CN111769297B - Cathode catalyst of aluminum-air battery and preparation method thereof - Google Patents
Cathode catalyst of aluminum-air battery and preparation method thereof Download PDFInfo
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- H01M12/00—Hybrid cells; Manufacture thereof
- H01M12/04—Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type
- H01M12/06—Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type with one metallic and one gaseous electrode
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Abstract
The invention discloses an aluminum-air battery cathode catalyst and a preparation method thereof, wherein the preparation method comprises the steps of adding an Ag source compound, a Ni source compound, an acid-base buffer, a reducing agent and a surfactant into a solvent, mixing, and carrying out solvothermal reaction to obtain a reaction solution; adding a Mn source compound and a C source into the reaction liquid obtained in the step one, and carrying out ultrasonic stirring to obtain a catalyst precursor; drying, ball-milling and sieving a catalyst precursor to obtain precursor powder; and calcining and cooling the precursor powder to obtain the aluminum-air battery cathode catalyst. The preparation method is simple, the raw materials are low in price, and the production cost of the battery material is greatly reduced; moreover, the Ag-Ni double-doped carbon-supported manganese catalyst is prepared, the catalytic activity is further improved on the basis of keeping the high catalytic activity of the Ag-based catalyst, and the oxygen reduction performance is excellent, so that the discharge performance of the aluminum-air battery is improved.
Description
Technical Field
The invention relates to the technical field of aluminum-air batteries, in particular to an aluminum-air battery cathode catalyst and a preparation method thereof.
Background
With the exhaustion of fossil energy, the development of new energy is becoming urgent. The metal-air battery uses active metal as an anode to carry out electron losing reaction, absorbs oxygen in the air as a cathode to carry out oxygen reduction reaction, does not discharge any pollution in the discharging process of the battery, and is a clean and efficient energy system. The theoretical energy density of the aluminum-air battery is only lower than that of the lithium-air battery in the metal-air battery, and compared with the metal lithium, the aluminum resource is more abundant and the price is low, so the aluminum-air battery has wide application prospect.
The serious polarization of the air electrode is a major problem affecting the industrial production of the aluminum-air battery at present. This is due to the low activity of the catalyst. The noble metals of platinum and silver have high oxygen reduction catalytic performance, but the commercialization process of the aluminum-air battery is greatly limited due to the high price of the noble metals.
Therefore, how to increase the catalytic activity of the cathode catalyst and reduce the production cost of the battery material is one of the problems to be solved urgently in the aluminum-air battery.
Disclosure of Invention
The invention provides an aluminum-air battery cathode catalyst and a preparation method thereof, and the Ag-Ni double-doped carbon-supported manganese catalyst is prepared and used as the aluminum-air battery cathode catalyst, so that the high catalytic activity of the Ag-based catalyst is maintained, and the production cost of a battery material is greatly reduced. At least part of the technical problems are solved. Specifically, the present invention includes the following.
In a first aspect of the present invention, there is provided a method for preparing a cathode catalyst for an aluminum-air battery, comprising the steps of:
adding an Ag source compound, a Ni source compound, an acid-base buffer, a reducing agent and a surfactant into a solvent, mixing, and carrying out solvothermal reaction to obtain a reaction solution;
adding a Mn source compound and a C source into the reaction liquid obtained in the step one, and performing ultrasonic stirring to obtain a catalyst precursor;
drying, ball-milling and sieving the catalyst precursor to obtain precursor powder;
and step four, calcining and cooling the precursor powder to obtain the aluminum-air battery cathode catalyst.
Preferably, the dosage of the Ag source compound is 1-5 g, the dosage of the Ni source compound is 1-5 g, the dosage of the acid-base buffer agent is 10-50 mL, the dosage of the reducing agent is 5-10 mL, the dosage of the surfactant is 5-10 g, the dosage of the solvent is 10-50 mL, the dosage of the Mn source compound is 2-10 g, and the dosage of the C source is 2-10 g.
In certain exemplary embodiments, the Ag source compound is silver nitrate and/or silver acetate and the Ni source compound is nickel nitrate and/or nickel acetate.
In certain exemplary embodiments, the acid-base buffer is selected from one or more of urea, ammonium chloride, aqueous ammonia, and ammonium carbonate.
In certain exemplary embodiments, the reducing agent is hydrogen peroxide or hydrazine hydrate.
In certain exemplary embodiments, the surfactant is selected from one of tetrabutylammonium bromide, sodium dodecylbenzenesulfonate, cetyltrimethylammonium bromide, and polyethylene glycol.
In certain exemplary embodiments, the Mn source compound is manganese nitrate and/or manganese acetate and the C source is selected from one or more of activated carbon, acetylene black, carbon nanotubes, and graphene.
Due to the unique electronic arrangement, multiple valence state distribution and excellent oxygen adsorption and reduction performance of the transition metals Mn and Ni, the finally prepared catalyst further improves the catalytic activity on the basis of keeping the high catalytic activity of the Ag-based catalyst.
In certain exemplary embodiments, the solvent is deionized water or absolute ethanol.
In certain exemplary embodiments, in the first step, the temperature of the solvothermal reaction is 20 to 100 ℃ and the time of the solvothermal reaction is 0.5 to 40 hours. The apparatus for the solvothermal reaction of the present invention is not particularly limited, and the reaction may be carried out by using a solvothermal reaction apparatus known to those skilled in the art. In the invention, the solution reaction device is arranged in a fume hood for carrying out.
In certain exemplary embodiments, in the second step, the time of ultrasonic agitation is 0.5 to 40 hours. The speed of ultrasonic stirring is not limited in any way, and stirring is carried out at a stirring speed which is well known to those skilled in the art, so that the aim of uniformly mixing is fulfilled.
In certain exemplary embodiments, in the third step, the drying temperature is 50 to 150 ℃, the drying time is 10 to 500min, and the ball milling time is 10 to 200 min. The invention does not have any special limitation on the aperture of the screen to be screened, a screening device well known to those skilled in the art is adopted, and the aperture of the screen is set according to the actual requirement.
In certain exemplary embodiments, in the fourth step, the calcination temperature is 100 to 500 ℃ and the calcination time is 10 to 500 min. The cooling method of the present invention is not particularly limited, and a cooling method known to those skilled in the art is used. In the present invention, natural cooling may be specifically selected.
In a second aspect of the invention, the aluminum-air battery cathode catalyst obtained by the preparation method of the first aspect of the invention is provided.
The invention has the beneficial effects that:
the invention provides a preparation method of an aluminum-air battery cathode catalyst, which is simple in preparation method and low in raw material price, and greatly reduces the production cost of battery materials; moreover, the Ag-Ni double-doped carbon-supported manganese catalyst is prepared, the catalytic activity is further improved on the basis of keeping the high catalytic activity of the Ag-based catalyst, and the oxygen reduction performance is excellent, so that the discharge performance of the aluminum-air battery is improved.
Drawings
Fig. 1 is an XRD pattern of an aluminum air cell cathode catalyst obtained by an exemplary preparation method of the present invention.
Fig. 2 is a graph comparing the discharge patterns of the cathode catalyst of the aluminum-air battery obtained by using the exemplary preparation method of the present invention and the aluminum-air battery using Ag as the cathode catalyst at different current densities.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that the upper and lower limits of the range, and each intervening value therebetween, is specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
Example 1
Step one, 1g of silver nitrate and 1.5g of nickel nitrate are taken and added into 20ml of deionized water for dissolving, then a proper amount of urea is added for adjusting the pH value of the solution, a proper amount of hydrogen peroxide is slowly added as a reducing agent, and a proper amount of polyethylene glycol is used as a surfactant; reacting in water bath at 50 ℃ for 30min to obtain reaction liquid;
step two, adding 5g of manganese nitrate and 5g of activated carbon into the reaction solution obtained in the step one, and ultrasonically stirring for 1 hour to obtain a catalyst precursor;
step three, putting the catalyst precursor into an oven to be dried for 120min at the temperature of 80 ℃, transferring the dried solid into a ball mill to be ball-milled for 60min, and sieving to obtain precursor powder;
and step four, putting the precursor powder into a crucible, calcining the precursor powder in a muffle furnace at 200 ℃ for 180min, and naturally cooling to obtain the Ag-Ni double-doped carbon-supported manganese catalyst, thus obtaining the aluminum-air battery cathode catalyst.
Example 2
Step one, 1.5g of silver acetate and 1g of nickel acetate are taken and added into 20ml of deionized water for dissolution, then a proper amount of ammonium carbonate is added for adjusting the pH value of the solution, a proper amount of hydrazine hydrate is slowly added as a reducing agent, and a proper amount of sodium dodecyl benzene sulfonate is used as a surfactant; reacting in water bath at 90 ℃ for 50min to obtain reaction liquid;
step two, adding 10g of manganese acetate and 5g of acetylene black into the reaction solution obtained in the step one, and ultrasonically stirring for 40min to obtain a catalyst precursor;
step three, putting the catalyst precursor into an oven to be dried for 300min at 120 ℃, transferring the dried solid into a ball mill to be ball-milled for 50min, and sieving to obtain precursor powder;
and step four, putting the precursor powder into a crucible, calcining for 60min at 400 ℃ in a muffle furnace, and naturally cooling to obtain the Ag-Ni double-doped carbon-supported manganese catalyst, namely the aluminum-air battery cathode catalyst.
Example 3
Step one, 1.5g of silver acetate and 1g of nickel nitrate are taken and added into 10ml of absolute ethyl alcohol for dissolving, then a proper amount of ammonia water is added for adjusting the pH value of the solution, a proper amount of hydrogen peroxide is slowly added as a reducing agent, and a proper amount of hexadecyl trimethyl ammonium bromide is used as a surfactant; reacting in water bath at 60 deg.C for 50min to obtain reaction solution;
step two, adding 10g of manganese acetate and 5g of carbon nano tube into the reaction solution obtained in the step one, and ultrasonically stirring for 30min to obtain a catalyst precursor;
step three, putting the catalyst precursor into an oven to be dried for 500min at 60 ℃, transferring the dried solid into a ball mill to be ball-milled for 50min, and sieving to obtain precursor powder;
and step four, putting the precursor powder into a crucible, calcining for 360min at 500 ℃ in a muffle furnace, and naturally cooling to obtain the Ag-Ni double-doped carbon-supported manganese catalyst, namely the aluminum-air battery cathode catalyst.
FIG. 1 is an XRD pattern of the cathode catalyst of the aluminum-air battery prepared in examples 1-3, and it can be confirmed through crystal form confirmation that the XRD pattern of the catalyst prepared by the invention is Ag simple substance, Ni simple substance, MnO and Mn 3 O 4 And C, so that the Ag-Ni double-doped carbon-supported manganese catalyst is obtained.
The Ag-Ni double-doped carbon-supported manganese catalyst prepared in examples 1 to 3 and the noble metal Ag were respectively prepared into an air electrode, a cathode film, an electrolyte, an aluminum anode and the like, and the air electrode, the cathode film, the electrolyte and the aluminum anode were assembled into an aluminum-air battery, and discharge was performed at different current densities. As shown in FIG. 2, the discharge results indicate that the use of different current densitiesThe discharge voltage and power density of the aluminum-air battery with the cathode catalyst are higher than those of the aluminum-air battery with noble metal Ag as the catalyst, and the performance of the aluminum-air battery with the cathode catalyst exceeds that of the aluminum-air battery with noble metal Ag as the catalyst. 100mA/cm 2 During discharging, the discharge voltage reaches 1.25V, and the power density reaches 125mW/cm 2 。
While the present invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. Many modifications and variations may be made to the exemplary embodiments of the present description without departing from the scope or spirit of the present invention. The scope of the claims is to be accorded the broadest interpretation so as to encompass all modifications and equivalent structures and functions.
Claims (7)
1. A preparation method of an aluminum-air battery cathode catalyst is characterized by comprising the following steps:
adding an Ag source compound, a Ni source compound, an acid-base buffer, a reducing agent and a surfactant into a solvent, mixing, and carrying out solvothermal reaction to obtain a reaction solution; the reducing agent is hydrogen peroxide or hydrazine hydrate;
step two, adding a Mn source compound and a C source into the reaction liquid obtained in the step one, and performing ultrasonic stirring to obtain a catalyst precursor;
drying, ball-milling and sieving the catalyst precursor to obtain precursor powder;
calcining and cooling the precursor powder to obtain the aluminum-air battery cathode catalyst;
the method comprises the following steps of A, preparing a silver source compound, namely a silver nitrate and/or silver acetate, and preparing a Ni source compound, namely nickel nitrate and/or nickel acetate; and secondly, the Mn source compound is manganese nitrate and/or manganese acetate, and the C source is selected from one or more of activated carbon, acetylene black, carbon nano tubes and graphene.
2. The method for preparing an aluminum-air battery cathode catalyst according to claim 1, wherein the acid-base buffer is one or more selected from urea, ammonium chloride, aqueous ammonia, and ammonium carbonate.
3. The method of preparing an aluminum-air battery cathode catalyst according to claim 1, wherein the surfactant is one selected from the group consisting of tetrabutylammonium bromide, sodium dodecylbenzenesulfonate, cetyltrimethylammonium bromide and polyethylene glycol.
4. The method for preparing the cathode catalyst of the aluminum-air battery according to claim 1, wherein in the first step, the temperature of the solvothermal reaction is 20-100 ℃, and the time of the solvothermal reaction is 0.5-40 h; in the second step, the time of ultrasonic stirring is 0.5-40 h.
5. The method for preparing the cathode catalyst of the aluminum-air battery according to claim 1, wherein in the third step, the drying temperature is 50-150 ℃, the drying time is 10-500 min, and the ball milling time is 10-200 min.
6. The method for preparing the cathode catalyst of the aluminum-air battery according to claim 1, wherein in the fourth step, the calcination temperature is 100 to 500 ℃ and the calcination time is 10 to 500 min.
7. An aluminum-air battery cathode catalyst, characterized by being obtained by the production method according to any one of claims 1 to 6.
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| CN113270594B (en) * | 2021-05-19 | 2022-11-18 | 郑州佛光发电设备股份有限公司 | Preparation method of waterproof breathable film, waterproof breathable film and application |
| CN114388822B (en) * | 2022-01-11 | 2024-02-09 | 华东师范大学重庆研究院 | Aluminum air battery cathode C@Ni@MnO 2 Catalytic material and preparation method thereof |
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