CN109116256B - Three-electrode system electrochemical testing device and electrochemical testing method thereof - Google Patents
Three-electrode system electrochemical testing device and electrochemical testing method thereof Download PDFInfo
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- CN109116256B CN109116256B CN201811100016.4A CN201811100016A CN109116256B CN 109116256 B CN109116256 B CN 109116256B CN 201811100016 A CN201811100016 A CN 201811100016A CN 109116256 B CN109116256 B CN 109116256B
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
Abstract
The utility model discloses a three-electrode system electrochemical testing device and an electrochemical testing method thereof. The device comprises a cathode mould, a reference mould, a cathode mould, an elastic pressing plate device, a cathode plate, a diaphragm, a reference lug, an anode lug, an upper guide sleeve, a lower guide sleeve, a reference electrode and a reference electrode, wherein the cathode mould is provided with a cavity, the reference mould is provided with an annular cavity, the anode mould is provided with a blind hole and is internally provided with an anode post, the upper end of the anode post extends to the annular cavity, the cavity is internally provided with the elastic pressing plate device, the lower end of the anode post extends to the annular cavity, the upper end of the anode post is sequentially provided with the anode plate, the diaphragm and the cathode plate and is tightly pressed and fixed through the elastic pressing plate device, the annular cavity is provided with the upper guide sleeve and the lower guide sleeve which are vertically laminated and are insulated outside the anode plate, the diaphragm and the cathode plate, the reference electrode is arranged between the upper guide sleeve and the lower guide sleeve, the cathode plate is electrically connected with the cathode mould through the elastic pressing plate device, the anode post is electrically connected with the anode plate, and the cathode mould, and the cathode lug is respectively provided with the cathode lug, the reference lug and the reference electrode. The method comprises the steps of lower connection, reference electrode connection, other electrode connection, integral connection, electrode adjustment and test.
Description
Technical Field
The utility model belongs to the technical field of electrochemical testing, and particularly relates to a three-electrode system electrochemical testing device with simple structure, convenient assembly, good tightness, good reference electrode adaptability, stable performance, closest to the structure of an actual battery and high reference property and an electrochemical testing method thereof.
Background
Lithium ion batteries and supercapacitors have been increasingly used in the fields of various electronic products, energy storage systems, rail transportation, and the like due to the advantages of small volume, high energy density, high power density, no environmental pollution, and the like. In recent years, as the performance requirements of lithium ion batteries and super capacitors are continuously improved, researches on materials, performances, safety and the like of the lithium ion batteries and super capacitors are continuously conducted.
The charging and discharging process of the lithium ion battery and the super capacitor is a process that the positive electrode and the negative electrode work simultaneously. In the charge and discharge process, the change of the positive and negative electrode potential plays an important role in the performance of the lithium ion battery or the super capacitor. The three-electrode system is adopted to carry out comparative analysis and research on the positive and negative electrode potentials and the reference electrode potential of the battery or the capacitor, the change characteristics of the positive and negative electrode potentials in the electrochemical reaction process can be directly obtained, and further, the respective performance characteristics of the positive and negative electrodes are deeply and effectively researched from the internal reaction mechanism of the battery, and the performances of battery circulation, high-low temperature charge and discharge, multiplying power charge and discharge and the like are purposefully improved under the condition of avoiding side reactions in the battery. Has very important guiding significance for structural design, pole piece design, anode-cathode ratio, material collocation, electrolyte component optimization and the like of the battery or the capacitor. Therefore, it is very important to provide a three-electrode test system with stable performance, simple structure and convenient operation.
The utility model (patent number ZL 200820210512.0) discloses a three-electrode testing system for simulating a button-type lithium ion battery, which consists of an upper die and a lower die, is internally provided with a cavity for accommodating an electrode, a diaphragm, electrolyte and the like, can be used for testing the performance of an anode and a cathode of the button-type battery in the charge and discharge processes, and is convenient and quick to test. However, the reference electrode of the three-electrode system can only adopt a metal lithium strip, only the tip part of the reference electrode contacts with the electrolyte, and the effective area is small. The utility model patent (CN 103500859A) discloses a three-electrode device for a lithium ion battery, which comprises a shell, an upper cover, a battery core baffle plate and bolts, wherein the battery core baffle plate and the bolts are arranged in the shell, the first bolt and the fourth bolt are connected with reference electrode metal posts and serve as reference electrode binding posts, the second bolt and the third bolt are connected with positive and negative electrode metal posts respectively serve as positive and negative electrode binding posts, the electrode posts are directly connected with the electrode lugs of the battery core and the reference electrode through electrode lugs, and the battery core is fixed through the bolts. The utility model has good sealing performance and contact performance, but the whole device is made of metal materials, the reference electrode column manufacturing and assembling method is complex in process and high in cost, and the difference between the cell structure and the structure of an actual battery is large, so that the reference electrode column is poor in borrowing performance. In addition, conventional three-electrode test systems place the reference electrode between the negative and positive electrode sheets, typically within the separator, such that the separator may need to be composed of a specific material (e.g., fiberglass) and/or have a specific thickness (e.g., at least 0.9mm thick), and the reference electrode may also need to be in a specific form (e.g., wire-like) and/or may require special tools to accomplish insertion of the reference electrode, which may increase the cost of such conventional three-electrode test systems. In addition, since conventional three-electrode test systems may be expensive and therefore require reusability, the materials used for sealing may need to be sufficiently weak that they are easily destroyed/removed and replaced during subsequent use. However, such weaker seals may allow air to enter the three-electrode test system, which in turn may cause its testing to become unreliable and/or may not complete longer cycle testing.
The existing three-electrode test system has various defects such as complex structure, poor sealing performance, large difference between the structure and a solid battery, poor reference electrode selectivity (only metallic lithium can be used) and unstable performance, and cannot truly reflect the actual performance characteristics of the positive electrode and the negative electrode of the battery or the capacitor in the charge and discharge process. In addition, the electrolyte is more or less filled, which causes the change of the polarization effect inside the battery, and the side reaction between the electrolyte and the three-electrode test system (especially the reference system made of the metal material) and other problems, and the accurate characterization of the positive and negative electrode performances of the battery or the capacitor can not be realized.
Disclosure of Invention
Aiming at the problems and the defects existing in the prior art, the utility model provides the three-electrode system electrochemical testing device which has the advantages of simple structure, convenient assembly, good sealing performance, good adaptability of the reference electrode, stable performance and high reference property, is closest to the structure of an actual battery, and also provides an electrochemical testing method of the three-electrode system electrochemical testing device.
The three-electrode system electrochemical testing device is realized by the following steps: including mutual insulating and sealing connection's negative pole mould, reference mould, positive pole mould in proper order, the negative pole mould is provided with the cavity, the reference mould is provided with upper and lower open-ended annular cavity, the top of positive pole mould is provided with the blind hole, be provided with "T" shape metallic positive pole post in the blind hole, the upper end of positive pole post extends to in the annular cavity, be provided with the elastic pressing plate device in the cavity, the lower extreme of elastic pressing plate device extends to in the annular cavity and is relative with the upper end of positive pole post, the upper end of positive pole post has set gradually positive pole piece, diaphragm, negative pole piece and compresses tightly fixedly through the elastic pressing plate device in the annular cavity, be provided with upper and lower range upon range of and insulating upper and lower guide sleeve outside positive pole piece, diaphragm and the negative pole piece, be provided with the reference electrode between upper guide sleeve and the lower guide pin bushing, the negative pole piece passes through the elastic pressing plate device and is connected with negative pole mould electricity, the outside of positive pole post and positive pole piece electricity is provided with the reference pole, the positive pole, the reference pole, the positive pole is connected with positive pole, positive pole and negative pole, positive pole and positive pole, positive pole and negative pole mould and positive pole, positive pole and negative pole mould are connected.
The electrochemical testing method of the three-electrode system electrochemical testing device is realized by the following steps: the method comprises the following steps of lower connection, reference electrode connection, other electrode connection, integral connection, electrode adjustment and test, and the specific steps are as follows:
A. the lower part is connected with: sealing, insulating, fastening and connecting the positive electrode die with the reference die;
B. the reference electrode is connected: sequentially filling a positive pole, a lower guide sleeve and a reference electrode in cavities of a positive pole die and a reference die, enabling one end of the reference electrode to be in contact with a platinum sheet at the bottom end of a tabletting groove, and then filling an upper guide sleeve;
C. other electrode connections: sequentially loading a positive plate, a diaphragm and a negative plate on the upper end face of a positive pole post, loading a tabletting device I on the upper end of the positive plate, and loading a tabletting device II into a tabletting groove;
D. and (3) integral connection: aligning the circular arc bottom end of the metal column I in the negative electrode mould with a circular arc groove with holes of the tabletting device I, and carrying out sealing, insulating, fastening and connecting the negative electrode mould with the positive electrode mould and the reference mould;
E. electrode adjustment: adding a certain amount of electrolyte into a liquid injection hole formed from the top opening of the cavity, adjusting the position of the metal column II to enable the positive plate, the diaphragm and the negative plate to be positioned at the same horizontal plane with the reference electrode, and screwing the sealing cover;
F. and (3) testing: and (3) electrically connecting the test instrument and the equipment with the negative electrode tab, the reference electrode tab and the positive electrode tab respectively, and then carrying out three-electrode test.
Compared with the prior art, the utility model has the following beneficial effects:
1. the three-electrode system electrochemical testing device is composed of the detachable negative electrode die, the reference die, the positive electrode die and the internal components thereof, wherein the positive electrode plate, the diaphragm, the negative electrode plate and the reference electrode are pressed and fixed by the pressing mechanism and can be freely detached and adjusted, the stability is ensured, meanwhile, the flexibility is considered, the structure is simple, the assembly is convenient and fast, the sealing performance is good, the three-electrode system electrochemical testing device is closest to an actual battery structure, the reference performance is high, the disassembly and the cleaning are easy after the testing are finished, and the three-electrode system electrochemical testing device can be repeatedly used.
2. The relative positions of the positive plate, the diaphragm, the negative plate and the reference electrode of the three-electrode system electrochemical testing device can be adjusted by the elastic pressing plate device, so that the accuracy of the testing result can be effectively improved.
3. The reference electrode in the three-electrode system electrochemical testing device is arranged on the outer sides of the positive plate, the diaphragm and the negative plate, so that the diaphragm can be a single-layer porous film of Cellulose Acetate (CA), polyethylene (PE), polypropylene (PP), a blend of PE and PP or a multi-layer structured porous film of PE and/or PP, and the thickness of the diaphragm can be selected according to requirements; the reference electrode can be made of metals such as lithium, silver, copper and the like with electrochemical activity in different shapes such as rings, wires, strips, bars and the like, and the diaphragm and the reference electrode have good selectivity, strong adaptability and stable performance, so that the cost of the utility model can be effectively controlled.
4. The utility model can detect the potential change of the positive electrode and the negative electrode of the battery or the capacitor in the charging and discharging processes at the same time, and can purposefully improve and study the performances of the positive electrode and the negative electrode.
5. The reference mould of the three-electrode system electrochemical testing device is made of materials with excellent mechanical strength, such as polyether ether ketone (PEEK), polytetrafluoroethylene (PTFE), high-density polyethylene (HDPE) or organic glass (PMMA), and the like, which are electrically insulated and electrochemically inert, and has no side reaction with electrolyte and stable performance.
6. According to the three-electrode system electrochemical testing device, the electrolyte is added through the liquid injection hole, so that safety and convenience are improved, and the electrolyte is accommodated in the closed cavity in the main body formed by the negative electrode die, the reference die and the positive electrode die, so that the influence of external environment is reduced, the three-electrode system electrochemical testing device is fully contacted with the reference electrode with a larger area, and the external negative electrode tab, the reference tab and the positive electrode tab are prevented from being contacted with the electrolyte, so that the accuracy of a testing result is improved.
7. The positive plate, the diaphragm, the negative plate and the electrolyte adopted by the three-electrode system electrochemical testing device are consistent with those of the button cell or the capacitor, and the preparation process is simple, and special structures and processes are not needed.
8. The component parts of the three-electrode system electrochemical testing device can be reused, and compared with button cells or capacitors, the three-electrode system electrochemical testing device has the remarkable characteristics of lower cost and the like; in addition, the three-electrode system electrochemical testing device can be assembled into a two-electrode battery or a capacitor without using a reference electrode, so that the adaptability is better.
Therefore, the utility model has the advantages of simple structure, convenient assembly, good tightness, good adaptability of the reference electrode, stable performance, and high borrowability, and the internal structure is closest to the structure of the actual battery.
Drawings
FIG. 1 is a side cross-sectional view of a three-electrode system electrochemical test device of the present utility model;
FIG. 2 is a schematic perspective view of the reference mold of FIG. 1;
FIG. 3 is a graph showing the charge and discharge performance of the three-electrode electrochemical test device according to the present utility model;
in fig. 1 and 2: 1-negative electrode mould, 1A-cavity, 2-reference mould, 2A-annular cavity, 2B-tabletting groove, 2C-countersink II, 2D-through hole II, 3-positive electrode mould, 3A-blind hole, 4-positive electrode column, 4A-metal round table, 4B-metal spring, 5-elastic pressing plate device, 5A-metal column I, 5B-elastic element, 5C-metal column II, 6-upper guide sleeve, 7-lower guide sleeve, 8-reference electrode, 9-tabletting device I, 10-negative electrode tab, 11-reference tab, 12-positive electrode tab, 13-tabletting device II, 14-sealing cover, 15-insulating spacer, 16-sealing ring, 17-screw II, 18-bolt I, 19-injection hole, 20-diaphragm, 21-insulating sleeve.
Detailed Description
The utility model is further illustrated in the following figures and examples, which are not intended to be limiting in any way, and any alterations or modifications based on the teachings of the utility model are within the scope of the utility model.
As shown in fig. 1 and 2, the electrochemical testing device of the three-electrode system comprises a negative electrode mould 1, a reference mould 2 and a positive electrode mould 3 which are mutually insulated and connected in sequence in a sealing way, wherein the negative electrode mould 1 is provided with a cavity 1A, the reference mould 2 is provided with an annular cavity 2A with an upper opening and a lower opening, the top end of the positive electrode mould 3 is provided with a blind hole 3A, a positive electrode column 4 of T-shaped metal is arranged in the blind hole 3A, the upper end of the positive electrode column 4 extends into the annular cavity 2A, an elastic pressing plate device 5 is arranged in the cavity 1A, the lower end of the elastic pressing plate device 5 extends into the annular cavity 2A and is opposite to the upper end of the positive electrode column 4, the upper end of the positive electrode column 4 in the annular cavity 2A is sequentially provided with a positive electrode plate, a diaphragm 20 and a negative electrode plate and is pressed and fixed through the elastic pressing plate device 5, the annular cavity 2A is internally provided with an upper guide sleeve 6 and a lower guide sleeve 7 which are vertically laminated and insulated outside a positive plate, a diaphragm 20 and a negative plate, a reference electrode 8 is arranged between the upper guide sleeve 6 and the lower guide sleeve 7, the negative plate is electrically connected with a negative electrode die 1 through an elastic pressing plate device 5, a positive electrode post 4 is electrically connected with the positive plate, the outsides of the negative electrode die 1, a reference die 2 and a positive electrode die 3 are respectively and correspondingly provided with a negative electrode tab 10, a reference tab 11 and a positive electrode tab 12, the negative electrode tab 10 is electrically connected with the negative electrode die 1, the reference tab 11 is electrically connected with the reference electrode 8, and the positive electrode tab 12 is electrically connected with the positive electrode die 3.
The negative plate is characterized in that a tabletting device I9 is arranged between the negative plate and the elastic pressing plate device 5, a circular arc groove with holes is formed in the top end of the tabletting device I9, the negative plate die 1 is of a flange structure, the cavity 1A is opened up and down and is provided with threads, the elastic pressing plate device 5 comprises a T-shaped metal column I5A with the bottom end being arc-shaped, an annular elastic element 5B and a stepped metal column II 5C with the upper portion being externally threaded, the elastic element 5B is sleeved on the upper portion of the metal column I5A and is in contact with the bottom end of the metal column II 5C, the metal column II 5C is connected with the negative plate die 1 through threads, the arc-shaped bottom end of the metal column I5A is in close contact with the circular arc groove with holes of the tabletting device I9, and the upper end of the cavity 1A of the negative plate die 1 is in threaded connection with a sealing cover 14.
The top end of the metal column II 5C is provided with a straight groove, a cross groove or a countersunk polygonal groove, the tabletting device I9 is of a cake-shaped or plate-shaped metal structure with a circular arc groove with holes at the top end, and the positive plate, the diaphragm 20 and the negative plate are positioned on the same horizontal plane with the reference electrode 8 by adjusting the position of the metal column II 5C.
The side wall of the annular cavity 2A is provided with a tabletting groove 2B, a platinum sheet is arranged at the bottom end of the tabletting groove 2B, and the reference electrode 8 is in close contact with the platinum sheet through a tabletting device II 13 arranged in the tabletting groove 2B.
The upper end face of the tabletting device II 13 is higher than the upper surface of the annular cavity 2A.
The side wall of the reference die 2 is provided with a connecting hole penetrating through the side wall at the lower part of the tabletting groove 2B, and the reference electrode 8 penetrates through the connecting hole to be electrically connected with the reference electrode lug 11 and is sealed.
The positive pole 4 comprises a T-shaped metal round table 4A and a metal spring 4B, the metal spring 4B is sleeved on the lower portion of the metal round table 4A, the bottom of the metal spring is in contact with the bottom of the blind hole 3A, and the positive pole piece is placed on the upper end face of the metal round table 4A.
The flange plate of the flange structure of the cathode mould 1 is provided with a plurality of screw holes I or through holes I, the reference mould 2 is of an annular structure, the periphery of the upper surface of the reference mould is provided with a plurality of countersunk holes II 2C and through holes II 2D corresponding to the screw holes I or through holes I, the anode mould 3 is of a disc-shaped structure, the flange plate is provided with a plurality of countersunk holes III corresponding to the through holes II 2D and screw holes III or through holes III corresponding to the countersunk holes II 2C respectively, the reference mould 2 is in fastening connection with the anode mould 3 through screws II 17 or bolts II penetrating through the countersunk holes II 2C and the screw holes III or through holes III, and the cathode mould 1 is in fastening connection with screws I or bolts I18 penetrating the screw holes I or through holes I and II 2D and the countersunk holes III.
The inner wall of the countersink II 2C or the screw hole III and the inner wall of the through hole III are provided with an insulating sleeve 21 or an insulating coating, and the inner wall of the through hole II 2D or the countersink III is provided with the insulating sleeve 21 or the insulating coating.
An insulating gasket 15 is arranged between two adjacent surfaces among the negative electrode die 1, the reference die 2 and the positive electrode die 3, at least one adjacent surface among the negative electrode die 1, the reference die 2 and the positive electrode die 3 is provided with a sealing groove among a through hole, a screw hole or a countersink and the annular cavity 2A, and a sealing ring 16 is arranged in the sealing groove.
The upper guide sleeve 6 and/or the lower guide sleeve 7 are provided with a plurality of through holes IV penetrating through the upper end face and the lower end face, and the upper guide sleeve 6 and/or the lower guide sleeve 7 are also provided with side holes penetrating through the side walls and communicated with the through holes IV.
The side holes are arranged on the adjacent surfaces between the upper guide sleeve 6 and/or the lower guide sleeve 7.
The reference mold 2 is made of polyether ether ketone (PEEK), polytetrafluoroethylene (PTFE), high-density polyethylene (HDPE), organic glass (PMMA) or quartz glass, the upper guide sleeve 6, the lower guide sleeve 7, the tabletting device II 13, the insulating gasket 15 and the sealing ring 16 are made of polyether ether ketone, polytetrafluoroethylene, rubber or high-density polyethylene, and the elastic element 5B is a metal spring, a rubber spring or a nylon spring.
The negative electrode die 1, the positive electrode die 3, the elastic pressing plate device 5, the positive electrode post 4, the screw II 17 or the bolt II, the screw I or the bolt I18, the sealing cover 14, the negative electrode tab 10 and the positive electrode tab 12 are made of stainless steel, aluminum or aluminum alloy; the reference tab 11 is made of a gold-plated copper bar, stainless steel, aluminum or aluminum alloy.
The separator 20 is a single layer or a multi-layer laminate manufactured by a dry process or a wet process.
The separator 20 is a multilayer stack of multiple discrete layers of similar or dissimilar polyolefins and/or polymers.
The polyolefin may be a homopolymer (derived from a single monomer component) or a heteropolymer (derived from more than one monomer component), and may be linear or branched.
The polyolefin may be Cellulose Acetate (CA), polyethylene (PE), polypropylene (PP), a blend of PE and PP, or a purely structured porous film or a multi-layered structured porous film of PE and/or PP.
The polymer includes one or a combination of several of polyethylene terephthalate (PET), polyvinylidene fluoride (PVdF), polyamide (Nylon), polyurethane, polycarbonate, polyester, polyetheretherketone (PEEK), polyethersulfone (PES), polyimide (PI), polyamide-imide, polyether, polyoxymethylene (such as acetal (acetate)), polybutylene terephthalate, polyethylene naphthalate, polybutylene, polyolefin copolymer, acrylonitrile-butadiene-styrene copolymer (ABS), polystyrene copolymer, polymethyl methacrylate (PMMA), polyvinyl chloride (PVC), polysiloxane polymer (such as Polydimethylsiloxane (PDMS)), polybenzimidazole (PBI), polybenzoxazole (PBO), polyphenylenes, polyarylene ether ketone, polyvinylperfluorocyclobutane, polytetrafluoroethylene (PTFE), polyvinylidene fluoride copolymer and terpolymer, polyvinylidene chloride, polyvinylfluoride, polyaramide, polyphenylene oxide.
The electrochemical test method of the three-electrode system electrochemical test device comprises the following steps of lower connection, reference electrode connection, other electrode connection, integral connection, electrode adjustment and test, and the specific steps are as follows:
A. the lower part is connected with: sealing, insulating, fastening and connecting the positive electrode die with the reference die;
B. the reference electrode is connected: sequentially filling a positive pole, a lower guide sleeve and a reference electrode in cavities of a positive pole die and a reference die, enabling one end of the reference electrode to be in contact with a platinum sheet at the bottom end of a tabletting groove, and then filling an upper guide sleeve;
C. other electrode connections: sequentially loading a positive plate, a diaphragm and a negative plate on the upper end face of a positive pole post, loading a tabletting device I on the upper end of the positive plate, and loading a tabletting device II into a tabletting groove;
D. and (3) integral connection: aligning the circular arc bottom end of the metal column I in the negative electrode mould with a circular arc groove with holes of the tabletting device I, and carrying out sealing, insulating, fastening and connecting the negative electrode mould with the positive electrode mould and the reference mould;
E. electrode adjustment: adding a certain amount of electrolyte into a liquid injection hole formed from the top opening of the cavity, adjusting the position of the metal column II to enable the positive plate, the diaphragm and the negative plate to be positioned at the same horizontal plane with the reference electrode, and screwing the sealing cover;
F. and (3) testing: and (3) electrically connecting the test instrument and the equipment with the negative electrode tab, the reference electrode tab and the positive electrode tab respectively, and then carrying out three-electrode test.
Example (supercapacitor charge-discharge performance test):
1. and installing a sealing ring 16 into a sealing groove of the positive electrode die 3 and/or the reference die 2, and then carrying out sealing, insulating and fastening connection on the positive electrode die 3 and the reference die 2 through a screw II 17 or a bolt II and an insulating gasket 15.
2. The cavities of the positive electrode die 3 and the reference die 2 are sequentially filled with a positive electrode column 4, a lower guide sleeve 7 and a reference electrode 8, one end of the reference electrode 8 is contacted with a platinum sheet at the bottom end of the tabletting groove 2B, and then the upper guide sleeve 6 is filled.
3. The upper end face of the positive electrode post 4 is sequentially provided with a positive electrode plate (active carbon electrode), a diaphragm 20 (cellulose acetate diaphragm) and a negative electrode plate (active carbon electrode), then the upper end of the positive electrode plate is provided with a tabletting device I9, and then a tabletting device II 13 is provided with a tabletting groove 2B.
4. The circular arc bottom end of a metal column I5A in the negative electrode mould 1 is aligned with a circular arc groove with holes of a tabletting device I9, a sealing ring 16 is arranged in a sealing groove of the negative electrode mould 1 and/or a reference mould 2, and the negative electrode mould 1, the positive electrode mould 3 and the reference mould 2 are in sealing, insulating and fastening connection through a screw I or a bolt I18 and an insulating gasket 15.
5. An electrolyte (1M/L TEA-BF) was added to the electrolyte-filled hole 19 formed from the top of the cavity 1A 4 ACN), the position of the metal column ii 5C is adjusted so that the positive, diaphragm 20 and negative plates are in the same horizontal plane as the reference electrode 8, and then the sealing cap 14 is screwed.
6. The instrument and the equipment are respectively electrically connected with the cathode tab 10, the reference tab 11 and the anode tab 12, and then the charge and discharge performance test is carried out under the room temperature condition: firstly, standing for 60 min, then, carrying out one-time charging and discharging at a current density of 0.2A/g and 0-2.7V, then, carrying out 10-time charging and discharging at a current density of 1A/g and 0-2.7V, and then, respectively carrying out 5-time charging and discharging at a current density of 0.5A/g within voltage ranges of 0-2.7V, 0-2.85V, 0-3.0V, 0-3.2V and 0-3.5V, and recording experimental data of a full capacitor and positive and negative electrodes forming the capacitor in the whole test process.
7. Test results
Such as the charge-discharge performance test curve of fig. 3.
8. Analysis of results
As can be seen from fig. 3: in the charging voltage range (2.7-3.5V), the measured charging and discharging curves of the capacitor and the anode and the cathode are stable, which shows that the reference die does not have side reaction with electrolyte in the testing process, and the reference electrode has stable performance and potential. Meanwhile, the three-electrode system electrochemical testing device and the electrochemical testing method thereof can timely and accurately measure the voltage (E) of the full capacitor under different charge and discharge voltages we – E ce ) A positive-reference electrode potential (E we – E re ) Negative electrode-reference electricityPolar potential (E) ce – E re ) The actual performance characteristics of the positive electrode and the negative electrode of the capacitor in the charging and discharging processes are truly reflected. As shown in fig. 3, when the charge cutoff voltage was set to 3.0V, positive and negative charge cutoff potentials at this time were +1.277V and-1.723V, respectively, and positive and negative potential contributions at this time were 1.317V and 1.683V, respectively, were measured. Therefore, the three-electrode system electrochemical testing device and the electrochemical testing method can be used for effectively researching the positive electrode and the negative electrode.
Claims (8)
1. The utility model provides a three-electrode system electrochemical testing device, its characterized in that, including mutual insulating and sealing connection's negative pole mould (1), reference mould (2), anodal mould (3) in proper order, negative pole mould (1) are provided with cavity (1A), cavity (1A) open-ended top forms annotates liquid hole (19), reference mould (2) are provided with upper and lower open-ended annular cavity (2A), the top of anodal mould (3) is provided with blind hole (3A), be provided with positive pole post (4) of "T" shape metal in blind hole (3A), the upper end of positive pole post (4) extends to in annular cavity (2A), be provided with elastic pressing plate device (5) in cavity (1A), the lower extreme of elastic pressing plate device (5) extends to in annular cavity (2A) and is relative with the upper end of positive pole post (4), the upper end of positive pole post (4) is provided with positive pole piece, diaphragm, negative pole piece and compresses tightly positive pole piece (5) through elastic pressing plate device, the upper and lower guide pin bushing (6) are provided with in proper order, and outside the laminating between positive pole piece (6) and the guide pin bushing (6) are provided with in proper order under the positive pole post (2A) and the guide pin bushing (6), the negative electrode plate is electrically connected with a negative electrode die (1) through an elastic pressing plate device (5), the positive electrode column (4) is electrically connected with the positive electrode plate, negative electrode lugs (10), reference lugs (11) and positive electrode lugs (12) are respectively and correspondingly arranged on the outer sides of the negative electrode die (1), the reference dies (2) and the positive electrode dies (3), the negative electrode lugs (10) are electrically connected with the negative electrode die (1), the reference lugs (11) are electrically connected with the reference electrodes (8), and the positive electrode lugs (12) are electrically connected with the positive electrode dies (3); the positive pole (4) comprises a T-shaped metal round table (4A) and a metal spring (4B), the metal spring (4B) is sleeved on the lower part of the metal round table (4A) and the bottom of the metal round table is contacted with the bottom of the blind hole (3A), and the positive pole piece is arranged on the upper end face of the metal round table (4A); the side wall of the annular cavity (2A) is provided with a tabletting groove (2B), the bottom end of the tabletting groove (2B) is provided with a platinum sheet, and the reference electrode (8) is tightly contacted with the platinum sheet through a tabletting device II (13) arranged in the tabletting groove (2B); the reference mould (2) is made of polyether-ether-ketone, polytetrafluoroethylene, high-density polyethylene, organic glass or quartz glass.
2. The three-electrode system electrochemical testing device according to claim 1, wherein a tabletting device I (9) is arranged between the negative electrode plate and the elastic pressing plate device (5), a perforated circular arc groove is formed in the top end of the tabletting device I (9), the negative electrode die (1) is of a flange structure, the upper and lower openings of the cavity (1A) are provided with threads, the elastic pressing plate device (5) comprises a T-shaped metal column I (5A) with an arc bottom end, a ring-shaped elastic element (5B) and a stepped metal column II (5C) with an external upper thread, the elastic element (5B) is sleeved on the upper part of the metal column I (5A) and is in contact with the bottom end of the metal column II (5C), the metal column II (5C) is connected with the negative electrode die (1) through threads, the arc bottom end of the metal column I (5A) is in close contact with the perforated circular arc groove of the tabletting device I (9), and a sealing cover (14) is connected to the upper end of the cavity (1A) of the negative electrode die (1) through threads.
3. The three-electrode system electrochemical testing device according to claim 2, wherein the top end of the metal column II (5C) is provided with a straight groove, a cross groove or a countersunk polygonal groove, the tablet device I (9) is of a cake-shaped or plate-shaped metal structure with a circular arc groove with holes at the top end, and the positive electrode plate, the diaphragm and the negative electrode plate are positioned on the same horizontal plane with the reference electrode (8) by adjusting the position of the metal column II (5C).
4. The three-electrode system electrochemical testing device according to claim 2, wherein the flange plate of the flange structure of the negative electrode mold (1) is provided with a plurality of screw holes I or through holes I, the reference mold (2) is of an annular structure, the periphery of the upper surface of the reference mold is provided with a plurality of countersunk holes II (2C) and through holes II (2D) corresponding to the screw holes I or through holes I, the positive electrode mold (3) is of a disc-shaped structure, the flange plate is provided with a plurality of countersunk holes III corresponding to the through holes II (2D) and screw holes III or through holes III corresponding to the countersunk holes II (2C), the reference mold (2) is fixedly connected with the positive electrode mold (3) through screws II (17) or bolts II penetrating through the countersunk holes II (2C) and the screw holes III or through holes II (2D), and the negative electrode mold (1) is fixedly connected with the screws I or bolts I (18) penetrating the countersunk holes II (2D).
5. The electrochemical testing device of the three-electrode system according to claim 4, wherein the inner wall of the countersink II (2C) or the screw hole III and the inner wall of the through hole III are provided with an insulating sleeve or an insulating coating, and the inner wall of the through hole II (2D) or the countersink III is provided with an insulating sleeve or an insulating coating.
6. The three-electrode system electrochemical testing device according to claim 1, wherein an insulating gasket (15) is arranged between two adjacent surfaces among the negative electrode die (1), the reference die (2) and the positive electrode die (3), at least one adjacent surface among two adjacent surfaces among the negative electrode die (1), the reference die (2) and the positive electrode die (3) is provided with a sealing groove between a through hole, a screw hole or a countersunk hole and the annular cavity (2A), and a sealing ring (16) is arranged in the sealing groove.
7. The electrochemical testing device of the three-electrode system according to claim 1, wherein the upper guide sleeve (6) and/or the lower guide sleeve (7) are provided with a plurality of through holes IV penetrating through the upper end face and the lower end face, and the upper guide sleeve (6) and/or the lower guide sleeve (7) are also provided with side holes penetrating through the side walls and communicated with the through holes IV.
8. An electrochemical testing method based on the three-electrode system electrochemical testing device according to any one of claims 1-7, which is characterized by comprising the following specific steps of lower connection, reference electrode connection, other electrode connection, integral connection, electrode adjustment and testing:
A. the lower part is connected with: the positive electrode die (3) and the reference die (2) are connected in a sealing, insulating and fastening manner;
B. the reference electrode is connected: the positive pole (4), the lower guide sleeve (7) and the reference electrode (8) are sequentially arranged in the cavities of the positive pole die (3) and the reference die (2), one end of the reference electrode (8) is contacted with a platinum sheet at the bottom end of the tabletting groove (2B), and then the upper guide sleeve (6) is arranged;
C. other electrode connections: sequentially loading a positive plate, a diaphragm and a negative plate on the upper end face of a positive pole column (4), loading a tabletting device I (9) on the upper end of the positive plate, and loading a tabletting device II (13) into a tabletting groove (2B);
D. and (3) integral connection: aligning the circular arc bottom end of a metal column I (5A) in the negative electrode mould (1) with a circular arc groove with holes of a tabletting device I (9), and carrying out sealing, insulating and fastening connection on the negative electrode mould (1) with the positive electrode mould (3) and the reference mould (2);
E. electrode adjustment: adding a certain amount of electrolyte into a liquid injection hole (19) formed by the opening at the top of the cavity (1A), adjusting the position of the metal column II (5C) to enable the positive plate, the diaphragm, the negative plate and the reference electrode (8) to be positioned at the same horizontal plane, and screwing the sealing cover (14);
F. and (3) testing: and (3) electrically connecting the test instrument and the equipment with the negative electrode tab (10), the reference tab (11) and the positive electrode tab (12) respectively, and then carrying out three-electrode test.
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CN113092355A (en) * | 2021-04-06 | 2021-07-09 | 上海建冶科技股份有限公司 | Detection apparatus for real-time detection metal corrosion rate |
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