CN117867568A - Rapid preparation method and application of transition metal oxide/carbon fiber composite electrocatalyst - Google Patents
Rapid preparation method and application of transition metal oxide/carbon fiber composite electrocatalyst Download PDFInfo
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- CN117867568A CN117867568A CN202311318871.3A CN202311318871A CN117867568A CN 117867568 A CN117867568 A CN 117867568A CN 202311318871 A CN202311318871 A CN 202311318871A CN 117867568 A CN117867568 A CN 117867568A
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- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 104
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 101
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 101
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 239000002131 composite material Substances 0.000 title claims abstract description 99
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910000314 transition metal oxide Inorganic materials 0.000 title claims abstract description 17
- 229920000742 Cotton Polymers 0.000 claims abstract description 29
- -1 transition metal salt Chemical class 0.000 claims abstract description 20
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000002485 combustion reaction Methods 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 25
- 229910052799 carbon Inorganic materials 0.000 claims description 25
- 238000000227 grinding Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 238000001179 sorption measurement Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 3
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 2
- 150000000703 Cerium Chemical class 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 150000001868 cobalt Chemical class 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims description 2
- 150000002505 iron Chemical class 0.000 claims description 2
- 150000002696 manganese Chemical class 0.000 claims description 2
- 150000002815 nickel Chemical class 0.000 claims description 2
- 150000003057 platinum Chemical class 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- SDKPSXWGRWWLKR-UHFFFAOYSA-M sodium;9,10-dioxoanthracene-1-sulfonate Chemical compound [Na+].O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2S(=O)(=O)[O-] SDKPSXWGRWWLKR-UHFFFAOYSA-M 0.000 claims description 2
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 15
- 238000000354 decomposition reaction Methods 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 48
- 229910052760 oxygen Inorganic materials 0.000 description 48
- 239000001301 oxygen Substances 0.000 description 48
- 239000005751 Copper oxide Substances 0.000 description 26
- 229910000431 copper oxide Inorganic materials 0.000 description 26
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 25
- 229910000428 cobalt oxide Inorganic materials 0.000 description 21
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 21
- 229910000480 nickel oxide Inorganic materials 0.000 description 21
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 20
- VREFGVBLTWBCJP-UHFFFAOYSA-N alprazolam Chemical compound C12=CC(Cl)=CC=C2N2C(C)=NN=C2CN=C1C1=CC=CC=C1 VREFGVBLTWBCJP-UHFFFAOYSA-N 0.000 description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 11
- 229910052739 hydrogen Inorganic materials 0.000 description 11
- 239000001257 hydrogen Substances 0.000 description 11
- 229910000863 Ferronickel Inorganic materials 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- FWZLXRFUDMNGDF-UHFFFAOYSA-N [Co].[Cu]=O Chemical compound [Co].[Cu]=O FWZLXRFUDMNGDF-UHFFFAOYSA-N 0.000 description 7
- YTBWYQYUOZHUKJ-UHFFFAOYSA-N oxocobalt;oxonickel Chemical compound [Co]=O.[Ni]=O YTBWYQYUOZHUKJ-UHFFFAOYSA-N 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 238000001556 precipitation Methods 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 238000003917 TEM image Methods 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 230000010287 polarization Effects 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 5
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 5
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 5
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 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 4
- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- CJTCBBYSPFAVFL-UHFFFAOYSA-N iridium ruthenium Chemical compound [Ru].[Ir] CJTCBBYSPFAVFL-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 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
- 239000011148 porous material Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
Abstract
The invention discloses a rapid preparation method and application of a transition metal oxide/carbon fiber composite electrocatalyst, which comprises the following preparation steps: preparing transition metal salt aqueous solution, immersing absorbent cotton in the solution, taking out, drying, igniting in air, and after combustion, obtaining black substance as target catalyst, and applying the catalyst in the field of electrocatalytic water decomposition. The preparation method of the electrocatalyst is simple, convenient to operate, free of complex experimental equipment, short in catalyst preparation time, high in efficiency, and good in industrial application prospect, and the prepared electrocatalyst has excellent electrocatalytic water decomposition activity and can be applied to the field of electrocatalytic water decomposition.
Description
Technical Field
The invention relates to the field of clean energy hydrogen energy, in particular to a rapid preparation method of a transition metal oxide/carbon fiber composite electrocatalyst and application thereof in the field of hydrogen production, belonging to the field of electrocatalytic decomposition of water to produce hydrogen.
Technical Field
Along with the serious pollution caused by fossil energy, the development of clean sustainable new energy has long become the consensus of scientific researchers in various countries. The electrocatalytic decomposition water hydrogen production process has become one of the most promising hydrogen production technologies at present due to the advantages of simple process, high hydrogen production purity, no pollution in hydrogen combustion and the like. The electrocatalytic decomposition water reaction comprises two important half reactions, namely a hydrogen precipitation reaction of a cathode and an oxygen precipitation reaction of an anode, but the kinetics in the oxygen precipitation reaction is slow in the oxygen production process due to multi-electron and multi-step processes, and the theoretical potential is 1.23V and is far greater than the potential required by electrocatalytic hydrogen precipitation, so that the electrocatalytic decomposition water reaction is a main energy consumption reaction for preparing hydrogen by electrolyzing water. This limits the further development of electrocatalytic water splitting technology and has become an important technical bottleneck in the water electrolysis hydrogen production industry. Therefore, the development of a high-efficiency electrocatalytic oxygen evolution catalyst has important significance for promoting the commercialization development of electrolyzed water.
At present, iridium (ruthenium) noble metal electrocatalysts are the most effective oxygen evolution catalysts, but the large-scale commercial application thereof is severely limited due to the high price, low storage capacity and the like. Transition metal compounds such as iron, cobalt, nickel-based oxides, sulfides and composite materials thereof have stronger application prospect in the field of electrochemical catalytic water decomposition oxygen precipitation due to the characteristics of low cost, easy combination regulation and control and the like.
Disclosure of Invention
Aiming at the current demands for low-cost, high-efficiency and electrocatalytic water oxidation electrode materials, the invention provides a rapid preparation method of a transition metal oxide/carbon fiber composite electrocatalyst and application of the catalyst prepared by the method in the field of electrocatalytic water decomposition.
The invention aims at a rapid preparation method of a transition metal oxide/carbon fiber composite electrocatalyst, which is realized by the following technical scheme, and comprises the following specific steps:
step A: preparing transition metal salt aqueous solution according to a proportion, soaking a proper amount of absorbent cotton in the solution, taking out and drying after full absorption;
and (B) step (B): and D, igniting the product obtained in the step A in air, and grinding the obtained black material into powder after combustion is finished, thus obtaining the target catalyst.
When the absorbent cotton carrier with the adsorbed metal salt is ignited in the air, the ignition modes include, but are not limited to, matches, lighters, alcohol burners, flame ejectors and the like.
Preferably, in the step a, the transition metal salt used is a water-soluble transition metal salt, including but not limited to nickel salt, iron salt, cobalt salt, manganese salt, silver salt, platinum salt, gold salt and cerium salt.
Preferably, in the step a, the transition metal salt used is one of nitrate, chloride, sulfate and acetylacetonate.
Preferably, in the step a, the metal salt adsorption carrier is at least one of absorbent cotton, sanitary cotton and medical cotton, and the adsorption time is 1-4 hours.
Still preferably, in the step a, the volume ratio of the total molar amount of the transition metal salt to the deionized water is 1:1-10, and the molar ratio of the transition metal salt to the absorbent cotton is 1:0.5 to 5.
The application of the transition metal oxide/carbon fiber composite electrocatalyst in the field of electrocatalytic water splitting.
Compared with the electrocatalytic oxygen precipitation catalyst in the prior art, the transition metal oxide/carbon fiber composite electrocatalyst provided by the invention has the following advantages:
1. the electrocatalyst is mixed and uniformly dispersed with common additives, and then is simply coated or sprayed on one side of commercial carbon paper and carbon cloth to be used as a working electrode, so that the electrocatalyst is simple and convenient.
2. The transition metal oxide has multiple valence states and a modulated electronic structure, and can play a role in synergy among components, so that the prepared catalyst has excellent performance.
3. The preparation reaction process is simple, does not need complex equipment, and is convenient for mass preparation.
4. The transition metal oxide/carbon fiber composite electrocatalyst provided by the invention has various valence and adjustable electronic structure, and therefore, the catalyst shows excellent electrocatalytic water decomposition activity.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1a is an X-ray diffraction chart obtained after combustion of absorbent cotton not adsorbed with metal salt ions prepared in example 1 of the present invention.
FIG. 1b is a scanning electron micrograph of absorbent cotton without adsorbed metal salt ions prepared in example 1 of the present invention after combustion.
FIG. 2a is an X-ray diffraction pattern of a cobalt oxide/carbon fiber composite electrocatalyst prepared in example 1 according to the invention.
FIG. 2b is a low power scanning electron microscope photograph of the cobalt oxide/carbon fiber composite electrocatalyst prepared in example 1 of the present invention.
FIG. 2c is a high power scanning electron microscope photograph of the cobalt oxide/carbon fiber composite electrocatalyst prepared in example 1 of the present invention.
FIG. 2d is a transmission electron micrograph of a cobalt oxide/carbon fiber composite electrocatalyst prepared according to example 1 of the invention.
FIG. 2e is a graph showing the energy spectrum of the cobalt oxide/carbon fiber composite electrocatalyst prepared in example 1 of the invention.
FIG. 2f is an elemental distribution diagram of a cobalt oxide/carbon fiber composite electrocatalyst prepared according to example 1 of the invention.
FIG. 3a is an oxygen evolution polarization curve of a cobalt oxide/carbon fiber composite electrocatalyst (coated on commercial carbon paper) prepared in example 1 of the invention and commercial carbon paper.
FIG. 3b shows the Tafil's slope during oxygen evolution of the cobalt oxide/carbon fiber composite electrocatalyst prepared in example 1 of the invention.
FIG. 4 is an X-ray diffraction pattern of the nickel oxide/carbon fiber composite electrocatalyst prepared in example 2 of the invention.
FIG. 5a is a high power scanning electron microscope photograph of the nickel oxide/carbon fiber composite electrocatalyst prepared in example 2 of the present invention.
FIG. 5b is a low power scanning electron microscope photograph of the nickel oxide/carbon fiber composite electrocatalyst prepared in example 2 of the invention.
FIG. 5c is a transmission electron micrograph of the nickel oxide/carbon fiber composite electrocatalyst prepared in example 2 of the invention.
Fig. 5d is a picture of the elemental distribution of the nickel oxide/carbon fiber composite electrocatalyst prepared in example 2 of the invention.
FIG. 6a is an oxygen evolution polarization curve of a nickel oxide/carbon fiber composite electrocatalyst (coated on commercial carbon paper) prepared according to example 2 of the invention.
FIG. 6b shows the Tafil's slope during oxygen evolution of the nickel oxide/carbon fiber composite electrocatalyst prepared in example 2 of the invention.
FIG. 7a is an X-ray diffraction pattern of a copper oxide/carbon fiber composite electrocatalyst prepared in example 3 according to the invention.
FIG. 7b is a low power scanning electron micrograph of a copper oxide/carbon fiber composite electrocatalyst prepared according to example 3 of the invention.
FIG. 7c is a high power scanning electron microscope photograph of the copper oxide/carbon fiber composite electrocatalyst prepared in example 3 of the present invention.
FIG. 7d is a transmission electron micrograph of a copper oxide/carbon fiber composite electrocatalyst prepared according to example 3 of the invention.
FIG. 8a is an oxygen evolution polarization curve of a copper oxide/carbon fiber composite electrocatalyst (coated on commercial carbon paper) prepared according to example 3 of the invention.
FIG. 8b shows the Tafil's slope during oxygen evolution of the copper oxide/carbon fiber composite electrocatalyst prepared in example 3 of the invention.
FIG. 9a is an oxygen evolution polarization curve of a copper oxide/carbon fiber composite electrocatalyst (coated on commercial carbon paper) prepared according to example 4 of the invention.
FIG. 9b shows the Tafil's slope during oxygen evolution of the copper oxide/carbon fiber composite electrocatalyst prepared in example 4 of the invention.
FIG. 10a is an oxygen evolution polarization curve of a copper oxide/carbon fiber composite electrocatalyst (coated on commercial carbon paper) prepared according to example 5 of the invention.
FIG. 10b shows the Tafil's slope during oxygen evolution of the copper oxide/carbon fiber composite electrocatalyst prepared in example 5 of the invention.
FIG. 11a is an oxygen evolution polarization curve of a copper oxide/carbon fiber composite electrocatalyst (coated on commercial carbon paper) prepared according to example 6 of the invention.
FIG. 11b shows the Tafil's slope during oxygen evolution of the copper oxide/carbon fiber composite electrocatalyst prepared in example 6 of the invention.
Detailed description of the preferred embodiments
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
In order to more clearly show the technical scheme and the technical effects provided by the invention, the preparation method and the application of the transition metal oxide/carbon fiber composite electrocatalyst provided by the invention are described in detail by using specific embodiments.
Example 1
The preparation method of the transition metal Co oxide/carbon fiber composite electrocatalyst comprises the following steps:
step A: preparing 5ml of cobalt nitrate (2 mmol) aqueous solution, immersing 2g of absorbent cotton into the solution, reacting for 2 hours, taking out the absorbent cotton and drying;
and (B) step (B): and C, igniting the sample obtained in the step A by using an alcohol burner, and grinding the obtained black material to powder after combustion is finished, thus obtaining the cobalt oxide/carbon fiber composite electrocatalyst.
Specifically, the cobalt oxide/carbon fiber composite electrocatalyst prepared in example 1 of the present invention was tested as follows:
fig. 1a shows an X-ray diffraction pattern obtained after combustion of absorbent cotton, to which metal ions are not adsorbed, in air, showing an amorphous characteristic peak, indicating that the obtained carbon is amorphous. Fig. 1b is a scanning electron micrograph of absorbent cotton, which has not adsorbed metal ions, after burning in air, which shows a typical fiber structure and has a smooth surface.
The phase composition of the cobalt oxide/carbon fiber composite electrocatalyst is characterized by adopting X-ray diffraction, and the result shows that the characteristic peak of cobaltosic oxide appears in the graph of fig. 2a, and the characteristic peak shows that the obtained cobalt oxide is cobaltosic oxide, and compared with the graph of fig. 1a, the characteristic peak shows that after adsorbing cobalt ions, absorbent cotton is burnt in air, and a new phase is generated. Fig. 2b and 2c are scanning electron micrographs of a cobalt oxide/carbon fiber composite electrocatalyst, respectively, showing that the oxide particles are uniformly supported on the carbon fiber surface, and the variation is significant compared with the smooth surface of fig. 1 b.
Fig. 2d is a transmission electron micrograph of a cobalt oxide/carbon fiber composite electrocatalyst, showing oxide particles supported on carbon plates. As can be seen from the energy spectrum of fig. 2e, the sample contains three elements, cobalt, oxygen and carbon.
Fig. 2f is a picture of the elemental distribution of a cobalt oxide/carbon fiber composite electrocatalyst, from which it can be seen that the cobalt, oxygen and carbon elements are uniformly distributed throughout the sample.
The oxygen evolution activity of the cobalt oxide/carbon fiber composite electrocatalyst was studied using a standard three electrode system, in whichThe cobalt oxide coated carbon paper was used as the working electrode, hg/HgO as the reference electrode and Pt mesh as the counter electrode, the test electrolyte was 1.0M KOH, the scan rate was 5.0mV/s, as shown in FIG. 3a, and as can be seen from the figure, 10mA/cm was reached 2 The desired overpotential was 293mV, while the oxygen evolution overpotential of pure commercial carbon paper was 490mV, indicating that cobalt oxide has excellent oxygen evolution activity. FIG. 3b shows the Tafil slope (derived from FIG. 3 a) of 106.3mV/dec during oxygen evolution of the cobalt oxide/carbon fiber composite electrocatalyst, which indicates that the cobalt oxide/carbon fiber composite electrocatalyst has superior kinetic behavior during the electrocatalytic oxygen evolution.
Example 2
The preparation method of the transition metal nickel oxide/carbon fiber composite electrocatalyst comprises the following steps:
step A: preparing 5ml of nickel nitrate (3 mmol) aqueous solution, immersing 2g of absorbent cotton into the solution, reacting for 2 hours, taking out the absorbent cotton and drying;
and (B) step (B): and D, igniting the sample obtained in the step A by using an alcohol burner, and grinding the obtained black material to powder after combustion is finished, thus obtaining the nickel oxide/carbon fiber composite electrocatalyst.
Specifically, the cobalt oxide/carbon fiber composite electrocatalyst prepared in example 2 of the present invention was tested as follows:
the phase composition of the nickel oxide/carbon fiber composite electrocatalyst was characterized by X-ray diffraction, and the results indicate that characteristic peaks of nickel oxide appear in fig. 4, indicating that the obtained nickel oxide is nickel oxide. Fig. 5a and 5b are low-power and high-power scanning electron micrographs of the nickel oxide/carbon fiber composite electrocatalyst, respectively, and it can be seen that the oxide particles are uniformly supported on the surface of the carbon fiber, specifically, the oxide is embedded into the carbon fiber, so that the oxide particles are not easy to fall off, and the variation is obvious compared with the smooth surface of fig. 1 b.
Fig. 5c is a transmission electron micrograph of a nickel oxide/carbon fiber composite electrocatalyst, showing that the oxide particles are supported on the surface of the carbon sheet.
Fig. 5d is a graph showing the distribution of elements of the nickel oxide/carbon fiber composite electrocatalyst, wherein the sample contains three elements, i.e., nickel, oxygen, and carbon, and it can be seen from the graph that the nickel, oxygen, and carbon elements are uniformly distributed throughout the sample.
The oxygen evolution activity of the nickel oxide/carbon fiber composite electrocatalyst was studied using a standard three electrode system in which nickel oxide/carbon fiber composite electrocatalyst coated carbon paper was used as the working electrode, hg/HgO as the reference electrode and Pt mesh as the counter electrode, the test electrolyte was 1.0M KOH, the scan rate was 5.0mV/s, as shown in fig. 6a, to 10mA/cm 2 The desired overpotential was 305mV indicating that nickel oxide has excellent oxygen evolution activity. FIG. 6b shows the Tafil slope (derived from FIG. 6 a) of 116.2mV/dec during oxygen evolution of the nickel oxide/carbon fiber composite electrocatalyst, which indicates that the nickel oxide/carbon fiber composite electrocatalyst has superior kinetic behavior during the electrocatalytic oxygen evolution.
Example 3
The preparation method of the transition metal copper oxide/carbon fiber composite electrocatalyst comprises the following steps:
step A: preparing 5ml of copper nitrate (1 mmol) aqueous solution, immersing 0.5g of absorbent cotton into the solution, reacting for 2 hours, taking out the absorbent cotton and drying;
and (B) step (B): and D, igniting the sample obtained in the step A by using an alcohol burner, and grinding the obtained black substance to powder after combustion is finished, thus obtaining the copper oxide/carbon fiber composite electrocatalyst.
Specifically, the copper oxide/carbon fiber composite electrocatalyst prepared in example 3 of the present invention was tested as follows:
the phase composition of the copper oxide/carbon fiber composite electrocatalyst is characterized by adopting X-ray diffraction, and the result shows that the characteristic peaks of the copper simple substance and the copper oxide appear in the graph 7a, and the obtained copper oxide is copper oxide and metallic copper simple substance. Fig. 7b and 7c are scanning electron micrographs of the copper oxide/carbon fiber composite electrocatalyst, respectively, showing that the oxide particles are uniformly embedded on the carbon fiber surface and exhibit a distinct pore structure, with a distinct change compared to the smooth surface of fig. 1 b.
Fig. 7d is a transmission electron micrograph of a copper oxide/carbon fiber composite electrocatalyst, it being seen that oxide particles are deposited on the carbon fibers.
The oxygen evolution activity of the copper oxide/carbon fiber composite electrocatalyst was studied using a standard three electrode system, wherein copper oxide coated carbon paper was used as the working electrode, hg/HgO as the reference electrode and Pt mesh as the counter electrode, the test electrolyte was 1.0M KOH, the scan rate was 5.0mV/s, as shown in FIG. 8a, from the graph, 10mA/cm was reached 2 The required overpotential was 325mV indicating that the copper oxide/carbon fiber composite electrocatalyst had excellent oxygen evolution activity. FIG. 8b shows the Tafil slope (derived from FIG. 8 a) of 69.6mV/dec during oxygen evolution of the copper oxide/carbon fiber composite electrocatalyst, which indicates that the copper oxide/carbon fiber composite electrocatalyst has superior dynamic behavior during the electrocatalytic oxygen evolution.
Example 4
The preparation method of the transition metal nickel cobalt oxide/carbon fiber composite electrocatalyst comprises the following steps:
step A: preparing 5ml of aqueous solution of cobalt nitrate and nickel nitrate (2 mmol, the mol ratio of the cobalt nitrate to the nickel nitrate is 1:1), immersing 1g of absorbent cotton into the solution, reacting for 6 hours, taking out the absorbent cotton and drying;
and (B) step (B): and D, igniting the sample obtained in the step A by using an alcohol burner, and grinding the obtained black material to powder after combustion is finished, thus obtaining the nickel-cobalt oxide/carbon fiber composite electrocatalyst.
Specifically, the nickel cobalt oxide/carbon fiber composite electrocatalyst prepared in example 4 of the present invention was tested as follows:
the oxygen evolution activity of the nickel cobalt oxide/carbon fiber composite electrocatalyst was studied using a standard three electrode system, wherein nickel cobalt oxide/carbon fiber composite electrocatalyst coated carbon paper was used as the working electrode, hg/HgO as the reference electrode and Pt mesh as the counter electrode, the test electrolyte was 1.0M KOH, the scan rate was 5.0mV/s, as shown in fig. 9a, reaching 10mA/cm 2 Is 336mV, indicating nickel cobalt oxide/carbon fiberThe vitamin composite electrocatalyst has excellent oxygen precipitation activity. FIG. 9b shows the Tafil slope (derived from FIG. 9 a) of 80.8mV/dec during oxygen evolution of the nickel cobalt oxide/carbon fiber composite electrocatalyst, which indicates that the nickel cobalt oxide/carbon fiber composite electrocatalyst has superior kinetic behavior during the electrocatalytic oxygen evolution.
Example 5
The preparation method of the transition metal ferronickel oxide/carbon fiber composite electrocatalyst comprises the following steps:
step A: preparing 5ml of aqueous solution of nickel nitrate and ferric nitrate (3 mmol, the mol ratio of the nickel nitrate to the ferric nitrate is 2:1), immersing 1g of absorbent cotton into the solution, reacting for 2 hours, taking out the absorbent cotton and drying;
and (B) step (B): and D, igniting the sample obtained in the step A by using an alcohol burner, and grinding the obtained black material to powder after combustion is finished, thus obtaining the ferronickel oxide/carbon fiber composite electrocatalyst.
Specifically, the ferronickel oxide/carbon fiber composite electrocatalyst prepared in example 5 of the present invention was tested as follows:
the oxygen evolution activity of the ferronickel oxide/carbon fiber composite electrocatalyst was studied using a standard three electrode system, wherein ferronickel oxide/carbon fiber composite electrocatalyst coated carbon paper was used as the working electrode, hg/HgO as the reference electrode and Pt mesh as the counter electrode, the test electrolyte was 1.0M KOH, the scan rate was 5.0mV/s, as shown in FIG. 10a, reaching 10mA/cm 2 The required overpotential was 285mV, indicating that the ferronickel oxide/carbon fiber composite electrocatalyst has excellent oxygen evolution activity. FIG. 10b is a Tafil slope (derived from FIG. 10 a) of 72.5mV/dec during oxygen evolution of the ferronickel oxide/carbon fiber composite electrocatalyst, indicating superior kinetic behavior of the ferronickel oxide/carbon fiber composite electrocatalyst during electrocatalytic oxygen evolution.
Example 6
The preparation method of the transition metal cobalt copper oxide/carbon fiber composite electrocatalyst comprises the following steps:
step A: preparing 5ml of aqueous solution of cobalt nitrate and copper nitrate (1 mmol, the mol ratio of the cobalt nitrate to the copper nitrate is 1:1), immersing 1g of absorbent cotton into the solution, reacting for 2 hours, taking out the absorbent cotton and drying;
and (B) step (B): and C, igniting the sample obtained in the step A by using an alcohol burner, and grinding the obtained black substance to powder after combustion is finished, thus obtaining the cobalt-copper oxide/carbon fiber composite electrocatalyst.
Specifically, the cobalt copper oxide/carbon fiber composite electrocatalyst prepared in example 6 of the present invention was tested as follows:
the oxygen evolution activity of the cobalt copper oxide/carbon fiber composite electrocatalyst was studied using a standard three electrode system, wherein cobalt copper oxide/carbon fiber composite electrocatalyst coated carbon paper was used as the working electrode, hg/HgO as the reference electrode and Pt mesh as the counter electrode, the test electrolyte was 1.0M KOH, the scan rate was 5.0mV/s, as shown in FIG. 11a, reaching 10mA/cm 2 The required overpotential was 346mV, indicating that the cobalt copper oxide/carbon fiber composite electrocatalyst has excellent oxygen evolution activity. FIG. 11b shows the Tafil slope (derived from FIG. 11 a) of 51.6mV/dec during oxygen evolution of the cobalt copper oxide/carbon fiber composite electrocatalyst, which indicates that the cobalt copper oxide/carbon fiber composite electrocatalyst has superior kinetic behavior during the electrocatalytic oxygen evolution.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the scope of the present invention should be included in the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims (6)
1. A rapid preparation method of a transition metal oxide/carbon fiber composite electrocatalyst is characterized by comprising the following preparation steps:
step A: preparing transition metal salt aqueous solution according to a proportion, soaking a proper amount of absorbent cotton in the solution, taking out and drying after full absorption;
and (B) step (B): and D, igniting the product obtained in the step A in air, and grinding the obtained black material into powder after combustion is finished, thus obtaining the target catalyst.
2. The method for preparing the transition metal oxide/carbon fiber composite electrocatalyst according to claim 1, wherein the transition metal salt used in step a is a water-soluble transition metal salt including, but not limited to, nickel salt, iron salt, cobalt salt, manganese salt, silver salt, platinum salt, gold salt, and cerium salt.
3. The method for preparing the transition metal oxide/carbon fiber composite electrocatalyst according to claim 1, wherein the transition metal salt used in step a is at least one of nitrate, chloride, sulfate, and acetylacetonate.
4. The method for preparing the transition metal oxide/carbon fiber composite electrocatalyst according to claim 1, wherein in the step a, the metal salt adsorption carrier is one of absorbent cotton, sanitary cotton and medical cotton, and the adsorption time is 1-4 hours.
5. The method for preparing the transition metal oxide/carbon fiber composite electrocatalyst according to claim 1, wherein in the step a, the volume ratio of the molar amount of the transition metal salt to deionized water is 1:1-10, and the mass ratio of the molar amount of the transition metal salt to absorbent cotton is 1:0.5 to 5.
6. Use of an electrocatalyst prepared by the rapid preparation method of a transition metal oxide/carbon fibre composite electrocatalyst according to any one of claims 1 to 5 in the field of electrocatalytic water splitting.
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