CN109856115A - The device of in-situ test can be carried out to metal ion battery - Google Patents
The device of in-situ test can be carried out to metal ion battery Download PDFInfo
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- CN109856115A CN109856115A CN201910110436.9A CN201910110436A CN109856115A CN 109856115 A CN109856115 A CN 109856115A CN 201910110436 A CN201910110436 A CN 201910110436A CN 109856115 A CN109856115 A CN 109856115A
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Abstract
The invention patent discloses a kind of device that in-situ test can be carried out to metal ion battery, belong to battery material test equipment and research field, the present apparatus can carry out optical microscopy and Confocal laser-scanning microscopy test in situ to metal ion battery during charge discharge, tracking can also be sampled to the variation of gas generated in charge and discharge process and electrolyte, simultaneously a required gas test environment can be provided to the test of metal ion battery, reduce the resistance of device by the design of positive fixinig plate, improve sensitivity and repeatability, the present apparatus is conducive to collect optical signalling to greatest extent, performance for Electrode material provides information, with easy for assemble or unload, the advantages that suitable for in-situ observation in long-term cyclic process.
Description
Technical field
The present invention relates to carry out optics and Raman light in situ to the electrode material of metal ion battery in electrochemical process
Test apparatus field is composed, also includes the alkali metal such as sodium ion and potassium ion, alkaline-earth metal electricity especially for lithium ion battery
The electrode material in pond carries out optics and Raman spectrum test in situ.
Background technique
Lithium ion battery is widely used in Portable movable electronic equipment at present, with the development of New Energy Industry and right
The increasingly increase of the demand of green clean energy resource, it is cheap, performance stablize, cycle performance it is excellent can charge-discharge battery skill
Art, including lithium ion battery and other high-capacity battery technologies, it has also become section produces the most important thing ground.How the property of battery is improved
Can be to reach people to battery capacity, the urgent problem to be solved of the demand of battery life and battery cost.High capacity high-performance
Can the progress of charge-discharge battery technology depend on to novel metal ion battery (including sodium ion, magnesium ion and aluminium ion electricity
Pond) and metal-air battery research.Electrode material be can charge-discharge battery important component, to electrode material in electrification
The physical structure in charge and discharge process is learned, chemical component and stress carry out system and comprehensively studies, to electrode material in charge and discharge
Differentiation and agine mechaism in the process is explored, and is the premise for further increasing battery performance.Currently, to metal ion battery
Research means are mostly ex situs, i.e., cannot constantly be detected to variation of the electrode material in charge and discharge process, and are needed
Battery is opened when charge and discharge are to certain phase, the electrode material of the inside is studied, during the test, electrode material with
Moisture content and oxygen in air will continue to be reacted, or change the physicochemical properties of intermediate product by self-discharge processes,
To seriously affect the authenticity of experimental result.More accurate data will be provided by carrying out on-spot study to metal ion battery,
And the research and development of the relevant apparatus of on-spot study can be carried out to metal ion battery also in the initial stage, such as publication No. is CN
The Chinese invention patent of 108344781 A discloses a kind of " battery tester ", and the device is by utilizing its upper cover, pedestal
And the centerbody being suspended among pedestal is that three electrodes carry out charge and discharge research to electrode material therein.Such device is measuring
When be affected by environment and self-resistance, while the sealing means of form provided by the patent there are gas leakage can
Can property, made in the way of boss and washer mutually insulated between electrode in the way of may be only available for the electrode materials of specific thicknesses
Material.So can accurately regulate and control the charge and discharge process of metal ion battery by three-electrode method, it can be with system coordination electrode
Space length between the material and device for carrying out optics and Raman spectrum test in situ on this basis still lacks.To sum up institute
It states, carrying out in-situ test to battery electrode material is to study the effective research means for how further increasing battery performance, at present
The research and development of the in-situ testing device of metal ion battery have just been started, there are still problems, therefore there is an urgent need to one kind can
The charge and discharge process of metal ion battery is accurately controlled, and the performance with high reproducibility can be carried out to electrode material
Test, and the structure of device is simply easy to be assembled in glove box, the dress that device air-tightness is high, disassembly, cleaning are easy to maintain
It sets and optic test and Raman spectrum test in situ is carried out to metal ion battery.
Summary of the invention
To achieve the above object, the technical solution adopted by the present invention is that: building can carry out light in situ to metal ion battery
The device of test is learned, wherein cabinet includes upper and lower two parts, pedestal and the seat of honour, forms cavity for electrode material by O-type sealing ring
Material is sealed, while three identical fixing screws will be consolidated by bolt of lower base hole and seat of honour bolt hole by box main body is tested
It is fixed;Test box can provide two electrodes and three electrode two ways and carry out charge and discharge to battery material, have cathode in front of pedestal thus
Interface, right front portion are equipped with reference electrode interface, and test box seat of honour right front portion is equipped with anode interface, and three interfaces have cylinder
Or hexagonal column connected in star, for being attached with the banana plug being separately equipped with, banana plug is connected with external electrochemical workstation,
For accurately controlling electric current and voltage, reference electrode interface passes through reference electrode connecting column with cathode interface respectively and connect with cathode
Column with place reference electrode material in the cavity and negative electrode material is connected, anode interface passes through spill anode fixinig plate and placement
Positive electrode in the cavity is connected;The seat of honour is equipped with one or two multifunctional gas/liquid displacement open channel, can be used as
Gas/liquid inlet and outlet are sampled tracking, and another configuration to the variation of gas generated in charge and discharge process and electrolyte
Liquid/gas transfer device be used cooperatively, or with sealing bolt closing passage formed closed environment;Circle is provided at the top of the seat of honour
Shape window opening, in order to the disengaging of light/laser, for acquiring optics or raman spectral signal, form passes through interchangeable glass
Piece and O-type sealing ring are by box sealing.Above-mentioned cabinet has one or two multifunctional gas/liquid displacement opening logical
Road can detect the airtight performance of cavity, it is possible to provide the gas circuit of gas collecting, it is possible to provide the access of electrolyte acquisition, it can
The access of addition electrolyte is provided, by closing external valve, it is possible to provide the space of gas storage is suitable for metal ion battery
In-situ test under particular atmosphere.Multifunctional gas/liquid displacement open channel, positioned at the side wall of cabinet, height and electrode
Material is close, and progress is closed in the form of crimp contact, and in the case where not needing to carry out gas/liquid exchange, channel can
To close to form closed environment with sealing bolt.
Above-mentioned positive fixinig plate is concave structure, and circular open is arranged at bottom, and positive electrode is placed in concave inside, and anode is solid
Stator and the distance between reference electrode connecting column and cathode connecting column can pass through reference electrode connecting column and cathode connecting column
Height be adjusted, provide the space length of optimization for electrode material.
The device of above-mentioned test has reference electrode, the setting of three electrode of positive electrode and negative electrode, in use, three can be carried out
The electrochemistry experiment of electrode is tested, and the experiment test of two electrode electro Chemicals can also be carried out.Electrode interface be suitably inserted into banana plug with
External circuit connection can carry out the constantly regulation of Current Voltage to tested electrode material.
Reference electrode connecting column is annular in the device of above-mentioned test, annular reference electrode can be placed above, and is joined
It can come than the distance between electrode and cathode connecting column by adjusting the size of reference electrode connecting column and cathode connecting column real
It is existing.
Seat of honour medium design in above-mentioned test device has circular window opening and borosilicate glass, quartz, blue
The made sight glass of the multiple materials such as jewel is used cooperatively, and is tested for optic test and Raman spectrum, the window opening
Size can be sealed by the O-ring between sight glass and the seat of honour, sight glass and institute from 1 millimeter to 15 millimeter
The electrode material of research is in contact, and the minimum range between electrode material and the optical microscopy objective lens configured is only to regard
The thickness of glass pane is conducive to collect optical signalling to greatest extent, improves sensitivity.
The invention has the advantages that two electrodes or three electrode charge and discharges can be carried out to electrode material in closed cabinet
Electricity regulation, and by the test of window structure progress optics in situ and Raman spectrum above cabinet, reference electrode area is big, with
The distance between cathode is adjustable according to experiment needs, can obtain accurate voltage signal, the electrode material suitable for different-thickness
Test, the minimum range between electrode material and the optical microscopy objective lens configured is only the thickness of sight glass,
Be conducive to collect optical signalling to greatest extent, improve sensitivity, it can be in case by multifunctional gas/liquid displacement open channel
One controllable measurement atmosphere is provided in vivo, and the addition and taking-up of electrolyte can be carried out, can also be carried out in particular atmosphere
The test of lower metal ion battery.
Detailed description of the invention
The invention patent is further described with reference to the accompanying drawings and examples.
Fig. 1 is the schematic diagram of device involved by this patent;
Fig. 2 is the top view of device involved by this patent;
Fig. 3 is the schematic diagram along line A-A in Fig. 2;
Fig. 4 is the schematic diagram along line B-B in Fig. 2;
Fig. 5 is the chassis interior schematic diagram of device involved by this patent.
Fig. 6 is that there are two top views when multifunctional gas/liquid displacement open channel for the tool of device involved by this patent;
01. pedestal in figure, 02. pedestal, 03. seat of honour, 04. sealing bolt, 05. multifunctional gas/liquid displacement opening are logical
Road, 06. reference electrode interface, 07. anode interface, 08. cathode interface, 09. window opening, 10. form seal grooves, 11. casees
Body sealing ring slot, 12. positive fixinig plates, 13. reference electrode connecting columns, 14. cathode connecting columns, 15. bolt of lower base holes, 16 seats of honour
Bolt hole, 17 fixing screws.
Specific embodiment
[embodiment 1]
As depicted in figs. 1 and 2, test box outer body involved in the present invention is made of pedestal 02 and the seat of honour 03, test box
There is cathode interface 08 in front of pedestal 02, right front portion is equipped with reference electrode interface 06, and 03 right front portion of the seat of honour is equipped with anode interface 07, and three
A interface internal has cylindrical or hexagonal column connected in star (Fig. 3), for being attached with the banana plug being separately equipped with, banana plug
Head is connected with external electrochemical workstation, for accurately controlling electric current and voltage.The top at the seat of honour 03 is provided with round window opening
09, in order to the disengaging of light/laser, for acquiring optics or raman spectral signal.
As shown in Figures 2 and 4,03 left side of the seat of honour is equipped with multifunctional gas/liquid displacement open channel 05, is connect using pressing
The form of head, it is closed by sealing bolt 04 and polymer pressure ring (not marking in the example shown) progress, when sealing bolt 04 is tightened
When, front end gasket is pressed on multifunctional gas/liquid displacement open channel 05 access, provides closed loop for test box
Border.The pedestal 02 of test box phosphor bodies and the seat of honour 03 are sealed by the O-type sealing ring being placed in box sealing ring recess 11, together
When three identical fixing screws 17 will be fixed by seat of honour bolt hole 16 and bolt of lower base hole 15 by box main body is tested.Form is opened
O-type sealing ring and borosilicate glass piece or quartz plate or indigo plant of the mouth 09 by being placed in the form seal groove 10 at the seat of honour 03
The slides such as jewel piece are sealed, and preferred glass thickness is 300 microns.
As shown in figure 3, cathode interface 08 is attached using externally threaded form with pedestal 02, the front end of cathode interface 08
With 02 contact position of pedestal, it is placed with teflon gasket (not marking in the example shown) and is sealed.06 He of reference electrode interface
Anode interface 07 uses identical connection and sealing means.
As shown in Figure 3 and Figure 4, cathode interface 08 is attached by way of screw thread with cathode connecting column 14, reference electricity
Pole interface 06 is connect using identical connection type with reference electrode connecting column 13.07 front end of anode interface is prominent positive with spill
The side wall of fixinig plate 12 is in contact, and is connect by positive fixinig plate 12 with positive electrode.
In use, by above-mentioned connection type by pedestal 02 and the seat of honour 03 and reference electrode interface 06, cathode interface 08 and just
The assembling of each component of pole interface 07,0- type sealing ring is placed in box sealing ring recess 11, then in glove box, by the seat of honour 03
It is just being placed on station with the face of lower seated connection touching, in installing 0- type sealing ring in form seal groove 10, in being placed on sealing ring
Then slide is sequentially placed anode electrode piece (mesh electrode piece or the intermediate electrode slice for being provided with hole), positive 12 He of fixinig plate
Diaphragm (diameter is greater than reference electrode), and electrolyte is added dropwise.Pedestal 02 is just being set, cathode and annular reference electrode (Fig. 5) are placed,
Overturning is aligned with the seat of honour 03, fixed by three bolt of lower base holes 15 and seat of honour bolt hole 16 with fixing screws 17.In glove box
It is interior with sealing bolt 04 that device is closed.By test device after being removed in glove box, device is placed in not by pedestal 01
With instrument platform on, then device can be connected at anode interface 07 and cathode interface 08 by reference electrode interface 06
External circuit is optics in situ and the Raman spectrum survey realized to battery electrode material under test mode by window opening 09
Examination.
[embodiment 2]
As shown in fig. 6, device of the present invention can have two multifunctional gas/liquid displacement open channel 05, it is right
The variation of generated gas and electrolyte is studied in metal ion battery charge and discharge process.In use, pressing embodiment 1
Described in device is installed, sealing bolt 04 is changed into the intermediate screw for having channel, in multifunctional gas/liquid displacement
05 external connection valve of open channel, by valve by the gas of generation or electrolyte guiding device, two multifunctional gas/liquid
Body displacement open channel 05 can be interchanged as in/out channel.It can also be open by two multifunctional gas/liquid displacement logical
Road 05 adds electrolyte, to judge whether the reason of battery performance declines is since consuming excessively for electrolyte causes.
Claims (6)
1. the device that one kind can carry out in-situ test to metal ion battery, it is characterised in that: the device is cabinet design, including
Pedestal and the seat of honour are sealed by upper and lower two parts, pedestal (02) and the seat of honour (03) by O-type sealing ring, electrode material when use
Material will be placed in the seal cavity to be formed, while three by being placed in bolt of lower base hole (15) and seat of honour bolt hole (16)
A identical fixing screws (17) are fixed box main body is tested, and have cathode interface (08), right front portion in front of test box pedestal (02)
Equipped with reference electrode interface (06), the test box seat of honour (03) right front portion is equipped with anode interface (07), and three interfaces can pass through circle
Cylindricality or hexagonal column connected in star and the banana plug being separately equipped with are attached, and banana plug is connected with external electrochemical workstation,
For accurately controlling electric current and voltage, reference electrode interface (06) and cathode interface (08) pass through reference electrode connecting column respectively
(13) with cathode connecting column (14) with place reference electrode material in the cavity and negative electrode material connect, anode interface (07) is led to
It crosses positive fixinig plate (12) to be connected with the positive electrode of placement in the cavity, the seat of honour (03) is equipped with one or two Multifunctional, air
Body/liquid displacement open channel (05) can be used as gas/liquid inlet and outlet, and the liquid/gas transfer device separately configured is matched
It closes and uses, or form closed environment with sealing bolt (04) closing passage, the seat of honour is provided with round window opening at the top of (03)
(09), in order to the disengaging of light/laser, for acquiring optics or raman spectral signal, with interchangeable slide and O- at form
The sealing of type sealing ring.
2. the device according to claim 1 that in-situ test can be carried out to metal ion battery, it is characterized in that: above-mentioned case
Body has one or two multifunctional gas/liquid displacement open channel (05), can detect to the airtight performance of cavity,
It can provide the gas circuit of gas collecting, it is possible to provide the access of electrolyte acquisition, it is possible to provide the access for adding electrolyte, it is outer by closing
It sets valve or uses sealing bolt (04), the space of gas storage can be provided in cabinet, be suitable for metal ion battery in spy
Determine the optic test in situ under atmosphere.
3. it is according to claim 1 can to metal ion battery carry out in-situ test device, it is characterized in that: it is above-mentioned just
Pole fixinig plate (12) is concave structure, and circular open is arranged at bottom, and positive electrode is placed in concave inside, with reference electrode connecting column
(13) and the distance between cathode connecting column (14) can pass through the height of reference electrode connecting column (13) and cathode connecting column (14)
Degree is adjusted, and provides the space length of optimization for electrode material.
4. the device according to claim 1 that in-situ test can be carried out to metal ion battery, it is characterized in that: above-mentioned survey
The device of examination has reference electrode, the setting of three electrode of positive electrode and negative electrode, in use, the electrochemistry experiment of three electrodes can be carried out
Test can also carry out the experiment test of two electrode electro Chemical of positive electrode and negative electrode.
5. according to claim 1 with described in 4 can to metal ion battery carry out in-situ test device, it is characterized in that: above-mentioned
Test device in reference electrode connecting column (13) be annular, annular reference electrode can be placed above, reference electrode and negative
The distance between pole connecting column (14) can come by adjusting the size of reference electrode connecting column (13) and cathode connecting column (14)
It realizes.
6. the device according to claim 1 that in-situ test can be carried out to metal ion battery, it is characterized in that: above-mentioned survey
Trial assembly set in the seat of honour (03) medium design have circular window opening (09) and borosilicate glass, quartz, sapphire etc. is more
The made sight glass of kind material is used cooperatively, and is tested for optic test and Raman spectrum, the size of the window opening can
With adjustment, from 1 millimeter to 15 millimeter, be sealed by the O-ring between sight glass and the seat of honour, sight glass with ground
The electrode material studied carefully is in contact, and the minimum range between electrode material and the optical microscopy objective lens configured is only form
The thickness of glass is conducive to collect optical signalling to greatest extent, improves sensitivity.
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Cited By (5)
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 |
CN110361337A (en) * | 2019-08-20 | 2019-10-22 | 南杰智汇(深圳)科技有限公司 | A kind of transmission mode electrochemical in-situ optical testing device |
CN110412013A (en) * | 2019-08-20 | 2019-11-05 | 南杰智汇(深圳)科技有限公司 | One kind being suitable for button cell original position optical testing device |
CN110987978A (en) * | 2019-12-20 | 2020-04-10 | 中国科学院青岛生物能源与过程研究所 | Device for observing battery pole piece and electrolyte in situ |
CN112461902A (en) * | 2020-12-10 | 2021-03-09 | 南杰智汇(深圳)科技有限公司 | Detachable multifunctional soft package battery mold |
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CN104297274A (en) * | 2014-11-07 | 2015-01-21 | 广西师范大学 | In-situ XRD reaction chamber for testing electrochemical reaction process |
CN206248605U (en) * | 2016-10-17 | 2017-06-13 | 东莞市凯欣电池材料有限公司 | A kind of three-electrode cell |
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CN103308726A (en) * | 2013-06-26 | 2013-09-18 | 西南石油大学 | Scanning electrochemical microscope experimental device for tests in various environments |
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CN110987978A (en) * | 2019-12-20 | 2020-04-10 | 中国科学院青岛生物能源与过程研究所 | Device for observing battery pole piece and electrolyte in situ |
CN112461902A (en) * | 2020-12-10 | 2021-03-09 | 南杰智汇(深圳)科技有限公司 | Detachable multifunctional soft package battery mold |
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Application publication date: 20190607 |