CN115719816A - Preparation method of composite electrode for zinc-air battery - Google Patents
Preparation method of composite electrode for zinc-air battery Download PDFInfo
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- CN115719816A CN115719816A CN202211474441.6A CN202211474441A CN115719816A CN 115719816 A CN115719816 A CN 115719816A CN 202211474441 A CN202211474441 A CN 202211474441A CN 115719816 A CN115719816 A CN 115719816A
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Abstract
The present disclosure provides a method for preparing a composite electrode for a zinc-air battery, the method comprising: uniformly dispersing a monatomic metal catalyst into a mixed solution of a perfluorosulfonic acid polymer and ethanol to obtain a precursor A; dripping the precursor A onto a carbon carrier, and drying to obtain a precursor B; preparing a foam metal catalyst as a precursor C; and pressing the precursor B and the precursor C to obtain the composite electrode combining the oxygen reduction reaction catalyst and the oxygen evolution reaction catalyst. And (3) taking the zinc sheet as an anode and the composite electrode as a cathode to obtain the zinc-air battery. According to the composite electrode prepared by the invention, the porous foam metal catalyst is used, so that the air bubble discharge can be accelerated, the electron mass transfer capacity of the electrode can be accelerated, the three-dimensional structure can provide a larger active surface area and show better performance, the carbon carrier can effectively prevent the electrolyte from leaking, and the service life of the battery is prolonged.
Description
Technical Field
The disclosure relates to the technical field of electrocatalysis, in particular to a preparation method of a composite electrode for a zinc-air battery.
Background
The Zinc-Air Battery (ZAB) is also called as a Zinc-oxygen Air Battery, and is an environment-friendly Battery which has small volume, large charge capacity, small mass, normal operation in a wide temperature range, no corrosion, and safe and reliable operation. Rechargeable zinc-air battery with high energy density (1086 Wh kg) -1 ) The electrochemical energy storage technology has the advantages of low cost, safety, environmental protection and the like, and is considered to have great potential.
For rechargeable zinc-air batteries, it is necessary to develop a high-efficiency bifunctional catalyst to solve the slow kinetics of oxygen in oxygen reduction (ORR) and Oxygen Evolution Reaction (OER), thereby improving the charge-discharge efficiency of the battery and reducing energy loss.
Disclosure of Invention
The present disclosure provides a method for preparing a composite electrode for a zinc-air battery, so as to at least solve the above technical problems in the prior art.
According to a first aspect of the present disclosure, there is provided a method of preparing a composite electrode for a zinc-air battery, the method comprising:
uniformly dispersing a monatomic metal catalyst into a mixed solution of a perfluorosulfonic acid polymer and ethanol to obtain a precursor A;
dripping the precursor A onto a carbon carrier, and drying to obtain a precursor B;
preparing a foam metal catalyst as a precursor C;
and pressing the precursor B and the precursor C to obtain the composite electrode combining the oxygen reduction reaction catalyst and the oxygen evolution reaction catalyst.
In one embodiment, the monatomic metal catalyst is a nitrogen-doped monatomic metal.
In one embodiment, the ratio of the mass of the monatomic metal catalyst to the volume of the mixed solution is 4 to 6 mg.
In one embodiment, the volume ratio of the perfluorosulfonic acid-type polymer to ethanol is 1.
In one embodiment, the metal foam catalyst comprises: foamed nickel, foamed copper, foamed iron supported catalysts.
In one implementation mode, the precursor B is prepared by infrared lamp drying for 40-80min.
In one embodiment, the dropping amount of the precursor A dropped on the carbon paper is 0.5-1.2mg/cm 2 。
In one implementation mode, the monatomic metal catalyst is uniformly dispersed into the mixed solution of the perfluorosulfonic acid polymer and the ethanol by ultrasonic treatment, wherein the ultrasonic treatment time is 60-120min and the temperature is 20-30 ℃.
In one embodiment, the sizes of the laminating surfaces of the precursor B and the precursor C are the same, and the ratio of the thickness of the precursor B to the thickness of the precursor C is 1:3-5.
According to a second aspect of the present disclosure, there is provided a zinc-air battery having a zinc sheet as an anode and a composite electrode prepared by the above method as a cathode.
The disclosure provides a preparation method of a composite electrode for a zinc-air battery, which comprises the steps of dispersing a monatomic metal catalyst in a mixed solution of a perfluorosulfonic acid polymer and ethanol to prepare a precursor A; then dropwise adding the precursor A onto a carbon carrier, and drying to obtain a precursor B, wherein the precursor B is used as an oxygen reduction reaction catalyst; preparing a foam metal catalyst as a precursor C, and playing a role of an oxygen evolution reaction catalyst; and pressing the precursor B and the precursor C to obtain the composite electrode. And (3) taking the zinc sheet as an anode and the composite electrode as a cathode to obtain the zinc-air battery. The composite electrode prepared by the invention at least has the following beneficial effects:
(1) The composite cathode uses the porous foam metal catalyst to accelerate the discharge of bubbles and the electron mass transfer capacity of the electrode, the three-dimensional structure can provide larger active surface area and show better performance, and the carbon paper can effectively prevent the leakage of electrolyte and prolong the service life of the battery, so that the composite cathode has good electrochemical activity and high stability;
(2) The preparation method is simple and is beneficial to large-scale production;
(3) The composite electrode can be applied to the fields of organic catalysis, biological diagnosis and treatment and the like besides electrocatalysis.
It should be understood that the statements in this section do not necessarily identify key or critical features of the embodiments of the present disclosure, nor do they limit the scope of the present disclosure. Other features of the present disclosure will become apparent from the following description.
Drawings
The above and other objects, features and advantages of exemplary embodiments of the present disclosure will become readily apparent from the following detailed description, which proceeds with reference to the accompanying drawings. Several embodiments of the present disclosure are illustrated by way of example, and not by way of limitation, in the figures of the accompanying drawings and in which:
in the drawings, like or corresponding reference characters designate like or corresponding parts.
Fig. 1 shows a schematic flow chart of a method for manufacturing a composite electrode for a zinc-air battery according to an embodiment of the present disclosure;
fig. 2 shows a schematic structural diagram of a zinc-air cell of an embodiment of the disclosure;
fig. 3 shows a schematic discharge curve of a test cell of example 1 of the present disclosure;
figure 4 shows a schematic discharge curve of a test cell of example 2 of the present disclosure;
fig. 5 shows a schematic of the discharge curve of a test cell of comparative example 1 of the present disclosure.
Detailed Description
In order to make the objects, features and advantages of the present disclosure more apparent and understandable, the technical solutions in the embodiments of the present disclosure will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present disclosure, and it is apparent that the described embodiments are only a part of the embodiments of the present disclosure, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments disclosed herein without making any creative effort, shall fall within the protection scope of the present disclosure.
Currently, a single bifunctional catalyst is mostly adopted for the rechargeable zinc-air battery, for example, mu et al prepares a Co-Nx/C nanorod array catalyst with double functions of OER and ORR, and the catalyst has more excellent electrocatalytic performance to OER and ORR compared with a commercial catalyst (Liu S, liu X, mu S, et al. Chem. Eng.J.,2018,342, 163-170.). Although the bifunctional OER and ORR activities of Co-based catalysts have satisfied the needs for zinc-air battery activity, the durability and stability of transition metal catalysts have not yet satisfied the needs for zinc-air battery activity. This is mainly due to the decay of the catalytic activity caused by the dissolution and leaching of non-noble metals under strong electrolytes. (Deng D, yu L, bao X, et al, angew chem. Int.Ed.,2013,52,371-5) reported encapsulation of transition metal NPs into carbon materials with a stable carbon layer protecting the internal metals from corrosion and dissolution in harsh reaction environments. Electrons from the active metal can transfer to the carbon layer, and therefore, the carbon layer becomes a part of the catalyst, promoting O 2 The ORR and OER are initiated, however, when the armor layer is too thick, the inner NPs have little effect on the outer carbon shell. Thus, the carbon layer thickness is the primary factor in determining the catalytic activity of the armor catalyst. However, because the formation of the carbon layer is affected by various factors such as temperature, time, and environment, it is difficult to precisely control the thickness of the carbon layer, and the thicker layer also limits the transfer of electrons to the outer carbon layer, which is not conducive to achieving effective activity of the armor catalyst.
Based on the problem that the electrochemical activity and stability of the existing bifunctional catalyst are poor, the invention provides a composite electrode for a zinc-air battery, which is used for solving the technical problem.
The first aspect of the present invention provides a method for preparing a composite electrode for a zinc-air battery, as shown in fig. 1, the method comprises the following steps:
s1, uniformly dispersing a monatomic metal catalyst into a mixed solution of a perfluorosulfonic acid polymer (Nafion) and ethanol to obtain a precursor A;
wherein the monoatomic metal catalyst is nitrogen-doped monoatomic metal, the metal is one of zinc, manganese and platinum, and the volume ratio of the perfluorosulfonic acid polymer to the ethanol is 1:5. The monatomic metal catalyst is dispersed in the mixed solution by ultrasonic treatment for 60-120min at 20-30 ℃.
S2, dripping the precursor A onto a carbon carrier, and drying to obtain a precursor B;
the carbon carrier is used for providing a carrier support function for the catalyst, and can be carbon paper, carbon cloth, carbon felt and the like.
The dripping amount of the precursor A is 0.5-1.2mg/cm 2 For example, the size of the carbon paper is 3X 3cm, and the drop amount of the precursor A is 4.5-10.8mg.
S3, preparing a foam metal catalyst as a precursor C;
the foam metal precursor is a catalyst loaded by foam nickel, foam copper and foam iron.
And S4, pressing the precursor B and the precursor C to obtain the composite electrode combining the oxygen reduction reaction catalyst and the oxygen evolution reaction catalyst.
And combining the precursor B and the precursor C in a physical pressing mode to form the composite electrode, wherein the pressing surfaces of the precursor B and the precursor C have the same size, and the thickness ratio of the precursor B to the precursor C is 1:3-5.
As shown in fig. 2, which is a schematic structural diagram of a zinc-air battery, the zinc-air battery comprises a cathode and an anode, a zinc sheet is used as the anode, and a composite electrode prepared by the invention is used as the cathode.
The disclosure provides a preparation method of a composite electrode for a zinc-air battery, which comprises the steps of dispersing a monatomic metal catalyst in a mixed solution of a perfluorosulfonic acid polymer and ethanol to prepare a precursor A; then dropwise adding the precursor A onto a carbon carrier, and drying to obtain a precursor B which is used as an oxygen reduction reaction catalyst; preparing a foam metal catalyst as a precursor C, and playing a role of an oxygen evolution reaction catalyst; and pressing the precursor B and the precursor C to obtain the composite electrode. And (3) taking the zinc sheet as an anode and the composite electrode as a cathode to obtain the zinc-air battery. The composite cathode has good electrochemical activity and high stability.
The composite electrode of the present invention will be described in detail with reference to specific examples.
Example 1
A method for preparing a composite electrode for a zinc-air battery, i.e., a monoatomic metal catalyst (ORR) and foamed metal catalyst (OER) (SAC-Zn/NC, coPx), comprising the steps of:
(1) Preparation of monatomic metal catalyst precursor 1: adding 25mL of hydrochloric acid into 120mL of ultrapure water, then adding 100mg of zinc chloride into a beaker, adding 9g of melamine, stirring, transferring into an oil bath kettle, and evaporating at 110 ℃ to dryness to obtain a precursor 1;
(2) Preparation of monoatomic metal catalyst precursor 2: and (2) sintering the precursor 1 prepared in the step (1) in a muffle furnace, adding 1.5g of a sample into 50mL of buffer solution, performing ultrasonic treatment to uniformly disperse the sample, adding 0.7g of dopamine hydrochloride, performing full reaction, performing suction filtration, and drying in a vacuum oven. And sintering the dried precursor of 100mg in a tube furnace to obtain the monatomic metal catalyst, namely SAC-Zn/NC. Wherein the temperature of the vacuum oven is 70 ℃, and the heat preservation time is 12h; the temperature of the tube furnace is 900 ℃, the heating rate is 5 ℃/min, and the heat preservation time is 120min.
(3) Preparation of precursor A: weighing a certain amount of monoatomic metal catalyst, then adding a mixed solution of Nafion and ethanol, and performing ultrasonic treatment to uniformly disperse the mixed solution to obtain a precursor A;
(4) Preparation of precursor B: dropwise adding the dispersed precursor A on carbon paper with a certain size (for example, 3X 0.1 cm) for multiple times in a small amount, drying by using an infrared lamp, and continuously drying by using a vacuum oven to obtain a precursor B;
(5) Preparation of foam metal catalyst precursor 3: firstly, cutting foamed nickel into a size of 3 multiplied by 3cm, then respectively ultrasonically cleaning the foamed nickel by using acetone, hydrochloric acid, ethanol and ultrapure water for ten minutes, and then transferring the foamed nickel to a vacuum oven for drying to obtain a precursor of the foamed metal catalyst; wherein the temperature of the vacuum oven is 70 ℃, and the heat preservation time is 12h.
(6) Preparation of foam metal catalyst precursor 4: placing the precursor 3 prepared in the step (5) in a polytetrafluoroethylene reaction kettle containing a mixed solution of a cobalt source, ammonium fluoride and urea, keeping the hydrothermal temperature at 120 ℃ for 6 hours, cooling to room temperature, taking out, washing with ultrapure water and ethanol, and drying in a vacuum oven to obtain a precursor 4; wherein the temperature of the vacuum oven is 70 ℃, and the heat preservation time is 12h.
(7) Preparation of foam metal catalyst precursor C: respectively placing a phosphorus source (500 mg) and a precursor 4 (2 multiplied by 3 cm) at the upstream and the downstream of a tubular furnace, and obtaining a transition metal phosphide catalyst by adopting a vapor deposition method; wherein the temperature of the tubular furnace is 300 ℃, and the heating rate is as follows: 5 ℃/min and the heat preservation time is 120min.
(8) Preparing a composite electrode: physically combining the precursor B with a precursor C with a certain size to obtain a composite electrode;
performance testing of composite electrodes
The test is carried out by adopting a three-electrode system, a zinc sheet is taken as a reference electrode and a counter electrode, a composite electrode is taken as a working electrode, and the discharge curve of the test battery is shown in figure 3.
Example 2
A method for preparing a composite electrode for a zinc-air battery, i.e., a monoatomic metal catalyst (OER) and a foamed metal catalyst (ORR) (SAC-Mn/NC, niPx), comprising the steps of:
(1) Preparation of monatomic metal catalyst precursor 1: firstly, adding 25mL of hydrochloric acid into 120mL of ultrapure water, then adding 70mg of manganese chloride into a beaker, adding 9g of melamine, stirring, transferring into an oil bath kettle, and evaporating at 110 ℃ to dryness to obtain a precursor 1.
(2) Preparation of the monatomic metal catalyst precursor 2: and sintering the precursor 1 in a muffle furnace, adding 1.5g of sample into 50mL of buffer solution, performing ultrasonic treatment to make the sample uniform, adding 0.7g of dopamine hydrochloride, performing full reaction, performing suction filtration, and drying in a vacuum oven. And sintering the dried precursor of 100mg in a tube furnace to obtain the monatomic powder catalyst, namely SAC-Mn/NC. Wherein the temperature of the vacuum oven is 70 ℃, and the heat preservation time is 12h; the temperature of the tube furnace is 900 ℃, the heating rate is 5 ℃/min, and the heat preservation time is 120min.
(3) Preparation of precursor A: weighing a certain amount of monoatomic powder catalyst, then adding a mixed solution of Nafion and ethanol, and performing ultrasonic treatment to uniformly disperse the mixed solution to obtain a precursor A;
(4) Preparation of precursor B: dropwise adding the dispersed precursor A on carbon paper with a certain size (for example, 3 x 3 cm) for multiple times in a small amount, drying by using an infrared lamp, and continuously drying by using a vacuum oven to obtain a precursor B;
(5) Preparation of foam metal catalyst precursor 3: firstly, cutting foamed nickel into a size of 3 multiplied by 3cm, then respectively ultrasonically cleaning the foamed nickel for ten minutes by using acetone, hydrochloric acid, ethanol and ultrapure water, and then transferring the foamed nickel to a vacuum oven for drying to obtain a precursor 3; wherein the temperature of the vacuum oven is 70 ℃, and the heat preservation time is 12h.
(6) Preparation of foam metal catalyst precursor 4: placing the precursor 3 in a polytetrafluoroethylene reaction kettle containing a mixed solution of a nickel source, ammonium fluoride and urea, carrying out hydrothermal temperature of 120 ℃, keeping the temperature for 6 hours, cooling to room temperature, taking out, washing with ultrapure water and ethanol, and drying in a vacuum oven to obtain a precursor 4; wherein the temperature of the vacuum oven is 70 ℃, and the heat preservation time is 12h.
(7) Preparation of foam metal catalyst precursor C: respectively placing a phosphorus source (500 mg) and a precursor 4 (2 multiplied by 3 cm) at the upstream and the downstream of a tubular furnace, and obtaining a transition metal phosphide catalyst by adopting a vapor deposition method; wherein the temperature of the tubular furnace is 300 ℃, and the heating rate is as follows: 5 ℃/min and the heat preservation time is 120min.
(8) Preparing a composite electrode: physically combining the precursor B with a precursor C with a certain size to obtain a composite electrode;
performance testing of composite electrodes
The test is carried out by adopting a three-electrode system, a zinc sheet is taken as a reference electrode and a counter electrode, a composite electrode is taken as a working electrode, and the discharge curve of the test battery is shown in figure 4.
Comparative example
A method for preparing a composite electrode for a zinc-air cell, i.e. a monatomic metal catalyst (ORR) and a cellPreparation of Metal foam catalyst (OER) (Pt/C, cu) 2 P) comprising the steps of:
(1) Preparation of precursor A: weighing a certain amount of Pt/C powder catalyst, then adding a mixed solution of Nafion and ethanol, and performing ultrasonic treatment to uniformly disperse the mixed solution to obtain a precursor A;
(2) Preparation of precursor B: dropwise adding the dispersed precursor A on carbon paper with a certain size (3 multiplied by 3 cm) for a few times, drying by adopting an infrared lamp, and continuously drying by using a vacuum oven to obtain a precursor B;
(3) Preparation of foam metal catalyst precursor 3: firstly cutting the foamed nickel into a size of 3 multiplied by 3cm, then respectively ultrasonically cleaning the foamed nickel for ten minutes by using acetone, hydrochloric acid, ethanol and ultrapure water, and then transferring the foamed nickel to a vacuum oven for drying to obtain a precursor 3; wherein the temperature of the vacuum oven is 70 ℃, and the heat preservation time is 12h.
(4) Preparation of foam metal catalyst precursor 4: placing the precursor 3 in a polytetrafluoroethylene reaction kettle containing a mixed solution of copper nitrate, ammonium fluoride and urea, carrying out hydrothermal temperature of 120 ℃, keeping the temperature for 6 hours, cooling to room temperature, taking out, washing with ultrapure water and ethanol, and drying in a vacuum oven to obtain a precursor 4; wherein the temperature of the vacuum oven is 70 ℃, and the heat preservation time is 12h.
(5) Preparation of foam metal catalyst precursor C: respectively placing a phosphorus source (500 mg) and a precursor 4 (2 multiplied by 3 cm) at the upstream and the downstream of a tubular furnace, and obtaining a transition metal phosphide catalyst by adopting a vapor deposition method; wherein the temperature of the tubular furnace is 300 ℃, and the heating rate is as follows: 5 ℃/min and the heat preservation time is 120min.
(6) Preparing a composite electrode: physically combining the precursor B with a precursor C with a certain size to obtain a composite electrode;
performance testing of composite electrodes
The test is carried out by adopting a three-electrode system, a zinc sheet is taken as a reference electrode and a counter electrode, a composite electrode is taken as a working electrode, and the discharge curve of the test battery is shown in figure 5. By comparing the discharge curves of fig. 3 to 5, the composite electrodes prepared in examples 1 to 2 according to the present invention have electrochemical activity equivalent to that of the composite electrode prepared in comparative example 1, but are lower in cost and more economical than the noble metal used in the comparative example.
It should be understood that various forms of the flows shown above may be used, with steps reordered, added, or deleted. For example, the steps described in the present disclosure may be executed in parallel, sequentially, or in different orders, as long as the desired results of the technical solutions disclosed in the present disclosure can be achieved, and the present disclosure is not limited herein.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or to implicitly indicate the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present disclosure, "a plurality" means two or more unless specifically limited otherwise.
The above description is only for the specific embodiments of the present disclosure, but the scope of the present disclosure is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present disclosure, and all the changes or substitutions should be covered within the scope of the present disclosure. Therefore, the protection scope of the present disclosure should be subject to the protection scope of the claims.
Claims (10)
1. A preparation method of a composite electrode for a zinc-air battery is characterized by comprising the following steps:
uniformly dispersing a monatomic metal catalyst into a mixed solution of a perfluorosulfonic acid polymer and ethanol to obtain a precursor A;
dripping the precursor A onto a carbon carrier, and drying to obtain a precursor B;
preparing a foam metal catalyst as a precursor C;
and pressing the precursor B and the precursor C to obtain the composite electrode combining the oxygen reduction reaction catalyst and the oxygen evolution reaction catalyst.
2. The method of claim 1, wherein the monatomic metal catalyst is a nitrogen-doped monatomic metal.
3. The method according to claim 1, wherein the ratio of the mass of the monoatomic metal catalyst to the volume of the mixed solution is 4 to 6 mg.
4. The method of claim 1, wherein the volume ratio of perfluorosulfonic acid polymer to ethanol is 1.
5. The method of claim 1, wherein the metal foam catalyst comprises: foamed nickel, foamed copper, foamed iron supported catalysts.
6. The method according to claim 1, wherein the precursor B is prepared by infrared lamp drying for 40-80min.
7. The method of claim 1, wherein the precursor A is dripped onto the carbon paper in an amount of 0.5 to 1.2mg/cm 2 。
8. The method of claim 1, wherein the monatomic metal catalyst is uniformly dispersed into the mixed solution of the perfluorosulfonic acid-type polymer and ethanol by sonication for 60 to 120min at 20 to 30 ℃.
9. The method of claim 1, wherein the dimensions of the bonding surfaces of precursor B and precursor C are the same, and the ratio of the thickness of precursor B to the thickness of precursor C is 1:3-5.
10. A zinc-air cell, wherein the zinc-air cell comprises a zinc sheet as an anode and a composite electrode prepared by the method of any one of claims 1 to 9 as a cathode.
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| CN117219927A (en) * | 2023-09-20 | 2023-12-12 | 海南深远海新能源科技有限公司 | Zinc-air battery, composite electrode for zinc-air battery and preparation method of composite electrode |
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| CN117219927A (en) * | 2023-09-20 | 2023-12-12 | 海南深远海新能源科技有限公司 | Zinc-air battery, composite electrode for zinc-air battery and preparation method of composite electrode |
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