CN213337697U

CN213337697U - Atmosphere temperature adjustable scanning electrochemistry-glove box combined device

Info

Publication number: CN213337697U
Application number: CN202021098684.0U
Authority: CN
Inventors: 阎兴斌; 陈江涛; 杨兵军; 马鹏军; 郎俊伟
Original assignee: Lanzhou Institute of Chemical Physics LICP of CAS
Current assignee: Lanzhou Institute of Chemical Physics LICP of CAS
Priority date: 2020-06-15
Filing date: 2020-06-15
Publication date: 2021-06-01
Anticipated expiration: 2030-06-15

Abstract

The utility model discloses a scanning electrochemistry-glove box combined device with adjustable atmosphere temperature, which is based on the combined use of a scanning electrochemistry workstation and a glove box and realizes the electrochemical analysis test with adjustable atmosphere and different states; the coupling device comprises a circuit connection interface, a sealing interface, a small electrolytic cell, a glove box, an anhydrous oxygen-free system and two electrochemical workstations. The combined device can not only realize corrosion in atmospheric atmosphere and conventional electrochemical test of electrode materials such as a water system capacitor, but also realize scanning electrochemical test of novel energy storage devices such as lithium ions, sodium ions, potassium ions and the like in the atmosphere of anhydrous and oxygen-free inert gases, and solves the problems of discontinuous test and poor reliability of the traditional sealed electrolytic cell and the like. The device completes stable and continuous real-time monitoring of the novel energy storage electrode material, and provides a stable and high-reliability platform for energy storage mechanism discussion. The utility model is suitable for a fields such as corruption, electrochemistry normal position analysis.

Description

Atmosphere temperature adjustable scanning electrochemistry-glove box combined device

Technical Field

The utility model belongs to the technical field of novel energy storage material, energy storage device and electrochemical analysis, a scanning electrochemistry-glove box allies oneself with and uses device of atmosphere temperature adjustable is related to.

Background

As widely used secondary batteries, such as lithium (sodium potassium) ion batteries and organic system supercapacitors, have very high energy density or power density, are widely used in portable electronic devices such as electric vehicles, mobile phones and computers, and are ubiquitous in modern social life. In the past reports, researchers have paid high attention to the preparation of high-performance materials, but have not conducted intensive and systematic investigation on the key scientific problems relating to the output characteristics, stability and safety of electrodes and devices, which are the surface interface physicochemical characteristics of electrode materials. In the prior art, the electrochemical test method, such as a conventional cyclic voltammetry curve and constant current charge and discharge characteristics, reflects the whole information of the electrode, and cannot reflect the local electrochemical information of the electrode material. The sealed electrolytic cell in the prior art can realize three-electrode test, but has a plurality of interference factors and low data reliability. However, the organic electrolyte of active metals, such as sodium and potassium, is very susceptible to air and moisture, and is difficult to obtain reliable and accurate data, and it is more difficult to realize two-dimensional scanning test of micro-area electrochemistry. The micro-area scanning electrochemical in-situ analysis with high spatial resolution and high sensitivity is adopted as a core means, and the electrochemical reaction activity of the surface interface in the ion extraction process is visually detected on line, so that the surface interface electrochemical information which cannot be obtained by other conventional electrochemical and other characterization means can be obtained, and the surface interface characteristics of the carbon cathode and the characteristic relationship between the carbon cathode and the anode and cathode materials can be explained from a microscopic level; further clarifying the performance attenuation process and internal cause of the electrode material, and disclosing the energy storage mechanism and performance improvement strategy of the electrode material.

Disclosure of Invention

The utility model aims at providing an atmosphere temperature adjustable scanning electrochemistry-glove box allies oneself with device realizes the real-time on-line measuring on electrode material surface under the different electrolyte systems, adjusts the transform gas atmosphere simultaneously and carries out the electrochemistry test.

In order to achieve the above object, the utility model adopts the following technical scheme: a scanning electrochemistry-glove box combined device with adjustable atmosphere temperature is based on the combined use of a scanning electrochemistry workstation and a glove box, and realizes electrochemical analysis tests with adjustable atmosphere and different states; the coupling device comprises a circuit connection interface, a sealing interface, a small electrolytic cell, a glove box, an anhydrous oxygen-free system and two electrochemical workstations.

The analysis and test method in the prior art can not monitor the running process of the battery and can not obtain the information of the in-situ chemical reaction process in real time. The utility model discloses ally oneself with device and carry out real-time normal position on-line analysis sign to novel energy storage material electrochemical reaction such as lithium, sodium, potassium, cryogenic cooling system provides the characteristic sign under the low temperature simultaneously, all will be to further understanding electrode material reaction process and mechanism, and it has the significance to improve energy storage device electrode material performance to can extend its application in fields such as catalysis, photoelectrochemistry.

The utility model discloses ally oneself with beneficial effect who uses the device:

1) the in-situ analysis and test platform for the electrochemical process and behavior of the novel energy storage material in the charging and discharging process is provided, and experimental basis can be provided for realizing the development of high-performance energy storage device materials and technologies;

2) the test environment at low temperature is provided, an experimental platform can be provided for the performance of the energy storage material and the electrolyte at low temperature, and an experimental basis is provided for developing low-temperature resistant devices;

3) the method can realize the conversion between atmospheres such as argon inert atmosphere and an open system, meet the requirements of conventional tests or different environmental conditions, and provide a platform for researches such as corrosion, energy storage, photocatalysis and the like.

The utility model discloses the antithetical couplet is put not only can realize opening the conventional electrochemistry test under the system, and the most important mechanism research that can realize novel energy storage material under the anhydrous anaerobic condition obtains the electrochemistry characteristic under the different temperatures through temperature regulation. The method has the greatest advantages of monitoring the electrochemical activity of the surface of the electrode material on line and carrying out accurate, stable and continuous real-time detection.

Meanwhile, the novel electrode material can be subjected to performance and mechanism research at different temperatures, and a low-temperature test environment is provided.

The combined device comprises a micro-area scanning electrochemical test system (a micro-area scanning electrochemical module and a micro-area impedance module), can provide electrochemical scanning tests under different atmospheres, can realize corrosion under the atmosphere and conventional electrochemical tests of electrode materials such as a water system capacitor, and the like, can also realize scanning electrochemical tests under the atmosphere of anhydrous and oxygen-free inert gases required by novel energy storage devices such as lithium ions, sodium ions, potassium ions and the like, and overcomes the problems of discontinuous tests and poor reliability of the traditional sealed electrolytic cell and the like. The device completes stable and continuous real-time monitoring of the novel energy storage electrode material, and provides a stable and high-reliability platform for energy storage mechanism discussion. The utility model is suitable for a fields such as corruption, electrochemistry normal position analysis.

Drawings

Fig. 1 is a schematic view of a first embodiment of the combination device of the present invention.

Fig. 2 is a schematic view of a second embodiment of the coupling device of the present invention.

Fig. 3 is a schematic view of a third embodiment of the combination device of the present invention.

Fig. 4 is a schematic view of a fourth embodiment of the combination device of the present invention.

FIG. 5 is a schematic diagram of a small and medium electrolytic cell, a probe system and a cryogenic cooling system of the combined device of the present invention.

In the figure: 1. the device comprises a glove box, 2, a sealed signal connector, 3, a first signal connector, 4, a second signal connector, 5, a cooling medium inlet, 6, a cooling medium outlet, 7, an electrochemical workstation, 8, a scanning electrochemical microscope module, 9, a stepping motor, 10, an anti-seismic optical platform, 11, an optical imaging system, 12, a local alternating current impedance module, 13, a cryogenic cooling system, 14, an electrolytic cell, 15, a reference electrode, 16, a cooling coil, 17, a test frame fixing bolt, 18, a sealing and electrode lead, 19, a counter electrode and 20, and a probe.

Detailed Description

The following further description of the present invention will be made with reference to the accompanying drawings and embodiments to help further understanding of the present invention.

As shown in fig. 1, the utility model discloses a first embodiment of the combined device, including a glove box 1 and two scanning electrochemical workstations 7; the glove box 1 comprises a shell, wherein a plurality of sealing type signal connectors 2, a plurality of first signal conversion heads 3 and a plurality of second signal conversion heads 4 are arranged on the shell; the bottom of the shell is also provided with a refrigerant medium inlet 5 and a refrigerant medium outlet 6. Electrode leads of a working electrode, a reference electrode and the like of the scanning electrochemical workstation 7 are connected with the sealing signal connector 2 (BNC).

In the first embodiment of the combined device, electrode leads such as a working electrode, a reference electrode and the like of a scanning electrochemical workstation 7 are connected into the glove box 1 through a sealing signal connector 2; the conventional tests of the three-electrode material such as cyclic voltammetry, constant current charging and discharging, impedance spectroscopy and the like can be realized.

As shown in fig. 2, the second embodiment of the combination device of the present invention comprises a glove box 1, a scanning electrochemical microscope control module 8, a stepping motor 9, an anti-seismic optical platform 10, an optical imaging system 11 and two scanning electrochemical workstations 7, wherein the stepping motor 9, the anti-seismic optical platform 10 and the optical imaging system 11 are respectively disposed inside the glove box 1 for probe control, anti-seismic and observation. The glove box 1 comprises a shell, wherein a plurality of sealing type signal connectors 2, a plurality of first signal conversion heads 3 and a plurality of second signal conversion heads 4 are arranged on the shell; the bottom of the shell is also provided with a refrigerant medium inlet 5 and a refrigerant medium outlet 6. Electrode leads of a working electrode, a reference electrode and the like of the scanning electrochemical workstation 7 are connected with the sealing signal connector 2 (BNC).

The utility model discloses in the embodiment of combined device second, through electrode, scanning electrochemical microscope control module 8, circuit switching back, accomplish lithium ion battery cathode material's surperficial electrochemical characteristics through scanning electrochemical workstation 7, ultramicro probe and control module and change, observe the generating conditions such as solid electrolyte membrane among the cyclic process. Wherein, the control module, the circuit and the ultramicro probe are all arranged in the glove box 1. In the test process, different leads are selected for different tests.

In the second embodiment, the electrodes are connected by selection of the test module, and the line switching is performed by a switching panel on the glove box 1.

As shown in fig. 3, the third embodiment of the combined device of the present invention comprises a glove box 1, a stepping motor 9, an anti-seismic optical platform 10, an optical imaging system 11, a local ac impedance module 12 and two scanning electrochemical workstations 7, wherein signal lines are connected or selected between the components according to the module requirements, and no special device is provided; the glove box 1 comprises a shell, wherein a plurality of sealing type signal connectors 2, a plurality of first signal conversion heads 3 and a plurality of second signal conversion heads 4 are arranged on the shell; the bottom of the shell is also provided with a refrigerant medium inlet 5 and a refrigerant medium outlet 6. Electrode leads of a working electrode, a reference electrode and the like of the scanning electrochemical workstation 7 are connected with the sealing signal connector 2 (BNC).

The utility model discloses ally oneself with and use device third kind embodiment, through electrode, control module, circuit switching back, accomplish lithium ion battery cathode material's surface impedance characteristic through scanning electrochemistry workstation, ultramicro probe and control module and change, observe solid state electrolyte membrane in the cyclic process and generate and surface electrochemistry impedance spectrum two dimension and three-dimensional map.

As shown in fig. 4, the fourth embodiment of the combined device of the present invention comprises a glove box 1, a stepping motor 9, an anti-seismic optical platform 10, an optical imaging system 11, a local ac impedance module 12, a cryogenic cooling system 13, and two scanning electrochemical workstations 7; the glove box 1 comprises a shell, wherein a plurality of sealing type signal connectors 2, a plurality of first signal conversion heads 3 and a plurality of second signal conversion heads 4 are arranged on the shell; the bottom of the shell is also provided with a refrigerant medium inlet 5 and a refrigerant medium outlet 6. The cold medium inlet 5 and the cold medium outlet 6 are respectively connected with a low-temperature cooling system. Electrode leads of a working electrode, a reference electrode and the like of the scanning electrochemical workstation 7 are connected with the sealing signal connector 2 (BNC). The cold medium inlet 5 and the cold medium outlet 6 are respectively connected with a low-temperature cooling system. The low-temperature cooling system can realize the measurement of-30 ℃ to room temperature.

The utility model discloses a combined device fourth embodiment, including two scanning electrochemistry workstations, local alternating current impedance module, step motor, antidetonation optical platform, optical imaging system and cryogenic cooling system. After the electrode, the control module and the circuit are connected in a switching mode, the performance test of the electrode material at low temperature is completed through the scanning electrochemical workstation, the ultramicro probe and the control module, and the low-temperature energy storage mechanism can be investigated.

The first signal adapter 3 adopts a 15-pin signal adapter; the second signal adapter 4 adopts a 9-pin signal adapter.

As shown in FIG. 5, the small electrolytic cell, the probe system and the low temperature cooling system in the combined device of the present invention comprise an electrolytic cell 14, wherein the outer diameter of the electrolytic cell 14 is 3 cm; the bottom of the electrolytic cell 14 is provided with a sealing and electrode lead 18, the outer wall of the electrolytic cell 14 is wound with a cooling coil 16, a reference electrode 15 and a counter electrode 19 are symmetrically arranged in the electrolytic cell 14, and the reference electrode 15 and the counter electrode 19 are both connected with the electrolytic cell 14 through fixing clamps. Two ports of the cooling coil 16 are respectively connected with the cold medium inlet 5 and the cold medium outlet 6. When the device is used, the electrolytic cell 14 is fixedly arranged on the anti-seismic optical platform 10 through at least two test frame fixing bolts 17, the three-dimensional directions of the probe 20, namely the X direction, the Y direction and the Z direction, are controlled and adjusted through the stepping motor, so that the probe 20 extends into the electrolytic cell 14, and various tests can be carried out.

The electrolytic cell 14 is made of quartz glass which is easy to process and insulate, so that optical positioning of probes, electrodes and the like is more convenient; most importantly, the amount of the electrolyte is reduced, and waste, corrosion to the interior of the glove box 1 and damage to purification materials are avoided.

Introducing a control module into the glove box 1 by adopting a preferred 15-pin adapter and a preferred 9-pin adapter to realize the control of X, Y, Z displacement system and data acquisition by a closed-loop piezoelectric motor;

the low-temperature-resistant solvent is used as cooling liquid, the interface is sealed by the cold medium inlet 5 and the cold medium outlet 6, and the glycol (or mixed liquid) cooling liquid is introduced into a metal such as a stainless steel pipe to be used as a low-temperature control medium, so that the low-temperature test is realized.

By adopting the electrolytic cell 14, the environmental test of a small amount of organic electrolyte is realized, and the electrolyte is prevented from being wasted and volatilized to corrode the glove box 1 cavity and the gloves.

Claims

1. A scanning electrochemistry-glove box combined device with adjustable atmosphere temperature is characterized by comprising a glove box (1) and two scanning electrochemistry workstations (7); the glove box (1) comprises a shell, wherein a plurality of sealing type signal connectors (2), a plurality of first signal conversion heads (3) and a plurality of second signal conversion heads (4) are arranged on the shell; the bottom of the shell is also provided with a refrigerant medium inlet (5) and a refrigerant medium outlet (6); the electrode leads of the working electrode and the reference electrode of the scanning electrochemical workstation (7) are connected with the sealed signal connector (2).

2. The utility model provides an atmosphere temperature adjustable scanning electrochemistry-glove box allies oneself with device which characterized in that: the system comprises a glove box (1), a scanning electrochemical microscope control module (8), a stepping motor (9), an anti-seismic optical platform (10), an optical imaging system (11) and two scanning electrochemical workstations (7), wherein the stepping motor (9), the anti-seismic optical platform (10) and the optical imaging system (11) are respectively arranged in the glove box (1) and used for probe control, anti-seismic and observation; the glove box (1) comprises a shell, wherein a plurality of sealing type signal connectors (2), a plurality of first signal conversion heads (3) and a plurality of second signal conversion heads (4) are arranged on the shell; the bottom of the shell is also provided with a refrigerant medium inlet (5) and a refrigerant medium outlet (6); the electrode leads of the working electrode and the reference electrode of the scanning electrochemical workstation (7) are connected with the sealed signal connector (2).