CN110530954A - A kind of non-precious metal catalyst membrane electrode durability test method - Google Patents
A kind of non-precious metal catalyst membrane electrode durability test method Download PDFInfo
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- CN110530954A CN110530954A CN201910803326.0A CN201910803326A CN110530954A CN 110530954 A CN110530954 A CN 110530954A CN 201910803326 A CN201910803326 A CN 201910803326A CN 110530954 A CN110530954 A CN 110530954A
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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 kind of non-precious metal catalyst membrane electrode durability test methods, including testing the initial polarization curve of membrane electrode, ohmage and cathode catalysis layer proton conduction resistance respectively, then the attenuation test of constant voltage discharge is carried out to membrane electrode, polarization curve, ohmage and cathode catalysis layer proton conduction resistance after the decaying of re-test membrane electrode, then it is passed through drying nitrogen purging to membrane electrode, finally purges after-polarization curve with electrochemical workstation test film electrode nitrogen.The present invention is directed to non-precious metal catalyst membrane electrode, discharged polarization curve, ohmage and the impedance of cathode catalysis layer proton of decaying front and back and the polarization curve of membrane electrode nitrogen purging front and back by test film electrode constant voltage, test condition is identical as membrane electrode test condition, and test data is true and reliable.Three angles that can polarize from activation polarization, ohmic polarization and mass transfer carry out membrane electrode durability test comprehensively, are of great significance to the exploitation of non-precious metal catalyst membrane electrode.
Description
Technical field
The present invention relates to field of fuel cell technology more particularly to a kind of non-precious metal catalyst membrane electrode durability tests
Method.
Background technique
Proton Exchange Membrane Fuel Cells directly converts electric energy for the chemical energy in fuel, because it is with low pollution, zero-emission
It puts and attracts attention the advantages that high conversion efficiency.However, the high performance performance of Proton Exchange Membrane Fuel Cells at present depends on
The precious metals pt catalyst of cathode.Pt metal there are reserves it is low, price is high and there are catalyst poisonings the problems such as, these problems
Constrain the scale application of Proton Exchange Membrane Fuel Cells.Therefore it finds and substitutes Pt using efficient non-precious metal catalyst
Catalyst is the key that develop this Proton Exchange Membrane Fuel Cells technology.
The non-precious metal catalyst of past people research can be mainly divided into following a few classes: palladium base or ruthenium-based catalyst, non-
Metal oxide containing precious metals, chalcogen compound, nitrogen oxides, N doping type carbon material, M/N/C catalyst and non-metallic catalyst.
Wherein, the Fe/N/C catalyst with organic metal framework structure and Co/N/C show very high redox reactions (ORR)
Activity is considered most promising.Transition-metal Fe, Co price are low, and reserves are more, since Jasinski in 1964 was reported
Crossing metalloporphyrin and phthalocyanine can be obviously improved after ORR catalytic activity, and transition metal doping N is begun to for being catalyzed ORR reaction
It is widely studied.2006, Zelenay synthesized the catalyst with Co-N structure, has remained and urge not by the method for pyrolysis
Preferable stability is shown while agent, but catalytic performance is not high.Imidazoles zeolite Zn is used in Dodelet in 2011 etc.
(II) metal-organic framework (MOF) is used as Fe, and N precursor is prepared for Fe/Phen/ZIF8 catalyst, rectifys in compensation resistance
When positive voltage is 0.8V, volume current density 230Acm3, performance is greatly improved.
Although there are many Fe/N/C the and Co/N/C catalyst synthesis technology research with M/N/C structure, membrane electrode
Durability is still the significant challenge that this non-precious metal catalyst large-scale application faces.This kind of non-precious metal catalyst membrane electrode
Performance can decline up to 50% in initial 20h under the conditions of constant voltage discharge.However it is decayed, mechanism is still not clear, resistance to its
The research of long property test is also rarely reported, also without the method for specific attenuation test.The past research of minority also only focuses on
Active reduce of activation polarization, that is, catalyst itself influences membrane electrode reduced performance.Ohmic polarization and the polarized influence of mass transfer
It is not considered;Transition metal can pollute the resin in membrane electrode under acidic environment, cause membrane electrode ohmage and catalysis
The rising of layer proton conduction resistance, and then membrane electrode performance is caused to decline;The water logging of active site can make yin in cathode catalysis layer
Pole oxygen transmission resistance rises, and also results in the decline of membrane electrode performance.Therefore research non-precious metal catalyst proton exchange membrane
Fuel cell membrane electrode durability test method, from activation polarization, ohmic polarization, the comprehensive test film electricity of three angles of mass transfer polarization
The reason of pole is decayed, is of great significance to the exploitation of Proton Exchange Membrane Fuel Cells non-precious metal catalyst membrane electrode.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that providing a kind of non-precious metal catalyst proton exchange membrane combustion
Expect cell membrane-electrode durability test method.
The purpose of the present invention is what is be achieved through the following technical solutions:
The present invention provides a kind of non-precious metal catalyst durability test method, the durability test method include with
Lower step:
A, the initial polarization curve of test membrane electrode, measures initial activity current density;
B, the impedance of membrane electrode initial ohmic and cathode catalysis layer proton impedance are tested;
C, constant voltage discharge attenuation test is carried out to membrane electrode;
D, the polarization curve after the decaying of test membrane electrode, measures activated currents density after decaying, after obtaining membrane electrode decaying
The test result that activity reduces;
E, ohmage and cathode catalysis layer proton impedance after the decaying of test membrane electrode, obtains impedance liter after membrane electrode decaying
High test result;
F, drying nitrogen is passed through to membrane electrode to be purged, tests the purged polarization curve of membrane electrode nitrogen, obtain film
Water logging influences the test result of membrane electrode performance after electrode decaying.
Preferably, the cathod catalyst in the membrane electrode is the non-precious metal catalyst with M/N/C structure, wherein gold
Category M is any one in iron Fe, cobalt Co or combinations thereof.
Preferably, the test method of the polarization curve is constant voltage discharge method.
Preferably, the constant voltage discharge method specifically uses: anode is passed through hydrogen, and cathode is passed through pure oxygen, relative humidity used
It is 80~100%, back pressure used is 50kPa~150kPa, and temperature used is 60 DEG C~80 DEG C;Voltage range be 0.2~
0.95V stablizes 60~300s, test and record discharge current every 0.05V.The present invention is directed to the spy of non-precious metal catalyst
The humidity of constant voltage electric discharge, back pressure, temperature and voltage tester interval is optimized in point, and test speed is fast, surveyed pole
It is stable, accurate to change Dependence Results.
Preferably, shown activated currents density is discharge current density of the membrane electrode in the case where voltage is 0.7~0.8V.
Preferably, the ohmage and the test method of cathode catalysis layer proton impedance are AC impedence method.
Preferably, the AC impedence method specifically uses: anode is passed through hydrogen, and cathode is passed through nitrogen, relative humidity used
It is 80~100%, back pressure used is 50kPa~150kPa, and temperature used is 60 DEG C~80 DEG C;Frequency range used 0.1~
100000Hz, applied voltage 0.2~0.4V of range, applied voltage perturbation amplitude are 5%~10%;Surveyed ac impedance spectroscopy real axis
Intercept be ohmage, 45 ° of line segments of high frequency region are projected as the equivalent proton conduction resistance of cathode catalysis layer real axis.The present invention
AC impedence method used is directed to the characteristics of non-precious metal catalyst membrane electrode, is optimized, avoids to test voltage range
The interference of electrochemical reaction, test result are accurate.
Preferably, the constant voltage discharge attenuation test specifically uses: discharge voltage is 0.4~0.6V, discharge time 20
~300h.
The present invention provides a kind of non-precious metal catalyst membrane electrode durability test methods, including with electrochemical workstation
Membrane electrode initial polarization curve, ohmage and cathode catalysis layer proton conduction resistance are tested respectively, and then membrane electrode is carried out
The attenuation test of constant voltage discharge, then urged with electrochemical workstation test film electrode decaying after-polarization curve, ohmage and cathode
Change layer proton conduction resistance, is then passed through drying nitrogen purging to membrane electrode, finally uses electrochemical workstation test film electrode nitrogen
After-polarization curve is swept in air-blowing.
Durability test method provided by the invention can not only test whole attenuation results, can also be with regard to the work
Change polarization, the durability of ohmic polarization and three aspects of mass transfer polarization specific test and analysis membrane electrode.And your non-gold demonstrated
The decaying of metal catalyst membrane electrode is to increase three aspect factors by the reduction of membrane electrode activity, impedance raising, resistance to mass tranfer to cause
's.
Compared with prior art, the present invention have it is following the utility model has the advantages that
The present invention is directed to non-precious metal catalyst membrane electrode, and the polarization before and after decaying of being discharged by test film electrode constant voltage is bent
The polarization curve of line, ohmage and the impedance of cathode catalysis layer proton and membrane electrode nitrogen purging front and back, test condition and film
Electrode test condition is identical, and test data is true and reliable.It is composed by test film electrode AC impedance, membrane electrode decaying can be obtained
The ohmage and cathode catalysis layer proton conduction resistance of front and back.Membrane electrode moisture is drained by nitrogen purging, it can be to avoid film
Membrane electrode mass transfer problem after decaying is investigated in electrode water logging.This method not only can be with catalyst activity reduction angle analysis membrane electrode
Decaying, three angles that can also polarize from activation polarization, ohmic polarization and mass transfer carry out membrane electrode durability test comprehensively, to non-
The exploitation of noble metal catalyst membrane electrode of fuel batter with proton exchange film is of great significance.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon:
Fig. 1 is that inventive film electrode constant voltage discharges attenuation test electric current with time changing curve figure;
Fig. 2 is inventive film electrode decaying front and back polarization curve;
Fig. 3 is AC impedance spectroscopy before and after inventive film electrode is decayed;
Fig. 4 is that inventive film electrode leads to polarization curve before and after nitrogen.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
Following embodiment provides a kind of non-precious metal catalyst durability test method, the durability test method packet
Include following steps:
A, the initial polarization curve of test membrane electrode, measures initial activity current density;
B, the impedance of membrane electrode initial ohmic and cathode catalysis layer proton impedance are tested;
C, constant voltage discharge attenuation test is carried out to membrane electrode;
D, the polarization curve after the decaying of test membrane electrode, measures activated currents density after decaying, after obtaining membrane electrode decaying
The test result that activity reduces;
E, ohmage and cathode catalysis layer proton impedance after the decaying of test membrane electrode, obtains impedance liter after membrane electrode decaying
High test result;
F, drying nitrogen is passed through to membrane electrode to be purged, tests the purged polarization curve of membrane electrode nitrogen, obtain film
Water logging influences the test result of membrane electrode performance after electrode decaying.
Cathod catalyst in the membrane electrode is the non-precious metal catalyst with M/N/C structure, and wherein metal M is iron
In Fe, cobalt Co any one or combinations thereof.
The test method of the polarization curve is constant voltage discharge method.
The constant voltage discharge method specifically uses: anode is passed through hydrogen, and cathode is passed through pure oxygen, and relative humidity used is 80~
100%, back pressure used is 50kPa~150kPa, and temperature used is 60 DEG C~80 DEG C;Voltage range is 0.2~0.95V, every
0.05V stablizes 60~300s, test and record discharge current.
The ohmage and the test method of cathode catalysis layer proton impedance are AC impedence method.
The AC impedence method specifically uses: anode is passed through hydrogen, and cathode is passed through nitrogen, and relative humidity used is 80~
100%, back pressure used is 50kPa~150kPa, and temperature used is 60 DEG C~80 DEG C;0.1~100000Hz of frequency range used,
Applied voltage 0.2~0.4V of range, applied voltage perturbation amplitude are 5%~10%;The intercept of surveyed ac impedance spectroscopy real axis is
Ohmage, 45 ° of line segments of high frequency region are projected as the equivalent proton conduction resistance of cathode catalysis layer real axis.
The constant voltage discharge attenuation test specifically uses: for discharge voltage for 0.4~0.6V, discharge time is 20~300h.
Embodiment 1
A kind of non-precious metal catalyst (Fe/N/C catalyst) membrane electrode durability test method is present embodiments provided, is wrapped
Include following steps:
1) decaying membrane electrode polarization curve is tested with electrochemical workstation
Membrane electrode anode is passed through hydrogen, and cathode is passed through pure oxygen.Relative humidity used is 100%, and back pressure used is 150kPa,
Temperature used is 80 DEG C.Voltage range is 0.2~0.95V, stablizes 60s, test and record discharge current every 0.05V.
2) decaying membrane electrode ohmage and Catalytic Layer proton conduction resistance are tested with electrochemical workstation
Membrane electrode anode is passed through hydrogen, and cathode is passed through nitrogen, and relative humidity used is 100%, and back pressure used is 150kPa,
Temperature used is 80 DEG C.0.1~100000Hz of frequency range used, applied voltage 0.4V, applied voltage perturbation amplitude are
5%.The intercept of surveyed ac impedance spectroscopy real axis is ohmage, and 45 ° of line segments of high frequency region are projected as cathode catalysis layer in real axis
Equivalent proton conduction resistance.
3) membrane electrode constant voltage discharge attenuation test
Membrane electrode anode is passed through hydrogen, and cathode is passed through pure oxygen.Relative humidity used is 100%, and back pressure used is 150kPa,
Temperature used is 80 DEG C.Constant voltage is 0.4V, and discharge 20h.Fig. 1 is that membrane electrode constant pressure attenuation test current density becomes at any time
Change curve graph, current density is from initial 2000mA/cm2, drop to 960mA/cm2。
4) decaying caudacoria electrode polarization curve is tested with electrochemical workstation
Membrane electrode anode is passed through hydrogen, and cathode is passed through pure oxygen.Relative humidity used is 100%, and back pressure used is 150kPa,
Temperature used is 80 DEG C.Voltage range is 0.2~0.85V, stablizes 60s, test and record discharge current every 0.05V.Fig. 2 is
Decaying front and back membrane electrode polarization curve comparison diagram.Activated currents density 160mA/cm under voltage 0.75V before decaying2, electric after decaying
Activated currents density drops to 50mA/cm under pressure 0.75V2.Activated currents density loss is more than 30% after decaying, illustrates membrane electrode
Catalyst activity decaying is serious.
5) decaying caudacoria electrode ohmic impedance and Catalytic Layer proton conduction resistance are tested with electrochemical workstation
Membrane electrode anode is passed through hydrogen, and cathode is passed through nitrogen, and relative humidity used is 100%, and back pressure used is 150kPa,
Temperature used is 80 DEG C.0.1~100000Hz of frequency range used, applied voltage 0.4V, applied voltage perturbation amplitude are
5%.The intercept of surveyed ac impedance spectroscopy real axis is ohmage, and 45 ° of line segments of high frequency region are projected as cathode catalysis layer in real axis
Equivalent proton conduction resistance.Fig. 3 is ac impedance spectroscopy comparison diagram before and after membrane electrode is decayed.Membrane electrode ohmage is from 70m Ω
cm2Rise to 100m Ω cm2, 43% is risen, is 1000mA/cm in current density2Place, the equivalent attenuation loss of voltage are
0.03V;The equivalent proton conduction resistance of cathode catalysis layer is from 202m Ω cm2Rise to 251m Ω cm2, 24% is risen, in electricity
Current density is 1000mA/cm2Place, the equivalent attenuation loss of voltage are 0.05V.Ohmage and the equivalent matter of cathode catalysis layer after decaying
Sub- impedance increase illustrates that the decaying of membrane electrode proton conducting ability is serious more than 20%.
6) drying nitrogen is passed through to the membrane electrode after decaying to be purged, drain moisture in membrane electrode, prevent water logging.
7) caudacoria polarization of electrode curve is purged with electrochemical workstation test nitrogen
Membrane electrode anode is passed through hydrogen, and cathode is passed through pure oxygen.Relative humidity used is 100%, and back pressure used is 150kPa,
Temperature used is 80 DEG C.Voltage range is 0.2~0.95V, stablizes 60s, test and record discharge current every 0.05V.Fig. 4 is
Nitrogen purging front and back and decaying front and back membrane electrode polarization curve comparison diagram, it can be seen that the shadow that discharge water logging decays for membrane electrode
After sound, membrane electrode performance is gone up, in current density 1000mA/cm2Place, membrane electrode voltage goes back up to 0.44V from 0.39V, because of water
The loss of voltage caused by flooding is 0.05V.After decaying, in current density 1000mA/cm2Place, the loss of voltage as caused by water logging surpass
0.01V is crossed, illustrates that the decaying of membrane electrode oxygen mass transfer ability is serious.
8) in current density 1000mA/cm2Place, membrane electrode voltage 0.55V before decaying drop to 0.39V after decaying, electricity
Crushing, which loses, amounts to 0.16V.The loss of voltage caused by wherein rising because of ohmage is 0.03V;Because of the equivalent proton conduction of Catalytic Layer
The loss of voltage caused by impedance rise is 0.05V;Membrane electrode due to water logging resistance to mass tranfer increase caused by the loss of voltage be
0.05V;Remainder is that the loss of voltage caused by declining because of membrane electrode activity is 0.03V.
There are many concrete application approach of the present invention, the above is only a preferred embodiment of the present invention.More than it should be pointed out that
Embodiment is merely to illustrate the present invention, and the protection scope being not intended to restrict the invention.For the common skill of the art
For art personnel, without departing from the principle of the present invention, several improvement can also be made, these improvement also should be regarded as this hair
Bright protection scope.
Claims (7)
1. a kind of non-precious metal catalyst membrane electrode durability test method, which is characterized in that the durability test method packet
Include following steps:
A, the initial polarization curve of test membrane electrode, measures initial activity current density;
B, the impedance of membrane electrode initial ohmic and cathode catalysis layer proton impedance are tested;
C, constant voltage discharge attenuation test is carried out to membrane electrode;
D, the polarization curve after the decaying of test membrane electrode, measures activated currents density after decaying, obtains activity after membrane electrode decaying
Reduced test result;
E, ohmage and cathode catalysis layer proton impedance after the decaying of test membrane electrode, impedance is raised after obtaining membrane electrode decaying
Test result;
F, drying nitrogen is passed through to membrane electrode to be purged, tests the purged polarization curve of membrane electrode nitrogen, obtain membrane electrode
Water logging influences the test result of membrane electrode performance after decaying.
2. non-precious metal catalyst durability test method according to claim 1, which is characterized in that in the membrane electrode
Cathod catalyst be the non-precious metal catalyst with M/N/C structure, wherein metal M is iron, any one or its in cobalt
Combination.
3. non-precious metal catalyst durability test method according to claim 1, which is characterized in that the polarization curve
Test method be constant voltage discharge method, activated currents density be membrane electrode discharge current density of the voltage at 0.7~0.8V.
4. non-precious metal catalyst durability test method according to claim 3, which is characterized in that the constant voltage discharge
Method specifically uses: anode is passed through hydrogen, and cathode is passed through pure oxygen, and relative humidity used is 80~100%, and back pressure used is 50kPa
~150kPa, temperature used are 60 DEG C~80 DEG C;Voltage range is 0.2~0.95V, stablizes 60~300s every 0.05V, is tested
With record discharge current.
5. non-precious metal catalyst membrane electrode durability test method according to claim 1, which is characterized in that the Europe
The test method of nurse impedance and cathode catalysis layer proton impedance is AC impedence method.
6. non-precious metal catalyst membrane electrode durability test method according to claim 5, which is characterized in that the friendship
Flow impedance method specifically uses: anode is passed through hydrogen, and cathode is passed through nitrogen, and relative humidity used is 80~100%, and back pressure used is
50kPa~150kPa, temperature used are 60 DEG C~80 DEG C;0.1~100000Hz of frequency range used, applied voltage range 0.2
~0.4V, applied voltage perturbation amplitude are 5%~10%;The intercept of surveyed ac impedance spectroscopy real axis is ohmage, high frequency region
45 ° of line segments are projected as the equivalent proton conduction resistance of cathode catalysis layer real axis.
7. according to non-precious metal catalyst membrane electrode durability test method described in right 1, which is characterized in that the constant voltage discharge
Attenuation test specifically uses: for discharge voltage for 0.4~0.6V, discharge time is 20~300h.
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