CN114112835A - Method for on-line testing oxygen permeation condition of proton exchange membrane through embedded microelectrode - Google Patents
Method for on-line testing oxygen permeation condition of proton exchange membrane through embedded microelectrode Download PDFInfo
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- 239000012528 membrane Substances 0.000 title claims abstract description 130
- 238000012360 testing method Methods 0.000 title claims abstract description 51
- 239000001301 oxygen Substances 0.000 title claims abstract description 47
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 47
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 38
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 26
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 26
- 239000002131 composite material Substances 0.000 claims abstract description 14
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 14
- 238000007731 hot pressing Methods 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 230000008859 change Effects 0.000 claims abstract description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 28
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 239000011889 copper foil Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 claims description 3
- 238000010023 transfer printing Methods 0.000 abstract description 2
- 230000035699 permeability Effects 0.000 description 10
- 239000007789 gas Substances 0.000 description 7
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 229910001882 dioxygen Inorganic materials 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
- 230000007246 mechanism Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000000243 solution Substances 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
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011066 ex-situ storage Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000002047 photoemission electron microscopy Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920001483 poly(ethyl methacrylate) polymer Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 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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Abstract
The invention relates to a method for testing the oxygen permeation condition of a proton exchange membrane on line through an embedded microelectrode, which comprises the following specific steps: the method comprises the steps of 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 a middle folding line of the sample membrane, covering a standard membrane on one side of the sample membrane where the Pt wires are fixed, covering a rectangular polytetrafluoroethylene membrane 2 on the surface of the standard membrane, carrying out hot pressing to obtain an embedded microelectrode composite proton exchange membrane, carrying out hot pressing transfer printing on a catalyst layer on each of the upper surface and the lower surface of the embedded microelectrode composite proton exchange membrane 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 progress of oxygen permeation in the proton exchange membrane, and judging the oxygen permeation condition of the proton exchange membrane to be tested according to the change of the potential difference.
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 oxygen permeation problem of Proton Exchange Membranes (PEM) has been receiving increasing attention from researchers, and various membrane oxygen permeation testing methods have been developed. For conventional Pt-free PEMs, there are a number of ex situ methods to measure oxygen permeation, such as by volumetric, time delay, gas chromatography, and the like. Lacoi and Sakai et al measured the permeability coefficient of oxygen in Nafion membranes using a volumetric method by passing oxygen gas on one side of the membrane and applying a higher relative pressure while measuring the permeability rate of oxygen gas on the other side to obtain the permeability coefficient of oxygen. The time delay method is similar to the volumetric method, except that it is primarily to test the time for oxygen to permeate to the other side of the membrane and fill a fixed volume. The advantage of this method is that the diffusion coefficient and the solubility coefficient can be decomposed from the permeability coefficient. Similarly, gas chromatography is mainly used to measure changes in oxygen concentration on the opposite side of the membrane to determine oxygen permeation. Another method of measuring the gas permeability coefficient of a PEM is to use electrochemical methods. Electrochemical methods, which can monitor the current over time to obtain diffusion limiting conditions across the membrane, are now 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 reactant gas is supplied to the other side of the membrane, and the current is measured across the membrane over time to estimate the diffusion coefficient and the solubility coefficient of the reactant in the membrane. Although the methods can effectively measure the oxygen permeation value of the PEM, the real oxygen permeation condition in the operation process of the fuel cell cannot be obtained because the methods adopt an off-line test. At the same time, it can only test the PEM without Pt, while for the PEM containing Pt, it cannot be tested by the traditional method because it must get the real oxygen permeation under the condition of introducing hydrogen gas into the anode side.
The method adopts an embedded microelectrode method to test the oxygen permeability of the proton exchange membrane, can test the oxygen permeability of the traditional proton exchange membrane on line in situ on a single cell, is also suitable for the composite proton exchange membrane containing the antioxidant permeability additive, and has important scientific significance.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for on-line testing the oxygen permeation condition of a proton exchange membrane through an embedded microelectrode aiming at the defects in the prior art, so that the real oxygen permeation condition in the operation process of a fuel cell can be obtained, and the accuracy is high.
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 a Pt wire on a folding line in the sample membrane, wherein two ends of the Pt wire exceed the sample membrane and do not exceed the PTFE membrane, fixing two ends of the Pt wire on the PTFE membrane 1, and respectively fixing a piece of copper foil between two ends of the Pt wire and junction points of the sample membrane and the PTFE membrane 1, and isolating the Pt wire and the middle of the membrane (for protecting the Pt wire);
2) covering a standard film with the same size as the sample film on one side of the sample film fixed with the Pt wires, covering a rectangular polytetrafluoroethylene film 2 with the same size as the rectangular polytetrafluoroethylene film 1 on the surface of the standard film, and carrying out hot pressing to obtain the embedded microelectrode composite proton exchange membrane;
3) respectively carrying out hot-pressing transfer printing on the upper surface and the lower surface of the embedded microelectrode composite proton exchange membrane prepared in the step 2) by adopting a membrane electrode (CCM) technology to form a catalyst layer, so as to obtain a battery with a sandwich structure, wherein one side of a sample membrane is a cathode of the battery, one side of a conical membrane is an anode of the battery, a battery test bench is used for testing the potential difference (voltage) of the anode of the battery and a microelectrode Pt wire under a certain current density, and the potential difference is gradually reduced along with the oxygen permeation in the proton exchange membrane;
4) and 3) 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 membrane 1 in the step 1) exceeds 6-8cm of the sample membrane, and the width of the polytetrafluoroethylene membrane exceeds 4-6cm of the sample membrane.
According to the scheme, the diameter of the Pt wire in the step 1) is 5-50 microns, and two ends of the Pt wire exceed the sample film by 1-2 cm.
According to the scheme, the standard membrane in the step 2) is a commercially available standard commercial membrane, such as a 12-micron composite proton exchange membrane manufactured by gore company in the united states.
According to the scheme, the hot pressing process conditions in the step 2) are as follows: hot pressing at 110-150 deg.c and 1.0-1.2MPa for 30-60 sec.
According to the scheme, the catalytic layer in the step 3) is a Pt-C catalyst, and the content of Pt in the catalytic layer at the cathode side of the cell is 0.4mg cm-2The Pt content in the anode side catalyst layer of the cell is 0.1mg cm-2。
According to the scheme, the battery test bench in the step 3) is a battery test bench produced by Greenlight, Canada.
The invention discloses a microelectrode which is manufactured by a method of hot-pressing a platinum wire in the middle of two layers of composite proton exchange membranes, and the gas permeation condition of the proton exchange membrane to be measured is reflected by monitoring the change of the potential difference between the anode of a battery and the microelectrode. The reaction of hydrogen and oxygen on the surface of the microelectrode can 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 amount, 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 not only 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 cell on line, but also can obtain the oxygen permeation value under specific conditions, has important scientific significance for the research and development of the Pt-doped proton exchange membrane and the evaluation of the cell operation condition, researches the oxygen permeation attenuation action mechanism of the membrane electrode according to the oxygen permeation attenuation action mechanism, and provides theoretical basis and detection means for the development of the anti-oxygen permeable 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 schematic diagram of a sandwich-structured battery prepared in example 1;
FIG. 3 is a test curve of a voltage difference between an anode and a micro-electrode at different current densities for the battery fabricated in example 1;
FIG. 4 is a test curve of a voltage difference between an anode and a micro-electrode at different current densities for the battery fabricated in example 2.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention is further described in detail below with reference to the accompanying drawings.
Example 1
A method for testing the oxygen permeation condition of a proton exchange membrane on line through an embedded microelectrode comprises the following specific steps:
1. cutting a proton exchange membrane to be detected (a platinum-doped composite proton exchange membrane of Goll company in America, the thickness of which is 15 microns) into a square sample membrane with the size of 10cm multiplied by 10cm, then placing the sample membrane in the middle of a rectangular PTFE membrane 1 with a larger area (the PTFE membrane 1 is 6cm longer than the sample membrane, the width of the PTFE membrane is 4 cm., placing Pt filaments (the diameter of the Pt filaments is 25 microns) on a folding line in the sample membrane, wherein two ends of the length of the Pt filaments exceed the sample membrane by about 2cm, the Pt filaments are shorter than the PTFE membrane 1 and are prevented from being broken by a press, fixing two ends of the Pt filaments on the PTFE membrane 1, and respectively fixing a piece of copper foil between two ends of the Pt filaments and a junction point of the sample membrane and the PTFE membrane 1;
2) covering a standard film with the same size as the sample film on one side of the sample film fixed with Pt wires, covering a rectangular PTFE film 2 with the same size as the rectangular PTFE film 1 on the surface of the standard film, and hot-pressing at 150 ℃ and 1.2MPa for 30s to obtain the embedded microelectrode composite proton exchange membrane as shown in figure 1;
3) respectively hot-pressing and transferring a catalyst layer on the upper surface and the lower surface of the embedded microelectrode composite proton exchange membrane prepared in the step 2) by adopting a membrane electrode (CCM) technology, wherein the Pt content in the catalyst layer on one side of the sample membrane is 0.4mg cm-2The Pt content in the catalytic layer at one side of the standard vertebra membrane is 0.1mg cm-2Obtaining a battery with a sandwich structure, wherein one side of the sample membrane is a cathode of the battery, one side of the standard conical membrane is an anode of the battery, and a photo of the battery is shown in figure 2;
4) the cell was mounted on a test fixture in a cell test stand (Greenlight, canada), and the potential difference (voltage difference) between the anode and cathode of the cell at a certain current density was tested after the fixture was linked to the various lines of the cell test stand. The test conditions were: the temperature is 75 ℃, the cathode transition coefficient is 2.0, the anode backpressure is 0kpa, and the test current density is respectively 100mA/cm by changing the cathode backpressure2,500mA/cm2,1000mA/cm2And 1500mA/cm2Potential difference (voltage) between the anode of the cell and the micro-electrode under the conditions. As shown in FIG. 3, it can be seen that the potential difference between the anode and the micro-electrode was substantially constant at different current densities by increasing the cathode back pressure, indicating that the permeation amount of oxygen was extremely low. This is because the platinum-doped proton exchange membrane used in this example can prevent oxygen from penetrating into the anode.
Example 2
A method for testing the oxygen permeation condition of a proton exchange membrane on line through an embedded microelectrode takes a composite proton exchange membrane which is not doped with platinum and is manufactured by Goll company in America as a proton exchange membrane to be tested, and the method for preparing the battery is the same as that of the embodiment 1.
The prepared battery was mounted on a test jig of a battery test stand (Greenlight, canada), and after the connection of the jig with each line of the single cell test stand was completed, the potential difference (voltage) between the anode and the microelectrode of the battery at a certain current density was tested. The test conditions were: the temperature is 75 ℃, the cathode transition coefficient is 2.0, the anode backpressure is 0kpa, and the test current density is respectively 100mA/cm by changing the cathode backpressure2,500mA/cm2,1000mA/cm2And 1500mA/cm2The potential difference (voltage) between the anode and the micro-electrode of the cell under the conditions, and the test data are shown in FIG. 4. By increasing the back pressure of the changed cathode, the potential difference between the anode and the microelectrode is obviously reduced, which indicates that the permeation quantity 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.
The test results of example 1 and example 2 show that the method of the invention is feasible and has high accuracy in testing the oxygen permeation of the proton exchange membrane.
Claims (8)
1. A method for testing the oxygen permeation condition of a proton exchange membrane on line through 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 polytetrafluoroethylene membrane 1 with a larger area, placing a Pt filament on a folding line in the sample membrane, wherein two ends of the Pt filament exceed the sample membrane and do not exceed the polytetrafluoroethylene membrane, fixing two ends of the Pt filament on the polytetrafluoroethylene membrane 1, and fixing a piece of copper foil between the two ends of the Pt filament and the junction points of the sample membrane and the polytetrafluoroethylene membrane 1 respectively, wherein the copper foil is separated between the Pt filament and the membrane;
2) covering a standard film with the same size as the sample film on one side of the sample film fixed with the Pt wires, covering a rectangular polytetrafluoroethylene film 2 with the same size as the rectangular polytetrafluoroethylene film 1 on the surface of the standard film, and carrying out hot pressing to obtain the embedded microelectrode composite proton exchange membrane;
3) hot-pressing and transferring a layer of catalyst layer on the upper surface and the lower surface of the embedded microelectrode composite proton exchange membrane prepared in the step 2) by adopting a membrane electrode technology to obtain a battery with a sandwich structure, wherein one side of a sample membrane is a cathode of the battery, one side of a conical membrane is an anode of the battery, a battery test bench is used for testing the potential difference of the anode of the battery and a microelectrode Pt wire under a certain current density, and the potential difference is gradually reduced along with the oxygen permeation in the proton exchange membrane;
4) and 3) 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 on-line testing of oxygen permeation condition of proton exchange membrane through embedded microelectrode 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 the oxygen permeation condition of the proton exchange membrane through the embedded microelectrode according to the claim 1, wherein the polytetrafluoroethylene membrane 1 in the step 1) has a length exceeding the sample membrane by 6-8cm and a width exceeding the sample membrane by 4-6 cm.
4. The method for on-line testing of the oxygen permeation condition of the proton exchange membrane through the embedded microelectrode according to claim 1, wherein the diameter of the Pt filament in the step 1) is 5-50 μm, and two ends of the Pt filament exceed the sample membrane by 1-2 cm.
5. The method for the on-line testing of the oxygen permeation of the proton exchange membrane through the embedded microelectrode of claim 1, wherein the standard membrane of step 2) is a commercially available standard commercial membrane.
6. The method for on-line testing the oxygen permeation condition of the proton exchange membrane through the embedded microelectrode according to the claim 1, wherein the hot pressing process condition of the step 2) is as follows: hot pressing at 110-150 deg.c and 1.0-1.2MPa for 30-60 sec.
7. The method for on-line testing of oxygen permeation condition of proton exchange membrane through embedded microelectrode according to claim 1, wherein the catalyst layer in step 3) is Pt-C catalyst, and the content of Pt in the catalyst layer at cathode side of the battery is 0.4mg cm-2The Pt content in the anode side catalyst layer of the cell is 0.1mg cm-2。
8. The method for the in-line testing of the oxygen permeation of the proton exchange membrane through the embedded microelectrode of claim 1, wherein the battery test bench of step 3) is a battery test bench manufactured by Greenlight, canada.
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