CN210775224U - Battery electrochemistry normal position raman spectroscopy test mould - Google Patents

Battery electrochemistry normal position raman spectroscopy test mould Download PDF

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CN210775224U
CN210775224U CN201921255968.3U CN201921255968U CN210775224U CN 210775224 U CN210775224 U CN 210775224U CN 201921255968 U CN201921255968 U CN 201921255968U CN 210775224 U CN210775224 U CN 210775224U
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window
electrode plate
battery
raman spectroscopy
plate electrode
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王亮
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Beijing Zhongke Wanyuan Technology Co Ltd
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Beijing Zhongke Wanyuan Technology Co Ltd
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Abstract

The utility model provides a battery electrochemistry normal position raman spectroscopy test mold, including the work plate electrode, there is the air inlet on the lateral wall of work plate electrode, the gas outlet, the top of work plate electrode is opened downwards has the window recess that holds the window board, the top of window recess is sealed through the top of apron with the work plate electrode, the bottom of work plate electrode is inwards opened and is held the anodal material and coat the board, the recess of isolating ring, the isolating ring is fixed at the top of reference plate electrode, the dead lever of work plate electrode bottom passes the reference plate electrode, use the bolt fastening behind the through-hole on the plate electrode, the work plate electrode, the isolating ring, the central point of reference plate electrode puts to open in proper order has the window through-hole that is located on the same axis, keep apart the. Test mould, can carry out normal position raman spectrum test under the electrochemistry condition to metal ion battery and metal air battery, safety, gas tightness are high, dismantle convenient, dismantle the convenience.

Description

Battery electrochemistry normal position raman spectroscopy test mould
Technical Field
The utility model belongs to battery normal position test mould field especially relates to a battery electrochemistry normal position raman spectroscopy test mould.
Background
The electrode material is an important component of the novel ion battery, the physical structure, chemical composition and stress of the electrode material in the electrochemical charging and discharging process are comprehensively researched systematically, and the evolution and aging mechanism of the electrode material in the charging and discharging process is explored, so that the electrode material is a premise for further improving the battery performance. The Raman spectrum technology can obtain the composition and structure of a substance by detecting the vibration of molecules, and can directly obtain the composition and structure information of the substance on an electrode reaction interface layer in the reaction process, so that the Raman spectrum technology is an important analysis method applied to molecular structure research.
At present, most of Raman spectrum detection of the metal-air battery is ex-situ, and only an in-situ detection mold is ventilated from a lower layer, so that reaction gas is in contact with metal to generate danger, and the metal-air battery has great potential safety hazard. In addition, the existing in-situ detection mold is not easy to disassemble and has poor sealing performance. Therefore, an in-situ Raman spectrum test of the metal-air battery under the electrochemical condition by using the test mold which has a stable structure, high air tightness and convenient disassembly and maintenance is urgently needed.
Disclosure of Invention
In view of this, the utility model aims at providing a battery electrochemistry normal position raman spectroscopy test mould can carry out normal position raman spectroscopy test under the electrochemistry condition to metal ion battery and metal air battery, and safety, gas tightness are high, the dismantlement is convenient.
In order to achieve the above purpose, the technical scheme of the utility model is realized like this:
the utility model provides a battery electrochemistry normal position raman spectroscopy test mold, including the work electrode board, there is the air inlet on the lateral wall of work electrode board, the gas outlet, the top of work electrode board is opened downwards has the window recess that holds the window board, the top of window recess is sealed through the top of apron with the work electrode board, the bottom of work electrode board is inwards opened has and is held anodal material coating board, the recess of isolating ring, the isolating ring is fixed at the top of reference electrode board, the dead lever of work electrode board bottom passes the reference electrode board, use the bolt fastening behind the through-hole on the counter electrode board, the work electrode board, the isolating ring, the central point of reference electrode board puts to open in proper order has the window through-hole that is located the same axis.
Furthermore, the air inlet and the air outlet are used for introducing reaction gas into the testing mold, and are suitable for Raman spectrum testing of metal air batteries, particularly lithium air batteries.
Further, the reaction gas to be introduced is preferably oxygen gas.
Further, the isolation ring is preferably made of polytetrafluoroethylene material.
Furthermore, the bottom of the reference electrode plate is provided with an annular outer groove and an annular inner groove which are used for accommodating the sealing ring, and the inner diameters of the outer groove and the inner groove are both larger than the inner diameter of the middle through hole.
Furthermore, the inner diameters of the middle through hole and the isolation through hole are larger than that of the window through hole.
Further, the area of the window plate is not smaller than the hole area of the window through hole.
Further, the vertical height of the isolating ring is not larger than that of the groove.
Furthermore, the bottom surface of the reference electrode plate is sequentially in contact connection with the battery and the top surface of the clamping cap, a clamping cap groove is formed in the bottom of the clamping cap inwards, a spring is arranged in the clamping cap groove, and the spring is in contact connection with the counter electrode plate.
Further, the positive electrode material coating plate is preferably an aluminum foil coated with a positive electrode material.
Further, the battery is sequentially assembled according to the sequence of aluminum foil, diaphragm, electrolyte and metallic lithium.
Further, the thickness of the battery electrochemical in-situ Raman spectrum testing mold is 17-30mm, and the temperature of the battery electrochemical in-situ Raman spectrum testing mold does not exceed 200 ℃.
Further, the thickness of more than 30mm is bulky and not suitable for the height of the diffractometer; if the thickness is less than 17mm, the internal space of the battery is compressed, the stress increases, and the mold having a thickness less than 17mm is easily deformed.
Further, the window plate is preferably a window plate made of sapphire or quartz glass.
Furthermore, the material of the window plate can be replaced and optimized according to different excitation wavelengths and purposes.
Furthermore, the outer walls of the working electrode plate and the counter electrode plate are respectively provided with a connecting wire contact port.
Furthermore, the connecting wire contact ports are respectively connected with the testing wires of the Raman spectrum testing instrument.
Compared with the prior art, the battery electrochemistry normal position Raman spectrum testing mold has the following advantages:
(1) the battery electrochemistry in-situ Raman spectrum testing mold of the utility model is widely applicable to various lithium ion battery anodes/cathodes; the positive/negative electrode material of the sodium ion battery and the positive/negative electrode material of the potassium ion battery are subjected to electrochemical in-situ Raman spectrum research in the charging and discharging process, and phase change research in the cyclic voltammetry and linear scanning voltammetry processes can be tested.
(2) Battery electrochemistry normal position raman spectroscopy test mould, but compatible lithium electricity, two kinds of modes of lithium sky are used, adopt the mode of ventilating to carry out the reaction of ventilating, both can make electrode material and reaction gas carry out the contact reaction, thereby can prevent again that gaseous and metal (for example lithium) contact from producing danger.
(3) Among the battery electrochemistry normal position raman spectroscopy test mould, there is the sealing washer reference plate's bottom, the unique design of double seal circle makes the leakproofness of mould better.
(4) Battery electrochemistry normal position raman spectroscopy test mould, easy and simple to handle, small in size, make things convenient for the dismouting, can change the window material as required.
(5) In battery electrochemistry normal position raman spectroscopy test mould, built-in spring and card cap between reference electrode board and the counter electrode board, can effectively utilize the spring to adjust the inside thickness of battery, ensure that the electrode contact is good to highly making it be applicable to multiple raman detection device through the spring adjustment battery.
(6) In the battery electrochemical in-situ Raman spectrum testing mold, the isolating ring is arranged between the working electrode plate and the reference electrode plate, on one hand, the gap between the inside of the battery and the shell is filled to ensure insulativity, and short circuit is not easy to occur; on the other hand, the coating is resistant to acid, alkali, organic solvent and high temperature.
(7) Among the battery electrochemistry normal position raman spectroscopy test mold, the window board that sapphire, quartz glass made has high light transmissivity, the little advantage of signal loss, reduces the signal loss in the use.
Drawings
The accompanying drawings, which form a part hereof, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention without undue limitation. In the drawings:
fig. 1 is a side-view exploded view of a test mold according to an embodiment of the present invention;
fig. 2 is a side view of a test mold according to an embodiment of the present invention;
fig. 3 is a top view of the testing mold according to the embodiment of the present invention.
Description of reference numerals:
1-an air inlet; 2-a working electrode plate; 3-window through holes; 4-a window plate; 5-coating a positive electrode material on a plate; 6-a spacer ring; 7-cover plate; 8-a reference electrode plate; 9-a battery; 10-a clamping cap; 11-a spring; 12-a pair of electrode plates; 13-a middle through opening; 14-isolating vias; 15-a groove; 16-an air outlet; 17-outer groove; 18-an inner groove; 19-fixing the rod.
Detailed Description
It should be noted that, in the present invention, the embodiments and features of the embodiments may be combined with each other without conflict.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are used merely for convenience of description and for simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be construed as limiting the present invention. Unless expressly stated or limited otherwise, the terms "mounted," "connected," and "connected" are intended to be inclusive and mean, for example, that they may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
The present invention will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
As shown in fig. 1, fig. 2 and fig. 3, the in-situ raman spectroscopy testing mold for electrochemical cell comprises a working electrode plate 2, wherein an air inlet 1 and an air outlet 16 are formed in the outer side wall of the working electrode plate 2, a window groove for accommodating a window plate 4 is formed downwards in the top of the working electrode plate 2, and the top of the window groove is sealed with the top of the working electrode plate 2 through a cover plate 7. The area of the window plate 4 is not less than the hole area of the window through hole 3. Ensuring that the X-ray can penetrate through the window plate 4 and the window through hole 3 and then irradiate on the anode material.
The window plate 4 is preferably a window plate 4 made of sapphire, quartz glass. The material of the window plate 4 can be changed and optimized according to different excitation wavelengths and purposes. The window plate 4 made of sapphire or quartz glass has the advantages of high light transmittance and small signal loss, and reduces the signal loss in the use process.
The air inlet 1 and the air outlet 16 are used for introducing reaction gas into the testing mold, and are suitable for Raman spectrum testing of metal air batteries, particularly lithium air batteries.
After the battery mold is assembled, the reaction gas is introduced from the gas inlet 1, so that the gas is in contact with the anode material on the anode material coating plate 5, and the gas flows out from the gas outlet 16 after the contact reaction. The positive electrode material coating plate 5, the isolating ring 6 and the reference electrode plate 8 are tightly pressed, so that gas cannot flow into the lower layer of the die and cannot contact with metal of the lower layer, and the die is very safe.
The ventilation mode can be compatible with the lithium battery, the lithium battery is used in a lithium air mode, the in-situ XRD of the lithium battery can be detected when the ventilation mode is not used, and the application range is wide.
The bottom of the working electrode plate 2 is provided with a groove 15 inwards for accommodating the anode material coating plate 5 and the spacer ring 6, and the spacer ring 6 is fixed on the top of the reference electrode plate 8. The central positions of the isolating ring 6 and the reference electrode plate 8 are sequentially provided with a window through hole 3, an isolating through hole 14 and a middle through hole 13 which are positioned on the same axis. The spacer ring is preferably a spacer ring made of a polytetrafluoroethylene material. The vertical height of the spacer ring 6 is not greater than the vertical height of said groove 15. The inner diameters of the middle through hole 13 and the isolation through hole 14 are larger than the inner diameter of the window through hole 3.
The spacer ring 6 is inserted into the recess 15 of the working electrode plate 2 in such a way that the contact connection provides a better sealing of the die and allows air to be squeezed out of it. An isolating ring 6 is arranged between the working electrode plate 2 and the reference electrode plate 8, so that on one hand, gaps between the interior of the battery and the shell are filled to ensure insulativity, and short circuit is not easy to occur; on the other hand, the coating is resistant to acid, alkali, organic solvent and high temperature.
The positive electrode material coating plate 5 is preferably an aluminum foil coated with a positive electrode material.
The fixing rod 19 at the bottom of the working electrode plate 2 penetrates through the through holes in the reference electrode plate 8 and the counter electrode plate 12 and then is fixed by using bolts, and the bolts are connected to enable the die to be simple and convenient to operate and disassemble and assemble, so that window materials can be conveniently replaced as required.
The bottom of the reference electrode plate 8 is provided with an annular outer groove 17 and an annular inner groove 18 for accommodating a sealing ring, and the inner diameters of the outer groove 17 and the inner groove 18 are both larger than the inner diameter of the middle through hole 13. The unique design of the double sealing rings enables the sealing performance of the die to be better.
The bottom surface of the reference electrode plate 8 is sequentially in contact connection with the battery 9 and the top surface of the clamping cap 10, a clamping cap groove is formed in the bottom of the clamping cap 10 inwards, a spring 11 is arranged in the clamping cap groove, and the spring 11 is in contact connection with the counter electrode plate 12. The battery 9 is a battery 9 assembled in sequence of aluminum foil, diaphragm, electrolyte and metallic lithium.
A spring 11 and a clamping cap 10 are arranged between the reference electrode plate 8 and the counter electrode plate 12, the internal thickness of the battery can be effectively adjusted by using the spring 11, good electrode contact is ensured, and the height of the battery is adjusted by the spring 11 so that the battery is suitable for various Raman detection devices. And the spring 11 can press the gap between the battery 9 and the reference electrode plate 8 to remove air therein.
The thickness of the battery electrochemical in-situ Raman spectrum testing mold is 17-30mm, and the temperature of the mold can not exceed 200 ℃. The thickness is larger than 30mm, the volume is heavy, and the height of the diffractometer is not suitable; if the thickness is less than 17mm, the internal space of the battery is compressed, the stress increases, and the mold having a thickness less than 17mm is easily deformed.
And the outer walls of the working electrode plate 2 and the counter electrode plate 12 are provided with connecting wire contact ports. And the connecting wire contact ports are respectively connected with the testing wires of the Raman spectrum testing instrument.
The test mould has smaller size and is more convenient to use. The lithium ion battery anode/cathode is widely applicable to various lithium ion batteries; the positive/negative electrode material of the sodium ion battery and the positive/negative electrode material of the potassium ion battery are subjected to electrochemical in-situ Raman spectrum research in the charging and discharging process, and phase change research in the cyclic voltammetry and linear scanning voltammetry processes can be tested.
The specific using process is as follows:
and preparing a positive electrode material, coating the positive electrode material on the aluminum foil to prepare a positive electrode material coating plate 5, wherein the coating area of the positive electrode material is larger than that of the window through hole 3. And drying the aluminum foil of the coating in vacuum, and cutting the aluminum foil into a size corresponding to the bottom surface of the groove 15. The positive electrode material coating plate 5 is placed in the groove 15 of the working electrode plate 2 and is pressed tightly by using the spacer ring 6 on the reference electrode plate 8.
And sequentially assembling the aluminum foil, the diaphragm, the electrolyte and the metal lithium to form a battery 9, contacting the battery 9 with the bottom surface of a reference electrode plate 8, then pressing a clamping cap 10 and a spring 11, finally adding a counter electrode plate 12, screwing a fixing rod for fixing the working electrode plate 2 by using a bolt, and completing the assembly of the die. The mold was placed under the confocal micro-raman spectrum, the test line was attached, focused using a laser, and the test was started after the signal from the sample was collected.
When the Raman spectrum test of the lithium air battery material is carried out, the air inlet 1 and the air outlet 2 are opened after the die assembly is completed, so that the gas is in contact reaction with the anode material, and the test is started after a period of time.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. The utility model provides a battery electrochemistry normal position raman spectroscopy test mould which characterized in that: the device comprises a working electrode plate (2), wherein an air inlet (1) and an air outlet (16) are formed in the outer side wall of the working electrode plate (2), a window groove for accommodating a window plate (4) is formed in the top of the working electrode plate (2) downwards, a cover plate (7) is sealed with the top of the working electrode plate (2) through the top of the window groove, a groove (15) for accommodating a positive electrode material coating plate (5) and an isolating ring (6) is formed in the bottom of the working electrode plate (2) inwards, the isolating ring (6) is fixed at the top of a reference electrode plate (8), a fixing rod (19) at the bottom of the working electrode plate (2) penetrates through the reference electrode plate (8), the fixing rod is fixed by using bolts after through holes in a counter electrode plate (12), window through holes (3) located on the same axis are sequentially formed in the center positions of the working electrode plate (2), the isolating ring (, A middle through opening (13).
2. The in-situ raman spectroscopy testing mold for electrochemical cells of claim 1, wherein: the bottom of the reference electrode plate (8) is provided with an annular outer groove (17) and an annular inner groove (18) which are used for accommodating a sealing ring, and the inner diameters of the outer groove (17) and the inner groove (18) are both larger than the inner diameter of the middle through hole (13).
3. The in-situ raman spectroscopy testing mold for electrochemical cells of claim 1, wherein: the inner diameters of the middle through hole (13) and the isolation through hole (14) are larger than the inner diameter of the window through hole (3).
4. The in-situ raman spectroscopy testing mold for electrochemical cells of claim 1, wherein: the area of the window plate (4) is not smaller than the hole area of the window through hole (3).
5. The in-situ raman spectroscopy testing mold for electrochemical cells of claim 1, wherein: the vertical height of the isolating ring (6) is not more than that of the groove (15).
6. The in-situ raman spectroscopy testing mold for electrochemical cells of claim 1, wherein: the bottom surface of the reference electrode plate (8) is sequentially in contact connection with the top surfaces of the battery (9) and the clamping cap (10), a clamping cap groove is formed in the bottom of the clamping cap (10) inwards, a spring (11) is arranged in the clamping cap groove, and the spring (11) is in contact connection with the counter electrode plate (12).
7. The in-situ raman spectroscopy testing mold for electrochemical cells of claim 1, wherein: the thickness of the battery electrochemical in-situ Raman spectrum testing mold is 17-30 mm.
8. The in-situ raman spectroscopy testing mold for electrochemical cells of claim 1, wherein: the window plate (4) is a window plate (4) made of sapphire or quartz glass.
9. The in-situ raman spectroscopy testing mold for electrochemical cells of claim 1, wherein: the positive electrode material coating plate (5) is an aluminum foil coated with a positive electrode material.
10. The in-situ raman spectroscopy testing mold for electrochemical cells of claim 1, wherein: the battery (9) is a battery (9) which is assembled in sequence according to the sequence of aluminum foil, diaphragm, electrolyte and metallic lithium.
CN201921255968.3U 2019-08-05 2019-08-05 Battery electrochemistry normal position raman spectroscopy test mould Active CN210775224U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111896518A (en) * 2020-06-22 2020-11-06 西安交通大学 Electrocatalytic CO2In-situ Raman detection electrochemical cell for reducing and synthesizing hydrocarbon fuel
CN114397346A (en) * 2022-01-13 2022-04-26 中国科学技术大学 Novel zinc-air battery charging process tail gas normal position quantitative analysis device
CN114486736A (en) * 2022-01-10 2022-05-13 山东大学 Multifunctional spectrum and X-ray diffraction in-situ reaction chamber and application

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111896518A (en) * 2020-06-22 2020-11-06 西安交通大学 Electrocatalytic CO2In-situ Raman detection electrochemical cell for reducing and synthesizing hydrocarbon fuel
CN114486736A (en) * 2022-01-10 2022-05-13 山东大学 Multifunctional spectrum and X-ray diffraction in-situ reaction chamber and application
CN114486736B (en) * 2022-01-10 2023-10-10 山东大学 Multifunctional spectrum and X-ray diffraction in-situ reaction chamber and application
CN114397346A (en) * 2022-01-13 2022-04-26 中国科学技术大学 Novel zinc-air battery charging process tail gas normal position quantitative analysis device

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