CN208688993U - A kind of sample cell in situ applied to lithium battery in-situ test - Google Patents
A kind of sample cell in situ applied to lithium battery in-situ test Download PDFInfo
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- CN208688993U CN208688993U CN201821417667.1U CN201821417667U CN208688993U CN 208688993 U CN208688993 U CN 208688993U CN 201821417667 U CN201821417667 U CN 201821417667U CN 208688993 U CN208688993 U CN 208688993U
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- lithium battery
- sample cell
- inner ring
- upper cover
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Abstract
The utility model discloses a kind of sample cells in situ applied to lithium battery in-situ test, comprising: upper cover;Inner ring, top and the upper cover following table face contact;Pedestal, top are contacted with the inner ring bottom end;Pillar is installed in the airtight cavity formed by upper cover, inner ring, pedestal;The pillar top upper surface is equipped with lithium battery, and pillar top upper surface is contacted with lithium cell cathode material;Extensible member, one end connection pillar bottom end, the other end connect on the inside of pedestal.The device of the utility model can realize X-ray diffraction and X-fluorescence measurement of the lithium battery in charge and discharge process, that is, realization is measured the changes in crystal structure in the true use process of lithium battery and chemical composition analysis.
Description
Technical field
The utility model relates to lithium battery evaluation test device, especially a kind of original position applied to lithium battery in-situ test
Sample cell.
Background technique
The chemical property and electronics and ion of lithium battery the transporting of body phase and interface, react, storage behavior it is related.From
Atomic scale to macro-scale, to battery material equilibrium state and nonequilibrium state process electronic structure, crystal structure, microcosmic shape
For understanding, all kinds of structure-activity relationships are most important in lithium ion battery for the evolution research of looks, chemical composition, physical property, in battery
Charge and discharge process in, crystalline types, crystal parameter of electrode material etc. can change.
X-ray diffraction is the diffraction phenomena by X-ray in the sample, position and intensity using diffraction maximum, is come qualitative
Crystalline types, crystal parameter, crystal defect, content of different structure phase of analysis of material etc..In the charge and discharge process of battery,
Crystalline types, crystal parameter of electrode material etc. can change, and in order to determine, electrode material is sent out in battery charge and discharge process
Raw specific variation, we can be used in-situ TiC particles and are observed in real time electrode material.So as to deduce in electrification
Learn the intermediary that generates in reaction process, by these intermediate products can deduce reaction mechanism.
Sample cell in situ applied to lithium battery in situ detection (in-situ TiC particles) is that in situ detection technology and equipment is essential
Part, provide sample lithium battery sample mounting stage, positive and negative anodes pick out, mounting base, transmission window etc..Wherein in situ sample cell
Structure design, design of material, window material are designed as the key technology of the utility model.
There is similar patented product in Rigaku company, but expensive, in common XRD or energy storage material ingredient and structure
Joint in situ detection equipment is not possible to be used cooperatively.
Existing original position sample cell or sample stage in situ are more absorbed in high/low temperature in-situ test, i.e., place tested material
In sample stage, be at it is certain at a temperature of carry out X-ray absorption, X-ray diffraction, the measurement such as low-angle scattering of X-rays, this
Kind sample cell in situ is the high/low temperature in situ measurement for being directed to material.Such as a kind of patent " in-situ test example platform "
104458780A。
The sample cell in situ for being directed to lithium battery in-situ test is only used for electrochemical test function, that is, simulates different-thickness
Button-type battery, for evaluating the chemical property of the components such as electrode of lithium cell, electrolyte and diaphragm.Such as a kind of patent " use
In three electrode electrolyser of laminated type of lithium battery test chemical in situ " 107102041A.
Existing original position sample cell insufficiency generally carries out diffractometry or only to material using under high/low temperature in-situ condition
For electrochemical in-situ performance measurement, it is not carried out the X-ray diffraction measurement being directed under charging and discharging lithium battery in-situ condition and X
Ray fluorescence measurement.The prior art cannot achieve lithium battery under charge and discharge home state to the crystal structure of battery material and change
It studies and point measures, only in this way could truly react the variation of the crystal structure of lithium battery in use.
Utility model content
Technical problem to be solved in the utility model is, in view of the shortcomings of the prior art, providing a kind of for realizing lithium electricity
The sample cell in situ applied to lithium battery in-situ test of X-ray diffraction and X-fluorescence measurement of the pond in charge and discharge process.
It is a kind of in situ applied to lithium battery that in order to solve the above technical problems, the technical scheme adopted by the utility model is:
The sample cell in situ of test, comprising:
Upper cover;
Inner ring, top and the upper cover following table face contact;
Pedestal, top are contacted with the inner ring bottom end;
Pillar is installed in the airtight cavity formed by upper cover, inner ring, pedestal;The pillar top upper surface is equipped with lithium
Battery, and pillar top upper surface is contacted with lithium cell cathode material;
Extensible member, one end connection pillar bottom end, the other end connect on the inside of pedestal.
Measurement window is offered on upper lid above the pillar, which is encapsulated by KAPTON film.
The KAPTON film is coated with aluminium layer on one side, which is electrically connected with aluminum cell.
The upper cover is made of aluminium alloy.
Compared with prior art, have the beneficial effect that the device of the utility model can realize lithium possessed by the utility model
X-ray diffraction and X-fluorescence measurement of the battery in charge and discharge process, are installed on XRD, XRF combined instrument for sample cell in situ, electrification
Learn work station and connect by conducting wire with the positive and negative anodes of original position sample cell, and set charge-discharge parameter, realize battery sample fill or
Person's electric discharge, at the same time, XRD pass through sample cell transmission window in situ and carry out crystal structure analysis to battery material, and XRF passes through original
Position sample cell transmission window carries out battery material constituent analysis;Sample making course is completed in glove box, and glove box provides indifferent gas
Body atmosphere, 1 atmospheric pressure;It only needs to open the upper cover of sample cell in situ, so that it may which by lithium battery anode, diaphragm, (drop is powered on
Solve liquid), cathode installation and column upper surface, then upper cover is fastened in inner ring, i.e. completion sample preparation;Upper cover and inner ring, inner ring with
Pedestal uses O-ring static sealing, airtight up to 24 hours in holding chamber body;X-ray diffraction reflection windows are provided, window material is
Kapton film.
Detailed description of the invention
Fig. 1 is the utility model embodiment structural schematic diagram.
Specific embodiment
As shown in Figure 1, the utility model original position sample cell is mainly by upper cover 1, inner ring 2, pedestal 3, outer ring 4, pillar 7, bullet
Spring 8 forms.
KAPTON film is packaged at circular window (i.e. by upper cover 1 with circular window, using corrosion-and high-temp-resistant silica gel
KAPTON film covers circular window), which is anode material of lithium battery measurement window, provides X-ray diffraction reflection for XRD and surveys
Amount mode;KAPTON film is aluminized on one side, and the face of aluminizing of KAPTON film is connect with lithium battery, which flows as the pole of lithium battery
Body;Upper cover material is light aluminum alloy, is connect using fastening screw with upper cover, and the anode as lithium battery original position sample cell is drawn
11, energy storage material ingredient is attached thereto with structural union situ detection system electrochemical test system positive wire.
Inner ring 2 is PTFE (polytetrafluoroethylene (PTFE)) or polyformaldehyde material, has good machining property and insulation performance,
Inner ring is installed on upper cover lower surface, and inner ring is provided with groove, and trench depth is less than O-ring seal line footpath, and groove is close for mounting O-shaped
After seal, inner ring and upper cover are screwed, O-ring seal is driven plain, and the contact surface of upper cover lower surface and inner ring upper surface can
Hermetic seal is realized by O-ring.
Pedestal 3 is installed on inner ring lower surface, and pedestal upper surface is provided with groove, and trench depth is less than the line of O-ring seal 10
Diameter, groove is used for mounting O-shaped sealing ring, and after pedestal and inner ring are screwed, inner ring lower surface and pedestal upper surface are indirectly
Contacting surface realizes hermetic seal by O-ring seal;Base material is aluminium alloy, is connected by spring, pillar and lithium cell cathode material
Logical, the cathode that screw is connected to lithium battery original position sample cell with pedestal draws 12, and energy storage material ingredient and structural union are in situ
Detection system electrochemical test system negative wire is attached thereto.
Outer ring 4 is fixedly connected by screw with inner ring, and outer ring is austenite stainless steel material, can directly adsorb in energy storage material
Quick despatch, it can be achieved that sample cell in situ is expected in ingredient and structural union situ detection system magnetic bracket.
Pillar 7 is installed in the airtight cavity formed by upper cover, inner ring, pedestal, and pillar upper surface is for installing lithium battery
Three-decker, pillar upper surface coat lithium cell cathode material;Stay material is brass, has electric conductivity, passes through spring, base
Seat is drawn 12 with cathode and is connect.
Spring 8 is installed in pedestal blind hole, and lithium battery three-decker is fixed on sample cell in situ by pillar and upper cover
Cavity in, and give certain assembling pressure.
Lithium battery is fitted into the step (i.e. sample preparation) in sample cell in situ: sample making course is completed in glove box, and glove box mentions
For atmosphere of inert gases, 1 standard atmospheric pressure;The upper cover of sample cell in situ is opened, then by lithium battery anode, diaphragm (drop
Upper electrolyte), cathode be placed on the upper surface of pillar 7, then upper cover be fastened in inner ring, i.e., completion sample preparation.
Sample cell in situ after completing sample preparation is mountable to energy storage material ingredient and structural union situ detection system
On magnetic bracket, electrochemical test system positive and negative anodes are connected with the positive and negative anodes of sample cell in situ, and start charge/discharge process, and
The synchronous diffractometry for carrying out XRD.
Claims (8)
1. a kind of sample cell in situ applied to lithium battery in-situ test characterized by comprising
Upper cover (1);
Inner ring (2), top and the upper cover (1) following table face contact;
Pedestal (3), top are contacted with the inner ring (2) bottom end;
Pillar (7) is installed in the airtight cavity formed by upper cover (1), inner ring (2), pedestal (3);Table on pillar (7) top
Face is equipped with lithium battery, and pillar (7) top upper surface is contacted with lithium cell cathode material;
Extensible member, one end connection pillar (7) bottom end, the other end connect on the inside of pedestal (3).
2. the sample cell in situ according to claim 1 applied to lithium battery in-situ test, which is characterized in that the pillar
(7) measurement window is offered in the upper cover (1) above, which is encapsulated by KAPTON film.
3. the sample cell in situ according to claim 2 applied to lithium battery in-situ test, which is characterized in that the measurement
Window is circle.
4. the sample cell in situ according to claim 2 applied to lithium battery in-situ test, which is characterized in that described
KAPTON film is coated with aluminium layer on one side, which is electrically connected with aluminum cell.
5. the sample cell in situ according to claim 1 applied to lithium battery in-situ test, which is characterized in that the upper cover
(1) it is made of aluminium alloy.
6. the sample cell in situ according to claim 1 applied to lithium battery in-situ test, which is characterized in that the inner ring
(2) it is located in outer ring (4).
7. the sample cell in situ according to claim 1 applied to lithium battery in-situ test, which is characterized in that the inner ring
(2) it is sealed by sealing ring between upper surface and upper cover (1), between inner ring (2) lower surface and pedestal (3).
8. the sample cell in situ according to claim 1 applied to lithium battery in-situ test, which is characterized in that described flexible
Part is spring (8).
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CN201821417667.1U CN208688993U (en) | 2018-08-31 | 2018-08-31 | A kind of sample cell in situ applied to lithium battery in-situ test |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110687146A (en) * | 2019-10-14 | 2020-01-14 | 北京工业大学 | X-ray diffraction in-situ testing device for electrochromic film |
CN111122626A (en) * | 2020-01-02 | 2020-05-08 | 中国科学院青岛生物能源与过程研究所 | Device for carrying out CT test on battery |
CN111638233A (en) * | 2020-04-26 | 2020-09-08 | 山东大学 | In-situ battery reaction chamber of multifunctional X-ray diffractometer and application |
-
2018
- 2018-08-31 CN CN201821417667.1U patent/CN208688993U/en active Active
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110687146A (en) * | 2019-10-14 | 2020-01-14 | 北京工业大学 | X-ray diffraction in-situ testing device for electrochromic film |
CN110687146B (en) * | 2019-10-14 | 2022-06-24 | 北京工业大学 | X-ray diffraction in-situ testing device for electrochromic film |
CN111122626A (en) * | 2020-01-02 | 2020-05-08 | 中国科学院青岛生物能源与过程研究所 | Device for carrying out CT test on battery |
CN111638233A (en) * | 2020-04-26 | 2020-09-08 | 山东大学 | In-situ battery reaction chamber of multifunctional X-ray diffractometer and application |
CN111638233B (en) * | 2020-04-26 | 2021-05-07 | 山东大学 | In-situ battery reaction chamber of multifunctional X-ray diffractometer and application |
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