CN110530954B - Method for testing durability of non-noble metal catalyst membrane electrode - Google Patents
Method for testing durability of non-noble metal catalyst membrane electrode Download PDFInfo
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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
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/04—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids
- H01M8/04298—Processes for controlling fuel cells or fuel cell systems
- H01M8/04313—Processes for controlling fuel cells or fuel cell systems characterised by the detection or assessment of variables; characterised by the detection or assessment of failure or abnormal function
- H01M8/04537—Electric variables
- H01M8/04634—Other electric variables, e.g. resistance or impedance
- H01M8/04641—Other electric variables, e.g. resistance or impedance of the individual fuel cell
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/04—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids
- H01M8/04298—Processes for controlling fuel cells or fuel cell systems
- H01M8/04313—Processes for controlling fuel cells or fuel cell systems characterised by the detection or assessment of variables; characterised by the detection or assessment of failure or abnormal function
- H01M8/04664—Failure or abnormal function
- H01M8/04671—Failure or abnormal function of the individual fuel cell
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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
Abstract
The invention discloses a method for testing the durability of a non-noble metal catalyst membrane electrode, which comprises the steps of respectively testing the initial polarization curve, ohmic impedance and cathode catalyst layer proton conduction impedance of the membrane electrode, then carrying out constant-voltage discharge attenuation test on the membrane electrode, then testing the polarization curve, ohmic impedance and cathode catalyst layer proton conduction impedance after membrane electrode attenuation, then introducing dry nitrogen into the membrane electrode for purging, and finally testing the polarization curve after membrane electrode nitrogen purging by using an electrochemical workstation. Aiming at the non-noble metal catalyst membrane electrode, the testing conditions are the same as the membrane electrode testing conditions by testing the polarization curve before and after the constant-voltage discharge attenuation of the membrane electrode, the ohmic impedance and the proton impedance of the cathode catalyst layer and the polarization curve before and after the nitrogen purging of the membrane electrode, and the testing data are real and reliable. The membrane electrode durability test can be comprehensively carried out from three angles of activation polarization, ohmic polarization and mass transfer polarization, and has important significance for the development of non-noble metal catalyst membrane electrodes.
Description
Technical Field
The invention relates to the technical field of fuel cells, in particular to a method for testing the durability of a non-noble metal catalyst membrane electrode.
Background
Proton exchange membrane fuel cells convert chemical energy in fuel directly into electrical energy, and are of great interest because of their advantages of low pollution, zero emissions, high conversion efficiency, and the like. However, the development of high performance of proton exchange membrane fuel cells at present relies on noble metal Pt catalysts for the cathode. The metal Pt has the problems of low reserves, high price, catalyst poisoning and the like, and the problems restrict the large-scale application of the proton exchange membrane fuel cell. Finding and using a highly efficient non-noble metal catalyst instead of a Pt catalyst is therefore key to the development of this pem fuel cell technology.
Non-noble metal catalysts studied in the past can be mainly classified into the following categories: palladium-based or ruthenium-based catalysts, non-noble metal oxides, chalcogenides, oxynitrides, nitrogen-doped carbon materials, M/N/C catalysts, and non-metallic catalysts. Among them, Fe/N/C catalyst and Co/N/C having an organometallic framework structure show high Oxygen Reduction Reaction (ORR) activity, and are considered to have the most promising development prospect. Transition metals Fe and Co are low in price and high in reserves, and since Jasinski reports that transition metal porphyrin and phthalocyanine can remarkably improve ORR catalytic activity in 1964, the transition metal doped with N is widely researched for catalyzing ORR reaction. In 2006, Zelenay synthesizes a catalyst with a Co-N structure without a pyrolysis method, retains the catalyst, shows good stability, and has low catalytic performance. In 2011, Dodelet et al prepares a Fe/Phen/ZIF8 catalyst by using an imidazole zeolite Zn (II) Metal Organic Framework (MOF) as a Fe and N precursor, and greatly improves the performance when the compensation resistance correction voltage is 0.8V and the volume current density is 230A-cm 3.
Although there are many studies on the synthesis technology of Fe/N/C and Co/N/C catalysts with M/N/C structure, the durability of membrane electrodes is still a major challenge for large-scale application of such non-noble metal catalysts. The performance of the non-noble metal catalyst membrane electrode can be reduced by up to 50% in the initial 20h under the condition of constant-voltage discharge. However, the attenuation mechanism is not clear, and studies on durability test are rarely reported, and there is no clear attenuation test method. Few studies in the past have also focused on the effect of the reduction in activation polarization, i.e., the activity of the catalyst itself, on the performance degradation of the membrane electrode. The effects of ohmic polarization and mass transfer polarization are not considered; the transition metal can pollute resin in the membrane electrode in an acid environment, so that ohmic impedance of the membrane electrode and proton conduction impedance of a catalyst layer are increased, and the performance of the membrane electrode is reduced; flooding of the active sites in the cathode catalytic layer can increase the cathode oxygen transmission resistance and also can lead to degradation of membrane electrode performance. Therefore, the method for testing the durability of the non-noble metal catalyst proton exchange membrane fuel cell membrane electrode is researched, the reason of membrane electrode attenuation is comprehensively tested from three angles of activation polarization, ohmic polarization and mass transfer polarization, and the method has important significance for the development of the non-noble metal catalyst membrane electrode of the proton exchange membrane fuel cell.
Disclosure of Invention
In view of this, the technical problem to be solved by the present invention is to provide a method for testing the durability of a non-noble metal catalyst membrane electrode of a proton exchange membrane fuel cell.
The purpose of the invention is realized by the following technical scheme:
the invention provides a durability test method of a non-noble metal catalyst, which comprises the following steps:
A. testing the initial polarization curve of the membrane electrode to obtain the initial active current density;
B. testing the initial ohmic impedance of the membrane electrode and the proton impedance of the cathode catalyst layer;
C. performing constant-voltage discharge attenuation test on the membrane electrode;
D. testing the polarization curve of the attenuated membrane electrode, and testing the density of the active current after attenuation to obtain the test result of the activity reduction of the attenuated membrane electrode;
E. testing the ohmic impedance of the attenuated membrane electrode and the proton impedance of the cathode catalyst layer to obtain a test result of the impedance rise of the attenuated membrane electrode;
F. and introducing dry nitrogen into the membrane electrode for purging, and testing the polarization curve of the membrane electrode after nitrogen purging to obtain the test result of the membrane electrode performance influenced by flooding after the membrane electrode is attenuated.
Preferably, the cathode catalyst in the membrane electrode is a non-noble metal catalyst with an M/N/C structure, wherein the metal M is any one or combination of Fe, Co and Co.
Preferably, the test method of the polarization curve is a constant voltage discharge method.
Preferably, the constant voltage discharge method specifically employs: introducing hydrogen into the anode, introducing pure oxygen into the cathode, wherein the relative humidity is 80-100%, the backpressure is 50-150 kPa, and the temperature is 60-80 ℃; the voltage range is 0.2-0.95V, the voltage is stabilized at intervals of 0.05V for 60-300 s, and the discharge current is tested and recorded. Aiming at the characteristics of non-noble metal catalysts, the invention optimizes the humidity, the back pressure, the temperature and the voltage test interval of the constant voltage discharge method, the test speed is high, and the measured polarization curve result is stable and accurate.
Preferably, the active current density is a discharge current density of the membrane electrode under a voltage of 0.7-0.8V.
Preferably, the ohmic impedance and the proton impedance of the cathode catalyst layer are measured by an alternating current impedance method.
Preferably, the ac impedance method specifically employs: introducing hydrogen into the anode, introducing nitrogen into the cathode, wherein the relative humidity is 80-100%, the backpressure is 50-150 kPa, and the temperature is 60-80 ℃; the frequency range is 0.1-100000 Hz, the voltage range is 0.2-0.4V, and the disturbance amplitude of the voltage is 5-10%; the intercept of the real axis of the measured AC impedance spectrum is ohmic impedance, and the projection of a 45-degree line segment in a high-frequency region on the real axis is the equivalent proton conduction impedance of the cathode catalyst layer. The alternating current impedance method used by the invention optimizes the test voltage range aiming at the characteristics of the non-noble metal catalyst membrane electrode, avoids the interference of electrochemical reaction and has accurate test result.
Preferably, the constant voltage discharge decay test specifically employs: the discharge voltage is 0.4-0.6V, and the discharge time is 20-300 h.
The invention provides a method for testing the durability of a non-noble metal catalyst membrane electrode, which comprises the steps of respectively testing an initial polarization curve, ohmic impedance and cathode catalyst layer proton conduction impedance of the membrane electrode by using an electrochemical workstation, then carrying out attenuation test on constant-voltage discharge on the membrane electrode, testing the polarization curve, ohmic impedance and cathode catalyst layer proton conduction impedance after the membrane electrode is attenuated by using the electrochemical workstation, then introducing dry nitrogen to the membrane electrode for purging, and finally testing the polarization curve after the membrane electrode is purged by using the electrochemical workstation.
The durability test method provided by the invention can test the integral attenuation result and can specifically test and analyze the durability of the membrane electrode in three aspects of activation polarization, ohmic polarization and mass transfer polarization. And the attenuation of the non-noble metal catalyst membrane electrode is verified, which is caused by the three factors of the reduction of the membrane electrode activity, the increase of the impedance and the increase of the mass transfer resistance.
Compared with the prior art, the invention has the following beneficial effects:
aiming at the non-noble metal catalyst membrane electrode, the testing conditions are the same as the membrane electrode testing conditions by testing the polarization curve before and after the constant-voltage discharge attenuation of the membrane electrode, the ohmic impedance and the proton impedance of the cathode catalyst layer and the polarization curve before and after the nitrogen purging of the membrane electrode, and the testing data are real and reliable. By testing the membrane electrode alternating current impedance spectrum, the ohmic impedance before and after the membrane electrode attenuation and the proton conduction impedance of the cathode catalyst layer can be obtained. The water of the membrane electrode is drained through nitrogen purging, so that membrane electrode flooding can be avoided, and the mass transfer problem of the membrane electrode after attenuation is inspected. The method can analyze the attenuation of the membrane electrode at the catalyst activity reduction angle, can comprehensively test the membrane electrode durability from three angles of activation polarization, ohmic polarization and mass transfer polarization, and has important significance for the development of the membrane electrode of the non-noble metal catalyst proton exchange membrane fuel cell.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a graph of the constant voltage discharge decay test current of the membrane electrode of the present invention as a function of time;
FIG. 2 is a plot of polarization before and after attenuation of a membrane electrode according to the present invention;
FIG. 3 is an AC impedance spectrum before and after the membrane electrode attenuation of the present invention;
FIG. 4 is a polarization curve diagram before and after nitrogen gas is introduced into the membrane electrode of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The following example provides a non-noble metal catalyst durability test method comprising the steps of:
A. testing the initial polarization curve of the membrane electrode to obtain the initial active current density;
B. testing the initial ohmic impedance of the membrane electrode and the proton impedance of the cathode catalyst layer;
C. performing constant-voltage discharge attenuation test on the membrane electrode;
D. testing the polarization curve of the attenuated membrane electrode, and testing the density of the active current after attenuation to obtain the test result of the activity reduction of the attenuated membrane electrode;
E. testing the ohmic impedance of the attenuated membrane electrode and the proton impedance of the cathode catalyst layer to obtain a test result of the impedance rise of the attenuated membrane electrode;
F. and introducing dry nitrogen into the membrane electrode for purging, and testing the polarization curve of the membrane electrode after nitrogen purging to obtain the test result of the membrane electrode performance influenced by flooding after the membrane electrode is attenuated.
The cathode catalyst in the membrane electrode is a non-noble metal catalyst with an M/N/C structure, wherein the metal M is any one or combination of Fe and Co.
The testing method of the polarization curve is a constant voltage discharge method.
The constant voltage discharge method specifically adopts: introducing hydrogen into the anode, introducing pure oxygen into the cathode, wherein the relative humidity is 80-100%, the backpressure is 50-150 kPa, and the temperature is 60-80 ℃; the voltage range is 0.2-0.95V, the voltage is stabilized at intervals of 0.05V for 60-300 s, and the discharge current is tested and recorded.
The testing method of the ohmic impedance and the proton impedance of the cathode catalyst layer is an alternating current impedance method.
The ac impedance method specifically employs: introducing hydrogen into the anode, introducing nitrogen into the cathode, wherein the relative humidity is 80-100%, the backpressure is 50-150 kPa, and the temperature is 60-80 ℃; the frequency range is 0.1-100000 Hz, the voltage range is 0.2-0.4V, and the disturbance amplitude of the voltage is 5-10%; the intercept of the real axis of the measured AC impedance spectrum is ohmic impedance, and the projection of a 45-degree line segment in a high-frequency region on the real axis is the equivalent proton conduction impedance of the cathode catalyst layer.
The constant voltage discharge decay test specifically adopts: the discharge voltage is 0.4-0.6V, and the discharge time is 20-300 h.
Example 1
The embodiment provides a method for testing the durability of a non-noble metal catalyst (Fe/N/C catalyst) membrane electrode, which comprises the following steps:
1) testing of membrane electrode polarization curves before attenuation with electrochemical workstation
The anode of the membrane electrode is filled with hydrogen, and the cathode is filled with pure oxygen. The relative humidity used was 100%, the back pressure used was 150kPa, and the temperature used was 80 ℃. The voltage range is 0.2-0.95V, the voltage is stabilized for 60s every 0.05V, and the discharge current is tested and recorded.
2) Testing the membrane electrode ohmic impedance and catalytic layer proton conduction impedance before attenuation with an electrochemical workstation
Introducing hydrogen into the anode of the membrane electrode, introducing nitrogen into the cathode, wherein the relative humidity is 100%, the backpressure is 150kPa, and the temperature is 80 ℃. The frequency range is 0.1-100000 Hz, the voltage is 0.4V, and the disturbance amplitude of the voltage is 5%. The intercept of the real axis of the measured AC impedance spectrum is ohmic impedance, and the projection of a 45-degree line segment in a high-frequency region on the real axis is the equivalent proton conduction impedance of the cathode catalyst layer.
3) Membrane electrode constant voltage discharge decay test
The anode of the membrane electrode is filled with hydrogen, and the cathode is filled with pure oxygen. The relative humidity used was 100%, the back pressure used was 150kPa, and the temperature used was 80 ℃. The voltage is constant at 0.4V, and the discharge time is 20 h. FIG. 1 is a graph of current density versus time for membrane electrode constant voltage decay test, from an initial 2000mA/cm2Decreased to 960mA/cm2。
4) Membrane electrode polarization curve after attenuation test by electrochemical workstation
The anode of the membrane electrode is filled with hydrogen, and the cathode is filled with pure oxygen. The relative humidity used was 100%, the back pressure used was 150kPa, and the temperature used was 80 ℃. The voltage range is 0.2-0.85V, the voltage is stabilized for 60s every 0.05V, and the discharge current is tested and recorded.FIG. 2 is a comparison of the polarization curves of the membrane electrode before and after attenuation. Active current density of 160mA/cm at voltage of 0.75V before attenuation2After attenuation, the active current density at a voltage of 0.75V is reduced to 50mA/cm2. The loss of the active current density after attenuation exceeds 30 percent, which indicates that the activity of the membrane electrode catalyst is seriously attenuated.
5) Testing ohmic impedance of membrane electrode and proton conduction impedance of catalytic layer after attenuation by electrochemical workstation
Introducing hydrogen into the anode of the membrane electrode, introducing nitrogen into the cathode, wherein the relative humidity is 100%, the backpressure is 150kPa, and the temperature is 80 ℃. The frequency range is 0.1-100000 Hz, the voltage is 0.4V, and the disturbance amplitude of the voltage is 5%. The intercept of the real axis of the measured AC impedance spectrum is ohmic impedance, and the projection of a 45-degree line segment in a high-frequency region on the real axis is the equivalent proton conduction impedance of the cathode catalyst layer. FIG. 3 is a comparison graph of AC impedance spectra before and after membrane electrode attenuation. The ohmic resistance of the membrane electrode is from 70m omega cm2Rise to 100m omega cm2Increased by 43 percent, and the current density is 1000mA/cm2The equivalent attenuation voltage loss is 0.03V; the equivalent proton conduction impedance of the cathode catalyst layer is from 202m omega cm2Rise to 251m omega cm2Increased by 24% and the current density is 1000mA/cm2The equivalent attenuation voltage loss was 0.05V. The ohmic resistance and the equivalent proton resistance of the cathode catalyst layer after attenuation both exceed 20 percent, which indicates that the proton conduction capability of the membrane electrode is seriously attenuated.
6) And introducing dry nitrogen into the attenuated membrane electrode for purging, draining the water in the membrane electrode and preventing flooding.
7) Testing polarization curve of membrane electrode after nitrogen purging by electrochemical workstation
The anode of the membrane electrode is filled with hydrogen, and the cathode is filled with pure oxygen. The relative humidity used was 100%, the back pressure used was 150kPa, and the temperature used was 80 ℃. The voltage range is 0.2-0.95V, the voltage is stabilized for 60s every 0.05V, and the discharge current is tested and recorded. FIG. 4 is a comparison graph of the polarization curves of the membrane electrode before and after nitrogen purging and before and after attenuation, which shows that the membrane electrode performance rises again when the current density is 1000mA/cm after the membrane electrode attenuation is affected by flooding2Voltage of membrane electrodeThe voltage rises from 0.39V to 0.44V, and the voltage loss caused by flooding is 0.05V. After attenuation, at a current density of 1000mA/cm2And the voltage loss caused by flooding exceeds 0.01V, which indicates that the mass transfer capacity of the membrane electrode oxygen is seriously attenuated.
8) At a current density of 1000mA/cm2At this point, the membrane electrode voltage dropped from 0.55V before the decay to 0.39V after the decay, with a total voltage loss of 0.16V. Wherein the voltage loss due to ohmic resistance rise is 0.03V; the voltage loss due to the increase of the equivalent proton conduction resistance of the catalytic layer was 0.05V; the voltage loss caused by the mass transfer resistance increase of the membrane electrode due to flooding is 0.05V; the remaining portion was 0.03V in voltage loss due to a decrease in membrane electrode activity.
The invention has many applications, and the above description is only a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention, and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that various modifications can be made without departing from the principles of the invention and these modifications are to be considered within the scope of the invention.
Claims (7)
1. A non-noble metal catalyst membrane electrode durability test method is characterized by comprising the following steps:
A. testing the initial polarization curve of the membrane electrode to obtain the initial active current density;
B. testing the initial ohmic impedance of the membrane electrode and the proton impedance of the cathode catalyst layer;
C. performing constant-voltage discharge attenuation test on the membrane electrode;
D. testing the polarization curve of the attenuated membrane electrode, and testing the density of the active current after attenuation to obtain the test result of the activity reduction of the attenuated membrane electrode;
E. testing the ohmic impedance of the attenuated membrane electrode and the proton impedance of the cathode catalyst layer to obtain a test result of the impedance rise of the attenuated membrane electrode;
F. and introducing dry nitrogen into the membrane electrode for purging, and testing the polarization curve of the membrane electrode after nitrogen purging to obtain the test result of the membrane electrode performance influenced by flooding after the membrane electrode is attenuated.
2. The non-noble metal catalyst membrane electrode durability test method according to claim 1, wherein the cathode catalyst in the membrane electrode is a non-noble metal catalyst having an M/N/C structure, wherein the metal M is any one of iron and cobalt or a combination thereof.
3. The method for testing the durability of the non-noble metal catalyst membrane electrode according to claim 1, wherein the method for testing the polarization curve is a constant voltage discharge method, and the active current density is the membrane electrode discharge current density under the voltage of 0.7-0.8V.
4. The non-noble metal catalyst membrane electrode durability test method according to claim 3, wherein the constant voltage discharge method specifically employs: introducing hydrogen into the anode, introducing pure oxygen into the cathode, wherein the relative humidity is 80-100%, the backpressure is 50-150 kPa, and the temperature is 60-80 ℃; the voltage range is 0.2-0.95V, the voltage is stabilized at intervals of 0.05V for 60-300 s, and the discharge current is tested and recorded.
5. The non-noble metal catalyst membrane electrode durability test method according to claim 1, wherein the test method of the ohmic resistance and the cathode catalyst layer proton resistance is an alternating current impedance method.
6. The non-noble metal catalyst membrane electrode durability test method according to claim 5, wherein the ac impedance method specifically employs: introducing hydrogen into the anode, introducing nitrogen into the cathode, wherein the relative humidity is 80-100%, the backpressure is 50-150 kPa, and the temperature is 60-80 ℃; the frequency range is 0.1-100000 Hz, the voltage range is 0.2-0.4V, and the disturbance amplitude of the voltage is 5-10%; the intercept of the real axis of the measured AC impedance spectrum is ohmic impedance, and the projection of a 45-degree line segment in a high-frequency region on the real axis is the equivalent proton conduction impedance of the cathode catalyst layer.
7. The method for testing the durability of the non-noble metal catalyst membrane electrode according to claim 1, wherein the constant voltage discharge decay test specifically adopts: the discharge voltage is 0.4-0.6V, and the discharge time is 20-300 h.
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| CN111060580A (en) * | 2019-12-26 | 2020-04-24 | 先进储能材料国家工程研究中心有限责任公司 | Acceleration evaluation test method for membrane electrode of fuel cell |
| CN111103545A (en) * | 2019-12-27 | 2020-05-05 | 浙江锋源氢能科技有限公司 | Fuel cell membrane electrode performance testing method |
| CN111458398A (en) * | 2020-03-25 | 2020-07-28 | 先进储能材料国家工程研究中心有限责任公司 | Accelerated evaluation method for catalyst material for fuel cell |
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| CN114725438B (en) * | 2021-01-05 | 2024-04-23 | 广州汽车集团股份有限公司 | Fuel cell water management method and system |
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| CN114976051A (en) * | 2022-05-26 | 2022-08-30 | 深圳航天科技创新研究院 | Method for regulating and controlling performance of non-platinum catalyst fuel cell |
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