CN110165241B - Graphitized carbon-based corrosion-resistant microporous layer of fuel cell and preparation method thereof - Google Patents
Graphitized carbon-based corrosion-resistant microporous layer of fuel cell and preparation method thereof Download PDFInfo
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- CN110165241B CN110165241B CN201910373801.5A CN201910373801A CN110165241B CN 110165241 B CN110165241 B CN 110165241B CN 201910373801 A CN201910373801 A CN 201910373801A CN 110165241 B CN110165241 B CN 110165241B
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
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- H—ELECTRICITY
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Abstract
The invention relates to a corrosion-resistant fuel cell microporous layer based on graphitized carbon and a preparation method thereof. The invention overcomes the defects that the prior common conductive carbon black materials have poor corrosion resistance, and the screen printing method and the blade coating method can not accurately control the carbon loading amount and the carbon distribution, and the like, and the microporous layer prepared by the method has excellent performance, thereby not only greatly improving the corrosion resistance of the gas diffusion layer of the fuel cell, but also effectively improving the water vapor transmission capability of the fuel cell.
Description
Technical Field
The invention relates to the technical field of fuel cells, in particular to a fuel cell corrosion-resistant microporous layer based on graphitized carbon and a preparation method thereof.
Background
The fuel cell is used for mixing fuel (H) under the action of catalyst2、CH3OH or CH4) The chemical energy in (1) is directly converted into electric energy through electrochemical reaction. A fuel cell is a device that can continue to provide electrical energy, similar to, but more advantageous than, an internal combustion engine. The fuel cell generates electricity through conversion of chemical energy and electric energy, has high conversion efficiency and is not limited by Carnot cycle; mechanical movement does not exist in the power generation process of the fuel cell, and noise is not generated; the fuel cell uses hydrogen as fuel, produces water and heat through proton exchange, and may generate a very small amount of carbon dioxide and other substances based on different fuels, thereby being cleaner and more environment-friendly. In a word, the fuel cell has the advantages of no pollution, low noise, high conversion rate and the like, and is known as green and environment-friendly energy in the 21 st century.
The cost and durability of current fuel cells remains a key obstacle to their further use. The corrosion resistance of the fuel cell is improved, so that the fuel cell can stably run for a longer time, and the effective service life of the fuel cell is prolonged. Yan et al [ Yan QG, Toghiani H, Lee YW, Liang KW, Causey H.Effect of sub-free temperature on a PEM fuel cell performance, startup and fuel cell porosity.J Power Sources 2006; 160: 1242-50. it was found that when the fuel cell is operated at low temperature, the microporous layer becomes rough due to the destruction of the teflon coating by ice to thereby reduce the moisture transport ability, affecting the performance and durability of the fuel cell. During the long-time operation of the fuel cell, the microporous layer is gradually corroded, the gas and water transmission capacity is reduced, the water and gas transmission and distribution in the cell are greatly influenced, and the durability and the performance of the fuel cell are finally reduced.
As the demand for durability and performance of fuel cells increases, the corrosion resistance of the microporous layer becomes more and more important. At present, the corrosion of the microporous layer mainly comprises the oxidation corrosion of carbon under high voltage and the loss of PTFE, so that the structure of the microporous layer is damaged, the hydrophilicity and the hydrophobicity of the surface are influenced, and the water management capability is reduced. The corrosion resistance of the microporous layer can be improved by mixing corrosion-resistant substances, such as SanyingHou et al [ Hou S, Chi B, Liu G, et al, enhanced performance of proton exchange membrane cell by integrating catalytic chemicals-doped CNTs in a bed catalyst layer and a gas diffusion layer [ J ]. Electrochimica Acta,2017: S0013417318200 ] by adding nitrogen-containing carbon nanotubes in the microporous layer, the corrosion resistance is enhanced, and the performance of the fuel cell is improved. Another method for improving the corrosion resistance of the microporous layer is to change the structure of the microporous layer so as to enhance the water and gas management capability thereof, for example, yanzhuqiang et al [ CN106784883A ] prepares two microporous layers with different carbon loads by a blade coating method, so that the surface of the microporous layer is smoother, and the performance of the fuel cell is improved.
The method of making the microporous layer also affects battery performance and durability. Wangqian et al [ CN 106299398A ] prepared a microporous layer with a double-layer structure by adding a pore-forming agent and adopting a screen printing and spraying method, improved the porosity and the performance of the fuel cell, but the method is more complicated and has higher cost. The existing method for preparing the gas microporous layer of the fuel cell mainly comprises a screen printing method, a blade coating method and a spraying method, wherein the screen printing method can print uniformly but cannot accurately control the carbon loading capacity, the blade coating method can self-determine the surface appearance of the microporous layer but cannot control the carbon distribution, and the spraying method can accurately control the carbon loading capacity but cannot control the surface appearance. In summary, the three methods for preparing the microporous layer, which are common at present, have certain problems.
Disclosure of Invention
The present invention is directed to overcoming the above problems of the prior art and providing a graphitized carbon-based fuel cell microporous layer having excellent corrosion resistance, which is prepared by the following steps:
(a) preparing suspension slurry by using graphitized carbon, a water repellent solution and an organic solvent as raw materials; (b) and spraying the suspension slurry on a substrate, drying and sintering.
Further, the process of preparing the suspension slurry is specifically as follows: mixing the graphitized carbon, the water repellent solution and the organic solvent according to the proportion, mechanically stirring for 0.5-1h, and then carrying out ultrasonic treatment until a uniform suspension is formed.
Further, the mass ratio of the graphitized carbon to the water repellent solution is 50-80:1, and the mass fraction of the graphitized carbon in the suspension slurry is 1.5-2.5%.
Further, the water repellent solution is a polytetrafluoroethylene aqueous solution with the mass fraction of 60% -80%.
Further, the organic solvent is an alcohol solvent, and comprises at least one of ethanol, isopropanol and ethylene glycol.
Furthermore, the organic solvent is formed by mixing isopropanol and ethylene glycol according to the mass ratio of 50: 1.
Further, the graphitized carbon particles have a particle size of not more than 500nm and are mainly formed by agglomeration of primary graphitized mesoporous carbon having a diameter of about 35 nm.
Further, the substrate is carbon paper or carbon cloth.
Further, the pressure at the time of spraying the slurry suspension was (0.5-1.5) MPa, and the distance between the nozzle and the substrate was 15 cm.
Further, the spraying process is repeated for a plurality of times until the carbon loading of the microporous layer is 0.5-2.5mg/cm2。
Further, the drying temperature is 60-90 ℃, and the calcining parameters are as follows: n is a radical of2Keeping the temperature for 45min from room temperature to 120 ℃ at the heating rate of 5 ℃/min, heating to 350 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 30min, and naturally cooling to room temperature.
The microporous layer prepared according to the above method has a single-layer structure. The microporous layer is attached to the carbon paper and is composed mainly of graphitized carbon and PTFE.
The invention adopts graphitized carbon as the carbon material of the microporous layer, because the graphitized carbon has better corrosion resistance and hydrophobic property compared with common carbon powder (such as XC-72, graphite black and the like). The slurry components which are most suitable for spraying construction are determined through a large number of experimental comparisons, on one hand, the carbon loading in the microporous layer can be accurately controlled, and on the other hand, the distribution of carbon on carbon paper can be accurately controlled, so that the performance and the durability of the fuel cell are improved. Compared with the prior art, the invention has the following beneficial effects:
1) the invention uses the alcoholic solution containing the dispersing agent as the dispersing medium, improves the dispersing ability of the water repellent solution, thereby being capable of uniformly dispersing the nano-grade graphitized carbon to avoid the agglomeration of the graphitized carbon, and the uniformity of the suspension slurry directly determines whether the graphitized carbon can be uniformly dispersed on the carbon paper substrate;
2) according to the invention, nano-grade graphitized carbon is used for replacing the traditional commercial conductive carbon black, which is beneficial to improving the corrosion resistance of the microporous layer;
3) the invention uses the spraying process to prepare the microporous layer, and solves the problem that the traditional screen printing method and the scraping method can not accurately control the carbon loading and the carbon distribution;
4) the method greatly improves the water vapor transmission capability and the output performance of the fuel cell under high current density, and the maximum output power can be 1.79w/cm when the humidification is 100%/100%2。
Drawings
FIG. 1 is an SEM photograph (magnification 200) of a corrosion-resistant microporous layer obtained in example 1 of the present invention;
FIG. 2 is a graph of the performance of a single cell assembled using microporous layers prepared in example 2 and comparative example 1;
FIG. 3 is a graph of single cell performance using microporous layers prepared in example 2 and comparative example 2 as cathode gas diffusion layers;
fig. 4 is a graph showing the performance of a single cell using the microporous layer prepared in comparative examples 1-2 as a cathode gas diffusion layer.
Detailed Description
In order to make those skilled in the art fully understand the technical solutions and advantages of the present invention, the following embodiments are further described.
The graphitized carbon has the structural characteristics of large embedding height, uniform structure, few surface functional groups, few defects and the like, and is endowed with excellent corrosion resistance. The graphitized carbon used in the present invention is mainly formed by agglomeration of primary graphitized mesoporous carbon with a diameter of about 35nm, and this ordered structure has a high electrical conductivity.
Example 1
1) Uniformly mixing isopropanol and ethylene glycol according to the mass ratio of 50:1 to obtain an alcoholic solution. Sequentially adding 60 mass percent of polytetrafluoroethylene aqueous solution and graphitized carbon (the particle size is not more than 500nm) into the alcohol solution, wherein the mass ratio of the PTFE to the graphitized carbon is 1: 4. After the feeding is finished, the mechanical stirring is carried out for 0.5 to 1 hour, and then the ultrasonic treatment is carried out for about 0.5 hour until uniform suspension slurry is formed. The mass fraction of graphitized carbon in the suspension slurry was 2%.
2) Preparing carbon paper with the thickness of 190 micrometers, the length of 6.5cm and the width of 6cm, adding the suspension slurry prepared in the step (1) into a spray pen, and spraying the suspension slurry on the carbon paper, wherein the spraying parameters are as follows: the spraying pressure is 0.5MPa, and the spraying distance is 15 cm. And after the spraying is finished, drying the carbon paper in a drying oven at the temperature of 90 ℃, and weighing after the drying is finished. Repeating the steps of spraying, drying and weighing for several times until the carbon loading of the microporous layer reaches 0.5mg/cm2。
3) Placing the microporous layer obtained in the step (2) in a muffle furnace, filling nitrogen for protection, heating from room temperature to 120 ℃ at a heating rate of 5 ℃/min, and preserving heat for 45 min; continuously heating to 350 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 30 min; and finally, naturally cooling to room temperature to obtain the corrosion-resistant microporous layer.
The SEM photograph of the microporous layer is shown in fig. 1. As can be seen, the surface of the microporous layer exhibits a porous morphology, which contributes to the water and gas management capability of the fuel cell and the performance of the fuel cell.
Example 2
This embodiment is substantially the same as embodiment 1 except that: the carbon loading of the microporous layer is accurately controlled to be 1mg/cm2。
Example 3
This embodiment is substantially the same as embodiment 1 except that: the carbon loading of the microporous layer is accurately controlled to be 1.5mg/cm2。
Example 4
This embodiment is substantially the same as embodiment 1 except that: the carbon loading of the microporous layer is accurately controlled to be 2mg/cm2。
Example 5
This embodiment is substantially the same as embodiment 1 except that: the carbon loading of the microporous layer is accurately controlled to be 2.5mg/cm2。
Comparative example 1
1) Uniformly mixing isopropanol and ethylene glycol according to the mass ratio of 50:1 to obtain an alcoholic solution. Sequentially adding 60% of polytetrafluoroethylene aqueous solution and XC-72 (the particle size is not more than 500nm) into the alcoholic solution, wherein the mass ratio of PTFE to XC-72 is 1: 4. After the feeding is finished, the mechanical stirring is carried out for 0.5 to 1 hour, and then the ultrasonic treatment is carried out for about 0.5 hour until uniform suspension slurry is formed. The mass fraction of XC-72 in the suspension slurry was 2%.
2) Preparing carbon paper with the thickness of 190 micrometers, the length of 6.5cm and the width of 6cm, adding the suspension slurry prepared in the step (1) into a spray pen, and spraying the suspension slurry on the carbon paper, wherein the spraying parameters are as follows: the spraying pressure is 0.5MPa, and the spraying distance is 15 cm. And after the spraying is finished, drying the carbon paper in a drying oven at the temperature of 90 ℃, and weighing after the drying is finished. Repeating the steps of spraying, drying and weighing for a plurality of times until the carbon loading of the microporous layer reaches 1mg/cm2。
3) Placing the carbon paper obtained in the step (2) in a muffle furnace, filling nitrogen for protection, heating from room temperature to 120 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 45 min; continuously heating to 350 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 30 min; and finally, naturally cooling to room temperature to obtain the microporous layer.
Comparative example 2
Two sets of three-electrode systems are formed by respectively using the microporous layers prepared in the example 2 and the comparative example 1 as working electrodes, using graphite rods as counter electrodes and using calomel electrodes as reference electrodes. And (3) placing the three-electrode system in a 0.5mol/L sulfuric acid aqueous solution, heating in a constant-temperature water bath at 70 ℃, and performing accelerated corrosion test on the three-electrode system by adopting an i-t module of an electrochemical workstation, wherein the accelerated voltage is 1.3V, and the corrosion time is 72 h. And after the test is finished, soaking the microporous layer for 24 hours by using distilled water, taking out the microporous layer, and fully drying the microporous layer in an oven at the temperature of 80 ℃ to obtain the corroded microporous layer.
Comparative example 3
The anode gas diffusion layer (new energy of wuhan principle corporation) of a common commercial fuel cell, the microporous layers obtained in example 2, comparative example 1 and comparative example 2 (after accelerated corrosion) were used as the cathode gas diffusion layer, and a CCM (new energy of wuhan principle corporation) was added to assemble a single cell, and a cell performance test was performed. The battery performance test conditions are as follows: temperature 75 ℃ H2The Air humidification degree is 100 percent, H2And an Air pressure of 150 kPa.
Fig. 2 is a graph showing initial performance of a single cell assembled using microporous layers prepared in comparative example 1 and example 2. As can be seen from FIG. 2, the current density of the battery of example 2 was 3500mA/cm when the voltage was 0.5V2The power density is 1.79w/cm2While the current density of the cell of comparative example 1 was 2300mA/cm2The power density is 1.19w/cm2The difference between the two performances is very obvious.
The results of cell performance tests assembled using the microporous layers obtained in examples, comparative example 2 as the cathode gas diffusion layer and the microporous layers obtained in comparative examples 1 to 2 as the cathode gas diffusion layer are shown in fig. 3 to 4. As can be seen from FIG. 3, when the current density was 2900mA/cm2In example 2, the cell voltage before and after accelerated corrosion of the microporous layer was reduced from 0.547V to 0.507V, and the power density was reduced from 1.58w/cm2The concentration is reduced to 1.47w/cm2The performance is reduced by 7.25%. From FIG. 4It can be seen that when the current density is 1600mA/cm2In comparative example 1, the voltage before and after accelerated etching of the microporous layer was decreased from 0.645V to 0.574V, and the power density was decreased from 1.03w/cm2Reduced to 0.918w/cm2The performance is reduced by 11.01%. This shows that after 72 hours of accelerated corrosion, the microporous layer in example 2 has a performance loss reduced from 11.01% to 7.25% and the corrosion resistance of the microporous layer is improved by 34.2% compared to the microporous layer in comparative example 1 (the main difference is graphitized carbon and XC-72). This result occurs mainly because the present invention employs graphitized carbon as conductive carbon black, which has excellent corrosion resistance and hydrophobic treatment ability; and a spraying process is combined to prepare the microporous layer, so that the loading amount of the conductive carbon black in the microporous layer is accurately controlled, and graphitized carbon can be uniformly dispersed on the substrate by adding the dispersing agent, so that the corrosion resistance and the water and gas management capacity of the microporous layer are further improved.
In conclusion, the microporous layer provided by the invention has higher single cell performance, and can maintain good cell performance after accelerated corrosion.
Claims (6)
1. The preparation method of the corrosion-resistant microporous layer of the fuel cell based on the graphitized carbon is characterized by comprising the following steps: (a) preparing suspension slurry by using graphitized carbon, a water repellent solution and an organic solvent as raw materials; (b) spraying the suspension slurry on a substrate, drying and sintering; the graphitized carbon particles have a particle size of no more than 500nm and are mainly formed by agglomeration of primary graphitized mesoporous carbon with a diameter of about 35 nm; the water repellent solution is polytetrafluoroethylene aqueous solution with the mass fraction of 60% -80%; the organic solvent is formed by mixing isopropanol and ethylene glycol according to the mass ratio of 50: 1; the substrate is carbon paper or carbon cloth; the drying temperature of the step (b) is 60-90 ℃, and the calcining parameters are as follows: n is a radical of2Keeping the temperature for 45min from room temperature to 120 ℃ at the heating rate of 5 ℃/min, heating to 350 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 30min, and naturally cooling to room temperature.
2. The method according to claim 1, wherein the step (a) is as follows: mixing the graphitized carbon, the water repellent solution and the organic solvent according to the proportion, mechanically stirring for 0.5-1h, and then carrying out ultrasonic treatment until a uniform suspension is formed.
3. The method of claim 1, wherein: the mass ratio of the graphitized carbon to the water repellent solution is 50-80:1, and the mass fraction of the graphitized carbon in the suspension slurry is 1.5-2.5%.
4. The method of claim 1, wherein: the pressure of the suspension slurry during spraying is 0.5-1.5 Mpa, and the distance between the nozzle and the substrate is 15 cm.
5. The method of claim 1, wherein: the spraying process is repeated for a plurality of times until the carbon loading of the microporous layer is 0.5-2.5mg/cm2。
6. A fuel cell corrosion resistant microporous layer made according to the method of any of claims 1-5, characterized in that the microporous layer is a single layer structure consisting essentially of graphitized carbon and PTFE attached to a carbon paper.
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