CN109470725A - The synchrotron radiation in-situ testing device of catalyst in fuel cell catalyst layer - Google Patents
The synchrotron radiation in-situ testing device of catalyst in fuel cell catalyst layer Download PDFInfo
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- CN109470725A CN109470725A CN201811051414.1A CN201811051414A CN109470725A CN 109470725 A CN109470725 A CN 109470725A CN 201811051414 A CN201811051414 A CN 201811051414A CN 109470725 A CN109470725 A CN 109470725A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
- G01N23/06—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption
- G01N23/083—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption the radiation being X-rays
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Abstract
The present invention provides a kind of synchrotron radiation in-situ testing devices of catalyst in fuel cell catalyst layer, including synchrotron radiation light source (1), preceding ionisation chamber, pond in situ and rear ionisation chamber or fluorescent probe (7)；X-ray projects premenstrual ionisation chamber from synchrotron radiation light source (1), pond in situ is incident upon on rear ionisation chamber or fluorescent probe (7).The original position pond includes working electrode side, auxiliary electrode side；The working electrode side is connected by through-hole mechanism, connector (15) with auxiliary electrode side.The present invention provides a kind of synchrotron radiation in-situ testing device of catalyst in fuel cell catalyst layer, suitable for the electrocatalytic reaction original position pond of in-situ synchronization radiation XAFS detection, to realize the crucial technical problem that real-time detection catalyst structure develops.
Description
Technical field
The present invention relates to, and in particular, to the synchrotron radiation in-situ test dress of catalyst in a kind of fuel cell catalyst layer
It sets more particularly to a kind of for the synchrotron radiation in-situ test of catalyst to fill in fuel cell catalyst layer under the effect of certain potential
It sets.
Background technique
Proton Exchange Membrane Fuel Cells is made of cathode catalysis layer, proton exchange membrane, anode catalyst layer, and wherein Catalytic Layer is
Core component in electrocatalytic reaction, at be grouped as with microstructure directly affect electrocatalytic reaction activity and energy turn
Change efficiency.During electrocatalytic reaction, researcher generallys use rotating disk electrode (r.d.e) cyclic voltammetry, linear voltammetric scan method
The catalytic activity and stability that catalyst is characterized with AC impedence method, spread out in conjunction with offline transmission electron microscope, X-ray
Penetrate, the methods of x-ray photoelectron spectroscopy and elemental analysis come characterize catalyst at being grouped as and microstructure, established with this
" structure effect " relationship between catalyst macroscopic view catalytic activity and microstructure.And in actual application, the surface of catalyst
At be grouped as with microstructure can with the variation of ambient enviroment (such as: reaction atmosphere, temperature, humidity and potential etc.) and it is real-time
Change.Off-line analysis method is difficult to capture catalyst real-time structure change rule in catalytic reaction process, thus not
It can truly reflect out the mechanism of action of catalyst, and then the catalyst that can not effectively take into account for design activity and stability mentions
For reliable theory support.Synchrotron radiation X-ray Absorption Fine Structure spectroscopy (X-ray Absorption Fine
Structure, XAFS) using a wide range of energy of synchrotron radiation X-ray high signal-to-noise characteristic can be reconciled to study the line of substance
Absorption coefficient with energy changing rule, to obtain absorb atom around Near-neighbor Structure information.It is mainly characterized by having
Element selectivity, and it is special to analyze certain in fuel cell catalyst layer by additional device (such as atmosphere, temperature, potential) in situ
Determine the near neighboring coordination atomic species of element, co-ordination distance, oxidation state and the electronic structure of ligancy and coordination atom etc. in real time
Structural information, for obtain many conventional methods be difficult to or the real-time structural information of substance that can not obtain provide it is extremely advantageous
Condition.
Real-time architecture information based on synchrotron radiation in situ detection catalyst during electrocatalytic reaction, it is necessary to using same
In the x-ray bombardment to membrane electrode in the operating condition for walking high-energy caused by radiating light source, high brightness, then collection membrane
The X-ray absorption signal of element is detected in electrode catalyst.
Summary of the invention
For the defects in the prior art, the object of the present invention is to provide in a kind of fuel cell catalyst layer catalyst it is same
Step radiation in-situ testing device.
The synchrotron radiation in-situ testing device of catalyst in a kind of fuel cell catalyst layer provided according to the present invention, including
Synchrotron radiation light source, preceding ionisation chamber, pond in situ and rear ionisation chamber or fluorescent probe；
X-ray is from synchrotron radiation light source projects premenstrual ionisation chamber, pond in situ is incident upon on rear ionisation chamber or fluorescent probe.
Preferably, the pond in situ includes working electrode side, auxiliary electrode side；
The working electrode side is connected by through-hole mechanism, connector with auxiliary electrode side.
Preferably, the working electrode side includes working electrode side fastening end plate, working electrode side insulation support plate；
The through-hole mechanism includes working electrode side through hole；
Work is provided between the side of the working electrode side fastening end plate, the side of working electrode side insulation support plate
Electrode side gasket；
The side of the working electrode side fastening end plate, the side of working electrode side insulation support plate are provided with position phase
Corresponding working electrode side through hole；
The working electrode side through hole constitutes the mounting hole of connector.
Preferably, the auxiliary electrode side includes auxiliary electrode side fastening end plate, auxiliary electrode side insulation support plate；
The through-hole mechanism includes auxiliary electrode side through hole；
The side of the auxiliary electrode side fastening end plate, the side of auxiliary electrode side insulation support plate are provided with position phase
Corresponding auxiliary electrode side through hole；
The position of the auxiliary electrode side through hole is corresponding with the position of working electrode side through hole of the through-hole mechanism；
The working electrode side passes through mounting hole by connector and is connected with auxiliary electrode side.
Preferably, the middle part of the working electrode side fastening end plate, a middle side part of working electrode side insulation support plate are equal
It is provided with working electrode side insulation support plate groove；
The quantity of the working electrode side is multiple；
Working electrode side insulation support plate groove phase between the middle part of the two neighboring working electrode side fastening end plate
To setting；
Multiple working electrode side insulation support plate grooves constitute the optical module accommodation space of working electrode side.
Preferably, auxiliary electrode side insulation support plate groove is provided in the middle part of the auxiliary electrode side fastening end plate；
Auxiliary electrode side insulation support plate groove is provided in the middle part of the other side of auxiliary electrode side insulation support plate；
The quantity of the auxiliary electrode side is multiple；
Auxiliary electrode side insulating supporting between in the middle part of the other side of two neighboring auxiliary electrode side insulation support plate
Plate groove is oppositely arranged；
Auxiliary electrode side insulation support plate groove is provided in the middle part of two neighboring auxiliary electrode side fastening end plate to set relatively
It sets；
Multiple auxiliary electrode side insulation support plate grooves constitute the optical module accommodation space of auxiliary electrode side；
The working electrode side of the position of the optical module accommodation space of the auxiliary electrode side and the working electrode side
The position of optical module accommodation space be oppositely arranged.
Preferably, the optical module of the working electrode side includes x-ray film, working electrode side seal pad；
The optical module of the working electrode side further includes working electrode side metal collector plate；
The side of the working electrode side seal pad, saturating x-ray film, working electrode side metal collector plate and membrane electrode
It is successively set in the optical module accommodation space of working electrode side.
Preferably, the optical module of the auxiliary electrode side includes that auxiliary electrode side metal collector plate, auxiliary electrode side are close
Packing；
The other side of membrane electrode, the auxiliary electrode side metal collector plate, auxiliary electrode side seal pad are successively set on auxiliary
It helps in the optical module accommodation space of electrode side；
The auxiliary electrode side metal collector plate, working electrode side metal collector plate are provided with external through-hole.
Preferably, it is all provided in the middle part of the middle part of the optical module of the auxiliary electrode side and the optical module of working electrode side
It is equipped with through-hole section；Wherein, the not set through-hole in middle part of the saturating x-ray film in the middle part of the optical module of the working electrode side
Portion；
The middle part of the side of working electrode side fastening end plate, the side of working electrode side insulation support plate middle part,
Through-hole section is provided in the middle part of the side of the auxiliary electrode side fastening end plate；
X-ray is from the through-hole section that synchrotron radiation light source projects premenstrual ionisation chamber, pond in situ is penetrated to rear ionisation chamber or glimmering
On optical detector.
Preferably, the working electrode side fastening end plate, auxiliary electrode side fastening end plate are provided with fastening end plate X-ray
Through window；
The side of working electrode side insulation support plate, the side of auxiliary electrode side insulation support plate are respectively arranged with work
Make electrode side insulation support plate groove, auxiliary electrode side insulation support plate groove；
The other side of the working electrode side fastening end plate, the other side of auxiliary electrode side fastening end plate are respectively arranged with work
Make electrode side insulation support plate X-ray transparent window, auxiliary electrode side insulation support plate X-ray transparent window；
Position, the position of auxiliary electrode side insulation support plate groove, work of the working electrode side insulation support plate groove
Make the position of electrode side insulation support plate X-ray transparent window, the position of auxiliary electrode side insulation support plate X-ray transparent window
It in the same horizontal line or is overlapped, and constitutes optical section；
The position at optics part center in the same horizontal line or is overlapped with the position of through-hole section；
The working electrode insulation support plate is provided with the electrolysis fluid through-hole of working electrode side；
The aperture position of the through-hole is located at the top of working electrode side insulation support plate groove.
Auxiliary electrode side insulation support plate is provided with the electrolyte injection orifice of auxiliary electrode side and reference electrode is placed
Through-hole；
The aperture position that the electrolyte injection orifice and reference electrode of the auxiliary electrode side place through-hole is located at auxiliary electrode
The top of side insulation support plate；
The tail portion outlet port that the electrolyte injection orifice and reference electrode of the auxiliary electrode side place through-hole is respectively positioned on auxiliary
It helps in electrode side insulation support plate groove.
Compared with prior art, the present invention have it is following the utility model has the advantages that
1, the present invention provides a kind of synchrotron radiation in-situ testing device of catalyst in fuel cell catalyst layer, is suitable for original
Bit synchronization radiates the electrocatalytic reaction original position pond of XAFS detection, to realize the key that real-time detection catalyst structure develops
Property technical problem.
2, the synchrotron radiation in-situ testing device of catalyst is used for electro-catalysis in fuel cell catalyst layer provided by the invention
The pond in situ of repercussion study, it is desirable that detection window will not only meet simultaneously to be transmitted and testing under fluorescence mode, but also detects window
Mouthful thickness and material need to avoid as far as possible to generate absorption to X-ray, with the integrality of this XAFS data-signal for ensuring to collect,
Accuracy and reliability.
3, simultaneously, the synchrotron radiation in-situ testing device of catalyst is applicable in fuel cell catalyst layer provided by the invention
It is tested in the In-situ XAFS of variety classes catalyst, sample cell meets replacement sample and assembling sample is simple and convenient, can be convenient
Ground obtains the transmission of certain element to be measured or fluorescent reflection signal in catalyst.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon:
Fig. 1 is the synchrotron radiation X AFS in situ detection device flow diagram provided by the present invention for electrocatalytic reaction.
Fig. 2 is the synchrotron radiation X AFS in situ detection sample cell section signal provided by the present invention for electrocatalytic reaction
Figure.
Fig. 3 is that working electrode side provided by the invention fastens end plate and auxiliary electrode side fastens end plate front and back sides structure chart.
Fig. 4 is the structure chart of working electrode side insulation support plate one side provided by the invention.
Fig. 5 is the structure chart of working electrode side insulation support plate another side provided by the invention.
Fig. 6 is the structure chart of auxiliary electrode side insulation support plate one side provided by the invention.
Fig. 7 is the structure chart of auxiliary electrode side insulation support plate another side provided by the invention.
Fig. 8 is the experimental result of the embodiment of the present invention 1.
Following table is the meaning of each appended drawing reference in Figure of description:
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, several changes and improvements can also be made.These belong to the present invention
Protection scope.
The synchrotron radiation in-situ testing device of catalyst, feature exist in a kind of fuel cell catalyst layer provided by the invention
In, including synchrotron radiation light source 1, preceding ionisation chamber, pond in situ and rear ionisation chamber or fluorescent probe 7；X-ray is from synchrotron radiation
Light source 1 projects premenstrual ionisation chamber, pond in situ is incident upon on rear ionisation chamber or fluorescent probe 7.
The original position pond includes working electrode side, auxiliary electrode side；The working electrode side by through-hole mechanism,
Connector 15 is connected with auxiliary electrode side.
The working electrode side includes working electrode side fastening end plate 11, working electrode side insulation support plate 12；It is described
Through-hole mechanism includes working electrode side through hole 36；The side of the working electrode side fastening end plate 11, working electrode side insulation branch
Working electrode gasket 17 is provided between the side of fagging 12；The side of the working electrode side fastening end plate 11, work electricity
The side of pole side insulation support plate 12 is provided with the corresponding working electrode side through hole 36 in position；The working electrode side through hole
36 constitute the mounting hole of connector 15.
The auxiliary electrode side includes auxiliary electrode side fastening end plate 14, auxiliary electrode side insulation support plate 13；It is described
Through-hole mechanism includes auxiliary electrode side through hole 37；The side of the auxiliary electrode side fastening end plate 14, auxiliary electrode side insulation branch
The side of fagging 13 is provided with the corresponding auxiliary electrode side through hole 37 in position；The position of the auxiliary electrode side through hole 37 with
The position of the working electrode side through hole 36 of the through-hole mechanism is corresponding；The working electrode side passes through peace by connector 15
Dress hole is connected with auxiliary electrode side.
The middle part of the working electrode side fastening end plate 11, a middle side part of working electrode side insulation support plate 12 are respectively provided with
There is working electrode side insulation support plate groove 24；The quantity of the working electrode side is multiple；The two neighboring work electricity
Working electrode side insulation support plate groove 24 between the middle part of pole side fastening end plate 11 is oppositely arranged；Multiple working electrodes
The optical module accommodation space of the composition of side insulation support plate groove 24 working electrode side.
The middle part of the auxiliary electrode side fastening end plate 14 is provided with auxiliary electrode side insulation support plate groove 28；It is described auxiliary
It helps in the middle part of the other side of electrode side insulation support plate 13 and is provided with auxiliary electrode side insulation support plate groove 28；The auxiliary electrode
The quantity of side is multiple；Auxiliary electrode between in the middle part of the other side of two neighboring auxiliary electrode side insulation support plate 13
Side insulation support plate groove 28 is oppositely arranged；The middle part of two neighboring auxiliary electrode side fastening end plate 14 is provided with auxiliary electrode side
Insulation support plate groove 28 is oppositely arranged；Multiple auxiliary electrode side insulation support plate grooves 28 constitute the light of auxiliary electrode side
Learn component accommodation space；The work of the position of the optical module accommodation space of the auxiliary electrode side and the working electrode side
The position of the optical module accommodation space of electrode side is oppositely arranged.
The optical module of the working electrode side includes x-ray film 16, working electrode side seal pad 17；The work
Electrode side gasket 17, saturating x-ray film 16, working electrode side metal collector plate 21, membrane electrode 20 side be successively set on
In the optical module accommodation space of working electrode side.
The optical module of the auxiliary electrode side includes auxiliary electrode side metal collector plate 19, auxiliary electrode side seal pad
18；The optical module of the working electrode side further includes working electrode side metal collector plate 21；The other side of membrane electrode 20, institute
State auxiliary electrode side metal collector plate 19, auxiliary electrode side seal pad 18 be successively set on auxiliary electrode side optical module accommodate
In space；The auxiliary electrode side metal collector plate 19, working electrode side metal collector plate 21 are provided with external through-hole.
The middle part of the optical module of the auxiliary electrode side and the optical module of working electrode side (in addition to saturating x-ray film)
Middle part be provided with through-hole section 34；More specifically；Saturating x-ray film 16 in the optical module of the working electrode side
The not set through-hole section 34 in middle part；And without saturating x-ray film in the optical module of the auxiliary electrode side；The working electrode side is tight
The middle part of the side of fixed end plate 11, the middle part of the side of working electrode side insulation support plate 12, auxiliary electrode side fastening end
Through-hole section 34 is provided in the middle part of the side of plate 14；X-ray is from synchrotron radiation light source 1 projects premenstrual ionisation chamber, pond in situ is penetrated
The through-hole section 34 to rear ionisation chamber or fluorescent probe 7 on.In the side of auxiliary electrode side insulation support plate 13
The not set through-hole section 34 in portion.
Working electrode side fastening end plate 11, that auxiliary electrode side fastening end plate 14 is provided with fastening end plate X-ray is saturating
Cross window 22；The side of working electrode side insulation support plate 12, the side of auxiliary electrode side insulation support plate 13 are set respectively
It is equipped with working electrode side insulation support plate groove 24, auxiliary electrode side insulation support plate groove 28；The working electrode side fastening
The other side of end plate 11, the other side of auxiliary electrode side fastening end plate 14 are respectively arranged with working electrode side insulation support plate X and penetrate
Line penetrates window 25, auxiliary electrode side insulation support plate X-ray transparent window 29；The electrode side insulation support plate groove 24
Position, the position of auxiliary electrode side insulation support plate groove 28, working electrode side insulation support plate X-ray transparent window 25 position
Set, the position of auxiliary electrode side insulation support plate X-ray transparent window 29 in the same horizontal line or is overlapped, and constitute optics
Portion；The position at optics part center in the same horizontal line or is overlapped with the position of through-hole section 34；The working electrode is exhausted
Edge support plate 12 is provided with the electrolysis fluid through-hole 26 of working electrode side；It is exhausted that the aperture position of the through-hole 26 is located at working electrode side
The top of edge support plate 12.
Auxiliary electrode side insulation support plate 13 is provided with the electrolyte injection orifice 30 and reference electrode of auxiliary electrode side
Place through-hole 31；The aperture position that the electrolyte injection orifice 30 and reference electrode of the auxiliary electrode side place through-hole 31 is located at auxiliary
Help the top of electrode side insulation support plate 13；The electrolyte injection orifice 30 and reference electrode of the auxiliary electrode side place through-hole
Tail portion outlet port 32 is respectively positioned in auxiliary electrode side insulation support plate groove 28.The electrolyte injection orifice of the auxiliary electrode side
30, it is bending that reference electrode, which places through-hole 31,.
Below to the synchrotron radiation in-situ testing device of catalyst in fuel cell catalyst layer provided by the invention carry out into
One step explanation:
It is provided by the invention it is a kind of under the effect of certain potential in fuel cell catalyst layer catalyst synchrotron radiation
In-situ testing device, working electrode side fasten end plate 11, working electrode side insulation support plate 12, working electrode side metal collector plate
21, auxiliary electrode side metal collector plate 19, auxiliary electrode side insulation support plate 13, auxiliary electrode side fasten the successively sequence of end plate 14
Overlapping tightens together；
Working electrode side, which fastens, is equipped with through-hole section 34 in the middle part of end plate 11, be convenient for X-ray transparent；Working electrode side metal afflux
A through-hole is equipped in the middle part of plate 21 and auxiliary electrode side metal collector plate 19, by working electrode side collector plate, i.e. working electrode side
Metal collector plate 21 and the external electrochemical workstation of auxiliary electrode side collector plate 19, the pole Catalytic Layer studied using it to needs
Apply potential.
Surface middle part of the working electrode side insulation support plate 12 close to 20 side of membrane electrode is equipped with through-hole section 34, far from film electricity
The surface middle part of 20 side of pole is equipped with working electrode side insulation support plate groove 24；It is close on working electrode side insulation support plate 12
The size of 20 side through-hole section 34 of membrane electrode is less than the ruler far from 20 side working electrode side insulation support plate groove 24 of membrane electrode
It is very little；The electrolysis fluid through-hole 26 of working electrode side, the opening of the through-hole 26 are provided at the top of working electrode side insulation support plate 12
Position is located at the top of working electrode side insulation support plate 12.Gasket, the saturating x-ray film that middle part is equipped with through-hole are sequentially placed
In the insulation support plate groove of working electrode side；The gasket refers to working electrode side seal pad 17.
Surface middle part of the auxiliary electrode side insulation support plate 13 close to 20 side of membrane electrode is equipped with auxiliary electrode side insulation branch
Fagging groove 28, the surface middle part far from 20 side of membrane electrode are equipped with auxiliary electrode side insulation support plate groove 28, in auxiliary electricity
Pole side insulation support plate 13 is put in the auxiliary electrode side insulation support plate groove 28 of the surface middle part of 20 side of membrane electrode
It sets middle part and is equipped with auxiliary electrode side seal pad 18；Auxiliary electrode side insulation support plate 13 is provided with the bending electrolysis of auxiliary electrode side
Liquid injection orifice, i.e. the electrolyte injection orifice 30 and bending reference electrode of auxiliary electrode side place through-hole, i.e. reference electrode is placed logical
Hole 31, the bending electrolyte injection orifice (hereinafter referred to as bending electrolyte injection orifice) and bending reference electrode of the auxiliary electrode side
The aperture position for placing through-hole is located at the top of auxiliary electrode side insulation support plate 13, and bending electrolyte injection orifice and reference are electric
The tail portion outlet port 32 that through-hole is placed in pole is located in auxiliary electrode side insulation support plate groove 28.
The center of working electrode side insulation support plate groove 24 and the centre bit of auxiliary electrode side insulation support plate groove 28
It sets corresponding respectively；And working electrode side insulation support plate is greater than far from the size of 20 side through-hole section 34 of membrane electrode close to film electricity
The size of 20 side working electrode side insulation support plate groove 24 of pole；Auxiliary electrode side insulation support plate is close to 20 side of membrane electrode
The size of auxiliary electrode side insulation support plate groove 28 is greater than far from 20 side auxiliary electrode side insulation support plate groove of membrane electrode
28 size.
Working electrode side, which fastens, is equipped with working electrode gasket 17 between end plate 11 and working electrode side insulation support plate 12,
Auxiliary electrode side insulation support plate 13 and auxiliary electrode side collector plate are equipped with auxiliary that is, between auxiliary electrode side metal collector plate 19
Electrode side gasket 18.Through-hole section 34, and auxiliary electrode side seal pad 18 are designed among auxiliary electrode side metal collector plate 19
Through-hole section 34 size be greater than working electrode side seal pad 17 through-hole section 34 size.
Working electrode side insulation support plate 12, auxiliary electrode side insulation support plate 13 and working electrode side fasten end plate
11, the fastening corresponding position of end plate 14 in auxiliary electrode side is equipped with a circle screw and wears mouth, i.e. working electrode side through hole 36, auxiliary
Electrode side through hole 37.In other words, 12 surface of working electrode side insulation support plate, working electrode side fastening end plate 11 are provided with
Working electrode side through hole 36；Auxiliary electrode side insulation support plate 13, auxiliary electrode side fastening end plate 14 are provided with auxiliary electrode
Side through hole 37；The position of both the working electrode side through hole 36, auxiliary electrode side through hole 37 is mutual corresponding.
The working electrode side fastening end plate 11 in the original position pond, working electrode side insulation support plate 12, auxiliary electrode side are exhausted
Edge support plate 13,14 middle part of auxiliary electrode side fastening end plate all open up groove, and the center of groove is overlapped or is located at same
On one horizontal line.And their frame sizes having the same and corresponding screw perforation size；They are connected using screw rod
When getting up, it can guarantee that the intermediate groove center position for X-ray transparent is overlapped or is located at same horizontal line, guarantee X
Ray can be irradiated on membrane electrode 20.The groove opened up refers to that working electrode side insulation support plate groove 24, auxiliary are electric
Pole side insulation support plate groove 28；The potential in pond in situ is controlled using the metal collector plate of connection electrochemical workstation.
The original position pond is placed in synchrotron radiation X-ray Absorption Fine Structure spectrum (X-ray Absorption Fine
Structure, XAFS) in line station, the X-ray that synchrotron radiation light source issues enters the preceding ionization at XAFS line station by monochromator
Room, after be irradiated on membrane electrode 20, and by transmission or reflection mode mode reach after ionisation chamber or fluorescence detector 7, pass through
The transmission of each element to be measured or fluorescence XAFS signal in sample are collected, that is, realizes catalyst structure during electrocatalytic reaction
In-situ test；Synchrotron radiation issue X-ray pass through preceding ionisation chamber, after by working electrode side fasten 11 through-hole section of end plate
34, the through-hole section 34 of working electrode side seal pad 17, the through-hole section of saturating x-ray film 16, working electrode side insulation support plate 12
34,21 through-hole of working electrode side metal collector plate is irradiated on membrane electrode 20；
The synchrotron radiation in-situ testing device of catalyst is to be irradiated to film electricity in fuel cell catalyst layer provided by the invention
X-ray on pole 20 preferably has there are two types of light emission mode: one is pass through auxiliary electrode side metal afflux in transmission mode
The through-hole section 34 of plate 19, the through-hole section 34 of auxiliary electrode side seal pad 18, auxiliary electrode side insulation support plate 13 auxiliary electrode
The rear ionisation chamber at the through-hole arrival synchrotron radiation X AFS line station of side insulation support plate groove 28, auxiliary electrode side fastening end plate 14；
One is pass through working electrode side metal collector plate through-hole, working electrode side insulation support plate through-hole, saturating X in a manner of reflection to penetrate
Line film, working electrode side seal pad through-hole, working electrode side fastening end plate through-hole reach fluorescence detector.
Below to the synchrotron radiation in-situ testing device of catalyst in fuel cell catalyst layer provided by the invention carry out into
One step explanation, following for a kind of preference of the present invention:
Test the X-ray absorption fine structure of Proton Exchange Membrane Fuel Cells cathode Pt/C catalyst Pt under running conditions
Spectrum.Catalytic Layer is sprayed on film both sides using electrostatic spray, wherein auxiliary electrode, i.e. catalyst used in auxiliary electrode portion are
Pd/C catalyst, working electrode, i.e. catalyst used in working electrode portion are Pt/C catalyst, and proton exchange membrane is Du Pont
Nafion211.Utilize the XAFS signal of transmission mode original position pond detection working electrode Pt/C catalyst Pt.The assembling in pond in situ
Journey is as follows: processing a 3cm in 12 side of working electrode insulation support plate2Square groove, other side be machined with diameter be 5cm
Circular groove, be sequentially placed x-ray film 16 in circular groove, 3cm is opened in centre2The gasket of through-hole, the gasket refer to work
Make electrode side gasket 17, auxiliary electrode side seal pad 18；Then placing outer rim is 9cm*9cm, intermediate aperture 3cm2Through-hole
Working electrode side stainless steel fasten end plate；In auxiliary electrode side, 13 side of insulation support plate is machined with the circle that diameter is 5cm
Slot is machined with 3cm in the other side2Square groove, the square groove, circular groove refer to be auxiliary electrode side insulation support plate groove 28；
4cm is opened among placing in circular groove2The gasket of through-hole；Working electrode side fastening end plate 11, work are successively fastened using screw rod
Electrode side insulation support plate 12, working electrode side metal collector plate 21, assembled membrane electrode 20, auxiliary electrode side metal afflux
Plate 19, auxiliary electrode side insulation support plate, auxiliary electrode side fasten end plate 14, are then placed in nut and tighten to guarantee pond in situ not
Leakage；0.1M HClO is injected to 20 two sides of membrane electrode respectively4Solution, logical close to 13 top bending of auxiliary electrode side insulation board
Ag/AgCl reference electrode is inserted into hole；Apply different potentials to working electrode using electrochemical workstation, among pond in situ
Groove as detection window detection working electrode Pt/C catalyst Pt XAFS signal.It can be observed that with the increasing of potential
Add, the white line peak intensity of Pt gradually increases in Pt/C catalyst, and the oxidation state of Pt gradually rises, illustrate catalyst Pt surface with
The raising of potential can adsorption of oxygenates kind.The groove of the centre refers to working electrode side insulation support plate groove 24, work electricity
Pole side insulation support plate X-ray transparent window 25, auxiliary electrode side insulation support plate groove 28 and auxiliary electrode side insulation branch
Fagging X-ray transparent window 29.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make a variety of changes or modify within the scope of the claims, this not shadow
Ring substantive content of the invention.In the absence of conflict, the feature in embodiments herein and embodiment can any phase
Mutually combination.
Claims (10)
1. the synchrotron radiation in-situ testing device of catalyst in a kind of fuel cell catalyst layer, which is characterized in that including synchronous spoke
Penetrate light source (1), preceding ionisation chamber, pond in situ and rear ionisation chamber or fluorescent probe (7)；
X-ray projects premenstrual ionisation chamber from synchrotron radiation light source (1), pond in situ is incident upon on rear ionisation chamber or fluorescent probe (7).
2. the synchrotron radiation in-situ testing device of catalyst, feature in fuel cell catalyst layer according to claim 1
It is, the original position pond includes working electrode side, auxiliary electrode side；
The working electrode side is connected by through-hole mechanism, connector (15) with auxiliary electrode side.
3. the synchrotron radiation in-situ testing device of catalyst, feature in fuel cell catalyst layer according to claim 2
It is, the working electrode side includes working electrode side fastening end plate (11), working electrode side insulation support plate (12)；
The through-hole mechanism includes working electrode side through hole (36)；
It is provided between the side of working electrode side fastening end plate (11), the side of working electrode side insulation support plate (12)
Working electrode side seal pad (17)；
The side of working electrode side fastening end plate (11), the side of working electrode side insulation support plate (12) are provided with position
Set corresponding working electrode side through hole (36)；
The working electrode side through hole (36) constitutes the mounting hole of connector (15).
4. the synchrotron radiation in-situ testing device of catalyst, feature in fuel cell catalyst layer according to claim 2
It is, the auxiliary electrode side includes auxiliary electrode side fastening end plate (14), auxiliary electrode side insulation support plate (13)；
The through-hole mechanism includes auxiliary electrode side through hole (37)；
The side of auxiliary electrode side fastening end plate (14), the side of auxiliary electrode side insulation support plate (13) are provided with position
Set corresponding auxiliary electrode side through hole (37)；
The position of the auxiliary electrode side through hole (37) and the position of working electrode side through hole (36) of the through-hole mechanism are opposite
It answers；
The working electrode side passes through mounting hole by connector (15) and is connected with auxiliary electrode side.
5. the synchrotron radiation in-situ testing device of catalyst, feature in fuel cell catalyst layer according to claim 3
It is, the middle part of working electrode side fastening end plate (11), a middle side part of working electrode side insulation support plate (12) are all provided with
It is equipped with working electrode side insulation support plate groove (24)；
The quantity of the working electrode side is multiple；
Working electrode side insulation support plate groove between the middle part of two neighboring working electrode side fastening end plate (11)
(24) it is oppositely arranged；
Multiple working electrode side insulation support plate grooves (24) constitute the optical module accommodation space of working electrode side.
6. the synchrotron radiation in-situ testing device of catalyst, feature in fuel cell catalyst layer according to claim 4
It is, is provided with auxiliary electrode side insulation support plate groove (28) in the middle part of auxiliary electrode side fastening end plate (14)；
Auxiliary electrode side insulation support plate groove is provided in the middle part of the other side of auxiliary electrode side insulation support plate (13)
(28)；
The quantity of the auxiliary electrode side is multiple；
Auxiliary electrode side insulating supporting between in the middle part of the other side of two neighboring auxiliary electrode side insulation support plate (13)
Plate groove (28) is oppositely arranged；
Auxiliary electrode side insulation support plate groove (28) phase is provided in the middle part of two neighboring auxiliary electrode side fastening end plate (14)
To setting；
Multiple auxiliary electrode side insulation support plate grooves (28) constitute the optical module accommodation space of auxiliary electrode side；
The light of the working electrode side of the position of the optical module accommodation space of the auxiliary electrode side and the working electrode side
The position for learning component accommodation space is oppositely arranged.
7. the synchrotron radiation in-situ testing device of catalyst, feature in fuel cell catalyst layer according to claim 5
It is, the optical module of the working electrode side includes x-ray film (16), working electrode side seal pad (17)；
The optical module of the working electrode side further includes working electrode side metal collector plate (21)；
The working electrode side seal pad (17), saturating x-ray film (16), working electrode side metal collector plate (21) and film electricity
The side of pole (20) is successively set in the optical module accommodation space of working electrode side.
8. the synchrotron radiation in-situ testing device of catalyst in fuel cell catalyst layer according to claim 5 or 6, special
Sign is that the optical module of the auxiliary electrode side includes auxiliary electrode side metal collector plate (19), auxiliary electrode side seal pad
(18)；
The other side of membrane electrode (20), the auxiliary electrode side metal collector plate (19), auxiliary electrode side seal pad (18) are successively
It is arranged in the optical module accommodation space of auxiliary electrode side；
The auxiliary electrode side metal collector plate (19), working electrode side metal collector plate (21) are provided with external through-hole.
9. the synchrotron radiation in-situ testing device of catalyst, feature in fuel cell catalyst layer according to claim 8
It is, is provided with through-hole section in the middle part of the middle part of the optical module of the auxiliary electrode side and the optical module of working electrode side
(34)；Wherein, the not set through-hole section in middle part of the saturating x-ray film (16) in the middle part of the optical module of the working electrode side
(34)；(note: auxiliary electrode side does not have x-ray film, only the not set through-hole section 34 of auxiliary electrode side insulation support plate)
In the middle part of side of working electrode side fastening end plate (11), the side of working electrode side insulation support plate (12)
Portion, the auxiliary electrode side fastening end plate (14) side in the middle part of be provided with through-hole section (34)；
X-ray from the through-hole section (34) that synchrotron radiation light source (1) projects premenstrual ionisation chamber, pond in situ is penetrated to rear ionisation chamber or
On fluorescent probe (7).
10. the synchrotron radiation in-situ testing device of catalyst, feature in fuel cell catalyst layer according to claim 9
It is, it is saturating that working electrode side fastening end plate (11), auxiliary electrode side fastening end plate (14) are provided with fastening end plate X-ray
Cross window (22)；
The side of working electrode side insulation support plate (12), the side of auxiliary electrode side insulation support plate (13) are respectively set
There are working electrode side insulation support plate groove (24), auxiliary electrode side insulation support plate groove (28)；
The other side of working electrode side fastening end plate (11), the other side of auxiliary electrode side fastening end plate (14) are respectively set
There are working electrode side insulation support plate X-ray transparent window (25), auxiliary electrode side insulation support plate X-ray transparent window
(29)；
The position of the working electrode side insulation support plate groove (24), auxiliary electrode side insulation support plate groove (28) position
It sets, the position of working electrode side insulation support plate X-ray transparent window (25), auxiliary electrode side insulation support plate X-ray transparent
The position of window (29) in the same horizontal line or is overlapped, and constitutes optical section；
The position at optics part center in the same horizontal line or is overlapped with the position of through-hole section (34)；
The working electrode insulation support plate (12) is provided with the electrolysis fluid through-hole (26) of working electrode side；
The aperture position of the through-hole (26) is located at the top of working electrode side insulation support plate (12).
Auxiliary electrode side insulation support plate (13) is provided with the electrolyte injection orifice (30) and reference electrode of auxiliary electrode side
It places through-hole (31)；
The aperture position that the electrolyte injection orifice (30) and reference electrode of the auxiliary electrode side place through-hole (31) is located at auxiliary
The top of electrode side insulation support plate (13)；
The tail portion outlet port (32) that the electrolyte injection orifice and reference electrode of the auxiliary electrode side place through-hole is respectively positioned on auxiliary
It helps in electrode side insulation support plate groove (28).
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