Device for testing ionic conductivity of high-flux solid electrolyte

Abstract

The utility model belongs to the technical field of conductivity testing, and particularly relates to a high-flux solid electrolyte ionic conductivity testing device. The device comprises a hydraulic device; the XY two-dimensional displacement table is mounted on a working table of the hydraulic device; the base is installed on the XY two-dimensional displacement table, and the XY two-dimensional displacement table drives the base to move in the XY direction; a plurality of grooves for containing samples are formed in the base; the probe is mounted at the top of the hydraulic device and is arranged above the base; and the probe and the base are respectively connected with an electrochemical workstation. According to the device, the position of the base can be quickly and accurately adjusted, so that the probe is aligned with a measured channel, the time and errors of manual adjustment are reduced, the measurement efficiency is greatly improved, and a foundation is laid for realizing full-automatic measurement without manual intervention in the later period; in addition, a plurality of samples can be measured at the same time, and the test flux is improved.

Description

Technical Field

[0001] This utility model belongs to the field of conductivity testing technology, specifically relating to a high-throughput solid electrolyte ionic conductivity testing device. Background Technology

[0002] Accurate determination of the electrochemical performance of solid thin film and powder samples is crucial in the development of solid-state batteries and fuel cells, encompassing performance parameters such as ionic conductivity, electronic conductivity, and electrochemical window. Measuring the electrochemical performance of solid materials differs significantly from that of liquid materials, as solid materials exhibit higher hardness and lack fluidity. This easily leads to two key problems during measurement: first, ensuring good contact between the measuring electrode and the material; and second, if the solid material is in powder form, ensuring effective contact between particles within the sample. Applying pressure is the most direct means to improve these contact issues. Therefore, many existing technologies employ devices capable of applying external pressure to achieve accurate measurement of the electrochemical performance of solid materials.

[0003] For example, the patent application document with authorization announcement number CN103728472A mentions:

[0004] A fixture for measuring the proton conductivity of a proton exchange membrane includes an upper tab 54 located at the upper end of the upper electrode 51 and a lower tab 55 located at the lower end of the lower electrode 52, serving as the two electrodes of the test fixture. Label 53 indicates a sleeve, labels 57 and 58 indicate the two test surfaces, and label 56 indicates a glass window. The sample is applied between labels 57 and 58. The AC impedance of the thin film under test can be measured by connecting the two tabs 54 and 55 to an electrochemical workstation.

[0005] It is evident that the aforementioned measuring fixture is only suitable for measuring a single or small number of samples. However, in high-throughput experimental scenarios, the number of samples to be tested in a short period may reach dozens or even hundreds, a requirement that cannot be met by this single measuring device. The specific reasons are as follows:

[0006] Firstly, from a time perspective, measuring a single sample takes a considerable amount of time. The testing process involves steps such as loading the testing device, pressurizing and densifying the sample, maintaining the pressure, sealing the device, and performing measurement and cleaning. Typically, measuring a single sample takes more than 20 minutes. In high-throughput experiments, this significantly increases the overall experimental time, leading to inefficiency.

[0007] Secondly, from an operational perspective, single-channel measurements are cumbersome and time-consuming. Due to their design characteristics, multi-channel or rapid measurements are not feasible. This makes it difficult to meet the requirements of high-throughput experiments for efficient and rapid data acquisition when dealing with a large number of samples.

[0008] Based on this, the present invention provides a novel high-throughput solid electrolyte ionic conductivity testing device to overcome the above-mentioned defects. Utility Model Content

[0009] The purpose of this invention is to provide a high-throughput solid electrolyte ionic conductivity testing device. This device can quickly and accurately adjust the base position so that the probe is aligned with the channel being tested, reducing the time and error of manual adjustment and greatly improving the measurement efficiency. This lays the foundation for achieving fully automated measurement without human intervention in the future. In addition, it can measure multiple samples simultaneously, increasing the test throughput.

[0010] This utility model adopts the following technical solution: a high-throughput solid electrolyte ionic conductivity testing device, comprising:

[0011] Hydraulic devices;

[0012] An XY two-dimensional displacement stage is mounted on the worktable of the hydraulic device.

[0013] A base is mounted on the XY two-dimensional displacement stage and is driven to move in the XY direction by the XY two-dimensional displacement stage; the base has multiple grooves for holding samples.

[0014] A probe is mounted on top of the hydraulic device and positioned above the base; the probe and the base are respectively used to connect to an electrochemical workstation.

[0015] Furthermore, an insulating sleeve is fitted over the probe.

[0016] Furthermore, the insulating sleeve is made of PEEK plastic.

[0017] Furthermore, the bottom of the insulating sleeve is shaped like an inverted frustum.

[0018] Furthermore, the probe is made of stainless steel or high-purity titanium, and the diameter of the probe is less than or equal to 3 mm.

[0019] Furthermore, the base is made of stainless steel or high-purity titanium.

[0020] Furthermore, the grooves on the base are arranged in an array, and the grooves are circular.

[0021] Furthermore, the depth of the groove is less than or equal to 1 mm, the diameter of the groove is less than or equal to 3 mm, and the diameter of the probe is less than or equal to 3 mm.

[0022] Furthermore, the bottom of the hydraulic device's worktable is equipped with a lifting mechanism, which is connected to the worktable in a transmission manner to drive the worktable to move up and down.

[0023] Furthermore, the XY two-dimensional displacement stage includes an X-axis moving module mounted on the worktable and a Y-axis moving module mounted on the X-axis moving module, with the base fixedly mounted on the Y-axis moving module.

[0024] Compared with the prior art, the beneficial effects of this utility model are as follows:

[0025] In using this high-throughput solid electrolyte ionic conductivity testing device, the sample-containing base is first mounted on an XY two-dimensional displacement stage, and the probe is correspondingly connected to the base on an electrochemical workstation. Then, the position of the base is adjusted using the XY two-dimensional displacement stage so that the probe is aligned with the channel to be measured (i.e., a groove on the base). Next, the hydraulic device is activated to drive the movement of the probe or base, bringing them into contact and applying pressure until the set pressure is reached, thus completing the electrochemical impedance measurement of the sample. The hydraulic pressure allows the measuring electrode to be pressed against the surface of the solid material, making it adhere more tightly to the material and increasing the contact area. Furthermore, the pressure can reduce or even eliminate the gap between the electrode and the material. When pressure is applied, the electrode and material undergo slight deformation, filling the gap and improving the tightness of the contact. Good contact improves the accuracy and reliability of the measurement.

[0026] Meanwhile, the use of an XY two-dimensional displacement stage allows for rapid and accurate adjustment of the base position, ensuring the probe is aligned with the measured channel. This reduces the time and error associated with manual adjustments, improving measurement preparation efficiency. Existing technologies require approximately 20 minutes to complete a single ionic conductivity measurement, and 33 hours for 100 samples, involving significant manual operation. This new design, however, reduces the measurement time for a single sample to less than 2 minutes, and only 3 hours for 100 samples, greatly improving measurement efficiency and laying the foundation for fully automated, unmanned measurements in the future.

[0027] Furthermore, multiple grooves are formed on the base for holding samples, allowing for the simultaneous measurement of multiple samples and increasing test throughput. This device is also applicable to different types of solid materials, including solid films and powder samples, offering high flexibility and versatility to meet diverse research and development needs. Attached Figure Description

[0028] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0029] Figure 1 This is a schematic diagram of the structure of a fixture used in the prior art for measuring the proton conductivity of proton exchange membranes;

[0030] Figure 2 This is a schematic diagram of the fixture structure for measuring the proton conductivity of a proton exchange membrane in a specific embodiment of this utility model. Figure 1 ;

[0031] Figure 3 This is a schematic diagram of the fixture structure for measuring the proton conductivity of a proton exchange membrane in a specific embodiment of this utility model. Figure 2 ;

[0032] Figure 4 for Figure 2 Schematic diagram of the XY two-dimensional displacement stage and base structure;

[0033] The components include: hydraulic device 1, worktable 10, lifting mechanism 11; XY two-dimensional displacement stage 2, X-axis moving module 20, Y-axis moving module 21; base 3, groove 30; probe 4; upper electrode 51, lower electrode 52, sleeve 53, upper electrode lug 54, lower electrode lug 55, glass window 56, upper test surface 57, and lower test surface 58. Detailed Implementation

[0034] The technical solutions of the embodiments of this utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this utility model, and not all embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of this utility model.

[0035] The following is in conjunction with the appendix Figure 2 To be continued Figure 4 The present invention will be described in detail with reference to specific embodiments:

[0036] like Figure 2-4 As shown, this utility model provides a high-throughput solid electrolyte ionic conductivity testing device, mainly for high-throughput measurement of ionic conductivity in electrochemical performance. It includes a hydraulic device 1, an XY two-dimensional displacement stage 2, a base 3, and a probe 4. It adopts a two-electrode measurement mode, that is, the measuring probe 4 is one electrode, and the base 3 that loads the sample is the other electrode.

[0037] The XY two-dimensional displacement stage 2 is mounted on the worktable 10 of the hydraulic device 1; the base 3 is mounted on the XY two-dimensional displacement stage 2 and is driven by the XY two-dimensional displacement stage 2 to move along the XY direction; the base 3 has a plurality of grooves 30 for holding samples.

[0038] The probe 4 is mounted on top of the hydraulic device 1, positioned above the base 3. The probe 4 and base 3 are respectively used to connect to an electrochemical workstation to perform electrochemical impedance spectroscopy on the testing device.

[0039] In use, first install the sample-containing base 3 on the XY two-dimensional displacement stage 2, and connect the probe 4 to the electrochemical workstation accordingly. Then, adjust the position of the base 3 using the XY two-dimensional displacement stage 2 so that the probe 4 is aligned with the channel to be measured (i.e., a groove on the base 3). Next, activate the hydraulic device 1 to drive the movement of the probe 4 or the base 3, causing them to come into contact and apply pressure until the set pressure is reached. For example, the probe 4 can be driven downwards to stop at the corresponding position on the base 3 and pressure can be applied until the set pressure is reached; or the worktable 10 on the hydraulic device 1 can be driven upwards to stop at the probe 4 and pressure can be applied until the set pressure is reached. Finally, perform electrochemical impedance spectroscopy on the sample. In use, pressure is applied by the hydraulic device 1, which pressurizes the measuring electrode against the surface of the solid material, making it fit more tightly against the material and thus increasing the contact area. The pressure can also reduce or even eliminate the gap between the electrode and the material. When pressure is applied, the electrode and the material undergo slight deformation, filling the gap between them and improving the tightness of the contact. Ensuring good contact can improve the accuracy and reliability of the measurement, obtain more accurate electrochemical performance parameters, such as ionic conductivity, and provide more valuable data for the development of solid-state batteries and fuel cells.

[0040] This invention relates to a high-throughput solid electrolyte ionic conductivity testing device. It employs an XY two-dimensional displacement stage 2, which allows for rapid and accurate adjustment of the base 3, aligning the probe 4 with the measured channel. This reduces manual adjustment time and errors, improving measurement preparation efficiency. Existing technologies require approximately 20 minutes to complete a single ionic conductivity measurement, and 33 hours for 100 samples, involving significant manual operation. This new design, however, reduces the measurement time for a single sample to less than 2 minutes, and only 3 hours for 100 samples, greatly improving measurement efficiency and laying the foundation for fully automated, unmanned measurement in the future.

[0041] Furthermore, the multiple grooves 30 on the base 3 can simultaneously hold multiple samples. Controlled by the XY two-dimensional displacement stage 2, multiple samples can be measured rapidly in sequence, achieving multi-channel measurement. This device is also applicable to different types of solid materials, including solid films and powder samples, offering high flexibility and versatility to meet diverse research and development needs.

[0042] Furthermore, in some specific embodiments, an insulating sleeve 40 is fitted over the probe 4. This insulating sleeve 40 is made of PEEK plastic. PEEK plastic has excellent insulation properties. Fitting the probe 4 with a PEEK plastic insulating sleeve 40 effectively prevents short circuits between the probe 4 and the surrounding environment, mitigating the problem of frequent short circuits. In electrochemical performance testing, especially when small-sized probes 4 and complex testing environments are involved, short circuits can lead to inaccurate measurement results or even damage to the testing equipment. Simultaneously, PEEK plastic has high mechanical strength and wear resistance, and the insulating sleeve 40 can protect the probe 4 from external physical damage, extending its service life. In actual testing, the probe 4 may be subjected to impacts, friction, or other external forces, and the insulating sleeve 40 can act as a buffer and protector.

[0043] In this embodiment, the bottom of the insulating sleeve 40 is shaped like an inverted frustum. During automated measurement, the inverted frustum shape helps the probe quickly and accurately locate the target position, improving measurement efficiency and accuracy. Simultaneously, when the probe 4 contacts the sample, the inverted frustum shape increases the contact area between the insulating sleeve 40 and the sample, helping to improve the stability of the probe 4 and reduce probe wobbling or displacement caused by external forces during measurement.

[0044] Specifically, in this embodiment, the probe 4 is made of stainless steel or high-purity titanium, and its diameter is less than or equal to 3 mm. Generally, high-purity titanium can achieve a purity of 99.99% or higher. Both stainless steel and high-purity titanium possess excellent electrical conductivity and corrosion resistance. In electrochemical performance testing, the probe 4 needs to maintain good electrical contact with the sample being tested, while also resisting corrosive factors in the testing environment. Probes made of stainless steel or high-purity titanium can meet these requirements, ensuring the accuracy and reliability of the measurement.

[0045] Meanwhile, compared to existing technologies that use a pole-shaped probe with a large cross-sectional area, requiring pressure in the ton range to maintain the same vertical pressure (300-400 MPa), and placing high demands on the pressurizing equipment, this device uses a probe 4 with a diameter of less than 3 mm, achieving a pressure of around 100 kg at the same pressure. This significantly reduces the required pressure and is more user-friendly for pressurizing equipment. This allows for the use of smaller, more economical pressurizing equipment, reducing equipment costs and maintenance difficulty, while also improving the reliability and stability of the equipment.

[0046] Furthermore, in some specific embodiments, the base 3 is made of stainless steel or high-purity titanium. Stainless steel and high-purity titanium have high strength and hardness, as well as good corrosion resistance, and can withstand greater pressure and weight. When testing solid materials containing acidic or alkaline substances, the base can avoid corrosion. At the same time, high-purity titanium has very high purity and extremely low impurity content, which ensures that the high-purity titanium base will not introduce additional impurities during electrochemical performance testing, thereby guaranteeing the accuracy and reliability of the test results.

[0047] Correspondingly, in this embodiment, the base 3 is disc-shaped, and the grooves 30 on the base 3 are arranged in an array, with each groove 30 being circular. The depth of each groove 30 is less than or equal to 1 mm, and the diameter of each groove 30 is less than or equal to 3 mm, matching the size of the probe 4. Each groove 30 can hold 10-100 mg of powder or slurry sample. The diameter of the groove 30 being less than 3 mm and matching the size of the probe 4 ensures that the probe 4 can accurately align with the sample in the groove 30 during measurement. This allows the measuring electrode to precisely contact a specific position on the sample, reducing measurement errors caused by positional deviations. Simultaneously, when the probe 4 and the groove 30 are matched in size, the probe 4 can stably contact the sample during pressurization. Furthermore, the depth of the groove 30 being less than 1 mm restricts the vertical movement of the sample, making the contact between the probe 4 and the sample more stable and reliable.

[0048] Furthermore, for solid film and powder samples, the sample size is often small. Designing grooves 30 with smaller diameters and depths better accommodates these small samples, avoiding material waste and facilitating handling and measurement. Multiple grooves 30 with smaller diameters and depths can be densely arranged on the base 3 to achieve high-throughput testing. This allows for simultaneous measurement of multiple samples in a single test, significantly improving testing efficiency.

[0049] Furthermore, in some specific embodiments, the probe 4 is fixed in position relative to the hydraulic device 1, while the worktable 10 can move up and down. The specific implementation method is as follows:

[0050] The hydraulic device 1 has a lifting mechanism 11 at the bottom of the worktable 10. The lifting mechanism 11 is connected to the worktable 10 to drive the worktable 10 to move up and down, that is, to move up and down along the Z-axis. At the same time, it applies pressure to the worktable 10, maintains it, and releases it.

[0051] Fixing the probe 4 relative to the hydraulic device, allowing only the worktable 10 to move, reduces vibration and shaking of the entire measurement system during operation. Because the probe 4 is fixed, its position will not change due to the movement of the hydraulic press, thus ensuring the relative stability of the measurement point. Simultaneously, fixing the probe 4 reduces the possibility of it being struck or damaged during movement. Since the probe 4 does not participate in movement, it will not accidentally collide with other components during equipment operation, thereby extending the service life of the probe 4.

[0052] It should be noted that the specific structure of the lifting mechanism 11 is not limited in this utility model. As long as it can drive the worktable 10, it is within the protection scope of this utility model.

[0053] Furthermore, in some specific embodiments, the specific structural design of the XY two-dimensional displacement stage 2 is given, and the specific design scheme is as follows:

[0054] The XY two-dimensional displacement stage 2 includes an X-axis moving module 20 mounted on the worktable 10 and a Y-axis moving module 21 mounted on the X-axis moving module 20. The base 3 is fixedly mounted on the Y-axis moving module 21. Dividing the displacement stage into the X-axis moving module 20 and the Y-axis moving module 21 allows for independent control of the base's movement in both the X and Y directions. This enables the operator to precisely adjust the position of the base 3, ensuring that the probe 4 is accurately aligned with the groove 30 on the base 3 and the sample, thus improving measurement accuracy.

[0055] It should be noted that the specific structure of the X-axis moving module 20 and the Y-axis moving module 21 in this utility model is not limited. They can be either ball screw linear modules or synchronous belt linear modules, etc. Using a ball screw linear module provides high precision and enables accurate linear positioning; using a synchronous belt linear module offers good transmission stability and lower cost. Specifically, those skilled in the art can design and choose according to actual conditions, and all such choices fall within the protection scope of this utility model.

[0056] Application examples of this high-throughput solid electrolyte ionic conductivity testing device include, for instance, the liquid-phase synthesis and ionic conductivity measurement of sulfide solid electrolytes. The specific steps are as follows:

[0057] 1) Parallel reactions of sulfide electrolytes and preparation of sample arrays were carried out using a high-throughput liquid-phase synthesis + direct writing device;

[0058] 2) Place the base 3 with arrayed grooves 30 on the XY two-dimensional displacement stage 2.

[0059] 3) Connect probe 4 and base 3 to the electrochemical workstation respectively.

[0060] 4) Move the XY two-dimensional displacement stage 2 and align the probe 4 with the channel to be measured; start the hydraulic device 1 to drive the base 3 to move upward and contact the probe 4, and apply pressure until the set pressure is reached (the set pressure in this embodiment is 116 kg).

[0061] 5) Perform electrochemical impedance spectroscopy on the sample and obtain the impedance value R1.

[0062] 6) Depressurize and move base 3 downwards to complete the measurement of a single channel.

[0063] 7) Repeat steps 4) to 6) to complete the measurement for each channel and obtain the corresponding impedance values ​​for each of the remaining channels: R2, R3, ..., R 16 .

[0064] 8) Obtain the film thickness values ​​for each channel using a thickness gauge or laser rangefinder: l1, l2, l3, ..., l 16 .

[0065] 9) Calculate the ionic conductivity value for each channel using the ionic conductivity formula: σ1, σ2, ..., σ 16 .

[0066] Formula for calculating ionic conductivity:

[0067] l represents the film thickness; R represents the impedance; and d represents the groove diameter.

[0068] 10) Draw the material gene phase diagram using the measured ionic conductivity.

[0069] The present invention has been further described above with reference to specific embodiments. However, it should be understood that the specific description herein should not be construed as limiting the substance and scope of the present invention. Various modifications made by those skilled in the art to the above embodiments after reading this specification are all within the scope of protection of the present invention.

Claims

1. A high-throughput solid electrolyte ionic conductivity testing device, characterized in that: include: Hydraulic devices; An XY two-dimensional displacement stage is mounted on the worktable of the hydraulic device. A base is mounted on the XY two-dimensional displacement stage and is driven by the XY two-dimensional displacement stage to move along the XY direction; the base has multiple grooves for holding samples. A probe is mounted on top of the hydraulic device and positioned above the base; the probe and the base are respectively used to connect to an electrochemical workstation.

2. The high-throughput solid electrolyte ionic conductivity testing device according to claim 1, characterized in that: An insulating sleeve is fitted over the probe.

3. The high-throughput solid electrolyte ionic conductivity testing device according to claim 2, characterized in that: The insulating sleeve is made of PEEK plastic.

4. The high-throughput solid electrolyte ionic conductivity testing device according to claim 2, characterized in that: The bottom of the insulating sleeve is shaped like an inverted frustum.

5. The high-throughput solid electrolyte ionic conductivity testing device according to claim 2, characterized in that: The probe is made of stainless steel or high-purity titanium, and the diameter of the probe is less than or equal to 3 mm.

6. The high-throughput solid electrolyte ionic conductivity testing device according to claim 1, characterized in that: The base is made of stainless steel or high-purity titanium.

7. The high-throughput solid electrolyte ionic conductivity testing device according to claim 1, characterized in that: The grooves on the base are arranged in an array, and the grooves are circular.

8. The high-throughput solid electrolyte ionic conductivity testing device according to claim 7, characterized in that: The depth of the groove is less than or equal to 1 mm, and the diameter of the groove is less than or equal to 3 mm; the diameter of the probe is less than or equal to 3 mm.

9. The high-throughput solid electrolyte ionic conductivity testing device according to claim 1, characterized in that: The hydraulic device has a lifting mechanism at the bottom of the worktable, which is connected to the worktable to drive the worktable to move up and down.

10. The high-throughput solid electrolyte ionic conductivity testing device according to claim 1, characterized in that: The XY two-dimensional displacement stage includes an X-axis moving module mounted on the worktable and a Y-axis moving module mounted on the X-axis moving module, with the base fixedly mounted on the Y-axis moving module.

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