CN209544410U - Battery in situ X-ray diffraction diffraction charge and discharge sealing device - Google Patents

Battery in situ X-ray diffraction diffraction charge and discharge sealing device Download PDF

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Publication number
CN209544410U
CN209544410U CN201920626503.8U CN201920626503U CN209544410U CN 209544410 U CN209544410 U CN 209544410U CN 201920626503 U CN201920626503 U CN 201920626503U CN 209544410 U CN209544410 U CN 209544410U
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situ
diffraction
battery
charge
hole
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孙洁
卢焕明
彭哲
王雪莹
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Ningbo Institute of Material Technology and Engineering of CAS
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Ningbo Institute of Material Technology and Engineering of CAS
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The utility model discloses a kind of battery in situ X-ray diffraction diffraction charge and discharge sealing devices, including shell and the positive plate being encapsulated in housing cavity, diaphragm, negative electrode tab and electrolyte, shell region corresponding with positive plate is provided at least one first through hole, the aperture of the first through hole is greater than or equal to the spot diameter of X-ray.For battery in situ X-ray diffraction diffraction charge and discharge sealing device provided by the embodiment of the utility model when being applied to in-situ TiC particles test, not only Sealing period is 60h, but also collected diffracted signal is clear, intensity is high.

Description

Battery in situ X-ray diffraction diffraction charge and discharge sealing device
Technical field
In particular to a kind of battery in situ X-ray diffraction diffraction charge and discharge sealing device of the utility model, belongs to lithium battery technology Field.
Background technique
X-ray diffractometer (X-ray diffractometer, be abbreviated as XRD) is research material composition and crystal structure Basic tool, the cell parameter, space group, macro-stress, object phase composition of substance can be obtained according to X-ray powder diffraction spectrum And content, the information such as crystallite dimension Types of Dislocations and concentration, thus it is widely used in metallurgy, petroleum, chemical industry, scientific research, aviation boat It, teaching, material production etc. fields.Two dimensional X ray diffraction (XRD2) it is a kind of new technology, it is not simple using two dimension spy Survey the diffractometer of device.It further include 2D image processing, the processing of 2D diffraction pattern and explanation other than 2D detector technology.Two dimension The advantage of diffraction is that recording data is the full debye ring in planar range, and information content is larger, and acquisition data are to scan simultaneously, entirely Dynamically Announce is composed, the record data speed of two-dimentional diffractometer is better than 1D.
Lithium ion battery is the current internationally recognized desirable chemical energy, and it is excellent to have that small in size, capacitance is big, voltage is high etc. Point is widely used in the electronic products such as mobile phone, laptop computer, and the electric car field being growing will give lithium ion battery Bring bigger development space.During researching and developing the lithium ion battery material of high-energy density, X-ray diffraction is characterization electrode The important means of material composition and different removal lithium embedded state flowering structure situations of change.But common X-ray diffractometer is not equipped with electricity Chemical in situ attachment, and the chemical property of electrode material of lithium battery is very active, electrochemical reaction product in an atmosphere steady It is qualitative also poor.In ex situ XRD test process, it is necessary to intermittently stop electrochemical reaction, battery is dismantled taking-up electricity Pole material is tested.Therefore, this test will use multiple batteries, and battery electrode material in disassembly and transfer process It is easy to that deformation occurs or reacts with air and water, so that the X-ray diffractogram spectrum information of electrode material be made to lose or change Become, the research changed to the Nomenclature Composition and Structure of Complexes of electrode material in electrochemical process brings great difficulty.Power lithium battery Characteristic be closely related with environment temperature, the capacity of battery reduces rapidly at low temperature, rises rapidly at high temperature, under high temperature Volume change speed is less than low temperature.The structure change situation of in-situ TiC particles measuring technology energy real-time monitoring material under various circumstances, There is the unrivaled application advantage of other means in materials synthesis and practical studies, is particularly suitable for having the dynamic of phase transition process State research, and the theoretical research based on common XRD, spectrum analysis technology are also fully applicable for the spectrum elucidation of in-situ TiC particles.From The abundant information of the dynamic change obtained in in-situ TiC particles spectrogram has been widely used the every field in investigation of materials.
There are mainly three types of the lithium battery encapsulation forms of mainstream, i.e., round, rectangular and Soft Roll, different encapsulating structure means Different characteristics.The popularity rate of rectangular cell is very high at home, but since quadrate lithium battery is determined according to the size of product Inhibition and generation production, there is thousands of kinds of models in the market, and technique is difficult unification, is unfavorable for standardized production;Soft-package battery safety Can be good, shortcoming is that consistency is poor, and higher cost is easy to happen leakage;Round lithium battery uses quite mature technique, High degree of automation, product pass stay in grade, and advantage of lower cost has obtained large-scale production in electric car industry.
Develop in-situ TiC particles measuring technology, material of real-time monitoring li-ion electrode materials during charge-discharge cycles Structure change situation can greatly improve the accuracy of data, eliminate sample preparation and transfer etc. in ex situ test process Bring uncertainty is operated, for understanding the electrochemical process of li-ion electrode materials, the new electrode material of research and development With great theoretical value.
Button cell is a kind of air locking, and a kind of sealing structure of button cell is as shown in Figure 1a in the prior art, and X is penetrated Line needs guiding through sealing material outer wall and collector, and sealing material can make diffracted signal strength reduction to the decaying of X-ray signal, surveys Try electrode material electric property when be by positive electrode be coated in aluminum foil current collector on, but aluminium foil be with certain thickness (15~ 25 μm) dense material, X-ray is difficult to penetrate aluminium foil, itself can generate very strong diffracted signal, can not obtain when testing in situ Obtain electrode material diffraction spectra.
Lithium battery in-situ TiC particles test device is commercialized not yet at present, and researcher needs voluntarily fixed according to testing requirement System processing lithium battery reaction in-situ device, processing charges is expensive and the process-cycle is longer;And existing air locking has mostly used For the metallic beryllium of poison as sealing material, metallic beryllium diffracted signal can generate more by force certain interference to electrode material;Work as Strong oxdiative When the compound of physical property is coated in beryllium window, metallic beryllium is easily oxidized to porous material, and sealing performance is caused to be deteriorated.
Utility model content
The main purpose of the utility model is to provide a kind of battery in situ X-ray diffraction diffraction charge and discharge sealing device, with gram Take deficiency in the prior art.
For the aforementioned purpose of utility model of realization, the technical solution adopted in the utility model includes:
The utility model embodiment provide a kind of battery in situ X-ray diffraction diffraction charge and discharge sealing device, including shell with And it is encapsulated in positive plate, diaphragm, negative electrode tab and electrolyte in housing cavity, it is set in shell region corresponding with positive plate It is equipped at least one first through hole, the aperture of the first through hole is greater than or equal to the spot diameter of X-ray.
Further, the shell includes anode cover and negative electrode casing, and the anode cover and negative electrode casing are tightly connected to form institute The inner cavity stated, the positive plate are arranged in the anode cover, and the negative electrode tab is arranged in the negative electrode casing, and described the One through-hole is distributed on the anode cover.
Further, shell region corresponding with positive plate is provided with multiple first through hole, the first through hole Aperture be 2mm-3mm.
Further, the positive plate includes the positive electrode of collector and distribution on a current collector, the anode material A side surface of the collector towards first through hole is arranged in material.
Further, the material of the collector is identical as the material of the diaphragm.
Further, it is additionally provided with conductive film between the positive plate and anode cover, is arranged on the conductive film There is at least one second through-hole, the aperture of second through-hole is not less than the aperture of first through hole, and X-ray can sequentially pass through the One through-hole, the second through-hole are irradiated on positive electrode without being irradiated on conductive film.
Further, the conductive film and anode cover are coaxially disposed.
Further, every one second through-hole is at least corresponding with a first through hole.
Further, the aperture of second through-hole is 3mm-5mm.
Further, the first through hole and/or the second through-hole are round hole.
Further, the conductive film is aluminium foil.
Further, it is additionally provided with sealing film in the outer surface of the anode cover, the sealing film at least covers First through hole.
Further, the sealing film includes Kapton Tape, and the Kapton Tape is pasted onto outside anode cover Side.
Further, the thickness of the Kapton Tape is less than 0.05mm.
Further, sealant is coated in the outer peripheral edge portion also glue that the sealing film is contacted with anode cover.
Further, the sealant includes AB glue, wherein A glue and B glue are uniformly mixed according to volume ratio 1: 1, under room temperature 3-5min completes primary solidification, and time≤for 24 hours is fully cured, can stablize use at -50 DEG C -100 DEG C.
Further, be additionally provided with supporting element between the negative electrode tab and negative electrode casing, the supporting element include gasket and Elastic slice, the gasket are arranged between elastic slice and negative electrode tab.
Further, the negative electrode tab is lithium anode.
Compared with prior art, include: the advantages of the utility model
1) the battery in situ X-ray diffraction diffraction charge and discharge sealing device provided after cell package in use, be not susceptible to short Road and open circuit, raw material are easy to obtain, structure is simple, easy to use, save the cost;
2) for the battery in situ X-ray diffraction diffraction charge and discharge sealing device provided when carrying out in-situ TiC particles test, Sealing period is long It is 60h;
3) provide battery in situ X-ray diffraction diffraction charge and discharge sealing device in, using Kapton Tape as sealing material, with Diaphragm is collector, and Kapton Tape and diaphragm have good penetrability to X-ray, thus can collect it is clear and strong Spend high diffracted signal;
4) the battery in situ X-ray diffraction diffraction charge and discharge sealing device provided can be used in combination with alternating temperature sample stage, penetrate X Line diffractometer has the ability of Microstructure Development process at a temperature of in-situ observation electrode material varying environment, can study -40 DEG C The relationship of battery material charge-discharge performance and structure is tested within the scope of~80 DEG C.
Detailed description of the invention
Fig. 1 a is a kind of sealed structural schematic diagram of button cell in the prior art;
Fig. 1 b is a kind of lithium battery in situ X-ray diffraction diffraction charge and discharge sealing device in one exemplary embodiments of the utility model Structural schematic diagram;
Fig. 2 is the diffraction spectrogram of Kapton Tape and wheat membrane;
Fig. 3 is a kind of lithium battery in-situ TiC particles test macro schematic diagram;
Fig. 4 a be measurement obtain lithium battery in situ X-ray diffraction diffraction charge and discharge sealing device in electrode material at -40 DEG C Under the conditions of in-situ TiC particles test diffraction spectra;
Fig. 4 b be measurement obtain lithium battery in situ X-ray diffraction diffraction charge and discharge sealing device in electrode material at -40 DEG C Under the conditions of charging and discharging curve;
Fig. 5 a be measurement obtain lithium battery in situ X-ray diffraction diffraction charge and discharge sealing device in electrode material in 25 DEG C of items In-situ TiC particles test diffraction spectra under part;
Fig. 5 b be measurement obtain lithium battery in situ X-ray diffraction diffraction charge and discharge sealing device in electrode material in 25 DEG C of items Charging and discharging curve under part;
Fig. 6 a be measurement obtain lithium battery in situ X-ray diffraction diffraction charge and discharge sealing device in electrode material in 80 DEG C of items In-situ TiC particles test diffraction spectra under part;
Fig. 6 b be measurement obtain lithium battery in situ X-ray diffraction diffraction charge and discharge sealing device in electrode material in 80 DEG C of items Charging and discharging curve under part;
Fig. 7 is a kind of lithium battery in situ X-ray diffraction diffraction charge and discharge sealing device in one exemplary embodiments of the utility model Sealing period test result.
Specific embodiment
In view of deficiency in the prior art, inventor is studied for a long period of time and is largely practiced, and is able to propose that this is practical new The technical solution of type.The technical solution, its implementation process and principle etc. will be further explained as follows.
The utility model embodiment proposes a kind of charging and discharging lithium battery sealing device, and the in situ of X-ray diffractometer is cooperated to become High/low temperature electric property and micro-structural test in situ may be implemented in temperature function:
1) the punching size of battery case is determined
X-ray light spot is tested having a size of 1mm or 2mm in battery charging and discharging and in-situ TiC particles during in-situ test In the process, penetrating due to temperature control system heating, chemical reaction and X-ray, battery ambient temperature can increase, and make the temperature of electrolyte Degree increases, and battery case aperture is excessive to make battery that open circuit occur vulnerable to thermal expansion;Therefore the aperture of battery case (i.e. aforementioned positive electrode shell) (i.e. first through hole) is sized to the circular hole of diameter 2mm-3mm, to ensure that hot spot is not irradiated on battery case to battery signal Generate interference, while irradiation electrode material as much as possible again.
2) sealing material and collector are screened
A variety of sealing materials and collector are screened to improve diffracted signal intensity, as the result is shown Kapton Tape and wheat Membrane can meet the requirement of X-ray penetrability, but wheat membrane diffracted signal relatively by force can produce the diffracted signal of sample Raw certain interference (such as Fig. 2), therefore use Kapton Tape (thickness < 0.05mm) sealed button cell.
It is found in development process, although carbon paper good conductivity, carbon paper is frangible, and the electrolyte of absorption is few, as afflux Body easily causes battery short circuit;Clear pure diffraction spectra can be obtained when electrode material is coated on diaphragm, can reduce collector Influence of the diffracted signal to electrode material, while diaphragm has good flexibility, can absorb more electrolyte, enhances button The electric conductivity of inside battery.Therefore, diaphragm is the ideal material for substituting aluminium foil as collector.
3) button cell design of Sealing Structure
Lithium ion battery electrolyte is to air, moisture-sensitive, so the assembling process of lithium ion battery need to be in glove box It carries out.When encapsulation, negative electrode casing, negative electrode tab, diaphragm, positive plate, positive cover (i.e. aforementioned positive electrode shell, similarly hereinafter) are put in order; Cell package schematic diagram is as shown in Figure 1 b, and the collector in the utility model is identical as the material of diaphragm, reduces collector to X-ray Absorption and interference to diffraction spectrogram, electrode (anode) material is towards battery case (anode cover) opening direction when cell package;
For the conduction for enhancing battery, one layer of punching aluminium foil is added between positive electrode and anode cover, aluminium foil punching is straight Diameter is not less than the aperture of battery case aperture, with battery case coaxial placement when installation, avoids x-ray bombardment to aluminium foil, aluminium foil punches (multiple second through-holes are provided on aluminium foil) diameter 3mm-5mm;Kapton Tape (thickness < 0.05mm) is pasted onto electricity On the outside of the shell aperture of pond;AB glue is uniformly applied to the extension cell sealing time around Kapton Tape again.
Specifically, Fig. 1 b is please referred to, a kind of lithium battery in situ X-ray diffraction diffraction charge and discharge sealing device, including anode cover 1, Negative electrode casing 2 and the aluminium foil 6 being successively sealed between anode cover and negative electrode casing, positive plate 3, diaphragm 5, negative electrode tab 4, supporting element 7;Anode cover 1 and negative electrode casing 2 are tightly connected and then form the inner cavity of encapsulation between anode cover 1 and negative electrode casing;Anode cover 1 It specifies and is provided at least one first through hole (not shown) on region (such as on one end end face of anode cover), first The aperture of through-hole is more than or equal to the spot diameter of X-ray;Positive plate 3 includes collector 32 and is coated in collector towards first (material of diaphragm can use those skilled in the art for positive electrode 31 on one side surface of through-hole, collector 32 and diaphragm Known material, details are not described herein) 5 material is identical;Aluminium foil 6 and anode cover 1 are coaxially disposed, and are provided on aluminium foil 6 Multiple second through-hole (not shown)s, each second through-hole is corresponding at least one first through hole, second through-hole Aperture be not less than first through hole aperture, X-ray can sequentially pass through first through hole, the second through-hole is irradiated on positive electrode and It will not be irradiated on aluminium foil 6;Supporting element 7 includes the gasket 71 and elastic slice 72 set gradually;It is also viscous in the outer surface of anode cover 1 Kapton Tape 8 is posted, Kapton Tape 8 at least covers first through hole, in all because of anode cover of Kapton Tape 8 1 joint is also coated with AB glue.A glue and B glue are uniformly mixed according to volume ratio 1: 1, and 3-5min completes primary solidification under room temperature, Time≤for 24 hours is fully cured, can stablize use at -50 DEG C -100 DEG C;The AB glue of use can be Kraft extra-heavy power AB Glue, large fibre 8317AB glue etc., can pass through commercially available acquisition.
4) lithium battery in-situ TiC particles charge-discharge test is carried out
Since lithium ion battery charge and discharge cycles are continuous continual processes, if the not test program of continuous operation It cannot will reflect in real time the structure change of electrode material;Electrode material of lithium battery structure can be studied and continuously become by first having to build one kind The XRD in-situ test system (as shown in Figure 3) of change, according to the Mass Calculation electricity of active material on the capacity and pole piece of electrode material The time required to chemical reaction, the angular range and acquisition time of the software setting diffraction spectra then carried using diffractometer are realized To the real-time detection of the structure change situation of battery electrode material under varying temperature environment;It provides such as the lithium battery original position X in Fig. 1 b XRD in-situ test system in x ray diffraction charge and discharge sealing device and Fig. 3, it is close to lithium battery in situ X-ray diffraction diffraction charge and discharge Electrode material (i.e. positive electrode) in seal apparatus is tested, and electrode material in-situ TiC particles under the conditions of -40 DEG C test diffraction spectra As shown in fig. 4 a, charging and discharging curve figure is as shown in Figure 4 b;Electrode material in-situ TiC particles under the conditions of 25 DEG C test diffraction spectra such as Fig. 5 a Shown, charging and discharging curve figure is as shown in Figure 5 b;Electrode material in-situ TiC particles test diffraction spectra under the conditions of 80 DEG C is as shown in Figure 6 a, Charging and discharging curve figure is as shown in Figure 6 b.
Battery in situ X-ray diffraction diffraction charge and discharge sealing device provided by the embodiment of the utility model is in use, battery seals It is not susceptible to short circuit and open circuit after dress, raw material are easy to obtain, structure is simple, easy to use, save the cost;Also, using this The battery in situ X-ray diffraction diffraction charge and discharge sealing device that utility model embodiment provides carries out in-situ TiC particles test, Sealing period It is long, sealing device Sealing period up to 60h (as shown in Figure 7) provided by the embodiment of the utility model;And the utility model In the battery in situ X-ray diffraction diffraction charge and discharge sealing device of offer, using Kapton Tape as sealing material, using diaphragm as afflux Body, and Kapton Tape and diaphragm have good penetrability to X-ray, therefore can collect clear and high intensity diffraction Signal;Also, battery in situ X-ray diffraction diffraction charge and discharge sealing device provided by the utility model can combine with alternating temperature sample stage It uses, the ability of Microstructure Development process at a temperature of making X-ray diffractometer have in-situ observation electrode material varying environment can The relationship of battery material charge-discharge performance and structure is tested within the scope of -40 DEG C~80 DEG C of research.
It should be appreciated that above-described embodiment is only to illustrate the technical ideas and features of the present invention, it is ripe its object is to allow The personage for knowing technique can understand the content of the utility model and implement accordingly, can not limit the utility model with this Protection scope.All equivalent change or modifications according to made by the spirit of the present invention essence, should all cover in the utility model Within protection scope.

Claims (16)

1. a kind of battery in situ X-ray diffraction diffraction charge and discharge sealing device, including shell and the anode being encapsulated in housing cavity Piece, diaphragm, negative electrode tab and electrolyte, it is characterised in that: shell region corresponding with positive plate is provided at least one First through hole, the aperture of the first through hole are greater than or equal to the spot diameter of X-ray.
2. battery in situ X-ray diffraction diffraction charge and discharge sealing device according to claim 1, it is characterised in that: the shell packet Anode cover and negative electrode casing are included, the anode cover and negative electrode casing are tightly connected to form the inner cavity, and the positive plate is arranged in institute It states in anode cover, the negative electrode tab is arranged in the negative electrode casing, and the first through hole is distributed on the anode cover.
3. battery in situ X-ray diffraction diffraction charge and discharge sealing device according to claim 1 or claim 2, it is characterised in that: in the shell Body region corresponding with positive plate is provided with multiple first through hole, and the aperture of the first through hole is 2 mm-3 mm.
4. battery in situ X-ray diffraction diffraction charge and discharge sealing device according to claim 2, it is characterised in that: the positive plate Collector is arranged in towards first through hole in positive electrode including collector and distribution on a current collector, the positive electrode One side surface.
5. battery in situ X-ray diffraction diffraction charge and discharge sealing device according to claim 4, it is characterised in that: in the anode It is additionally provided with conductive film between piece and anode cover, is provided at least one second through-hole on the conductive film, described second The aperture of through-hole is not less than the aperture of first through hole, and X-ray can sequentially pass through first through hole, the second through-hole is irradiated to positive material Without being irradiated on conductive film on material.
6. battery in situ X-ray diffraction diffraction charge and discharge sealing device according to claim 5, it is characterised in that: the conduction Film and anode cover are coaxially disposed.
7. battery in situ X-ray diffraction diffraction charge and discharge sealing device according to claim 5, it is characterised in that: every one second is logical Hole is at least corresponding with a first through hole.
8. battery in situ X-ray diffraction diffraction charge and discharge sealing device according to claim 7, it is characterised in that: described second is logical The aperture in hole is 3 mm-5 mm.
9. battery in situ X-ray diffraction diffraction charge and discharge sealing device according to claim 7, it is characterised in that: described first is logical Hole and/or the second through-hole are round hole.
10. battery in situ X-ray diffraction diffraction charge and discharge sealing device according to claim 6, it is characterised in that: the conductive thin Film is aluminium foil.
11. battery in situ X-ray diffraction diffraction charge and discharge sealing device according to claim 2, it is characterised in that: in the anode The outer surface of shell is additionally provided with sealing film, and the sealing film at least covers first through hole.
12. battery in situ X-ray diffraction diffraction charge and discharge sealing device according to claim 11, it is characterised in that: the sealing Film includes Kapton Tape, and the Kapton Tape is pasted on the outside of anode cover.
13. battery in situ X-ray diffraction diffraction charge and discharge sealing device according to claim 12, it is characterised in that: the polyamides The thickness of imines adhesive tape is less than 0.05mm.
14. battery in situ X-ray diffraction diffraction charge and discharge sealing device according to claim 11, it is characterised in that: described close The outer peripheral edge portion that sealing film is contacted with anode cover also glue is coated with sealant.
15. battery in situ X-ray diffraction diffraction charge and discharge sealing device according to claim 2, it is characterised in that: in the cathode Supporting element is additionally provided between piece and negative electrode casing, the supporting element includes gasket and elastic slice, and the gasket setting is in elastic slice and bears Between pole piece.
16. battery in situ X-ray diffraction diffraction charge and discharge sealing device according to claim 15, it is characterised in that: the cathode Piece is lithium anode.
CN201920626503.8U 2019-05-05 2019-05-05 Battery in situ X-ray diffraction diffraction charge and discharge sealing device Active CN209544410U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111103398A (en) * 2019-11-28 2020-05-05 浙江浙能技术研究院有限公司 Detection method for lithium-embedded pole piece of lithium ion secondary battery
CN112255255A (en) * 2020-10-14 2021-01-22 中国工程物理研究院电子工程研究所 In-situ battery testing device and testing method based on neutron diffraction
CN115248236A (en) * 2021-12-31 2022-10-28 青岛大学 In-situ magnetoelectric test device and method

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111103398A (en) * 2019-11-28 2020-05-05 浙江浙能技术研究院有限公司 Detection method for lithium-embedded pole piece of lithium ion secondary battery
CN112255255A (en) * 2020-10-14 2021-01-22 中国工程物理研究院电子工程研究所 In-situ battery testing device and testing method based on neutron diffraction
CN112255255B (en) * 2020-10-14 2023-07-07 中国工程物理研究院电子工程研究所 In-situ battery testing device and testing method based on neutron diffraction
CN115248236A (en) * 2021-12-31 2022-10-28 青岛大学 In-situ magnetoelectric test device and method

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