.
Description
Technical Field
The invention belongs to the field of electrocatalysis, and relates to a preparation method of Mg-doped NiFe-based (oxy) hydroxide and application of oxygen evolution electrocatalysis.
Background
At present, the development of clean and efficient renewable energy sources to replace traditional fossil energy sources has great significance on the sustainable development of economy in China. The hydrogen energy is the most ideal clean energy at present due to the advantages of high combustion heat value, no toxicity, no harm, wide sources and the like. Among them, electrocatalytic water decomposition is one of the more desirable methods for exploiting hydrogen energy. Overall water splitting is composed of two half-reactions, namely the Hydrogen Evolution Reaction (HER) and the Oxygen Evolution Reaction (OER). Hydrogen evolution reaction (2H) 2 O+2e - →H 2 +2OH - ) And oxygen evolution reaction (4 OH) - →O 2 +2H 2 O+4e - ) There are problems such as slow kinetics, in particular oxygen evolution reactions, which require more energy consumption due to the transfer of 4 electrons involved. The high-efficiency catalyst can reduce overpotential, thereby improving the conversion efficiency of energy. At present, noble metals and their oxides (Pt, RuO) 2 And IrO 2 Etc.) are the most effective catalysts, but they are expensive and scarce and have been greatly limited in large-scale industrial application. In alkaline environment, transition metals (such as Ni, Co and Fe-based heterostructures) have high electrocatalytic activity theoretically and low cost, and can be proved to be effective non-noble metal electrocatalysts. However, the non-noble metal catalyst has a problem of low reaction efficiency instead of the noble metal catalyst, and it is very critical to improve the catalytic performance.
NiFe-based (oxy) hydroxides are a potential OER catalyst with controllable type and ratio of metal cations and with mobility and interchangeability of anions in the structure. The synergy between the oxide and the hydroxide enables the NiFe-based (oxy) hydroxide to have better OER performance. However, their intrinsic conductivity is poor, and powder materials are prone to structural curling and stacking during testing, which is detrimental to electron transfer and active site exposure during electrocatalysis. Effective metal atom doping can expose more active sites of the catalyst, optimize an electronic structure and optimize the adsorption of a reaction intermediate, so that the energy barrier of the reaction is reduced, and the intrinsic activity of the OER electrocatalyst is improved. Therefore, the design of the high-performance oxygen evolution electrocatalyst has important significance.
Disclosure of Invention
The invention aims to provide a preparation method of Mg-doped NiFe-based (oxy) hydroxide and oxygen evolution electrocatalysis application thereof, aiming at the problem that the catalytic activity of the NiFe-based (oxy) hydroxide needs to be further improved. The foamed iron is used as a substrate, and Mg-doped NiFe-based (oxy) hydroxide with a nanosheet structure is designed through a one-step corrosion method. The nano-sheet structure can increase the specific surface area of the catalyst, provide more active sites and enhance the electron transfer in the electrocatalysis process. The preparation method is simple and convenient, is easy to operate, and the Mg doping ensures that the catalyst obtains better stability and better inherent electrocatalytic activity.
The technical scheme of the invention is as follows:
a method for preparing Mg-doped NiFe-based (oxy) hydroxide, comprising the steps of:
(1) cleaning the foamed iron material: cutting the foam iron into 1 × 1.5cm 2 And (3) carrying out ultrasonic treatment on the small pieces in hydrochloric acid, then washing the small pieces with deionized water and ethanol, carrying out ultrasonic treatment in an ultrasonic machine for 8-10 min, and then drying the small pieces in a vacuum drying oven, wherein the acid is 1-3 mol/L hydrochloric acid.
(2) Mixing MgCl 2 、NiCl 2 ·6H 2 Dissolving O in deionized water, and stirring uniformly to obtain a mixed solution; and immersing the foamed iron in the mixed solution, stirring for 2-4 h, cleaning and drying to obtain the Mg-doped NiFe-based (oxy) hydroxide.
Wherein, Mg: the molar ratio of Ni is 1-3: 0.5 to 1; the total metal concentration of the mixed solution is 0.5-1 mol/L;
the application of the Mg-doped NiFe-based (oxy) hydroxide prepared by the method is used for electrocatalytic oxygen evolution reaction. The raw materials involved therein are all commercially available.
The invention has the beneficial effects that:
1) the nanosheet structure of the catalyst provides abundant mass transfer channels, increases active sites, and is beneficial to gas diffusion and electrolyte transmission.
2) The combination of NiFe-based (oxy) hydroxide with a conductive substrate to build a 3D self-supporting electrocatalyst can enhance the conductivity of the catalyst.
3) Suitable Mg doping gives better stability and higher intrinsic activity to the catalyst.
4) From a linear scan of the oxygen evolution reaction measured, it can be seen at 100mA cm -2 The overpotential of the lower Mg-doped NiFe-based (oxy) hydroxide catalyst was 330 mV. When not doped with Mg, the overpotential of the catalyst is 450 mV. Therefore, the Mg doping can show higher catalytic activity and can be well applied to high-activity oxygen evolution reaction catalysts. And at 100mA cm -2 Under the current density of the electrode, after a long-term durability test for 50 hours, the potential change of the electrode can be ignored, and the electrode has wide application prospect in the future energy industry.
Drawings
FIG. 1 is an SEM photograph of Mg-Ni/FF obtained in example 1.
FIG. 2 is a TEM image of Mg-Ni/FF obtained in example 1.
FIG. 3 is an X-ray diffraction chart of Mg-Ni/FF obtained in example 1.
FIG. 4 is an X-ray diffraction chart of Ni/FF obtained in example 2.
FIG. 5 is a graph of the Linear Scanning (LSV) of the Oxygen Evolution Reaction (OER) of Mg-Ni/FF, Ni/FF, Mg/FF, pure foam iron (FF) and commercial Ir/C obtained in examples 1 to 3 in an alkaline electrolyte.
FIG. 6 is a bar graph of overpotentials of Mg-Ni/FF, Ni/FF, Mg/FF, pure foam iron (FF) and commercial Ir/C obtained in examples 1-3 at different current densities.
FIG. 7 shows the Mg-Ni/FF ratio at 100mA cm obtained in example 1 -2 At a current density of (a), a long-term durability test of 50 hours was passed.
FIG. 8 is a graph of the Linear Sweep (LSV) of Oxygen Evolution Reaction (OER) in alkaline electrolyte for catalysts doped with different Mg contents (Mg contents 11mmol, 15mmol, 22mmol, respectively) in example 1, example 4, and example 5.
Detailed Description
The invention is described in more detail below with reference to specific examples, without limiting the scope of the invention.
Example 1:
(1) treatment of foamed iron
Mixing 1X 1.5cm 2 And (3) placing foamed iron (the porosity is 60-98%, the porosity is more than or equal to 98%, and the purity is 99.99%) with the thickness of 1mm in 3mol/L hydrochloric acid for ultrasonic treatment for 10min, removing an oxide layer, then washing with deionized water and ethanol, and drying.
(2) 1.428g of MgCl 2 (15mmol)，2.05g NiCl 2 ·6H 2 Dissolving O (7.5mmol) in 30mL of deionized water, and magnetically stirring at room temperature for 5min to dissolve the O into a uniform solution; immersing the foamed iron treated in the step (1) in the mixed solution, stirring for 2.5h, then washing off attachments on the catalyst by using water, and then drying in a vacuum oven.
The Mg-Ni/FF prepared in example 1 is characterized by using characterization means such as TEM, SEM and XRD. The microstructure of the electrocatalyst was studied by scanning electron microscopy (SEM, Quanta450FEG) and TEM (JEOL 2010F). Their crystal structures were investigated by X-ray diffraction (XRD, D8 Discovery). In a standard three-electrode system, the electrolysis reaction was measured using a CORRTESTCS2350 electrochemical workstation, with Mg-Ni/FF as the working electrode, a carbon rod as the counter electrode, a Saturated Calomel Electrode (SCE) as the reference electrode, and an electrolyte of 1mol KOH. The curve detection range of Linear Sweep Voltammetry (LSV) is 0-1V (relative to saturated calomel), and the sweep rate is 10mV s -1 According to E RHE ＝E Hg/HgCl +0.242+0.059pH converts the potential vs. hg/HgCl to the potential vs. standard hydrogen electrode (RHE).
As can be seen from the SEM and TEM images of FIGS. 1 and 2, the prepared Mg-Ni/FF is of a nanosheet structure, the active surface area of the catalyst is increased, the charge transfer is accelerated, and the oxygen evolution reaction is facilitated. From the XRD pattern of FIG. 3, it can be seen that Mg-Ni/FF is associated with NiFe-LDH (PDF #34-0205), FeOOH (PDF #18-0639) and Fe, respectively 2 O 3 The standard cards of (PDF #25-1402) are in agreement, indicating the successful synthesis of NiFe-based (oxy) hydroxides.
Example 2:
(1) treatment of foamed iron
Mixing 1X 1.5cm 2 And putting the foamed iron with the thickness of 1mm into 3mol/L hydrochloric acid for ultrasonic treatment for 10min, removing an oxide layer, then washing with deionized water and ethanol, and drying.
(2) 2.05g of NiCl 2 ·6H 2 Dissolving O (7.5mmol) in 30mL of deionized water, and magnetically stirring at room temperature for 5min to dissolve the O into a uniform solution; immersing the foamed iron treated in the step (1) in the mixed solution, stirring for 2.5h, then washing off attachments on the catalyst by using water, and then drying in a vacuum oven.
From the XRD pattern of FIG. 4, it can be seen that Ni/FF is associated with FeOOH (PDF #18-0639) and Fe, respectively 2 O 3 The standard cards of (PDF #25-1402) are identical. The 100mA overpotential of 450mV can be obtained by the LSV graph in FIG. 5.
The overpotential of Mg-Ni/FF is higher than that of Ni/FF, so that the doping of Mg improves the OER performance of the catalyst.
Example 3:
(1) treatment of foamed iron
Mixing 1X 1.5cm 2 The foamed iron with the thickness of 1mm is placed in 3mol/L hydrochloric acid for ultrasonic treatment for 10min, an oxidation layer is removed, and then deionized water and ethanol are used for washing and drying.
(2) 1.428g of MgCl 2 (15mmol) is dissolved in 30mL deionized water, and the solution is dissolved into uniform solution by magnetic stirring for 5min at room temperature; immersing the foamed iron treated in the step (1) in the mixed solution, stirring for 2.5h, then washing off attachments on the catalyst by using water, and then drying in a vacuum oven.
FIG. 5 is a LSV curve of examples 1-3, and it can be seen that the Mg-doped NiFe-based (oxy) hydroxide (example 1) has higher performance than the Mg-undoped or Mg-only doped catalysts (examples 2-3) under the premise of using foamed iron as a substrate. Comparing the Mg-Ni/FF catalyst obtained in example 1 with the Ni/FF catalyst obtained in example 2 without doping Mg element, the doping of Mg element can improve the performance of the catalyst. In connection with example 3, it is demonstrated that the synergy between MgNiFe-based (oxy) hydroxides together have a promoting effect on the electrocatalytic properties of the oxygen evolution reaction.
FIG. 6 is a histogram of overpotentials of Mg-Ni/FF, Ni/FF, Mg/FF, FF and commercial Ir/C obtained in examples 1-3 at different current densities, which shows that Mg-Ni/FF has a lower overpotential, exhibits the highest electrocatalytic activity and is beneficial to the reaction, and overpotentials of Ni/FF, Mg/FF, FF and commercial Ir/C at different current densities are all greater than that of Mg-Ni/FF. When the current density is 10mA cm -2 The OER overpotential on Mg-Ni/FF was 189 mV. And the overpotential of Ni/FF lacking Mg is higher, which shows that the doping of Mg plays a certain role in improving the OER catalytic performance. In a standard three-electrode system, the electrolysis reaction was measured using a corrtescs 2350 electrochemical workstation, with Mg-Ni/FF as working electrode, a carbon rod as counter electrode, a Saturated Calomel Electrode (SCE) as reference electrode, and an electrolyte of 1mol KOH (pH 13.7). The curve detection range of Linear Sweep Voltammetry (LSV) is 0-1V (relative to saturated calomel), and the sweep rate is 10mV s -1 . According to E RHE ＝E Hg/HgCl +0.242+0.059pH the potential vs. Hg/HgCl is converted to a potential vs. standard hydrogen electrode (RHE)
FIG. 7 shows the Mg-Ni/FF ratio at 100mA cm obtained in example 1 -2 At a current density of (a), a long-term durability test of 50 hours was passed. It can be seen from the figure that the potential change of the electrode is negligible, indicating that Mg-Ni/FF has better stability.
Example 4:
(1) treatment of foamed iron
Mixing 1X 1.5cm 2 And putting the foamed iron with the thickness of 1mm into 3mol/L hydrochloric acid for ultrasonic treatment for 10min, removing an oxide layer, then washing with deionized water and ethanol, and drying.
(2) 1.07g of MgCl 2 (11mmol)，2.05g NiCl 2 ·6H 2 Dissolving O (7.5mmol) in 30mL deionized water, and magnetically stirring at room temperature for 5min to obtain a uniform solution; immersing the foamed iron treated in the step (1) in the mixed solution, stirring for 2.5h, then washing off attachments on the catalyst by using water, and then drying in a vacuum oven.
Example 5:
(1) treatment of foamed iron
Mixing 1X 1.5cm 2 The foamed iron with the thickness of 1mm is placed in 3mol/L hydrochloric acid for ultrasonic treatment for 10min, an oxidation layer is removed, and then deionized water and ethanol are used for washing and drying.
(2) 2.14g of MgCl 2 (22mmol)，2.05g NiCl 2 ·6H 2 Dissolving O (7.5mmol) in 30mL deionized water, and magnetically stirring at room temperature for 5min to obtain a uniform solution; immersing the foamed iron treated in the step (1) in the mixed solution, stirring for 2.5h, then washing off attachments on the catalyst by using water, and then drying in a vacuum oven.
FIG. 8 is a graph of the Linear Sweep (LSV) of Oxygen Evolution Reaction (OER) in alkaline electrolyte for catalysts doped with different Mg contents (11 mmol, 15mmol, 22mmol Mg contents, respectively) obtained in example 1, example 4, and example 5. It can be seen from the figure that adjusting the content of doped Mg within a suitable range has better oxygen evolution reaction performance than that of examples 2 and 3.
The foregoing description and description of the embodiments are provided to facilitate the understanding and appreciation of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications can be made to these teachings and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above description and the description of the embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
The invention is not the best known technology.
Claims (3)
1. A method for preparing Mg-doped NiFe-based (oxy) hydroxide, characterized in that the method comprises the steps of:
mixing MgCl 2 、NiCl 2 ·6H 2 Dissolving O in deionized water, and stirring to obtain a mixed solution; immersing the processed foam iron in the mixed solution, stirring for 2-4 h, cleaning and drying to obtain Mg-doped NiFe-based (oxy) hydroxide;
wherein, Mg: the molar ratio of Ni is 1-3: 0.5 to 1; the total metal concentration of the mixed solution is 0.5-1 mol/L.
2. The method for preparing Mg-doped NiFe-based (oxy) hydroxide as set forth in claim 1, wherein the foamed iron in the step (1) is a cleaned material: sequentially placing the materials in hydrochloric acid, absolute ethyl alcohol and deionized water for ultrasonic cleaning, then performing ultrasonic cleaning for 8-10 min, respectively washing with ethyl alcohol and water, and then drying in a vacuum drying oven;
the concentration of the hydrochloric acid is 1-3 mol/L.
3. Use of Mg doped NiFe based (oxy) hydroxides prepared by the process of claim 1, characterized by electrocatalytic oxygen evolution reaction.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2024057717A1 (en) * | 2022-09-16 | 2024-03-21 | パナソニックＩｐマネジメント株式会社 | Water electrolysis electrode, water electrolysis cell, water electrolysis device, and method for manufacturing water electrolysis electrode |
| WO2024057715A1 (en) * | 2022-09-16 | 2024-03-21 | パナソニックＩｐマネジメント株式会社 | Water electrolysis cell electrode, water electrolysis cell, water electrolysis device, and method for producing water electrolysis cell electrode |
Citations (6)
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