CN109406593A - Electrochemical in-situ reacts X ray test device - Google Patents
Electrochemical in-situ reacts X ray test device Download PDFInfo
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- CN109406593A CN109406593A CN201811143429.0A CN201811143429A CN109406593A CN 109406593 A CN109406593 A CN 109406593A CN 201811143429 A CN201811143429 A CN 201811143429A CN 109406593 A CN109406593 A CN 109406593A
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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
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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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
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/301—Reference electrodes
Abstract
The invention belongs to electrochemical technology fields, are related to a kind of electrochemical in-situ reaction X ray test device, are mainly made of electrochemical reaction room and working electrode lid；Working electrode lid is mounted on the upper end of electrochemical reaction room；Electrochemical reaction chamber interior is equipped with working electrode, to electrode and reference electrode, and working electrode is covered equipped with test window and duct.Active material to be tested is coated in working electrode top, without using metal collector, the problems such as absorption so as to avoid collector to X-ray, X-ray signal is weak, and as a result accuracy is low.The device of the invention have it is small in size, structure is simple, assemble it is convenient, it is reusable the features such as.The present invention can carry out follow-on test to same pole piece, gained map signal-to-noise ratio is high, working electrode currents even density, and test potential is accurate, it is tested suitable for two electrode systems and three-electrode system, and shows extremely excellent accuracy and stability in aqueous electrolyte.
Description
Technical field
The invention belongs to electrochemical technology fields, are related to a kind of electrochemical in-situ reaction X ray test device.
Background technique
As global environmental pollution and energy crisis are increasingly serious, exploitation clean and effective energy storage device is extremely urgent.It can fill
Battery is because having the features such as high efficiency energy storage, high security, environment friendly, it is considered to be most potential energy stores
System.Important component of the electrode material as battery, largely determines the overall performance of rechargeable battery.
In charge and discharge process, a series of physical and chemical change, such as phase transformation and structure cracking can occur for electrode material.
These variations will affect the chemical property of rechargeable battery, or even play a decisive role.In-situ TiC particles technology is as current energy storage
Important analysis means in area research, it can not only exclude the influence that extraneous factor generates electrode material, improve monitoring number
According to authenticity and reliability, can also carry out real-time monitoring to the electrochemical process of electrode material, and disclose its intrinsic reaction machine
System.In-situ TiC particles (XRD, that is, X-ray diffractometer) measuring technology is a kind of X ray test technology with fastest developing speed at present.In short
It, in-situ TiC particles are to make sample motionless, measure same sample spreading out under different conditions (such as temperature, Current Voltage, atmosphere etc.)
Penetrate map.The advantages of in-situ test, is constantly monitor the variation that sample is occurred when condition changes, can truly react
The actual change of system under prescribed conditions.Therefore, in-situ TiC particles characterization technique can truly monitor sample interior structure with reaction
The introducing of the variation of condition (temperature, Current Voltage, atmosphere), can promote our understandings to the intrinsic energy storage mechanism of electrode material,
And the development that will quickly push high-performance energy storage device.
In-situ TiC particles technology can be used for studying the mechanism of reaction, the specific generating process of phase transformation and the catalysis of catalyst
Mechanism etc..Therefore, the test function of Extended X-ray diffractometer is developed, increases in-situ TiC particles measuring technology to research reaction power
, electrode process, catalytic mechanism and interfacial reaction have great importance.
For study battery material its structure change in charge and discharge process, in-situ TiC particles method need not pause charge and discharge and
Battery is dismantled, thus can accurately measure current potential and variation of the follow-on test electrode material crystal structure in charge and discharge process,
In-situ TiC particles technology is to confirm that material is conducive to Electrode mistake with the presence or absence of the powerful measure of phase transformation in electrode charge and discharge process
The mechanism of journey.
For in-situ TiC particles reaction chamber, the in situ X-ray diffraction electrolytic cell for having Bruker company to produce being commercialized at present is tested
Instrument reaction chamber, it is the reaction chamber for being specially designed to carry out in situ X-ray diffraction diffraction experiment, but it is expensive, maintenance
It is inconvenient, it is often more important that, when it tests water system battery, under the conditions of applied voltage, electrolyte Yi Yuqi electrolytic cell hair
Raw reaction, influences the accuracy of its test result.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of electrochemical in-situ reaction X ray test device.Especially when it
When testing water system battery or water system capacitor, excellent homogeneity and stability are shown.The prior art can be supplemented in water system
Its electrochemical signals inaccuracy leads to the insincere factor of test result under electrolyte.It is same that the present invention is applicable not only to aqueous electrolyte
Sample is also applied for organic electrolyte and ionic liquid.
Technical solution of the present invention:
A kind of electrochemical in-situ reaction X ray test device, is mainly made of electrochemical reaction room 9 and working electrode lid 1；
The working electrode lid 1 is mounted on the upper end of electrochemical reaction room 9；
The electrochemical reaction room 9 is the hollow cylindrical structure of upper end opening, and bottom is set there are three threaded
Through-hole, for installment work electrode 4, to electrode 6 and reference electrode 8；The working electrode 4, to electrode 6 and reference electrode 8,
The lower end of three is mounted in the threaded through-hole of electrochemical reaction room 9, and bottom end is located at outside electrochemical reaction room 9,
Remaining part quartile is in contact in the inside of electrochemical reaction room 9 with electrolyte；The bottom of the working electrode 4 is connected with work
Electrode terminal 5, the bottom to electrode 6 are connected with to electrode terminal 7, and the bottom of the reference electrode 8 connects
There is a reference electrode binding post, working electrode binding post 5, to electrode terminal 7 and reference electrode binding post and electrochemical workstation
It is connected；
The working electrode lid 1 be it is discoid, connect with the threaded upper ends of electrochemical reaction room 9；Working electrode lid 1
Test window 2 is equipped at center, test window 2 is located at the top of working electrode 4, film, work to be tested are posted on test window 2
Property material be coated in 4 top of working electrode, and it is seamless between 4 top of the lower surface of film and working electrode；On working electrode lid 1
Equipped with duct 3, duct 3 is located at 8 top of reference electrode, for injecting electrolyte；
When carrying out the in-situ TiC particles test of three-electrode system, working electrode 4 works to electrode 6 and reference electrode 8；When
When carrying out the in-situ TiC particles test of two electrode systems, reference electrode 8 is dismantled, and block 9 bottom of electrochemical reaction room with sealing-plug
For installing the through-hole of reference electrode 8.
The material of the electrochemical reaction room 9 and working electrode lid 1 is polytetrafluoroethylene (PTFE).
The material of film on the test window 2 is Kapton.
When electrolyte is water system, working electrode 4 is glass-carbon electrode.
The working electrode 4, to being cased with rubber at the connector of electrode 6 and reference electrode 8 and electrochemical reaction room 9
Circle, prevents electrolyte loss.
Described is platinum electrode or graphite electrode to electrode 6.
Described replaces electrode 6 and the experimental specific requirement of reference electrode 8.
Beneficial effects of the present invention:
1, the configuration of the present invention is simple, it is small in size, be easily assembled to and dismantle, is light easy to carry, cheap, and the present invention
In without using diaphragm and collector.
2, the present invention is suitable for the in-situ TiC particles test of two electrode systems and three-electrode system, especially when test water system electricity
When solving liquid, extremely excellent accuracy and stability are shown.The present invention is not only applicable to aqueous electrolyte, equally applicable
In other type electrolyte.
3, the present invention can control electric current and voltage simultaneously；X-ray transparent test window is mapped on active material to be measured,
Then it being reflected on the detector of XRD, detector again reflects its signal intensity onto computer in the form of XRD spectrum, thus
Accurately test out the minor change that sample occurs in electrochemical process.
4, the present invention can carry out follow-on test to same pole piece, and gained map signal-to-noise ratio is high, and working electrode currents density is equal
Even, test potential is accurate.
Detailed description of the invention
Fig. 1 is the schematic diagram of apparatus of the present invention；
Fig. 2 (a) is that existing in-situ TiC particles electrolytic cell tests acidic electrolysis bath CV schematic diagram data；
Fig. 2 (b) is the CV schematic diagram data that apparatus of the present invention are tested under the same electrolyte of same material；
Fig. 3 (a) is that apparatus of the present invention test Ti3C2In-situ TiC particles schematic diagram data under acidic electrolysis bath；
Fig. 3 (b) is that apparatus of the present invention test V2In-situ TiC particles schematic diagram data of the C under acidic electrolysis bath；
Fig. 4 (a) is that apparatus of the present invention test V2In-situ TiC particles schematic diagram data of the C under neutral electrolyte；
Fig. 4 (b) is that apparatus of the present invention test V2In-situ TiC particles schematic diagram data of the C under alkaline electrolyte.
In figure: 1 working electrode lid；2 test windows；3 ducts；4 working electrodes；5 working electrode binding posts；6 pairs of electrodes；7
To electrode terminal；8 reference electrodes；9 electrochemical reaction rooms.
Specific embodiment
Below in conjunction with attached drawing and technical solution, a specific embodiment of the invention is further illustrated.
As shown in Figure 1, a kind of electrochemical in-situ of the present invention reacts X ray test device, including electrochemical reaction
Working electrode 4 is arranged, to electrode 6 and reference electrode 8 in room 9 and working electrode lid 1, the inside of electrochemical reaction room 9.Working electrode
Lid 1 is located at the upper end of electrochemical reaction room 9.
The electrochemical reaction room 9 is in hollow cylindrical, and upper surface, which is equipped with, connect required spiral shell with working electrode lid 1
Line.
The working electrode 4, to electrode 6 and reference electrode 8, be connected by screw thread with the bottom of electrochemical reaction room 9
It connects, preferably can be cased with rubber ring at its connector prevents electrolyte loss.
The electrochemical reaction room 9 is connected with 1 the two of electrode work lid by screw thread, in electrode work lid 1
Test window 2 is provided at the heart.The underface of test window 2 is working electrode 4, is coated between working electrode 4 and test window 2
Active material to be measured, without gap and without diaphragm between working electrode 4 and test window 2.
Described can carry out any change, such as the platinum and valence of optional stable operating voltage according to experiment to electrode 6
The cheap graphite rod etc. of lattice.Its reference electrode 8 similarly, can carry out any change according to experiment type.
The electrochemical reaction room 9 and electrolyte contacts part, is not necessarily to metal connection column, avoids aqueous electrolyte and exist
A series of side reaction occurs with electrolyte under conditions of applied voltage, keeps measurement result more accurate.
A circular duct 3 can be opened on the working electrode lid 1, and injection system can be used to be added needed for electrochemical process
Electrolyte.
Posted on the test window 2 under X-ray diffraction without dephasign peak and cheap polyimide film.
The electrochemical reaction room 9 and working electrode lid 1 is made with polytetrafluoroethylene (PTFE) (PTEE) material.
In the present invention without using collector, directly active material to be measured can be born by the modes such as coating or depositing
It is downloaded on working electrode 4；When using collector, collector can absorb a large amount of X-ray signal, so in existing original position
In XRD electrolytic cell, it has to the extremely strong metallic beryllium of at high price and toxicity is used, to enhance X-ray signal.
Assembled chemical reaction chamber 9 is fixed on to the sample stage position of X-ray diffractometer.Then successively start X-ray
Diffractometer and electrochemical workstation, and relevant parameter is set by test request, it is tested.
It is tested shown in CV data such as Fig. 2 (a) under acidic electrolysis bath using existing in-situ TiC particles electrolytic cell；Use the present invention
Shown in CV data such as Fig. 2 (b) under the same electrolyte of device to test same material.
Ti is tested using apparatus of the present invention3C2Shown in in-situ TiC particles data such as Fig. 3 (a) under acidic electrolysis bath；Use this
Invention device tests V2Shown in the in-situ TiC particles data such as Fig. 3 (b) of C under acidic electrolysis bath.
V is tested using apparatus of the present invention2Shown in the in-situ TiC particles data such as Fig. 4 (a) of C under neutral electrolyte；Use this hair
Bright device to test V2Shown in the in-situ TiC particles data such as Fig. 4 (b) of C under alkaline electrolyte.
Claims (10)
1. a kind of electrochemical in-situ reacts X ray test device, which is characterized in that the test device is mainly anti-by electrochemistry
Room (9) and working electrode lid (1) is answered to form；The working electrode lid (1) is mounted on the upper end of electrochemical reaction room (9)；
The electrochemical reaction room (9) is the hollow cylindrical structure of upper end opening, and bottom is set to be led to there are three threaded
Hole, for installment work electrode (4), to electrode (6) and reference electrode (8)；The working electrode (4), to electrode (6) and ginseng
Than electrode (8), the lower end of three is mounted in the threaded through-hole of electrochemical reaction room (9), and to be located at electrochemistry anti-for bottom end
Answer room (9) external, rest part is located at the inside of electrochemical reaction room (9), is in contact with electrolyte；The working electrode
(4) bottom is connected with working electrode binding post (5), and the bottom to electrode (6) is connected with to electrode terminal (7),
The bottom of the reference electrode (8) is connected with reference electrode binding post, working electrode binding post (5), to electrode terminal (7)
It is connected with reference electrode binding post with electrochemical workstation；
The working electrode lid (1) be it is discoid, connect with the threaded upper ends of electrochemical reaction room (9)；Working electrode lid (1)
Center at be equipped with test window (2), test window (2) is located at the top of working electrode (4), and test window posts film on (2),
Active material to be tested is coated in working electrode (4) top, and seamless between the lower surface of film and working electrode (4) top
Gap；Working electrode lid (1) is equipped with duct (3), and duct (3) are located above reference electrode (8), for injecting electrolyte；
When carrying out the in-situ TiC particles test of three-electrode system, working electrode (4) works to electrode (6) and reference electrode (8)；
When carrying out the in-situ TiC particles test of two electrode systems, reference electrode (8) are dismantled, and block electrochemical reaction room with sealing-plug
(9) bottom is used to install the through-hole of reference electrode (8).
2. a kind of electrochemical in-situ according to claim 1 reacts X ray test device, which is characterized in that the electricity
The material of chemical reaction chamber (9) and working electrode lid (1) is polytetrafluoroethylene (PTFE)；The material of film on the test window (2)
For Kapton.
3. a kind of electrochemical in-situ according to claim 1 or 2 reacts X ray test device, which is characterized in that described
Electrode (6) and reference electrode (8) experimental specific requirement are replaced.
4. a kind of electrochemical in-situ according to claim 1 or 2 reacts X ray test device, which is characterized in that described
It is platinum electrode or graphite electrode to electrode (6).
5. a kind of electrochemical in-situ according to claim 3 reacts X ray test device, which is characterized in that pair
Electrode (6) is platinum electrode or graphite electrode.
6. a kind of according to claim 1, electrochemical in-situ reaction X ray test device described in 2 or 5, which is characterized in that work as electricity
When solution liquid is water system, working electrode (4) is glass-carbon electrode.
7. a kind of electrochemical in-situ according to claim 3 reacts X ray test device, which is characterized in that work as electrolyte
When for water system, working electrode (4) is glass-carbon electrode.
8. a kind of electrochemical in-situ according to claim 4 reacts X ray test device, which is characterized in that work as electrolyte
When for water system, working electrode (4) is glass-carbon electrode.
9. a kind of according to claim 1, electrochemical in-situ reaction X ray test device described in 2,5,7 or 8, which is characterized in that
The working electrode (4), to being cased with rubber at the connector of electrode (6) and reference electrode (8) and electrochemical reaction room (9)
Circle, prevents electrolyte loss.
10. a kind of electrochemical in-situ according to claim 6 reacts X ray test device, which is characterized in that the work
Make electrode (4), to rubber ring is cased at the connector of electrode (6) and reference electrode (8) and electrochemical reaction room (9), prevents electricity
Liquid stream is solved to lose.
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| CN201811143429.0A CN109406593B (en) | 2018-09-28 | 2018-09-28 | Electrochemical in-situ reaction X-ray testing device |
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| CN201811143429.0A CN109406593B (en) | 2018-09-28 | 2018-09-28 | Electrochemical in-situ reaction X-ray testing device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110361403A (en) * | 2019-08-20 | 2019-10-22 | 南杰智汇(深圳)科技有限公司 | X-ray diffraction analysis sample stage with three-electrode electro Chemical test function |
| CN110687146A (en) * | 2019-10-14 | 2020-01-14 | 北京工业大学 | X-ray diffraction in-situ testing device for electrochromic film |
| CN113376188A (en) * | 2021-05-12 | 2021-09-10 | 中国科学院高能物理研究所 | In-situ X-ray absorption spectrum measuring system and measuring method |
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| CN113376188B (en) * | 2021-05-12 | 2022-11-01 | 中国科学院高能物理研究所 | In-situ X-ray absorption spectrum measuring system and measuring method |
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