CN206848208U - A kind of in-situ test fixture and system for solid polymer electrolyte system - Google Patents
A kind of in-situ test fixture and system for solid polymer electrolyte system Download PDFInfo
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- CN206848208U CN206848208U CN201720702942.3U CN201720702942U CN206848208U CN 206848208 U CN206848208 U CN 206848208U CN 201720702942 U CN201720702942 U CN 201720702942U CN 206848208 U CN206848208 U CN 206848208U
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Abstract
The utility model belongs to elctro-catalyst activity rating method field, discloses a kind of in-situ test fixture and system for solid polymer electrolyte system.Carbon paper is put in respectively on the electrode of miniaturization membrane/electrode assembly both sides and drawn with wire, whole electrode is placed among electrode fixed plate, then sealed, connected by working electrode side and reference, the connector to electrode side, it is attached in test system and connects the measure that electrochemical workstation carries out relevant parameter, the device can solve the problems, such as the membrane swelling in test process well, so as to which more accurately and efficiently in-situ evaluation is used for the chemical property of polymer electrolyte fuel cells and water electrolysis elctro-catalyst.
Description
Technical field
The utility model belongs to electroanalysis test device field, particularly a kind of to be used for solid polymer electrolyte body
The in-situ test fixture and system of system.
Background technology
Solid polymer electrolyte has been widely used in fuel as a kind of safe, green electrolyte
In battery and water electrolysis.In order to improve electrocatalysis characteristic and reduce catalyst cost, the catalyst of high performance-price ratio is by people's
Extensive concern, therefore a kind of evaluation method that can be efficiently used for elctro-catalyst performance and course of reaction and measure device are ten
Divide important.
At present, the evaluation method for catalyst performance has two kinds, and one kind is liquid electrolyte three-electrode system, that is, is used
As electrolyte, the glass-carbon electrode for being loaded with catalyst pulp is urged as working electrode progress electricity for certain density acid or aqueous alkali
Change performance evaluation.Although the evaluation method system is simple and convenient to operate, quick, catalyst usage amount is few, cost is low, test
The gap of environment and actual application environment is larger, as electrolyte phase is compatible with species difference, solid solid interface and solid liquid interface
Property it is different, and anion can disturb the electrocatalysis characteristic of catalyst.Another method is exactly to prepare membrane electrode assembly to carry out electricity
Chemical property is evaluated, and this method is that the evaluation of battery performance is carried out under application conditions, can comprehensively evaluate elctro-catalyst
Catalytic performance, but the manufacture craft of membrane electrode assembly is cumbersome, required catalyst amount is more, cost is high, influence factor compared with
For complexity, so not being suitable for the performance evaluation of novel electro-catalytic agent.
Patent 201610924577.0 discloses one kind and urged for solid polymer electrolyte fuel cell and water electrolysis electricity
The evaluating apparatus of agent performance, it uses the method for hot pressing to connect collector and electrode, so carrying out water electrolysis and small molecule
During organic matter electroxidation, separated because the swelling of film is easily caused electrode with collector, so as to increase the resistance of test；When
During using conducting resin adhesion electrode cable and collector, it is understood that there may be the composition dissolving in conducting resinl, and then influence test result
Accuracy；For the electrochemical reaction under the fluid conditions such as water electrolysis and small molecule electroxidation, it is necessary to be stirred using magneton electromagnetism
Mix and carry out pressure mass transfer, the mass transport process in actual operating condition can not be simulated.
The content of the invention
In order to overcome now widely used liquid three-electrode system evaluation method, membrane electrode assembly evaluation method and above-mentioned
The deficiency of microelectrode, the purpose of the present utility model are：For solid polymer electrolyte fuel cell and water electrolysis electricity
Catalyst performance evaluation requirement, there is provided one kind prepare be simple and convenient to operate, cost is cheap and it is organic to be generally applicable to small molecule
The evaluating apparatus of thing electrochemical reaction.
To achieve the above object, the technical solution of the utility model is：
A kind of in-situ test fixture and system for solid polymer electrolyte system, the utility model are gathered using solid
Compound carries out the electrocatalysis characteristic test under in-situ condition, it is characterised in that include as electrolyte：Composite micro-electrode, afflux
The in-situ testing device fixture that body, extraction wire, sealing gasket, electrode fixed plate are formed, and supply, processing, circulation by gas
And tapping equipment forms test system.；
The both sides of composite micro-electrode are provided with collector and extraction wire, with electrode fixed plate that it is integrally fixed, by it
It is connected in test system, and the test of chemical property is carried out using electrochemical workstation.
In the above-mentioned technical solutions, composite micro-electrode is the polytetrafluoroethyl-ne that will be carved with required electrode shape and area hole
Alkene film is placed in solid polymer dielectric film both sides and hot pressing, and the slurry of required test catalyst is then added dropwise on the working electrode (s
Material, to Pt/C catalyst pulps are added dropwise on electrode and reference electrode, reference electrode is used as by the use of reversible hydrogen electrode.
In the above-mentioned technical solutions, collector is selected according to different using object；Oxidation reaction, oxygen for hydrogen
The electro-oxidation reaction of organic molecule and the electrolysis evolving hydrogen reaction of water such as reduction reaction, methanol and formic acid, using carbon paper or
Carbon cloth is as collector；Electrolysis oxygen evolution reaction for water, collector is used as using titanium net etc..
In the above-mentioned technical solutions, collector and extraction wire are respectively arranged with the counter electrode of composite micro-electrode both sides,
Then it is placed in the electrode fixed plate added with sealing gasket and uses fastened by screw.
In the above-mentioned technical solutions, in electrode fixed plate, the position contacted with working electrode, to electrode and reference electrode is set
Put sphere of movements for the elephants shape hole so that reactant smoothly reaches electrode surface, while has part sheet material to be contacted with electrode surface so as to have
Effect prevents the swelling of film, deformation.
The material of electrode fixed plate is polytetrafluoroethylene (PTFE), bakelite etc..
In the above-mentioned technical solutions, the part material that test system is connected with in-situ testing device fixture is glass, can
Bottleneck shape and ground is made, the groove of respective shapes can be also set in the fixed plate of docking, adds sealing gasket, with improve with
Electrode fixed plate contacts sealing.
To meet requirement of the gas as the high and low temperature performance test of reactant, deformed as one kind of the present utility model,
Also in-situ testing device fixture of the present utility model can be placed on and be provided with the hermetically sealed can of contact conductor leadout hole, outside
Portion winds heating tape and sets temperature control thermocouple, carries out high-temperature behavior test；Heating tank can be also placed in circulating cooling water bath
Interior progress cryogenic property test.
In the above-mentioned technical solutions, test system is selected according to different using object, oxidation and oxygen for hydrogen
The gas such as reduction be raw material electrocatalytic reaction, working electrode is directly purged using the gas of certain humidity；For methanol and
The liquid such as the electroxidation of the organic molecules such as formic acid, the electrolysis liberation of hydrogen of water, oxygen evolution reaction are the electrocatalytic reaction of raw material, and use is compacted
Dynamic pump carries out the liquid flowing in liquid circulation simulation practical operation.
The present utility model has the characteristics that：
（1）The utility model has the advantages of liquid three-electrode system and membrane electrode assembly evaluation catalytic perfomance, mould concurrently
Intend operating environment and carry out electrochemical property test；
（2）It is molten can be effectively prevented from film in the evaluation for carrying out small organic molecule chemical property for the utility model
Resistance becomes big problem caused by swollen problem；
（3）The utility model can be preferably in simulation practical application mass transfer situation, especially liquid mass transfer state；
（4）The utility model is simple in construction, easy to operate, reduces the waste of catalyst, and cost is cheap.
Brief description of the drawings
The structural representation of Fig. 1 the present utility model in-situ testing device fixtures, 1 film/electrode combination, 2 affluxs
Body, 3 extraction wires, 4 sealing gaskets, 5 electrode fixed plates.
The structural representation of the section components overlapping of Fig. 2 the present utility model in-situ testing device fixtures, it is preceding：Sealing
Pad, after：Reference electrode and to electrode lateral electrode fixed plate.
The structural representation of the section components overlapping of Fig. 3 the present utility model in-situ testing device fixtures, it is preceding：Film/electricity
Pole combination, after：Working electrode lateral electrode fixed plate.
The structural representation of the section components overlapping of Fig. 4 the present utility model in-situ testing device fixtures, it is preceding：Film/electricity
Pole combination, in：Working electrode side collector, after：Working electrode lateral electrode fixed plate.
The structural representation of the section components overlapping of Fig. 5 the present utility model in-situ testing device fixtures, it is preceding：Reference electricity
Pole and to electrode side collector, in：Sealing gasket, after：Reference electrode and to electrode lateral electrode fixed plate.
The structural representation of the section components overlapping of Fig. 6 the present utility model in-situ testing device fixtures, it is preceding：Film/electricity
Pole combination, in：Reference electrode and to electrode side collector, after：It is sealing gasket, last：Reference electrode and electrode lateral electrode is consolidated
Fixed board.
Fig. 7 the present utility model test system schematic diagrames, 1 discharging opening, 2 working electrode side connectors, 3 charging apertures, 4
Firm banking, 5 fasteners, 6 in-situ testing device fixtures, 7 references, to electrode side connector, 8 gas vents, 9 gas feeds.
Fig. 8 the present utility model embodiment 1 is used for the test system schematic diagram of room temperature air electrocatalytic reaction, 1 reaction
Gas, 2 gas control valves, 3 gas circuits, 4 humidification devices, 5 in-situ testing device fixtures, 6 hydrogen.
Test system schematic diagram of Fig. 9 the present utility model embodiment 2 and 3 for liquor sample electrocatalytic reaction, 1
Heater, 2 certain density reaction solutions, 3 gas circuits, 4 peristaltic pumps, 5 in-situ testing device fixtures, 6 gas control valves, 7 hydrogen.
Embodiment
The present utility model is described in further detail with reference to specific embodiment, its specific works step is such as
Under：
Embodiment 1 tests oxygen reduction reaction in the electrolyte of Nafion 115
A. the preparation of electrolyte substrate：The polytetrafluoroethylene film thick by the use of 30 microns, will as electrolyte base material
It cuts the shape as 60mm*60mm, then carves out two 5mm*5mm hole, spacing therebetween therebetween
Control is in 5mm；Then it is in the clean film both sides of Nafion 115, hot pressing pressure by the polytetrafluoroethylene film hot pressing prepared
10MPa, hot pressing time 180s.
B. working electrode, reference electrode are identical with the catalyst pulp to electrode.Its compound method is：Claimed with one-level balance
20%Pt/C catalyst 5mg are taken, add 50 microlitres of 5%Nafion solution and 950 microlitres of ethanol, ultrasonic mixing to Pt/C is in solution
In it is dispersed.
C. the preparation of solid electrolyte electrode：The catalyst pulp configured is added dropwise in counter electrode position respectively, its
Middle working electrode is added dropwise 5 microlitres, and after its drying, electrolyte substrate is overturn, and to electrode being added dropwise 10 microlitres, reference electrode drips
Add 5 microlitres.
D. the installation of in-situ testing device fixture：5mm*20mm is cut into as collector, working electrode side using carbon paper
Shape, reference, the L shape that wide 10mm under wide 5mm* on high 20mm* is cut into electrode side；Using diameter 0.5mm Pt silks
As electrode extraction wire；The sealing gasket of corresponding bore hole size is made using thickness 1mm Silicone Rubber；Will be solid by Fig. 1 order
Body electrolyte-electrode, collector, extraction wire and sealing gasket are arranged between positive and negative electrode fixed plate, use fastened by screw.
E. the test of oxygen reduction reaction：By the in-situ testing device fixture prepared installation in a test system, exist first
Working electrode and nitrogen 30min is each led into electrode side with the oxygen in removing device, be then passed through 35 in working electrode side
DEG C humidification air, flow velocity is 2 Lmin-1, hydrogen is being passed through to electrode side, flow velocity is 300 mLmin-1, connection electrification
Learn work station and carry out the electrochemical property tests such as cyclic voltammetric, AC impedance.
Embodiment 2 tests methanol electro-oxidizing reaction in the electrolyte of Nafion 115
A. the preparation of electrolyte substrate：The polytetrafluoroethylene film thick by the use of 30 microns, will as electrolyte base material
It cuts the shape as 60mm*60mm, then carves out two 5mm*5mm hole, spacing therebetween therebetween
Control is in 5mm；Then it is in the clean film both sides of Nafion 115, hot pressing pressure by the polytetrafluoroethylene film hot pressing prepared
10MPa, hot pressing time 180s.
B. working electrode catalyst utilizes 20%Pt10%Ru/C, is 20%Pt/C to electrode and reference electrode catalyst, it is matched somebody with somebody
Method processed is：Weighed with one-level balance and weigh catalyst 5mg respectively, add 50 microlitres of 5%Nafion solution and 950 microlitres of second
Alcohol, ultrasonic mixing solution to catalyst are dispersed in the solution.
C. the preparation of solid electrolyte electrode：The catalyst pulp configured is added dropwise in counter electrode position respectively, its
5 microlitres of 20%Pt10%Ru/C catalyst pulps are added dropwise in middle working electrode, after its drying, electrolyte substrate are overturn, to electricity
10 microlitres of 20%Pt/C catalyst pulps are added dropwise in pole, and 5 microlitres of 20%Pt/C catalyst pulps are added dropwise in reference electrode.
D. the installation of in-situ testing device fixture：5mm*20mm is cut into as collector, working electrode side using carbon paper
Shape, reference, the L shape that wide 10mm under wide 5mm* on high 20mm* is cut into electrode side；Using diameter 0.5mm Pt silks
As electrode extraction wire；The sealing gasket of corresponding bore hole size is made using thickness 1mm Silicone Rubber；Will be solid by Fig. 1 order
Body electrolyte-electrode, collector, extraction wire and sealing gasket are arranged between positive and negative electrode fixed plate, use fastened by screw.
E. the test of methanol electro-oxidizing reaction：By the in-situ testing device fixture prepared installation in a test system, to
1M methanol solution is added in working electrode side, then using nitrogen deoxygenation 30min, is passed through nitrogen 30min to electrode side to remove
Oxygen in device, then peristaltic pump is utilized to be passed through hydrogen to electrode side, flow velocity is with mass transfer enhancement in working electrode side
300mL/min, connection electrochemical workstation carry out the electrochemical property tests such as cyclic voltammetric, AC impedance.
Embodiment 3 tests the electrolysis evolving hydrogen reaction of water in the dielectric film electrolytic cells of Nafion 115
A. the preparation of electrolyte substrate：The polytetrafluoroethylene film thick by the use of 30 microns, will as electrolyte base material
It cuts the shape as 60mm*60mm, then carves out two 5mm*5mm hole, spacing therebetween therebetween
Control is in 5mm；Then it is in the clean film both sides of Nafion 115, hot pressing pressure by the polytetrafluoroethylene film hot pressing prepared
10MPa, hot pressing time 180s.
B. working electrode, identical with reference electrode catalyst pulp to electrode, its compound method is：Weighed with one-level balance
20%Pt/C catalyst 5mg, 50 microlitres of 5%Nafion solution and 950 microlitres of ethanol are added, ultrasonic mixing to Pt/C is in the solution
It is dispersed.
C. the preparation of solid electrolyte electrode：The catalyst pulp configured is added dropwise in counter electrode position respectively, its
Middle working electrode is added dropwise 5 microlitres, and after its drying, electrolyte substrate is overturn, and to electrode being added dropwise 10 microlitres, reference electrode drips
Add 5 microlitres.
D. the installation of in-situ testing device fixture：5mm*20mm is cut into as collector, working electrode side using carbon paper
Shape, reference, the L shape that wide 10mm under wide 5mm* on high 20mm* is cut into electrode side；Using diameter 0.5mm Pt silks
As electrode extraction wire；The sealing gasket of corresponding bore hole size is made using thickness 1mm Silicone Rubber；Will be solid by Fig. 1 order
Body electrolyte-electrode, collector, extraction wire and sealing gasket are arranged between positive and negative electrode fixed plate, use fastened by screw.
E. the test of evolving hydrogen reaction：By the in-situ testing device fixture prepared installation in a test system, it is connected to survey
Test system, distilled water is added to working electrode side, then using nitrogen deoxygenation 30min, electrode side is passed through nitrogen 30min with except
The oxygen gone in device, then peristaltic pump is utilized to be passed through hydrogen to electrode side, flow velocity is with mass transfer enhancement in working electrode side
300 mL·min-1, connect electrochemical workstation and carry out the electrochemical property tests such as chrono-amperometric, AC impedance.
Claims (9)
1. a kind of in-situ test fixture and system for solid polymer electrolyte system, it is characterised in that in-situ test fills
Fixture is put to include：Composite micro-electrode film/electrode combination（1）, collector（2）, extraction wire（3）, sealing gasket（4）Consolidate with electrode
Fixed board（5）；In-situ testing device fixture by working electrode side and reference, electrode side connector sealed, connected, with grinding
Study carefully electrode reaction solution or gas and reference electrode, the supply to electrode reaction gas, processing, circulation and tapping equipment are formed and surveyed
Test system；
Described composite micro-electrode film/electrode combination（1）Both sides be provided with collector（2）And extraction wire（3）, reference electricity
Pole, sealing gasket is set to electrode side（4）, with electrode fixed plate（5）It is integrally fixed, it is attached in test system and connects electricity
Chem workstation carries out the test of chemical property.
2. a kind of in-situ test fixture and system for solid polymer electrolyte system according to claim 1, its
It is characterised by：Composite micro-electrode film/electrode combination（1）It is the polytetrafluoroethyl-ne that will be carved with required electrode shape and area hole
Alkene film is placed in solid polymer dielectric film both sides and hot pressing, and the slurry of catalyst to be measured is then added dropwise on the working electrode (s,
To Pt/C catalyst pulps are added dropwise on electrode and reference electrode, reference electrode is used as by the use of reversible hydrogen electrode.
3. a kind of in-situ test fixture and system for solid polymer electrolyte system according to claim 1, its
It is characterised by：Collector（2）Selected according to different research objects；The reduction of oxidation reaction, oxygen for hydrogen is anti-
Should, organic molecule methanol and the electro-oxidation reaction of formic acid and the electrolysis evolving hydrogen reaction of water, using carbon paper or carbon cloth as collection
Fluid；Electrolysis oxygen evolution reaction for water, titanium net can be used as collector.
4. a kind of in-situ test fixture and system for solid polymer electrolyte system according to claim 1, its
It is characterised by：Collector（2）Electrode surface is covered in, and is fully contacted with extraction wire.
5. a kind of in-situ test fixture and system for solid polymer electrolyte system according to claim 1, its
It is characterised by：In composite micro-electrode film/electrode combination（1）Collector is respectively arranged with the counter electrode of both sides（2）And extraction
Wire（3）, then it is placed on reference electrode, sealing gasket is added with to electrode side（4）Two pieces of electrode fixed plates（5）In be used in combination
Fastened by screw.
6. a kind of in-situ test fixture and system for solid polymer electrolyte system according to claim 1, its
It is characterised by：In electrode fixed plate（5）On, set respectively in " field " with working electrode, and the position contacted to electrode, reference electrode
Font hole so that reactant smoothly reaches electrode surface, while has part sheet material to be compressed on electrode surface to reduce the molten of film
Bulging deformation.
7. a kind of in-situ test fixture and system for solid polymer electrolyte system according to claim 1, its
It is characterised by：Electrode fixed plate（5）Material for polytetrafluoroethylene (PTFE), bakelite, thickness 5-10mm.
8. a kind of in-situ test fixture and system for solid polymer electrolyte system according to claim 1, its
It is characterised by：In-situ testing device fixture in working electrode side and reference, be glass to the material of electrode side connector, with electrode
Fixed plate（5）The port of contact is ground.
9. a kind of in-situ test fixture and system for solid polymer electrolyte system according to claim 1, its
It is characterised by：Test system is selected according to different research objects, for the electrocatalytic reaction using gas as research object,
The oxidation of hydrogen and the reduction of oxygen, working electrode is directly purged using the gas of certain humidity；For using liquid as research pair
The electrocatalytic reaction of elephant, organic molecule methanol, the electroxidation of formic acid, electrolysis liberation of hydrogen, the oxygen evolution reaction of water, is entered using peristaltic pump
Liquid flowing in the simulation practical operation of row liquid circulation.
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| CN201720702942.3U CN206848208U (en) | 2017-06-16 | 2017-06-16 | A kind of in-situ test fixture and system for solid polymer electrolyte system |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107014884A (en) * | 2017-06-16 | 2017-08-04 | 济南大学 | A kind of in-situ test fixture and system for solid polymer electrolyte system |
| CN110146821A (en) * | 2019-05-27 | 2019-08-20 | 清华大学深圳研究生院 | Battery tester and its application method |
-
2017
- 2017-06-16 CN CN201720702942.3U patent/CN206848208U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107014884A (en) * | 2017-06-16 | 2017-08-04 | 济南大学 | A kind of in-situ test fixture and system for solid polymer electrolyte system |
| CN110146821A (en) * | 2019-05-27 | 2019-08-20 | 清华大学深圳研究生院 | Battery tester and its application method |
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