CN114018797A - Corrosion resistance testing method for fuel cell metal bipolar plate coating - Google Patents
Corrosion resistance testing method for fuel cell metal bipolar plate coating Download PDFInfo
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- CN114018797A CN114018797A CN202111166383.6A CN202111166383A CN114018797A CN 114018797 A CN114018797 A CN 114018797A CN 202111166383 A CN202111166383 A CN 202111166383A CN 114018797 A CN114018797 A CN 114018797A
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- 238000005260 corrosion Methods 0.000 title claims abstract description 78
- 230000007797 corrosion Effects 0.000 title claims abstract description 78
- 238000000576 coating method Methods 0.000 title claims abstract description 63
- 239000011248 coating agent Substances 0.000 title claims abstract description 61
- 239000000446 fuel Substances 0.000 title claims abstract description 41
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 39
- 239000002184 metal Substances 0.000 title claims abstract description 39
- 238000012360 testing method Methods 0.000 title claims abstract description 24
- 230000010287 polarization Effects 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000006056 electrooxidation reaction Methods 0.000 claims abstract description 5
- 238000004806 packaging method and process Methods 0.000 claims abstract description 5
- 238000004458 analytical method Methods 0.000 claims abstract description 3
- 238000010998 test method Methods 0.000 claims description 11
- 238000005530 etching Methods 0.000 claims description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 2
- 229910000372 mercury(II) sulfate Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 238000010828 elution Methods 0.000 claims 1
- 238000013461 design Methods 0.000 abstract description 2
- 238000011161 development Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 20
- 150000002500 ions Chemical class 0.000 description 7
- 239000012528 membrane Substances 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
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- 239000012495 reaction gas Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/02—Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement
Abstract
The invention provides a corrosion resistance testing method of a fuel cell metal bipolar plate coating, which comprises the following steps: (1) packaging the metal bipolar plate to be tested in an electrochemical corrosion test pool, and adding a corrosion solution; (2) a three-electrode measuring system is adopted to control the characteristic parameters of polarization potential, and the fuel cell simulates the corrosion process of the metal bipolar plate coating under the actual operating condition; (3) and analyzing and characterizing the coating of the metal bipolar plate, and finally evaluating the corrosion resistance of the coating based on the analysis results of contact resistance, ion release concentration and film falling surface after the coating is corroded. The method is simple and easy to operate, can accurately reflect the real operating environment of the fuel cell, is used for quickly evaluating the corrosion resistance of the coating in the real operating environment of the fuel cell, and guides the design and development of the coating process.
Description
Technical Field
The invention belongs to the technical field of fuel cells, and particularly relates to a corrosion resistance testing method of a fuel cell metal bipolar plate coating.
Background
Proton Exchange Membrane Fuel cells (Proton Exchange Membrane Fuel cells, PEMFCs for short) generate electricity by using hydrogen as Fuel, and the product is water without pollution, so that the Proton Exchange Membrane Fuel cells are very environment-friendly, have been applied to automobiles, unmanned aerial vehicles, stationary power stations and the like, and have wide application prospects in various fields. The fuel cell bipolar plate plays an important role in the proton exchange membrane fuel cell stack, plays a role in collecting electrons, distributing reaction gas, discharging reaction generated water, supporting a membrane electrode and the like in the stack, occupies 80 percent of the weight of the stack and 45 percent of the cost of the stack, and has important influence on the performance of the fuel cell stack.
The proton exchange membrane fuel cell bipolar plate material mainly comprises metal, graphite, composite materials and the like. Compared with a graphite bipolar plate, the metal bipolar plate has excellent electric and thermal conductivity and good mechanical properties, and a galvanic pile formed by assembling the metal bipolar plates has the advantages of high power density, quick cold start, good vibration resistance, suitability for mass production and the like, and is a preferred choice of a fuel cell polar plate material.
However, the operating environment of the fuel cell is an acid environment (pH is approximately equal to 3) with the temperature of 60-90 ℃, the metal bipolar plate which is not subjected to modification treatment is easily corroded and oxidized in the acid potential environment of the fuel cell, and a compact oxide film is generated on the surface to reduce the conductivity of the bipolar plate; and metal ions can be released in the corrosion process, and the released ions can pollute the catalyst and the membrane electrode, so that the output performance of the fuel cell stack is further reduced. Therefore, the surface of the metal bipolar plate is coated with the conductive corrosion-resistant coating so as to meet the use requirement of the fuel cell.
In order to evaluate the corrosion resistance of the metal bipolar plate coating, the existing method mostly adopts an off-line evaluation method, a simulated corrosion solution is added into a three-electrode electrochemical measurement system, and the corrosion resistance of the coating is tested through short-time constant potential or potentiodynamic polarization. None of the currently simulated corrosive solutions completely contain the highly corrosive media generated in the fuel cell operating environment. Meanwhile, the simulated constant potential polarization or electrokinetic potential polarization cannot reflect the potential change characteristics of the fuel cell in the real operation process. Because the current testing method for the corrosion resistance of the metal bipolar plate coating does not accurately simulate the real environment of the operation of a fuel cell, especially the influence of corrosion products generated in the fuel cell on the corrosion of the coating is not fully considered, the corrosion resistance of the metal bipolar plate coating in the actual operation environment of the cell cannot be truly reflected, and the testing result of the corrosion resistance of the coating is greatly different from the corrosion resistance result of the coating in the actual operation environment of the cell. Therefore, a testing method which can reflect the corrosion process of the metal bipolar plate coating in the actual operation environment of the fuel cell more truly and effectively needs to be found to evaluate the corrosion resistance of the coating.
Disclosure of Invention
The invention aims to provide a corrosion resistance test method of a fuel cell metal bipolar plate coating, which solves the problems that the prior test method can not truly reflect the corrosion of the metal bipolar plate coating in the actual operation environment of a fuel cell and the like, so as to more truly reflect the corrosion resistance of the coating.
In order to achieve the above object of the present invention, the following technical solutions will be adopted.
A corrosion resistance test method of a fuel cell metal bipolar plate coating is characterized by comprising the following steps:
(1) packaging the metal bipolar plate to be tested in an electrochemical corrosion test pool, and adding a corrosion solution; (2) a three-electrode measuring system is adopted to control the characteristic parameters of polarization potential, and the fuel cell simulates the corrosion process of the metal bipolar plate coating under the actual operating condition; (3) analyzing and characterizing the coating of the metal bipolar plate, and finally evaluating the corrosion resistance of the coating based on the analysis results of contact resistance, ion release concentration and film falling surface after the coating is corroded;
the corrosion solution is H with the pH value of 3-52SO4Adding mass concentration into aqueous solution0.01 to 100ppm of HF and 0.01 to 100ppm of H2O2A mixture of (a); the corrosion solution should fill the corrosion tank and completely immerse the polar plate.
The three-electrode measuring system comprises a working electrode consisting of a metal bipolar plate coated with a coating, an auxiliary electrode consisting of a platinum sheet, and an auxiliary electrode consisting of Hg/HgSO4A reference electrode formed;
the simulated actual operation working condition refers to the condition that the battery potential is high or low and the duration time is used for potential polarization in the simulated actual operation working condition. According to the actual operation condition of the fuel cell and the national standard GB/T38914-; the three working conditions are simulated by constant potential electrochemical polarization, the polarization potential and time are consistent with the polarization potential characteristics in the actual battery, wherein the polarization potential is 1.6V in the start-stop working condition, and the duration time is 1s in a single cycle; polarization potential is 0.84V under the idle working condition, and the single cycle duration is 21 min; the polarization potential of the rated working condition is 0.6V, the duration time of the single cycle is 18min, the variable load working condition is simulated by adopting the electrokinetic potential polarization, the polarization potential height and time are consistent with the polarization potential characteristics of the actual battery, wherein the potential linearly changes in the range of 0.6-0.84V, the single potential loading time is 30s, the single load shedding time is 16s, and the loading and the load shedding are respectively carried out 27 times in the single cycle. In the testing process, the concentration, the testing temperature and the duration of the corrosion solution are determined according to the concentration, the testing temperature and the length of the corrosion solution in the galvanic pile under the actual operation working condition, and then the testing is carried out.
Further, the temperature of the corrosion solution is kept at 20-80 ℃.
Further, the duration of the corrosion process is 1-200 h.
Further, the corrosion resistance of the coating is evaluated mainly by analyzing parameters such as contact resistance, film falling area, porosity and ion precipitation concentration of the coating of the metal bipolar plate.
Further, if desired, metal pairs for fuel cellsThe polar plate coating is subjected to accelerated test, and the corrosion resistance test method can consider electrochemical polarization and also can not consider the electrochemical polarization, and has the difference that the acceleration coefficients are different. For example: when only the focus is mainly H2O2In the case of the corrosive effect on the coating, the electrochemical polarization of step (2) can be omitted by soaking the coated metal bipolar plate in the corrosion solution and then evaluating the corrosion resistance of the coating to the corrosive medium (e.g., example 2). When the focus is on H2O2The corrosion resistance of the coating combined with the potential makes it impossible to omit the electrochemical polarization of step (2) (e.g., example 1).
Compared with the prior art, the invention has the following beneficial effects:
the corrosion resistance test method of the fuel cell metal bipolar plate coating comprehensively considers the corrosion medium generated in the main reaction and the side reaction of the fuel cell and the working condition characteristic of actual vehicle-mounted operation, and carries out external off-line electrochemical test through a three-electrode system; the method is simple and easy to operate, can accurately reflect the real operating environment of the fuel cell, is used for quickly evaluating the corrosion resistance of the coating in the real operating environment of the fuel cell, and guides the design and development of the coating process.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 shows the optical microscopic morphology of the coating after etching in example 1 of the present invention.
FIG. 2 is an optical microscopic image of the coating after etching in example 2 of the present invention.
FIG. 3 is an optical microscopic image of the plate coating after etching in comparative example 1 of the present invention.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
Example 1
Packaging the metal bipolar plate to be tested containing the plating coating in an electrochemical corrosion testing tank, fully adding a prepared corrosion solution, and completely soaking the bipolar plate to be tested; and simulating the potential characteristics of the actual vehicle-mounted plug-in working condition, performing electrochemical polarization by adopting a three-electrode measurement system, and analyzing the corrosion current density, the contact resistance and the morphology change of an optical microscope of the coating after measuring for 150 hours.
The etching solution is H at pH =32SO40.1ppm of a mixed solution of HF was added to the aqueous solution, and 100ppm of H was added to the etching solution every 12 hours during the test2O2. The temperature of the corrosion solution is kept at 80 ℃, the potential characteristics of the simulated vehicle-mounted working condition are shown in figure 1, each hour is one cycle, and 150 cycles, namely 150 hours, are tested.
The appearance of the coating before and after corrosion is shown in figure 1, after 150 hours of corrosion, the coating has obvious corrosion shedding phenomenon, the film shedding area is 39.75 percent, and the Fe ion precipitation concentration is 0.363 ppm; 3.53 before corrosion of the coating contact resistance under the pressing force of 0.6MPa
Increased to 22.96
。
Example 2
Packaging the metal bipolar plate to be tested containing the plating coating in an electrochemical corrosion testing tank, fully adding a prepared corrosion solution, and completely soaking the bipolar plate to be tested; because only the focus is mainly H2O2The electrochemical polarization of the step (2) can be omitted due to the influence of corrosion on the coating; after soaking for 150h, the corrosion current density and the contact resistance of the coating are analyzedAnd the shape change of the optical microscope.
The etching solution is H at pH =32SO40.1ppm of a mixed solution of HF was added to the aqueous solution, and 100ppm of H was added to the etching solution every 12 hours during the test2O2. The temperature of the etching solution was maintained at 80 ℃.
The appearance of the coating before and after corrosion is shown in figure 2, after 150 hours of corrosion, the coating has obvious corrosion shedding phenomenon, the film shedding area is 42.59%, and the Fe ion precipitation concentration is 0.463 ppm. 4.06 of the coating before corrosion under the pressing force of 0.6MPa
To 88.62
。
Comparative example 1
The comparative example 1 is a bipolar plate after an actual fuel cell stack runs for 2000h, the surface micro-topography of the bipolar plate is shown in the attached figure 3, the coating has obvious corrosion and peeling phenomena, and the phenomena are basically consistent with the film peeling phenomena in the example 1 and the example 2. In addition, the practical potential characteristics of the vehicle-mounted plug-in working condition are simulated in the embodiment 1, the electrochemical polarization is carried out by adopting a three-electrode measuring system, the concentration of the released metal Fe ions after corrosion is 0.363ppm, and is similar to the concentration of the released metal Fe ions after 2000 hours of test in the comparative example, which is 0.403 ppm.
Compared with the actual comparison example, the testing method provided by the invention is closer to the corrosion state of the metal bipolar plate coating in the real operating environment of the fuel cell, and has more testing significance.
Claims (7)
1. A corrosion resistance test method of a fuel cell metal bipolar plate coating is characterized by comprising the following steps:
(1) packaging the metal bipolar plate to be tested in an electrochemical corrosion test pool, and adding a corrosion solution; (2) a three-electrode measuring system is adopted to control the characteristic parameters of polarization potential, and the fuel cell simulates the corrosion process of the metal bipolar plate coating under the actual operating condition; (3) and analyzing and characterizing the coating of the metal bipolar plate, and finally evaluating the corrosion resistance of the coating based on the analysis results of contact resistance, ion release concentration and film falling surface after the coating is corroded.
2. The method for testing corrosion resistance according to claim 1, wherein the corrosion solution is H having a pH of 3 to 52SO4Adding HF with mass concentration of 0.01-100 ppm and H with mass concentration of 0.01-100 ppm into the water solution2O2A mixture of (a); the corrosion solution should fill the corrosion tank and completely immerse the polar plate.
3. The corrosion resistance test method of claim 1, wherein the three-electrode measurement system comprises a working electrode composed of a coated metal bipolar plate, an auxiliary electrode composed of a platinum sheet, and a measuring electrode composed of Hg/HgSO4A reference electrode formed; the simulated actual operation working condition refers to the condition that the battery potential is high or low and the duration time is used for potential polarization in the simulated actual operation working condition.
4. The corrosion resistance test method according to claim 1, wherein the temperature of the etching solution is maintained at 20 to 80 ℃.
5. The corrosion resistance test method according to claim 1, wherein the duration of the corrosion process is 1 to 200 hours.
6. The corrosion resistance test method according to claim 1, wherein the corrosion resistance of the coating is evaluated by mainly analyzing parameters of contact resistance, film falling area, porosity, ion elution concentration, and the like of the coating of the metallic bipolar plate.
7. The corrosion resistance test method according to claim 1, wherein when the fuel cell metal bipolar plate coating is subjected to the accelerated test, the electrochemical polarization of step (2) is omitted directly by immersing the coated metal bipolar plate in the corrosion solution, and then evaluating the corrosion resistance of the coating against the corrosion medium.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114976135A (en) * | 2022-05-11 | 2022-08-30 | 上海大学 | System and method for testing corrosion resistance of metal bipolar plate and plating layer of hydrogen fuel cell for automobile |
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