CN115656006A - Gas diffusion layer accelerated attenuation test method and application thereof - Google Patents
Gas diffusion layer accelerated attenuation test method and application thereof Download PDFInfo
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Abstract
The invention provides a gas diffusion layer accelerated attenuation test method and application thereof, wherein the test method comprises the steps of compressing a gas diffusion layer to be tested to a certain compression ratio, then using the gas diffusion layer as a working electrode, carrying out accelerated attenuation test under a standard three-electrode system, then carrying out physical property test, and repeating the accelerated attenuation test and the physical property test at least three times in sequence, thereby analyzing and evaluating the data of the three times and obtaining the durability result of the gas diffusion layer. The invention does not need to assemble a membrane electrode or a fuel cell, is simple and convenient, and carries out accelerated attenuation test on the compressed gas diffusion layer, so that the compressed gas diffusion layer is closer to the actual working state, the accuracy of life prediction is favorably improved, and the test result can show the durability under different compression ratios, thereby indicating the selection of the optimal compression ratio of the gas diffusion layer, guiding the optimization of related assembly or compression processes, and further prolonging the service life of the gas diffusion layer in the actual working.
Description
Technical Field
The invention relates to the field of proton exchange membrane fuel cells, in particular to a gas diffusion layer accelerated attenuation test method and application thereof.
Background
At present, proton exchange membrane fuel cells have gradually become a hotspot in the field of new energy due to the advantages of no pollution, environmental friendliness, high energy conversion rate, wide application scene and the like. However, the short lifetime of the pem fuel cell is one of the important reasons that limit its development.
The gas diffusion layer is one of the core components in the fuel cell, and is disposed in the membrane electrode, and is mainly used to provide electron conduction between the catalytic layer and the bipolar plate, and to provide a gas and moisture transmission path between the bipolar plate and the proton exchange membrane, so the durability of the gas diffusion layer directly affects the lifetime of the membrane electrode. The factors affecting the durability of the gas diffusion layer are mainly classified into: mechanical attenuation and physicochemical attenuation. The mechanical attenuation mainly refers to the attenuation of the gas diffusion layer caused by a certain pressure, such as the attenuation caused by gas scouring and the attenuation caused by water scouring; and the physicochemical degradation is mainly due to chemical corrosion and electrochemical corrosion caused by a weakly acidic environment inside the membrane electrode.
In order to test the durability of the gas diffusion layer to guide the optimization and improvement of the gas diffusion layer, CN110850320a discloses a durability test method for a hydrogen fuel cell, which comprises assembling the gas diffusion layer to be tested into the hydrogen fuel cell, and activating the single cell of the cell; collecting polarization curves of a membrane electrode before and after the hydrogen fuel cell is operated under an open-circuit voltage working condition; judging the durability of the hydrogen fuel cell according to the polarization curve, the alternating current impedance spectrum, the linear sweep voltammetry curve, the section view of the catalyst layer and the fluorine ion concentration of the membrane electrode before and after the hydrogen fuel cell is operated under the open-circuit voltage working condition; according to the invention, through collecting relevant experimental data of the hydrogen fuel cell and analyzing the attenuation mechanism of the corresponding membrane electrode, the durability, namely the service life, of the hydrogen fuel cell is calculated, the service life test of the hydrogen fuel cell can be accelerated, and the hydrogen fuel cell with long service life is developed.
CN110412103A discloses a membrane electrode durability evaluation method of a proton exchange membrane fuel cell, which separates a gas diffusion layer in a membrane electrode after durability test, assembles an old gas diffusion layer membrane electrode with the same model as the membrane electrode with a new proton exchange membrane and a catalyst layer, takes a new membrane electrode with the same model, and respectively carries out electrochemical performance test on the new membrane electrode and the old gas diffusion layer membrane electrode; and calculating an influence factor E of the gas diffusion layer on the diffusion polarization loss of the membrane electrode under a certain current density according to the electrochemical performance data of the membrane electrode before and after the durability test and the electrochemical performance data of the new membrane electrode and the old gas diffusion layer membrane electrode obtained by the test to show the influence, thereby guiding the research on the durability of the membrane electrode.
The two schemes need to assemble the gas diffusion layer into the membrane electrode or the fuel cell, then carry out the required test, increase the complexity of the test, have low test efficiency, and are not suitable for large-scale evaluation and test environments. Therefore, there is still a need to develop a simple and convenient testing scheme capable of reducing the attenuation of the gas diffusion layer in the actual working state, so that the durability test result of the gas diffusion layer is more accurate.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a gas diffusion layer accelerated attenuation test method and application thereof, wherein the test method comprises the steps of compressing a gas diffusion layer to be tested to a certain compression ratio, then using the gas diffusion layer as a working electrode, carrying out accelerated attenuation test under a standard three-electrode system, then carrying out physical property test, and repeating the accelerated attenuation test and the physical property test at least three times in sequence, so that three times of data are analyzed and evaluated, and a durability result of the gas diffusion layer is obtained. The invention does not need to assemble a membrane electrode or a fuel cell, is simple and convenient, and carries out accelerated attenuation test on the compressed gas diffusion layer to make the gas diffusion layer closer to the actual working state, thereby being beneficial to improving the accuracy of life prediction, and the test result can show the durability under different compression ratios, thereby indicating the selection of the optimal compression ratio of the gas diffusion layer, guiding the optimization of related assembly or compression process and further prolonging the service life of the gas diffusion layer in the actual working.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for testing the accelerated decay of a gas diffusion layer, the method comprising the steps of:
(1) Compressing a gas diffusion layer to be tested;
(2) Taking the compressed gas diffusion layer obtained in the step (1) as a working electrode, and carrying out accelerated attenuation test in a standard three-electrode system;
(3) Carrying out physical property test on the gas diffusion layer obtained in the step (2) after the accelerated attenuation test;
(4) And (4) repeating the step (2) and the step (3) at least three times in sequence.
The gas diffusion layer is compressed to reach a certain compression ratio and then subjected to an accelerated attenuation test so as to be closer to the actual working state, and the gas diffusion layer is an elastic part and can be stressed and compressed when being assembled into a membrane electrode or a fuel cell, so that the compression can cause the influence of breakage and the like of a part of fiber structures in the gas diffusion layer, and further the durability of the actual working is influenced. The method can test the gas diffusion layers in the same batch at different compression ratios, and further explore the durability of the gas diffusion layers at different compression ratios, so that the method can guide the selection of the optimal compression ratio of the gas diffusion layers, guide the optimization of related assembly or compression processes, and further prolong the service life of the gas diffusion layers in actual work.
The following are preferred embodiments of the present invention, but are not intended to limit the scope of the invention. The technical purpose and the beneficial effects of the invention can be better achieved and realized through the following technical scheme.
In a preferred embodiment of the present invention, the compression ratio in step (1) is greater than 0 and less than 30%, for example, 1%, 2%, 5%, 8%, 10%, 15%, 20%, 25%, or 30%, and the compression ratio is preferably 10% to 30%, for example, 10%, 12%, 14%, 16%, 18%, 20%, 22%, 24%, 26%, 28%, or 30%, but is not limited to the recited values, and other values not recited in the above range of values are also applicable.
The compressibility in the present invention means a change rate of the gas diffusion layer after compression compared to the initial state, for example, when the compressibility is 30%, the thickness of the gas diffusion layer after compression is reduced by 30% compared to the initial thickness.
Preferably, the compression is performed in a press.
As a preferred technical scheme of the invention, the electrolyte used in the accelerated degradation test in the step (2) is a mixed solution of hydrogen peroxide and sulfuric acid.
According to the invention, hydrogen peroxide with a specific concentration is added into common electrolyte sulfuric acid, so that the mixed solution has more severe erosion and oxidation effects on the gas diffusion layer, and the corrosion capability on each part of the gas diffusion layer in a compressed state is improved.
Preferably, the hydrogen peroxide concentration is 12 to 18wt%, such as 12wt%, 13wt%, 14wt%, 15wt%, 16wt%, 17wt%, or 18wt%, but is not limited to the recited values, and other values not recited within the above range of values are also applicable.
Preferably, the concentration of the sulfuric acid in the mixed solution is 0.3 to 0.7mol/L, for example, 0.3mol/L, 0.4mol/L, 0.5mol/L, 0.6mol/L, or 0.3mol/L, but is not limited to the recited values, and other values not recited in the above numerical range are also applicable.
Preferably, the three-electrode system in step (2) comprises a working electrode, a counter electrode and a reference electrode.
Preferably, the counter electrode is a graphite electrode.
Preferably, the reference electrode is a saturated calomel electrode.
As a preferable technical solution of the present invention, in the accelerated degradation test in the step (2), the gas diffusion layer is always completely immersed in the electrolyte.
The invention aims to research and detect the overall durability of a compressed gas diffusion layer, so that the gas diffusion layer is required to be immersed in electrolyte all the time for accelerated attenuation during testing so as to ensure the accuracy of the overall physical property test of the gas diffusion layer.
As a preferred technical scheme of the invention, the accelerated degradation test in the step (2) is carried out under heating.
Preferably, the target temperature of the heating is 70 to 90 ℃, for example, 70 ℃, 72 ℃, 74 ℃, 76 ℃, 78 ℃, 80 ℃, 82 ℃, 74 ℃, 76 ℃, 78 ℃ or 80 ℃, but is not limited to the recited values, and other values not recited in the above numerical range are also applicable.
Preferably, in the accelerated decay test in the step (2), inert gas is introduced into the system;
preferably, the inert gas comprises nitrogen.
In a preferred embodiment of the present invention, the accelerated degradation test includes a potentiostatic accelerated oxidation test, in which the test voltage is 1.1 to 1.3V, for example, 1.1V, 1.12V, 1.14V, 1.16V, 1.18V, 1.2V, 1.22V, 1.24V, 1.26V, 1.28V, or 1.3V, but is not limited to the recited values, and other values not recited in the above range of values are also applicable.
Preferably, the time of the potentiostatic accelerated oxidation test is 10 to 14 hours, for example 10 hours, 10.5 hours, 11 hours, 11.5 hours, 12 hours, 12.5 hours, 13 hours, 13.5 hours or 14 hours, but is not limited to the recited values, and other values not recited in the above numerical ranges are equally applicable.
As a preferable embodiment of the present invention, after the step (2) of performing the acceleration decay test and before the step (3) of performing the physical property test, the gas diffusion layer obtained in the step (2) after the acceleration decay test is sequentially washed and dried.
Preferably, the washing comprises a plurality of water washes.
Preferably, the drying comprises vacuum drying.
Preferably, the temperature of the vacuum drying is 50 to 70 ℃, for example, 50 ℃, 52 ℃, 54 ℃, 56 ℃, 58 ℃, 60 ℃, 62 ℃, 64 ℃, 66 ℃, 68 ℃ or 70 ℃, but is not limited to the recited values, and other values not recited in the above numerical range are also applicable.
Preferably, the vacuum drying time is 4 to 8 hours, for example, 4 hours, 4.5 hours, 5 hours, 5.5 hours, 6 hours, 6.5 hours, 7 hours, 7.5 hours, or 8 hours, but is not limited to the recited values, and other values not recited within the above range of values are also applicable.
In a preferred embodiment of the present invention, the physical property test in step (3) includes thickness, air permeability, and vertical resistivity in the thickness direction.
As a preferred technical scheme of the invention, the test method comprises the following steps:
(1) Putting a gas diffusion layer to be tested into a press machine for compression, wherein the compression rate of the compression is 10-30%;
(2) Taking the compressed gas diffusion layer obtained in the step (1) as a working electrode, forming a standard three-electrode system with a graphite electrode and a saturated calomel electrode, and using a mixed solution of 12-18 wt% of hydrogen peroxide and sulfuric acid as an electrolyte, wherein the concentration of the sulfuric acid is 0.3-0.7 mol/L; completely immersing the gas diffusion layer in the electrolyte all the time, heating the electrolyte to 70-90 ℃, introducing saturated nitrogen into the electrolyte, setting the test voltage to be 1.1-1.3V vs. RHE, and carrying out a constant potential accelerated oxidation test for 10-14 h;
(3) Washing the gas diffusion layer subjected to the accelerated attenuation test in the step (2) for multiple times, then carrying out vacuum drying for 4-8 h at 50-70 ℃, and then carrying out physical property test to obtain the thickness, air permeability and vertical resistivity along the thickness direction of the gas diffusion layer;
(4) And (4) repeating the step (2) and the step (3) at least three times in sequence.
In a second aspect, the present invention provides a use of the gas diffusion layer accelerated degradation testing method of the first aspect in the manufacture of a proton exchange membrane fuel cell.
Compared with the prior art, the invention has at least the following beneficial effects: the testing method does not need to assemble the membrane electrode or the fuel cell, is simple and convenient, and is beneficial to improving the testing efficiency; the compressed gas diffusion layer is subjected to accelerated attenuation test, so that the gas diffusion layer is closer to the actual working state, the accuracy of service life prediction is improved, and the test result can show the durability under different compression ratios, so that the selection of the optimal compression ratio of the gas diffusion layer is indicated, the optimization of related assembly or compression processes is guided, and the service life of the gas diffusion layer in the actual working process is further prolonged.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
The gas diffusion layers used in the following examples and comparative examples were commercially available, and had a two-layer structure of a substrate layer and a microporous layer, and a circular shape with a diameter of 33 mm; the thickness of the gas diffusion layer is 228 μm; air permeability of 270mL/m 2 Pa · s; the vertical resistivity in the thickness direction was 9.9 m.OMEGA.cm 2 。
The standard three-electrode system in the following examples and comparative examples, in which the counter electrode was a platinum electrode and the reference electrode was a saturated calomel electrode, was attached to an electrochemical workstation (model number CHI 760D) produced by the shanghai chenhua instrument to perform an accelerated decay test.
Example 1
The embodiment provides a gas diffusion layer accelerated attenuation test method, which comprises the following steps:
(1) Putting the gas diffusion layer to be tested into a press machine for compression and maintaining the pressure for 5min to enable the compression rate to reach 10%;
(2) Connecting the compressed gas diffusion layer obtained in the step (1) as a working electrode, and a standard three-electrode system consisting of a graphite electrode and a saturated calomel electrode to an electrochemical workstation, then placing the electrochemical workstation into a reaction container, pouring electrolyte into the reaction container, wherein the electrolyte is a mixed solution of hydrogen peroxide and sulfuric acid with the concentration of 15wt%, the concentration of the sulfuric acid is 0.5mol/L, so that the gas diffusion layer is always completely immersed, heating the electrolyte to 80 ℃, introducing saturated nitrogen with the flow of 0.5L/min into the electrolyte, setting the test voltage to be 1.2V vs.RHE after the temperature is stable, and carrying out a 12-hour constant potential accelerated oxidation test;
(3) Washing the gas diffusion layer subjected to the accelerated attenuation test obtained in the step (2) for multiple times, then carrying out vacuum drying for 6 hours at the temperature of 60 ℃, and then carrying out physical property test to obtain the thickness, air permeability and vertical resistivity along the thickness direction of the gas diffusion layer;
(4) And (4) repeating the step (2) and the step (3) for three times in sequence to obtain three groups of data.
Example 2
This example provides a gas diffusion layer accelerated attenuation test method which is identical to that of example 1 except that the compressibility is adjusted from 10% to 1% in step (1).
Example 3
This example provides a gas diffusion layer accelerated attenuation test method exactly the same as example 1 except that the compressibility was adjusted from 10% to 5% in step (1).
Example 4
This example provides a gas diffusion layer accelerated attenuation test method which is identical to that of example 1 except that the compressibility is adjusted from 10% to 20% in step (1).
Example 5
This example provides a gas diffusion layer accelerated attenuation test method which is identical to that of example 1 except that the compressibility is adjusted from 10% to 30% in step (1).
Example 6
This example provides a gas diffusion layer accelerated attenuation test method which is identical to that of example 1 except that the compressibility is adjusted from 10% to 35% in step (1).
Example 7
This example provides a gas diffusion layer accelerated decay test method which is identical to that of example 1 except that the electrolyte used in step (2) is a 0.5mol/L aqueous sulfuric acid solution, and hydrogen peroxide is not contained.
Comparative example 1
This comparative example provides a gas diffusion layer accelerated decay test method exactly the same as example 1 except that step (1) was not performed, i.e., the gas diffusion layer was not compressed.
In the step (3) of each example and comparative example, the thickness was repeatedly measured three times using a thickness gauge with an accuracy of 0.001mm, and an average value was calculated;
adopting a Gurley air permeability tester, according to an air permeability testing method in the determination (Gurley method) of the air permeability of the paper and the paperboard of the national standard GB/T5402-2003, enabling the MPL side (the microporous layer side) of the gas diffusion layer to face upwards, testing the time of transmitting the same air amount, calculating the air permeability of the gas diffusion layer through a formula, and repeatedly measuring for three times and taking an average value;
adopting a contact resistance tester for vertical resistivity along the thickness direction, and calculating the resistivity of the gas diffusion layer in the vertical direction according to a formula according to a vertical direction resistivity test method in a national standard GB/T20042.7-2014 carbon paper characteristic test method;
after obtaining the values of thickness, air permeability and vertical resistivity, the thickness change rate, air permeability change rate and vertical resistivity change rate after each attenuation were calculated with respect to the initial thickness, air permeability and vertical resistivity of the original gas diffusion layer that was not subjected to the compression and accelerated attenuation tests, and the obtained data were recorded in table 1.
TABLE 1
As can be seen from table 1:
the gas diffusion layers of examples and comparative examples were reduced in thickness, gradually increased in gas permeability, and greatly increased in vertical resistivity after undergoing a durability test for multiple accelerated decay. The gas diffusion layer in comparative example 1 is not compressed, compared with the gas diffusion layers in examples 1 to 6, which are compressed to different degrees, it can be seen that, after compression, the thickness, the air permeability and the vertical resistivity of the gas diffusion layer are different from those in comparative example 1, and along with the gradual increase of the compression rate, the change rates of the thickness, the air permeability and the vertical resistivity of the gas diffusion layer after accelerated attenuation for the same times are all larger, on one hand, the fact that the gas diffusion layer is compressed in advance before the accelerated attenuation test is explained, so that the gas diffusion layer can be closer to the working state in practical application during the test, and the tested data are more accurate; on the other hand, in view of the influence of different compressibility on the gas diffusion layer, the compressibility can cause the carbon fibers in the gas diffusion layer to break, thereby accelerating the carbon corrosion rate of the gas diffusion layer, and the excessive compressibility causes the practical durability test result to deviate from the practical application to be too large, so the compressibility should be preferably selected to be between 10% and 30%; because the gas diffusion layer is compressed, the mechanical structure of the gas diffusion layer is slightly changed, and the compaction degree of a part of areas is increased, the accelerated attenuation is carried out on the electrolyte only containing sulfuric acid, as in example 7, the accelerated attenuation effect cannot be well realized, and after hydrogen peroxide is added, the erosion capacity of the electrolyte is obviously improved, so that the whole gas diffusion layer is completely accelerated and attenuated, and the accuracy of a test result is ensured;
it can be seen from the above that the invention does not need to assemble the membrane electrode or the fuel cell, is simple and convenient, and carries out the accelerated attenuation test on the compressed gas diffusion layer, so that the compressed gas diffusion layer is closer to the actual working state, the accuracy of life prediction is improved, and the test result can show the durability under different compression ratios, thereby indicating the selection of the optimal compression ratio of the gas diffusion layer, guiding the optimization of the related assembly or compression process, and further prolonging the service life of the gas diffusion layer in the actual working.
The present invention is illustrated by the above examples, but the present invention is not limited to the above detailed process equipment and process flow, which means that the present invention must not be implemented by the above detailed process equipment and process flow. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A gas diffusion layer accelerated decay test method, comprising the steps of:
(1) Compressing a gas diffusion layer to be tested;
(2) Taking the compressed gas diffusion layer obtained in the step (1) as a working electrode, and carrying out accelerated attenuation test under a standard three-electrode system;
(3) Carrying out physical property test on the gas diffusion layer obtained in the step (2) after the accelerated attenuation test;
(4) And (4) repeating the step (2) and the step (3) at least three times in sequence.
2. The accelerated attenuation test method for the gas diffusion layer according to claim 1, wherein the compression rate of the compression in the step (1) is greater than 0 and less than or equal to 30%, and the preferred compression rate is 10% to 30%;
preferably, the compression is performed in a press.
3. The accelerated decay test method for a gas diffusion layer according to claim 1 or 2, wherein the electrolyte used in the accelerated decay test of the step (2) is a mixed solution of hydrogen peroxide and sulfuric acid;
preferably, the concentration of the hydrogen peroxide is 12 to 18wt%;
preferably, the concentration of the sulfuric acid in the mixed solution is 0.3-0.7 mol/L;
preferably, the three-electrode system in step (2) comprises a working electrode, a counter electrode and a reference electrode;
preferably, the counter electrode is a graphite electrode;
preferably, the reference electrode is a saturated calomel electrode.
4. The accelerated decay test method for the gas diffusion layer according to any one of claims 1 to 3, wherein in the accelerated decay test of the step (2), the gas diffusion layer is always completely immersed in the electrolyte.
5. The gas diffusion layer accelerated decay test method of any of claims 1-4, wherein the accelerated decay test of step (2) is performed under heat;
preferably, the target temperature of heating is 70-90 ℃;
preferably, in the accelerated decay test in the step (2), inert gas is introduced into the system;
preferably, the inert gas comprises nitrogen.
6. The accelerated decay test method for the gas diffusion layer according to any one of claims 1 to 5, wherein the accelerated decay test comprises a potentiostatic accelerated oxidation test, and the test voltage of the potentiostatic accelerated oxidation test is 1.1 to 1.3V;
preferably, the time of the constant potential accelerated oxidation test is 10-14 h.
7. The accelerated degradation testing method of a gas diffusion layer according to any one of claims 1 to 6, wherein after the accelerated degradation test is performed in the step (2) and before the physical property test in the step (3), the gas diffusion layer after the accelerated degradation test obtained in the step (2) is sequentially washed and dried;
preferably, the washing comprises a plurality of water washes;
preferably, the drying comprises vacuum drying;
preferably, the temperature of the vacuum drying is 50-70 ℃;
preferably, the vacuum drying time is 4-8 h.
8. The accelerated attenuation test method for a gas diffusion layer according to any one of claims 1 to 7, wherein the physical property test of the step (3) includes thickness, air permeability, and vertical resistivity in a thickness direction.
9. The gas diffusion layer accelerated decay test method of any of claims 1-8, wherein the test method comprises the steps of:
(1) Putting a gas diffusion layer to be tested into a press machine for compression, wherein the compression rate of the compression is 10-30%;
(2) Taking the compressed gas diffusion layer obtained in the step (1) as a working electrode, forming a standard three-electrode system with a graphite electrode and a saturated calomel electrode, and using a mixed solution of 12-18 wt% of hydrogen peroxide and sulfuric acid as an electrolyte, wherein the concentration of the sulfuric acid is 0.3-0.7 mol/L; completely immersing the gas diffusion layer in the electrolyte all the time, heating the electrolyte to 70-90 ℃, introducing saturated nitrogen into the electrolyte, setting the test voltage to be 1.1-1.3V vs. RHE, and carrying out a constant potential accelerated oxidation test for 10-14 h;
(3) Washing the gas diffusion layer subjected to the accelerated attenuation test in the step (2) for multiple times, then carrying out vacuum drying for 4-8 h at 50-70 ℃, and then carrying out physical property test to obtain the thickness, air permeability and vertical resistivity along the thickness direction of the gas diffusion layer;
(4) And (4) repeating the step (2) and the step (3) at least three times in sequence.
10. Use of a gas diffusion layer accelerated decay test method according to any of claims 1 to 9 in the manufacture of a proton exchange membrane fuel cell.
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