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Device and method for testing electric conductivity of powder material and impedance of membrane electrode

A technology for testing devices and powder materials, applied in the direction of measuring resistance/reactance/impedance, measuring devices, measuring electrical variables, etc., can solve the problems of reducing the contact resistance between the compact and the wire, high test cost, high test accuracy, etc., to achieve Inexpensive, easy to master, and simple to test for effects

Active Publication Date: 2013-06-12
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the results published in the "Journal of East China University of Science and Technology", Qin Changyong et al. added ATO powder into the cavity of the tablet press and formed it under a certain pressure to obtain a compact. Then, the resistance value at both ends of the compact was measured by a multimeter, and the powder Bulk conductivity, this method is easy to operate, but the error is large, and the ionic conductivity of the mixed charged powder material cannot be measured; Chen Weizhong et al. in their invention patent (application number: 200810216653. The tablet press was compacted, and the test device was connected after the metal powder was coated on both sides of the compact. The electronic and ion conductivity of the mixed charged powder material was obtained by the DC shunt method and the AC impedance method. The metal powder reduced the compaction. The contact resistance with the wire, this method has high test accuracy, but it cannot measure the electronic and ionic conductivity characteristics of mixed charged powder materials at different temperatures and humidity
In addition, the membrane electrode prepared by mixing charged powder materials has both electron conduction and proton conductivity, and its thickness is about 70-200 μm, which requires high test accuracy, and temperature and humidity have a great impact on the impedance of the membrane electrode. influence, which makes it more difficult to test the membrane electrode impedance
Most researchers test the membrane electrode impedance in a single cell. The three-electrode method is used to test the AC impedance of the working electrode, and the electron and proton impedance obtained by the equivalent circuit fitting have large errors. Because the impedance value includes the circuit, the salt bridge to the electrolyte resistance of the working electrode, etc., not only the test process is complicated, but also a lot of material waste is caused, and the test cost is high

Method used

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  • Device and method for testing electric conductivity of powder material and impedance of membrane electrode

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Grind the ATO powder material with electronic conductivity, obtain a certain particle size powder conductive material with a 200-mesh sieve, weigh 0.5 g, dry it in a vacuum oven at 80 °C for 12 h, and briquette.

[0041] Then, the dried ATO powder material was placed in a commercial briquetting machine to prepare briquettes with a diameter of 10 mm, and the thickness of the briquettes was measured by a vernier caliper.

[0042] Take out the briquetting block, press the porous stainless steel mesh-briquetting block 7-stainless steel mesh figure 2 After assembly, obtain the test sample of the sandwich structure. like Figure 1a As shown, it is placed in the sample chamber to be tested consisting of the upper pressing rod 1, the base 10 and the temperature control sleeve 4, and the pressing block 7 is compressed by the upper fastening screw 2 and the lower fastening screw 11, each screw The torque is 1 N m.

[0043] The test temperature of the sample chamber can be con...

Embodiment 2

[0048] The test material was changed to ATO-SnP with both electronic and proton conductivity 2 o 7 Mix the charged powder materials, grind the powder materials, use a 200-mesh sieve to obtain powder materials with a certain particle size, weigh 0.5 g, and dry them in a vacuum oven at 80 °C for 12 h before briquetting.

[0049] Dry ATO-SnP 2 o 7 The powder material was placed in a commercial briquetting machine to prepare briquettes, the diameter of the briquettes was 10 mm, and the thickness of the briquettes was measured by a vernier caliper.

[0050] Take out the briquetting block, press the porous stainless steel mesh-briquetting block-stainless steel mesh figure 2 After assembly, obtain the test sample of the sandwich structure. like Figure 1a As shown, it is placed in the sample chamber composed of the upper pressing rod 1, the base 10 and the temperature control sleeve 4, and the pressing block 7 is compressed by the upper fastening screw 2 and the lower fastening...

Embodiment 3

[0060] This example institute, adopts catalyst IrO 2 / ATO, IrO 2 / Cs 1.5 HWA–ATO prepared membrane electrode, the specific method is as follows:

[0061] First, the above-mentioned catalyst and 5% PTFE emulsion are mixed in a certain volume of isopropanol in a certain proportion, and the spray slurry is obtained after hundreds of times of ultrasonication in an ice bath, and then the PTFE film is used as the substrate, and the catalytic layer is prepared by heating and spraying. as attached image 3 , and finally the PTFE film with the anode catalytic layer 142, the Nafion membrane 143, and the PTFE film of the cathode catalytic layer 144 are placed under a pressure of 750 N cm -2 The PTFE film was peeled off by hot pressing at a temperature of 135 °C to obtain the tested membrane electrode. Among them, MEA-1 and MEA-2 are IrO 2 / ATO and IrO 2 / Cs 1.5 Membrane electrode prepared by HWA-ATO two catalysts.

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Abstract

The invention provides a device and a method for testing the electric conductivity of a powder material and the impedance of a membrane electrode, which can meet two measurement modes: a powder material electric conductivity measurement mode and a membrane electrode impedance measurement mode. The powder material electric conductivity measurement mode comprises the steps of putting a testing sample of prepared powder press cake in a sample testing cell, testing by using an assembled die, obtaining the total impedance and electron impedance of powder respectively, obtaining proton impedance by combining an impedance parallel-connection formula and calculating to obtain electron conductivity, proton conductivity and total conductivity; and the membrane electrode impedance measurement mode comprises the steps of putting a testing sample of the prepared membrane electrode in the sample testing cell, testing by using the assembled die and obtaining the impedance of a membrane electrode. The testing device is provided with a temperature control sleeve and a humidifying pipeline, so that the electric conductivity of the powder material and the impedance of the membrane electrode under different temperature and humidity can be tested. The testing device is simple in equipment, easy to operate and precise in measurement result; meanwhile, the testing device is applicable for testing the electric conductivity of a mixed charged powder material and the impedance of the membrane electrode in a simulative PEM (Polymer Electrolyte Membrane) electrolytic tank environment; and therefore, the feasibility, the necessity and the importance of the device are further highlighted.

Description

technical field [0001] The invention relates to a method for testing material properties method , especially involving the relationship between the conductivity of a powder material and the impedance of the membrane electrode Test device and method . Background technique [0002] At present, mixed charged powder materials with both electron and proton conductivity, because they can significantly optimize the electron and proton channel transport capabilities of proton exchange membrane fuel cells and water electrolysis cell membrane electrodes, and then improve the interface reaction characteristics, have been widely studied by many researchers. Used for catalytic layer modification materials and catalyst carrier materials. Among them, the measurement of the electronic and proton conductivity properties of powder materials is an indispensable physical parameter in the process of evaluating the application of powder materials. Therefore, it is extremely critical to optimi...

Claims

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Application Information

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IPC IPC(8): G01R27/02
Inventor 王新东刘高阳许军元刘桂成蒋钜明王一拓彭冰霜
Owner UNIV OF SCI & TECH BEIJING
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