CN113328149A - Can observe normal position optics comprehensive testing arrangement at solid-state and liquid battery interface - Google Patents
Can observe normal position optics comprehensive testing arrangement at solid-state and liquid battery interface Download PDFInfo
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- CN113328149A CN113328149A CN202010131034.XA CN202010131034A CN113328149A CN 113328149 A CN113328149 A CN 113328149A CN 202010131034 A CN202010131034 A CN 202010131034A CN 113328149 A CN113328149 A CN 113328149A
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- 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
- H01M10/4285—Testing apparatus
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- 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
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention relates to an in-situ optical comprehensive testing device capable of observing solid and liquid battery interfaces, belongs to the technical field of lithium batteries, and solves the problem that the lithium deposition and dissolution behavior of an electrode/electrolyte interface cannot be observed in situ in the prior battery technology. An in-situ optical comprehensive test device capable of observing solid and liquid battery interfaces comprises a battery fixing table, a lower sealing shell and an upper sealing shell; the upper sealing shell and the lower sealing shell are fixedly connected through bolts; the battery fixing table is connected with the lower sealing shell through screws. The invention realizes the assembly and electrochemical test of the solid battery and the liquid battery and correspondingly performs in-situ optical observation of the electrode interface process of different battery systems.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to an in-situ optical comprehensive testing device capable of observing solid and liquid battery interfaces.
Background
Lithium ion batteries are widely used in the field of consumer electronics because of their excellent comprehensive electrochemical properties. The properties of the interface between the positive electrode and the negative electrode in the battery and the electrolyte have important influence on the charge-discharge efficiency, the energy density, the power density, the cyclicity, the service life, the safety, the self-discharge and other characteristics of the lithium ion battery. The interface problem is the core of basic research on lithium ion batteries.
Meanwhile, in recent years, the development of electric automobiles, large-scale energy storage equipment and the like urgently needs secondary lithium batteries with higher power density, higher energy density, longer cycle life and better safety, and solid-state batteries are widely concerned at home and abroad due to the huge potential in the aspects of energy density, safety performance and the like. In the research of solid-state battery technology, the problem of the interface between the electrode and the solid-state electrolyte is still the key and difficult point of research, such as the problems of large interface resistance, volume change and the like. Different types of electrolytes are adopted to assemble the battery, and in-situ observation is realized on the change of the battery interface in the charge-discharge cycle process, so that the method can help us to deeply explore the mechanism and the influence factors of the battery interface problem in the actual process, and further guide the solution of the interface problem in solid and liquid lithium batteries.
The adoption of the metallic lithium with extremely high theoretical specific capacity is an important scheme for improving the energy density of the lithium battery and is a research hotspot in the field of the lithium battery at present. However, in the traditional lithium ion battery, lithium dendrites are easily generated in the metal lithium negative electrode in the circulation process, and if the lithium dendrites fall off from the surface of a battery pole piece to form dead lithium, the effective active lithium content can be reduced, so that the battery capacity is reduced; if the dendrite grows on the surface of the lithium negative electrode and further pierces the separator to contact the positive electrode, the battery is internally short-circuited, and serious fire and even explosion are caused. A solid electrolyte having high mechanical strength can theoretically effectively suppress the penetration of lithium dendrites, but actually the problem of the growth of lithium dendrites still remains and is not completely solved. However, at present, the research on the in-situ process and the reaction mechanism of the electrode interface lithium deposition dissolution in the liquid battery is insufficient, the research on the interface process in the solid battery is quite lacking, the mechanism of the solid electrolyte for inhibiting lithium dendrite is also unclear, and a continuous real-time characterization means is lacking for observing the interface process of the electrode and the electrolyte, so that a simple and effective in-situ observation device matched with various in-situ test means and methods is urgently needed for carrying out in-situ observation on the lithium deposition dissolution behavior of the electrode/electrolyte interface and further researching the influencing factors and the reaction mechanism of the interface process.
Disclosure of Invention
In view of the foregoing analysis, an embodiment of the present invention is directed to provide an in-situ optical comprehensive testing apparatus capable of observing an interface between a solid-state battery and a liquid-state battery, so as to solve the problem that the existing lithium ion battery cannot perform in-situ observation on a lithium deposition and dissolution behavior of an electrode or an electrolyte interface, and further study the influence of the interface process and the reaction mechanism.
The invention is realized by the following technical scheme:
an in-situ optical comprehensive test device capable of observing solid and liquid battery interfaces comprises a battery fixing table, a lower sealing shell and an upper sealing shell; the upper sealing shell and the lower sealing shell are fixedly connected through bolts; the battery fixing table is connected with the lower sealing shell through screws.
Furthermore, the battery fixing table is two surfaces, namely the front surface of the battery fixing table and the back surface of the battery fixing table; the front surface of the battery fixing table comprises an annular liquid groove for assembling a liquid battery; the reverse side of the battery fixing table is a plane and is used for assembling the solid-state battery; a liquid battery quartz plate with gold plated surface is fixed at the center of the bottom of the annular liquid tank on the front surface of the battery fixing table; a solid-state battery quartz plate with gold-plated surface is fixed at the center of the reverse side of the battery fixing table.
Furthermore, a first round hole and a first threaded hole which penetrate through the upper surface and the lower surface of the battery fixing table are respectively formed at two ends of the battery fixing table; the first round hole is used for fixing a battery cathode communicated with the lower sealing shell, and the first threaded hole is used for fixing a battery anode communicated with the upper sealing shell.
Further, the upper sealing shell comprises a first insulating disc, a first sealing ring, a quartz plate, a second sealing ring, a first conductive disc and a third sealing ring; a first observation port is arranged in the center of the first insulating disc, and a second observation port is arranged in the center of the first conductive disc; a first groove for placing a first sealing ring is formed in the center of the lower surface of the first insulating disc; the upper surface of the first conductive disc is provided with a second groove for placing a second sealing ring.
Further, a first conductive disc in the upper sealing shell is connected with a first insulating disc through a bolt; the lower surface of the first conductive disc is connected with the front surface of the battery fixing table, and a third groove for placing a third sealing ring is formed in the lower surface of the first conductive disc;
furthermore, the quartz plate is arranged between the first sealing ring and the second sealing ring.
Further, the first conductive disc is made of stainless steel, and the first insulating disc is made of polytetrafluoroethylene.
Further, the lower sealing shell comprises a second insulating disc and a second conductive disc; the second insulating disc is provided with a cylindrical groove for placing a battery fixing table, the bottom surface of the cylindrical groove is in contact with the reverse side of the battery fixing table, and the bottom surface of the cylindrical groove is provided with a second round hole corresponding to the first round hole of the battery fixing table in position.
Further, the second conductive disc is connected with the second insulating disc through bolts; the second conductive disk is provided with a third threaded hole corresponding to the second round hole of the second insulating disk.
Furthermore, the second conductive disc is made of stainless steel, and the second insulating disc is made of polytetrafluoroethylene.
Compared with the prior art, the invention can realize at least one of the following beneficial effects:
1. the battery testing device provided by the invention designs the front surface and the back surface of the battery fixing table to respectively place the liquid battery and the solid battery. An annular liquid groove is designed on the front surface of the battery fixing table, so that the liquid battery assembling part is skillfully and simply concentrated on the front surface of the battery fixing table; in consideration of the fixity of the solid-state battery, the original plane is reserved on the reverse side of the battery fixing table, the solid-state battery is concentrated on the reverse side of the battery fixing table through the threaded hole and the fixing hole, finally, the solid-state battery and the liquid-state battery can be respectively fixed on the battery fixing table, and the integrated dual-purpose test device is a comprehensive test device capable of supporting in-situ optical observation of electrode interfaces of the solid-state battery (particularly gel electrolyte type batteries) and the liquid-state battery.
2. The battery fixing table enables solid and liquid batteries to be fixed and electrically contacted with the upper and lower sealing shells through screws, simplifies connection of various leads, and enables the whole installation of the device to be simpler and the connection to be stable and reliable.
3. According to the invention, the first insulating disc and the first conducting disc in the upper sealing shell are made of stainless steel or polytetrafluoroethylene materials, the light transmittance is poor, and in order to ensure the permeability of the whole observation light path, the upper sealing shell is provided with the first observation port and the second observation port for observing the charging and discharging behaviors in the liquid battery; a simple plane is arranged on the reverse side of the battery fixing table and in the lower sealing shell for observing the charging and discharging behaviors of the solid battery, so that in-situ optical imaging of a battery interface in the charging and discharging circulation process of the solid and liquid batteries is realized, and the device is applicable to various optical instruments: optical microscope, infrared spectrometer, Raman spectrometer, etc. and has wide application range. The invention has simple integral structure, convenient installation, good sealing performance, safety and stability, thereby being widely applied to the observation and test of solid and liquid batteries.
4. In the application, the first sealing ring and the second sealing ring are arranged in the upper sealing shell to ensure the sealing property of the quartz plate; simultaneously in this application at the lower surface of last seal shell's first electrically conductive disc set up the third sealing washer, guarantee the leakproofness between last seal shell and the lower seal shell, guarantee that the battery reaction reacts under the completely sealed state, guarantee the accuracy of experimental result.
5. In the invention, besides a plurality of sealing rings are arranged to ensure the air tightness of the device, threaded holes arranged in the upper and lower sealing shells are correspondingly arranged and distributed with fixing holes, for example, a first conductive disc is provided with a third fixing hole and a second threaded hole corresponding to the first fixing hole and the second fixing hole, and the first insulating disc and the first conductive disc are fixedly connected through bolts penetrating through the second fixing hole and the second threaded hole; and a fourth fixing hole and a fifth fixing hole are formed in the second insulating disc at intervals, a fourth threaded hole and a fifth threaded hole which correspond to the fourth fixing hole and the fifth fixing hole in position are formed in the second conductive disc, and the second insulating disc and the second conductive disc are fixedly connected through bolts penetrating through the fifth fixing hole and the fifth threaded hole. The air tightness in the whole device assembling process can be fully ensured by the arrangement.
6. A piece of quartz plate with gold-plated surface is fixed at the middle of the front surface and the back surface of the fixing table by double faced adhesive tape, so that the function of reflecting light is achieved, and the brightness and the definition of an optical imaging visual field are improved.
In the invention, the technical schemes can be combined with each other to realize more preferable combination schemes. Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and drawings.
Drawings
The drawings are only for purposes of illustrating particular embodiments and are not to be construed as limiting the invention, wherein like reference numerals are used to designate like parts throughout.
FIG. 1 is a schematic front view of a battery mounting plate according to the present invention;
FIG. 2 is a schematic view of the reverse side of the battery fixing table structure according to the present invention;
FIG. 3 is a schematic structural view of an upper sealing housing according to the present invention;
FIG. 4 is a schematic view of the structure of the lower sealing housing of the present invention;
FIG. 5 is a schematic diagram of an assembly of a liquid cell according to the present invention;
FIG. 6 is a schematic diagram of a solid state battery assembly according to the present invention;
FIG. 7 is an optical image of the growing of lithium dendrites of the solid-state battery according to the present invention.
Reference numerals:
11-battery mounting plate front; 12-the reverse side of the battery fixing table; 13-annular liquid tank; 14-a first circular aperture; 15-a first threaded hole; 21-a first insulating disk; 22-a first sealing ring; 23-quartz plate; 24-a second sealing ring; 25-a first conductive disc; 26-a third seal ring; 211 — a first fixation hole; 212-a second fixation hole; 213-first viewing port; 214-a first groove; 251-a third fixing hole; 252-a second threaded hole; 253-a second viewing port; 254-a second recess; 255-a third groove; 31-a second insulating disk; 32-a second conductive disk; 311-fourth fixing hole; 312-fifth fixation hole; 313-a cylindrical recess; 314-a second circular hole; 321-a fourth threaded hole; 322-fifth threaded hole; 323-third threaded hole; 41-liquid battery negative plate; 42-liquid battery positive plate; 43-liquid state battery quartz plate; 44-solid state battery negative plate; 45-solid-state battery positive plate; 46-solid state battery quartz plate.
Detailed Description
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate preferred embodiments of the invention and together with the description, serve to explain the principles of the invention and not to limit the scope of the invention.
The invention provides an in-situ optical observation solid or liquid battery interface comprehensive testing device which is simple and convenient to operate and easy to assemble for researching the problems, and as shown in figures 1-6, the technical scheme adopted by the invention is as follows: an in-situ optical comprehensive test device capable of observing solid and liquid battery interfaces comprises a battery fixing table, an upper sealing shell and a lower sealing shell; the upper sealing shell and the lower sealing shell are fixedly connected through bolts, and the battery fixing platform is connected with the upper sealing shell and the lower sealing shell through screws to realize fixation; the battery fixing table is used for assembling a battery (comprising a positive electrode, a negative electrode and electrolyte), wherein the negative electrode part of the battery is communicated with the lower sealing shell, and the positive electrode part of the battery is communicated with the upper sealing shell. The invention can respectively realize the assembly and electrochemical test of the solid battery and the liquid battery by replacing the placing modes of the upper sealing shell and the lower sealing shell, and correspondingly carry out in-situ optical observation on the electrode interface process of different battery systems.
The battery fixing table is made of polytetrafluoroethylene materials, as shown in fig. 1 and fig. 2, and comprises a front surface 11 of the battery fixing table and a back surface 12 of the battery fixing table, wherein the front surface 11 of the battery fixing table comprises an annular liquid groove 13 for assembling a liquid battery and observing and testing a liquid battery interface; the back surface 12 of the battery fixing table is a plane and does not contain a ring-shaped liquid groove, and the battery fixing table is used for assembling a solid battery and observing and testing the interface of the solid battery, and the electrolyte of the solid battery comprises organic electrolyte, inorganic electrolyte and inorganic-organic composite electrolyte. The two ends of the battery fixing table are provided with a first round hole 14 and a first threaded hole 15, the first round hole 14 penetrates through the front surface 11 and the back surface 12 of the battery fixing table, the first round hole 14 is used for fixing a battery cathode communicated with the lower sealing shell, and the first threaded hole 15 is used for fixing a battery anode communicated with the upper sealing shell.
The upper sealing shell comprises a first insulating disc 21, a first sealing ring 22, a quartz plate 23, a second sealing ring 24, a first conductive disc 25 and a third sealing ring 26; a first observation port 213 is arranged at the center of the first insulating disk 21, and a first groove 214 is arranged at the center of the lower surface of the first insulating disk 21 and used for placing the first sealing ring 22 and the second sealing ring 24;
the first conductive disc 25 is connected with the first insulating disc 21 through bolts, a second observation port 253 is arranged in the center of the first conductive disc 25, the lower surface of the first conductive disc is in contact with the upper surface of the battery fixing table, and grooves for placing the first sealing ring 22 and the second sealing ring 24 are formed in the upper surface of the first conductive disc; the lower surface of the first conductive disc is provided with a second groove 254 for placing a third sealing ring; the quartz plate 23 is arranged between the first observation port 213 and the second observation port 253 of the first insulating disc and the first conductive disc, the quartz plate 23 is arranged between the first sealing ring 22 and the second sealing ring 24, the first sealing ring is positioned on the upper surface of the quartz plate 23, and the second sealing ring 24 is positioned on the lower surface of the quartz plate; a third seal 26 is provided where the first conductive disc 25 and the second insulating disc 31 meet.
The first conductive disc is made of stainless steel, and the first insulating disc is made of polytetrafluoroethylene.
The lower sealed shell comprises a second insulating disk 31 and a second conductive disk 32; the second insulating disc 31 is provided with a cylindrical groove 313 for placing a battery fixing table, the bottom surface of the cylindrical groove is in contact with the reverse side of the battery fixing table, and the bottom surface of the cylindrical groove 313 is provided with a second round hole 314 corresponding to the first round hole of the battery fixing table; the second conductive disk 32 is connected with the second insulating disk 31 by bolts, and the second conductive disk is provided with a third threaded hole 323 corresponding to the second round hole 314 of the second insulating disk;
the second conductive disc is made of stainless steel, and the second insulating disc is made of polytetrafluoroethylene.
The invention provides a comprehensive testing device for in-situ optical observation of solid and liquid battery interfaces, which comprises a battery fixing table, an upper sealing shell and a lower sealing shell, wherein the upper sealing shell and the lower sealing shell are fixedly connected through bolts, and the battery fixing table and the lower sealing shell are fixedly connected through bolts. The battery fixing table is used for assembling and fixing a battery structure, communicating the positive electrode part of the solid-state battery with the upper sealing shell and communicating the negative electrode part of the solid-state battery with the lower sealing shell.
As shown in fig. 1, the battery holder is an insulating cylinder, and includes a front surface 11 and a back surface 12. The battery fixing table front 11 is used for observing and measuring the liquid battery and comprises an annular liquid tank 13 for containing liquid electrolyte; the back surface 12 of the battery fixing table is a plane, does not contain an annular liquid groove and is used for assembling and placing a gel electrolyte type solid battery, and the gel electrolyte before solidification is quantitatively dripped in the central position of the back surface 12 of the battery fixing table; near the both ends of cyclic annular liquid groove 13 seted up one respectively and run through its tow sides first round hole 14 and first screw hole 15, first round hole 14 is used for fixed battery negative pole (including liquid battery and solid-state battery) that are linked together with lower seal shell, and first screw hole 15 is used for fixed battery positive pole (including liquid battery and solid-state battery) that are linked together with last seal shell.
As shown in fig. 3, the upper sealing case includes first insulating and conductive disks 21 and 25, a quartz plate 23, a first sealing ring 22, a second sealing ring 24, and a third sealing ring 26. A first observation port 213 is arranged at the center of the first insulating disk 21, and a first groove 214 for placing a small sealing ring is arranged at the center of the lower surface of the first conductive disk 25; the first conductive disc 25 is connected with the first insulating disc 21 through bolts, a second observation port 253 is arranged in the center of the first conductive disc 25, a groove for placing the second sealing ring 24 is formed in the upper surface of the first conductive disc 25, and a third groove 255 for placing the third sealing ring 26 is formed in the lower surface of the first conductive disc 25; the quartz plate 23 is disposed between the first viewing port 213 and the second viewing port 253 of the first insulating disk 21 and the first conductive disk 25; the first sealing ring 22 is arranged in the first groove 214 on the lower surface of the first insulating disk 21, and the second sealing ring 24 is arranged in the second groove 254 on the upper surface of the first conductive disk 25; the third seal ring 26 is disposed in a third groove 255 in the lower surface of the first conductive disk 25 in contact with a second insulating disk 31 described below.
As shown in fig. 4, the lower sealed housing includes a second insulating disk 31, a second conductive disk 32. The center of the second insulating disk 31 is provided with a cylindrical groove 313 for placing the battery fixing table, the bottom of the cylindrical groove 313 is contacted with the reverse surface 12 of the battery fixing table, and a second round hole 314 corresponding to the first round hole 14 of the battery fixing table is arranged in the cylindrical groove 313 of the second insulating disk 31 near the center. The second conductive disk 32 is bolted to the second insulating disk 31, and the second conductive disk 32 is provided with a third threaded hole 323 corresponding to the first round hole 14 and the second round hole 314.
In the above embodiment, the battery fixing table is made of teflon, the first insulating disk 21 is made of teflon, the first conductive disk 25 is made of stainless steel, the second insulating disk 31 is made of teflon, and the second conductive disk 32 is made of stainless steel.
In the above embodiments, the first insulating disk 21 is provided with the first fixing hole 211 and the second fixing hole 212 at intervals, the first conductive disk 25 is provided with the third fixing hole 251 and the second threaded hole 252 corresponding to the first fixing hole 211 and the second fixing hole 212, and the first insulating disk 21 and the first conductive disk 25 are fixedly connected by the bolt passing through the second fixing hole 212 and the second threaded hole 252.
In the above embodiments, the second insulating disk 31 is provided with the fourth fixing hole 311 and the fifth fixing hole 312 at intervals, the second conductive disk 32 is provided with the fourth threaded hole 321 and the fifth threaded hole 322 corresponding to the fourth fixing hole 311 and the fifth fixing hole 312, and the second insulating disk 31 and the second conductive disk 32 are fixedly connected by the bolt passing through the fifth fixing hole 312 and the fifth threaded hole 322.
In order to improve the brightness of the optical imaging field of vision, the invention is realized by arranging a quartz plate on the battery fixing table, as shown in fig. 5, the liquid battery adopts a battery fixing table front face 11, and the center of an annular liquid groove 13 of the battery fixing table front face 11 is fixed with a gold-plated liquid battery quartz plate 43 by a double-sided adhesive tape. As shown in fig. 6, the solid-state battery employs a battery holder back side 12 which is placed upside down in a cylindrical recess 313 in the center of the second insulating disk 31. The center of the back surface 12 of the battery fixing table is fixed with a solid-state battery quartz plate 46 with gold plating on the surface by using double-sided adhesive tape.
In order to ensure the insulation property of the battery, one end of the liquid battery negative plate 41 is fixed near the first round hole 14 of the battery fixing table through a double-sided adhesive tape, and a current collector of a small piece of negative electrode is cut to cover the end of the liquid battery negative plate 41; one end of the liquid battery positive plate 42 is fixed on the threaded hole 15 of the battery fixing table through a double-sided adhesive tape. One end of the solid-state battery negative plate 44 is fixed near the first round hole 14 of the battery fixing table through double-sided adhesive tape, and the current collector of the cut small negative electrode covers the upper surface of the end of the negative plate; the other end of the positive electrode sheet 45 of the solid-state battery is extended to the vicinity of the center of the reverse surface, opposite to but spaced apart from the negative electrode sheet 44 of the solid-state battery.
The working principle of the invention is as follows: for the operation principle of the liquid battery, as shown in fig. 5, the battery holder is placed with the front side 11 of the battery holder facing upward in the cylindrical groove 313 in the center of the second insulating disk 31. The center of the bottom of the annular liquid groove 13 on the front surface 11 of the battery fixing table is fixed with a liquid battery quartz plate 43 with gold plated surface by a double-sided adhesive tape so as to improve the brightness of the optical imaging visual field. Then, assembling the battery, fixing one end of the liquid battery negative plate 41 near the first round hole 14 of the battery fixing table through a double-sided adhesive tape, cutting a small negative current collector to cover the upper surface of the end of the liquid battery negative plate 41, sequentially penetrating the negative current collector, the first round hole 14, the second round hole 314 and the third threaded hole 323 through long screws, fixing the battery fixing table to the lower sealing shell, and fixing and communicating the whole negative part of the battery to the second conductive disc 32; in order to prevent the negative electrode part of the battery from contacting the first conductive disc 25 in the whole device assembling process, a small section of double-sided adhesive needs to be covered on the long screw nut so as to ensure that the negative electrode part is completely insulated from the first conductive disc 25; the other end of the negative electrode sheet is bent and then placed in the annular liquid tank 13. Fixing one end of a liquid battery positive plate 42 near a threaded hole 15 of a battery fixing table through double faced adhesive tape, cutting a small piece of positive current collector to cover the negative plate, sequentially penetrating the positive current collector and the first threaded hole 15 through short screws, fixing the battery positive part on the battery fixing table, bending the other end of the liquid battery positive plate 42, placing the bent end in an annular liquid groove 13, and placing the bent end opposite to the liquid battery negative plate 41 with a certain distance. The two oppositely arranged positive and negative plates in the annular liquid tank 13 are opposite to the first observation port 213 and the first observation port 253 of the first insulating disk 21 and the first conductive disk 25 in the upper sealed shell, so that the positive and negative electrodes and the electrolyte interface can be observed by an optical microscope. And a proper amount of electrolyte is dripped into the annular liquid tank 13, and the amount of the electrolyte ensures that the oppositely arranged positive and negative electrode parts in the annular liquid tank 13 can be immersed.
The battery operating principle of a solid-state battery is substantially the same as that of a liquid-state battery, and there are some differences in detail. As shown in fig. 6, the solid-state battery employs a battery holder back side 12 which is placed upside down in a cylindrical recess 313 in the center of the second insulating disk 31. The center of the back surface 12 of the battery fixing table is fixed with a solid-state battery quartz plate 46 with gold plating on the surface by a double-sided adhesive tape so as to improve the brightness of the optical imaging visual field. Then, assembling the battery, namely fixing one end of a solid-state battery negative plate 44 near the first round hole 14 of the battery fixing table through a double-sided adhesive tape, cutting a small negative current collector to cover the negative plate, sequentially penetrating the negative current collector, the first round hole 14, the second round hole 314 and the third threaded hole 323 through long screws, fixing the battery fixing table on the lower sealed shell, and fixing and communicating the whole negative part of the battery to the second conductive disc 32; in order to prevent the negative electrode part of the battery from contacting the first conductive disc 25 in the whole device assembling process, a small section of double-sided adhesive needs to be covered on the long screw nut so as to ensure that the negative electrode part is completely insulated from the first conductive disc 25; the other end of the solid-state battery negative electrode sheet 44 is extended to the vicinity of the center of the reverse surface. Fixing one end of a solid-state battery positive plate 45 near a first threaded hole 15 of a battery fixing table through a double-sided adhesive tape, cutting a small piece of positive current collector to cover the negative plate, sequentially penetrating the positive current collector and the first threaded hole 15 through short screws, fixing the battery positive part on the battery fixing table, extending the other end of the solid-state battery positive plate 45 to the vicinity of the center of the reverse side, and keeping a certain distance from the solid-state battery negative plate 44. The two oppositely arranged positive and negative plates in the annular liquid tank 13 are opposite to the first observation port 213 and the second observation port 253 of the first insulating disk 21 and the first conductive disk 25 in the upper sealed shell, so that the positive and negative electrodes and the electrolyte interface can be observed by an optical microscope. And a proper amount of gel electrolyte before curing is dripped into the center of the back surface, and the amount of the gel electrolyte ensures that the positive and negative electrode parts near the center of the back surface can be soaked.
The assembly of the upper sealing case is performed by assembling the first insulating disk 21, the sealing ring 22, the quartz plate 23, the sealing ring 24, the first conductive disk 25 and the third sealing ring 26 in this order, and aligning the second fixing hole 212 and the second screw hole 252 to be fixed together by screws.
The assembly of the lower hermetic case is performed by fixing the second insulating disk 31 and the second conductive disk 32 together through the fifth fixing hole 312 and the fifth screw hole 322.
The assembled liquid or solid battery is fixed to the second conductive disc 32 in the lower sealed shell by screws passing through the first round hole 14 on the battery fixing table, the second round hole 314 in the cylindrical groove of the second insulating disc 31 and the third threaded hole 323 on the second conductive disc 32, and the negative part of the liquid or solid battery is in electrical contact with the second conductive disc 32 in the lower sealed shell.
And (3) placing a third sealing ring 26 in a third groove 255 reserved in the first conductive disc 25 in the upper sealing shell, finally covering the upper sealing shell, and sequentially passing through the first fixing hole 211 on the first insulating disc 21, the third fixing hole 251 on the first conductive disc 25, the fourth fixing hole 311 on the second insulating disc 31 and the fourth threaded hole 321 on the second conductive disc 32 by using screws, so that the whole observation device can be fixed, and when the sealing ring 26 is pressed, the positive electrode part of the liquid or solid battery is contacted with the first conductive disc 25 in the upper sealing shell through the screws inserted into the first threaded hole 15 on the battery fixing table.
And leads which are respectively communicated with the anode and the cathode are respectively connected from the first conductive disk 25 and the second conductive disk 32, so that a series of electrochemical tests can be carried out on the liquid or solid battery. When the electrochemical test is carried out, the device is placed under an optical microscope lens, and the in-situ observation of the electrode/electrolyte interface of the liquid or solid battery can be realized through the first observation port 213 and the second observation port 253 on the upper sealing shell and the transparent quartz plate 23, so that the in-situ process of lithium deposition and dissolution of the cathode and the electrolyte interface in the liquid or solid battery can be obtained. As shown in fig. 7, in the battery interface reaction of the solid-state battery, metallic lithium is deposited on the surface of the copper sheet, and lithium dendrite is generated when lithium is deposited to a certain extent.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (10)
1. An in-situ optical comprehensive testing device capable of observing solid and liquid battery interfaces is characterized by comprising a battery fixing table, a lower sealing shell and an upper sealing shell; the upper sealing shell and the lower sealing shell are fixedly connected through bolts; the battery fixing table is connected with the lower sealing shell through screws.
2. The in-situ optical integrated test device for observing the interface between a solid battery and a liquid battery according to claim 1, wherein the battery fixing platform has two surfaces, namely a front surface of the battery fixing platform and a back surface of the battery fixing platform; the front surface of the battery fixing table comprises an annular liquid groove for assembling a liquid battery; the reverse side of the battery fixing table is a plane and is used for assembling the solid-state battery; a liquid battery quartz plate with gold plated surface is fixed at the center of the bottom of the annular liquid tank on the front surface of the battery fixing table; a solid-state battery quartz plate with gold-plated surface is fixed at the center of the reverse side of the battery fixing table.
3. The in-situ optical comprehensive test device for observing the interfaces of the solid and liquid batteries according to claim 2, wherein the two ends of the battery fixing platform are respectively provided with a first round hole and a first threaded hole which penetrate through the upper surface and the lower surface of the battery fixing platform; the first round hole is used for fixing a battery cathode communicated with the lower sealing shell, and the first threaded hole is used for fixing a battery anode communicated with the upper sealing shell.
4. The in-situ optical integrated test apparatus for observing solid and liquid battery interfaces as claimed in claim 3, wherein the upper sealing housing comprises a first insulating disk, a first sealing ring, a quartz plate, a second sealing ring, a first conductive disk and a third sealing ring; a first observation port is arranged in the center of the first insulating disc, and a second observation port is arranged in the center of the first conductive disc; a first groove for placing a first sealing ring is formed in the center of the lower surface of the first insulating disc; the upper surface of the first conductive disc is provided with a second groove for placing a second sealing ring.
5. The in-situ optical integrated test apparatus for observing solid and liquid battery interfaces as claimed in claim 4, wherein the first conductive disk and the first insulating disk in the upper sealed housing are bolted together; the lower surface of the first conductive disc is connected with the front surface of the battery fixing table, and a third groove for placing a third sealing ring is formed in the lower surface of the first conductive disc.
6. The apparatus of claim 5, wherein the quartz plate is disposed between the first and second seal rings.
7. The integrated in-situ optical testing device for observing solid and liquid battery interfaces as claimed in claim 6, wherein the first conductive disk is stainless steel and the first insulating disk is ptfe.
8. The in-situ optical integrated test device for observable solid and liquid battery interfaces of claim 1, wherein the lower hermetic shell comprises a second insulating disk, a second conductive disk; the second insulating disc is provided with a cylindrical groove for placing a battery fixing table, the bottom surface of the cylindrical groove is in contact with the reverse side of the battery fixing table, and the bottom surface of the cylindrical groove is provided with a second round hole corresponding to the first round hole of the battery fixing table in position.
9. The in-situ optical integrated test apparatus for observing solid and liquid battery interfaces as claimed in claim 8, wherein the second conductive disk is bolted to the second insulating disk; the second conductive disk is provided with a third threaded hole corresponding to the second round hole of the second insulating disk.
10. The in-situ optical integrated test device capable of observing solid and liquid battery interfaces of claim 9, wherein the second conductive disk is stainless steel and the second insulating disk is ptfe.
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| CN202010131034.XA CN113328149A (en) | 2020-02-28 | 2020-02-28 | Can observe normal position optics comprehensive testing arrangement at solid-state and liquid battery interface |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115275308A (en) * | 2022-08-11 | 2022-11-01 | 扬州大学 | Integrated forming device of flexible surface type solid-state battery and working method thereof |
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2020
- 2020-02-28 CN CN202010131034.XA patent/CN113328149A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115275308A (en) * | 2022-08-11 | 2022-11-01 | 扬州大学 | Integrated forming device of flexible surface type solid-state battery and working method thereof |
| CN115275308B (en) * | 2022-08-11 | 2023-03-14 | 扬州大学 | Integrated forming device of flexible surface type solid-state battery and working method thereof |
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