CN203164294U - Apparatus for testing conductivity and membrane electrode impedance of power material - Google Patents
Apparatus for testing conductivity and membrane electrode impedance of power material Download PDFInfo
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- CN203164294U CN203164294U CN 201320082844 CN201320082844U CN203164294U CN 203164294 U CN203164294 U CN 203164294U CN 201320082844 CN201320082844 CN 201320082844 CN 201320082844 U CN201320082844 U CN 201320082844U CN 203164294 U CN203164294 U CN 203164294U
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Abstract
The utility model relates to an apparatus for testing conductivity and membrane electrode impedance of a power material, wherein the apparatus can meet requirements of two kinds of measurement modes. In the terms of the measurement mode for conductivity of the powder material, a prepared tested powder press block sample is placed in a small tested sample chamber; a die is assembled to carry out testing, thereby respectively obtaining the electron impedance and the total impedance of the powder; an impedance parallel connection formula is combined to obtain proton impedance; and the electron conductivity, the proton conductivity, and the total conductivity are obtained by calculation. And in the terms of the measurement mode for membrane electrode impedance, a prepared tested membrane electrode sample is placed in a small tested sample chamber; and a die is assembled to carry out testing, thereby obtaining the impedance of the membrane electrode. According to the utility model, the testing apparatus is configured with a temperature controlling casing tube and a humidification pipeline. The conductivity and the membrane electrode impedance of the powder material in different temperature and humidity environments can be tested. The apparatus with the simple structure is easy to operate; and the measurement result is precise. Moreover, the testing apparatus is suitable for conductivity testing of a mixed charged powder material and membrane electrode impedance testing in a simulated PEM water electrolytic tank environment; and thus the feasibility, the essentiality and the importance of the device are highlighted.
Description
Technical field
The utility model relates to a kind of test material performance
Device, particularly relate to a kind of electrical conductivity of powdered material and membrane electrode impedance
Proving installation
Background technology
Have the charged powder body material of mixing of electronics, proton electrical conductance at present concurrently, because it can significantly optimize electronics, the proton channel transmittability of Proton Exchange Membrane Fuel Cells, water electrolytic cell membrane electrode, and then improve the interfacial reaction characteristic, be used for Catalytic Layer decorative material, catalyst carrier material by a large amount of researchers.Wherein the measurement of the electronics of powder body material, proton conductivity performance is to estimate indispensable physical parameter in the powder body material application process.Therefore extremely crucial to the performance of improving Proton Exchange Membrane Fuel Cells or water electrolytic cell by selection and the membrane electrode preparation technology of conductivity test optimization catalysis material.
The method of testing electrical conductivity of powdered material mainly contains briquetting method, four probe method etc. at present.The brave grade of Qin head delivered in the achievement at " East China University of Science's journal ", behind ATO powder adding sheeter cavity, obtain briquetting at the certain pressure compacted under, measure briquetting two ends resistance value by universal electric meter then, calculate and obtain the powder conductivity, this method easy operating, but error is bigger, can not measure the ionic conductivity of mixing charged powder body material; People such as Chen Weizhong are (application number: 200810216653.8) in its patent of invention, earlier tested powder body material is passed through the sheeter briquetting, and after covering metal powder, the briquetting both sides connect proving installation, electronics, the ionic conductivity of charged powder body material have been obtained to mix by direct current shunting and AC impedence method, metal powder has reduced the contact resistance of briquetting and lead, the method measuring accuracy is higher, but can not measure electronics, the ionic conductivity characteristic of mixing charged powder body material under different temperatures, the humidity.In addition, have electronic conduction and proton electrical conductance concurrently for mixing the prepared membrane electrode of charged powder body material, and its thickness is about 70-200 μ m, needs higher measuring accuracy, temperature, humidity produce a very large impact the impedance of membrane electrode, have more strengthened the difficulty of test of membrane electrode impedance.Most of researcher carries out at Dan Chizhong for the test of membrane electrode impedance, by three-electrode method working electrode is carried out ac impedance measurement, the electronics, the proton impedance that utilize the equivalent electrical circuit match to obtain, there is very mistake in the method, because this resistance value comprises circuit, salt bridge to working electrode bath resistance etc., not only test process is numerous and diverse, also causes the lot of materials waste, and testing cost is higher.
On many researchers' working foundation,
Summary of the invention
The utility modelPurpose is to solve the problems that exist in the electrical conductivity of powdered material membrane electrode testing impedance prepared with it, provides a kind of powder body material electronics, proton conductivity and by its preparation membrane electrode impedance test device and method.
The utility modelBy designed mould and electrochemical workstation, obtain powder body material electronics, proton conductivity and by the impedance of its preparation membrane electrode.And the sample preparation step is simple, and error is little, can reflect electronics, the proton conductivity size of different catalysis materials under different temperatures, damp condition more really.
The technical solution of the utility model is: the proving installation of a kind of electrical conductivity of powdered material and membrane electrode impedance, this device comprisesUpperpush rod, tighten screw rod, temperature control sleeve pipe, base and following fastening screw;
Upper end one side of described upperpush rod is provided with binding post, insert in the described temperature control sleeve pipe lower end of described upperpush rod, described upperpush rod and described temperature control sleeve pipe are fixed by the described screw rod that tightens, and the teflon sleeve of insulating effect is played in described upperpush rod and the setting of described temperature control sleeve pipe contact portion;
One side of described lower end base is provided with down binding post, and described lower end base and described temperature control sleeve pipe are fixed by described fastening screw down;
Described upperpush rod is provided with for adding wet channel on the inlet and outlet piping of water vapor, and described lower end base is provided with the following wet channel that adds for the inlet and outlet piping of water vapor.
Further, described upperpush rod, tighten screw rod, temperature control sleeve pipe, base and following fastening screw material for through the 316L of annealing in process stainless steel, carbon steel, bearing steel or chromium 12 materials.
The beneficial effects of the utility model are: owing to adopt technique scheme, the device of the testing electrical conductivity of powdered material that the utility model provides and prepared membrane electrode impedance thereof can be tested electronics, proton conductivity and the membrane electrode impedance of powder body material under different temperatures, under the humidity, test operation is simple, is easy to grasp; On the basis that obtains high-precision test result, test process does not use Die with High Precision and Complex equipment, and is with low cost.
Description of drawings
Fig. 1 a is the diagrammatic cross-section under survey electronics, the proton mixed conductivity of the utility model measurement mechanism used.
Fig. 1 b is the diagrammatic cross-section under the test membrane electrode of the utility model measurement mechanism is used.
Fig. 2 is the sandwich structure synoptic diagram of tested electronics, proton mixed conductivity powder briquetting.
Fig. 3 is the sandwich structure synoptic diagram of tested membrane electrode.
Fig. 4 a is the analog equivalent circuit diagram of ac impedance measurement in the utility model embodiment.
Fig. 4 b is the reduced graph of the analog equivalent circuit of ac impedance measurement in this utility model embodiment.
Fig. 5 is the conductivity data according to ATO powder under the different temperatures of the powder conductivity measurement pattern acquisition of example 1.
Mix charged powder body material ATO-SnP under Fig. 6 different condition that according to the facts the powder conductivity measurement pattern of example 2 obtains
2O
7The conductivity data of powder.
Accompanying drawing 7 mixes the impedance data that charged powder prepares membrane electrode according to the difference of the membrane electrode impedance measurement pattern acquisition of example 3.
Among the figure: 1: upperpush rod, 2: go up binding post, 3: fastening screw, 4: the temperature control sleeve pipe, 5: teflon sleeve, 6: on add wet channel, 7: detected sample powder briquetting, 8: add down wet channel, 9: following binding post, 10: base, 11: following fastening screw, 12: tested membrane electrode, 71: go up stainless (steel) wire, 72: tested electronics, proton mixed conductivity powder briquetting, 73: following stainless (steel) wire, 121: carbon paper, 122: anode catalyst layer, the 123:Nafion film, 124: negative electrode utmost point Catalytic Layer, 125: carbon paper.
Embodiment
Below in conjunction with accompanying drawing and example this utility model is described in further details.
Shown in Fig. 1 a and Fig. 1 b, the proving installation of a kind of electrical conductivity of powdered material of the utility model and membrane electrode impedance, this device comprises Upperpush rod 1, tighten screw rod 3, temperature control sleeve pipe 4, base 10 and following fastening screw 11;
Upper end one side of described upperpush rod 1 is provided with binding post 2, insert in the described temperature control sleeve pipe 4 lower end of described upperpush rod 1, described upperpush rod 1 is fixed by the described screw rod 3 that tightens with described temperature control sleeve pipe 4, and the teflon sleeve 5 of insulating effect is played in described upperpush rod 1 and described temperature control sleeve pipe 4 contact portion settings;
One side of described lower end base 10 is provided with down binding post 9, and described lower end base 10 is fixing by described fastening screw 11 down with described temperature control sleeve pipe 4;
Described upperpush rod 1 is provided with for adding wet channel 6 on the inlet and outlet piping of water vapor, and described lower end base 10 is provided with the following wet channel 8 that adds for the inlet and outlet piping of water vapor.
The utility model provides a kind of device of testing powder body material electronics, proton conductivity and prepared membrane electrode impedance thereof, powder body material or prepared membrane electrode are placed the detected sample cell, obtain respectively to cause impedance and the resulting impedance that is caused by electronics, proton conduction by electronic conduction with ac impedance measurement by the test of direct current polarization curve after connecting electrochemical workstation, and according to the conductivity formula
, calculating can get powder body material electronic conductivity and total conductivity (electronic conductivity and proton conductivity influence jointly), wherein
Be electronic conductivity or total conductivity, L is compressing tablet thickness, and R is resistance, and S is the compressing tablet area.Above-mentioned resulting impedance is equivalent to mixes the resulting impedance in parallel that electronics, proton conduction in the charged powder body material cause impedance, and its equivalent electrical circuit can be with reference to accompanying drawing 4a, wherein R
Int, R
i, R
eBe respectively interface impedance, electronic conduction causes that impedance, proton conduction cause impedance, W is Warburg impedance, C
CellBe space geometry electric capacity, C
IntBe interface capacitance.Because it is definite value that the testing impedance process does not have electrochemical reaction and interface impedance and interface capacitance, equivalent electrical circuit can be reduced to accompanying drawing 4b, and the relation of resulting impedance, electronic impedance, proton impedance can be represented by the equivalent resistance formula
, wherein electronic impedance, resulting impedance can obtain by the test of direct current polarization curve and ac impedance measurement respectively.
The ATO powder body material of tool electron conduction is ground, and with the powder conductive material of 200 order mesh screens acquisition certain particle size, weighing 0.5 g places 80 ℃ of vacuum drying chamber inner drying 12 h, briquetting.
Then, place commercial cuber to prepare briquetting the ATO powder body material of drying, the briquetting diameter is 10 mm, and briquetting thickness is recorded by vernier caliper.
Take out briquetting, after the stainless (steel) wire-briquetting 7-stainless (steel) wire of porous press Fig. 2 and assembled, obtain the detected sample of sandwich structure.As shown in Figure 1a, be placed on by upperpush rod 1, base 10 and temperature control sleeve pipe 4 and form the detected sample cell, compress by tightening screw rod 2 and 11 pairs of briquettings 7 of following fastening screw, the moment of torsion of each screw rod is 1 N m.
Can control the probe temperature of test sample cell by temperature control sleeve pipe 4; By adding wet channel 6 and adding the humidity that wet channel 8 is controlled the test sample cells down;
To go up wiring 2, down binding post 9 adopts two electrode modes to connect the VMP2 electrochemical workstation, carries out the test of direct current polarization curve, obtains its electronic impedance R by measuring electric current with the variation relation of voltage
e, again in conjunction with the area S on briquetting thickness L, the briquetting, according to the Conductivity Calculation formula
Calculate the powder electronic conductivity, finally obtain the electronic conductivity of ATO powder body material under the different temperatures.
Direct current polarization curve test process voltage range is 0-10 V, and the response current magnitude range is 0-2 A.
As accompanying drawing 5, by temperature control sleeve pipe control temperature, obtain the conductivity of ATO powder body material under the different temperatures, can find along with the conductivity variations of the rising ATO powder body material of temperature not, this is that temperature influence is very little because ATO is the electronic conduction phase.
Test material then is changed to the ATO-SnP that has electronics, proton conductive concurrently
2O
7Mix charged powder body material, powder body material is ground, with the powder body material of 200 order mesh screens acquisition certain particle size, weighing 0.5 g places 80 ℃ of vacuum drying chamber inner drying 12 h, treats briquetting.
ATO-SnP with drying
2O
7Powder body material places commercial cuber to prepare briquetting, and the briquetting diameter is 10 mm, and briquetting thickness is recorded by vernier caliper.
Take out briquetting, after the stainless (steel) wire-briquetting-stainless (steel) wire of porous press Fig. 2 and assembled, obtain the detected sample of sandwich structure.As shown in Figure 1a, be placed on by upperpush rod 1, base 10 and temperature control sleeve pipe 4 and form the detected sample cell, compress by tightening screw rod 2 and 11 pairs of briquettings 7 of following fastening screw, the moment of torsion of each screw rod is 1 N m.
Can control the probe temperature of test sample cell by temperature control sleeve pipe 4; By adding wet channel 6 and adding the humidity that wet channel 8 is controlled the test sample cells down;
To go up binding post 2, descend binding post 9 to adopt two electrode modes to connect the VMP2 electrochemical workstation, measure its electronic impedance and resulting impedance by the test of direct current polarization curve with ac impedance measurement, again in conjunction with briquetting thickness, briquetting sectional area, calculate the impedance of acquisition proton according to the equivalent resistance formula, finally obtain ATO-SnP under different temperatures, the humidity
2O
7The total conductivity of powder body material, electronics and proton conductivity.
Direct current polarization curve test process voltage range is 0-10 V, and the response current magnitude range is 0-2 A.
The condition of ac impedance measurement is 10 Hz-100 KHz for its frequency range, and amplitude is 10 mV.
Can find for mixing charged powder body material from accompanying drawing 6, temperature and humidity is very big to its total conductivity influence, this mainly is because the conductivity of the proton conductive phase in the charged powder body material of mixing increases along with temperature raises, the conductivity that adds proton conductive phase under the wet environment increases, and then causes total conductivity to increase.Represent 1/R by the equivalent resistance formula
Always=1/R
i+ 1/R
eCalculate, table 1 by accompanying drawing 6 proton conductivity, electronic conductivity, the total conductivity data of survey powder body material under different test conditions.
Table 1
ATO-SnP
2O
7Middle SnP
2O
7Doping ratio is 20%:
This example institute, employing catalyst I rO
2/ ATO, IrO
2/ Cs
1.5HWA – ATO prepares membrane electrode, and concrete grammar is as follows:
At first above-mentioned catalyzer, 5 % PTFE emulsions are mixed according to a certain ratio in the isopropyl alcohol of certain volume, up to a hundred backs of ice-bath ultrasonic obtain the spraying slurry, be matrix with the PTFE film then, adopt the hot spraying method to prepare Catalytic Layer, as accompanying drawing 3, will have the PTFE film of PTFE film, Nafion film 143, cathode catalysis layer 144 of anode catalyst layer 142 at last at pressure 750 N cm
-2Down, the PTFE film is peelled off in 135 ℃ of following hot pressing of temperature, obtains tested membrane electrode.Wherein MEA-1, MEA-2 are respectively IrO
2/ ATO and IrO
2/ Cs
1.5The membrane electrode of two kinds of Preparation of Catalyst of HWA – ATO.
Claims (2)
1.
The proving installation of a kind of electrical conductivity of powdered material and membrane electrode impedance is characterized in that, this device comprisesUpperpush rod (1), tighten screw rod (3), temperature control sleeve pipe (4), base (10) and following fastening screw (11);
Upper end one side of described upperpush rod (1) is provided with binding post (2), insert in the described temperature control sleeve pipe (4) lower end of described upperpush rod (1), described upperpush rod (1) is fixed by the described screw rod (3) that tightens with described temperature control sleeve pipe (4), and the teflon sleeve (5) of insulating effect is played in described upperpush rod (1) and described temperature control sleeve pipe (4) contact portion setting;
One side of described lower end base (10) is provided with down binding post (9), and described lower end base (10) is fixed by described fastening screw (11) down with described temperature control sleeve pipe (4);
Described upperpush rod (1) is provided with for adding wet channel (6) on the inlet and outlet piping of water vapor, and described lower end base (10) is provided with the following wet channel (8) that adds for the inlet and outlet piping of water vapor.
2. proving installation as claimed in claim 1, it is characterized in that, described upperpush rod (1), tighten screw rod (3), temperature control sleeve pipe (4), base (10) and following fastening screw (11) material for through the 316L of annealing in process stainless steel, carbon steel, bearing steel or chromium 12 materials.
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Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 201320082844 CN203164294U (en) | 2013-02-22 | 2013-02-22 | Apparatus for testing conductivity and membrane electrode impedance of power material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103149439A (en) * | 2013-02-22 | 2013-06-12 | 北京科技大学 | Device and method for testing electric conductivity of powder material and impedance of membrane electrode |
| CN105974199A (en) * | 2016-07-15 | 2016-09-28 | 中国科学院福建物质结构研究所 | Solid powder DC resistance and AC impedance test apparatus |
| JP2018048865A (en) * | 2016-09-21 | 2018-03-29 | パナソニックＩｐマネジメント株式会社 | Resistance measurement device and method thereof |
-
2013
- 2013-02-22 CN CN 201320082844 patent/CN203164294U/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103149439A (en) * | 2013-02-22 | 2013-06-12 | 北京科技大学 | Device and method for testing electric conductivity of powder material and impedance of membrane electrode |
| CN103149439B (en) * | 2013-02-22 | 2015-06-17 | 北京科技大学 | Device and method for testing electric conductivity of powder material and impedance of membrane electrode |
| CN105974199A (en) * | 2016-07-15 | 2016-09-28 | 中国科学院福建物质结构研究所 | Solid powder DC resistance and AC impedance test apparatus |
| JP2018048865A (en) * | 2016-09-21 | 2018-03-29 | パナソニックＩｐマネジメント株式会社 | Resistance measurement device and method thereof |
| US10302582B2 (en) * | 2016-09-21 | 2019-05-28 | Panasonic Intellectual Property Management Co., Ltd. | Resistance-measurement apparatus and method for measuring resistance of powdery materials |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20130828 Effective date of abandoning: 20150617 |
|
| RGAV | Abandon patent right to avoid regrant |