CN115863699A - Activation method of fuel cell stack - Google Patents
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Abstract
The invention provides an activation method of a fuel cell stack, belonging to the technical field of fuel cells. The invention utilizes the membrane electrode preactivation and the electric pile wave trough type activation method to realize the rapid activation of the fuel cell electric pile, the preactivation aims to ensure that the whole membrane electrode is wetted, the membrane wrinkle caused by the overdrying of the membrane electrode during the pile loading is avoided, the cleaning of a proton exchange membrane, the removal of catalyst impurities and the reduction of oxides are realized, the maximum utilization rate of the catalyst is realized, the wave trough type current activation method activates the membrane electrode by alternately applying currents with different sizes, so that the catalyst activities of different gaps of the membrane electrode are all excited, the catalyst of different gaps is exposed, and the maximum utilization of the catalyst is realized.
Description
Technical Field
The invention relates to the technical field of fuel cells, in particular to an activation method of a fuel cell stack.
Background
The core component of the fuel cell stack is the Membrane Electrode Assembly (MEA), and the quality of the membrane electrode assembly determines the quality of the whole fuel cell stack. Although the performance of the membrane electrode depends on the performance of the catalyst, the diffusion layer and the proton exchange membrane, the MEA needs to be activated in order to achieve the best performance of the stack during operation, and the MEA needs to be activated before the MEA is stored for a period of time and operates again.
The mechanism of activation is rather complex and is generally considered to include the following processes: (1) humidifying the proton exchange membrane; (2) Establishing process of substance (electron, gas, water) transmission channel; (3) optimizing the electrode structure; and (4) improving the activity and the utilization rate of the catalyst layer. Currently, the activation method is rarely studied, and the common activation methods include steam activation, CO adsorption oxidation activation, and the like. The traditional activation mode takes a long time, usually one day or even several days, not only consumes a large amount of hydrogen, but also prolongs the production period of the galvanic pile.
Disclosure of Invention
In view of the above, the present invention provides a method for activating a fuel cell stack. The invention utilizes the membrane electrode preactivation and the electric pile wave trough activation method to realize the rapid activation of the fuel cell electric pile.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides an activation method of a fuel cell stack, which comprises the following steps:
preactivating the membrane electrode in preactivating solution to obtain an activated membrane electrode; the pre-activation liquid comprises the following components in volume fraction: 5-40% of hydrogen peroxide, 10-50% of dilute sulfuric acid and 20-60% of water, wherein the mass concentration of the hydrogen peroxide is 3-5%, and the mass concentration of the dilute sulfuric acid is 3-5%;
performing stacking in-situ activation on the activated membrane electrode, wherein the stacking in-situ activation comprises the following steps:
switching the cathode and the anode to humidifying nitrogen, and purging the galvanic pile;
switching the anode into humidified hydrogen and the cathode into humidified air, firstly increasing the current to 30A, staying for 30-50 s, then increasing the current to 570A, staying for 30-50 s, then decreasing the current to 60A, staying for 30-50 s, then increasing the current to 540A, staying for 30-50 s, and so on, and when the current reaches 300A, performing constant-current activation for 20-30 min, finally decreasing the current to 30A, staying for 20-30 s, and completing the activation of the first section of trough;
increasing the current to 570A, staying for 10-20 s, decreasing the current to 60A, staying for 10-20 s, increasing the current to 540A, staying for 10-20 s, decreasing the current to 90A, staying for 10-20 s, and so on, when the current reaches 300A, performing constant-current activation for 5-10 min, finally decreasing the current to 30A, staying for 10-20 s, and completing second-stage trough activation, wherein the first trough activation cycle comprises first-stage trough activation and second-stage trough activation;
and (5) circulating for activation of the valley 3-5 times.
Preferably, the pre-activation liquid comprises the following components in volume fraction: 30-35% of hydrogen peroxide, 20-25% of dilute sulfuric acid and 40-50% of water, wherein the mass fraction of the hydrogen peroxide is 3%, and the mass fraction of the dilute sulfuric acid is 5%.
Preferably, the time for purging is 30 to 40min.
Preferably, the purging process comprises: the temperature is increased from 30 ℃ to 78 ℃, and the temperature increasing rate of the temperature increase is 2 ℃/min.
Preferably, the anode is in a stoichiometric ratio of 1.6 to 2.5, and the cathode is in a stoichiometric ratio of 2.8 to 3.5.
Preferably, the humidity of the anode is 40-60%, and the humidity of the cathode is 60-80%.
Preferably, the back pressure of the anode is 13-110 kPa, and the back pressure of the cathode is 33-130 kPa.
Preferably, the lifting and lowering load speed of the current in the process of pile loading in-situ activation is independently 5-20A/s.
Preferably, the preactivation time is 0.5 to 1 hour.
Preferably, the number of the membrane electrodes in the stacking in-situ activation is 90-120, and the power is independently 30-50 kW.
The invention utilizes the membrane electrode preactivation and the electric pile wave trough type activation method to realize the rapid activation of the fuel cell electric pile, the preactivation aims to ensure that the whole membrane electrode is wetted, the membrane wrinkle caused by the overdrying of the membrane electrode during the pile loading is avoided, the cleaning of a proton exchange membrane, the removal of catalyst impurities and the reduction of oxides are realized, the maximum utilization rate of the catalyst is realized, the wave trough type current activation method activates the membrane electrode by alternately applying currents with different sizes, so that the catalyst activities of different gaps of the membrane electrode are all excited, the catalyst of different gaps is exposed, and the maximum utilization of the catalyst is realized.
Compared with the prior art, the invention has the following advantages:
(1) The activation time is greatly shortened, and compared with the activation time of a few days or even a few days, the activation time is shortened, the consumption of hydrogen is reduced, and the delivery quantity of the galvanic pile is increased;
(2) The pre-activated membrane electrode can improve the performance of the membrane electrode as a whole, improve the utilization rate of the catalyst, and adopt a trough type current activation method, the electric pile forms a stable electric transmission channel and a stable mass transmission channel by utilizing different currents, and after several trough type activations, the activation effect can ensure that the current density of 0.65V reaches 1.5A/cm 2 The above.
Drawings
FIG. 1 is a schematic diagram of the voltage variation of in-situ activation of a stack according to the present invention;
FIG. 2 is a polarization curve before and after activation in example 1;
FIG. 3 is a polarization curve before and after activation in example 2;
FIG. 4 is a polarization curve before and after activation of comparative example 1;
figure 5 is a graph of cell stack uniformity after activation for example 1 and comparative example 1.
Detailed Description
The invention provides an activation method of a fuel cell stack, which comprises the following steps:
preactivating the membrane electrode in preactivating solution to obtain an activated membrane electrode; the pre-activation liquid comprises the following components in volume fraction: 5-40% of hydrogen peroxide, 10-50% of dilute sulfuric acid and 20-60% of water, wherein the mass concentration of the hydrogen peroxide is 3-5%, and the mass concentration of the dilute sulfuric acid is 3-5%;
performing stacking in-situ activation on the activated membrane electrode, wherein the stacking in-situ activation comprises the following steps:
switching the cathode and the anode to humidifying nitrogen, and purging the galvanic pile;
switching the anode into humidified hydrogen and the cathode into humidified air, firstly increasing the current to 30A, staying for 30-50 s, then increasing the current to 570A, staying for 30-50 s, then decreasing the current to 60A, staying for 30-50 s, then increasing the current to 540A, staying for 30-50 s, and so on, and when the current reaches 300A, performing constant-current activation for 20-30 min, finally decreasing the current to 30A, staying for 20-30 s, and completing the activation of the first section of trough;
increasing the current to 570A, staying for 10-20 s, decreasing the current to 60A, staying for 10-20 s, increasing the current to 540A, staying for 10-20 s, decreasing the current to 90A, staying for 10-20 s, and so on, when the current reaches 300A, performing constant-current activation for 5-10 min, finally decreasing the current to 30A, staying for 10-20 s, and completing second-stage trough activation, wherein the first trough activation cycle comprises first-stage trough activation and second-stage trough activation;
and (5) circulating for activation of the valley 3-5 times.
The membrane electrode is preactivated in preactivating solution to obtain an activated membrane electrode; the pre-activation liquid comprises the following components in volume fraction: 5-40% of hydrogen peroxide, 10-50% of dilute sulfuric acid and 20-60% of water, wherein the mass concentration of the hydrogen peroxide is 3-5%, and the mass concentration of the dilute sulfuric acid is 3-5%.
In the present invention, the pre-activation liquid preferably comprises the following components in volume fraction: 30-35% of hydrogen peroxide, 20-25% of dilute sulfuric acid and 40-50% of water, wherein the mass concentration of the hydrogen peroxide is preferably 3%, and the mass concentration of the dilute sulfuric acid is preferably 5%.
The preparation method of the preactivating solution is not particularly limited in the present invention, and may be prepared by a method known to those skilled in the art, such as stirring.
In the present invention, the water is preferably deionized water.
In the present invention, the time for the pre-activation is preferably 0.5 to 1 hour.
In the invention, preferably, a flat clamp is used for clamping the frame of the membrane electrode, the frame is vertically inserted into the preactivation solution, and the membrane electrode is laid flat and fully soaked for preactivation.
In the present invention, the flat clip is preferably a rubber product.
After the pre-activation is completed, the invention preferably adopts dust-free paper or dust-free cloth to absorb the redundant pre-activation solution.
After the activated membrane electrode is obtained, the activated membrane electrode is subjected to stacking in-situ activation, and the stacking in-situ activation comprises the following steps:
switching the cathode and the anode to humidifying nitrogen, and purging the galvanic pile;
switching the anode into humidified hydrogen and the cathode into humidified air, firstly increasing the current to 30A, staying for 30-50 s, then increasing the current to 570A, staying for 30-50 s, then decreasing the current to 60A, staying for 30-50 s, then increasing the current to 540A, staying for 30-50 s, and so on, and when the current reaches 300A, performing constant-current activation for 20-30 min, finally decreasing the current to 30A, staying for 20-30 s, and completing the activation of the first section of trough;
increasing the current to 570A, staying for 10-20 s, decreasing the current to 60A, staying for 10-20 s, increasing the current to 540A, staying for 10-20 s, decreasing the current to 90A, staying for 10-20 s, and so on, when the current reaches 300A, performing constant-current activation for 5-10 min, finally decreasing the current to 30A, staying for 10-20 s, and completing second-stage trough activation, wherein the first trough activation cycle comprises first-stage trough activation and second-stage trough activation;
and (5) circulating for activation of the valley 3-5 times.
In the present invention, the time for purging is preferably 30 to 40min.
In the present invention, the purging preferably includes: and heating from 30 ℃ to 78 ℃, wherein the heating rate of the heating is 2 ℃/min, and the purging has the function of wetting the activated membrane electrode, establishing a transmission channel and enabling the galvanic pile structure to be more stable.
In the present invention, the anode is preferably 1.6 to 2.5 in terms of the stoichiometric ratio, and the cathode is preferably 2.8 to 3.5 in terms of the stoichiometric ratio.
In the present invention, the humidity of the anode is preferably 40% to 60%, and the humidity of the cathode is preferably 60% to 80%.
In the present invention, the back pressure of the anode is preferably 13 to 110kPa, and the back pressure of the cathode is preferably 33 to 130kPa.
In the present invention, the rate of current lift and drop during the in situ activation of the charge is independently preferably 5 to 20A/s.
In the invention, the number of the membrane electrodes in the stacking in-situ activation is preferably 90-120, and the power is independently preferably 30-50 kW.
In the invention, the lowest voltage setting in the pile loading in-situ activation is preferably more than or equal to 0.3V, and the system can automatically stop when the voltage is lower than 0.3V.
FIG. 1 is a schematic diagram of the voltage change of the in-situ activation of the stack according to the present invention.
In the present invention, the process of the first stage trough activation is shown in table 1.
TABLE 1 Process for first stage trough activation
In the present invention, the process of the second stage of trough activation is shown in Table 2.
TABLE 2 second stage trough activation Process
To further illustrate the present invention, the activation method of the fuel cell stack according to the present invention will be described in detail with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Configuration of35 parts by volume of 3% mass concentration H 2 O 2 25 parts of 5% by mass H 2 SO 4 40 parts of deionized water, stirring for 0.5h, and uniformly mixing. Clamping the membrane electrode by using a flat clamp, vertically placing the membrane electrode into the prepared solution, slowly placing the solution horizontally, standing for 0.5h, absorbing excessive moisture by using dust-free cloth, preparing 90 membrane electrodes according to the operation, stacking the membrane electrodes prepared by pretreatment, and preparing an activation test.
And starting a temperature control program and a cooling water program on the assembled galvanic pile, controlling the cathode back pressure to be 33kPa, and controlling the anode back pressure to be 13kPa. Anode metering 2.5, cathode metering 3.5, anode humidity was always controlled to 40% rh, cathode humidity was always controlled to 60% rh, manual temperature control, stack temperature start 30 ℃,2 ℃/min adjustment, gradual temperature rise to 78 ℃, steady purge 10min, nitrogen purge completed.
The anode is switched to be humidified hydrogen, the cathode is switched to be humidified air, the cathode metering ratio is gradually increased from 2.5 to 3.5, the anode metering ratio is gradually increased from 1.6 to 2.5, the anode back pressure is gradually increased from 13 to 100kPa, the cathode back pressure is gradually increased from 33 to 120kPa, the operation temperature is 75 ℃ at the anode, 75 ℃ at the cathode and 78 ℃ at the galvanic pile. The method comprises the steps of starting a load, increasing the current to 30A, operating for 30s, increasing the current to 570A, operating for 30s, decreasing the current to 60A, operating for 30s, increasing the current to 540A, operating for 30s.. The like (the current increasing rate is 15A/s), and repeating the steps until the current reaches 300A, operating for 20min at a constant current of 300A, decreasing the current to 30A, operating for 20s, and completing the activation of a first section of trough, wherein the parameters of the activation of the first section of trough are shown in Table 1.
After the activation of the first section of wave trough is finished, the current stays for 10s from 30A, then rises to 570A, runs for 10s, then falls to 60A, runs for 10s, then rises to 540A, runs for 10s, falls to 90A, runs for 10, and so on, when the current reaches 300A, constant current loading is carried out for 10min, then the current falls to 30A, runs for 20s, and second section of wave trough activation is finished, wherein the parameters of the second section of wave trough activation are shown in table 2, so that the first-time wave trough activation is finished in a summary manner, and three cycles are circulated, so that the activation of the galvanic pile is finished (polarization tests are required before and after the activation of the galvanic pile).
Conditions of polarization test: 30-570A as scanning current density, 30s of operation at each current, 15A/s of current load rate, 2.2 anode metering ratio and 3.5 cathode metering ratio. Anode humidity 40% RH, cathode humidity 60% RH, hydrogen back pressure 120kPa, air back pressure 100kPa, anode 75 ℃, cathode 75 ℃, and stack temperature 78 ℃.
Example 2
Preparing 30 parts by volume of 3% H 2 O 2 20 parts of 5% by mass H 2 SO 4 50 parts of deionized water, stirring for 0.5 hour, and uniformly mixing. And clamping the membrane electrode by using a flat-mouth clamp, vertically placing the membrane electrode into the prepared solution, slowly placing the solution horizontally, standing the solution for 0.5h, absorbing excessive moisture by using dust-free paper, preparing 90 membrane electrodes according to the operation, stacking the membrane electrodes prepared by pretreatment, and preparing an activation test.
And starting a temperature control program and a cooling water program on the assembled galvanic pile, controlling the cathode back pressure to be 40kPa, and controlling the anode back pressure to be 20kPa. The anode measurement ratio 2.2, the cathode measurement ratio 3, and the anode humidity were controlled to 50% RH at all times, and the cathode humidity was controlled to 50% RH at all times. And manually controlling the temperature, starting the temperature of the galvanic pile to be 30 ℃, adjusting the temperature at 2 ℃/min, gradually increasing the temperature to 78 ℃, and stably purging for 10min to finish nitrogen purging.
The anode is switched to be humidified hydrogen, the cathode is switched to be humidified air, the cathode metering ratio is gradually increased from 2.2 to 3, the anode metering ratio is gradually increased from 1.2 to 2, the anode back pressure is gradually increased from 20kPa to 110kPa, the cathode back pressure is gradually increased from 40kPa to 130kPa, the operation temperature is 75 ℃ at the anode, 75 ℃ at the cathode and 78 ℃ at the galvanic pile. And (3) starting a load, increasing the current to 30A, operating for 40s, increasing the current to 570A, operating for 40s, decreasing the current to 60A, operating for 40s, increasing the current to 540A, operating for 40s (the current load increasing rate is 20A/s), and so on until the current reaches 300A, operating for 30min at constant current 300A, decreasing the current to 30A, operating for 20s, and completing the activation of the first section of trough, wherein the parameters of the activation of the first section of trough are shown in Table 1.
After the activation of the first section of wave trough is finished, the current stays for 10s from 30A, then rises to 570A, runs for 15s, then falls to 60A, runs for 15s, then rises to 540A, runs for 15s, falls to 90A, runs for 15s, and repeats the same, when the current reaches 300A, the constant current is loaded for 10min, then the current falls to 30A, runs for 20s, and finishes the activation of the second section of wave trough, the parameters of the activation of the second section of wave trough are shown in table 2, so that the first wave trough activation is finished, and three cycles are circulated, so that the activation of the electric pile is finished (polarization tests are required before and after the activation of the electric pile).
Comparative example 1
Preparing 35 parts by volume of 3% H 2 O 2 25 parts of 5% by mass H 2 SO 4 40 parts of deionized water, stirring for 0.5h, and uniformly mixing. Clamping the membrane electrode by using a flat clamp, vertically placing the membrane electrode into the prepared solution, slowly placing the solution horizontally, standing for 0.5h, absorbing excessive moisture by using dust-free cloth, preparing 90 membrane electrodes according to the operation, stacking the membrane electrodes prepared by pretreatment, and preparing an activation test.
And starting a temperature control program and a cooling water program on the assembled galvanic pile, controlling the cathode back pressure to be 33kPa, and controlling the anode back pressure to be 13kPa. The anode measurement ratio was 2.5, the cathode measurement ratio was 3.5, and the anode humidity was always controlled at 40% RH and the cathode humidity was always controlled at 60% RH. And manually controlling the temperature, starting the temperature of the galvanic pile to be 30 ℃, adjusting the temperature at 2 ℃/min, gradually increasing the temperature to 78 ℃, and stably purging for 10min to finish nitrogen purging.
The anode is switched to be humidified hydrogen, the cathode is switched to be humidified air, the cathode metering ratio is gradually increased from 2.5 to 3.5, the anode metering ratio is gradually increased from 1.6 to 2.5, the anode back pressure is gradually increased from 13 to 100kPa, the cathode back pressure is gradually increased from 33 to 120kPa, the operation temperature is 75 ℃ at the anode, 75 ℃ at the cathode and 78 ℃ at the galvanic pile.
And starting a load, operating the current for 30A for 5min, slowly increasing the current to 300A, operating the current for 3h under the condition of constant current of 300A, then reducing the current to 30A, and operating the current for 10min to complete the activation of the constant-current galvanic pile, wherein the constant-current activation program of the galvanic pile is shown in a table 3.
Table 3 comparative example 1 pile constant current activation procedure
FIG. 2 is a polarization curve before and after activation in example 1, and it can be seen from FIG. 2 that example 1 is before activationThe current density at 0.65V was 1.52A/cm 2 After activation, the concentration of the active carbon can reach 1.68A/cm 2 。
FIG. 3 is a polarization curve before and after activation in example 2, and it can be seen from FIG. 3 that the current density at 0.65V before activation in example 2 is 1.57A/cm 2 The current density after activation can reach 1.72A/cm 2 The results show that the trough type current activation mode improves the oxygen transmission channel, so that the utilization rate of Pt is the highest, and the overall performance of the membrane electrode is improved.
FIG. 4 is a polarization curve before and after the activation of comparative example 1, and it can be seen from FIG. 4 that the current density of comparative example 1 at 0.65V before the activation was 1.48A/cm 2 The current density after activation at 0.65V was 1.51A/cm 2 It is demonstrated that constant current activation does not improve membrane electrode performance in a short period of time.
Fig. 5 is a uniformity curve of the activated stacks in example 1 and comparative example 1, which shows that the voltage uniformity of each cell is better after the trough activation process, and the voltage still jumps after the constant current activation. It is shown that the activation method of the present invention can be applied not only to new membrane electrodes, but also to long-standing galvanic piles.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention in any way. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications can be made, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (10)
1. A method of activating a fuel cell stack, comprising the steps of:
preactivating the membrane electrode in preactivating solution to obtain an activated membrane electrode; the pre-activation liquid comprises the following components in volume fraction: 5% -40% of hydrogen peroxide, 10% -50% of dilute sulfuric acid and 20% -60% of water, wherein the mass concentration of the hydrogen peroxide is 3% -5%, and the mass concentration of the dilute sulfuric acid is 3% -5%;
performing stack in-situ activation on the activated membrane electrode, wherein the stack in-situ activation comprises the following steps:
switching the cathode and the anode to humidifying nitrogen, and purging the galvanic pile;
switching the anode into humidified hydrogen and the cathode into humidified air, firstly increasing the current to 30A, staying for 30-50 s, then increasing the current to 570A, staying for 30-50 s, then decreasing the current to 60A, staying for 30-50 s, then increasing the current to 540A, staying for 30-50 s, and so on, and when the current reaches 300A, performing constant-current activation for 20-30 min, finally decreasing the current to 30A, staying for 20-30 s, and completing the activation of the first section of trough;
increasing the current to 570A, staying for 10-20 s, decreasing the current to 60A, staying for 10-20 s, increasing the current to 540A, staying for 10-20 s, decreasing the current to 90A, staying for 10-20 s, and so on, when the current reaches 300A, performing constant-current activation for 5-10 min, finally decreasing the current to 30A, staying for 10-20 s, and completing second-stage trough activation, wherein the first trough activation cycle comprises first-stage trough activation and second-stage trough activation;
and (5) circulating for activation of the valley 3-5 times.
2. The activation method according to claim 1, wherein the pre-activation liquid comprises the following volume fractions of components: 30-35% of hydrogen peroxide, 20-25% of dilute sulfuric acid and 40-50% of water, wherein the mass fraction of the hydrogen peroxide is 3%, and the mass fraction of the dilute sulfuric acid is 5%.
3. The activation method according to claim 1, wherein the time for purging is 30 to 40min.
4. The activation method according to claim 1 or 3, wherein the purging process comprises: the temperature is increased from 30 ℃ to 78 ℃, and the temperature increasing rate of the temperature increase is 2 ℃/min.
5. The activation method according to claim 1, wherein the anode is provided at a metering ratio of 1.6 to 2.5, and the cathode is provided at a metering ratio of 2.8 to 3.5.
6. The activation method according to claim 1 or 5, wherein the humidity of the anode is 40% to 60%, and the humidity of the cathode is 60% to 80%.
7. The activation method according to claim 1, wherein the anode has a back pressure of 13 to 110kPa, and the cathode has a back pressure of 33 to 130kPa.
8. The activation method according to claim 1, wherein the current lift/lower load rate during in-situ activation of the pile is independently 5 to 20A/s.
9. The activation process according to claim 1, wherein the pre-activation time is between 0.5 and 1 hour.
10. The activation method according to claim 1, wherein the number of the membrane electrodes in the stacked in-situ activation is 90 to 120, and the power is independently 30 to 50kW.
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