CN112993280B - Preparation method of microporous layer of gas diffusion layer of lithium air battery - Google Patents
Preparation method of microporous layer of gas diffusion layer of lithium air battery Download PDFInfo
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- CN112993280B CN112993280B CN202110265775.1A CN202110265775A CN112993280B CN 112993280 B CN112993280 B CN 112993280B CN 202110265775 A CN202110265775 A CN 202110265775A CN 112993280 B CN112993280 B CN 112993280B
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- mixed slurry
- ptfe
- microporous layer
- slurry
- film
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 16
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000009792 diffusion process Methods 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 22
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 22
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 20
- 239000011268 mixed slurry Substances 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002002 slurry Substances 0.000 claims abstract description 15
- 239000011230 binding agent Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000003085 diluting agent Substances 0.000 claims abstract description 8
- 239000002048 multi walled nanotube Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000006230 acetylene black Substances 0.000 claims abstract description 5
- 238000007865 diluting Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 4
- 238000007650 screen-printing Methods 0.000 abstract description 4
- 238000005507 spraying Methods 0.000 abstract description 2
- 238000010345 tape casting Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 10
- 239000011148 porous material Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000002238 carbon nanotube film Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- H01M4/8803—Supports for the deposition of the catalytic active composition
- H01M4/8807—Gas diffusion layers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M12/00—Hybrid cells; Manufacture thereof
- H01M12/08—Hybrid cells; Manufacture thereof composed of a half-cell of a fuel-cell type and a half-cell of the secondary-cell type
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inert Electrodes (AREA)
Abstract
The invention belongs to the field of lithium air batteries, and mainly relates to a preparation method of a microporous layer of a gas diffusion layer of a lithium air battery. Firstly, preparing mixed slurry, wherein the mixed slurry is prepared by mixing 25mg of acetylene black, 25mg of multi-wall carbon nano tubes and 500mg of 1% PTFE diluent, then adding the mixed slurry into 50ml of ethanol, stirring and mixing uniformly, or mixing 50mg of multi-wall carbon nano tubes and 500mg of 1% PTFE diluent, and then adding the mixed slurry into 50ml of ethanol, stirring and mixing uniformly; filtering the mixed slurry to form a film, and drying; and (3) sticking the film on carbon paper by using the corresponding slurry as a binder. Compared with the traditional knife coating method, the method reduces the influence of human factors, reduces the operation time and the operation difficulty compared with the spraying method, reduces the dependence on screen printing machines compared with the screen printing method, and is suitable for large-scale production.
Description
Technical Field
The invention belongs to the field of lithium air batteries, and mainly relates to an improvement of a preparation method of a microporous layer of a gas diffusion layer of a lithium air battery.
Background
Lithium air batteries are high specific capacity battery technologies that utilize the reversible reaction of lithium metal with oxygen in the air. The theoretical energy density upper limit reaches 11000Wh/Kg, which is far higher than the actual energy density of 200Wh/Kg of the current lithium ion battery. The gas diffusion layer plays important roles in supporting the catalytic layer, collecting current, conducting gas and blocking moisture in air in the lithium air battery. Plays an important role in the performance of the positive electrode catalyst of the lithium air battery.
The current preparation method of the gas diffusion layer is to knife-coat, spray and screen-print a layer of carbon black or carbon nano tube as a microporous layer on carbon paper. The microporous layer has high conductivity, low porosity and high hydrophobicity, and is an important part for ensuring that the gas diffusion layer collects current, conducts gas and blocks water in air. The method for adding the microporous layer by knife coating is to pour the carbon powder slurry on carbon paper, scrape the carbon powder slurry with a scraper and then dry the carbon powder slurry to prepare the microporous layer. The method for spraying and adding the microporous layer is to spray the carbon powder slurry on the carbon paper through a high-pressure spray gun and dry the carbon paper to prepare the microporous layer, and the microporous layer prepared by the method has good uniformity and long time consumption, usually takes more than 30 minutes, and is difficult to use on a large scale. The method for adding the microporous layer by screen printing adopts a screen printer to add the microporous layer on the carbon paper, and corresponding screen printing equipment is needed. Therefore, improvements to existing preparation methods are needed to simplify the preparation process and shorten the preparation time.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a preparation method of a microporous layer of a gas diffusion layer of a lithium air battery.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention provides a preparation method of a microporous layer of a gas diffusion layer of a lithium air battery, which comprises the following steps:
(1) Diluting PTFE solution:
diluting the PTFE concentrated solution with the mass fraction of 60% by deionized water to obtain PTFE diluted solution with the mass fraction of 1%;
(2) Preparing microporous layer slurry:
taking 25mg of acetylene black, 25mg of multi-wall carbon nano tubes and 500mg of 1% PTFE diluent, pouring the diluted solution into 50ml of ethanol, and carrying out ultrasonic stirring to prepare mixed slurry;
(3) Filtering the mixed slurry, forming a film, and drying;
(4) And (3) dropwise adding the mixed slurry prepared in the step (2) on carbon paper as a binder, and pressing the film prepared in the step (3) on the carbon paper for binding.
The invention also provides a preparation method of the microporous layer of the gas diffusion layer of the lithium air battery, which comprises the following steps:
(1) Diluting PTFE solution:
diluting the PTFE concentrated solution with the mass fraction of 60% by deionized water to obtain PTFE diluted solution with the mass fraction of 1%;
(2) Preparing microporous layer slurry:
pouring 50mg of multiwall carbon nanotubes and 500mg of 1% PTFE diluent into 50ml of ethanol, and stirring by ultrasonic to prepare mixed slurry;
(3) Filtering the mixed slurry, forming a film, and drying;
(4) And (3) dropwise adding the slurry prepared in the step (2) on carbon paper as a binder, and pressing the film prepared in the step (3) on the carbon paper for binding.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a novel microporous layer preparation method, which comprises the steps of firstly preparing a film from mixed slurry, and then sticking the prepared film on carbon paper by using the corresponding slurry as a binder. The microporous layer prepared by the method has high surface flatness, and the pore diameter of the microporous layer is effectively changed by controlling the type of carbon powder, so that the charge and discharge performance of the lithium air battery is further affected; the preparation method is simple and convenient, has short time consumption and is beneficial to large-scale industrial production for preparing the microporous layer on the carbon paper.
Drawings
FIG. 1 is a BET characterization of microporous layer of example 1;
FIG. 2 is a pore size distribution diagram of a microporous layer according to example 1;
FIG. 3 is a BET characterization of microporous layer of example 2;
FIG. 4 is a pore size distribution diagram of the microporous layer of example 2.
Detailed Description
The invention is further illustrated below in connection with specific examples, but is not limited in any way.
Example 1
1) Diluting the PTFE concentrated solution with the mass fraction of 60% to 1% by deionized water, and performing ultrasonic dispersion;
2) 25mg of acetylene black, 25mg of multi-wall carbon nano tubes and 500mg of 1% PTFE diluent are weighed and poured into 50ml of ethanol, and the mixture is stirred by ultrasonic waves to prepare mixed slurry. Filtering the slurry to form a film, and drying at 50-60 ℃.
3) And (3) dropwise adding a small amount of the slurry on commercial carbon paper to serve as a binder, and using a steel plate to adhere the prepared film on the carbon paper through the binder to obtain the microporous layer.
The membrane material was BET-characterized (fig. 1, fig. 2). As can be seen from the results of FIGS. 1 and 2, the microporous layer prepared in this example has a specific surface area of 120.807m 2 And/g, average pore diameter of 3.020nm. The thickness error of the prepared microporous layer measured by a micrometer is within 10 micrometers, and the flatness is good.
Example 2
1) Diluting the PTFE concentrated solution with the mass fraction of 60% to 1% by deionized water, and performing ultrasonic dispersion;
2) 50mg of multi-wall carbon nano tube and 500mg of 1% PTFE diluent are weighed and poured into 50ml of ethanol, and the mixture is stirred by ultrasonic waves to prepare mixed slurry. Filtering the slurry to form a film, and drying at 50-60 ℃.
3) And (3) dropwise adding a small amount of the slurry on commercial carbon paper to serve as a binder, and using a steel plate to adhere the prepared film on the carbon paper through the binder to obtain the microporous layer.
The membrane material was BET-characterized (fig. 3, fig. 4). As can be seen from the results of FIGS. 3 and 4, the microporous layer prepared in this example has a specific surface area of 184.699m 2 And/g, average pore diameter of 30.663nm. The thickness error of the prepared microporous layer measured by a micrometer is within 10 micrometers, and the flatness is good.
Table 1 comparing the specific surface area and the average pore diameter of the microporous layers prepared in example 1 and example 2, it can be seen that the pore diameter can be reduced and the specific surface area can be reduced by adding a small amount of acetylene black material to the microporous layer material. That is, the pore diameter and specific surface area of the microporous layer can be controllably changed by changing the content of carbon black in the microporous layer material.
TABLE 1 BET specific surface area and average pore size data for microporous layers
Specific surface area | Average pore diameter | |
Carbon nanotube and carbon black film | 120.807m 2 /g | 3.020nm |
Carbon nanotube film | 184.699m 2 /g | 30.663nm |
Many possible variations and modifications of the disclosed technology can be made by anyone skilled in the art without departing from the scope of the technology, or the technology can be modified to be equivalent. Therefore, any simple modification, equivalent variation and modification of the above embodiments according to the technical substance of the present invention shall still fall within the scope of the technical solution of the present invention.
Claims (2)
1. A method for preparing a microporous layer of a gas diffusion layer of a lithium air battery, which is characterized by comprising the following steps:
(1) Diluting PTFE solution:
diluting the PTFE concentrated solution with the mass fraction of 60% by deionized water to obtain PTFE diluted solution with the mass fraction of 1%;
(2) Preparing microporous layer slurry:
taking 25mg of acetylene black, 25mg of multi-wall carbon nano tubes and 500mg of 1% PTFE diluent, pouring the diluted solution into 50ml of ethanol, and carrying out ultrasonic stirring to prepare mixed slurry;
(3) Filtering the mixed slurry, forming a film, and drying;
(4) And (3) dropwise adding the mixed slurry prepared in the step (2) on carbon paper as a binder, and pressing the film prepared in the step (3) on the carbon paper for binding.
2. A method for preparing a microporous layer of a gas diffusion layer of a lithium air battery, which is characterized by comprising the following steps:
(1) Diluting PTFE solution:
diluting the PTFE concentrated solution with the mass fraction of 60% by deionized water to obtain PTFE diluted solution with the mass fraction of 1%;
(2) Preparing microporous layer slurry:
pouring 50mg of multiwall carbon nanotubes and 500mg of 1% PTFE diluent into 50ml of ethanol, and stirring by ultrasonic to prepare mixed slurry;
(3) Filtering the mixed slurry, forming a film, and drying;
(4) And (3) dropwise adding the mixed slurry prepared in the step (2) on carbon paper as a binder, and pressing the film prepared in the step (3) on the carbon paper for binding.
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