CN111398683A - Solid electrolyte ionic conductivity test fixture and test method - Google Patents
Solid electrolyte ionic conductivity test fixture and test method Download PDFInfo
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- CN111398683A CN111398683A CN202010215687.6A CN202010215687A CN111398683A CN 111398683 A CN111398683 A CN 111398683A CN 202010215687 A CN202010215687 A CN 202010215687A CN 111398683 A CN111398683 A CN 111398683A
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- solid electrolyte
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R27/00—Arrangements for measuring resistance, reactance, impedance, or electric characteristics derived therefrom
- G01R27/02—Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant
- G01R27/08—Measuring resistance by measuring both voltage and current
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R1/00—Details of instruments or arrangements of the types included in groups G01R5/00 - G01R13/00 and G01R31/00
- G01R1/02—General constructional details
- G01R1/04—Housings; Supporting members; Arrangements of terminals
- G01R1/0408—Test fixtures or contact fields; Connectors or connecting adaptors; Test clips; Test sockets
- G01R1/0425—Test clips, e.g. for IC's
Abstract
The invention provides an ion conductivity test fixture for solid electrolyte, which comprises at least two fixture units fixedly connected with each other, wherein each fixture unit is of a container structure with an electrolyte filling inlet, a sealing part is installed on each electrolyte filling inlet, a cavity is formed in each fixture unit, each electrolyte filling inlet is communicated with the corresponding cavity, a through hole communicated with the corresponding cavity is further formed in the outer wall of each fixture unit, the solid electrolyte is fixed at the through hole, a current electrode positioning part for fixing a current electrode is arranged on the inner wall of each cavity, the current electrode positioning part is communicated with a current electrode threading hole, a voltage electrode positioning part for fixing a voltage electrode is arranged on the outer wall of each fixture unit, the voltage electrode positioning part is communicated with the through hole, and the current electrodes and the voltage electrodes are arranged in parallel. The invention also provides a test method of the ion conductivity test fixture for the solid electrolyte. Compared with the prior art, the test cost is lower, the clamp structure is simple, the operation is convenient, and the test accuracy is high.
Description
Technical Field
The invention relates to the field of lithium ion battery material testing, in particular to an ionic conductivity testing clamp and a testing method for a solid electrolyte.
Background
The lithium ion battery plays an important role in daily life, including the fields of electronic consumption, power automobiles, energy storage and the like, however, with the rapid development of society, higher requirements on the performance of the lithium ion battery are provided, higher energy density and longer cycle life are achieved, and the lithium ion battery is safer and cheaper and becomes the research focus of the current lithium ion battery. The traditional lithium ion battery adopts liquid electrolyte, but the thermal stability is poor, and the safety accidents such as combustion, even explosion and the like are easily caused under the conditions of high temperature, short circuit, overcharge or physical collision. The all-solid-state battery adopts solid electrolyte to replace traditional liquid electrolyte, is not easy to burn, and ensures the safety performance, so the all-solid-state battery is concerned.
The solid electrolyte is an important component of the solid-state battery, and the preparation of the solid electrolyte with high ionic conductivity is the key to obtaining the high-performance solid-state battery, so that the ionic conductivity as an important parameter is often required to be rapidly detected in the performance test of the solid-state electrolyte. However, the current method for testing the ion conductivity of the solid electrolyte still has a plurality of defects. The conventional detection method is that after a solid electrolyte is pressed into a sheet or made into a film, gold is sprayed on the surface of the solid electrolyte film or the sheet, finally, the gold-sprayed electrolyte film or the sheet is placed in a blocking electrode for alternating current impedance test, and the ionic conductivity of the electrolyte is calculated according to an analog circuit. The method for testing the solid electrolyte firstly needs the noble metal gold powder to be sprayed on the surface of the electrolyte material, has higher cost, secondly uses an alternating current impedance method, needs an accurate analog circuit to calculate and distinguish the ionic conductivity and the electronic conductivity, and has complex process.
Disclosure of Invention
In view of this, the invention provides the solid electrolyte ionic conductivity test fixture and the test method, which have the advantages of lower test cost, simple fixture structure, convenient operation and high test accuracy.
Therefore, on one hand, the invention provides an ion conductivity test fixture for solid electrolyte, which comprises at least two fixture units fixedly connected with each other, wherein each fixture unit is of a container structure with an electrolyte filling inlet, a sealing part is installed on each electrolyte filling inlet, a cavity is formed in each fixture unit, each electrolyte filling inlet is communicated with the cavity, through holes communicated with the cavity are further formed in the outer wall of each fixture unit, after the two adjacent fixture units are butted, the through holes of the two fixture units are communicated, the solid electrolyte is fixed at the through holes, a current electrode positioning part for fixing current electrodes is arranged on the inner wall of the cavity, the current electrode positioning part is communicated with current electrode threading holes, wire outlets of the current electrode threading holes extend to the outer wall of each fixture unit, and a voltage electrode positioning part for fixing voltage electrodes is arranged on the outer wall of each fixture unit, the voltage electrode positioning component is communicated with the through hole, and the current electrode and the voltage electrode are arranged in parallel.
Further, the sealing member is a sealing cap body for blocking the electrolyte filling inlet.
Furthermore, the current electrode positioning part is a positioning groove body arranged on the inner wall of the cavity.
Furthermore, the voltage electrode positioning component is a hole body.
Further, the through hole is formed at an end portion on the outer wall of the holder unit to form a positioning groove in which the solid electrolyte is fixed.
Furthermore, a connecting screw hole penetrating through the clamp units is formed in each clamp unit, and a screw penetrates through the connecting screw hole between every two adjacent clamp units to fixedly connect the two adjacent clamp units together.
Furthermore, the overall shape of the clamp unit is a rectangular body.
Furthermore, the clamp unit is made of polytetrafluoroethylene.
In another aspect, the present invention provides a method for testing an ion conductivity test fixture for a solid electrolyte, comprising the steps of:
1) before the conductivity test of the solid electrolyte, pressing the solid electrolyte powder into a sheet or manufacturing the solid electrolyte powder into a film, placing the film at the joint between two adjacent clamp units, fastening the two adjacent clamp units together, placing a metal wire at a voltage electrode positioning part, bending one end of the metal wire to be close to the solid electrolyte, and keeping two voltage electrodes and two current electrodes parallel;
2) opening the sealing part, filling electrolyte into the electrolyte filling inlet so that the liquid level of the added electrolyte is higher than the upper part of the solid electrolyte, and then closing the sealing part, wherein the whole process of adding the electrolyte is carried out in a glove box or a drying room with controlled humidity;
3) transferring the whole clamp filled with the solid electrolyte to an electrochemical workstation, connecting a current voltage wire, applying a voltage with any magnitude, and testing to obtain corresponding current;
according to the formula:
obtaining a resistance value;
according to the formula:
calculating to obtain the conductivity of the solid electrolyte;
wherein σ is the conductivity (S/cm) of the solid electrolyte;
s is the area (cm) of the central circular hole of the clamp2)；
L is the thickness (cm) of the solid electrolyte sheet or film;
u is the applied voltage magnitude (V);
i is the corresponding measured current magnitude (A) after voltage is applied;
r is the resistance (omega) obtained by a direct current method.
Furthermore, the voltage electrode is made of a lithium wire close to one end of the solid electrolyte, the other end of the lithium wire is connected with the metal wire, the other end of the metal wire extends out to be connected with the electrochemical workstation, and the lithium wire is bent to be close to the surface of the solid electrolyte during testing.
The method utilizes a four-electrode direct current method to measure the ionic conductivity of the solid electrolyte, avoids the complex processes of introducing an analog circuit and calculating and the like in the test of an alternating current impedance method, solves the problem of interface resistance because the surface of the solid electrolyte is directly contacted with a liquid ionic conductor (electrolyte), avoids introducing gold spraying equipment and a noble metal gold target, and has lower cost;
meanwhile, the invention utilizes the electrochemical workstation to test the conductivity of the solid electrolyte according to the principle of four electrodes, is suitable for the measurement of the ionic conductivity of a solid electrolyte sheet or film made of ceramic oxide or polymer or the mixture of the ceramic oxide and the polymer.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a perspective view of an ion conductivity test fixture for a solid electrolyte according to the present invention;
FIG. 2 is a top view of an ion conductivity test fixture for a solid electrolyte in accordance with the present invention;
FIG. 3 is a cross-sectional view taken along line A-A of FIG. 2;
FIG. 4 is a schematic diagram showing an external structure of a holder unit in an ion conductivity test holder for a solid electrolyte according to the present invention;
fig. 5 is a schematic diagram illustrating an internal structure of a clamp unit in the ion conductivity test clamp for a solid electrolyte according to the present invention.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
Referring to fig. 1 to 5, which illustrate an ion conductivity testing fixture for a solid electrolyte provided by an embodiment of the present invention, the testing fixture is composed of two fixture units 1 that are fixedly connected and symmetrical, the overall appearance of the fixture unit 1 is a rectangular body, the fixture unit 1 is a container structure having an electrolyte filling inlet 11 with a top, a sealing member 111 is installed on the electrolyte filling inlet 11, the sealing member 111 is a sealing cover body that blocks the electrolyte filling inlet 11, a cavity 12 is formed in the fixture unit 1, the electrolyte filling inlet 11 is communicated with the cavity 12, a through hole 13 communicated with the cavity 12 is further formed on an outer wall of the fixture unit 1, after two adjacent fixture units 1 are butted, the through holes 13 of the two fixture units 1 are communicated with each other, a circular positioning groove 131 is formed at an end of the through hole 13 on the outer wall of the fixture unit 1, and the solid electrolyte is fixed in the positioning groove 131, be provided with the current electrode locating component 21 of fixed current electrode 2 on the inner wall of cavity 12, current electrode locating component 21 specifically is the location cell body of seting up on the inner wall of cavity 12, current electrode locating component 21 intercommunication current electrode through wires hole 22, the outlet of current electrode through wires hole 22 extends to on the outer wall of anchor clamps unit 1, be provided with the voltage electrode locating component 31 of fixed voltage electrode 3 on the outer wall of anchor clamps unit 1, voltage electrode locating component 31 specifically is a hole body, voltage electrode locating component 31 intercommunication through-hole 13, parallel arrangement between current electrode 2 and the voltage electrode 3.
Referring to fig. 1 to 5, the clamp units 1 are provided with connecting screw holes 14 penetrating through the clamp units 1, and between two adjacent clamp units 1, screws penetrate into the connecting screw holes 14 to fixedly connect the two adjacent clamp units 1 together.
Specifically, the clamp unit 1 and the sealing member 111 are made of polytetrafluoroethylene, so that electrolyte corrosion resistance is guaranteed, and sealing performance is good during testing.
In one embodiment, a quantity of solid electrolyte L i is taken1.5Al0.5Ge1.5P3O12(L AGP) powder is pre-pressed into tablets in a tablet press under the pressure of 3MPa, then pressed into tablets under the pressure of 20MPa and formed in an isostatic press, and finally calcined for 4 hours in the air atmosphere at the temperature of 800 ℃;
the fixture is placed in a glove box, and a lithium sheet is pressed on the metal plates of the current electrodes at two ends of the fixture respectively, wherein one electrode is used as a working electrode, and the other electrode is used as a counter electrode. Taking out the solid electrolyte sheet, putting the solid electrolyte sheet into the central opening of the clamp, then putting screws into the screw through holes on the periphery of the clamp, and screwing and fixing the left part and the right part;
cutting two lithium wires, respectively putting the two lithium wires into the two voltage electrode through holes, wherein one end of each lithium wire is bent to be close to the surface of the solid electrolyte sheet, the other end of each lithium wire is connected with a copper wire in a winding manner, and the other end of each copper wire is led out to be connected with an electrochemical workstation clamp; adding conventional electrolyte at an electrolyte filling inlet, wherein the height of the electrolyte level exceeds the upper end of the solid electrolyte sheet, and then adding a sealing part at the opening for sealing;
and respectively connecting the two current electrodes and the voltage electrode with an electrochemical workstation, applying a constant voltage, testing to obtain a corresponding current result, and calculating to obtain the ionic conductivity of the solid electrolyte sheet according to the thickness and the area of the solid electrolyte sheet.
With reference to fig. 1 to 5, a specific test method includes the following steps:
s1: before the solid electrolyte conductivity test, pressing solid electrolyte powder into a sheet (aiming at ceramic oxide solid electrolyte) or a film (aiming at polymer electrolyte), placing the sheet at the joint between two adjacent clamp units 1, placing screws in through holes at four corners of the clamp and screwing, fastening the left clamp unit and the right clamp unit 1 together, placing a metal wire at a voltage electrode positioning part 31, bending one end of the metal wire close to the solid electrolyte, and keeping two voltage electrodes parallel to two current electrodes;
s2: opening the sealing member 111, filling the electrolyte into the electrolyte filling inlet 11 so that the liquid level of the added electrolyte is higher than the upper part of the solid electrolyte, and then closing the sealing member 111, wherein the whole process of adding the electrolyte is carried out in a glove box or a drying room with controlled humidity;
s3: transferring the whole clamp filled with the solid electrolyte to an electrochemical workstation, connecting a current voltage wire, applying a voltage with any magnitude, and testing to obtain corresponding current;
according to the formula:
obtaining a resistance value;
according to the formula:
calculating to obtain the conductivity of the solid electrolyte;
wherein σ is the conductivity S/cm of the solid electrolyte;
s is the size area cm of the central circular hole of the clamp2；
L is the thickness cm of the solid electrolyte sheet or film;
u is the applied voltage magnitude V;
i is the current A measured correspondingly after voltage is applied;
r is the resistance omega obtained by a direct current method.
The voltage electrode is made of a material, one end of the voltage electrode, which is close to the solid electrolyte, is provided with a lithium wire, the other end of the lithium wire is connected with a metal wire, the other end of the metal wire extends out to be connected with an electrochemical workstation, and the lithium wire is bent to be close to the surface of the solid electrolyte during testing.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. The utility model provides an ionic conductivity test fixture of solid state electrolyte which characterized in that: the clamp comprises at least two clamp units (1) fixedly connected with each other, the clamp units (1) are of a container structure with an electrolyte filling inlet (11), a sealing part (111) is installed on the electrolyte filling inlet (11), a cavity (12) is formed in each clamp unit (1), the electrolyte filling inlet (11) is communicated with the cavity (12), through holes (13) communicated with the cavity (12) are further formed in the outer wall of each clamp unit (1), after the two adjacent clamp units (1) are butted, the through holes (13) of the two clamp units (1) are communicated with each other, solid electrolyte is fixed at the through holes (13), a current electrode positioning part (21) for fixing a current electrode (2) is arranged on the inner wall of each cavity (12), and the current electrode positioning part (21) is communicated with a current electrode threading hole (22), the wire outlet of the current electrode threading hole (22) extends to the outer wall of the clamp unit (1), a voltage electrode positioning part (31) for fixing the voltage electrode (3) is arranged on the outer wall of the clamp unit (1), the voltage electrode positioning part (31) is communicated with the through hole (13), and the current electrode (2) and the voltage electrode (3) are arranged in parallel.
2. The ionic conductivity test fixture of solid electrolyte as claimed in claim 1, wherein: the sealing component (111) is a sealing cover body for blocking the electrolyte filling inlet (11).
3. The ionic conductivity test fixture of solid electrolyte as claimed in claim 1, wherein: the current electrode positioning part (21) is a positioning groove body arranged on the inner wall of the cavity (12).
4. The ionic conductivity test fixture of solid electrolyte as claimed in claim 1, wherein: the voltage electrode positioning part (31) is a hole body.
5. The ionic conductivity test fixture of solid electrolyte as claimed in claim 1, wherein: the end part of the through hole (13) positioned on the outer wall of the clamp unit (1) forms a positioning groove (131), and the solid electrolyte is fixed in the positioning groove (131).
6. The ionic conductivity test fixture of solid electrolyte as claimed in claim 1, wherein: the clamp unit (1) is provided with a connecting screw hole (14) penetrating through the clamp unit (1), a screw penetrates between every two adjacent clamp units (1) through the connecting screw hole (14) to fixedly connect the two adjacent clamp units (1) together.
7. The ionic conductivity test fixture of solid electrolyte as claimed in claim 1, wherein: the overall appearance of the clamp unit (1) is a rectangular body.
8. The ion conductivity test fixture for solid electrolyte as claimed in claim 1 or 8, wherein: the clamp unit (1) is made of polytetrafluoroethylene.
9. The method for testing an ion conductivity test jig for a solid electrolyte according to any one of claims 1 to 8, wherein: the method comprises the following steps:
1) before the conductivity test of the solid electrolyte, pressing solid electrolyte powder into a sheet or manufacturing a film, placing the sheet or the film at the joint between two adjacent clamp units (1), fastening the two adjacent clamp units (1) together, placing a metal wire at the position of the voltage electrode positioning part (31), wherein one end of the metal wire is bent to be close to the solid electrolyte, and two voltage electrodes and two current electrodes are kept parallel;
2) opening the sealing part (111), filling the electrolyte into the electrolyte filling inlet (11) to enable the liquid level of the added electrolyte to be higher than the upper part of the solid electrolyte, and then closing the sealing part (111), wherein the whole process of adding the electrolyte is carried out in a glove box or a drying room with controlled humidity;
3) transferring the whole clamp filled with the solid electrolyte to an electrochemical workstation, connecting a current voltage wire, applying a voltage with any magnitude, and testing to obtain corresponding current;
according to the formula:
obtaining a resistance value;
according to the formula:
calculating to obtain the conductivity of the solid electrolyte;
wherein σ is the conductivity (S/cm) of the solid electrolyte;
s is the area (cm) of the central circular hole of the clamp2)；
L is the thickness (cm) of the solid electrolyte sheet or film;
u is the applied voltage magnitude (V);
i is the corresponding measured current magnitude (A) after voltage is applied;
r is the resistance (Q) obtained by a direct current method.
10. The method of claim 9, wherein the step of testing the ion conductivity test fixture for the solid electrolyte comprises: the voltage electrode is made of a material, one end of the voltage electrode, which is close to the solid electrolyte, is provided with a lithium wire, the other end of the lithium wire is connected with the metal wire, the other end of the metal wire extends out to be connected with the electrochemical workstation, and the lithium wire is bent to be close to the surface of the solid electrolyte during testing.
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| CN202010215687.6A CN111398683B (en) | 2020-03-24 | 2020-03-24 | Solid electrolyte ionic conductivity test fixture and test method |
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| CN112033927A (en) * | 2020-08-07 | 2020-12-04 | 合肥国轩高科动力能源有限公司 | Detection method for ion conductivity of solid electrolyte |
| CN112748160A (en) * | 2020-12-18 | 2021-05-04 | 天津力神电池股份有限公司 | Method for testing lithium ion migration number of lithium ion battery electrolyte |
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