CN112151898A - Neutron in-situ device - Google Patents
Neutron in-situ device Download PDFInfo
- Publication number
- CN112151898A CN112151898A CN202010940214.2A CN202010940214A CN112151898A CN 112151898 A CN112151898 A CN 112151898A CN 202010940214 A CN202010940214 A CN 202010940214A CN 112151898 A CN112151898 A CN 112151898A
- Authority
- CN
- China
- Prior art keywords
- neutron
- positive electrode
- support body
- current collector
- sealing ring
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/48—Accumulators combined with arrangements for measuring, testing or indicating the condition of cells, e.g. the level or density of the electrolyte
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to the field of neutron scattering technology application, and particularly relates to a neutron in-situ device, which comprises a cavity (9) formed by a sealing ring (5), a sheet-shaped anode and a sheet-shaped cathode, wherein the cavity (9) is used for containing electrolyte and active substances wrapped by a diaphragm; the positive electrode comprises a first support body (1), a connecting layer (2), a positive electrode current collector (3) and a positive electrode material (4) which are sequentially stacked; the negative electrode comprises a second support body (8), a negative current collector (7) and a negative material (6) which are sequentially stacked. The invention provides a novel device for in-situ measurement of a microstructure of a solid electrolyte interface film of a lithium/sodium ion battery by adopting a neutron reflection spectrometer; compared with other devices for measuring the microstructure of the solid electrolyte interface film of the lithium/sodium ion battery, the invention is nondestructive in-situ measurement and can directly measure under working conditions, thereby obtaining the solid electrolyte interface film structure of the same battery under different states.
Description
Technical Field
The invention belongs to the field of neutron scattering technology application, and particularly relates to a neutron in-situ device.
Background
The neutron reflection spectrometer is an instrument for measuring microstructure information such as sample surface/interface roughness, thickness and components of each layer and the like, and is widely applied to research of interface structures, biological membranes and the like of magnetic films and films in polymers. Because neutrons are sensitive to light elements, isotopes and adjacent elements, and have the characteristics of deep penetrability, anti-interference performance and the like, the neutron reflection spectrometer is theoretically suitable for measuring the microstructure of the solid electrolyte interface film of the lithium/sodium ion battery. The microstructure of the solid electrolyte interface film of the lithium/sodium ion battery is closely related to the charge and discharge times, charge and discharge time, charge and discharge voltage and current and the like of the battery, and the film is easily oxidized by oxygen in the air and easily reacts with water vapor in the air, so that almost no equipment can comprehensively obtain the microstructure information of the solid electrolyte interface film of the lithium/sodium ion battery, and a neutron reflection spectrometer can not even directly perform the measurement work.
Disclosure of Invention
The invention aims to provide a device for in-situ measurement of microstructure information of a solid electrolyte interface film of a lithium/sodium ion battery by using a neutron reflection spectrometer, so as to comprehensively obtain the microstructure information of the solid electrolyte interface film of the lithium/sodium ion battery.
In order to achieve the purposes, the invention adopts the technical scheme that the neutron in-situ device comprises a cavity body which is formed by a sealing ring, a sheet-shaped positive electrode and a sheet-shaped negative electrode, wherein the cavity body is used for containing electrolyte and active substances wrapped by a diaphragm; the positive electrode comprises a first support body, a connecting layer, a positive current collector and a positive material which are sequentially stacked; the negative electrode comprises a second support body, a negative current collector and a negative electrode material which are sequentially stacked.
Further, the active substance is elementary lithium, or elementary sodium, or lithium salt, or sodium salt.
Further, in the present invention,
in the positive electrode, the first support body is positioned on an opening at one end of the sealing ring, and the connecting layer, the positive current collector and the positive material are positioned in the cavity;
in the negative electrode, the second support is located on the other end opening of the sealing ring, and the negative current collector and the negative electrode material are located inside the cavity.
Further, the first support body and the second support body are monocrystalline silicon wafers or silicon dioxide wafers, and the thickness of the first support body and the second support body is 0.2mm-3mm or 8mm-45 mm; the area is 5cm2-100cm2。
Further, the connecting layer is a plating layer arranged on the first support body, is made of titanium, platinum or chromium, and has a thickness of 2nm-15 nm.
Further, the positive electrode current collector is a plating layer arranged on the connecting layer, is made of gold, platinum or aluminum and has the thickness of 10nm-60 nm.
Further, the negative current collector is a plating layer arranged on the second support body, is made of gold, platinum or copper, and has a thickness of 10nm-60 nm.
Further, the sealing ring is made of silica gel or polytetrafluoroethylene, and the best area surrounded by the sealing ring is 5cm2-80cm2。
Further, the thickness of the anode material and the cathode material is 10nm-100 nm.
Further, the sealing ring, the positive electrode and the negative electrode are fixed into a whole by a clamp.
The invention has the beneficial effects that:
the brand new device for in-situ measurement of the microstructure of the solid electrolyte interface film of the lithium/sodium ion battery by adopting the neutron reflection spectrometer is provided; compared with other devices for measuring the microstructure of the solid electrolyte interface film of the lithium/sodium ion battery, the invention is non-destructive in-situ measurement (measuring the microstructure information of the solid electrolyte interface film), or can directly measure under the working condition, thereby obtaining the structure of the solid electrolyte interface film of the same battery under different states; in addition, compared with equipment such as an X-ray phonon spectrometer (XPS), an X-ray diffraction (XRD), a Surface Enhanced Raman Spectrometer (SERS) and an in-situ Fourier change infrared spectrometer, the neutron reflection spectrometer has the advantages of large sampling, good statistics, sensitivity of neutrons to light elements and the like, and the measurement result is more objective and reliable.
Drawings
Fig. 1 is a schematic diagram of a neutron in-situ device according to an embodiment of the present invention (the left side is a schematic diagram of a longitudinal cross section of the neutron in-situ device, and the right side is a schematic diagram of a structure of the neutron in-situ device after being decomposed), in which a thickness of a first support 1 and a second support 8 of the neutron in-situ device is 0.2mm to 3mm, and is used for measuring a lithium/sodium ion battery solid electrolyte by neutron beam incident from an upper surface of the first support 1;
fig. 2 is a schematic diagram of a neutron in-situ device according to an embodiment of the present invention (the left side is a schematic diagram of a longitudinal cross section of the neutron in-situ device, and the right side is a schematic diagram of a structure of the neutron in-situ device after being decomposed), in which a thickness of a first support 1 and a thickness of a second support 8 of the neutron in-situ device are 8mm to 45mm, and the neutron beam is incident from a side of the first support 1 to measure a lithium/sodium ion battery solid electrolyte;
FIG. 3 is a graph of reflectivity curves of a solid electrolyte interface film of a lithium ion battery obtained from neutron reflectivity test experiments before and after charging of the neutron in-situ device according to an embodiment of the present invention;
in the figure: 1-a first support, 2-a connecting layer, 3-an anode current collector, 4-an anode material, 5-a sealing ring, 6-a cathode material, 7-a cathode current collector, 8-a second support and 9-a cavity.
Detailed Description
The invention is further described below with reference to the figures and examples.
As shown in fig. 1 and 2, the neutron in-situ device provided by the invention comprises a cavity 9 formed by a sealing ring 5, a sheet-shaped positive electrode and a sheet-shaped negative electrode, wherein the cavity 9 is used for containing electrolyte and active substances wrapped by a diaphragm; the positive electrode comprises a first support body 1, a connecting layer 2, a positive current collector 3 and a positive material 4 which are sequentially stacked; the negative electrode comprises a second support body 8, a negative current collector 7 and a negative material 6 which are sequentially stacked; the volume of electrolyte and active substances sealed by a diaphragm is determined by a sealing ring 5, a positive electrode and a negative electrode with current collectors, so that the special battery capable of being penetrated by neutrons to directly measure the solid electrolyte interface film of the lithium/sodium ion battery is formed, and a neutron reflection spectrometer can be used for in-situ measurement of the solid electrolyte interface film of the lithium/sodium ion battery.
The active substance is one of simple substance lithium, simple substance sodium, lithium salt or sodium salt; the electrolyte and the separator are commercial products of lithium/sodium ion batteries, respectively.
In the positive electrode, a first support body 1 is positioned on an opening at one end of a sealing ring 5, a connecting layer 2, a positive current collector 3 and a positive material 4 are positioned in a cavity 9, and the positive material 4 is tightly attached to an electrolyte and an active substance wrapped by a diaphragm;
in the negative electrode, a second support body 8 is positioned on the opening at the other end of the sealing ring 5, a negative current collector 7 and a negative material 6 are positioned inside a cavity 9, and the negative material 6 is tightly attached to the electrolyte and the active material wrapped by the diaphragm.
The first support body 1 and the second support body 8 are monocrystalline silicon wafers or silicon dioxide wafers, and the thickness is 0.2mm-3mm or 8mm-45 mm; the area is 5cm2-100cm2。
The connecting layer 2 is a plating layer arranged on the first support 1, is made of titanium, platinum or chromium, and has a thickness of 2nm-15 nm.
The positive current collector 3 is a plating layer disposed on the connecting layer 2, and is made of gold, platinum or aluminum, and has a thickness of 10nm-60 nm.
The negative current collector 7 is a plating layer disposed on the second support 8, and is made of gold, platinum or copper, and has a thickness of 10nm to 60 nm.
The sealing ring 5 is made of silica gel or polytetrafluoroethyleneThe optimal area enclosed by the alkene material and the sealing ring 5 is 5cm2-80cm2。
The thickness of the anode material 4 and the cathode material 6 is 10nm-100 nm.
And the device also comprises a clamp used for fixing the sealing ring 5, the positive electrode and the negative electrode into a whole.
The device according to the present invention is not limited to the embodiments described in the specific embodiments, and those skilled in the art can derive other embodiments according to the technical solutions of the present invention, and also belong to the technical innovation scope of the present invention.
Claims (10)
1. A neutron normal position device, characterized by: the electrolyte separator comprises a cavity (9) which is formed by a sealing ring (5), a sheet-shaped positive electrode and a sheet-shaped negative electrode, wherein the cavity (9) is used for containing electrolyte and active substances wrapped by a diaphragm; the positive electrode comprises a first support body (1), a connecting layer (2), a positive electrode current collector (3) and a positive electrode material (4) which are sequentially stacked; the negative electrode comprises a second support body (8), a negative current collector (7) and a negative material (6) which are sequentially stacked.
2. The neutron in-situ device of claim 1, wherein: the active substance is simple substance lithium, simple substance sodium, lithium salt or sodium salt.
3. The neutron in-situ device of claim 1, wherein:
in the positive electrode, the first support body (1) is positioned on an opening at one end of the sealing ring (5), and the connecting layer (2), the positive electrode current collector (3) and the positive electrode material (4) are positioned in the cavity (9);
in the negative electrode, the second support body (8) is positioned on the other end opening of the sealing ring (5), and the negative electrode current collector (7) and the negative electrode material (6) are positioned inside the cavity (9).
4. The neutron in-situ device of claim 1, wherein: the first support body (1) and the second support body (8) are singleA crystal silicon wafer or a silicon dioxide wafer, the thickness of which is 0.2mm-3mm or 8mm-45 mm; the area is 5cm2-100cm2。
5. The neutron in-situ device of claim 1, wherein: the connecting layer (2) is a plating layer arranged on the first support body (1), is made of titanium, platinum or chromium, and has a thickness of 2nm-15 nm.
6. The neutron in-situ device of claim 1, wherein: the positive electrode current collector (3) is a plating layer arranged on the connecting layer (2), is made of gold, platinum or aluminum, and has a thickness of 10nm-60 nm.
7. The neutron in-situ device of claim 1, wherein: the negative electrode current collector (7) is a plating layer arranged on the second support body (8), is made of gold, platinum or copper, and has a thickness of 10nm-60 nm.
8. The neutron in-situ device of claim 1, wherein: the sealing ring (5) is made of silica gel or polytetrafluoroethylene, and the optimal area enclosed by the sealing ring (5) is 5cm2-80cm2。
9. The neutron in-situ device of claim 1, wherein: the thickness of the positive electrode material (4) and the negative electrode material (6) is 10nm-100 nm.
10. The neutron in-situ device of claim 1, wherein: the sealing ring device further comprises a clamp used for fixing the sealing ring (5), the positive electrode and the negative electrode into a whole.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010940214.2A CN112151898A (en) | 2020-09-09 | 2020-09-09 | Neutron in-situ device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010940214.2A CN112151898A (en) | 2020-09-09 | 2020-09-09 | Neutron in-situ device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112151898A true CN112151898A (en) | 2020-12-29 |
Family
ID=73890105
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010940214.2A Pending CN112151898A (en) | 2020-09-09 | 2020-09-09 | Neutron in-situ device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112151898A (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9022652B2 (en) * | 2012-09-28 | 2015-05-05 | Uchicago Argonne, Llc | Transmission-geometry electrochemical cell for in-situ scattering and spectroscopy investigations |
| CN104833687A (en) * | 2015-05-06 | 2015-08-12 | 中国工程物理研究院核物理与化学研究所 | Hot stage for small-angle scattering experiment |
| JP6306456B2 (en) * | 2014-07-10 | 2018-04-04 | 国立大学法人北海道大学 | Diagnostic device and diagnostic method |
| CN108398446A (en) * | 2018-05-04 | 2018-08-14 | 中国科学技术大学 | Device in situ for the synchrotron radiation X-ray absorption spectra for testing battery electrode material |
| CN108956666A (en) * | 2018-07-27 | 2018-12-07 | 中国科学院合肥物质科学研究院 | A kind of separation superconducting magnet structure applied to neutron scattering experiment |
| 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 |
| CN110632107A (en) * | 2019-11-12 | 2019-12-31 | 中国工程物理研究院核物理与化学研究所 | All-solid-state battery small-angle neutron scattering test device and use method |
| CN211061445U (en) * | 2019-11-12 | 2020-07-21 | 中国工程物理研究院核物理与化学研究所 | All-solid-state battery small-angle neutron scattering test device |
-
2020
- 2020-09-09 CN CN202010940214.2A patent/CN112151898A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9022652B2 (en) * | 2012-09-28 | 2015-05-05 | Uchicago Argonne, Llc | Transmission-geometry electrochemical cell for in-situ scattering and spectroscopy investigations |
| JP6306456B2 (en) * | 2014-07-10 | 2018-04-04 | 国立大学法人北海道大学 | Diagnostic device and diagnostic method |
| CN104833687A (en) * | 2015-05-06 | 2015-08-12 | 中国工程物理研究院核物理与化学研究所 | Hot stage for small-angle scattering experiment |
| CN108398446A (en) * | 2018-05-04 | 2018-08-14 | 中国科学技术大学 | Device in situ for the synchrotron radiation X-ray absorption spectra for testing battery electrode material |
| CN108956666A (en) * | 2018-07-27 | 2018-12-07 | 中国科学院合肥物质科学研究院 | A kind of separation superconducting magnet structure applied to neutron scattering experiment |
| 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 |
| CN110632107A (en) * | 2019-11-12 | 2019-12-31 | 中国工程物理研究院核物理与化学研究所 | All-solid-state battery small-angle neutron scattering test device and use method |
| CN211061445U (en) * | 2019-11-12 | 2020-07-21 | 中国工程物理研究院核物理与化学研究所 | All-solid-state battery small-angle neutron scattering test device |
Non-Patent Citations (1)
| Title |
|---|
| 韩文泽，魏国海，郭浩，焦学胜，孙凯，陈东风: "《锂离子电池机理研究中的中子粉末衍射技术》", 《中国核科学技术进展报告（第六卷）——中国核学会2019年学术年会论文集第7册（计算物理分卷、核物理分卷、粒子加速器分卷、核聚变与等离子体物理分卷、脉冲功率技术及其应用分卷、辐射物理分卷、核工程力学分卷、核测试与分析分卷）》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP2952307B2 (en) | Apparatus and method for in situ x-ray experiments on chemical cells | |
| CN106645240B (en) | A kind of electrolytic cell reaction chamber and test method for in-situ TiC particles test | |
| JP4784939B2 (en) | Electrochemical infrared spectroscopic apparatus and electrochemical infrared spectroscopic measurement method | |
| CN102980903B (en) | A kind of synchrotron radiation X ray device for analyzing electrode material electrochemical performance and application thereof | |
| CN108827766A (en) | In situ measurement lithium battery active young modulus of material and stress test system and method | |
| CN108987659A (en) | A kind of four electrode system of lithium ion soft-package battery and preparation method thereof | |
| CN110261380A (en) | A kind of in-situ synchronization observation system of lithium ion cell electrode reaction | |
| Wang et al. | In situ neutron techniques for studying lithium ion batteries | |
| CN113702248A (en) | Method for testing wettability of diaphragms made of different materials for lithium ion battery | |
| CN112903539A (en) | Imaging detection device and method for diffusion coefficient of electrolyte of flow battery | |
| JP2015117973A (en) | Sample holder and X-ray analysis method | |
| CN112151898A (en) | Neutron in-situ device | |
| CN110987978A (en) | Device for observing battery pole piece and electrolyte in situ | |
| CN110361337B (en) | Transmission mode electrochemistry normal position optical testing arrangement | |
| RU2654317C1 (en) | Electrochemical cell for reflectometric studies | |
| CN113432766A (en) | Device for in-situ observation of battery operation | |
| Louie | Electrocatalysis in solid acid fuel cells | |
| RU2654314C1 (en) | Electrochemical cell with graphene electrode for in situ research of electrode materials and solid or gel electrolytes | |
| CN111830416A (en) | Device and method for in-situ detection of silicon cathode expansion and failure mechanism of lithium ion battery | |
| CN206849980U (en) | A kind of observation device of electrodes of lithium-ion batteries electrochemical reaction process | |
| CN111122626A (en) | Device for carrying out CT test on battery | |
| Weininger et al. | State‐of‐Charge Indicator for Lead‐Acid Batteries | |
| JPH05129036A (en) | Closed type secondary battery | |
| KR102337139B1 (en) | In-situ cell | |
| CN211627415U (en) | Device for observing battery pole piece and electrolyte in situ |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20201229 |
|
| RJ01 | Rejection of invention patent application after publication |