Multi-channel closed high-temperature solid electrolyte conductivity in-situ test fixture

Abstract

The invention provides a multi-channel closed high-temperature solid electrolyte conductivity in-situ test fixture, which comprises a base, a plurality of groups of pre-tightening sliding connecting rods and a circuit module, the base comprises a metal supporting assembly, a plurality of preformed holes are formed in the metal supporting assembly, a plurality of spring hole positions are reserved in the front surface of the base, and the pre-tightening sliding connecting rods are connected with the circuit module. The pre-tightening sliding connecting rod comprises a sliding rod, a positioning pipe and a spring component; the positioning pipe is fixed on the base through a spring hole site and a pre-tightening bolt on the base, the spring is arranged at the bottom end in the positioning pipe, one end of the sliding rod is arranged on the spring, and the other end of the sliding rod abuts against the top end of the positioning pipe; the circuit module comprises a current collector, an electrode wire and a change-over plug, and the electrode wire is connected with the current collector and is led out from the preformed hole of the base along the fixing pipe. Modularized component design enables installation to be simple and convenient, self-supporting of the spring is used for replacing manual pressure adjustment, and the problem that a sample is in poor contact with the surface of an electrode in a high-temperature environment is solved.

Description

Technical Field

[0001] The present application relates to the technical field of conductivity testing, and in particular to a multi-channel closed high-temperature solid electrolyte conductivity in-situ testing fixture. Background Art

[0002] Ionic conductivity is one of the key indicators for measuring the conductive properties of materials, especially for materials that work in high temperature environments and specific atmospheres (such as fuel cell electrolytes and solid-state battery electrolytes). Highly conductive materials help improve the electrochemical performance of devices and can be widely used in the development of fuel cells, solid-state batteries, gas sensors, and catalytic materials. Therefore, ionic conductivity testing can be used to screen out materials with more application prospects.

[0003] The need to test ionic conductivity at high temperatures has led to the development of a variety of testing schemes. Currently, the commonly used testing devices are mostly single-channel testing systems. This type of device obtains ionic conductivity data by testing a single sample one by one. Figure 1 As shown: The sample to be tested is fixed by the upper and lower pressure plates, and the whole set of fixtures only provides one test channel ( Figure 1 ). At the same time, the square design is not convenient for sealing the sample test environment and cannot isolate the external air, so it is not possible to conduct gas atmosphere test experiments.

[0004] Another high temperature conductivity test fixture such as Figure 2 As shown, the platinum sheet, the solid electrolyte sheet, and the platinum sheet are stacked in order on the contact surfaces of the first fixture part 1 and the second fixture part 2 whose contact surfaces completely overlap, and are aligned, and pressure sensors are installed between the first fixture part 1 and the solid electrolyte sheet and between the second fixture part 2 and the solid electrolyte sheet. The technician reads the pressure value displayed on the pressure gauge and adjusts the relative position of the first fixture part 1 and the second fixture part 2 according to the displayed pressure value, that is, adjusts the tightening position of the nut 6 on the bolt 5, so that the pressure value displayed on the pressure gauge is within the preset threshold range, so as to avoid excessive pressure applied by the fixture to damage the solid electrolyte 3. Figure 2 In the figure, numeral 4 denotes a blocking electrode element, 7 denotes an insulating sleeve, and 8 denotes a wire.

[0005] Combination Figure 1 and Figure 2It can be seen that because there is only one effective test channel for the sample, it is impossible to test multiple samples in parallel under the same conditions, so the detection efficiency is low, and it is difficult to monitor multiple samples simultaneously under the same high temperature environment, resulting in a lack of consistency in data under different test conditions. Secondly, since the shape of the fixture is not suitable for testing in a closed environment, it cannot effectively protect air-sensitive samples, so the use scenarios of this type of fixture are greatly limited. In addition, the fixture components are not modularly designed, and the installation steps are very complicated and highly correlated, such as Figure 2 As shown, the nuts on the four angles need to be fixed on the same horizontal plane to provide an effective electrode contact surface, which is not easy to operate in practice. Summary of the invention

[0006] In view of this, the present application provides a multi-channel closed high-temperature solid electrolyte conductivity in-situ testing fixture to meet the needs of synchronous monitoring of multiple samples under high temperature conditions.

[0007] To achieve the above purpose, the technical solution adopted in this application is as follows: A multi-channel closed high-temperature solid electrolyte conductivity in-situ test fixture, comprising a base, multiple groups of pre-tightened sliding connecting rods and a circuit module, the base comprising a metal support component, the metal support component having a plurality of first reserved holes and a plurality of second reserved holes, a plurality of spring holes are reserved on the front of the base, the pre-tightened sliding connecting rod comprises a sliding rod, a positioning tube and a plurality of spring components, the plurality of spring components are respectively located in the plurality of spring holes; the positioning tube is fixed to the base through the spring holes on the front of the base and the pre-tightening bolts, the positioning tube is central The circuit module comprises a hollow structure, wherein the spring is placed at the bottom end of the positioning tube, one end of the sliding rod is placed on the spring, and the other end is against the top end of the positioning tube; a notch is provided on the positioning tube for adjusting the sliding rod and placing the sample; the circuit module comprises a current collector, an electrode wire and a conversion plug, the current collector is placed between the top end of the sliding rod and the top end of the positioning tube, and is used to connect the upper and lower electrodes of the sample to be tested; the electrode wire is connected to the current collector, and is led out from the reserved hole of the base along the fixing tube, and is connected to the external conversion plug; the current collector and the electrode wire are fixed to the positioning tube by a metal wire.

[0008] Furthermore, the conductivity in-situ test fixture also includes a temperature testing module, which includes a thermocouple probe and a thermocouple meter. The thermocouple probe and the thermocouple meter are connected by a wire, and the thermocouple probe is placed near the sample to be tested. The metal support component is provided with a thermocouple assembly hole, and the thermocouple probe is fixed through the thermocouple assembly hole. The wire of the thermocouple probe is led out of the area to be tested through a reserved hole and connected to the thermocouple meter.

[0009] Furthermore, the conductivity in-situ test fixture also includes an air inlet pipe and a gas protection shell. The metal support assembly is also provided with an air inlet hole and an exhaust hole. The gas protection shell is sleeved on the outside of the multiple groups of pre-tightened sliding connecting rods. The gas protection shell and the base are sealed by a flange and a sealing ring.

[0010] Furthermore, the positioning tube and the sliding rod are made of ceramic material.

[0011] Furthermore, the sliding rod is designed with a plurality of grooves to facilitate adjustment of its overall height, thereby fixing the sample to be tested.

[0012] Furthermore, the circuit module also includes a hollow ceramic tube, and the electrode wire is placed in the hollow ceramic tube to isolate electromagnetic effects.

[0013] Furthermore, the sample to be tested includes a solid electrolyte in the form of a thin film or a block.

[0014] Furthermore, the thermocouple probe is inserted into the thermocouple assembly hole and sealed by high temperature glue.

[0015] Furthermore, the air inlet pipe is connected to the metal support assembly through the air inlet hole, and the length of the air inlet pipe is such that the end of the pipe is close to the sample testing position.

[0016] Compared with the prior art, the beneficial effects of this application are: 1. By assembling multiple sets of sliding rod modules on the metal base, each set of rod modules provides a sample test slot, thereby achieving simultaneous measurement of multiple samples, greatly improving data collection efficiency, and being able to test multiple samples at the same time, reducing testing costs and shortening time; 2. The circuit connection of this application is simple. Each test slot has only two electrode wires connected to the outside. It can be used with a multi-channel electrochemical workstation or impedance meter to achieve simple and fast multi-sample testing; 3. The modular component design makes installation easy, and uses the self-support of the spring instead of manual pressure adjustment to overcome the problem of poor contact between the sample and the electrode surface in a high temperature environment. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for use in the embodiments will be briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present application and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without paying creative work.

[0018] Figure 1 It is a structural diagram of a ceramic conductivity testing device in the prior art; Figure 2 It is a structural diagram of a solid electrolyte ion conductivity test fixture in the prior art; Figure 3 is a top view of the base of the present application; Figure 4 It is a structural diagram of the sliding rod of the present application; Figure 5 It is a structural diagram of the positioning tube of this application; Figure 6 This is the front view of the base and the spring structure of this application; Figure 7 This is a top view of the base and reserved spring holes for this application; Figure 8 This is the assembly effect diagram of the conductivity test fixture for this application. DETAILED DESCRIPTION

[0019] In order to make the purpose, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below in combination with the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments.

[0020] like Figure 3-7 As shown, a multi-channel closed high-temperature solid electrolyte conductivity in-situ test fixture includes a base, multiple groups of pre-tightened sliding connecting rods and circuit modules, the base includes a metal support component 9, the metal support component 9 is provided with multiple first reserved holes 15 and multiple second reserved holes 13, the front of the base is provided with multiple spring holes, the pre-tightened sliding connecting rod includes a sliding rod, a positioning tube and multiple spring components, the multiple spring components are respectively located in the multiple spring holes; the positioning tube is fixed to the base through the spring holes and pre-tightening bolts 14 on the front of the base, the positioning tube is a hollow structure, the spring is placed at the bottom end of the positioning tube, one end of the sliding rod is placed on the spring, and the other end is against the top of the positioning tube; a notch 17 is provided on the positioning tube for adjusting the sliding rod and placing the sample; The circuit module includes a current collector, an electrode wire and a conversion plug. The current collector is placed between the top of the sliding rod and the top of the positioning tube, and is used to connect the upper and lower electrodes of the sample to be tested; the electrode wire is connected to the current collector and is led out from the reserved hole 15 of the base along the fixed tube and connected to the external conversion plug; the current collector and the electrode wire are fixed to the positioning tube by a metal wire.

[0021] The positioning tube can be fixed by adjusting the tightness of the knob 14. The lower part of the positioning tube is placed in the spring hole on the front of the base. After the knob 14 is tightened, the top of the knob will abut against the outer wall of the positioning tube, thereby fixing it in the spring hole.

[0022] The base can be a metal base for supporting the entire fixture. The material of the metal base is one or more alloys of stainless steel, copper, aluminum, etc.

[0023] As an optional embodiment, the base is divided into two parts, the upper part is cylindrical with several openings inside, and the lower part is a supporting component, and the two parts are connected by screws and threaded holes.

[0024] The sliding rod and the positioning tube are matched to form a sample test slot. Multiple test slots can be used simultaneously in the fixture to perform synchronous testing of multiple samples.

[0025] One end of the sliding rod is connected to a spring, and the spring is connected to a metal base. The sliding rod fixes the sample between the top end of the sliding rod and the top end of the inner side of the positioning tube under stress by relying on the elasticity of the spring.

[0026] The second reserved hole 13 is used for passing the hollow ceramic shielding tube with the electrode wire.

[0027] The first reserved hole 15 is used to provide a channel connected to an external detection device.

[0028] The current collector and the electrode wire are both made of metal, such as one or more of platinum, gold, nickel, etc.

[0029] The samples to be tested include but are not limited to thin films, blocks and other solid electrolytes or ceramic materials.

[0030] The present application provides a multi-channel (number of channels ≥ 3) sealed high-temperature conductivity test fixture, which improves the sample testing efficiency through the multi-channel design. In addition, the modular component design makes installation easy, and the self-support of the spring is used instead of manual pressure adjustment to overcome the problem of poor contact between the sample and the electrode surface in a high temperature environment.

[0031] As a further embodiment, the conductivity in-situ test fixture also includes a temperature testing module, which includes a thermocouple probe and a thermocouple meter. The thermocouple probe and the thermocouple meter are connected by a wire, and the thermocouple probe is placed near the sample to be tested. The metal support component 9 is provided with a thermocouple assembly hole 12, and the thermocouple probe is fixed through the thermocouple assembly hole 12. The wire of the thermocouple probe is led out of the area to be tested through the reserved hole 15 and connected to the thermocouple meter.

[0032] As a further embodiment, Figure 8 As shown, the conductivity in-situ test fixture also includes an air inlet pipe and a gas protection shell. The metal support component 9 is also provided with an air inlet hole 10 and an exhaust hole 11. The gas protection shell is sleeved on the outside of the multiple groups of pre-tightened sliding connecting rods. The gas protection shell and the base are sealed by a flange and a sealing ring.

[0033] The base is connected to the gas protection cover, and the interface is sealed by a flange and a sealing ring to form a gas isolation environment.

[0034] This application introduces components such as a gas protection cover and a gas passage to provide different atmosphere conditions for the sample in a high-temperature test environment, which is conducive to a comprehensive evaluation of the high-temperature stability of the sample.

[0035] As a further embodiment, the positioning tube and the sliding rod are made of ceramic material.

[0036] As a further embodiment, Figure 4 As shown, the sliding rod is designed with a plurality of grooves 16 to facilitate adjustment of its overall height, thereby fixing the sample to be tested.

[0037] The sliding rod can be manually pressed down by pressing the groove 16 on the sliding rod with a finger. Since a spring is installed under the sliding rod, the sample can be clamped and fixed by utilizing its elastic force.

[0038] As a further embodiment, the circuit module further includes a hollow ceramic tube, and the electrode wire is placed in the hollow ceramic tube to isolate electromagnetic effects.

[0039] As a further embodiment, the thermocouple probe is inserted into the thermocouple assembly hole 12 and sealed by high temperature glue.

[0040] As a further embodiment, the air inlet pipe is connected to the metal support assembly 9 through the air inlet hole 10, and the length of the air inlet pipe is such that the end of the pipe is close to the sample testing position.

[0041] This application follows these steps when installed: 1. Place the base with the front side facing up on a horizontal surface, and place multiple springs in the reserved spring holes on the front side of the base. Figure 6 As shown, the sliding rod is then installed into the positioning tube, the spring is inserted into the positioning tube and placed under the sliding rod, and finally the positioning tube is fixed inside the spring hole of the base by tightening the pre-tightening bolts; 2. String the hollow ceramic tube on the electrode wire, connect one end of the electrode wire to the current collector, fix the current collector and the electrode wire on the positioning tube through the metal wire, separate the positive and negative electrodes, and lead the electrode wire through the reserved hole of the metal base; 3. Screw the air inlet pipe into the reserved air inlet hole on the metal base and secure it; 4. Insert the thermocouple probe into the metal base and seal it with high temperature glue; 5. Put on the gas protection cover and seal it with flange and sealing ring; 6. Complete the assembly effect Figure 8 .

[0042] Sample testing method: During the test, you only need to unscrew the flange, open the gas protection cover, load multiple samples into the test position, and connect the electrode wire conversion plug to external equipment such as AC impedance meter to conduct the conductivity test. If high temperature testing is required, the fixture can be inserted into a tube furnace for heating, the actual sample temperature can be read through a K-type thermocouple and a thermocouple meter, the heating power can be adjusted until the preset temperature is reached, and then the test can be carried out; If gas control is required, the gas protective cover must be put back, sealed through the flange, and then a ventilation test experiment must be carried out.

[0043] This application solves the problems of single channel, single sample environment, weak electromagnetic shielding and complex assembly of traditional conductivity test fixtures; by assembling multiple sets of sliding connecting rod modules on a metal base, each set of connecting rod modules provides a sample test slot, thereby realizing simultaneous measurement of multiple samples, greatly improving data acquisition efficiency, and being able to test multiple samples at the same time, reducing testing costs and shortening time. At the same time, the gas passage and gas protection cover of this application can ensure the testing of samples in a special gas atmosphere, effectively expanding the use scenarios of the device. Finally, the circuit connection of this application is simple, and each test slot has only two electrode wires connected to the outside, which can be used in conjunction with a multi-channel electrochemical workstation or impedance meter to achieve simple and quick multi-sample testing.

[0044] The above are only specific implementations of the present application, but the protection scope of the present application is not limited thereto. Any technician familiar with the technical field can easily think of changes or substitutions within the technical scope disclosed in the present application, which should be included in the protection scope of the present application. Therefore, the protection scope of the present application should be based on the protection scope of the claims.

Claims

1. A multi-channel closed high-temperature solid electrolyte conductivity in-situ test fixture, characterized in that: The invention comprises a base, a plurality of groups of pre-tightened sliding links and a circuit module, wherein the base comprises a metal support assembly, the metal support assembly is provided with a plurality of first reserved holes and a plurality of second reserved holes, a plurality of spring holes are reserved on the front of the base, the pre-tightened sliding link comprises a sliding rod, a positioning tube and a plurality of spring components, and the plurality of spring components are respectively located in the plurality of spring holes; the positioning tube is fixed to the base through the spring holes and pre-tightened bolts on the base, the positioning tube is a hollow structure, the spring is placed at the bottom end inside the positioning tube, one end of the sliding rod is placed on the spring, and the other end is against the top end of the positioning tube; a notch is provided on the positioning tube for adjusting the sliding rod and placing the sample; the circuit module comprises a current collector, an electrode wire and a conversion plug, the current collector is placed between the top end of the sliding rod and the top end of the positioning tube, and is used to connect the upper and lower electrodes of the sample to be tested; the electrode wire is connected to the current collector, and is led out from the reserved hole of the base along the fixing tube, and is connected to the external conversion plug; the current collector and the electrode wire are fixed to the positioning tube through a metal wire.

2. A multi-channel closed high-temperature solid electrolyte conductivity in-situ test fixture as claimed in claim 1, characterized in that: The conductivity in-situ test fixture also includes a temperature test module, which includes a thermocouple probe and a thermocouple meter. The thermocouple probe and the thermocouple meter are connected by a wire. The thermocouple probe is placed near the sample to be tested. The metal support component is provided with a thermocouple assembly hole. The thermocouple probe is fixed through the thermocouple assembly hole. The wire of the thermocouple probe is led out of the area to be tested through a reserved hole and connected to the thermocouple meter.

3. A multi-channel closed high-temperature solid electrolyte conductivity in-situ test fixture as described in claim 1 or 2, characterized in that: The conductivity in-situ test fixture also includes an air inlet pipe and a gas protection shell. The metal support assembly is also provided with an air inlet hole and an exhaust hole. The gas protection shell is sleeved on the outside of the multiple groups of pre-tightened sliding connecting rods. The gas protection shell and the base are sealed by a flange and a sealing ring.

4. A multi-channel closed high-temperature solid electrolyte conductivity in-situ test fixture as claimed in claim 3, characterized in that: The positioning tube and the sliding rod are made of ceramic material.

5. A multi-channel closed high-temperature solid electrolyte conductivity in-situ test fixture as claimed in claim 4, characterized in that: The sliding rod is designed with a plurality of grooves to facilitate adjustment of its overall height, thereby fixing the sample to be tested.

6. A multi-channel closed high-temperature solid electrolyte conductivity in-situ test fixture as claimed in claim 5, characterized in that: The circuit module also includes a hollow ceramic tube, and the electrode wire is placed in the hollow ceramic tube to isolate electromagnetic effects.

7. A multi-channel closed high-temperature solid electrolyte conductivity in-situ test fixture as claimed in claim 6, characterized in that: The sample to be tested includes a solid electrolyte in a thin film or bulk form.

8. A multi-channel closed high-temperature solid electrolyte conductivity in-situ test fixture as claimed in claim 7, characterized in that: The thermocouple probe is inserted into the thermocouple assembly hole and sealed by high temperature glue.

9. A multi-channel closed high-temperature solid electrolyte conductivity in-situ test fixture as claimed in claim 8, characterized in that: The air inlet pipe is connected to the metal support assembly through the air inlet hole, and the length of the air inlet pipe is such that the end of the pipe is close to the sample testing position.

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