CN109755600B - Carbon cloth loaded nickel-cobalt-oxygen nanosheet composite material, preparation method thereof and application of electrode - Google Patents
Carbon cloth loaded nickel-cobalt-oxygen nanosheet composite material, preparation method thereof and application of electrode Download PDFInfo
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- CZAYMIVAIKGLOR-UHFFFAOYSA-N [Ni].[Co]=O Chemical compound [Ni].[Co]=O CZAYMIVAIKGLOR-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 239000002135 nanosheet Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title abstract description 7
- 229910052799 carbon Inorganic materials 0.000 title abstract description 7
- 239000004744 fabric Substances 0.000 title abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- 239000003054 catalyst Substances 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000002244 precipitate Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- 239000012266 salt solution Substances 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 239000002243 precursor Substances 0.000 claims abstract description 14
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract 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 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000001681 protective effect Effects 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 27
- 239000001301 oxygen Substances 0.000 claims description 27
- 229910052760 oxygen Inorganic materials 0.000 claims description 27
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 239000007789 gas Substances 0.000 abstract description 5
- 238000000975 co-precipitation Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 11
- 238000001816 cooling Methods 0.000 description 10
- 238000004321 preservation Methods 0.000 description 10
- 238000006722 reduction reaction Methods 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 6
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- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002114 nanocomposite Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000001588 bifunctional effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910021397 glassy carbon Inorganic materials 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000004098 selected area electron diffraction Methods 0.000 description 2
- 229910020647 Co-O Inorganic materials 0.000 description 1
- 229910020704 Co—O Inorganic materials 0.000 description 1
- 230000010757 Reduction Activity Effects 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002120 nanofilm Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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Abstract
The invention relates to a carbon cloth loaded nickel cobalt oxygen nanosheet composite material, a preparation method thereof and application of an electrode; dissolving cobalt nitrate and nickel nitrate in deoxidized deionized water, and stirring and dissolving in a gas protective atmosphere to obtain a mixed salt solution; uniformly stirring a sodium hydroxide solution and a mixed salt solution at room temperature, centrifuging to obtain a precipitate, and cleaning with deionized water and absolute ethyl alcohol; and drying the obtained precipitate in vacuum to obtain a precursor, and sintering to obtain the nickel-cobalt-oxygen nanosheet composite catalyst for the cathode of the air battery. The nickel-cobalt-oxygen nano-sheet composite material is made of Ni 0.6 Co 2.4 O 4 And NiO, wherein the diameter of the nano sheet is 100-150 nm, and the thickness of the nano sheet is 10-30 nm. The preparation method provided by the invention realizes the preparation of the nickel-cobalt-oxygen porous nanosheet composite catalyst applied to the cathode of the air battery by using a coprecipitation and sintering method, and has the advantages of simple experimental steps and excellent electrode catalytic performance.
Description
Technical Field
The invention belongs to the field of metal-air battery electrocatalysis, relates to a preparation method of an efficient and cheap air battery oxygen electrode nano composite material, and particularly relates to a carbon cloth loaded nickel-cobalt-oxygen nano sheet composite material, a preparation method thereof and application of an electrode.
Background
With the exhaustion of fossil energy and a series of environmental problems, renewable, clean and sustainable energy conversion devices are becoming the focus of research. Metal-air batteries are considered the most desirable energy storage devices due to their extremely high theoretical energy density. The zinc-air battery mainly comprises three parts: zinc metal anode, air cathode and isolating layer. Among them, the main problem of commercialization of the rechargeable zinc-air battery is to prepare an air cathode material with low price and high efficiency. The current cathode catalyst has great challenges due to the influence of oxygen precipitation reaction, slow kinetics of oxygen reduction reaction and larger overpotential on the cycle charge-discharge life and charge-discharge efficiency of the battery.
As a non-noble metal catalyst, the spinel-type transition metal oxide becomes one of the substitutes of noble metal catalytic materials due to the advantages of low cost, rich resources, environmental friendliness and the like, and is widely applied to the fields of super capacitor electrode materials, solid-state sensors, optical devices and the like. However, the single metal oxide electrode material has a single active site, poor conductivity and low activity, and the bimetallic composite material becomes a new research direction. In practical application and catalysis, in order to further improve the activity of the material: on one hand, the material is nano-sized, and the nano-scale catalytic material increases the active area of the electrode catalytic reaction to a certain extent and promotes the catalytic reaction. On the other hand, the conductivity of a single metal oxide is generally poor, and in order to increase the intrinsic electron conduction efficiency, a proper metal is selected for doping, electronic structures between different metals are mutually influenced, and the conductivity of the material is enhanced. In addition, the catalytic performance of the material can also be improved by increasing the active area of the material. Therefore, the nickel-cobalt-oxygen porous nanosheet composite catalyst has an excellent bifunctional electrocatalysis function.
Disclosure of Invention
The invention aims to provide a carbon cloth loaded nickel cobalt oxygen nanosheet composite material, a preparation method thereof and application of an electrode, wherein the method is simple, environment-friendly, efficient and cheap. The bifunctional catalyst with excellent performance is prepared by adopting a coprecipitation and sintering method, and can be used for preparing an air electrode in an air battery for generating oxygen evolution reaction and oxygen reduction reaction.
The invention aims to provide a preparation method of a nickel-cobalt-oxygen porous nanosheet composite catalyst applied to an air battery cathode by combining the optimization method. The preparation process is simple, convenient to operate and high in repeatability.
The purpose of the invention is realized by the following technical scheme:
a carbon cloth carried Ni-Co-O nano sheet composite material is prepared from Ni 0.6 Co 2.4 O 4 And NiO, wherein the diameter of the nano sheet is 100-150 nm, and the thickness of the nano sheet is 10-30 nm.
The invention discloses a preparation method of a carbon cloth loaded nickel cobalt oxygen nanosheet composite material, which comprises the following steps:
1) dissolving cobalt nitrate and nickel nitrate in deoxidized deionized water, and stirring and dissolving in a gas protection atmosphere to obtain a mixed salt solution;
2) uniformly stirring the sodium hydroxide solution and the mixed salt solution at room temperature, centrifuging to obtain a precipitate, and cleaning with deionized water and absolute ethyl alcohol;
3) and (3) drying the precipitate obtained in the step (2) in vacuum to obtain a precursor, and sintering to obtain the nickel-cobalt-oxygen nanosheet composite catalyst for the cathode of the air battery.
Preferred conditions are as follows:
in the step 1), the use amounts of the cobalt nitrate and the nickel nitrate are respectively 3-5 mmol and 12-20 mmol.
In the step 1), the gas is N 2 ，O 2 Or air.
In the step 1), the stirring speed is 200-600 r/min, and the stirring time is 0.5-1.5 h.
In the step 2), the concentration of the sodium hydroxide solution is 2-4.2 mol/L.
In the step 3), the vacuum drying temperature is 25-35 ℃, and the drying time is 9-15 h; the sintering temperature is 300-375 ℃, and the corresponding sintering time is 2.5-3 h.
The nickel-cobalt-oxygen porous nanosheet composite material is applied to an electrode; as a catalyst to catalyze the oxygen reaction at the cathode of the air cell.
The nickel cobalt oxygen porous nanosheet composite material is coated on a glassy carbon electrode and used for testing the electrocatalytic oxygen reduction/oxygen precipitation performance in an alkaline three-electrode system, the glassy carbon electrode coated with the nickel cobalt oxygen porous nanosheet composite material is used as a working electrode, a saturated calomel electrode is used as a reference electrode, a platinum sheet is used as a counter electrode, and a KOH solution is used as an electrolyte to form the three-electrode system.
The phase morphology of the catalyst used by the electrode is characterized by using transmission electron microscope Selected Area Electron Diffraction (SAED) and Transmission Electron Microscope (TEM), and the porous and hexagonal sheet-shaped nickel-cobalt-oxygen nano composite material prepared by the method basically has no agglomeration phenomenon.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation method provided by the invention realizes the preparation of the nickel-cobalt-oxygen porous nanosheet composite catalyst applied to the cathode of the air battery by using a coprecipitation and sintering method, and has the advantages of simple experimental steps and excellent electrode catalytic performance.
(2) The invention utilizes the battery cathode produced in industrialization, reduces the quality of the electrode slice, improves the electrode performance and is suitable for commercial application.
(3) The preparation method realizes the controllable adjustment of the porous and hexagonal sheet-shaped nickel-cobalt-oxygen composite material of the catalyst, and has great guiding significance for practical application.
Drawings
Fig. 1 is a diffraction diagram of the nickel-cobalt-oxygen porous nanosheet composite cathode catalyst prepared by the method.
Fig. 2 is a scanning diagram of the nickel-cobalt-oxygen porous nanosheet composite cathode catalyst prepared by the method.
Fig. 3 is a transmission electron microscope image of the nickel-cobalt-oxygen porous nanosheet composite cathode catalyst prepared by the method.
Fig. 4 is a transmission electron microscope image of the nickel-cobalt-oxygen porous nano-film composite cathode catalyst prepared by the method.
FIG. 5 is an oxygen precipitation performance curve of the nickel-cobalt-oxygen porous nanosheet composite cathode catalyst prepared by the method.
FIG. 6 is an oxygen reduction performance curve of the nickel-cobalt-oxygen porous nanosheet composite cathode catalyst prepared by the method.
Fig. 7 shows the oxygen precipitation stability of the nickel-cobalt-oxygen porous nanosheet composite cathode catalyst prepared by the method.
FIG. 8 shows the oxygen reduction stability of the nickel-cobalt-oxygen porous nanosheet composite cathode catalyst prepared by the method.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The invention relates to a nickel-cobalt-oxygen porous nanosheet composite catalyst applied to an air battery cathode, wherein the nickel-cobalt-oxygen nanosheet composite is made of Ni 0.6 Co 2.4 O 4 And NiO, wherein the diameter of the nano sheet is 110-150 nm, and the thickness of the nano sheet is 10-30 nm.
The preparation method of the nickel-cobalt-oxygen porous nanosheet composite material comprises the following steps:
1) dissolving cobalt nitrate and nickel nitrate in deoxidized deionized water, and stirring and dissolving in a gas protective atmosphere to obtain a mixed salt solution;
2) uniformly stirring the sodium hydroxide solution and the mixed salt solution at room temperature, centrifuging to obtain a precipitate, and cleaning with deionized water and absolute ethyl alcohol;
3) and (3) drying the precipitate obtained in the step (2) in vacuum to obtain a precursor, and sintering to obtain the nickel-cobalt-oxygen nanosheet composite catalyst for the cathode of the air battery.
The dosage of the cobalt nitrate and the nickel nitrate is 3-5 mmol and 12-20 mmol;
the dosage of the deionized water is 50 mL;
the protective gas in the step 1) is N 2 ，O 2 Or air; the stirring speed is 200-600 r/min, the time is 0.5-1.5 h, and the temperature is room temperature;
the dosage of the sodium hydroxide solution in the step 2) is 20-25 mL, and the concentration is 2-4.2 mol/L;
the temperature of the vacuum drying temperature in the step 3) is 25-35 ℃, and the drying time is 9-15 h; the sintering temperature is 300-375 ℃, and the sintering heat preservation time is 2.5-3 h.
Example 1
12mmoL of cobalt nitrate and 3mmoL of nickel nitrate were dissolved in 50mL of deionized water with oxygen removed in N 2 Stirring for 1.5h in protective atmosphere at the stirring speed of 200r/min to obtain mixed salt solution. Adding 25mL of 2M NaOH into the mixed salt solution, uniformly stirring, washing the obtained dark green precipitate with deionized water and absolute ethyl alcohol for three times, then placing the washed dark green precipitate into a vacuum oven, and drying the washed dark green precipitate for 10 hours at the temperature of 30 ℃ under the vacuum condition to obtain a precursor. And (2) putting the precursor into a well-type muffle furnace for sintering, wherein the heating rate is 3-4 ℃/min, the heat preservation temperature is 300 ℃, the heat preservation time is 3h, and cooling is carried out under the air cooling condition to obtain the hexagonal sheet-shaped nickel-cobalt-oxygen nanocomposite material with the surface being 5-20 nanometers, and the diameter being 130-150 nanometers.
The diffraction pattern of the nickel-cobalt-oxygen porous nanosheet composite material prepared in the above example is shown in fig. 1, and the inner ring and the outer ring respectively correspond to the crystal faces of nickel cobaltate and nickel oxide (220), which indicates that the catalyst consists of Ni 0.6 Co 2.4 O 4 And NiO two phases. A scanning electron microscope is shown in figure 2, which shows a hexagonal sheet structure of the nickel-cobalt-oxygen nanosheet composite material, a transmission electron microscope is shown in figure 3, the particle size of the nanosheet is 100-150 nanometers, and the structure is beneficial to exposing active sites and improving the activity of a catalyst.
The electrochemical performance research of the nickel-cobalt-oxygen porous nanosheet composite material comprises the following steps:
fig. 5 and 6 are graphs of oxygen evolution in nitrogen saturated 1.0mol/L KOH and oxygen reduction performance in oxygen saturated 0.1mol/L KOH, respectively, for the nickel-cobalt-oxygen porous nanosheet composite catalyst prepared in the above example. The oxygen precipitation activity of the nickel-cobalt-oxygen porous nanosheet composite material related to the invention is higher than that of the noble metal RuO 2 More excellent, and the oxygen reduction current is higher than that of commercial Pt/C at low potential. As shown in FIG. 7, the stability of oxygen evolution of the catalyst was measured at 10mA currentAfter 500min, the potential does not change obviously; in fig. 8, the stability of the nickel-cobalt-oxygen composite material is superior to that of Pt/C, which shows that the nickel-cobalt-oxygen composite material prepared by the present invention has excellent oxygen precipitation and oxygen reduction activity and stability as an oxygen electrode, and has good application prospects in electrolytic water, fuel cells and metal-air batteries.
Example 2
16mmoL of cobalt nitrate and 4mmoL of nickel nitrate were dissolved in 50mL of deionized water with oxygen removed in N 2 Stirring for 1h in protective atmosphere at the stirring speed of 400r/min to obtain a mixed salt solution. Adding 25mL of 2.7M NaOH into the mixed salt solution, uniformly stirring, washing the obtained dark green precipitate with deionized water and absolute ethyl alcohol for three times, then placing the washed dark green precipitate into a vacuum oven, and drying the washed dark green precipitate for 15 hours at the temperature of 25 ℃ under the vacuum condition to obtain a precursor. And (3) putting the precursor into a well-type muffle furnace for sintering, wherein the heating rate is 4-5 ℃/min, the heat preservation temperature is 325 ℃, the heat preservation time is 3h, and cooling is carried out under the air cooling condition to obtain the hexagonal plate-shaped nickel-cobalt-oxygen composite cathode catalyst with the long hole of 5-20 nanometers in surface and the diameter of 130-140 nanometers.
Example 3
20mmoL of cobalt nitrate and 5mmoL of nickel nitrate were dissolved in 50mL of deionized water with oxygen removed in N 2 Stirring for 0.5h in protective atmosphere at the stirring speed of 600r/min to obtain mixed salt solution. Adding 20mL of 4.2M NaOH into the mixed salt solution, stirring uniformly, washing the obtained dark green precipitate with deionized water and absolute ethyl alcohol for three times, then placing the washed dark green precipitate into a vacuum oven, and drying the washed dark green precipitate for 9 hours at the temperature of 35 ℃ under the vacuum condition to obtain a precursor. And (3) putting the precursor into a well-type muffle furnace for sintering, wherein the heating rate is 5-6 ℃/min, the heat preservation temperature is 350 ℃, the heat preservation time is 2.5h, and cooling is carried out under the air cooling condition to obtain the hexagonal plate-shaped nickel-cobalt-oxygen composite cathode catalyst with 10-20 nanometer macropores on the surface and 120-130 nanometer diameter.
Example 4
Dissolving 12mmoL of cobalt nitrate and 3mmoL of nickel nitrate in 50mL of deionized water with oxygen removed, and stirring for 1h in air atmosphere at the stirring speed of 400r/min to obtain a mixed salt solution. Adding 20mL of 2.5M NaOH into the mixed salt solution, uniformly stirring, washing the obtained dark green precipitate with deionized water and absolute ethyl alcohol for three times, then placing the washed dark green precipitate into a vacuum oven, and drying the washed dark green precipitate for 10 hours at the temperature of 30 ℃ under the vacuum condition to obtain a precursor. And (3) putting the precursor into a well-type muffle furnace for sintering, wherein the heating rate is 4-5 ℃/min, the heat preservation temperature is 375 ℃, the heat preservation time is 2.5h, and cooling is carried out under the air cooling condition to obtain the hexagonal plate-shaped nickel-cobalt-oxygen composite cathode catalyst with the surface being 20-30 nanometer macropores and the diameter being 110-120 nanometers.
Example 5
12mmoL of cobalt nitrate and 3mmoL of nickel nitrate were dissolved in 50mL of deionized water with oxygen removed in O 2 Stirring for 1h in protective atmosphere at the stirring speed of 400r/min to obtain a mixed salt solution. Adding 20mL of 2.5M NaOH into the mixed salt solution, uniformly stirring, washing the obtained dark green precipitate with deionized water and absolute ethyl alcohol for three times, then placing the washed dark green precipitate into a vacuum oven, and drying the washed dark green precipitate for 10 hours at the temperature of 30 ℃ under the vacuum condition to obtain a precursor. And (3) sintering the precursor in a well-type muffle furnace at the heating rate of 3-4 ℃/min and the heat preservation temperature of 300 ℃ for 3h, and cooling under the air cooling condition, as shown in a transmission electron microscope 4, so as to obtain the surface porous membrane-shaped nickel-cobalt-oxygen composite cathode catalyst.
All methods and techniques disclosed and suggested herein may be readily adapted by those skilled in the art to perform the procedures described herein, including by reference to the accompanying text, by appropriate changes in the materials and procedures, and although the methods and techniques of the present invention have been described in terms of preferred embodiments, it will be apparent to those skilled in the art that modifications and rearrangements of the methods and techniques described herein may be made to achieve the desired results without departing from the spirit, scope, or spirit of the invention. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and content of the invention.
Claims (4)
1. A preparation method of a nickel-cobalt-oxygen nanosheet composite material is provided, wherein the nickel-cobalt-oxygen nanosheet composite material is prepared from Ni 0.6 Co 2.4 O 4 And NiO, the diameter of the nano sheet is 100-150 nanometers, and the thickness of the nano sheet is 10-3 nanometers0 nm; the method is characterized by comprising the following steps:
1) dissolving cobalt nitrate and nickel nitrate in deoxidized deionized water in the presence of oxygen 2 Or stirring and dissolving in air protective atmosphere to obtain mixed salt solution;
2) adding a sodium hydroxide solution into the mixed salt solution, uniformly stirring at room temperature, centrifuging to obtain a precipitate, and cleaning with deionized water and absolute ethyl alcohol;
3) vacuum drying the precipitate obtained in the step 2) to obtain a precursor, and sintering to obtain the nickel-cobalt-oxygen nanosheet composite catalyst for the cathode of the air battery;
in the step 1), the use amounts of the nickel nitrate and the cobalt nitrate are respectively 3-5 mmol and 12-20 mmol; in the step 3), the sintering temperature is 300-375 ℃, and the corresponding sintering time is 2.5-3 h.
2. The method according to claim 1, wherein in the step 1), the stirring speed is 200 to 600r/min, and the stirring time is 0.5 to 1.5 hours.
3. The method as set forth in claim 1, wherein in the step 2), the concentration of the sodium hydroxide solution is 2 to 4.2mol/L.
4. The method as set forth in claim 1, wherein in the step 3), the vacuum drying temperature is 25 to 35 ℃ and the drying time is 9 to 15 hours.
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| CN111118564B (en) * | 2019-10-17 | 2021-06-11 | 天津大学 | Nickel-nickel oxide ultrathin nanosheet material and electrodeposition preparation method and application thereof |
| CN111732129B (en) * | 2020-01-13 | 2023-04-07 | 天津大学 | Preparation method and application of oxygen-assisted double hydroxide self-assembled thin-layer layered structure |
| CN114705737B (en) * | 2021-11-29 | 2024-02-06 | 苏州科技大学 | Nickel cobaltate nanosheet array composite material derived from metal organic framework modified on surface of carbon cloth and preparation and application thereof |
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| CN107293713A (en) * | 2017-06-19 | 2017-10-24 | 中国科学院长春应用化学研究所 | A kind of super-low-temperature lithium-ion cell composite positive pole and preparation method thereof |
| CN107910557A (en) * | 2017-10-20 | 2018-04-13 | 天津大学 | The preparation method of graphene-supported cobaltosic oxide nano crystal composite material and its application in zinc-air battery air cathode |
| CN108598502A (en) * | 2018-03-23 | 2018-09-28 | 广东工业大学 | A kind of Ni-Co metal oxides air cell electrode catalyst and its preparation method and application |
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