CN112433095B - Method for measuring water content in proton exchange membrane fuel cell membrane - Google Patents

Method for measuring water content in proton exchange membrane fuel cell membrane Download PDF

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CN112433095B
CN112433095B CN202011317283.4A CN202011317283A CN112433095B CN 112433095 B CN112433095 B CN 112433095B CN 202011317283 A CN202011317283 A CN 202011317283A CN 112433095 B CN112433095 B CN 112433095B
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孙树成
杨小康
孙嘉琦
俞红梅
邵志刚
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Dalian Institute of Chemical Physics of CAS
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Abstract

The invention discloses a method for measuring water content in a proton exchange membrane fuel cell membrane, which belongs to the technical field of fuel cells and comprises the following steps: the method comprises the following steps of measuring a non-membrane resistance part in the internal resistance of the fuel cell in advance and presetting the non-membrane resistance part in a fuel cell system; when the water content in the membrane is measured, the internal resistance of the fuel cell is collected through resistance measuring devices arranged at the two ends of the anode and the cathode of the proton exchange membrane fuel cell, a preset non-membrane resistance part is deducted from the internal resistance of the fuel cell to obtain the membrane resistance of the proton exchange membrane fuel cell, and the water content in the proton exchange membrane is calculated according to the membrane resistance of the fuel cell. The invention can realize the on-line accurate monitoring of the water content in the fuel cell membrane. The problem that the prior art can not accurately measure the water content in the membrane of the fuel cell is solved.

Description

Method for measuring water content in proton exchange membrane fuel cell membrane
Technical Field
The invention relates to the technical field of proton exchange membrane fuel cells, in particular to a method for measuring water content in a membrane of a proton exchange membrane fuel cell.
Background
Under the dual challenges of energy crisis and environmental issues, the pem fuel cell is receiving attention due to its characteristics of high efficiency and low emission, and is considered to be an ideal candidate for replacing an internal combustion engine as a power source of a new energy automobile. As pem fuel cells are gradually commercialized, their performance stability and service life are more and more important. Water management, as an important issue in the practical application of pem fuel cells, greatly affects the cell performance and service life, for example: flooding may cause severe mass transfer polarization, which may affect the battery performance if not, and cause local reversal if not; the over-drying of water can cause the conductivity of the proton exchange membrane to be reduced and the internal resistance of the battery to be increased; in addition, under the subzero temperature condition, the battery is permanently damaged due to the fact that the internal water content of the battery is too high after the battery is shut down, and the service life of the battery is greatly shortened. Therefore, monitoring of water content within the pem fuel cell membrane is particularly important as a guide for fuel cell system control.
In the prior art, electrochemical impedance is often used as a tool for judging the internal water content of a fuel cell, an alternating current disturbance signal continuously changing from high frequency to low frequency or a single high frequency alternating current disturbance signal is applied to the fuel cell, and various resistance information including membrane resistance, mass transfer polarization resistance, charge transfer resistance and the like can be accurately obtained by performing parameter fitting on a response signal. The method has the advantages that the measurement is convenient, the data can reflect the real state in the battery, and the obtained high-frequency resistance can be associated through a mathematical model to obtain the water content of the film.
In fact, however, the high-frequency resistance obtained by fitting the full-band impedance spectrum and the high-frequency resistance obtained by measuring the single high frequency cannot be completely equivalent to the film resistance, because the high-frequency resistance to be measured includes the electronic resistance of each electronic conductor and the non-film resistance part such as the contact resistance between different components in addition to the film resistance. If a high-frequency resistor is adopted to approximate the membrane resistance, membrane resistance errors of a few milliohms level are caused, and the authenticity and the accuracy of water content measurement are seriously influenced.
Disclosure of Invention
The invention aims to provide a method for measuring the non-membrane resistance and the water content in a membrane of a proton exchange membrane fuel cell, which is used for solving the problem that the water content in the membrane of the proton exchange membrane fuel cell cannot be accurately measured in the prior art.
The invention provides a method for measuring a non-membrane resistance part in the internal resistance of a proton exchange membrane fuel cell, which comprises the following steps: the internal resistance of the proton exchange membrane fuel cell comprises a membrane resistance part for proton conduction in the membrane and a non-membrane resistance part outside the membrane, wherein the non-membrane resistance part refers to the part except the membrane resistance of the proton conduction membrane in the internal resistance of the fuel cell;
(1) and (3) purging the proton exchange membrane fuel cell for a long time at a small air quantity by using gas with certain relative humidity.
(2) And monitoring the resistance between the anode and the cathode of the proton exchange membrane fuel cell in the purging process, and stopping purging and recording the current resistance value when the resistance reaches a balance value.
(3) And (3) deducting the film resistance obtained by calculating the certain humidification degree in the step (1) from the resistance value obtained in the step (2) to obtain the resistance value of the non-film resistance part.
Based on the above scheme, preferably, the non-membrane-resistance part comprises a current collecting plate, a bipolar plate, an electronic conduction resistor on the electrode, and a contact resistor inside the bipolar plate/current collecting plate, the electrode/bipolar plate and the electrode.
Based on the scheme, the non-membrane resistance part is a constant value in the range that the water content of the membrane is lambda larger than 2.98 (the water molecule ratio is larger than the number of the sulfonate groups).
Based on the above, it is preferable that the relative humidity of the gas of a certain relative humidity is in a range of 45% to 100%, and it is known in the art that the relative humidity is with respect to the operating temperature and pressure of the battery.
Based on the technical scheme, preferably, the gas amount range of the small gas amount purging is 25-125mL min-1 cm-2 Electrode area。
Based on the technical scheme, the time for long-time purging is preferably more than 3 hours, and preferably 3-6 hours.
Based on the above further scheme, preferably, the formula of calculating the film resistance from a certain humidification degree is as follows:
Figure BDA0002788337690000021
Figure BDA0002788337690000022
Figure BDA0002788337690000023
Figure BDA0002788337690000024
wherein R ismFor membrane resistance, L is the proton exchange membrane thickness, σ is the proton conductivity of the membrane, A is the effective area of the membrane, λ is the water content in the membrane, α is the water vapor activity (i.e., equal to the gas relative humidity) on the membrane surface, x is the mole fraction of water vapor on the membrane surface, P is the membrane surface pressuresatAnd T is the operating temperature of the proton exchange membrane fuel cell.
The above calculation process is as follows: obtaining a numerical value alpha from the relative humidity of the gas, substituting alpha into a formula (3) to obtain lambda, substituting lambda into a formula (2) to obtain sigma, and substituting sigma into a formula (1) to obtain the membrane resistance Rm(ii) a Deducting the film resistance R from the resistance value obtained in the step (2)mThe resistance value of the non-film-resistance portion can be obtained.
The invention also provides a method for measuring the water content in the membrane of the proton exchange membrane fuel cell, which comprises the following steps:
(1) the method is adopted to measure the resistance value of the non-membrane resistance part in the internal resistance of the proton exchange membrane fuel cell, and the resistance value is preset in a fuel cell system;
(2) and connecting a resistance measuring device at the two ends of the anode and the cathode of the proton exchange membrane fuel cell, and measuring the resistance at the two ends of the anode and the cathode of the proton exchange membrane fuel cell on line to obtain the internal resistance of the proton exchange membrane fuel cell.
(3) Deducting a preset non-membrane resistance part from the internal resistance of the proton exchange membrane fuel cell to obtain the membrane resistance of the proton exchange membrane fuel cell;
(4) and calculating the water content in the membrane of the proton exchange membrane fuel cell according to the membrane resistance of the proton exchange membrane fuel cell.
Based on the above, it is preferable that the water content in the film is measured in a range of λ > 2.98.
Based on the scheme, the method for measuring the water content in the membrane of the proton exchange membrane fuel cell is characterized in that the average water content in the membrane of the proton exchange membrane fuel cell is calculated by adopting the formulas (1) to (6):
Rm＝R-R0 (1)
Figure BDA0002788337690000031
Figure BDA0002788337690000032
Figure BDA0002788337690000033
Figure BDA0002788337690000034
Figure BDA0002788337690000035
wherein R is the resistance between the anode and the cathode of the proton exchange membrane fuel cell, R0Is a non-membrane barrier, RmFor membrane resistance, L is the proton exchange membrane thickness, σ is the proton conductivity of the membrane, λ is the water content in the membrane, A is the effective area of the membrane, α is the water vapor activity (approximately equal to the gas relative humidity) at the membrane surface, x is the water vapor mole fraction at the membrane surface, P is the membrane surface pressuresatAnd T is the operating temperature of the proton exchange membrane fuel cell.
The determination process of the water content in the membrane of the proton exchange membrane fuel cell comprises the following steps: obtaining the internal resistance R of the proton exchange membrane fuel cell through the step (2), and comparing the R with the previously measured resistance value R of the non-membrane resistance part0Substituting into formula (1) to obtain RmR is to bemAnd (6) substituting the formula to obtain the water content in the membrane of the proton exchange membrane fuel cell.
The invention has the beneficial effects that:
(1) the preset non-membrane resistance part can be set as a fixed value through the previous measurement before delivery and is preset in the fuel cell system. The adopted measuring method enables the water content of the membrane and the relative humidity of the purge gas to be balanced through balanced purging, can realize accurate control of the water content of the membrane, and obtains the relation between the membrane resistance and the water content according to the empirical relation between the proton conductivity of the membrane and the water content of the membrane.
(2) The part of non-film resistance is deducted from the internal resistance measured by the resistance measuring device, and only the film resistance directly related to the water content is obtained, so that the measuring result is more accurate.
(3) The invention can also monitor the water content of the film in real time during the operation of the battery so as to reasonably and effectively manage water, improve the performance stability of the battery and prolong the service life of the battery.
(4) The resistance measuring device is directly connected with two poles of the fuel cell, the internal resistance of the fuel cell is monitored on line, the operation is convenient, and the data can truly reflect the internal state of the cell.
Drawings
FIG. 1 illustrates the principle of separating non-membrane barriers in the present invention.
Fig. 2 shows the water content in the membrane corresponding to the internal resistance of the proton exchange membrane fuel cell measured at 65 ℃.
Detailed Description
Example 1
Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The effective area adopted in the example is 5cm2The monocell as the research object adopts a gas diffusion layer composed of a metal bipolar plate, a graphite flow field, carbon paper coated with a microporous layer and platinum catalyst loading of a cathode and an anode of 0.4mg/cm respectively2And 0.2mg/cm2And a perfluorosulfonic acid proton exchange membrane (Nafion 211).
In order to illustrate that the non-membrane resistance part in the internal resistance of the fuel cell is a constant value in a certain water content range, the following method is adopted:
by fixing the fuel cell temperature at 65 ℃, varying the dew point temperature within the bubbling humidifier, a series of nitrogen gases with different relative humidities were obtained, 20%, 30%, 40%, 45%, 50%, 60%, 80% and 100%. And introducing the nitrogen into two poles of the fuel cell at the flow rate of 500ml/min, and monitoring the impedance value of the cell at the frequency of 10kHz in real time by using an electrochemical workstation. When the impedance value changes within three minutes and does not exceed 0.01mohm, the impedance value at the moment is recorded as the internal resistance of the battery, and because the water vapor activity alpha on the surface of the membrane is approximately equal to the relative humidity of gas, the relative humidity of nitrogen is substituted into the following formula (2) to obtain lambda, and the relation between the lambda and the internal resistance of the battery is shown in figure 2.
The impedance value changes by no more than 0.01mohm within three minutes, so that the inside of the battery is considered to reach an equilibrium state, and the corresponding membrane proton conductivity can be calculated through formulas (1) and (2), namely, the lambda obtained through the following formula (2) is substituted into the following formula (1) to obtain the corresponding membrane proton conductivity.
Figure BDA0002788337690000051
λ＝0.043+17.81α-39.85α2+36.0α3 0＜α≤1 (2)
Fitting the internal resistance and the membrane proton conductivity found that, in the range of water content λ > 2.98 (the equilibrium water content corresponding to a purge gas relative humidity > 45%), the cell internal resistance is linear with the reciprocal of the membrane proton conductivity (R0.00276/o +0.0439), and the internal resistance is composed of a total of two parts, namely the membrane resistance related to the membrane proton conductivity (0.00276/σ) and a fixed intercept (0.0439), as shown in fig. 1.
The fixed value intercept is the non-membrane resistance part in the internal resistance, and the intercept is not changed along with the change of the water content in the membrane within the range of lambda being more than 2.98 (so the water content range of the membrane applicable to the measuring method is lambda being more than 2.98).
According to the characteristics, the non-membrane resistance part of the corresponding battery in the range of the water content lambda being more than 2.98 in the membrane can be obtained by measuring under the condition of relative humidity for one time, and the specific steps are as follows:
setting the dew point temperature in the bubbling humidifier to 65 ℃ to obtain 100% humidified nitrogen, and adding 100% humidified nitrogen for 100mL min-1Introducing positive and negative electrodes of the fuel cell, monitoring the high-frequency resistance value during balance by using an electrochemical workstation, taking the value during balance of the high-frequency resistance as the internal resistance of the fuel cell, wherein the value is 43.3mohm cm2。
When the 100% humidified nitrogen is in equilibrium with the water content in the membrane, the membrane resistance is calculated according to the following formula:
Figure BDA0002788337690000052
Figure BDA0002788337690000053
λ＝0.043+17.81α-39.85α2+36.0α3 0＜α≤1 (3)
Figure BDA0002788337690000054
the film resistance calculation result is as follows: 23.6mohm cm2。
According to the internal resistance and the membrane resistance of the fuel cell, subtracting the non-membrane resistance from the internal resistance to obtain the non-membrane resistance part of the fuel cell as follows: 19.7mohm cm2。
When measuring the water content in the membrane of the proton exchange membrane fuel cell, the fuel cell is at 1000mA/cm2The current density is firstly operated for 30min, then the battery is purged for 10min by dry nitrogen at a rate of 1L/min, and after purging is finished, an electrochemical workstation is adopted to measure the high-frequency resistance of the battery, and the value is as follows: 52.0mohm cm2。
Deducting the non-film resistance part to obtain the film resistance as follows: 32.3mohm cm2。
The corresponding film moisture content was calculated to be 10.38 using the following formula:
Figure BDA0002788337690000061
comparative example 1
Comparative examples the data from the examples are still used, but the non-film-blocking fraction is not subtracted.
In the examples, the high frequency resistance of the cell measured after the purge was completed was 52.0mohm cm2If the non-film resistance part is ignored and the high-frequency resistance value is approximately considered as the film resistance, the film resistance is 52.0mohm cm2。
The water content of the corresponding film is calculated by the following formula: 6.69:
Figure BDA0002788337690000062
it can be seen that, under the experimental conditions shown, if the high-frequency resistance is approximately equal to the film resistance, ignoring the non-film resistance, an error of 10.38-6.69 to 3.69 moisture content is caused.
Although the wetting degree of the proton exchange membrane can be qualitatively judged in practical application by neglecting the non-membrane resistance, the non-membrane resistance is not neglected in part in order to accurately measure and reflect the actual state in the membrane.

Claims (6)

1. A method for measuring water content in a membrane of a proton exchange membrane fuel cell, which is characterized by comprising the following steps:
(1) measuring the resistance value of a non-membrane resistance part in the internal resistance of the proton exchange membrane fuel cell, and presetting the resistance value into a fuel cell system; the resistance value of the non-membrane resistance part is the resistance except the membrane resistance of the conduction of the proton in the membrane in the internal resistance of the proton exchange membrane fuel cell;
(2) connecting a resistance measuring device at the two ends of the anode and the cathode of the proton exchange membrane fuel cell, and measuring the resistance at the two ends of the anode and the cathode of the proton exchange membrane fuel cell on line to obtain the internal resistance of the proton exchange membrane fuel cell;
(3) deducting a preset non-membrane resistance from the internal resistance of the proton exchange membrane fuel cell to obtain a membrane resistance of the proton exchange membrane fuel cell;
(4) calculating the water content in the membrane of the proton exchange membrane fuel cell according to the membrane resistance of the proton exchange membrane fuel cell;
in the step (1), the step of measuring the resistance value of the non-membrane resistance part of the proton exchange membrane fuel cell comprises the following steps:
1) purging the proton exchange membrane fuel cell with a gas having humidity;
2) monitoring the resistance between the anode and the cathode of the proton exchange membrane fuel cell in the purging process, and stopping purging and recording the current resistance value when the resistance reaches a balance value;
3) deducting the film resistance obtained by the humidity increasing calculation in the step 1) from the resistance obtained in the step 2) to obtain the resistance of a non-film resistance part;
the water content lambda in the film is more than 2.98, and the water content lambda in the non-film resistance film is a fixed value when the water content lambda in the film is more than 2.98.
2. The method of measurement according to claim 1, wherein the relative humidity of the gas having humidity of step 1) is in a range of 45% to 100%.
3. The method for measuring according to claim 1, wherein the amount of gas purged in step 1) is 25-125mL min-1cm-2 Electrode area(ii) a The purging time is 3-6 h.
4. The measurement method according to claim 1, wherein the non-membrane resistances comprise collector plates, bipolar plates, resistances of electron conduction on the electrodes and contact resistances of the bipolar plates/collector plates, electrodes/bipolar plates, and the inside of the electrodes.
5. The method of claim 1, wherein the membrane resistance is calculated by a humidimeter as follows:
Figure FDA0003306234700000011
Figure FDA0003306234700000012
Figure FDA0003306234700000013
Figure FDA0003306234700000021
wherein R ismIs membrane resistance, L is the thickness of the proton exchange membrane, A is the effective area of the membrane, sigma is the proton conductivity of the membrane, lambda is the water content in the membrane, alpha is the water vapor activity on the surface of the membrane, x is the mole fraction of water vapor on the surface of the membrane, P is the pressure on the surface of the membranesatAnd T is the operating temperature of the proton exchange membrane fuel cell.
6. The method of measurement according to claim 1, wherein the average water content in the pem fuel cell membrane is calculated using equations (1) - (6):
Rm＝R-R0 (1)
Figure FDA0003306234700000022
Figure FDA0003306234700000023
Figure FDA0003306234700000024
Figure FDA0003306234700000025
Figure FDA0003306234700000026
wherein R is the resistance between the anode and the cathode of the proton exchange membrane fuel cell, R0Is a non-membrane barrier, RmIs membrane resistance, L is the thickness of the proton exchange membrane, sigma is the proton conductivity of the membrane, A is the effective area of the membrane, lambda is the water content in the membrane, alpha is the water vapor activity on the surface of the membrane, x is the mole fraction of water vapor on the surface of the membrane, P is the pressure on the surface of the membranesatAnd T is the operating temperature of the proton exchange membrane fuel cell.
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