CN111198178A - Electrochemical in-situ online detection device and use method thereof - Google Patents

Electrochemical in-situ online detection device and use method thereof Download PDF

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CN111198178A
CN111198178A CN202010017393.2A CN202010017393A CN111198178A CN 111198178 A CN111198178 A CN 111198178A CN 202010017393 A CN202010017393 A CN 202010017393A CN 111198178 A CN111198178 A CN 111198178A
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cell body
groove
metal sheet
counter electrode
hole
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王丹
杨梅
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Institute of Process Engineering of CAS
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Institute of Process Engineering of CAS
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65Raman scattering
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N24/00Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
    • G01N24/08Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
    • G01N24/088Assessment or manipulation of a chemical or biochemical reaction, e.g. verification whether a chemical reaction occurred or whether a ligand binds to a receptor in drug screening or assessing reaction kinetics

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Abstract

The invention relates to an electrochemical in-situ online detection device and a use method thereof, wherein the device comprises a window sealing cover, a main cell body and a cell body counter electrode shell which are sequentially connected, and the device can be used for researching the physical and chemical properties of various electrochemical energy storage devices such as lithium ion batteries, sodium ion batteries, zinc ion batteries, aluminum ion batteries, super capacitors, alkaline batteries and the like, is an electrochemical in-situ online detection device suitable for various detection technologies, is detachable and washable, and is simple and convenient to operate.

Description

Electrochemical in-situ online detection device and use method thereof
Technical Field
The invention belongs to the field of electrochemical detection, and relates to an electrochemical in-situ online detection device and a use method thereof.
Background
The problems of energy shortage, environmental pollution and the like are core problems influencing the development of the current and future society, and electrochemical energy storage devices such as lithium ion batteries, super capacitors and the like have the characteristics of high energy density, high conversion efficiency, convenience in storage and transportation and the like, are green and environment-friendly, provide an effective way for solving the problems of energy and environment, and are widely concerned by people.
The existing electrochemical energy storage device is often a complex system with multiple components, multiple reactions and multiple influence factors, and the electrochemical performance of the existing electrochemical energy storage device is closely related to the transport, reaction and storage behaviors of electrons and ions in a bulk phase and an interface. In order to better understand the relationship and rule of the structure, reaction, material transmission and performance, the electronic structure, crystal structure, micro-morphology, chemical composition, physical property and evolution process of the electrode material in the equilibrium state and the non-equilibrium state process need to be comprehensively and deeply researched from the atomic scale to the macro scale. However, in the conventional research, the battery is often split according to the structural composition and is respectively performed on different parts such as a negative electrode, a positive electrode, an electrolyte and the like, so that various problems are caused when the battery is used for a full battery; aiming at different targets, the structure, the appearance characteristic and the final energy storage performance of the material are mostly separated, the structure, the appearance characteristic and the final energy storage performance of the material are usually 'point-by-point', ex-situ observation is mostly adopted, the difference in electrode and battery space is not considered, and the change condition in the charging and discharging process is rarely observed; in terms of performance, the change of the performance with time is more concerned, the difference of different space positions of the battery is rarely considered, the obtained information is limited, and the obtained principle contents of reaction, interface, substance transmission and the like are generally conjectured.
In-situ online detection has gained increasing attention in recent years, for example: research results such as in-situ transmission electron microscopy, in-situ X-ray diffraction, in-situ magnetic resonance, in-situ Raman, in-situ infrared, in-situ optical imaging, in-situ electrochemical microbalance, small-angle neutron diffraction and the like are continuously reported. However, because the components and reaction processes of the electrochemical system are very complicated, the devices or characterization methods used in these studies are often designed for specific systems or simplified approximate processes, such as in-situ transmission electron microscope characterization of lithium ion batteries, most of which are to perform one-time charging or discharging on electrode material particles, have no electrolyte and no counter electrode, are far from the actual system, are not true batteries, and are not compatible and universal between the in-situ online detection devices. In fact, due to the limitation of a single detection technology, the detection technology is usually only used for peeping leopard in a tube, only one spot is seen, and the completeness is difficult to achieve, and the consistency and the accuracy of a test result are difficult to ensure due to the difference of positions and time of tests by different means.
Therefore, different technologies need to be combined for verification and integrated complementation, and various characterization means are used for associating each partially-masked feature with the overall performance, so that an electrochemical in-situ online detection device which is universal and is simultaneously suitable for characterization of different technologies is needed, but at present, the device is blank at home and abroad, and no relevant report is found.
Disclosure of Invention
The invention aims to provide an electrochemical in-situ online detection device and a using method thereof, wherein the device comprises a window sealing cover, a main cell body and a cell body counter electrode shell, and can be used for researching the physical and chemical properties of various electrochemical energy storage devices such as lithium ion cells, sodium ion cells, zinc ion cells, aluminum ion cells, super capacitors, alkaline cells and the like, so that the electrochemical in-situ online detection device is suitable for various detection technologies, is detachable and washable, and is simple and convenient to operate.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides an electrochemical in-situ online detection device, which comprises a window sealing cover, a main cell body and a cell body counter electrode shell, wherein the window sealing cover is provided with a through hole, and an optical window for light to pass through is arranged at a position, opposite to the through hole, on the main cell body; a groove is formed in the main tank body, one end of the optical window is embedded into the bottom of the groove, and light can enter the groove through the optical window; a first metal sheet is arranged around the periphery of the optical window at the inner side of the bottom of the groove and connected with a first lead; the cell body counter electrode shell is connected with the opening end of the groove in a sealing way; the end face of one end, connected with the groove, of the cell body antipole shell is provided with a second metal sheet, and the second metal sheet is connected with a second lead.
A through hole is formed in a sealing cover of a viewing window in the electrochemical in-situ online detection device, and an optical window for light to pass through is arranged at the position, opposite to the through hole, of a main tank body; incident light and reflected light can pass through the through hole and the optical window, so that input and collection of optical signals can be performed, and further the optical signal can be used for detection of a spectrum technology. The electrochemical in-situ online detection device comprises a main tank body, wherein a groove is formed in the main tank body, one end of an optical window is embedded into the bottom of the groove, a first metal sheet is arranged on the inner side of the bottom of the groove and positioned on the periphery of the optical window, in the electrochemical in-situ online detection process, an element to be detected is attached to the first metal sheet, then a second metal sheet is attached to the element to be detected, and in-situ online detection is carried out.
The first metal sheet is here a ring-shaped metal sheet, which surrounds the optical window around its circumference.
Preferably, the second metal sheet is a circular metal sheet, which is beneficial to improving the circuit connection performance of the device.
The sealed connection between the cell body counter electrode shell and the opening end of the groove means that a sealed space is formed inside the groove after the cell body counter electrode shell is connected with the opening end of the groove.
Preferably, the part of the optical window not embedded into the bottom of the groove is provided with a first external thread, one end of the through hole opposite to the optical window is provided with a first internal thread, and the window sealing cover is connected with the main tank body through the first external thread and the first internal thread in a screwing manner.
Preferably, a second internal thread is arranged in the groove, a second external thread is arranged at one end of the cell body antipole shell, and the main cell body is in screwed connection with the cell body antipole shell through the second internal thread and the second external thread.
The end, connected with the opening end of the groove, of the counter electrode shell of the tank body is cylindrical, and the side surface of the cylinder is provided with a second external thread which can be connected with a second internal thread arranged on the inner side wall surface of the groove in a screwing and sealing manner; in the in-situ online detection process, the second metal sheet positioned on the end surface of the cylinder is closely connected with the element to be detected; thereby being beneficial to improving the connectivity of the circuit.
The element to be tested comprises various electrochemical energy storage devices such as a lithium ion battery, a sodium ion battery, a zinc ion battery, an aluminum ion battery, a super capacitor and an alkaline battery.
The detection device has the characteristics of convenience in disassembly and cleaning and simplicity in operation.
Preferably, a first sealing ring is arranged at the joint of the first external thread and the first internal thread.
Preferably, a second sealing ring is arranged at the joint of the second external thread and the second internal thread.
According to the device, the sealing rings are arranged between the first external thread and the first internal thread and between the second external thread and the second internal thread, and the sealing rings are uniformly deformed in the screwing connection process, so that air leakage is prevented, and the sealing requirement of an electrochemical device system can be met.
Preferably, the first sealing ring and the second sealing ring are both O-shaped sealing rings.
Preferably, the first lead and the second lead are used for connecting with an external circuit.
Preferably, the first lead is connected with one side of the first metal sheet, which faces away from the cell counter-pole shell.
Preferably, one end of the first lead connected with the first metal sheet is embedded in the main tank body, and the other end of the first lead is arranged outside the main tank body and used for connecting an external circuit.
Preferably, the second lead is connected to a side of the second metal sheet facing away from the optical window.
Preferably, one end of the second lead connected with the second metal sheet is embedded into the cell body counter electrode shell, and the other end of the second lead is outside the cell body counter electrode shell and is used for connecting an external circuit.
Preferably, the through hole is a two-stage stepped hole, the two-stage stepped hole comprises a first-stage hole and a second-stage hole, and the diameter of the first-stage hole is larger than that of the second-stage hole.
Preferably, one end of the window sealing cover corresponding to the first-stage hole is connected with the main tank body.
Preferably, the optical window is of a two-stage cylindrical structure and comprises a first-stage cylinder and a second-stage cylinder, the diameter of the first-stage cylinder is larger than that of the second-stage cylinder, the second-stage cylinder is embedded into the bottom of the groove, and one end of the first-stage cylinder is opposite to the through hole.
Preferably, the materials of the window sealing cover, the main tank body and the counter electrode shell of the tank body are respectively and independently selected from non-metallic materials.
The materials of the window sealing cover, the main tank body and the counter electrode shell of the tank body do not comprise metal sheets (a first metal sheet and a second metal sheet) and an optical window.
The threads are directly processed on the sealing cover, the tank body and the counter electrode shell of the tank body, and the material of the threads is the same as that of the main body.
Preferably, the non-metallic material is selected from any one of polyetheretherketone, polytetrafluoroethylene, polymethacrylate or polyvinyl chloride, preferably polyetheretherketone.
Preferably, the material of the optical window is quartz.
Preferably, the first metal sheet and the second metal sheet are made of non-magnetic materials.
Preferably, the non-magnetic material is selected from any one of gold, titanium, copper or aluminum, preferably gold or titanium.
The detection device provided by the invention adopts the material, and the material does not interfere the acquisition of nuclear magnetic signals, so that the device can also be used for nuclear magnetic resonance detection.
In a second aspect, the present invention provides a method for using the electrochemical in-situ online detection device according to the first aspect, the method comprising the following steps:
(1) placing an electrode plate to be tested at the bottom of the groove of the main tank body, and covering the first metal sheet and the optical window;
(2) dropwise adding electrolyte on the surface of the electrode slice to be detected in the step (1), and putting a diaphragm;
(3) and (3) dropwise adding electrolyte on the diaphragm in the step (2), then putting a counter electrode, covering and connecting one end of the counter electrode shell of the cell body, which is provided with the second metal sheet, with the counter electrode, and then carrying out electrochemical in-situ online detection.
Preferably, before the step (1), the window sealing cover and the main tank body are screwed and connected through a first internal thread at one end of the through hole on the window sealing cover and a first external thread at one end of the optical window which is not embedded into the bottom of the groove.
Preferably, when the first internal thread and the first external thread are screwed to each other, a sealing ring is arranged at the joint for sealing the joint.
Preferably, the end of the cell body antipole shell provided with the second metal sheet is provided with a second external thread, the inner wall of the groove is provided with a second internal thread, and the cell body antipole shell and the inner wall of the groove are screwed and connected through the second external thread and the second internal thread.
Preferably, a sealing ring is arranged at the joint of the second external thread and the second internal thread and used for sealing the joint.
Preferably, the electrochemical in-situ online detection in the step (3) comprises online detection of raman spectroscopy and/or nuclear magnetic resonance.
Preferably, the electrochemical in-situ online detection in the step (3) is to perform raman spectrum detection and nuclear magnetic resonance detection simultaneously in the charging and discharging processes.
In the using process of the electrochemical in-situ online detection device, an element to be detected is placed at the bottom of the inner side of the groove of the main tank body, the first metal sheet and the optical window are covered, and then the second metal sheet is closely covered on the surface of one side, back to the first metal sheet, of the element to be detected; the first metal sheet and the second metal sheet are respectively connected with an external circuit; in the detection process, the through hole and the optical window on the window sealing cover can facilitate incident light and reflected light to pass through, so that in-situ spectrum on-line detection is realized, and the in-situ spectrum on-line detection device can be used for nuclear magnetic resonance detection.
Compared with the prior art, the invention has the following beneficial effects:
(1) the electrochemical in-situ online detection device comprises a window sealing cover, a main tank body and a tank body counter electrode shell, wherein a through hole in the window sealing cover is arranged opposite to an optical window at the bottom of a groove in the main tank body, so that incident light and reflected light can pass through the through hole, the spectral technology detection can be carried out, a first metal sheet is arranged around the circumference of the optical window at the inner side of the bottom of the groove, and the first metal sheet is connected with a first lead; a second metal sheet is arranged on the end face of one end of the cell body counter electrode shell connected with the groove, and the second metal sheet is connected with a second lead, so that electrochemical in-situ online detection is realized;
(2) the electrochemical in-situ on-line detection device can carry out on-line detection technology including Raman spectrum detection and/or nuclear magnetic resonance detection, and has the most prominent functions of: in the charging and discharging process, the device can simultaneously carry out Raman spectrum detection and nuclear magnetic resonance detection;
(3) the electrochemical in-situ online detection device disclosed by the invention is simple in structure, convenient to disassemble and clean and simple to operate.
Drawings
FIG. 1 is a schematic view of a sealing cover for a window according to embodiment 1 of the present invention;
FIG. 2 is a schematic structural diagram of the main tank body in embodiment 1 of the present invention;
FIG. 3 is a schematic structural diagram of a counter electrode shell of the cell body in example 1 of the present invention;
FIG. 4 is a schematic structural diagram of an electrochemical in-situ online detection apparatus in embodiment 1 of the present invention (the dotted line in the figure indicates the joint between the window sealing cover and the main tank body);
FIG. 5 is a first charge-discharge curve diagram of the electrochemical in-situ on-line detection device in application example 1 of the present invention;
FIG. 6 is a spectrum of on-line detection of Raman spectrum in application example 1 of the present invention;
FIG. 7 is a graph of free induction decay signal data of a lithium metal electrode for on-line nuclear magnetic resonance detection in application example 2 of the present invention;
fig. 8 is an amplitude spectrum of a lithium metal electrode for nuclear magnetic resonance online detection in application example 2 of the present invention;
fig. 9 is a diagram of the original CPMG echo of the lithium metal electrode for the nuclear magnetic resonance online detection in application example 2 of the present invention;
FIG. 10 is a graph of echo attenuation data for a lithium metal electrode for on-line nuclear magnetic resonance in application example 2 of the present invention;
FIG. 11 is a relaxation spectrum of a lithium metal electrode for nuclear magnetic resonance online detection in application example 2 of the present invention;
FIG. 12 is a Raman spectrum of a silicon electrode under magnetic field-free and magnetic field conditions when Raman spectroscopy and NMR are simultaneously performed on-line in application example 3 of the present invention;
fig. 13 is a nuclear magnetic resonance imaging diagram of a lithium metal electrode when laser is incident when raman spectroscopy and nuclear magnetic resonance online detection are performed simultaneously in application example 3 of the present invention (light-colored regions within a dotted line frame in the diagram are images of metal lithium);
1-through hole, 2-first internal thread, 3-groove, 4-optical window, 5-first external thread, 6-second internal thread, 7-first metal sheet, 8-first lead, 9-second external thread, 10-second metal sheet, 11-second lead.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The electrochemical in-situ online detection device comprises a window sealing cover, a main tank body and a tank counter electrode shell;
the structure schematic diagram of the window sealing cover is shown in fig. 1, as can be seen from fig. 1, the window sealing cover is cylindrical, a through hole 1 is formed in the window sealing cover along the axis direction of the window sealing cover, the through hole is a two-stage stepped hole, the two-stage stepped hole comprises a first-stage hole and a second-stage hole, the diameter of the first-stage hole is larger than that of the second-stage hole, and a first internal thread 2 is formed in the inner wall of the first-stage hole;
the structural schematic diagram of the main tank body is shown in fig. 2, as can be seen from fig. 2, the main tank body is cylindrical, a groove 3 is formed in the end face of one side of the cylinder, the groove is cylindrical, an optical window 4 is embedded and connected to the bottom of the groove, and the optical window 4 is arranged opposite to a through hole 1 in the window sealing cover; a first external thread 5 is arranged at one end, not embedded into the bottom of the groove, of the optical window 4, and the first external thread 5 is used for being screwed with the first internal thread 2; a second internal thread 6 is arranged on the inner wall of one side of the opening end of the groove 3; a first metal sheet 7 is arranged at the bottom of the groove 3 around the optical window 4, and the first metal sheet 7 is of an annular structure; one side, back to the opening end of the groove 3, of the first metal sheet 7 is connected with a first lead 8, one end, connected with the first metal sheet 7, of the first lead 8 is embedded into the main cell body, and the other end of the first lead is exposed out of the main cell body and is used for being connected with an external circuit;
meanwhile, as can be seen from fig. 2, the optical window is a two-stage cylindrical structure, and includes a first-stage cylinder and a second-stage cylinder, the diameter of the first-stage cylinder is greater than that of the second-stage cylinder, and one end of the second-stage cylinder is embedded into the bottom of the groove. The first-stage cylinder is exposed outside the groove;
the structural schematic diagram of the cell body counter electrode shell is shown in fig. 3, as can be seen from fig. 3, the cell body counter electrode shell is cylindrical, a second external thread 9 is arranged at one end of the cell body counter electrode shell, a second metal sheet 10 is arranged on the end surface of one side provided with the second external thread, the second metal sheet 10 is connected with a second lead 11, and the second lead 11 is embedded into the cell body counter electrode shell;
the structural schematic diagram of the electrochemical in-situ online detection device in this embodiment is shown in fig. 4, and as can be seen from fig. 4, the window sealing cover and the main tank body are screwed and connected through a first internal thread and a first external thread, and a sealing ring is arranged between the first internal thread and the first external thread; the main tank body and the tank body antipodal shell are connected through a second internal thread and a second external thread in a screwing mode, and a sealing ring is arranged between the second internal thread and the second external thread. After the second internal thread and the second external thread are connected in a screwed mode, a sealing space is formed in the groove, and the sealing ring is beneficial to preventing air leakage, so that the sealing requirement of an electrochemical device system is met. Here the sealed space is used for placing electrode pads and diaphragms.
The method for the electrochemical in-situ online detection of the detection device comprises the following steps:
firstly, the window sealing cover and the main tank body are connected through a first internal thread and a first external thread in a screwing mode, and a sealing ring is arranged between the first internal thread and the first external thread; then placing the electrode plate to be tested on the first metal sheet and the optical window in the groove; then, electrolyte is dripped, a diaphragm is placed, the electrolyte is dripped, and a counter electrode is placed; and the main tank body and the counter electrode shell of the tank body are connected by screwing through a second internal thread and a second external thread, so that a second metal sheet is tightly attached to the counter electrode, and a sealing ring is arranged between the second internal thread and the second external thread.
In this embodiment, the window sealing cover, the main tank body and the counter electrode casing of the tank body are all made of polyether ether ketone.
The first metal sheet and the second metal sheet are made of titanium.
Application example 1
The application example adopts the device as described in example 1, and lithium cobaltate material is coated on aluminum foil to obtain the anode, and the lithium sheet is used as the cathode;
the components are sequentially arranged in the groove by adopting the using method of the device, the detection device is installed, charging and discharging are carried out, and the Raman spectrum is acquired in situ on line in real time;
the test results of this application example show that, as shown in fig. 5 and 6, the lithium ion battery assembled with the device under test can be normally charged and discharged in the detection apparatus described in example 1, the sealing performance is excellent, and the test results are in line with expectations.
Application example 2
The device is adopted in the application example as described in embodiment 1, the metal lithium is used as the positive electrode and the negative electrode, the use method of the device is that the lithium sheets are sequentially arranged in the grooves, the detection device is installed for charging and discharging, and the nuclear magnetic resonance signals of the lithium metal electrode are acquired in situ and on line in real time under the magnetic field strength of 0.5 Tesla;
the test results are shown in fig. 7-11, which show that the device of example 1 can be used to charge and discharge normally under the magnetic field condition, and the nuclear magnetic signal of the lithium metal electrode can be obtained, and the test results are in accordance with expectations.
Application example 3
The application example adopts the device as described in example 1, silicon powder material is coated on the aluminum foil to be used as the battery anode, and the lithium metal sheet is used as the cathode;
the parts are sequentially arranged in the groove by adopting the using method of the device, the detection device is installed, charging and discharging are carried out, the in-situ online acquisition of the Raman spectrum and the nuclear magnetic resonance imaging result of the lithium sheet is carried out simultaneously, and the magnetic field intensity is 0.5 Tesla.
The above test results are shown in fig. 12 to fig. 13, and it can be seen from fig. 12 that the nmr test does not interfere with the test results of the raman spectroscopy, and the nmr graph 13 can observe the image of the lithium metal (i.e. the light color area in the dashed line frame in the graph, and the test magnetic field strength is 0.5 tesla), so that the raman spectroscopy test does not interfere with the nmr process, and therefore, it indicates that the device described in example 1 of the present invention can be normally charged and discharged under the condition of the magnetic field, and the spectrum and the magnetic field do not interfere with each other, and the test results are in accordance with the expectation.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.

Claims (10)

1. An electrochemical in-situ online detection device is characterized by comprising a window sealing cover, a main cell body and a cell body counter electrode shell, wherein the window sealing cover is provided with a through hole, and an optical window for light to pass through is arranged at the position, opposite to the through hole, of the main cell body; a groove is formed in the main tank body, one end of the optical window is embedded into the bottom of the groove, and light can enter the groove through the optical window; a first metal sheet is arranged around the periphery of the optical window at the inner side of the bottom of the groove and connected with a first lead; the cell body counter electrode shell is connected with the opening end of the groove in a sealing way; the end face of one end, connected with the groove, of the cell body antipole shell is provided with a second metal sheet, and the second metal sheet is connected with a second lead.
2. The detection apparatus according to claim 1, wherein a portion of the optical window that is not embedded in the bottom of the groove is provided with a first external thread, an end of the through hole opposite to the optical window is provided with a first internal thread, and the window sealing cover is screwed with the main tank body through the first external thread and the first internal thread;
preferably, a second internal thread is arranged in the groove, a second external thread is arranged at one end of the cell body antipole shell, and the main cell body is in screwed connection with the cell body antipole shell through the second internal thread and the second external thread.
3. The detection device as claimed in claim 1 or 2, wherein a first sealing ring is arranged at the connection part of the first external thread and the first internal thread;
preferably, a second sealing ring is arranged at the joint of the second external thread and the second internal thread;
preferably, the first sealing ring and the second sealing ring are both O-shaped sealing rings.
4. A testing device according to any of claims 1-3 wherein the first and second leads are adapted to be connected to an external circuit.
5. The detection apparatus according to any one of claims 1 to 4, wherein the first lead is connected to a side of the first metal sheet facing away from the counter-electrode housing of the cell body;
preferably, one end of the first lead connected with the first metal sheet is embedded into the main tank body, and the other end of the first lead is arranged outside the main tank body and used for connecting an external circuit;
preferably, the second lead is connected with one side of the second metal sheet, which faces away from the optical window;
preferably, one end of the second lead connected with the second metal sheet is embedded into the cell body counter electrode shell, and the other end of the second lead is outside the cell body counter electrode shell and is used for connecting an external circuit.
6. The device according to any one of claims 1 to 5, wherein the through hole is a two-step stepped hole comprising a first-step hole and a second-step hole, the first-step hole having a diameter larger than that of the second-step hole;
preferably, one end of the window sealing cover corresponding to the first-stage hole is connected with the main tank body.
7. The detecting device for detecting the rotation of a motor rotor as claimed in any one of claims 1 to 6, wherein the optical window is of a two-stage cylindrical structure and comprises a first-stage cylinder and a second-stage cylinder, the diameter of the first-stage cylinder is larger than that of the second-stage cylinder, the second-stage cylinder is embedded in the bottom of the groove, and one end of the first-stage cylinder is arranged opposite to the through hole.
8. The testing device according to any one of claims 1 to 7, wherein the materials of the window sealing cover, the main cell body and the counter electrode casing of the cell body are independently selected from non-metallic materials;
preferably, the non-metallic material is selected from any one of polyetheretherketone, polytetrafluoroethylene, polymethacrylate or polyvinyl chloride, preferably polyetheretherketone;
preferably, the first metal sheet and the second metal sheet are made of non-magnetic materials;
preferably, the non-magnetic material is selected from any one of gold, titanium, copper or aluminum, preferably gold or titanium.
9. The use method of the electrochemical in-situ on-line detection device as claimed in any one of claims 1 to 8, wherein the method comprises the following steps:
(1) placing an electrode plate to be tested at the bottom of the groove of the main tank body, and covering the first metal sheet and the optical window;
(2) dropwise adding electrolyte on the surface of the electrode slice to be detected in the step (1), and putting a diaphragm;
(3) dropwise adding electrolyte on the diaphragm in the step (2), then putting a counter electrode, covering and connecting one end of a counter electrode shell of the cell body, which is provided with a second metal sheet, with the counter electrode, and then carrying out electrochemical in-situ online detection;
preferably, before the step (1), the window sealing cover and the main tank body are screwed and connected through a first internal thread at one end of a through hole on the window sealing cover and a first external thread at one end of the optical window which is not embedded into the bottom of the groove;
preferably, a sealing ring is arranged at the joint when the first internal thread and the first external thread are screwed for connecting, so as to seal the joint;
preferably, a second external thread is arranged at one end of the cell body counter electrode shell, which is provided with a second metal sheet, and a second internal thread is arranged on the inner wall of the groove, so that the cell body counter electrode shell and the inner wall of the groove are connected by screwing through the second external thread and the second internal thread;
preferably, a sealing ring is arranged at the joint of the second external thread and the second internal thread and used for sealing the joint;
10. the method of claim 9, wherein the electrochemical in-situ in-line detection of step (3) comprises in-line detection of raman spectroscopy and/or nuclear magnetic resonance;
preferably, the electrochemical in-situ online detection in the step (3) is to perform raman spectrum detection and nuclear magnetic resonance detection simultaneously in the charging and discharging processes.
CN202010017393.2A 2020-01-08 2020-01-08 Electrochemical in-situ online detection device and use method thereof Pending CN111198178A (en)

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