CN112763392B - Method for accelerating evaluation of durability of proton exchange membrane for fuel cell - Google Patents
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- 239000012528 membrane Substances 0.000 title claims abstract description 89
- 239000000446 fuel Substances 0.000 title claims abstract description 65
- 238000011156 evaluation Methods 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000001257 hydrogen Substances 0.000 claims abstract description 46
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 46
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000012360 testing method Methods 0.000 claims abstract description 21
- 238000009423 ventilation Methods 0.000 claims abstract description 21
- 230000008859 change Effects 0.000 claims abstract description 11
- 238000012854 evaluation process Methods 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims description 29
- 230000008569 process Effects 0.000 claims description 8
- 238000009792 diffusion process Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 230000003197 catalytic effect Effects 0.000 claims description 6
- 230000001133 acceleration Effects 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000007493 shaping process Methods 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 238000010926 purge Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 description 13
- 230000004888 barrier function Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- 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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- Chemical & Material Sciences (AREA)
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- Life Sciences & Earth Sciences (AREA)
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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention provides a method for accelerating evaluation of durability of a proton exchange membrane for a fuel cell, which comprises the following steps: s1, preparing a full-size membrane electrode assembly; s2, assembling the fuel cell by utilizing the full-size membrane electrode assembly, introducing hydrogen into an anode side flow field of the fuel cell, and introducing air into a cathode side flow field of the fuel cell; s3, controlling the temperature of the battery according to the general running state of the fuel battery; s4, synchronously switching the humidity of the input hydrogen and the humidity of the air according to a fixed time interval; s5, obtaining hydrogen permeation current and ventilation time of the fuel cell in the evaluation process until any one of the hydrogen permeation current and ventilation time reaches a preset test termination condition; s6, obtaining an evaluation result of the durability of the proton exchange membrane according to the change curve of the hydrogen permeation current and the ventilation time. According to the invention, the full-size proton exchange membrane is adopted for durability evaluation, so that the influence of the size on the durability is effectively avoided.
Description
Technical Field
The invention relates to the technical field of proton exchange membrane fuel cells, in particular to a method for accelerating evaluation of durability of a proton exchange membrane for a fuel cell.
Background
Proton Exchange Membrane Fuel Cells (PEMFCs) are considered to be most promising for applications in the fields of vehicle-mounted power systems, stationary power stations, and the like, due to their compact structure, high power density, environmental friendliness, no pollution, and room temperature startup. The proton exchange membrane is used as a key material of the PEMFC and mainly plays roles in conducting protons and separating cathode and anode gases, and the durability of the proton exchange membrane directly influences the durability of the whole PEMFC.
The durability of the proton exchange membrane is divided into two aspects of mechanical durability and chemical durability, wherein the mechanical durability mainly refers to the gas barrier property attenuation caused by swelling and shrinkage of the proton exchange membrane due to the difference of water content in the membrane during the operation of the fuel cell; chemical durability mainly refers to the reduction of gas barrier property and proton conductivity of a proton exchange membrane caused by the breakage of a high polymer generated by the attack of free radicals in the operation process of a fuel cell.
In recent studies, researchers mostly use mechanical durability evaluation methods and chemical durability evaluation methods published by the U.S. department of energy (DOE) for proton exchange membranes [1]. The mechanical durability evaluation method adopts that air is introduced into two sides of a Membrane Electrode Assembly (MEA) made of a proton exchange membrane to be evaluated, and the relative humidity (from 0% RH to 100% RH) of the air is switched every 2min, and 20000 times of circulation are carried out. The chemical durability evaluation method adopts that hydrogen and air are respectively introduced into two sides of an MEA (membrane electrode assembly) manufactured by adopting a proton exchange membrane to be evaluated, the relative humidity of an anode and a cathode is maintained to be 30%, and the test is continued for 200 hours.
Although DOE has proposed a durability evaluation method for mechanical durability and chemical durability of proton exchange membrane, respectively, it has a major drawback in practical application. Firstly, simply evaluating the mechanical durability and chemical durability of the proton exchange membrane is significant for scientific research, and is helpful for carrying out corresponding optimization on the proton exchange membrane material, but the method can not provide a comprehensive evaluation means, because the mechanical attenuation and chemical attenuation of the proton exchange membrane exist simultaneously in the practical application environment of the proton exchange membrane, and obvious coupling phenomenon exists between the mechanical attenuation and the chemical attenuation of the proton exchange membrane. Specifically, on one hand, the chemical attenuation rate of the proton exchange membrane is obviously accelerated along with the decrease of the mechanical property of the proton exchange membrane, because the gas barrier property is reduced due to the decrease of the mechanical property, the amount of air passing through the proton exchange membrane is gradually increased, the air reaches the hydrogen side and then undergoes a reduction reaction through a two-electron reaction mechanism to generate more hydroxyl free radicals, and the free radicals attack the high polymer to accelerate the chemical attenuation process of the proton exchange membrane. In addition, when the DOE is adopted to select the proton exchange membrane material, although a certain proton exchange membrane can simultaneously meet the mechanical durability and chemical durability requirements specified by the DOE, the durability of the proton exchange membrane can only reach about 2000 hours when the proton exchange membrane is applied to a fuel cell, and the proton exchange membrane can not meet the commercial application requirements far.
In order to realize the commercialized application of PEMFC, not only the performance requirement is satisfied, but also good stability is required. As a primary place for ion transfer to occur, the durability of the proton exchange membrane directly affects the performance and stability of the overall fuel cell.
However, the time required for the durability evaluation using the normal operation condition of the fuel cell is excessively long, which is extremely disadvantageous to the development process of the PEMFC, and thus a method for rapidly evaluating the durability of the proton exchange membrane for the fuel cell is urgently required.
Disclosure of Invention
According to the technical problem that the durability evaluation needs too long under the normal operation condition of the fuel cell, the method for accelerating the durability evaluation of the proton exchange membrane for the fuel cell is provided, the durability evaluation is carried out by a method combining a dry-wet cycle and an open circuit experiment, and the mechanical durability evaluation and the chemical durability evaluation of the proton exchange membrane are both considered.
The invention adopts the following technical means:
A method of accelerating the evaluation of proton exchange membrane durability for a fuel cell comprising:
s1, preparing a full-size membrane electrode assembly;
s2, assembling the fuel cell by utilizing the full-size membrane electrode assembly, introducing hydrogen into an anode side flow field of the fuel cell, and introducing air into a cathode side flow field of the fuel cell;
S3, controlling the temperature of the battery according to the general running state of the fuel battery;
s4, synchronously switching the humidity of the input hydrogen and the humidity of the air according to a fixed time interval, wherein the relative humidity of the hydrogen and the air is switched between 0% RH and 100% RH;
S5, obtaining hydrogen permeation current and ventilation time of the fuel cell in the evaluation process until any one of the hydrogen permeation current and ventilation time reaches a preset test termination condition;
And S6, drawing a change curve of hydrogen permeation current and ventilation time in the test process, and obtaining an evaluation result of the durability of the proton exchange membrane according to the change curve of the hydrogen permeation current.
Further, the termination condition of the preset test is that the hydrogen permeation current is more than 10mA/cm 2 or the ventilation time is less than 1s.
Further, the preparing of the full-sized membrane electrode assembly includes:
cutting the proton exchange membrane to obtain the proton exchange membrane with the size completely consistent with that in the actual application scene of the fuel cell, and evaluating the durability;
According to the actual shaping process, preparing catalytic layers on two sides of the proton exchange membrane to be evaluated, and matching corresponding gas diffusion layers and frames, thereby obtaining the full-size membrane electrode assembly.
Further, obtaining hydrogen permeation current of the fuel cell in the evaluation process includes:
purging the fuel cell by taking hydrogen as anode gas of the fuel cell and taking nitrogen as cathode gas of the fuel cell;
controlling the open circuit voltage of the fuel cell to be 0.1V;
Adopting a potentiostat to perform linear voltage scanning operation on the fuel cell, wherein the scanning range is 0.1V-0.6V, and the scanning speed is 0.002V/s;
And obtaining the corresponding current density when the scanning voltage is 0.45V as hydrogen permeation current.
Further, obtaining the ventilation time of the fuel cell during the evaluation process includes:
Maintaining a gas pressure in the anode-side flow field of the fuel cell at 100kPa;
The total volume of gas permeated from the anode side to the cathode side of the fuel cell was tested to reach 0.5ml as the permeation time.
Compared with the prior art, the invention has the following advantages:
1. The invention simultaneously combines the mechanical durability evaluation and the chemical durability evaluation of the proton exchange membrane, and has guiding significance for the proton exchange membrane type selection in the fuel cell research and development process.
2. According to the invention, the full-size proton exchange membrane is adopted for durability evaluation, so that the influence of the size on the durability is effectively avoided.
3. The durability evaluation method provided by the invention is simple to operate and convenient to implement.
Based on the reasons, the invention can be widely popularized in the field of proton exchange membrane testing for fuel cells.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to the drawings without inventive effort to a person skilled in the art.
FIG. 1 is a flow chart of a method of accelerating the evaluation of durability of a proton exchange membrane for a fuel cell according to the present invention.
Fig. 2 is a schematic diagram of a cell structure in an embodiment.
FIG. 3 is a graph comparing the results of permeation hydrogen current during accelerated durability testing of different proton exchange membranes in the examples.
FIG. 4 is a graph comparing the results of permeation time during accelerated durability testing of different proton exchange membranes in the examples.
In the figure: 1. a unipolar plate with an anode flow field; 2. an anode gas diffusion layer; 201. an anode carbon paper substrate; 202. an anode microporous layer; 3. an anode catalytic layer; 4. a proton exchange membrane; 5. a cathode catalytic layer; 6. a cathode gas diffusion layer; 601. a cathode carbon paper substrate; 602. a cathode microporous layer; 7. monopolar plates with cathode flow fields.
Detailed Description
In order that those skilled in the art will better understand the present invention, a technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in which it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
As shown in fig. 1, an embodiment of the present invention provides a method for accelerating evaluation of durability of a proton exchange membrane for a fuel cell, including:
S1, preparing a full-size membrane electrode assembly. The durability evaluation is carried out by adopting the proton exchange membrane with the size completely consistent with that in the practical application scene, so that the durability change caused by the size change can be avoided. By adopting the proton exchange membrane, the catalytic layers are prepared on the two sides of the proton exchange membrane according to the actual shaping process, and the full-size Membrane Electrode Assembly (MEA) is prepared by matching with the corresponding Gas Diffusion Layer (GDL) and the frame.
S2, assembling the fuel cell by using the full-size membrane electrode assembly, introducing hydrogen into an anode side flow field of the fuel cell, and introducing air into a cathode side flow field of the fuel cell.
And S3, controlling the temperature of the battery according to the general operation state of the fuel battery. The cell temperature is preferably controlled to 80 c, which is the normal operating temperature of the fuel cell.
S4, synchronously switching the humidity of the input hydrogen and the humidity of the air according to a fixed time interval, wherein the relative humidity of the hydrogen and the air is switched between 0% RH and 100% RH.
S5, obtaining hydrogen permeation current and ventilation time of the fuel cell in the evaluation process until any one of the hydrogen permeation current and ventilation time reaches the termination condition of the preset test.
And S6, drawing a change curve of hydrogen permeation current and ventilation time in the test process, and obtaining an evaluation result of the durability of the proton exchange membrane according to the change curve of the hydrogen permeation current.
The following further describes the scheme and effects of the present invention through specific application examples.
(1) The proton exchange membrane with the size completely consistent with the actual application scene is adopted, and the Pt/C catalyst and the mass fraction of the catalyst are 0.5 percentPreparing slurry from the solution according to the mass ratio of 1:7, preparing a catalytic layer on the surface of a proton exchange membrane (or a gas diffusion layer) by adopting the slurry, and matching the corresponding gas diffusion layer and a frame after spraying to prepare the full-size Membrane Electrode Assembly (MEA).
(2) And (2) assembling the single cell by adopting the MEA (1), assembling the single cell as shown in fig. 2, then connecting the single cell into a fuel cell test system, respectively introducing hydrogen and air into the cathode and the anode, and adjusting related parameters (such as cell temperature, gas flow rate, gas relative humidity and the like) to normal working conditions.
(3) The humidity of the hydrogen gas and the air were switched every 2min from a completely dry gas (relative humidity 0% rh) to a saturated humidified gas (relative humidity 100% rh), and the humidity of the hydrogen gas and the air were changed synchronously.
(4) The hydrogen permeation current and the permeation time of the fuel cell are measured at regular intervals, and the measurement interval is preferably 46h.
(5) The hydrogen permeation current testing method comprises the following steps: the anode gas of the battery still keeps unchanged hydrogen, the cathode gas is switched from air to nitrogen to sweep the battery, the Open Circuit Voltage (OCV) of the battery is reduced to about 0.1V, a potentiostat is adopted to carry out cyclic voltammetry scanning operation on the battery, the scanning range is 0.1V-0.6V, the scanning speed is 0.002V/s, and the current density corresponding to 0.45V is hydrogen permeation current.
(6) The ventilation time test method comprises the following steps: the total volume of gas permeated from the anode side to the cathode side was tested for the time required to reach 0.5ml while maintaining the gas pressure in the anode side flow field at 100 kPa.
(7) Stopping the experiment when the hydrogen permeation current is more than 10mA/cm 2 or the ventilation time is less than 1 s.
(8) The durability test is carried out on the No. 1 proton exchange membrane and the No. 2 proton exchange membrane by adopting the method, and the hydrogen permeation current and the ventilation time in the durability process are tested, for example, as shown in the graph of FIG. 3 and the graph of FIG. 4.
The comparison of the two samples is used here to illustrate the effectiveness of the method, with the results obtained being different for samples of different durability. If a single sample is evaluated, the end point of the experiment need only be determined according to the criteria described in item (7).
(9) From the results of fig. 3-4, it can be seen that when the permeation time is less than 1s, the hydrogen permeation current of the proton exchange membrane does not change significantly, so that the change of the gas barrier property of the proton exchange membrane cannot be visually represented by using the hydrogen permeation current. As can be seen from the results of FIG. 4, the ventilation time of the No. 1 proton exchange membrane is less than 1s after 368h acceleration test; the ventilation time of the No. 2 proton exchange membrane is less than 1s after being subjected to 2162h acceleration test, namely the No. 2 proton exchange membrane can withstand longer acceleration evaluation. Thus, the proton exchange membrane #2 has much better durability than the proton exchange membrane # 1.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (3)
1. A method for accelerating the evaluation of durability of a proton exchange membrane for a fuel cell, comprising:
s1, preparing a full-size membrane electrode assembly;
s2, assembling the fuel cell by utilizing the full-size membrane electrode assembly, introducing hydrogen into an anode side flow field of the fuel cell, and introducing air into a cathode side flow field of the fuel cell;
S3, controlling the temperature of the battery according to the general running state of the fuel battery; controlling the temperature of the battery to be 80 ℃;
s4, synchronously switching the humidity of the input hydrogen and the humidity of the air according to a fixed time interval, wherein the relative humidity of the hydrogen and the air is switched between 0% RH and 100% RH;
S5, obtaining hydrogen permeation current and ventilation time of the fuel cell in the evaluation process until any one of the hydrogen permeation current and ventilation time reaches a preset test termination condition;
Obtaining hydrogen permeation current of the fuel cell in the evaluation process comprises the following steps:
purging the fuel cell by taking hydrogen as anode gas of the fuel cell and taking nitrogen as cathode gas of the fuel cell;
controlling the open circuit voltage of the fuel cell to be 0.1V;
Adopting a potentiostat to perform linear voltage scanning operation on the fuel cell, wherein the scanning range is 0.1V-0.6V, and the scanning speed is 0.002V/s;
obtaining the corresponding current density when the scanning voltage is 0.45V as hydrogen permeation current;
obtaining a gas permeation time of the fuel cell during the evaluation process, comprising:
Maintaining a gas pressure in the anode-side flow field of the fuel cell at 100kPa;
Testing the total volume of gas permeated from the anode side to the cathode side of the fuel cell to 0.5ml as a permeation time;
And S6, drawing a change curve of hydrogen permeation current and ventilation time in the test process, and obtaining an evaluation result of the durability of the proton exchange membrane according to the change curve of the hydrogen permeation current, wherein the time of the acceleration test duration is obtained when the ventilation time is less than 1S, and the longer the time of the acceleration test duration is when the ventilation time is less than 1S, the stronger the durability of the proton exchange membrane can be.
2. The method for accelerated evaluation of durability of proton exchange membrane for fuel cell as claimed in claim 1, wherein the termination condition of the preset test is hydrogen permeation current of more than 10mA/cm 2 or permeation time of less than 1s.
3. The method for accelerated evaluation of durability of proton exchange membrane for fuel cell according to claim 1, wherein the preparing of the full-size membrane electrode assembly comprises:
cutting the proton exchange membrane to obtain the proton exchange membrane with the size completely consistent with that in the actual application scene of the fuel cell, and evaluating the durability;
According to the actual shaping process, preparing catalytic layers on two sides of the proton exchange membrane to be evaluated, and matching corresponding gas diffusion layers and frames, thereby obtaining the full-size membrane electrode assembly.
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CN117250130B (en) * | 2023-11-20 | 2024-02-06 | 华电重工机械有限公司 | Proton exchange membrane hydrogen permeation testing method |
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