CN110880612A - Low-temperature storage strategy of high-temperature proton exchange membrane fuel cell - Google Patents
Low-temperature storage strategy of high-temperature proton exchange membrane fuel cell Download PDFInfo
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- CN110880612A CN110880612A CN201811036766.XA CN201811036766A CN110880612A CN 110880612 A CN110880612 A CN 110880612A CN 201811036766 A CN201811036766 A CN 201811036766A CN 110880612 A CN110880612 A CN 110880612A
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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
- H01M8/043—Processes for controlling fuel cells or fuel cell systems applied during specific periods
- H01M8/04303—Processes for controlling fuel cells or fuel cell systems applied during specific periods applied during shut-down
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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
- H01M8/04223—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids during start-up or shut-down; Depolarisation or activation, e.g. purging; Means for short-circuiting defective fuel cells
- H01M8/04228—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids during start-up or shut-down; Depolarisation or activation, e.g. purging; Means for short-circuiting defective fuel cells during shut-down
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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
- H01M8/10—Fuel cells with solid electrolytes
- H01M2008/1095—Fuel cells with polymeric electrolytes
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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
Aiming at the problem of low-temperature storage of the high-temperature proton exchange membrane fuel cell, the invention regulates and controls the concentration of phosphoric acid electrolyte in a membrane electrode of the fuel cell after shutdown by regulating the loading current, the feeding amount and the shutdown temperature in the shutdown process of the high-temperature proton exchange membrane fuel cell, and indirectly judges the change trend of the concentration of phosphoric acid in the membrane electrode by testing the internal resistance of the fuel cell through an electrochemical impedance method, thereby avoiding the solidification of the electrolyte in the membrane electrode during low-temperature storage, reducing the damage of the phase state and volume change of the electrolyte to the membrane electrode during low-temperature storage and further slowing down the performance attenuation of the fuel cell after low-temperature storage.
Description
Technical Field
The invention relates to the technical field of fuel cells, in particular to a low-temperature storage strategy of a high-temperature proton exchange membrane fuel cell.
Background
Compared with a low-temperature proton exchange membrane fuel cell (PEMFC, about 80 ℃), a high-temperature proton exchange membrane fuel cell (HT-PEMFC, 150-200 ℃) has the advantages of accelerated electrode reaction rate, higher tolerance to impurities, simpler hydrothermal management and the like, so the high-temperature proton exchange membrane fuel cell is widely concerned. The proton exchange membrane fuel cell has the outstanding advantages of high energy conversion efficiency, environmental friendliness and the like, and has the characteristics of high specific power energy and the like, thereby being a very promising power source.
The application of fuel cells in power sources inevitably faces difficulties in storage under low temperature conditions. For a high-temperature proton exchange membrane fuel cell with the working temperature of 150-200 ℃, the high-temperature proton exchange membrane fuel cell is usually based on a phosphoric acid-doped high-temperature electrolyte membrane, and the proton conducting substance in the electrolyte membrane and the membrane electrode is phosphoric acid. FIG. 1 is a phase diagram of a phosphoric acid solution, which causes partial phosphoric acid solidification when the concentration of phosphoric acid is too low or too high in an environment below 0 ℃; after the concentration of the phosphoric acid is higher than 62.5%, the freezing point is increased along with the increase of the concentration of the phosphoric acid. After the phosphoric acid solution is solidified, the volume is reduced due to the reduction of intermolecular gaps, when the battery is started again, the density of the phosphoric acid solution is reduced along with the increase of temperature, the volume is changed along with the change of the density, and repeated phase change can greatly influence the electrolyte membrane material and the membrane electrode structure, so that the performance and the service life of the battery are influenced. U.S. patent No. WO 2016/168112a1 reports that the freezing point of a phosphoric acid solution is lowered by adding a small amount of another substance to the phosphoric acid solution, thereby preventing the phosphoric acid solution from solidifying. For fuel cell applications, however, the introduction of other substances can cause other problems, such as contamination of the membrane electrode, poisoning of the electrocatalyst, etc.
Aiming at the problems, the invention provides a method for adjusting the internal resistance of a single cell before the cell is shut down by utilizing the optimization of a shutdown strategy of a high-temperature proton exchange membrane fuel cell, so that the concentration of phosphoric acid in a membrane electrode after shutdown is controlled, the phosphoric acid solidification during low-temperature storage is further avoided, and the problem of difficult low-temperature storage can be effectively solved.
Disclosure of Invention
The method comprises the steps of adjusting the operation conditions (including loading current during shutdown, feeding amount control, temperature before shutdown of the fuel cell and the like) of the high-temperature proton exchange membrane fuel cell during shutdown, and then testing the internal resistance of the cell by an electrochemical impedance method to detect the concentration change trend of the phosphoric acid electrolyte in the membrane electrode, so as to regulate and control the concentration of the phosphoric acid electrolyte in the membrane electrode of the fuel cell after shutdown, further avoid the solidification of the electrolyte in the membrane electrode during low-temperature storage, reduce the damage of the phase state and volume change of the electrolyte to the membrane electrode during low-temperature storage, and further slow down the performance attenuation of the fuel cell after low-temperature storage.
A low-temperature storage strategy of a high-temperature proton exchange membrane fuel cell is provided, wherein an electrolyte membrane of the high-temperature proton exchange membrane fuel cell is a high-temperature electrolyte membrane doped based on phosphoric acid, and the shutdown process of the high-temperature proton exchange membrane fuel cell is controlled by adopting one or more than two control methods including loading current control before shutdown, feeding control before shutdown and temperature control before shutdown; the internal resistance of a single battery is controlled to be 160-250 m omega cm2。
The internal resistance test of the fuel cell is to indirectly know the concentration of phosphoric acid electrolyte in a membrane electrode after the fuel cell is shut down, and the internal resistance of the fuel cell is tested by adopting an alternating current impedance method. For the high-temperature proton exchange membrane fuel cell based on the phosphoric acid doped high-temperature electrolyte membrane, the internal resistance of the fuel cell is mainly controlled by the internal resistance of the electrolyte membrane, the internal resistance of the electrolyte membrane is influenced by the conductivity of the membrane, the conductivity of the electrolyte membrane is influenced by the concentration of the doped acid in the membrane, and the specific conductivity of phosphoric acid solutions with different concentrations at different temperatures is different, so that the internal resistance of the fuel cell can indirectly reflect the concentration of the phosphoric acid in the membrane electrode. For the battery to be stored at 0-40 ℃, the internal resistance of a single battery is recommended to be 160-250 m omega cm when the fuel battery is shut down2。
The loading current control in the shutdown process is as follows: setting the loading current before shutdown under the condition of ensuring that the discharge voltage of a single battery is not lower than 0.3V, and controlling the output current of the fuel cell to be 50mA/cm by adjusting the resistance value of a load when the fuel cell discharges2～300mA/cm2(ii) a The discharge voltage of the fuel cell is reduced along with the increase of the discharge current, the temperature of the fuel cell is reduced before shutdown, the loading current needs to be reduced, and if the loading current is too large, the discharge voltage of the fuel cell is too small, so that the stability is not facilitated; in addition, the current loading before shutdown also affects the water produced by the cathode, and simultaneously affects the water quantity reversely diffused from the cathode to the anode, so as to affect the concentration of phosphoric acid in the membrane electrode after shutdown. Aiming at different high-temperature proton exchange membrane fuel cells based on phosphoric acid doped high-temperature electrolyte membranes, the high-temperature electrolyte membrane material and the membrane are usedThe discharging performance of the electrode structure is different, and the loading current before shutdown is 50mA/cm under the condition of ensuring that the discharging voltage of a single battery is not lower than 0.3V2～300mA/cm2It is more suitable.
The feeding control in the shutdown process is as follows: controlling the stoichiometric ratio of the anode feeding amount to the theoretical feeding amount to be 1.2-3.0, and controlling the stoichiometric ratio of the cathode feeding amount to the theoretical feeding amount to be 1.5-2.5; when the anode and the cathode are fed with different stoichiometric ratios, the back diffusion of water generated by the cathode to the anode is different, thereby influencing the concentration of phosphoric acid in the membrane electrode after shutdown. The stoichiometric ratio of anode feeding is 1.2-3.0, the stoichiometric ratio of cathode feeding is 1.5-2.5, and the influence on the concentration of phosphoric acid in the electrode is minimum.
The temperature control before shutdown is as follows: and when the temperature of the battery is reduced to 120-100 ℃, disconnecting the load, closing the cathode and anode feeding, and sealing the inlet and the outlet of the cathode and the anode to complete shutdown. The working temperature of the proton exchange membrane fuel cell is 150-200 ℃, if the temperature before shutdown is too high, the fuel cell is easy to damage electrode parts under high temperature and high potential, and phosphoric acid electrolyte polycondensation can be caused under high temperature; if the temperature before shutdown is lower than 100 ℃, water generated by the electrochemical reaction of the cathode is in a liquid state, and the liquid water brings away part of the phosphoric acid electrolyte, so that the phosphoric acid electrolyte in the membrane electrode is reduced, and the internal resistance of the membrane electrode is increased to reduce the performance of the membrane electrode; therefore, after the temperature is reduced to 120-100 ℃, the loading is closed, and the cathode and anode feeding is closed.
The low temperature of the low-temperature storage means 0 to-40 ℃.
For a high-temperature proton exchange membrane fuel cell with an external heating system, the external heating system needs to be closed before shutdown.
The phosphoric acid-doped high-temperature electrolyte membrane is any one of poly (2, 5-benzimidazole) (AB-PBI), poly (2,2 '-m-tolyl-5, 5' -dibenzoimidazole) (PBI), poly (4,4 '-diphenyl ether group-5, 5' -dibenzoimidazole) (OPBI), sulfonated PBI, PBI/Polyimide (PI), polyether ether ketone (PEEK), sulfonated polyether ether ketone (SPEEK), PBI/ABPBI, PBI/PEEK, PBI/SPEEK and alkyl polybenzimidazole (PPS).
Compared with the prior art, the invention is simple, convenient and economic, and only needs to be controlled by operation in the shutdown process without introducing other additives, thereby not causing pollution and poisoning influence on the battery.
Drawings
FIG. 1 is a phase diagram of phosphoric acid solution.
Figure 2 is a graph of fuel cell refrigeration cycle performance results using the strategy of example 1.
Figure 3 is a graph of fuel cell freeze cycle performance results using the strategy of example 2.
Figure 4 is a graph of fuel cell freeze cycle performance results using the strategy of example 3.
Fig. 5 is a graph of the performance of the battery after-40 c freeze cycle after this shut down procedure.
Detailed Description
The cryogenic storage strategy proposed by the present invention comprises: the method comprises the steps of controlling the loading current in the shutdown process and the feeding quantity in the shutdown process, and testing the temperature of the fuel cell before shutdown and the internal resistance of the fuel cell.
Example 1
Experiments were performed with high temperature proton exchange membrane fuel cells based on phosphoric acid doped poly (4,4 '-diphenyl ether-5, 5' -bisbenzimidazole) high temperature electrolyte membranes.
When the fuel cell is ready to be shut down, the discharge current is adjusted to 100mA/cm2The anode feeding stoichiometric ratio is set to be 1.2, the cathode feeding stoichiometric ratio is set to be 2.5, and after the temperature of the fuel cell is reduced by 100 ℃, the loading is closed, and the cathode feeding and the anode feeding are closed. Testing the internal resistance of the fuel cell membrane electrode after shutdown by using an alternating current impedance method, and measuring the internal resistance to be 240m omega cm2。
In order to investigate the performance change condition of the fuel cell after the shutdown strategy is stored for 24 hours at the temperature of minus 40 ℃, the fuel cell after shutdown is put into a thermostat at the temperature of minus 40 ℃ for 24 hours, the fuel cell is taken out and then heated again to test the performance of the fuel cell, then the fuel cell is shut down again according to the shutdown strategy, then the fuel cell is frozen at the temperature of minus 40 ℃, then the performance is tested again, and thus the fuel cell is continuously shut down, frozen and tested, and the discharge performance of the fuel cell after each freezing is recorded. Figure 2 is a graph of the performance of a high temperature pem fuel cell based on a phosphoric acid doped poly (4,4 '-diphenyl ether-5, 5' -dibenzoimidazole) high temperature electrolyte membrane after a-40 c freeze cycle following the shut-down strategy of example 1.
Example 2
Experiments were performed using high temperature proton exchange membrane fuel cells based on phosphoric acid doped poly (2, 5-benzimidazole) high temperature electrolyte membranes.
When the fuel cell is ready to be shut down, the discharge current is adjusted to 150mA/cm2And the anode feeding stoichiometric ratio is set to be 2, the cathode feeding stoichiometric ratio is set to be 2, and after the temperature of the fuel cell is reduced to 110 ℃, the loading is closed, and the cathode feeding and the anode feeding are closed. Testing the internal resistance of the membrane electrode of the fuel cell by using an alternating current impedance method, wherein the internal resistance is 200m omega cm2。
In order to verify the performance change condition of the fuel cell after shutdown by the shutdown strategy after 24 hours of storage at-40 ℃, the shutdown-freezing-performance test was performed by the same test method as in example 1, and the discharge performance of the fuel cell after each freezing was recorded. Figure 3 is a graph of the performance of a polybenzimidazole membrane based high temperature pem fuel cell after-40 c freeze cycle after the shutdown strategy of example 2.
Example 3
Experiments were performed using high temperature proton exchange membrane fuel cells based on phosphoric acid doped poly (2,2 '-m-tolyl-5, 5' -dibenzoimidazole) high temperature electrolyte membranes.
When the fuel cell is ready to be shut down, the discharge current is adjusted to 200mA/cm2The anode feeding stoichiometric ratio is set to be 2.5, the cathode feeding stoichiometric ratio is set to be 1.2, and after the temperature of the fuel cell is reduced to 120 ℃, the loading is closed, and the cathode feeding and the anode feeding are closed. Testing the internal resistance of the membrane electrode of the fuel cell by using an alternating current impedance method, wherein the internal resistance is 170m omega cm2。
In order to verify the performance change condition of the fuel cell after shutdown by the shutdown strategy after 24 hours of storage at-40 ℃, the shutdown-freezing-performance test was performed by the same test method as in example 1, and the discharge performance of the fuel cell after each freezing was recorded. Figure 4 is a graph of the performance of a polybenzimidazole membrane based high temperature pem fuel cell after-40 c freeze cycle after the shutdown strategy of example 3. Comparative example
Experiments were performed using high temperature proton exchange membrane fuel cells based on phosphoric acid doped poly (2, 5-benzimidazole) high temperature electrolyte membranes.
When the fuel cell is ready to be shut down, the discharge current is adjusted to 20mA/cm2The anode feeding stoichiometric ratio is set to be 1.2, the cathode feeding stoichiometric ratio is set to be 1.2, and after the temperature of the fuel cell is reduced to 95 ℃, the loading is closed, and the cathode feeding and the anode feeding are closed. Testing the internal resistance of the membrane electrode of the fuel cell by using an alternating current impedance method, and measuring the internal resistance to be 362m omega cm2. After the cell was stored at-40 ℃ for 24 hours, the shutdown-freezing-performance test was performed by the same test method as in example 1, and the discharge performance of the fuel cell after each freezing was recorded. Fig. 5 shows the performance of the cell after the freezing cycle at-40 ℃ after the shutdown method is adopted, and it can be seen from fig. 5 that the open-circuit voltage decay is not severe, but the performance decay is severe, mainly because the shutdown method of the comparative example is easy to cause partial crystallization and loss of electrolyte phosphoric acid in the membrane electrode, thereby causing severe performance decay after low-temperature freezing.
Claims (7)
1. A low-temperature storage strategy of a high-temperature proton exchange membrane fuel cell is characterized in that: the electrolyte membrane of the high-temperature proton exchange membrane fuel cell is based on phosphoric acid doping, and the internal resistance of a single section of the high-temperature proton exchange membrane fuel cell is controlled at 160-250 m omega-cm by adopting one or more control methods of controlling the loading current, the feeding amount before shutdown and the temperature in the shutdown process of the high-temperature proton exchange membrane fuel cell2And then disconnecting the load, closing the cathode and anode feeding, and sealing the inlet and the outlet of the cathode and the anode to complete shutdown.
2. A low temperature storage strategy for a high temperature pem fuel cell according to claim 1 wherein: the loading current control in the shutdown process is as follows: setting the loading current before shutdown under the condition of ensuring that the discharge voltage of a single battery is not lower than 0.3V, and adjusting the resistance value of a load when the fuel cell dischargesControlling the output current of the fuel cell to be 50mA/cm2～300mA/cm2。
3. A low temperature storage strategy for a high temperature pem fuel cell according to claim 1 wherein: the feeding control in the shutdown process is as follows: and controlling the stoichiometric ratio of the anode feeding amount to the theoretical feeding amount to be 1.2-3.0, and controlling the stoichiometric ratio of the cathode feeding amount to the theoretical feeding amount to be 1.5-2.5.
4. A low temperature storage strategy for a high temperature pem fuel cell according to claim 1 wherein: and controlling the temperature before shutdown to be reduced to 120-100 ℃.
5. The cryogenic storage strategy of claim 1, wherein: the low temperature of the low-temperature storage means 0 to-40 ℃.
6. The cryogenic storage strategy of claim 4, wherein: for a high-temperature proton exchange membrane fuel cell with an external heating system, the external heating system needs to be closed before shutdown.
7. Cryogenic storage strategy according to any of claims 1 to 6, wherein: the phosphoric acid-doped high-temperature electrolyte membrane is any one of poly (2, 5-benzimidazole) (AB-PBI), poly (2,2 '-m-tolyl-5, 5' -dibenzoimidazole) (PBI), poly (4,4 '-diphenyl ether group-5, 5' -dibenzoimidazole) (OPBI), sulfonated PBI, PBI/Polyimide (PI), polyether ether ketone (PEEK), sulfonated polyether ether ketone (SPEEK), PBI/ABPBI, PBI/PEEK, PBI/SPEEK and alkyl polybenzimidazole (PPS).
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| US20090081487A1 (en) * | 2007-06-27 | 2009-03-26 | Christos Chochos | Acid-Doped Polyelectrolyte Modified Carbon Nanotubes and their Use in High Temperature PEM Fuel Cell Electrodes |
| CN103682403A (en) * | 2013-12-24 | 2014-03-26 | 武汉理工大学 | Fuel cell low-temperature quick-starting system and method adopting staged temperature control |
| CN105702979A (en) * | 2014-11-27 | 2016-06-22 | 中国科学院大连化学物理研究所 | Starting method for fuel cell stack in environment below zero |
| CN105742649A (en) * | 2014-12-11 | 2016-07-06 | 中国科学院大连化学物理研究所 | High-temperature proton exchange membrane fuel cell membrane electrode and preparation method thereof |
| CN105762398A (en) * | 2014-12-16 | 2016-07-13 | 中国科学院大连化学物理研究所 | Fuel cell combined power supply system and control method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090081487A1 (en) * | 2007-06-27 | 2009-03-26 | Christos Chochos | Acid-Doped Polyelectrolyte Modified Carbon Nanotubes and their Use in High Temperature PEM Fuel Cell Electrodes |
| CN103682403A (en) * | 2013-12-24 | 2014-03-26 | 武汉理工大学 | Fuel cell low-temperature quick-starting system and method adopting staged temperature control |
| CN105702979A (en) * | 2014-11-27 | 2016-06-22 | 中国科学院大连化学物理研究所 | Starting method for fuel cell stack in environment below zero |
| CN105742649A (en) * | 2014-12-11 | 2016-07-06 | 中国科学院大连化学物理研究所 | High-temperature proton exchange membrane fuel cell membrane electrode and preparation method thereof |
| CN105762398A (en) * | 2014-12-16 | 2016-07-13 | 中国科学院大连化学物理研究所 | Fuel cell combined power supply system and control method thereof |
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