CN116791123A - Preparation method and application of cerium-doped nickel-iron oxide gas diffusion electrode - Google Patents
Preparation method and application of cerium-doped nickel-iron oxide gas diffusion electrode Download PDFInfo
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- 238000009792 diffusion process Methods 0.000 title claims abstract description 26
- DMTIXTXDJGWVCO-UHFFFAOYSA-N iron(2+) nickel(2+) oxygen(2-) Chemical compound [O--].[O--].[Fe++].[Ni++] DMTIXTXDJGWVCO-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title abstract description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000002243 precursor Substances 0.000 claims abstract description 33
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 229910052742 iron Inorganic materials 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 6
- 150000000703 Cerium Chemical class 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 21
- 238000005868 electrolysis reaction Methods 0.000 claims description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 239000004202 carbamide Substances 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 10
- 238000005470 impregnation Methods 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 239000006260 foam Substances 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 4
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical group [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 239000000446 fuel Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000000877 morphologic effect Effects 0.000 claims 1
- 238000007598 dipping method Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 34
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 24
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 12
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000126 substance Substances 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000008151 electrolyte solution Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 239000012695 Ce precursor Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000002064 nanoplatelet Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910000863 Ferronickel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001588 bifunctional effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229960001545 hydrotalcite Drugs 0.000 description 1
- 229910001701 hydrotalcite Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- QJSRJXPVIMXHBW-UHFFFAOYSA-J iron(2+);nickel(2+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Fe+2].[Ni+2] QJSRJXPVIMXHBW-UHFFFAOYSA-J 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
Classifications
-
- 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
- Y02E60/50—Fuel cells
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Abstract
The invention discloses a preparation method and application of a cerium-doped nickel-iron oxide gas diffusion electrode. The method comprises the following steps: (1) hydrothermal reaction: dissolving nickel inorganic salt, an iron inorganic salt precursor and an alkali source in water, and stirring to obtain a precursor solution; immersing a porous metal substrate in the precursor solution, performing hydrothermal reaction, then cooling to room temperature, washing an electrode, and drying for later use; (2) dipping and roasting: dissolving cerium salt precursor in water, and stirring until a transparent solution is obtained to obtain an impregnating solution; and (3) sequentially carrying out first-stage roasting treatment and second-stage roasting treatment on the electrode obtained in the step (1) to obtain the electrode. According to the invention, the hydrothermal synthesis and the dipping roasting are combined, so that the effective doping of Ce element is realized on the surface of the ordered support electrode, the electrode preparation success rate is improved, and the electrode preparation method has better activity and stability.
Description
Technical Field
The invention belongs to the technical field of water electrolysis, and particularly relates to a preparation method and application of a cerium-doped nickel-iron oxide gas diffusion electrode.
Background
In recent years, the worldwide renewable energy consumption continues to increase, and the water electrolysis hydrogen production technology has become mature and can be applied for 50 years ago. However, the specific gravity of the hydrogen produced in this way in the total world hydrogen production remains very small. Alkaline liquid electrolyzer water electrolysis is a relatively mature technology, and the number of units operated in 1902 years reaches more than 400. The service life of the alkaline water electrolyzer can reach 15 years, and the alkaline water electrolyzer electrolysis technology becomes the commercial water electrolysis hydrogen production technology with the longest operation time all over the world. The core in the electrolysis process is the electrocatalyst required for the electrochemical reaction, which directly affects the electrolysis efficiency, electrolysis energy consumption, electrolysis cost and the lifetime of the electrolysis cell. There is a recent trend towards increasing research on non-noble metal oxygen evolution catalysts used under alkaline conditions.
Patent CN104659357a discloses a preparation method of a carbon-supported nickel-iron hydroxide composite material. Although the catalyst prepared by the method has good oxygen evolution electrocatalytic activity under alkaline conditions, the catalyst cannot overcome the defects that the supported catalyst taking a carbon material as a carrier has serious corrosion problem of the carrier under the electrolysis voltage tested by an alkaline full-electrolysis cell, and the long-term operation life of the full-electrolysis cell is influenced. Patent CN105618060a discloses a non-metal bifunctional oxygen catalyst of graphene/ferronickel hydrotalcite, and in the practical application process, catalyst particles are difficult to be orderly arranged, so that higher dispersity is difficult to obtain, and the utilization rate of the catalyst is not high.
Disclosure of Invention
The invention aims to provide a preparation method and application of a cerium-doped nickel-iron oxide gas diffusion electrode, and the gas diffusion oxygen evolution electrode prepared by the method can enable oxygen evolution reaction in an electrochemical process to be carried out efficiently under a small external bias.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the invention provides a preparation method of a cerium-doped nickel-iron oxide gas diffusion electrode, which comprises the following steps:
(1) Hydrothermal reaction: dissolving nickel inorganic salt, an iron inorganic salt precursor and an alkali source in water, and stirring to obtain a precursor solution; immersing a porous metal substrate in the precursor solution, performing hydrothermal reaction, then cooling to room temperature, washing an electrode, and drying for later use;
(2) And (3) soaking and roasting: dissolving cerium salt precursor in water, and stirring to obtain impregnation liquid; and (3) carrying out first-stage roasting treatment on the electrode obtained in the step (1), immersing the roasted electrode in impregnating solution, taking out the electrode, and carrying out second-stage roasting treatment to obtain the cerium-doped nickel-iron oxide gas diffusion electrode.
In the technical scheme, in the step (1), the hydrothermal reaction temperature is 100-180 ℃ and the hydrothermal reaction time is 5-15 h;
the drying is vacuum drying, the drying temperature is 50-80 ℃, and the drying time is 6-12 h;
in the precursor salt solution, the mass concentration of the total substances of the nickel inorganic salt and the iron inorganic salt precursor is 0.1-3 mM, and the mass ratio of the nickel to the iron is 1:9-1:1;
the alkali source is one or more of urea, potassium hydroxide and sodium hydroxide, and the mass concentration of the alkali source in the precursor solution is 10-50 mM.
In the above technical scheme, in step (1), the time required for stirring to obtain the transparent solution is more than 30 min.
In the above technical solution, in step (1), the porous metal substrate further includes any one of foam nickel, nickel felt, nickel mesh, stainless steel felt, and stainless steel mesh.
In the above technical scheme, in the step (2), the mass concentration of the cerium salt precursor in the impregnating solution is 0.1-3 mM;
the temperature of the first stage roasting treatment is 400-450 ℃ and the time is 3-15 h, and the roasting is performed in air atmosphere; the temperature of the second stage roasting treatment is 100-200 ℃ and the time is 3-15 h, and roasting is performed in air atmosphere.
In the above technical scheme, in step (2), the time required for stirring to obtain the transparent solution is more than 30 min.
In the above technical scheme, further, in the step (2), the obtained product is a cerium doped nickel-iron oxide gas diffusion electrode, the electrode comprises a porous metal substrate and a nickel-iron oxide adhesion layer covered on the surface of the porous metal substrate, and the final morphology characteristics of the nickel-iron oxide adhesion layer are as follows: the diameter is 2-3 mu m, the thickness is 50-100 nm, the surface of the nanometer sheet is rough.
The invention also provides an application of the cerium-doped nickel-iron oxide gas diffusion electrode, wherein the electrode is used as an oxygen evolution catalyst and applied to RFC, photoelectrocatalysis, APE water electrolysis cells or alkaline water electrolysis hydrogen generators and oxygen evolution reactions of metal-air fuel cells.
The beneficial effects of the invention are as follows:
1. the conventional impregnation method is difficult to prepare ordered, thinner and uniform electrode catalytic layers, and the hydrothermal synthesis method can realize accurate regulation and control of electrode structures and controllable preparation of ordered electrodes. However, mixing Ce precursor in the precursor solution of the hydrothermal reaction may cause pulverization of the electrode substrate, and it is difficult to ensure the success rate of electrode preparation. According to the invention, after staged roasting treatment, the electrode is heated and decomposed to form oxide in the first stage of roasting, and the oxide is converted from a smooth surface to a rough surface, so that a cavity structure favorable for impregnation is formed. The main microstructure of the gas diffusion electrode is formed after the first stage roasting, so that in the second stage roasting process, by reducing the roasting temperature, the Ce precursor is doped in a cavity formed by decomposing hydroxide, and meanwhile, the substrate structure formed by the first stage roasting is kept, so that the cerium doped nickel-iron oxide gas diffusion electrode which is more stable than the Ce precursor solution is added into the reaction solution is obtained, and further, the activity and the stability are better.
2. The traditional dipping roasting method does not consider substrate change caused by repeated high-temperature roasting, and is only optimized for the development and preparation of the catalyst supported by the electrode, and the method adopts the combination of hydrothermal synthesis and dipping roasting, so that the effective doping of Ce element can be realized on the surface of the ordered supporting electrode, and the electrode preparation success rate is improved.
Drawings
FIG. 1 is an electron micrograph of the Ce-doped electrode powder particles of example 1 before and after baking, a being before baking and b being after baking;
FIG. 2 shows polarization curves of oxygen evolution reactions of electrodes obtained in example 1, example 2, comparative example 1, and comparative example 2.
Detailed Description
The preparation method, characteristics and application of the cerium-doped nickel-iron oxide gas diffusion electrode are further described below with reference to the accompanying drawings:
example 1
The method adopts two-stage roasting to carry out the dipping roasting of Ce element, and comprises the following steps:
(1) Hydrothermal reaction:
dissolving nickel nitrate, ferric nitrate and urea in deionized water, and fully stirring for 30 minutes to obtain a clear and transparent precursor solution, wherein the total mass of the nickel nitrate and the ferric nitrate in the precursor solution is 3mM, the mass ratio of the nickel nitrate to the ferric nitrate is 1:3, and the urea is 10mM; immersing the cleaned foam nickel vertically into a precursor solution, carrying out hydrothermal reaction for 8 hours at 140 ℃, and carrying out vacuum drying at 80 ℃ for 12 hours; as shown in fig. 1 (a), the product obtained after drying is a smooth-surface, nearly hexagonal nanoplatelet.
(2) And (3) soaking and roasting:
dissolving cerium nitrate in water, stirring for 30 minutes until a transparent solution is obtained, and preparing a 2mM cerium nitrate solution, namely an impregnating solution; roasting the electrode obtained after the hydrothermal reaction for 5 hours at 450 ℃, carrying out first-stage roasting, immersing the product in impregnating solution, taking out the electrode after 3 minutes, carrying out second-stage roasting after 150 ℃ impregnating roasting for 5 hours, repeating the two-stage impregnating roasting for 5 times, and washing and drying for later use to obtain the cerium-doped nickel-iron oxide gas diffusion electrode. As shown in fig. 1 (b), the product obtained after drying was approximately hexagonal nanoplatelets with rough surface.
Example 2
The method adopts two-stage roasting to carry out the dipping roasting of Ce element, and comprises the following steps:
(1) Hydrothermal reaction:
dissolving nickel nitrate, ferric nitrate and urea in deionized water, and fully stirring for 30 minutes to obtain a clear and transparent precursor solution, wherein the total substances of the nickel nitrate and the ferric nitrate in the precursor solution are 3mM, the ratio of the substances of the nickel nitrate to the ferric nitrate is 1:3, and the urea is 10mM; immersing the cleaned foam nickel vertically into a precursor solution, carrying out hydrothermal reaction for 8 hours at 140 ℃, and carrying out vacuum drying at 80 ℃ for 12 hours;
(2) And (3) soaking and roasting:
dissolving cerium nitrate in water, stirring for 30 minutes until a transparent solution is obtained, and preparing a 2mM cerium nitrate solution, namely an impregnating solution; and (3) roasting the electrode obtained after the hydrothermal reaction for 5 hours at 450 ℃ for a first stage of roasting, immersing the product in an impregnating solution, taking out the electrode after 3 minutes, carrying out the second stage of roasting after the impregnation roasting for 5 hours at 350 ℃, repeating the two stages of impregnation roasting for 5 times, and washing and drying for standby to obtain the cerium-doped nickel-iron oxide gas diffusion electrode.
Comparative example 1
The dipping roasting of Ce element is completed by adopting one-time roasting, which comprises the following steps:
(1) The hydrothermal reaction process comprises the following steps:
dissolving nickel nitrate, ferric nitrate and urea in deionized water, fully stirring for 30 minutes to obtain a clear and transparent precursor solution, wherein the total substance amount of the nickel nitrate and the ferric nitrate in the precursor solution is 3mM, the ratio of the nickel nitrate to the ferric nitrate is 1:3, the urea is 10mM, vertically immersing the cleaned foam nickel in the precursor solution, carrying out hydrothermal reaction for 8 hours at 140 ℃, and carrying out vacuum drying at 80 ℃ for 12 hours;
(2) The dipping and roasting process comprises the following steps:
dissolving cerium nitrate in water, stirring for 30 minutes until a transparent solution is obtained, preparing a 2mM cerium nitrate solution, namely, immersing an electrode obtained after hydrothermal reaction in the immersion liquid, taking out the electrode after 3 minutes, roasting at 300 ℃ for 5 times, and carrying out repeated soaking roasting for 3 hours each time, washing and drying for later use to obtain the cerium-doped nickel-iron oxide gas diffusion electrode.
Comparative example 2
The preparation of the foam nickel electrode was completed using the same materials, steps, and conditions as in the hydrothermal reaction process of (1) in example 1, but without the cerium impregnation firing process.
Hydrothermal reaction: dissolving nickel nitrate, ferric nitrate and urea in deionized water, fully stirring for 30 minutes to obtain a clear and transparent precursor solution, wherein the total substance amount of the nickel nitrate and the ferric nitrate in the precursor solution is 3mM, the ratio of the nickel nitrate to the ferric nitrate is 1:3, the urea is 10M, vertically immersing the cleaned foam nickel into the precursor solution, carrying out hydrothermal reaction for 8 hours at 140 ℃, and carrying out vacuum drying at 80 ℃ for 12 hours to obtain the nickel-iron oxide gas diffusion electrode.
Test results:
the following half cell tests were performed for each of example 1, example 2, comparative example 1, and comparative example 2: the half cell system uses oxygen gas to saturated 1M KOH solution as electrolyte and the integrated electrode performs polarization curve scanning as shown in fig. 2.
Gas prepared by the method of example 1The bulk diffusion electrode was 2000mA/cm in a 1M KOH electrolyte solution 2 The potential at the electrolysis current density was 2.07V (vs. RHE).
The gas diffusion electrode prepared by the method of example 2 was subjected to 2000mA/cm in a 1M KOH electrolyte solution 2 The potential at the electrolysis current density was 2.14V (vs. RHE).
The gas diffusion electrode prepared by the method of comparative example 1 was 2000mA/cm in a 1M KOH electrolyte solution 2 The potential at the electrolysis current density was 2.25V (vs. RHE).
The gas diffusion electrode prepared by the method of comparative example 2 was 2000mA/cm in a 1M KOH electrolyte solution 2 The potential at the electrolysis current density was 2.28V (vs. RHE).
Example 1 uses a lower second stage firing temperature for staged firing for the impregnation firing of Ce element, and a lower electrolysis voltage is obtained in the specified conditions, which has better catalytic activity than example 2, comparative example 1, comparative example 2. Therefore, the gas diffusion electrode prepared by the technical scheme of the invention has good oxygen evolution electro-catalysis performance under alkaline conditions.
Claims (8)
1. A method for preparing a cerium-doped nickel-iron oxide gas diffusion electrode, which is characterized by comprising the following steps:
(1) Hydrothermal reaction: dissolving nickel inorganic salt, an iron inorganic salt precursor and an alkali source in water, and stirring to obtain a precursor solution; immersing a porous metal substrate in the precursor solution, performing hydrothermal reaction, then cooling to room temperature, washing an electrode, and drying for later use;
(2) And (3) soaking and roasting: dissolving cerium salt precursor in water, and stirring to obtain impregnation liquid; and (3) carrying out first-stage roasting treatment on the electrode obtained in the step (1), immersing the roasted electrode in impregnating solution, taking out the electrode, and carrying out second-stage roasting treatment to obtain the cerium-doped nickel-iron oxide gas diffusion electrode.
2. The method of manufacturing according to claim 1, characterized in that: in the step (1), the hydrothermal reaction temperature is 100-180 ℃ and the hydrothermal reaction time is 5-15 h;
the drying is vacuum drying, the drying temperature is 50-80 ℃, and the drying time is 6-12 h;
in the precursor solution, the total mass concentration of the nickel inorganic salt and the iron inorganic salt precursor is 0.1-3 mM, and the mass ratio of the nickel to the iron is 1:9-1:1;
the alkali source is one or more of urea, potassium hydroxide and sodium hydroxide, and the mass concentration of the alkali source in the precursor solution is 10-50 mM.
3. The method of manufacturing according to claim 1, characterized in that: in the step (1), the stirring time is more than 30 min.
4. The method of claim 1, wherein in step (1), the porous metal substrate comprises any one of nickel foam, nickel felt, nickel mesh, stainless steel felt, stainless steel mesh.
5. The method of manufacturing according to claim 1, characterized in that: in the step (2), the mass concentration of the cerium salt precursor in the impregnating solution is 0.1-3 mM;
the temperature of the first stage roasting treatment is 400-450 ℃ and the time is 3-15 h, and the roasting is performed in air atmosphere; the temperature of the second stage roasting treatment is 100-200 ℃ and the time is 3-15 h, and roasting is performed in air atmosphere.
6. The method of manufacturing according to claim 1, characterized in that: in the step (2), the stirring time is more than 30 min.
7. The method of manufacturing according to claim 1, characterized in that: in the step (2), the obtained product is a cerium doped nickel-iron oxide gas diffusion electrode, wherein the electrode comprises a porous metal substrate and a nickel-iron oxide adhesion layer covered on the surface of the porous metal substrate, and the final morphological characteristics of the nickel-iron oxide adhesion layer are as follows: the diameter is 2-3 mu m, the thickness is 50-100 nm, the surface of the nanometer sheet is rough.
8. Use of a cerium-doped nickel iron oxide gas diffusion electrode prepared by the method according to any one of claims 1 to 6, characterized in that: the electrode is used as an oxygen evolution catalyst for oxygen evolution reaction of RFC, photoelectrocatalysis, APE water electrolytic cells or alkaline water electrolysis hydrogen generators and metal air fuel cells.
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| CN202310644331.8A CN116791123A (en) | 2023-06-01 | 2023-06-01 | Preparation method and application of cerium-doped nickel-iron oxide gas diffusion electrode |
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