CN110320252A - A kind of oxygen transfer Resistance test methods of orderly electrode - Google Patents
A kind of oxygen transfer Resistance test methods of orderly electrode Download PDFInfo
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- CN110320252A CN110320252A CN201910346110.6A CN201910346110A CN110320252A CN 110320252 A CN110320252 A CN 110320252A CN 201910346110 A CN201910346110 A CN 201910346110A CN 110320252 A CN110320252 A CN 110320252A
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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
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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
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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 present invention relates to a kind of oxygen transfer Resistance test methods of orderly electrode.This method passes through magnetron sputtering first and prepares orderly electrode, after being prepared into membrane electrode, by its limiting current density under different oxygen concentrations of optimal inspection condition test, calculates oxygen mass transfer resistance according to the limiting current density measured.The method successfully measures the low orderly electrode of platinum and is prepared into its internal oxygen resistance to mass tranfer after MEA, is of great significance for studying the low orderly electrode oxygen transmission of platinum.It is particularly suitable for the test of the orderly electrode oxygen mass transfer resistance of the low platinum in Proton Exchange Membrane Fuel Cells field.
Description
Technical field
The present invention relates to field of fuel cell technology, and in particular to a kind of oxygen transfer Resistance test methods of orderly electrode.
Background technique
For Proton Exchange Membrane Fuel Cells (PEMFC) because of its low operation temperature, power density is high, and starting is fast, changes to load
Response is fast, is concerned in recent years.However, there is also some technologies for restricting its development and economy sides at present for this technology
The problem in face, such as largely caused using noble metal catalyst, cost is excessively high, service life falls short of.Currently, there is lot of documents
The research of electrode orderly for low platinum is reported, main purpose is to reduce the cost of Proton Exchange Membrane Fuel Cells, however low
The orderly electrode of platinum is extremely difficult to preferable performance under hydrogen empty condition, this is related with its local oxygen outflow, and oxygen really reaches platinum
There are resistances on surface, and this resistance shows especially prominent under low platinum, this becomes the difficult point of the orderly electrode research of low platinum
One of.The research of electrode oxygen transmission orderly for low platinum at present carries out qualitative analysis merely by test polarization curve, and
It can be to the orderly electrode interior oxygen transfer of low platinum if it can test out it in the oxygen mass transfer resistance under otherwise limit current density
Resistance carries out quantitative analysis.The research of this electrode interior oxygen transmission orderly for low platinum is of great significance.
Summary of the invention
The purpose of the present invention is to provide a kind of oxygen transfer Resistance test methods of orderly electrode, this method passes through magnetic first
Control sputtering prepares orderly electrode, after being prepared into MEA, passes through its limit electricity under different oxygen concentrations of optimal inspection condition test
Current density calculates oxygen mass transfer resistance according to the carrying current that measures, and the method successfully measures the low orderly electrode of platinum inside it
Oxygen mass transfer resistance.
In order to solve the above technical problems, The technical solution adopted by the invention is as follows:
A kind of oxygen transfer Resistance test methods of orderly electrode are provided, comprising the following steps:
(a) Pt is directly sputtered on GDL (gas diffusion layers) using magnetron sputtering technique and prepares orderly electrode as cathode
Then membrane electrode (MEA) is prepared；
(b) membrane electrode (MEA) is placed in monocell fixture, and loads onto fuel battery test platform and is tested；
(c) battery operating temperature, operating back pressure, anode and cathode throughput, anode and cathode humidification degree are set；
(d) anode is passed through hydrogen, and cathode is passed through nitrogen oxygen atmosphere, and the oxygen concentration that cathode gas is arranged is 6%~7%,
Electric current is slowly increased since 0, until voltage appearance sharply decline, record current density i.e. limiting current density at this time；
(e) oxygen concentration is gradually increased, and repeats the operation of step (d), obtains the carrying current under different oxygen concentrations
Density value；
(f) oxygen mass transfer resistance is calculated based on the above-mentioned limiting current density value measured.
Further, in step (a), the orderly electrode of magnetron sputtering preparation is the orderly electrode of low platinum, and Pt carrying capacity is
0.02~0.1mg/cm2。
Further, it is 2*1cm that monocell fixture, which selects runner effective dimensions, in step (b)2Straight flow field；Monocell
Assemble compressible rate be 15%~25%.
Further, in step (c) test condition be 60~80 DEG C of battery operating temperature, anode and cathode throughput be 1.5~
2.0L/min, gas backpressure are 50~200KPa.
Further, anode and cathode humidification degree is set as 50%~60% in step (c).
Further, in step (e), oxygen concentration range is 6%~49%.Oxygen concentration is low, and battery performance is low, the limit
Current density is difficult to observe.Oxygen concentration is high, and voltage is difficult to stablize under high current density, and test is difficult.Therefore it finally determines
Oxygen concentration range is 6%~49%.
Further, in step (e), gradually increasing oxygen concentration is 8,12,16,21,25,30,35,40,45,49%.
Further, start from scratch under given oxygen concentration and be slowly increased electric current, voltage is begun to decline, when under voltage
When dropping to 0.1~0.2V, voltage is difficult to stablize and sharply drop to zero at this time, and the current density recorded at this time is carrying current
Density.
Further, in step (e), after testing the limiting current density of an oxygen concentration, lead to the nitrogen of a period of time
Gas drops to 0.1V to voltage the moisture in battery is discharged, and then changes oxygen concentration and tests next limiting current density.
Further, oxygen mass transfer resistance R is calculated using following formulatot(s/m):
Wherein P in above-mentioned formulaabsIt is gas absolute pressure (Pa)；It is the saturated vapour pressure (Jmol of water-1K-1)；It is the total gas percentage of oxygen Zhan；R is gas constant (Jmol-1K-1)；F is Faraday constant (Cmol-1), T is electricity
The temperature (K) in pond, IlimIt is limiting current density value (Am-2)。
Beneficial effects of the present invention:
The exploitation of the low orderly electrode of platinum has important meaning for reducing fuel cell cost, the commercialization of propellant battery
Justice, however one of the Research Challenges of the orderly electrode of low platinum are that the surface of oxygen arrival catalyst Pt participates in reacting there are resistance,
Oxygen is difficult to observe in the transmission and reaction of the orderly electrode interior of low platinum.The research of electrode oxygen transmission orderly for low platinum at present
Qualitative analysis is carried out merely by test polarization curve, and if its oxygen under otherwise limit current density can be tested out
Resistance to mass tranfer then can carry out quantitative analysis to the orderly electrode interior oxygen transfer resistance of low platinum.The present invention tests the low orderly electrode of platinum,
By limiting current density of the control cathode side oxygen concentration range at 6%~49%, and pass through the tune of anode and cathode humidification degree
Control etc. (when humidification degree be greater than 70% when carrying current be difficult to observe, if humidification spend it is low, will affect proton exchange membrane moisten
Property, therefore final determining anode and cathode humidification degree is 50%~60%).This method can successfully observe the limit of the low orderly electrode of platinum
Current density, so that obtain it corresponds to internal oxygen resistance to mass tranfer under otherwise limit current density.It is orderly for studying low platinum
Electrode interior oxygen transmission has guiding significance.
Detailed description of the invention
Fig. 1 is the SEM figure of the orderly electrode of the present invention, as we can see from the figure the striped of orderly texture structure, after sputtering
The test of Pt carrying capacity is 0.04mg/cm2This electrode is the orderly electrode of low platinum；
Fig. 2,3 be respectively the polarization curve of the embodiment of the present invention 1,2, and the concentration polarization later period goes out as we can see from the figure
Existing limiting current density under higher current density, is extremely difficult to stablize, polarization is bent at this time when polarization curve voltage is in 0.2V
Vertically downward, therefore corresponding current density is limiting current density to line under 0.2V.It has successfully been measured under such test condition
Limiting current density of the sequence electrode under different back pressures；
Fig. 4,5 be the limiting current density of the embodiment of the present invention 1,2 with oxygen concentration variation relation, it can be seen that limit electricity
Current density is in a linear relationship with oxygen concentration, this meets the basic law of fuel battery inside reaction, therefore, it is considered that test result
It is correct.
Fig. 6,7 be according to the counted oxygen transfer resistance of step (c) in embodiment 1,2 with current density change curve, orderly
The oxygen transfer resistance of electrode is successfully measured.According to test result it can be seen that oxygen mass transfer resistance with limiting current density variation
Rule, and the oxygen mass transfer resistance under otherwise limit current density can be quantified.By curvilinear motion law discovery with carrying current
The increase of density, the presentation of oxygen mass transfer resistance first increase the trend fluctuated afterwards.This electrode oxygen transmission orderly for low platinum is ground
Study carefully with directive significance.
Specific embodiment
To make those of ordinary skill in the art fully understand technical solution of the present invention and beneficial effect, below in conjunction with specific
Embodiment is further described.
Embodiment 1
Orderly electrode preparation: 0.04mg/cm is sputtered on GDL using magnetron sputtering technique2Pt, prepare orderly electrode,
And MEA is made as cathode electrode；Fig. 1 is the SEM figure of the orderly electrode of the present invention, as we can see from the figure orderly texture
The striped of structure, Pt carrying capacity is 0.04mg/cm after tested2, it is the orderly electrode of low platinum；
Limiting current density test: the assemble compressible rate of monocell is 20%, and 80 DEG C of battery operating temperature, throughput is sun
Pole 1.6L/min, cathode 2.0L/min, anode and cathode humidification degree 50%, back pressure 100KPa, adjustment cathode side oxygen concentration are 6%,
Mixed gas is oxygen and nitrogen, starts test limits current density, is slowly increased electric current, and voltage is begun to decline, when voltage drop as low as
When 0.2V, voltage is difficult to stablize at this time, and drops to zero, and the current density recorded at this time is limiting current density.Stop surveying
Examination.After being passed through the purging that nitrogen carries out a period of time, continues to increase cathode oxygen to 8%, continue according to said method test pole
Current density of rationing the power supply to oxygen concentration be 49%.
Oxygen transfer drag evaluation: limiting current density is brought into and calculates oxygen mass transfer resistance Rtot(s/m) formula
Wherein, P in formulaabsIt is gas absolute pressure (Pa)；It is the saturated vapour pressure (Pa) of water；It is oxygen
The total gas percentage of Zhan；R is gas constant (Jmol-1K-1)；F is Faraday constant (Cmol-1), T is the temperature of battery
(K), IlimLimiting current density value (Am-2)。
Fig. 2 and Fig. 4 be respectively in embodiment 1 under 100KPa back pressure the polarization curve of test limits current density and pole
Current density of rationing the power supply is with the total gas percentage change curve of oxygen Zhan.
Embodiment 2
Orderly electrode preparation: 0.04mg/cm is sputtered on GDL using magnetron sputtering technique2Pt, and as cathode
Electrode fabrication MEA
Carrying current test: the assemble compressible rate of monocell is 15%, and 80 DEG C of battery operating temperature, throughput is anode
1.6L/min, cathode 2.0L/min, anode and cathode humidification degree 60%, back pressure are that 150KPa. adjustment cathode side oxygen concentration is 6%, are mixed
Gas be oxygen and nitrogen, start test limits current density, be slowly increased electric current, voltage is begun to decline, when voltage drop as low as
When 0.2V, voltage is difficult to stablize at this time, and drops to zero, and the current density recorded at this time is limiting current density.Stop surveying
Examination after being passed through the purging that nitrogen carries out a period of time, continues to increase cathode oxygen to 8%, continues according to said method test pole
Current density of rationing the power supply to oxygen concentration be 49%.
Oxygen transfer drag evaluation: limiting current density is brought into and calculates oxygen mass transfer resistance Rtot(s/m) formula
Wherein, P in formulaabsIt is gas absolute pressure (Pa)；It is the saturated vapour pressure (Pa) of water；It is oxygen
The total gas percentage of Zhan；R is gas constant (Jmol-1K-1)；F is Faraday constant (Cmol-1), T is the temperature of battery
(K), IlimLimiting current density value (Am-2)。
Fig. 3 and Fig. 5 be respectively in embodiment 2 under 150KPa back pressure the polarization curve of test limits current density and pole
Current density of rationing the power supply is with the total gas percentage change curve of oxygen Zhan.
Fig. 6,7 be respectively to be become according to the counted oxygen transfer resistance of step (c) with current density in embodiment 1 and embodiment 2
Change curve, the oxygen transfer resistance of orderly electrode is successfully measured.According to test result it can be seen that oxygen mass transfer resistance is with limit electricity
The changing rule of current density, and the oxygen mass transfer resistance under otherwise limit current density can be quantified.It is sent out by curvilinear motion rule
Now with the increase of limiting current density, oxygen mass transfer resistance is not steady constant, the presentation increase under lower current densities
Trend, be fluctuation under higher current density.The research of this electrode oxygen transmission orderly for low platinum has directive significance.
Claims (10)
1. a kind of oxygen transfer Resistance test methods of orderly electrode, it is characterised in that: the following steps are included:
(a) using magnetron sputtering technique, directly sputtering Pt prepares orderly electrode as cathode and then prepares film on the gas diffusion
Electrode；
(b) membrane electrode is placed in monocell fixture, and loads onto fuel battery test platform and is tested；
(c) battery operating temperature, operating back pressure, anode and cathode throughput, anode and cathode humidification degree are set；
(d) anode is passed through hydrogen, and cathode is passed through nitrogen oxygen atmosphere, and the oxygen concentration that cathode gas is arranged is 6%, and electric current is opened from 0
Beginning is slowly increased, until voltage appearance sharply decline, record current density i.e. limiting current density at this time；
(e) oxygen concentration is gradually increased, and repeats the operation of step (d), obtains the limiting current density under different oxygen concentrations
Value；
(f) oxygen mass transfer resistance is calculated based on the above-mentioned limiting current density value measured.
2. the oxygen transfer Resistance test methods of orderly electrode according to claim 1, it is characterised in that: in step (a), magnetic
The orderly electrode of control sputtering preparation is the orderly electrode of low platinum, and Pt carrying capacity is 0.02~0.1mg/cm2。
3. the oxygen transfer Resistance test methods of orderly electrode according to claim 1, it is characterised in that: single in step (b)
It is 2*1cm that battery clamp, which selects runner effective dimensions,2Straight flow field；The assemble compressible rate of monocell is 15%~25%.
4. the oxygen transfer Resistance test methods of orderly electrode according to claim 1, it is characterised in that: surveyed in step (c)
Strip part be 60~80 DEG C of battery operating temperature, anode and cathode throughput be 1.5~2.0L/min, gas backpressure be 50~
200KPa。
5. the oxygen transfer Resistance test methods of orderly electrode according to claim 1, it is characterised in that: negative in step (c)
Anode humidification degree is set as 50%~60%.
6. the oxygen transfer Resistance test methods of orderly electrode according to claim 1, it is characterised in that: in step (e), oxygen
Gas concentration range is 6%~49%.
7. the oxygen transfer Resistance test methods of orderly electrode according to claim 1, it is characterised in that: in step (e), by
Cumulative oxygenation gas concentration is 8,12,16,21,25,30,35,40,45,49%.
8. the oxygen transfer Resistance test methods of orderly electrode according to claim 1, it is characterised in that: in step (d):
To start from scratch under given oxygen concentration and is slowly increased electric current, voltage is begun to decline, when voltage drops to 0.1~0.2V, this
When voltage be difficult to stablize and sharply drop to zero, the current density recorded at this time is limiting current density.
9. the oxygen transfer Resistance test methods of orderly electrode according to claim 1, it is characterised in that: in step (e), survey
After the carrying current for having tried an oxygen concentration, the nitrogen of logical a period of time drops to 0.1V to voltage the water in battery is discharged
Point, then change oxygen concentration and tests next limiting current density.
10. the oxygen transfer Resistance test methods of orderly electrode according to claim 1, it is characterised in that: step (f) utilizes
Following formula calculate oxygen mass transfer resistance Rtot(s/m):
Wherein P in above-mentioned formulaabsIt is gas absolute pressure (Pa)；It is the saturated vapour pressure (Pa) of water；It is that oxygen accounts for
Total gas percentage；R is gas constant (Jmol-1K-1)；F is Faraday constant (Cmol-1), T is the temperature (K) of battery,
IlimIt is limiting current density value (Am-2)。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111413255A (en) * | 2020-03-31 | 2020-07-14 | 浙江大学 | Micro-electrode system and method for testing oxygen mass transfer coefficient of proton exchange membrane |
| CN112945719A (en) * | 2019-12-11 | 2021-06-11 | 中国科学院大连化学物理研究所 | Fuel cell membrane electrode testing device and method for testing membrane electrode performance |
| CN114112835A (en) * | 2021-11-04 | 2022-03-01 | 武汉理工大学 | Method for on-line testing oxygen permeation condition of proton exchange membrane through embedded microelectrode |
| CN114264709A (en) * | 2021-11-09 | 2022-04-01 | 深圳航天科技创新研究院 | Method for measuring mass transfer resistance of gas diffusion layer of hydrogen fuel cell and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112945719A (en) * | 2019-12-11 | 2021-06-11 | 中国科学院大连化学物理研究所 | Fuel cell membrane electrode testing device and method for testing membrane electrode performance |
| CN112945719B (en) * | 2019-12-11 | 2022-10-11 | 中国科学院大连化学物理研究所 | Fuel cell membrane electrode testing device and method for testing membrane electrode performance |
| CN111413255A (en) * | 2020-03-31 | 2020-07-14 | 浙江大学 | Micro-electrode system and method for testing oxygen mass transfer coefficient of proton exchange membrane |
| CN111413255B (en) * | 2020-03-31 | 2020-12-18 | 浙江大学 | Micro-electrode system and method for testing oxygen mass transfer coefficient of proton exchange membrane |
| CN114112835A (en) * | 2021-11-04 | 2022-03-01 | 武汉理工大学 | Method for on-line testing oxygen permeation condition of proton exchange membrane through embedded microelectrode |
| CN114112835B (en) * | 2021-11-04 | 2024-01-30 | 武汉理工大学 | Method for online testing oxygen permeation condition of proton exchange membrane through embedded microelectrode |
| CN114264709A (en) * | 2021-11-09 | 2022-04-01 | 深圳航天科技创新研究院 | Method for measuring mass transfer resistance of gas diffusion layer of hydrogen fuel cell and application thereof |
| CN114264709B (en) * | 2021-11-09 | 2023-12-19 | 深圳航天科技创新研究院 | Method for measuring mass transfer resistance of gas diffusion layer of hydrogen fuel cell and application thereof |
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