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 PDF

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Publication number
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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Prior art keywords
situ
lithium battery
sample cell
inner ring
upper cover
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李志娟
宋晓波
叶龙
刘泉
赵运兴
林美超
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Hunan Spaceflight Tian Lu New Material Inspection Co Ltd
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Hunan Spaceflight Tian Lu New Material Inspection Co Ltd
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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

A kind of sample cell in situ applied to lithium battery in-situ test
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).
CN201821417667.1U 2018-08-31 2018-08-31 A kind of sample cell in situ applied to lithium battery in-situ test Active CN208688993U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
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

Cited By (5)

* Cited by examiner, † Cited by third party
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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