CN113948726A - Flexible dual-functional electrocatalyst for zinc-air battery and preparation method thereof - Google Patents
Flexible dual-functional electrocatalyst for zinc-air battery and preparation method thereof Download PDFInfo
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- CN113948726A CN113948726A CN202111126994.8A CN202111126994A CN113948726A CN 113948726 A CN113948726 A CN 113948726A CN 202111126994 A CN202111126994 A CN 202111126994A CN 113948726 A CN113948726 A CN 113948726A
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- H—ELECTRICITY
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Abstract
The invention discloses a preparation method of a flexible bifunctional electrocatalyst and application of the flexible bifunctional electrocatalyst in a zinc-air battery. The catalyst is a carbon cloth coated with metal organic frame gel through high-temperature pyrolysis, and a carbon nanotube array bifunctional electrocatalyst material coated with cobalt nanoparticles grows in situ on the surface of a flexible carbon cloth fiber. The method comprises the following specific steps: mixing zinc nitrate, cobalt nitrate, an organic ligand, N-dimethylformamide and the like to form MOF gel, then coating the MOF gel on gauze, and then pyrolyzing the gauze at high temperature in a nitrogen atmosphere to generate the carbon cloth fiber loaded carbon nanotube array bifunctional electrocatalyst material coated with cobalt nanoparticles. The prepared bifunctional electrocatalyst is a carbon nano tube array structure grown by carbon cloth fibers, a conductive network with a high specific surface area can be directly formed by the structure, electron rapid transfer in a catalysis process is promoted, a mass transfer process in catalysis is facilitated, and meanwhile metal particles are coated in the carbon nano tube array, so that uniform active sites are formed, and the catalysis performance of the catalyst is improved.
Description
Technical Field
The invention belongs to the technical field of zinc-air battery catalysts, and particularly relates to a flexible dual-function electrocatalyst for a zinc-air battery and a preparation method thereof.
Background
The metal zinc has high compatibility with air and water, and the safety and low cost of the zinc-air battery are ensured due to the abundant storage amount of zinc in the earth crust. At the same time, the zinc-air cell can provide a relatively high energy density (1086Wh/kg) and good cell voltage (1.65V). Therefore, the zinc-air battery has received a wide range of scientific community. Meanwhile, the zinc-air battery combines the functions of a fuel battery and a lithium ion battery, and has great research significance and application prospect in sustainable and clean energy storage equipment, particularly portable and flexible equipment.
The zinc-air battery consists of four parts of a zinc metal electrode, an air cathode, a membrane separator and electrolyte, wherein in the discharging process of the zinc-air battery, the metal Zn electrode loses electrons to generate an oxidation reaction of an anode, O2An Oxygen Reduction Reaction (ORR) occurs at the air cathode by diffusion, and an Oxygen Evolution Reaction (OER) occurs at the air cathode during charging, however the kinetics of these two reactions are slow. Therefore, the development of a flexible dual-function electrocatalyst for a zinc-air battery becomes a research hotspot in the technical field of zinc-air battery catalyst synthesis.
The Metal Organic Frameworks (MOFs) are materials which are formed by connecting metal ions/clusters and organic ligands through coordination bonds and have periodic porous structures, have the characteristics of high specific surface area, special porosity, topology, adjustability of components and the like, and have great prospects in the field of electrocatalysis application. However, the catalyst prepared by directly pyrolyzing the MOFs and the derivatives thereof at high temperature is easy to cause the collapse of the pore structure, the prepared catalyst is usually a powder material, and not only can the corresponding electrode material be prepared by using a binder, but also the development of the technology is restricted by the characteristics that the powder catalyst is difficult to recover in use, easy to polymerize and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a flexible bifunctional electrocatalyst for a zinc-air battery, aiming at the defects in the prior art. The bifunctional electrocatalyst is an array carbon nanotube framework structure grown by carbon cloth fibers, and the structure can directly form a conductive network with a high specific surface area, promote the rapid transfer of electrons in a catalysis process, is favorable for a mass transfer process in catalysis, simultaneously provides countless attachment places for metal particles, forms uniform active sites, and improves the catalysis performance of the catalyst.
The technical scheme adopted by the invention for solving the problems is as follows:
a preparation method of a flexible bifunctional electrocatalyst for a zinc-air battery mainly comprises the following steps:
(1) mixing zinc salt, cobalt salt and organic ligand in a solvent to form metal organic framework gel (MOFs gel) under the action of triethylamine;
(2) coating the metal organic framework gel on gauze, and growing the carbon nano tube array bifunctional electrocatalyst material coated with the cobalt nano particles in situ through high-temperature pyrolysis in a nitrogen atmosphere, namely the flexible bifunctional electrocatalyst for the zinc-air battery.
According to the scheme, the zinc salt is selected from one or more of zinc nitrate, zinc acetate, zinc sulfate, zinc chloride, zinc acetylacetonate and the like.
According to the scheme, the cobalt salt is selected from one or more of cobalt nitrate, cobalt acetate, cobalt sulfate, cobalt chloride, cobalt acetylacetonate and the like.
According to the scheme, the organic ligand is dimethyl imidazole, terephthalic acid, mellitic acid and the like.
According to the scheme, the solvent is N, N-dimethylformamide, methanol, ethanol and the like.
According to the scheme, in the step (1), the molar ratio of zinc ions to cobalt ions in zinc salt and cobalt salt is 1: 1-2, and the molar ratio of zinc ions to cobalt ions to organic ligands is 1: 1-2: 4-5; the concentration of zinc ions in the solvent is 0.4-0.5 mol/L.
According to the scheme, in the step (1), the adding concentration range of triethylamine in the solvent is 2-4 mol/L.
According to the scheme, in the step (1), the solvent content of the metal organic framework gel is 50-60 wt%.
According to the scheme, in the step (2), the coating thickness of the metal organic framework gel on the gauze is 200-500 mu m.
According to the scheme, in the step (2), the temperature of high-temperature pyrolysis is 850-950 ℃, the heat preservation time is 2-4 h, and the heating rate is preferably 2 ℃/min.
Compared with the prior art, the invention has the following beneficial effects:
1. the carbon nanotube array bifunctional electrocatalyst material coated with the cobalt nanoparticles and loaded by the flexible carbon cloth fibers has a large specific surface area, and is beneficial to exposure of active sites, and meanwhile, a conductive network formed is beneficial to a mass transfer process, so that the electrocatalytic activity of the zinc-air battery is effectively improved.
2. The catalyst prepared by the invention has the characteristic of flexibility, can be used for preparing a flexible zinc-air battery, timely releases stress and adjusts volume change in the continuous charging and discharging process of the zinc-air battery, effectively inhibits electrochemical corrosion and swelling or shrinkage of the catalyst, and greatly improves the cycle stability of the zinc-air battery.
3. The prepared flexible carbon cloth fiber loaded carbon nanotube array bifunctional electrocatalyst material coated with cobalt nanoparticles uses MOFs gel coated on a cheap gauze carrier, and has the advantages of simple synthesis method, high reaction efficiency, low cost, good catalyst fixing effect and flexibility.
4. The catalyst prepared by the method directly realizes the solidification of the catalyst, maintains the high activity of the powder, is beneficial to the recycling of the catalyst, and has great application prospect in zinc-air batteries.
Drawings
FIG. 1 is a photograph of MOFs gel obtained in example 1.
Fig. 2 is a flexible bending picture of the carbon nanotube array bifunctional electrocatalyst material coated with cobalt nanoparticles loaded on the flexible carbon cloth fiber obtained in example 1.
Fig. 3 is an SEM image of the carbon nanotube array bifunctional electrocatalyst material coated with cobalt nanoparticles loaded on the flexible carbon cloth fiber obtained in example 1.
Fig. 4 is a test chart of orr (a) and oer (b) of the bifunctional electrocatalyst material for a carbon nanotube array coated with cobalt nanoparticles loaded on the flexible carbon cloth fiber obtained in example 1.
Fig. 5 is a charge-discharge curve diagram of the zinc-air battery prepared by using the carbon nanotube array bifunctional electrocatalyst material coated with cobalt nanoparticles and loaded on the flexible carbon cloth fibers obtained in example 1.
Detailed Description
In order to better understand the invention, the following embodiments further illustrate the content of the invention, but the invention is not limited to the following embodiments, and all the technologies based on the above content of the invention are within the scope of the invention.
Example 1
The preparation method of the flexible bifunctional electrocatalyst for the zinc-air battery comprises the following specific steps:
1.7489g (0.006mol) of zinc nitrate and 2.619g (0.009mol) of cobalt nitrate are dissolved in 6mL of DMF and are subjected to ultrasonic treatment for 0.5h to obtain a uniform and stable solution; 1.9704g (0.024mol) of dimethylimidazole were dissolved in 6mL of DMF and sonicated for 0.5h to give a homogeneous stable solution. Mixing the two, adding triethylamine (the concentration of the triethylamine in the mixed solution is 2mol/L), standing for 0.5h to obtain the MOF gel, wherein the prepared gel is shown in figure 1.
And (3) coating the prepared gel on gauze in a scraping manner, wherein the thickness of the gel is 200 mu m, then placing the gauze in a tubular furnace for carbonization treatment in the argon atmosphere, namely heating to 900 ℃ at the speed of 2 ℃/min, preserving the temperature for 3 hours, and naturally cooling to room temperature to obtain the carbon nanotube array bifunctional electrocatalyst material coated with cobalt nanoparticles and loaded on flexible carbon cloth fibers, namely the flexible bifunctional electrocatalyst for the zinc-air battery.
As can be seen from fig. 2(a) and 2(b), the prepared flexible catalytic material still has no brittle fracture and good flexibility when bent at 180 °.
Fig. 3 is an SEM image of the flexible bifunctional electrocatalyst for zinc-air battery obtained in example 1, in which fig. 3(a) shows a carbon nanotube material uniformly grown on the surface of the carbon cloth fiber, and fig. 3(b) is a partially enlarged view of fig. 3(a), from which it can be seen that the carbon nanotube is coated with large cobalt particles on the top. The catalyst has a carbon nano tube network structure coated with cobalt nano particles and a conductive network with high specific surface area, can promote the rapid transfer of electrons in the catalysis process, and is beneficial to the mass transfer process in the catalysis.
The flexible bifunctional electrocatalyst for zinc-air battery prepared in example 1 was cut into 1 × 1cm square pieces as working electrodes to test OER performance in 1M KOH solution, ORR performance in 0.1M KOH solution saturated with oxygen, and the performance of the catalyst was measured by electrochemical workstation using three-electrode system, and the results of the electrocatalytic performance test are shown in fig. 4. As can be seen from fig. 4 (a): the carbon nano tube array bifunctional electrocatalyst material coated with cobalt nano particles and loaded by carbon cloth fibers has the initial potential of 0.91V, the half-wave potential of 0.82V and the limiting current density of 6.2mA cm at the rotation speed of 1600rpm of an alkaline and rotating disk electrode-2From FIG. 4(b), it can be seen that the carbon cloth fiber loaded cobalt nanoparticle coated carbon nanotube array bifunctional electrocatalyst material is at 10mA cm-2The overpotential at the current density of (2) is 350mV, which indicates that the catalyst has good ORR&OER catalytic performance.
The flexible bifunctional electrocatalyst for the zinc-air battery prepared in example 1 was used as a catalytic layer of an air electrode of the zinc-air battery, zinc foil was used as an anode, nickel foam was used as a gas diffusion layer, and 6.0M KOH and 0.20M ZnCl were used2The results of the cycle performance tests performed on the zinc-air cells assembled with the electrolyte are shown in fig. 5. As can be seen from fig. 5, the discharge voltage of the zinc-air battery is 1.15V, the charge voltage is 2.15V, and the performance of the battery is still stable after 2 hours of circulation, which indicates that the prepared carbon cloth fiber-loaded cobalt nanoparticle-coated carbon nanotube array bifunctional electrocatalyst material has excellent zinc-air battery performance.
Example 2
1.7489g (0.006mol) of zinc nitrate and 1.0621g (0.006mol) of cobalt acetate are dissolved in 6mL of DMF and are subjected to ultrasonic treatment for 0.5h to obtain a uniform and stable solution; 1.9704g (0.024mol) of dimethylimidazole were dissolved in 6mL of DMF and sonicated for 0.5h to give a homogeneous stable solution. And mixing the two, adding 0.03mol of triethylamine, and standing for 0.5h to obtain the MOF gel. And (3) coating the prepared gel on gauze, then placing the gauze in a tubular furnace for carbonization treatment in argon atmosphere, namely heating to 850 ℃ at the speed of 2 ℃/min, preserving the temperature for 3 hours, and naturally cooling to room temperature to obtain the carbon cloth fiber-loaded carbon nanotube array bifunctional electrocatalyst material coated with cobalt nanoparticles, namely the flexible bifunctional electrocatalyst for the zinc-air battery.
Example 3
1.7489g (0.006mol) of zinc nitrate and 0.9300g (0.006mol) of cobalt sulfate are dissolved in 6mL of DMF, and ultrasonic treatment is carried out for 0.5h to obtain a uniform and stable solution; 1.9704g (0.024mol) of dimethylimidazole were dissolved in 6mL of DMF and sonicated for 0.5h to give a homogeneous stable solution. And mixing the two, adding 0.04mol of triethylamine, and standing for 0.5h to obtain the MOF gel. And (3) coating the prepared gel on gauze, then placing the gauze in a tubular furnace for carbonization treatment in an argon atmosphere, namely heating to 950 ℃ at the speed of 2 ℃/min, preserving the heat for 3 hours, and naturally cooling to room temperature to obtain the flexible carbon cloth fiber-loaded carbon nanotube array bifunctional electrocatalyst material coated with cobalt nanoparticles, namely the flexible bifunctional electrocatalyst for the zinc-air battery.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, many modifications and changes can be made without departing from the inventive concept of the present invention, and these modifications and changes are within the protection scope of the present invention.
Claims (10)
1. A preparation method of a flexible bifunctional electrocatalyst for a zinc-air battery is characterized by mainly comprising the following steps:
(1) mixing zinc salt, cobalt salt and an organic ligand in a solvent to form metal organic framework gel under the action of triethylamine;
(2) coating the metal organic framework gel on gauze, and growing the carbon nano tube array bifunctional electrocatalyst material coated with the cobalt nano particles in situ through high-temperature pyrolysis in a nitrogen atmosphere, namely the flexible bifunctional electrocatalyst for the zinc-air battery.
2. The method for preparing the flexible bifunctional electrocatalyst for the zinc-air battery according to claim 1, wherein the zinc salt is selected from one or more of zinc nitrate, zinc acetate, zinc sulfate, zinc chloride and zinc acetylacetonate.
3. The method for preparing the flexible bifunctional electrocatalyst for a zinc-air battery according to claim 1, wherein the cobalt salt is selected from one or more of cobalt nitrate, cobalt acetate, cobalt sulfate, cobalt chloride and cobalt acetylacetonate.
4. The preparation method of the flexible bifunctional electrocatalyst for the zinc-air battery according to claim 1, wherein the organic ligand is one or more of dimethylimidazole, terephthalic acid and mellitic acid.
5. The preparation method of the flexible bifunctional electrocatalyst for a zinc-air battery according to claim 1, wherein the solvent is one or more of N, N-dimethylformamide, methanol and ethanol.
6. The preparation method of the flexible bifunctional electrocatalyst for the zinc-air battery according to claim 1, wherein in the step (1), the molar ratio of zinc ions to cobalt ions in zinc salt and cobalt salt is 1: 1-2, and the molar ratio of zinc ions to cobalt ions to organic ligands is 1: 1-2: 4-5; the concentration of zinc ions in the solvent is 0.4-0.6 mol/L.
7. The preparation method of the flexible bifunctional electrocatalyst for the zinc-air battery according to claim 1, wherein in the step (1), the addition concentration range of triethylamine in the solvent is 2-4 mol/L; the solvent content of the metal organic framework gel is 50-60 wt%.
8. The method for preparing a flexible bifunctional electrocatalyst for a zinc-air battery according to claim 1, wherein in the step (2), the coating thickness of the metal-organic framework gel on the gauze is 200 to 500 μm.
9. The preparation method of the flexible bifunctional electrocatalyst for the zinc-air battery according to claim 1, wherein in the step (2), the temperature of the high-temperature pyrolysis is 850-950 ℃, the heat preservation time is 2-4 h, and the temperature rise rate is 1-3 ℃/min.
10. A flexible bifunctional electrocatalyst for zinc-air battery prepared according to the method of claim 1.
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| CN108736031A (en) * | 2018-05-21 | 2018-11-02 | 同济大学 | A kind of self-supporting PtCo alloy nanoparticle catalyst and the preparation method and application thereof |
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