CN114112835B - Method for online testing oxygen permeation condition of proton exchange membrane through embedded microelectrode - Google Patents
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- 239000012528 membrane Substances 0.000 title claims abstract description 141
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000001301 oxygen Substances 0.000 title claims abstract description 48
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 48
- 238000012360 testing method Methods 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 33
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 24
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 15
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 12
- 230000003197 catalytic effect Effects 0.000 claims abstract description 10
- 230000008859 change Effects 0.000 claims abstract description 10
- 238000007731 hot pressing Methods 0.000 claims abstract description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 26
- 239000003054 catalyst Substances 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 239000011889 copper foil Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 230000007423 decrease Effects 0.000 claims description 2
- 230000035699 permeability Effects 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 238000009792 diffusion process Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000002848 electrochemical method Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229920000557 Nafion® Polymers 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011066 ex-situ storage Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
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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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N2015/086—Investigating permeability, pore-volume, or surface area of porous materials of films, membranes or pellicules
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Pathology (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
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Abstract
The invention relates to a method for online testing oxygen permeation condition of a proton exchange membrane by an embedded microelectrode, which comprises the following specific steps: cutting a proton exchange membrane to be tested into a sample membrane, placing the sample membrane in the middle of a polytetrafluoroethylene membrane 1, placing Pt wires on fold lines in the sample membrane, covering one side of the sample membrane, on which the Pt wires are fixed, with a standard membrane, covering the surface of the standard membrane with a rectangular polytetrafluoroethylene membrane 2, hot-pressing to obtain an embedded microelectrode composite proton exchange membrane, hot-pressing the upper and lower surfaces of the embedded microelectrode composite proton exchange membrane to transfer a catalytic layer, respectively, so as to obtain a battery with a sandwich structure, testing the potential difference of a battery anode and the microelectrode Pt wires under a certain current density by using a battery test bench, gradually reducing the potential difference along with the oxygen permeation in the proton exchange membrane, and judging the oxygen permeation condition of the proton exchange membrane to be tested according to the potential difference change.
Description
Technical Field
The invention belongs to the technical field of testing the permeability, pore volume or pore surface area of a porous material, and particularly relates to a method for testing the oxygen permeation condition of a proton exchange membrane on line through an embedded microelectrode.
Background
In recent years, the problem of oxygen permeation of Proton Exchange Membranes (PEM) has been increasingly focused by researchers, and various membrane oxygen permeation testing methods have also been developed. For conventional Pt-free PEM, there are a variety of ex situ methods to test oxygen permeation, such as by volumetric methods, time-lapse methods, gas chromatography tests, and the like. LaConti and Sakai et al measured the permeability coefficient of oxygen in Nafion membranes by introducing oxygen on one side of the membrane and applying a higher relative pressure while measuring the permeability rate of oxygen on the other side to obtain the permeability coefficient of oxygen. The time delay method is similar to the volumetric method, except that the time for oxygen to permeate to the other side of the membrane and fill up with a fixed volume is mainly tested. The advantage of this method is that the diffusion coefficient and solubility coefficient can be decomposed from the permeability coefficient. Similarly, gas chromatography is mainly used to measure the change in oxygen concentration on the opposite side of the membrane to determine the oxygen permeation. Another type of method for measuring the gas permeability coefficient of a PEM is to use electrochemical methods. Electrochemical methods can monitor the current over time to obtain diffusion limiting conditions across the membrane and are currently widely used to characterize the gas permeability of the PEM. In this method a half-cell electrochemical system is used: one side of the membrane is in an acidic solution, a working electrode is placed on the surface of the membrane, and a counter electrode is placed in the solution, a reaction gas is supplied to the other side of the membrane, and the current across the membrane is measured over time to estimate the diffusion coefficient and the solubility coefficient of the reactant in the membrane. Although the above methods can effectively measure the oxygen permeation value of the PEM, the actual oxygen permeation condition during the operation of the fuel cell cannot be obtained due to the off-line test. While it is only possible to test a Pt-free PEM, it cannot be tested by conventional methods because it must be passed through the anode side with hydrogen to obtain its true oxygen permeation.
The invention adopts the embedded microelectrode method to test the oxygen permeation quantity of the proton exchange membrane, and the method can be used for in-situ on-line testing of the oxygen permeation condition of the traditional proton exchange membrane on a single cell, is also suitable for the composite proton exchange membrane containing the oxygen permeation resistant additive, and has important scientific significance.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art, and provides a method for online testing the oxygen permeation condition of a proton exchange membrane through an embedded microelectrode, which can obtain the real oxygen permeation condition in the operation process of a fuel cell and has high accuracy.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the method for testing the oxygen permeation condition of the proton exchange membrane on line through the embedded microelectrode comprises the following specific steps:
1) Cutting a proton exchange membrane to be detected into a square sample membrane with the side length of 10-20cm, then placing the sample membrane in the middle of a rectangular Polytetrafluoroethylene (PTFE) membrane 1 with a larger area, placing Pt wires on folding lines in the sample membrane, fixing two ends of the Pt wires on the PTFE membrane 1 after the two ends of the Pt wires exceed the sample membrane and do not exceed the PTFE membrane, respectively fixing a copper foil between two ends of the Pt wires and boundary points of the sample membrane and the PTFE membrane 1, and separating the Pt wires and the membrane (for protecting the Pt wires);
2) Covering a standard membrane with the same size as the sample membrane on the side of the sample membrane fixed with Pt wires, covering a rectangular polytetrafluoroethylene membrane 2 with the same size as the rectangular polytetrafluoroethylene membrane 1 on the surface of the standard membrane, and performing hot pressing to obtain the embedded microelectrode composite proton exchange membrane;
3) The upper surface and the lower surface of the embedded microelectrode composite proton exchange membrane prepared in the step 2) are respectively hot-pressed and transferred with a catalytic layer by adopting a membrane electrode (CCM) technology to obtain a cell with a sandwich structure, one side of a sample membrane is a cathode of the cell, one side of a standard vertebral membrane is an anode of the cell, a cell test bench is used for testing potential difference (voltage) of the anode of the cell and a microelectrode Pt wire under a certain current density, and the potential difference gradually decreases along with the progress of oxygen permeation in the proton exchange membrane;
4) Drawing a potential difference change curve of the proton exchange membrane to be tested under a certain current density according to the potential difference test result in the step 3), and judging the oxygen permeation condition of the proton exchange membrane to be tested according to the potential difference change curve.
According to the scheme, the thickness of the proton exchange membrane to be detected in the step 1) is 8-200 mu m.
According to the scheme, the length of the polytetrafluoroethylene film 1 in the step 1) exceeds the length of the sample film by 6-8cm, and the width exceeds the width of the sample film by 4-6cm.
According to the scheme, the diameter of the Pt wire in the step 1) is 5-50 mu m, and the two ends of the Pt wire exceed the sample film by 1-2cm.
According to the above scheme, the standard membrane in step 2) is a commercially available standard commercial membrane, such as a 12 μm composite proton exchange membrane manufactured by Golgi, inc. of America.
According to the scheme, the hot pressing process conditions in the step 2) are as follows: hot-pressing at 110-150deg.C and 1.0-1.2MPa for 30-60s.
According to the scheme, the catalytic layer in the step 3) is a Pt-C catalyst, and the Pt content in the catalytic layer on the cathode side of the battery is 0.4mg cm -2 The Pt content in the anode side catalytic layer of the battery is 0.1mg cm -2 。
According to the above scheme, the battery test stand in step 3) is a battery test stand manufactured by Greenlight corporation, canada.
The microelectrode is manufactured by a method of hot-pressing a platinum wire in the middle of the two layers of composite proton exchange membranes, and the gas permeation condition of the proton exchange membrane to be detected is reflected by monitoring the change of the potential difference between the anode of the battery and the microelectrode. The hydrogen and the oxygen react on the surface of the microelectrode to reduce the potential difference between the anode of the battery and the microelectrode, and the change of the potential difference can reflect the change of the gas permeation quantity, so that the online monitoring of the gas permeation condition can be realized by detecting the change of the potential difference.
The invention has the beneficial effects that: the method can be used for analyzing the oxygen permeation fluctuation condition of the proton exchange membrane under different working conditions in the working environment of the battery on line, and can obtain the oxygen permeation value under specific conditions, has important scientific significance for research and development of the Pt-doped proton exchange membrane and evaluation of the operating condition of the battery, so as to explore the oxygen permeation attenuation action mechanism of the membrane electrode, and provide theoretical basis and detection means for development of the oxygen permeation resistant membrane electrode.
Drawings
FIG. 1 is a photograph of an embedded microelectrode composite proton exchange membrane prepared in example 1 of the present invention;
FIG. 2 is a physical view of a sandwich cell prepared in example 1;
FIG. 3 is a graph showing the voltage difference between the anode and the microelectrode at different current densities of the cell prepared in example 1;
fig. 4 is a graph showing the voltage difference between the anode and the microelectrode at different current densities of the battery prepared in example 2.
Detailed Description
The present invention will be described in further detail below with reference to the accompanying drawings, so that those skilled in the art can better understand the technical scheme of the present invention.
Example 1
A method for online testing oxygen permeation condition of proton exchange membrane by embedded microelectrode comprises the following specific steps:
1. cutting a proton exchange membrane to be detected (platinum-doped composite proton exchange membrane with the thickness of 15 mu m of Gore corporation in America) into square sample membranes with the size of 10cm multiplied by 10cm, placing the sample membranes in the middle of a rectangular PTFE membrane 1 with larger area (the length of the PTFE membrane 1 is 6cm longer than that of the sample membranes and the width of the PTFE membrane is 4cm. Pt wires (the diameter of the Pt wires is 25 mu m) are placed on folding lines in the sample membranes, the two ends of the Pt wires exceed the sample membranes by about 2cm, the Pt wires are shorter than the PTFE membrane 1 and are prevented from being broken by a press, the two ends of the Pt wires are fixed on the PTFE membrane 1, and a piece of copper foil is respectively fixed between the two ends of the Pt wires and boundary points of the sample membrane and the PTFE membrane 1;
2) Covering a standard membrane with the same size as the sample membrane on the side of the sample membrane fixed with Pt wires, covering a rectangular PTFE membrane 2 with the same size as the rectangular PTFE membrane 1 on the surface of the standard membrane, and hot-pressing for 30s at 150 ℃ and 1.2MPa to obtain an embedded microelectrode composite proton exchange membrane as shown in figure 1;
3) The upper and lower surfaces of the embedded microelectrode composite proton exchange membrane prepared in the step 2) are respectively hot-pressed and transferred with a catalytic layer by adopting a membrane electrode (CCM) technology, and the Pt content in the catalytic layer at one side of the sample membrane is 0.4mg cm -2 The Pt content in the catalytic layer at one side of the standard vertebral membrane is 0.1mg cm -2 The battery with the sandwich structure is obtained, one side of the sample membrane is the cathode of the battery, one side of the standard vertebral membrane is the anode of the battery, and the photo of the battery is shown in figure 2;
4) The battery was mounted on a test fixture of a battery test stand (Greenlight, canada) and the fixture was clampedAfter the connection of each circuit with the single cell test bench is completed, the potential difference (voltage difference) of the anode and the cathode of the battery under a certain current density is tested. The test conditions were: the temperature was 75℃and the cathode transition coefficient was 2.0, the anode back pressure was 0kpa, and the test current densities were 100mA/cm, respectively, by changing the cathode back pressure 2 ,500mA/cm 2 ,1000mA/cm 2 And 1500mA/cm 2 The potential difference (voltage) between the anode and the microelectrode of the cell under the conditions. The test data is shown in fig. 3, and it can be seen from the graph that the potential difference between the anode and the microelectrode is basically unchanged by increasing the cathode back pressure at different current densities, which indicates that the permeation amount of oxygen is extremely low. This is because the platinum-doped composite proton exchange membrane used in this example can prevent oxygen from penetrating to the anode.
Example 2
A method for online testing oxygen permeation condition of proton exchange membrane by embedded microelectrode, which uses a composite proton exchange membrane without platinum doped by Golgi corporation in America as a proton exchange membrane to be tested, and the preparation method of the battery is the same as that of example 1.
The prepared battery is mounted on a test fixture of a battery test bench (Greenlight company, canada), and after the fixture is linked with each line of a single battery test bench, the potential difference (voltage) of the anode and the microelectrode of the battery under a certain current density is tested. The test conditions were: the temperature was 75℃and the cathode transition coefficient was 2.0, the anode back pressure was 0kpa, and the test current densities were 100mA/cm, respectively, by changing the cathode back pressure 2 ,500mA/cm 2 ,1000mA/cm 2 And 1500mA/cm 2 The potential difference (voltage) between the anode and the microelectrode of the cell under the conditions, and the test data are shown in fig. 4. By increasing the back pressure of the changing cathode, the potential difference between the anode and the microelectrode is obviously reduced, which indicates that the permeation amount of oxygen is larger. Therefore, the method can be used for accurately testing the oxygen permeation condition of the proton exchange membrane on line, and the more the potential difference is reduced, the larger the gas permeation quantity is indicated.
The test results of the embodiment 1 and the embodiment 2 show that the oxygen permeation condition of the proton exchange membrane is feasible to test by adopting the method of the invention, and the accuracy is high.
Claims (7)
1. A method for online testing the oxygen permeation condition of a proton exchange membrane by an embedded microelectrode is characterized by comprising the following specific steps:
1) Cutting a proton exchange membrane to be detected into a square sample membrane with the side length of 10-20cm, then placing the sample membrane in the middle of a rectangular first polytetrafluoroethylene membrane with a larger area, placing Pt wires on folding lines in the sample membrane, fixing two ends of the Pt wires on the first polytetrafluoroethylene membrane, and respectively fixing a copper foil between two ends of the Pt wires and boundary points of the sample membrane and the first polytetrafluoroethylene membrane and between the Pt wires and the membrane;
2) Covering a standard membrane with the same size as the sample membrane on the side of the sample membrane fixed with the Pt wire, covering a rectangular second polytetrafluoroethylene membrane with the same size as the rectangular first polytetrafluoroethylene membrane on the surface of the standard membrane, and performing hot pressing to obtain the embedded microelectrode composite proton exchange membrane;
3) The upper surface and the lower surface of the embedded microelectrode composite proton exchange membrane prepared in the step 2) are respectively hot-pressed and transferred with a catalytic layer by adopting a membrane electrode technology, a cell with a sandwich structure is obtained, one side of a sample membrane is a cathode of the cell, one side of a standard vertebral membrane is an anode of the cell, a cell test bench is used for testing the potential difference between the anode of the cell and a microelectrode Pt wire under a certain current density, and the potential difference gradually decreases along with the oxygen permeation in the proton exchange membrane;
4) Drawing a potential difference change curve of the proton exchange membrane to be tested under a certain current density according to the potential difference test result in the step 3), and judging the oxygen permeation condition of the proton exchange membrane to be tested according to the potential difference change curve.
2. The method for online testing of oxygen permeation conditions of a proton exchange membrane by embedded microelectrodes according to claim 1, wherein the thickness of the proton exchange membrane to be tested in step 1) is 8-200 μm.
3. The method for on-line testing of proton exchange membrane oxygen permeation through embedded microelectrodes according to claim 1, wherein the length of the first polytetrafluoroethylene membrane in step 1) exceeds the sample membrane by 6-8cm and the width exceeds the sample membrane by 4-6cm.
4. The method for online testing of oxygen permeation conditions of a proton exchange membrane by embedded microelectrodes according to claim 1, wherein in the step 1), the diameter of the Pt wire is 5-50 μm, and two ends of the Pt wire exceed 1-2cm of the sample membrane.
5. The method for on-line testing of proton exchange membrane oxygen permeation by embedded microelectrodes according to claim 1, wherein step 2) the standard membrane is a commercially available standard commercial membrane.
6. The method for on-line testing of oxygen permeation of proton exchange membrane by embedded microelectrode according to claim 1, wherein the hot pressing process conditions in step 2) are: hot-pressing at 110-150deg.C and 1.0-1.2MPa for 30-60s.
7. The method for on-line testing of oxygen permeation condition of proton exchange membrane by embedded microelectrode according to claim 1, wherein in step 3) the catalyst layer is Pt-C catalyst, and the Pt content in the cathode side catalyst layer of the cell is 0.4mg cm -2 The Pt content in the anode side catalytic layer of the battery is 0.1mg cm -2 。
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