CN118345422A - RuO with novel porous structure2Preparation and application of anode acid oxygen evolution catalyst - Google Patents
RuO with novel porous structure2Preparation and application of anode acid oxygen evolution catalyst Download PDFInfo
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- CN118345422A CN118345422A CN202410597252.0A CN202410597252A CN118345422A CN 118345422 A CN118345422 A CN 118345422A CN 202410597252 A CN202410597252 A CN 202410597252A CN 118345422 A CN118345422 A CN 118345422A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 103
- 239000002253 acid Substances 0.000 title claims abstract description 29
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 26
- 239000001301 oxygen Substances 0.000 title claims abstract description 26
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 12
- 238000006722 reduction reaction Methods 0.000 claims description 9
- 229910052717 sulfur Inorganic materials 0.000 claims description 8
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 7
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 7
- 239000011593 sulfur Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 230000002378 acidificating effect Effects 0.000 abstract description 5
- 238000000840 electrochemical analysis Methods 0.000 abstract description 2
- 239000008204 material by function Substances 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 238000012546 transfer Methods 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 15
- 230000000694 effects Effects 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009849 deactivation Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- XVMSFILGAMDHEY-UHFFFAOYSA-N 6-(4-aminophenyl)sulfonylpyridin-3-amine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=N1 XVMSFILGAMDHEY-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002981 blocking agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
Abstract
The invention relates to preparation and application of a RuO 2 anode acid oxygen evolution catalyst with a novel porous structure, and belongs to the technical field of functional materials and energy sources. The RuO 2 anode acid oxygen evolution catalyst with a porous structure composed of nano particles is prepared by combining solvothermal treatment and heat treatment, the microcosmic appearance of the catalyst is regulated and controlled by introducing pyridine so as to have rich active sites, the reaction kinetics of the catalyst is improved so that the catalyst is easy to carry out charge transfer, and the OER overpotential is reduced together. In addition, the residual S forms a stable Ru-S bond, which promotes the stability of RuO 2 under acidic conditions. The electrochemical test result shows that the oxygen evolution overpotential of the catalyst at the position of 10mA.cm ‑2 in the 0.5M H 2SO4 solution is only 146mV, the stability is as high as 1300h, and the catalyst has excellent catalytic activity and stability, so that the catalyst has a large-scale application prospect in the acid electrolytic water oxygen evolution reaction.
Description
Technical Field
The invention belongs to the technical field of functional materials and energy sources, and particularly relates to preparation and application of a RuO 2 anode acid oxygen evolution catalyst with a novel porous structure.
Background
The exhaustion of traditional energy sources and their impact on the environment has prompted the search for alternative energy solutions. Among these, green hydrogen energy is a promising candidate due to its high energy density and zero emissions. Electrochemical water splitting driven by renewable energy is an ideal method for large-scale production of green hydrogen. However, the Oxygen Evolution Reaction (OER) of the anode involves inherently slow kinetics of multiple proton-coupled electron transfer relative to the Hydrogen Evolution Reaction (HER) of the cathode, impeding the efficiency of the reaction, requiring higher energy to drive the reaction. In addition, compared with the electrolytic water of the alkaline medium, the acidic medium can reach larger current density, lower resistance loss, higher hydrogen pressure and minimum gas crossover, thus having very high practical application prospect. While harsh operating conditions and slow kinetics present serious challenges to the stability and activity of the catalyst. Among them, noble metal Ir-based catalysts have exhibited excellent OER stability and good activity, but low reserves and high costs have restricted their large-scale commercial application. Therefore, the use of a high-activity low-valence catalyst is of great importance for promoting the practical application of water decomposition under acidic conditions.
In recent years, ruO 2 -based catalysts have been widely studied for their relatively low price, easy-to-regulate electronic structure, and excellent activity. However, ru tends to generate high-valence species under anodic oxidation conditions, causing dissolution in an acidic medium and gradual deactivation thereof, which presents serious challenges for the stability of RuO 2 catalyst. At present, a great deal of research is focused on regulating and controlling the charge structure of RuO 2 so as to regulate and control the catalytic activity of the RuO 2, wherein the doping of metal elements in RuO 2 not only can promote the catalytic activity of the RuO, but also can relieve the deactivation problem, but as the doping elements are continuously dissolved, the Ru-based catalyst is slowly deactivated. Therefore, how to develop a Ru-based catalyst with high activity and high stability still faces serious challenges. Among them, the porous catalyst has abundant active centers and is widely used in various fields. The RuO 2 catalyst with a porous structure is prepared, and meanwhile, the stability is taken into consideration, so that the RuO 2 catalyst has important significance for improving the water decomposition in the acidic environment.
To solve this problem well, pyridine is introduced as a capping agent to prepare a porous Ru-based catalyst, which can maximize the utilization of active centers in the catalyst to reduce the voltage required at constant current density, alleviating its dissolution rate. In addition, the catalyst can form stable Ru-S bond locally during the heat treatment process, so that the stability under the acid condition is improved. Therefore, the aim of improving the activity and stability of the RuO 2 catalyst is expected to be fulfilled.
Disclosure of Invention
The invention mainly solves the technical problem of preparing the RuO 2 oxygen evolution catalyst under the high-efficiency stable acidity. The RuO 2 acid oxygen-evolving catalyst with a novel porous structure is prepared by a mode of combining solvothermal treatment and heat treatment.
In order to solve the technical problems, the technical scheme of the invention is as follows:
the preparation method of the RuO 2 anode acid oxygen evolution catalyst with a novel porous structure comprises the following steps:
Step 1, ruCl 3 and 4-sulfur pyridine are dissolved in methanol solution;
Step 2, adding hydrazine hydrate into the solution to perform reduction reaction:
and step 3, after the reduction reaction is finished, sequentially performing centrifugal cleaning, freeze drying and heat treatment to obtain the catalyst.
In the technical scheme, 4-sulfur-based pyridine is used as a blocking agent to prevent particle agglomeration, hydrazine hydrate is used as a reducing agent to reduce, ultra-pure water centrifugation is used for replacing methanol to freeze-dry, and heat treatment is used for generating a porous RuO 2 catalyst from a reduction product.
Further, the RuCl 3 in the step 1 is used in an amount of 0.10g-0.12g, the 4-sulfur pyridine in an amount of 0.05g-0.17g, and the methanol solution in an amount of 30mL-50mL.
Further, the amount of hydrazine hydrate used in the step 2 is 200-260. Mu.L.
Further, the time of the reduction reaction in the step 2 is 3-7 h.
Further, the conditions of the centrifugal cleaning in the step 3 are as follows: the mixture was separately centrifugally washed 3 times with methanol and ultrapure water.
Further, the freeze drying time in the step 3 is 12-24 hours.
Further, the temperature rising rate of the treatment in the step 3 is 1 ℃/min-5 ℃/min, the temperature is 300 ℃ -500 ℃ and the time is 1h-20h.
RuO 2 anode acid oxygen-evolving catalyst with porous structure prepared by the preparation method is disclosed.
The application of the RuO 2 anode acid oxygen evolution catalyst with the porous structure is used in an acid electrolytic water oxygen evolution reaction.
The RuO 2 anode acid oxygen-evolving catalyst with a novel porous structure is prepared by adopting a simple and rapid solvothermal and thermal treatment combined mode. Compared with the particle RuO 2 catalyst, the introduction of pyridine regulates the microscopic morphology of the catalyst to make the catalyst have rich active sites, improves the reaction kinetics of the catalyst to make the catalyst easy to carry out charge transfer, and jointly reduces OER overpotential. In addition, part of S and Ru in pyridine form stable Ru-S bond locally in the catalyst in the heat treatment process, so that the stability of RuO 2 under the acid condition is improved. The electrochemical test result shows that the oxygen evolution overpotential of the catalyst at the position of 10mA.cm -2 in the 0.5M H 2SO4 solution is only 146mV, the stability is as high as 1300h, and the catalyst has extremely high activity and extremely excellent stability, so that the catalyst has a large-scale application prospect in the acid electrolytic water oxygen evolution reaction.
Compared with the prior art, the invention has the following beneficial effects:
(1) Excellent catalytic activity. The RuO 2 catalyst with a porous structure has rich active centers, can maximally utilize the active sites, and has very remarkable acid catalytic activity.
(2) Excellent stability. A stable local Ru-S bond structure is formed in the heat treatment process, so that the stability of the Ru-based catalyst in a strong acid medium is greatly improved.
(3) The invention has reasonable design thought, and the catalyst prepared by adopting a simple solvothermal and thermal treatment combined mode has very excellent catalytic performance and long-term stability, and has very good application prospect.
Drawings
FIG. 1 is an X-ray diffraction pattern of the catalyst prepared in example 1 and comparative example 1;
FIG. 2 is a Raman diagram of the catalysts prepared in example 1 and comparative example 1;
FIG. 3 is a BET plot of the catalysts prepared in example 1 and comparative example 1;
FIG. 4 is a graph showing pore size distribution of the catalysts prepared in example 1 and comparative example 1;
FIG. 5 is a scanning electron microscope image of the catalyst prepared in example 1 (a) and comparative example 1 (b);
FIG. 6 is an electrochemical performance test chart of the catalysts prepared in example 1 and comparative example 1;
FIG. 7 is a Tafel slope plot of the catalysts prepared in example 1 and comparative example 1;
FIG. 8 is an electrochemical stability profile of the catalyst prepared in example 1;
FIG. 9 is an electrochemical performance test chart of the catalysts prepared in example 2 and example 3;
fig. 10 is an electrochemical performance test chart of the catalysts prepared in example 4 and example 5.
Detailed Description
The present invention will be described more fully hereinafter in order to facilitate an understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Comparative example 1
A preparation method of a granular RuO 2 anode acid oxygen evolution catalyst comprises the following steps:
step 1, 0.1127g of RuCl 3 is dissolved in 40mL of methanol solution, and stirring is continued for 1h to form a uniform mixed solution;
Step 2, slowly adding 243 mu L of hydrazine hydrate into the mixed solution, and continuously stirring for 5 hours to perform reduction reaction;
step 3, after the reaction is finished, respectively centrifuging for 3 times by using methanol and ultrapure water for cleaning;
Step 4, freeze-drying the cleaned powder for one day;
And 5, placing the freeze-dried sample in a muffle furnace, and performing heat treatment at the temperature of 400 ℃ for 2 hours at the heating rate of 5 ℃/min to obtain the granular RuO 2 catalyst.
Example 1
A preparation method of a RuO 2 anode acid oxygen evolution catalyst with a novel porous structure comprises the following steps:
Step 1, 0.1127g of RuCl 3 and 0.0566g of 4-sulfur pyridine are dissolved in 40mL of methanol solution, and stirring is continued for 1h to form a uniform mixed solution;
Step 2, slowly adding 243 mu L of hydrazine hydrate into the mixed solution, and continuously stirring for 5 hours to perform reduction reaction;
step 3, after the reaction is finished, respectively centrifuging for 3 times by using methanol and ultrapure water for cleaning;
Step 4, freeze-drying the cleaned powder for one day;
And 5, placing the freeze-dried sample in a muffle furnace, and performing heat treatment at the temperature of 400 ℃ for 2 hours at the heating rate of 5 ℃/min to obtain the RuO 2 catalyst with a porous structure.
Fig. 1 is an X-ray diffraction pattern of the RuO 2 catalyst and the particulate RuO 2 catalyst of porous structures prepared in example 1 and comparative example 1, respectively. The diffraction peaks of the two catalysts are consistent with the result of the RuO 2 standard card, and the diffraction peaks of other species are not present, and the structure of the single catalyst is presented.
Fig. 2 is a Raman plot of the RuO 2 catalyst, the particulate RuO 2 catalyst, of porous structures prepared separately from example 1, comparative example 1. The diffraction peaks of the two materials are consistent and have the same structure.
Fig. 3 shows BET tests of RuO 2 catalyst and particulate RuO 2 catalyst of porous structures prepared in example 1 and comparative example 1, respectively. Compared to the particulate RuO 2 catalyst, the porous RuO 2 catalyst has a larger specific surface area due to the rich pore structure.
Fig. 4 is a pore size distribution diagram of RuO 2 catalyst and particulate RuO 2 catalyst of porous structures prepared in example 1 and comparative example 1, respectively. The porous RuO 2 catalyst has a rich pore size distribution, whereas the particulate RuO 2 catalyst has no apparent pore structure.
Fig. 5 is a scanning electron microscope image of the RuO 2 catalyst and the particle RuO 2 catalyst of porous structures prepared in example 1 and comparative example 1, respectively. The porous RuO 2 is clearly a catalyst rich in pores, consisting of a plurality of small particles, whereas the particles RuO 2 do not exhibit a distinct pore structure.
Fig. 6 is an electrochemical OER performance test of the RuO 2 catalyst, the particulate RuO 2 catalyst of porous structure prepared separately from example 1, comparative example 1. The prepared catalyst is dripped on carbon paper to be used as a working electrode, pt is used as a counter electrode, hg/Hg 2O4 is used as a doping electrode, and 0.5M H 2SO4 is used as electrolyte; electrochemical performance testing was performed in a standard three-electrode system at room temperature, normal pressure and room temperature. The results show that the overpotential required for the porous RuO 2 catalyst and the particulate RuO 2 catalyst to reach a current density of 10mA cm -2 is 146mV and 216mV, respectively.
Fig. 7 shows Tafel curves for the RuO 2 catalyst and the particulate RuO 2 catalyst having porous structures prepared in example 1 and comparative example 1, respectively. The results show that the kinetics of the porous RuO 2 is significantly better than that of the particulate RuO 2 catalyst.
Fig. 8 is a stability test of RuO 2 catalyst of porous structure prepared in example 1. The results show that RuO 2 of the porous structure possesses very long lasting stability.
Examples 2 to 3
The preparation procedure was essentially the same as in example 1, except that: the molar quantity of the 4-sulfur pyridine is respectively increased by 2 times and 3 times to obtain the corresponding RuO 2 catalyst with a porous structure.
The porous RuO 2 catalysts prepared in example 2 and example 3 were subjected to electrochemical performance testing, see example 1. The results showed that the overpotential required for the porous RuO 2 catalysts prepared in example 2 and example 3 to reach a current density of 10mA cm -2 was 160mV and 171mV, respectively (fig. 9).
Examples 4 to 5
The preparation procedure was essentially the same as in example 1, except that: the temperature in the muffle furnace is changed to 350 ℃ and 500 ℃ to obtain the RuO 2 catalyst with a corresponding porous structure.
The porous RuO 2 catalysts prepared in example 4 and example 5 were subjected to electrochemical performance testing, see example 1. The results showed that the overpotential required for the porous RuO 2 catalysts prepared in example 4 and example 5 to reach a current density of 10mA cm -2 was 143mV and 167mV, respectively (fig. 10). Although the catalyst prepared at 350 ℃ had a lower overpotential, the catalyst gradually deactivated as the voltage increased.
The foregoing is merely illustrative of the present invention and is not to be construed as limiting thereof, and it is intended to cover all modifications and equivalent arrangements included within the spirit and scope of the invention.
Claims (9)
1. The preparation method of the RuO 2 anode acid oxygen evolution catalyst with a novel porous structure is characterized by comprising the following steps:
Step 1, ruCl 3 and 4-sulfur pyridine are dissolved in methanol solution;
Step 2, adding hydrazine hydrate into the solution to perform reduction reaction:
and step 3, after the reduction reaction is finished, sequentially performing centrifugal cleaning, freeze drying and heat treatment to obtain the catalyst.
2. The method for preparing the RuO 2 anode acid oxygen evolution catalyst with the novel porous structure according to claim 1, wherein the dosage of RuCl 3 in the step 1 is 0.10g-0.12g, the dosage of 4-sulfur pyridine is 0.05g-0.17g, and the dosage of methanol solution is 30mL-50mL.
3. The method for preparing the RuO 2 anode acid oxygen evolution catalyst with the novel porous structure according to claim 1, wherein the amount of hydrazine hydrate used in the step 2 is 200-260 μl.
4. The method for preparing the RuO 2 anode acid oxygen evolution catalyst with a novel porous structure according to claim 1, wherein the time of the reduction reaction in the step 2 is 3-7 h.
5. The method for preparing the novel porous RuO 2 anode acid oxygen evolution catalyst according to claim 1, wherein the conditions of centrifugal cleaning in the step 3 are as follows: the mixture was separately centrifugally washed 3 times with methanol and ultrapure water.
6. The method for preparing the RuO 2 anode acid oxygen evolution catalyst with a novel porous structure according to claim 1, wherein the freeze drying time in the step 3 is 12-24 h.
7. The method for preparing the RuO 2 anode acid oxygen evolution catalyst with the novel porous structure according to claim 1, wherein the heating rate of the heat treatment in the step 3 is1 ℃/min-5 ℃/min, the temperature is 300 ℃ -500 ℃ and the time is 1h-20h.
8. The RuO 2 anode acid oxygen evolution catalyst of porous structure produced by the production method of any one of claims 1 to 7.
9. The use of a RuO 2 anode acid oxygen evolution catalyst of porous structure according to claim 8, characterized in that it is used in an acid electrolyzed water oxygen evolution reaction.
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| CN118345422A true CN118345422A (en) | 2024-07-16 |
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