CN106596686B - A kind of evaluating apparatus and evaluation method for solid polymer electrolyte fuel cell and water electrolysis elctro-catalyst performance - Google Patents
A kind of evaluating apparatus and evaluation method for solid polymer electrolyte fuel cell and water electrolysis elctro-catalyst performance Download PDFInfo
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- CN106596686B CN106596686B CN201610924577.0A CN201610924577A CN106596686B CN 106596686 B CN106596686 B CN 106596686B CN 201610924577 A CN201610924577 A CN 201610924577A CN 106596686 B CN106596686 B CN 106596686B
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- G—PHYSICS
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- 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
- G01N27/403—Cells and electrode assemblies
- G01N27/406—Cells and probes with solid electrolytes
Abstract
The present invention relates to a kind of evaluating apparatus and evaluation method for solid polymer electrolyte fuel cell and water electrolysis elctro-catalyst performance, belong to elctro-catalyst activity rating technical field.The technical problem for solving in now widely used liquid three-electrode system evaluation method that technique is cumbersome, required catalyst is more, of high cost, influence factor is complicated in elctro-catalyst local environment and practical application different problems and assembled battery evaluation method etc..Membrane electrode assembly is miniaturized the evaluating apparatus, and it adds reversible hydrogen electrode and tests electrocatalysis characteristic as reference electrode, the advantages of combining now widely used liquid three-electrode system and membrane electrode evaluation catalytic performance, and makes catalyst is in solid polymer electrolyte to measure its electrocatalysis characteristic, preferably simulate the catalytic performance test under actual application environment.The evaluation method can be accurate and effective evaluation be used for polymer electrolyte fuel cells and water electrolysis elctro-catalyst performance.
Description
Technical field
The invention belongs to elctro-catalyst activity rating technical fields, and in particular to one kind is fired for solid polymer electrolyte
Expect the evaluating apparatus and evaluation method of battery and water electrolysis elctro-catalyst performance.
Background technology
Solid polymer has been widely used as a kind of safety, environmentally protective electrolyte in fuel electricity
In pond and water electrolysis.In order to improve electrocatalysis characteristic and reduce catalyst cost, cost-effective elctro-catalyst becomes to be ground at present
One of Main way studied carefully.So a kind of effective catalytic performance test method is highly important.
Currently, for catalyst performance evaluation method there are two types of, one is liquid electrolyte three-electrode systems, that is, use
The certain density aqueous solution of acid or alkali is loaded with catalyst glass-carbon electrode and carries out elctro-catalyst as working electrode as electrolyte
The evaluation of performance.Although the evaluation method system is simple, swift and convenient to operate, catalyst usage amount is few, at low cost, with reality
The gap of border operating environment is larger, as electrolyte phase and type are different, the difference of solid solid interface and solid liquid interface compatibility, and
And solion may have an impact elctro-catalyst performance evaluation can not accurately evaluate the performance of elctro-catalyst.
Another method is exactly that assembled battery carries out performance evaluation, and this method is that commenting for battery performance is carried out under cell operating conditions
Valence can comprehensively evaluate the catalytic performance of elctro-catalyst, but the technique of assembled battery is cumbersome, required catalyst is more,
It is of high cost, influence factor is complicated, electrocatalysis characteristic depends on Multiple factors, such as bipolar plates, flow path designs.
Invention content
The invention solves elctro-catalyst local environment in now widely used liquid three-electrode system evaluation method with
Technique is cumbersome in practical application different problems and assembled battery evaluation method, required catalyst is more, of high cost, influence factor
The technical problem of complexity etc., provide it is a kind of prepare be simple and convenient to operate, be of low cost, can simulated operation environment, be used for solid
The evaluating apparatus and evaluation method of polymer electrolyte fuel cells and water electrolysis elctro-catalyst performance.
In order to solve the above-mentioned technical problem, technical scheme of the present invention is specific as follows:
A kind of evaluating apparatus for solid polymer electrolyte fuel cell and water electrolysis elctro-catalyst performance, including:
Collector, hydrophobic substrate membrane material, amberplex, catalyst pulp and conducting wire;
The both sides of the amberplex are provided with the hydrophobic group counterdie for the hole for carving out required electrode shape and area
Material, wherein side are working electrode, and the other side is to electrode and reference electrode, and working electrode is opposite with to electrode;
The catalyst pulp is added dropwise on the exposed amberplex of respective electrode;And it is solid respectively at three electrode
Surely upper collector;
Solid electrolyte electrode is become using conductive glue connection collector and wire producing;
The solid electrolyte electrode is mounted in test fixture, and the conducting wire picked out is connected to electrochemical workstation and carries out electricity
Chemical property is tested.
In the above-mentioned technical solutions, the hydrophobic substrate membrane material is polytetrafluoroethylene (PTFE) or polyether-ether-ketone.
In the above-mentioned technical solutions, the electrode shape is round or square.
In the above-mentioned technical solutions, the working electrode area is less than 1cm2, and working electrode is not less than to electrode area
Area.
In the above-mentioned technical solutions, the collector is carbon paper, carbon cloth or metal mesh.
In the above-mentioned technical solutions, the test fixture includes containing there are two the ground container and fastener of feed inlet, institutes
It states fastener to be fixed on solid electrolyte electrode among two opposite ground containers, the ground container upper end of working electrode side
There are one air inlet and inlet, side is there are one gas outlet, and to the ground container upper end of electrode side, there are one air inlet, sides
There are one gas outlets.
A kind of evaluation method for solid polymer electrolyte fuel cell and water electrolysis elctro-catalyst performance, including with
Lower step:
A. the preparation of electrolyte substrate
The hole for carving out required electrode shape and area respectively on two hydrophobic substrate membrane materials, then by hydrophobic group
Base film material distinguishes hot pressing and forms electrolyte substrate, hot pressing pressure 10MPa in the both sides of amberplex, and hot pressing time is
180s;
B. working electrode is prepared, to the catalyst pulp of electrode and reference electrode;
C. the preparation of solid electrolyte electrode
It is added dropwise respectively in counter electrode position by prepared working electrode, to the catalyst pulp of electrode and reference electrode
It sets, collector is cut into required shape, then hot pressing respectively uses conductive glue connection collector and lead at corresponding electrode
Line, which makes, becomes solid electrolyte electrode;
D. electrocatalysis characteristic is tested
The solid electrolyte electrode prepared is mounted in test fixture, the conducting wire picked out is connected to electrochemical workstation
Carry out electrochemical property test.
In the above-mentioned technical solutions, when the electrochemical property test is the test of hydroxide reaction, working electrode side
It is passed through H2;
Or the electrochemical property test, when being that organic molecule electroxidation is tested, working electrode side is respectively certain dense
The organic molecule solution of degree;
Or the electrochemical property test be oxygen reduction reaction test when, working electrode side is passed through O2;
Or the electrochemical property test be water electrolysis catalyst performance evaluation when, working electrode side be distilled water.
In the above-mentioned technical solutions, the catalyst pulp by catalyst, ion exchange electrolyte and dispersion solvent according to
Ratio mixes.
In the above-mentioned technical solutions, the catalyst loading on the working electrode is not more than 100 μ g cm-2, described to electrode
The catalyst used with reference electrode is platinum black or platinum carbon, using reversible hydrogen electrode as reference electrode.
The beneficial effects of the invention are as follows:
1, provided by the present invention for the evaluation of solid polymer electrolyte fuel cell and water electrolysis elctro-catalyst performance
Membrane electrode assembly is miniaturized device, and adds reversible hydrogen electrode and test electrocatalysis characteristic as reference electrode, combines at present
The advantages of widely used liquid three-electrode system and membrane electrode evaluation catalytic performance, and catalyst is made to be in solid polymerization
Its electrocatalysis characteristic is measured in object electrolyte, preferably simulates the catalytic performance test under actual application environment.
2, provided by the present invention for the evaluation of solid polymer electrolyte fuel cell and water electrolysis elctro-catalyst performance
Device, it is simple in structure, it is easy to operate, the waste of catalyst is reduced, it is of low cost.
3, provided by the present invention for the evaluation of solid polymer electrolyte fuel cell and water electrolysis elctro-catalyst performance
Method can be accurate and effective evaluation electrocatalysis characteristic in operating condition, simply and easily have rated catalyst in ion
The performance in solid electrolyte is exchanged, its comprehensive performance evaluation in practical applications is conducive to.
Description of the drawings
Invention is further described in detail with reference to the accompanying drawings and detailed description.
Fig. 1 is solid electrolyte electrode side view provided by the invention.
Fig. 2 is the front view of solid electrolyte electrode tow sides provided by the invention.
Fig. 3 is commenting provided by the present invention for solid polymer electrolyte fuel cell and water electrolysis elctro-catalyst performance
A kind of structural schematic diagram of valence device.
Reference numeral in figure is expressed as:
1- collectors, 2- hydrophobic substrates membrane material, 3- amberplexes, 4- catalyst pulps, 5- conducting wires, 4-1- are to electrode
Catalyst pulp, 4-2- reference electrodes catalyst pulp, 4-3- working electrodes catalyst pulp, 6- to electrode side, 7- fasteners,
8- solid electrolytes electrode, 9- working electrodes side, 10- air inlets, the gas outlets 11-, 12- magnetons, 13- inlets.
Specific implementation mode
The present invention is described in detail below in conjunction with the accompanying drawings.
Referring to attached drawing 1-3:One kind provided by the invention is urged for solid polymer electrolyte fuel cell and water electrolysis electricity
The evaluating apparatus of agent performance is urged using solid polymer electrolyte design microelectrode under the conditions of simulation practical operation
Change performance test.The evaluating apparatus includes:It collector 1, hydrophobic substrate membrane material 2, amberplex 3, catalyst pulp 4 and leads
Line 5;The both sides of the amberplex 3 are provided with the hydrophobic substrate membrane material for the hole for carving out required electrode shape and area
2, wherein side is working electrode, and the other side is to electrode and reference electrode, and working electrode is opposite with to electrode;The catalysis
Agent slurry 4 is added dropwise on the exposed amberplex 3 of respective electrode;And fix upper collector 1 respectively at three electrode;It adopts
Being made of conductive glue connection collector 1 and conducting wire 5 becomes solid electrolyte electrode 8;The solid electrolyte electrode 8, which is mounted on, to be surveyed
It tries in fixture, the conducting wire 5 picked out is connected to electrochemical workstation and carries out electrochemical property test.Attached drawing 2 is solid electrolyte electricity
The front view of pole tow sides shows in figure and has been added dropwise at three electrodes to electrode catalyst slurry 4-1, reference electrode catalyst
Design sketch after slurry 4-2, working electrode catalyst pulp 4-3.The hydrophobic substrate membrane material 2 is chemical and electrochemically stable
Good, the heat safe high score membrane material of property, preferably polytetrafluoroethylene (PTFE) or polyether-ether-ketone.The electrode shape it is generally circular or
Square.The electrode area can need to be adjusted according to experiment, in order to ensure that test result, working electrode area are general
Less than 1cm2, and working electrode area is not less than to electrode area.It is described to electrode and reference electrode in the same side, the two it
Between there are certain distances.The collector 1 is carbon paper, carbon cloth or metal mesh.A kind of concrete structure of the test fixture
For:Include containing there are two the ground container of feed inlet and fastener 7, solid electrolyte electrode 8 is fixed on phase by the fastener 7
To two ground containers among, there are one air inlet 10 and inlets 13 for the ground container upper end of working electrode side 9, and side has
One gas outlet 11, to the ground container upper end of electrode side 6 there are one air inlet 10, there are one gas outlets 11 for side.In reference
Electrode side is passed through hydrogen, and working electrode side 9 is determined according to test event and environment.When being evaluated for the electrocatalysis characteristic of liquid,
Magnetic agitation Accelerative mass transfer need to be carried out in working electrode side 9 with magneton 12;When being evaluated for gaseous electrocatalysis characteristic, work electricity
Pole side 9 is passed through the gas with certain humidity.
A kind of evaluation method for solid polymer electrolyte fuel cell and water electrolysis elctro-catalyst performance, including with
Lower step:
A. the preparation of electrolyte substrate
The hole for carving out required electrode shape and area respectively on two hydrophobic substrate membrane materials 2, then will be hydrophobic
Basement membrane material 2 distinguishes hot pressing and forms electrolyte substrate, hot pressing pressure 10MPa, hot pressing time in the both sides of amberplex 3
For 180s;
B. working electrode is prepared, to the catalyst pulp of electrode and reference electrode;
C. the preparation of solid electrolyte electrode 8
It is added dropwise respectively in counter electrode position by prepared working electrode, to the catalyst pulp of electrode and reference electrode
Set, collector be cut into required shape, respectively hot pressing at corresponding electrode, then use conductive glue connection collector 1 with
Conducting wire 5, which makes, becomes solid electrolyte electrode 8;
D. electrocatalysis characteristic is tested
The solid electrolyte electrode 8 prepared is mounted in test fixture, the conducting wire 5 picked out is connected to electrochemical operation
It stands and carries out electrochemical property test.
The electrocatalysis characteristic test is the test for hydroxide reaction, and working electrode side is passed through H2;For methanol,
The organic molecules electroxidation such as ethyl alcohol, formic acid is tested, and working electrode side is respectively that certain density methanol, ethyl alcohol, formic acid are molten
Liquid;Test for oxygen reduction reaction, working electrode side are passed through O2;Evaluation for water electrolysis catalyst performance, work electricity
Pole side is distilled water etc..
The catalyst pulp is proportionally mixed by catalyst, ion exchange electrolyte and dispersion solvent, ratio
Example relationship is related to catalyst type.The catalyst used to electrode and reference electrode is platinum catalyst, specially platinum black
Or platinum carbon, using reversible hydrogen electrode as reference electrode.Catalyst loading on the working electrode is not more than 100 μ g cm-2。
Embodiment 1 tests oxygen reduction reaction in 115 electrolyte of Nafion
A. the preparation of electrolyte substrate:Using the polytetrafluoroethylene film of 30 μ m-thicks as electrolyte base material, by it
The shape as 6cm*6cm is cut, the hole of two 5mm*5mm, spacing between the two control are then carved out among one
In 5mm;Then by the polytetrafluoro film hot-pressing prepared in the clean 115 film both sides Nafion, hot pressing pressure 10MPa, heat
The pressure time is 180s.
B. working electrode, identical with reference electrode catalyst pulp to electrode, preparation method is:It is weighed with level-one balance
20%Pt/C catalyst 5mg add 50 μ L 5%Nafion solution and 950 μ L ethyl alcohol, and ultrasonic mixing solution to Pt/C is in solution
In it is evenly dispersed.
C. the preparation of solid electrolyte electrode:The catalyst pulp configured is added dropwise respectively in counter electrode position,
5 μ L are added dropwise in middle working electrode, and after its drying, electrolyte substrate is overturn, and 10 μ L are added dropwise to electrode, 5 μ are added dropwise in reference electrode
L.Using carbon paper as collector, it is cut into the shape of 5mm*20mm, hot pressing is at corresponding electrode respectively, hot pressing condition
For 10MPa, 30s.Then conducting resinl is utilized to draw the conducting wire of each electrode position.
D. the test of oxygen reduction reaction:The solid electrolyte electrode prepared is mounted in test fixture, first in work
Make electrode and nitrogen 30min is each led into the oxygen in removing device to electrode side, is then passed through 35 DEG C in working electrode side
The air of humidification, flow velocity 2L/min are being passed through hydrogen to electrode side, flow velocity 300mL/min, connection electrochemical workstation into
The electrochemical property tests such as row cyclic voltammetric, AC impedance.
Embodiment 2 tests methanol electro-oxidizing reaction in 115 electrolyte of Nafion
A. the preparation of electrolyte substrate:Using the polytetrafluoroethylene film of 30 μ m-thicks as electrolyte base material, by it
The shape as 6cm*6cm is cut, the hole of two 5mm*5mm, spacing between the two control are then carved out among one
In 5mm;Then by the polytetrafluoro film hot-pressing prepared in the clean 115 film both sides Nafion, hot pressing pressure 10MPa, heat
The pressure time is 180s.
B. working electrode catalyst utilizes 20%Pt10%Ru/C, is 20%Pt/C to electrode and reference electrode catalyst,
Its preparation method is:It is weighed with level-one balance and weighs catalyst 5mg respectively, add 50 μ L 5%Nafion solution and 950 μ L second
Alcohol, ultrasonic mixing solution are evenly dispersed in the solution to catalyst.
C. the preparation of solid electrolyte electrode:The catalyst pulp configured is added dropwise respectively in counter electrode position,
5 μ L 20%Pt10%Ru/C catalyst pulps are added dropwise in middle working electrode, after its drying, electrolyte substrate are overturn, to electricity
10 μ L 20%Pt/C catalyst pulps are added dropwise in pole, and 5 μ L 20%Pt/C catalyst pulps are added dropwise in reference electrode.Using carbon paper conduct
Collector is cut into the shape of 5mm*20mm, and hot pressing is at corresponding electrode respectively, hot pressing condition 10MPa, 30s.So
Conducting resinl is utilized to draw the conducting wire of each electrode position afterwards.
D. the test of oxygen reduction reaction:The solid electrolyte electrode prepared is mounted in test fixture, to work electricity
The methanol solution of 1M is added in pole side, then utilizes nitrogen deoxygenation 30min, nitrogen 30min is passed through in removing device to electrode side
Oxygen, then working electrode side using rotation magneton mass transfer enhancement, hydrogen, flow velocity 300mL/ are being passed through to electrode side
Min, connection electrochemical workstation carry out the electrochemical property tests such as cyclic voltammetric, AC impedance.
Embodiment 3 tests water electrolysis evolving hydrogen reaction in the electrolysis of Nafion 115
A. the preparation of electrolyte substrate:Using the polytetrafluoroethylene film of 30 μ m-thicks as electrolyte base material, by it
The shape as 6cm*6cm is cut, the hole of two 5mm*5mm, spacing between the two control are then carved out among one
In 5mm;Then by the polytetrafluoro film hot-pressing prepared in the clean 115 film both sides Nafion, hot pressing pressure 10MPa, heat
The pressure time is 180s.
B. working electrode, identical with reference electrode catalyst pulp to electrode, preparation method is:It is weighed with level-one balance
20%Pt/C catalyst 5mg add 50 μ L 5%Nafion solution and 950 μ L ethyl alcohol, and ultrasonic mixing solution to Pt/C is in solution
In it is evenly dispersed.
C. the preparation of solid electrolyte electrode:The catalyst pulp configured is added dropwise respectively in counter electrode position,
5 μ L are added dropwise in middle working electrode, and after its drying, electrolyte substrate is overturn, and 10 μ L are added dropwise to electrode, 5 μ are added dropwise in reference electrode
L.Using carbon paper as collector, it is cut into the shape of 5mm*20mm, hot pressing is at corresponding electrode respectively, hot pressing condition
For 10MPa, 30s.Then conducting resinl is utilized to draw the conducting wire of each electrode position.
D. the test of oxygen reduction reaction:The solid electrolyte electrode prepared is mounted in test fixture, to work electricity
Distilled water is added in pole side, then utilizes nitrogen deoxygenation 30min, and nitrogen 30min is passed through with the oxygen in removing device to electrode side,
Then hydrogen, flow velocity 300mL/min, connection are being passed through to electrode side using rotation magneton mass transfer enhancement in working electrode side
Electrochemical workstation carries out the electrochemical property tests such as chrono-amperometric, AC impedance.
The polytetrafluoroethylene film may be replaced by polyether-ether-ketone or other chemistry and electrification in the above-described embodiments
Have good stability, heat safe high score membrane material, and the collector can also use carbon cloth or metal mesh etc., the electrode shape
Shape can also be circle etc., no longer enumerate here.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (9)
1. a kind of evaluating apparatus for solid polymer electrolyte fuel cell and water electrolysis elctro-catalyst performance, feature exists
In, including:Collector (1), hydrophobic substrate membrane material (2), amberplex (3), catalyst pulp (4) and conducting wire (5);
The both sides of the amberplex (3) are provided with the hydrophobic substrate membrane material for the hole for carving out required electrode shape and area
Expect (2), wherein side is working electrode, and the other side is to electrode and reference electrode, and working electrode is opposite with to electrode;
The catalyst pulp (4) is added dropwise on the exposed amberplex of respective electrode (3);And it is fixed respectively at three electrodes
Upper collector (1);
Being made of conductive glue connection collector (1) and conducting wire (5) becomes solid electrolyte electrode;
The solid electrolyte electrode is mounted in test fixture, and the conducting wire (5) picked out is connected to electrochemical workstation and carries out electricity
Chemical property is tested;
The test fixture includes containing there are two the ground container and fastener (7) of feed inlet, and the fastener (7) is electric by solid
Solution matter electrode (8) is fixed among two opposite ground containers, and there are one air inlets for the ground container upper end of working electrode side (9)
Mouthful (10) and inlet (13), side is there are one gas outlet (11), to air inlet there are one the ground container upper ends of electrode side (6)
(10), there are one gas outlets (11) for side.
2. evaluating apparatus according to claim 1, which is characterized in that the hydrophobic substrate membrane material (2) is polytetrafluoroethyl-ne
Alkene or polyether-ether-ketone.
3. evaluating apparatus according to claim 1, which is characterized in that the electrode shape is round or square.
4. evaluating apparatus according to claim 1, which is characterized in that the working electrode area is less than 1cm2, and to electrode
Area is not less than working electrode area.
5. evaluating apparatus according to claim 1, which is characterized in that the collector (1) is carbon paper, carbon cloth or metal
Net.
6. a kind of evaluation method for solid polymer electrolyte fuel cell and water electrolysis elctro-catalyst performance, including it is following
Step:
A. the preparation of electrolyte substrate
The hole for carving out required electrode shape and area respectively on two hydrophobic substrate membrane materials (2), then by hydrophobic group
Hot pressing forms electrolyte substrate, hot pressing pressure 10MPa, when hot pressing to base film material (2) in the both sides of amberplex (3) respectively
Between be 180s;
B. working electrode is prepared, to the catalyst pulp of electrode and reference electrode;
C. the preparation of solid electrolyte electrode (8)
It is added dropwise respectively in counter electrode position by prepared working electrode, to the catalyst pulp of electrode and reference electrode, it will
Collector (1) is cut into required shape, respectively hot pressing at corresponding electrode, then use conductive glue connection collector (1) with
Conducting wire (5), which makes, becomes solid electrolyte electrode (8);
D. electrocatalysis characteristic is tested
The solid electrolyte electrode (8) prepared is mounted in test fixture, the conducting wire (5) picked out is connected to electrochemical operation
It stands and carries out electrochemical property test.
7. evaluation method according to claim 6, which is characterized in that the electrochemical property test is hydroxide reaction
When test, working electrode side is passed through H2;
Or the electrochemical property test be organic molecule electroxidation test when, working electrode side is respectively certain density
Organic molecule solution;
Or the electrochemical property test be oxygen reduction reaction test when, working electrode side is passed through O2;
Or the electrochemical property test be water electrolysis catalyst performance evaluation when, working electrode side be distilled water.
8. evaluation method according to claim 6, which is characterized in that the catalyst pulp is by catalyst, ion exchange
Electrolyte and dispersion solvent proportionally mix.
9. according to the evaluation method described in claim 6-8 any one, which is characterized in that the catalyst on the working electrode
Carrying capacity is not more than 100 μ g cm-2, the catalyst that electrode and reference electrode are used for platinum black or platinum carbon, use reversible hydrogen electricity
Pole is as reference electrode.
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