CN111193037A - Preparation method of aluminum-air battery cathode reduction catalyst - Google Patents

Preparation method of aluminum-air battery cathode reduction catalyst Download PDF

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CN111193037A
CN111193037A CN201911006990.9A CN201911006990A CN111193037A CN 111193037 A CN111193037 A CN 111193037A CN 201911006990 A CN201911006990 A CN 201911006990A CN 111193037 A CN111193037 A CN 111193037A
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zinc oxide
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air battery
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CN111193037B (en
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阙奕鹏
齐敏杰
雷少帆
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Chaowei Power Group Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H01M4/8825—Methods for deposition of the catalytic active composition
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
    • H01M4/9041—Metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M2004/8678—Inert electrodes with catalytic activity, e.g. for fuel cells characterised by the polarity
    • H01M2004/8689—Positive electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

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Abstract

The invention relates to the technical field of aluminum-air batteries, and discloses a preparation method of an aluminum-air battery cathode reduction catalyst, aiming at the problem of complex preparation process of the aluminum-air battery cathode reduction catalyst in the prior art, which comprises the following steps: (1) preparing carbon-supported zinc oxide: mixing zinc oxide and active carbon, adding absolute ethyl alcohol, ball-milling for 6-8h, sieving the materials and drying; (2) preparing an air electrode: mixing carbon-loaded zinc oxide with acetylene black, conductive carbon black and PTFE solution, and pressing into an air electrode; (3) reduction of zinc oxide: in sodium hydroxide solution, the pure zinc sheet reduces the zinc oxide in the electrode into zinc; (4) preparing a catalyst silver: soaking the electrode in silver nitrate solution for 15-18h, cleaning, and vacuum drying to obtain the final product. The invention adopts an in-situ method to prepare the catalyst, the particle size of the catalyst is nano-scale, the catalyst has strong binding force with carrier carbon and is uniformly dispersed, the catalytic activity is good, the preparation process is simple, and the synthesis cost is low.

Description

Preparation method of aluminum-air battery cathode reduction catalyst
Technical Field
The invention relates to the technical field of aluminum-air batteries, in particular to a preparation method of a cathode reduction catalyst of an aluminum-air battery.
Background
The aluminum-air battery is a novel battery which is composed of oxygen in the air as a cathode active substance, metal aluminum as an anode active substance and an inorganic electrolyte, the theoretical specific energy of the battery is up to 8135Wh/kg, and the actual specific energy of the battery is up to 900 Wh/kg; it also has the advantages of large capacity, long service life, safe use, environmental protection, and the like; and thus has received extensive attention from researchers since its birth, and is called "green energy for the 21 st century".
The core technology of the aluminum-air battery is a cathode, which provides a place for oxygen to carry out reduction reaction and has waterproof, breathable, conductive and catalytic effects. The typical air electrode mainly comprises a current collector layer, a waterproof breathable diffusion layer and a catalytic layer. The current research focus is mainly on the catalytic layer of the battery cathode, where the high efficiency and stability of the catalyst have received extensive attention in recent years.
Patent No. CN201510210531.8, entitled "preparation and application of oxygen reduction cathode catalyst for aluminum air battery", includes the following steps: dispersing chitosan with a certain mass in deionized water, slowly dropwise adding a proper amount of aqueous solution of transition metal salt, stirring at room temperature for 2 hours to allow the chitosan to be fully chelated, washing the metal chelate with the deionized water for 2-3 times, adding nitrogen sources with different mass ratios, continuously stirring for 2 hours, evaporating the water at 50 ℃, and drying the obtained sample in a vacuum drying oven for 12 hours for later use; placing a proper amount of dried sample in a porcelain boat, placing in a tube furnace, heating to 800 ℃ at a heating rate of 5 ℃/min under the protection of nitrogen, preserving heat for 2 hours, and then naturally cooling to room temperature to obtain a black powdery substance; then it was added to 20mL0.5mol/L of H2SO4Stirring the solution for 8 hours at 80 ℃, washing the solution for 2 to 3 times by using deionized water, performing suction filtration, and drying the solution for 12 hours at 60 ℃ to obtain the aluminum-air battery cathode oxygen reduction catalyst.
The method has the disadvantages of complex preparation process, long preparation process time, agglomeration in the sintering process and large particle size of the obtained catalyst.
Disclosure of Invention
The invention aims to solve the problems of larger particle size and complex preparation process of the aluminum air battery cathode reduction catalyst in the prior art, and provides a preparation method of the aluminum air battery cathode reduction catalyst.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the aluminum-air battery cathode reduction catalyst comprises the following preparation steps:
(1) and preparing carbon-supported zinc oxide: mixing nanoscale zinc oxide with active carbon, adding absolute ethyl alcohol as a ball milling medium, performing ball milling, sieving and drying the ball-milled material to obtain carbon-loaded zinc oxide;
(2) preparing an air electrode: mixing the carbon-loaded zinc oxide with acetylene black, conductive carbon black and a PTFE solution, and pressing to form an air electrode;
(3) reducing the zinc oxide of the air electrode: reducing zinc oxide into zinc by taking an air electrode as a cathode and a pure zinc sheet as an anode in a sodium hydroxide solution;
(4) and preparing a catalyst silver: preparing silver nitrate solution, soaking the electrode reduced into zinc in the silver nitrate solution, cleaning with deionized water, and drying under vacuum to obtain the finished product.
The nano silver has the following effects: providing a place for oxygen reduction, and reducing the reaction free energy of oxygen reduction; carbon black XC-72 is a carrier of the catalyst, and can disperse the action of the catalyst and provide larger reaction active area; acetylene black: the conductive function can be realized, and the air hole channels in the air electrode can be increased; conductive carbon black ks-6: the conductive function is achieved; in step (3), an electro-reduction method is adopted according to Zn2++2e ═ Zn principle to reduce the zinc oxide of the air electrode; the reaction generated in the step (4) is Zn +2AgNO3＝Zn(NO3)2+2Ag, silver is the cathode reduction catalyst. The catalyst prepared by the method has the advantages of silver particle size less than or equal to 100nm, good dispersibility and strong bonding force with carrier carbon, so that the discharge performance of the battery can reach the best.
Preferably, the mass ratio of the nano zinc oxide to the activated carbon in the step (1) is 0.7-0.9: 8-9, wherein the ball milling time is 6-8h, and the active carbon is carbon black XC-72.
Preferably, the particle size of the material obtained after ball milling and sieving in the step (1) is less than or equal to 5 microns.
Preferably, the drying temperature in the step (1) is 78-82 ℃, and the drying time is 11-13 h.
Preferably, the mass ratio of the step (2) is carbon-supported zinc oxide: acetylene black: conductive carbon black: PTFE solution 1.8-1.9: 0.09-0.1: 0.04-0.05: 1.5-1.6, wherein the mass content of PTFE in the PTFE solution is 58-60%, and the conductive carbon black is ks-6.
Preferably, the pressing conditions in step (2) are as follows: the temperature is 148 ℃ and 152 ℃, the pressure is 3.8-4.2MPa, and the time is 15-20 min.
Preferably, the concentration of the sodium hydroxide in the step (3) is 3.8-4 mol/L.
Preferably, the concentration of the silver nitrate solution in the step (4) is 0.05-0.06mol/L, and the soaking time is 15-18 h.
Preferably, the particle size of the catalyst silver obtained in the step (4) is less than or equal to 100 nm.
Preferably, the vacuum drying temperature in the step (4) is 100 ℃ and 110 ℃, and the vacuum drying time is 2-2.5 h.
Therefore, the invention has the following beneficial effects:
(1) the catalyst prepared in situ has uniform particle size distribution, so that the specific surface area of the catalyst is increased, and the activity of the whole catalyst is enhanced;
(2) the particle size of the catalyst is in a nanometer level, the specific surface area of the catalyst is large, the catalyst can be fully contacted with the cathode material of the aluminum air battery, and the catalyst has strong binding force with carrier carbon and is uniformly dispersed;
(3) the catalytic activity is good, so that the cathode has higher electrode potential, the working voltage of the battery with higher potential is higher, the voltage is higher, the specific energy of the battery is higher, and the number of batteries connected in series can be reduced;
(4) the preparation process is simple, the synthesis period is short, the controllability of the process steps is good, the synthesis cost is low, and the synthesis efficiency is high.
Detailed Description
The invention is further described with reference to specific embodiments.
Example 1
The preparation method of the aluminum-air battery cathode reduction catalyst is characterized by comprising the following preparation steps:
(1) and preparing carbon-supported zinc oxide: mixing 0.749g of nano-zinc oxide and 8.99g of carbon black XC-72, adding 30ML of absolute ethyl alcohol as a ball milling medium, carrying out ball milling for 7 hours, sieving the ball-milled materials, drying the materials at 80 ℃ for 12 hours, and obtaining the carbon-loaded zinc oxide with the particle size of less than or equal to 5 micrometers;
(2) preparing an air electrode: mixing the 1.801g of carbon-loaded zinc oxide with 0.0956g of acetylene black, 0.0449g of conductive carbon black ks-6 and 1.55g of PTFE solution with the mass content of 60 percent, and pressing into an air electrode, wherein the pressing conditions are as follows: the temperature is 150 ℃, the pressure is 4MPa, and the time is 18 min;
(3) reducing the zinc oxide of the air electrode: according to Zn2+Adopting an electro-reduction method to reduce zinc oxide into zinc by taking an air electrode as a cathode and a pure zinc sheet as an anode in 30mL of 3.9mol/L sodium hydroxide solution;
(4) and preparing a catalyst silver: preparing silver nitrate solution, soaking the electrode reduced into zinc in the silver nitrate solution with the concentration of 0.055mol/L for 16h at normal temperature, cleaning with deionized water, and vacuum drying at 105 ℃ for 2.2h to obtain the finished product, wherein the particle size of the obtained catalyst silver is less than or equal to 100 nm.
Example 2
The difference from the example 1 is that the preparation method comprises the following preparation steps:
(1) and preparing carbon-supported zinc oxide: mixing 0.724g of nano-zinc oxide and 8.28g of carbon black XC-72, adding 30ML of absolute ethyl alcohol as a ball milling medium, carrying out ball milling for 6.5 hours, sieving the ball-milled materials, drying the materials at 79 ℃ for 11.5 hours, and obtaining the carbon-loaded zinc oxide, wherein the particle size of the obtained materials is less than or equal to 5 micrometers;
(2) preparing an air electrode: mixing the 1.836g of carbon-loaded zinc oxide with 0.0944g of acetylene black, 0.0428g of conductive carbon black ks-6 and 1.53g of PTFE with the mass content of 58 percent, and pressing into an air electrode under the following conditions: the temperature is 149 ℃, the pressure is 3.9MPa, and the time is 16 min;
(3) reducing the zinc oxide of the air electrode: according to Zn2++2e- ═ Zn by electroreduction in a 3.9mol/L sodium hydroxide solutionThe gas electrode is a cathode, and the pure zinc sheet is an anode to reduce zinc oxide into zinc;
(4) and preparing a catalyst silver: preparing silver nitrate solution, soaking the electrode reduced into zinc in the silver nitrate solution with the concentration of 0.053mol/L for 15.5h at normal temperature, cleaning with deionized water, and vacuum drying at 103 ℃ for 2.2h to obtain the finished product, wherein the particle size of the obtained catalyst silver is less than or equal to 100 nm.
Example 3
The difference from the example 1 is that the preparation method comprises the following preparation steps:
(1) and preparing carbon-supported zinc oxide: mixing 0.786g of nano-zinc oxide and 8.68g of carbon black XC-72, adding 30ML of absolute ethyl alcohol as a ball milling medium, carrying out ball milling for 7.5 hours, sieving the ball-milled materials, drying the materials at 81 ℃ for 12.5 hours, and obtaining carbon-loaded zinc oxide with the particle size of the obtained materials being less than or equal to 5 micrometers;
(2) preparing an air electrode: mixing 1.882g of carbon-loaded zinc oxide with 0.0964g of acetylene black, 0.0484g of conductive carbon black ks-6 and 1.58g of PTFE solution with the mass content of 60 percent, and pressing into the air electrode, wherein the pressing conditions are as follows: the temperature is 151 ℃, the pressure is 4.1MPa, and the time is 18 min;
(3) reducing the zinc oxide of the air electrode: according to Zn2+Adopting an electro-reduction method to reduce zinc oxide into zinc by taking an air electrode as a cathode and a pure zinc sheet as an anode in a sodium hydroxide solution with the concentration of 3.9 mol/L;
(4) and preparing a catalyst silver: preparing silver nitrate solution, soaking the electrode reduced into zinc in the silver nitrate solution with the concentration of 0.058mol/L for 17 hours at normal temperature, cleaning with deionized water, and vacuum drying at 108 ℃ for 2.4 hours to obtain a finished product, wherein the particle size of the obtained catalyst silver is less than or equal to 100 nm.
Example 4
The difference from the example 1 is that the preparation method comprises the following preparation steps:
(1) and preparing carbon-supported zinc oxide: mixing 0.7g of nano-zinc oxide and 8g of carbon black XC-72, adding 30ML of absolute ethyl alcohol as a ball milling medium, carrying out ball milling for 6 hours, sieving the ball-milled materials, drying the materials at 78 ℃ for 11 hours, and obtaining the carbon-loaded zinc oxide with the particle size of less than or equal to 5 micrometers;
(2) preparing an air electrode: mixing the 1.8g of carbon-loaded zinc oxide with 0.09g of acetylene black, 0.04g of conductive carbon black ks-6 and 1.5g of PTFE solution with the mass content of 58 percent, and pressing to form the air electrode, wherein the pressing conditions are as follows: the temperature is 148 ℃, the pressure is 3.8MPa, and the time is 15 min;
(3) reducing the zinc oxide of the air electrode: according to Zn2+Adopting an electro-reduction method to reduce zinc oxide into zinc by taking an air electrode as a cathode and a pure zinc sheet as an anode in a sodium hydroxide solution with the concentration of 3.8 mol/L;
(4) and preparing a catalyst silver: preparing silver nitrate solution, soaking the electrode reduced into zinc in the silver nitrate solution with the concentration of 0.05mol/L for 15h at normal temperature, cleaning with deionized water, and vacuum drying at 100 ℃ for 2h to obtain a finished product, wherein the particle size of the obtained catalyst silver is less than or equal to 100 nm.
Example 5
The difference from the example 1 is that the preparation method comprises the following preparation steps:
(1) and preparing carbon-supported zinc oxide: mixing 0.9g of nano-zinc oxide and 9g of carbon black XC-72, adding 30ML of absolute ethyl alcohol as a ball milling medium, carrying out ball milling for 8 hours, sieving the ball-milled materials, drying the materials at 82 ℃ for 13 hours, and obtaining the carbon-loaded zinc oxide with the particle size of less than or equal to 5 micrometers;
(2) preparing an air electrode: mixing the 1.9g of carbon-loaded zinc oxide with 0.1g of acetylene black, 0.05g of conductive carbon black ks-6 and 1.6g of a solution of PTFE with the mass content of 58%, and pressing to obtain the air electrode, wherein the pressing conditions are as follows: the temperature is 152 ℃, the pressure is 4.2MPa, and the time is 20 min;
(3) reducing the zinc oxide of the air electrode: according to Zn2+Adopting an electro-reduction method to reduce zinc oxide into zinc by taking an air electrode as a cathode and a pure zinc sheet as an anode in a sodium hydroxide solution with the concentration of 4 mol/L;
(4) and preparing a catalyst silver: preparing silver nitrate solution, soaking the electrode reduced into zinc in the silver nitrate solution with the concentration of 0.06mol/L for 18h at normal temperature, cleaning with deionized water, and vacuum drying at 110 ℃ for 2.5h to obtain a finished product, wherein the particle size of the obtained catalyst silver is less than or equal to 100 nm.
Comparative example 1
The difference from the example 1 is that the ball milling process is omitted in the process of preparing the carbon-supported zinc oxide in the step (1).
Comparative example 2
The difference from example 1 is that the concentration of the silver nitrate solution in step (4) exceeds the maximum upper limit of 0.15 mol/L.
Comparative example 3
The difference from example 1 is that the soaking time in the silver nitrate solution at normal temperature in the step (4) is only 10 hours in a short time.
The resulting data are shown in table 1:
TABLE 1 electrode potential of battery materials at an electrolyte temperature of 45 deg.C
Figure BDA0002243073700000051
And (4) conclusion: in examples 1 to 5, the catalyst prepared within the parameter range of the invention has small silver particle size, good dispersibility, a positive oxygen electrode polarization potential, strong bonding force with carrier carbon and long oxygen electrode life.
The negative electrode potential shift degree in the comparative examples 1-3 is increased, and for the comparative example 1, because the ball milling process is not carried out, the oxygen electrode prepared by the catalyst obtained by the method has poor bonding strength, is easy to fall off and has short service life; for the comparative example 2, the concentration of silver nitrate is too high, most of the catalyst prepared by the method is concentrated on the surface of the oxygen electrode, the production of internal silver particles is blocked, the effective area of catalytic reaction is reduced, and the polarization potential of the oxygen electrode is relatively negative; for comparative example 3, the amount of silver catalyst prepared by this method was small, the oxygen electrode polarization potential was negative, the performance of the catalyst was poor, and the catalytic efficiency was low because the soaking time in silver nitrate solution was not sufficient.
It can be seen from the data of examples 1-5 and comparative examples 1-3 that the above requirements can be satisfied in all aspects only by the schemes within the scope of the claims of the present invention, resulting in optimized schemes and resulting in aluminum air cell cathode reduction catalysts with optimal performance. The change of the mixture ratio, the replacement/addition/subtraction of raw materials or the change of the feeding sequence can bring corresponding negative effects.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.

Claims (10)

1. The preparation method of the aluminum-air battery cathode reduction catalyst is characterized by comprising the following preparation steps:
(1) and preparing carbon-supported zinc oxide: mixing nanoscale zinc oxide with active carbon, adding absolute ethyl alcohol as a ball milling medium, performing ball milling, sieving and drying the ball-milled material to obtain carbon-loaded zinc oxide;
(2) preparing an air electrode: mixing the carbon-loaded zinc oxide with acetylene black, conductive carbon black and a PTFE solution, and pressing to form an air electrode;
(3) reducing the zinc oxide of the air electrode: reducing zinc oxide into zinc by taking an air electrode as a cathode and a pure zinc sheet as an anode in a sodium hydroxide solution;
(4) and preparing a catalyst silver: preparing silver nitrate solution, soaking the electrode reduced into zinc in the silver nitrate solution, cleaning with deionized water, and drying under vacuum to obtain the finished product.
2. The method for preparing the cathode reduction catalyst of the aluminum-air battery as claimed in claim 1, wherein the mass ratio of the nano zinc oxide to the activated carbon in the step (1) is 0.7-0.9: 8-9, wherein the ball milling time is 6-8h, and the active carbon is carbon black XC-72.
3. The method for preparing an aluminum-air battery cathode reduction catalyst according to claim 1 or 2, wherein the particle size of the material obtained after ball milling and sieving in the step (1) is not more than 5 μm.
4. The method for preparing an aluminum-air battery cathode reduction catalyst according to claim 1, wherein the drying temperature in the step (1) is 78-82 ℃ and the drying time is 11-13 h.
5. The method for preparing an aluminum-air battery cathode reduction catalyst according to claim 1, wherein the mass ratio of the zinc oxide on carbon: acetylene black: conductive carbon black: PTFE solution = 1.8-1.9: 0.09-0.1: 0.04-0.05: 1.5-1.6, wherein the mass content of PTFE in the PTFE solution is 58-60%, and the conductive carbon black is ks-6.
6. The method for preparing an aluminum-air battery cathode reduction catalyst according to claim 1, wherein the pressing conditions in the step (2) are as follows: the temperature is 148 ℃ and 152 ℃, the pressure is 3.8-4.2MPa, and the time is 15-20 min.
7. The method for preparing an aluminum-air battery cathode reduction catalyst according to claim 1, wherein the concentration of the sodium hydroxide in the step (3) is 3.8 to 4 mol/L.
8. The method for preparing an aluminum-air battery cathode reduction catalyst according to claim 1, wherein the concentration of the silver nitrate solution in the step (4) is 0.05 to 0.06mol/L, and the soaking time is 15 to 18 hours.
9. The method for preparing an aluminum-air battery cathode reduction catalyst according to claim 1, wherein the particle size of the catalyst silver obtained in the step (4) is 100nm or less.
10. The method for preparing an aluminum-air battery cathode reduction catalyst as recited in claim 1, wherein the vacuum drying temperature in step (4) is 100-.
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