CN108051487B - A platform device for testing electrical properties of multifunctional solid oxides - Google Patents

Abstract

The invention discloses a platform device for testing the electrical characteristics of a multifunctional solid oxide, comprising a heating unit, a support platform, an external box, a test base, a sample support component, a protective sleeve and test accessories; the heating unit is fixedly installed on the support platform , there is an external box connected to the bottom of the test base, and the external box is equipped with several electrodes and thermocouple interfaces connected with external test equipment, as well as internal and external air inlet interfaces and internal and external air outlet interfaces for testing atmosphere control; sample support components, protective sleeves One end of the test fitting and the test fitting are respectively sealed and connected to the corresponding interface of the test base, and the test fitting and the sample support assembly are located in the protective casing; the other end of the protective casing, the test fitting, and the sample support assembly for placing the test sample is located in the heating unit. The invention has the advantages of simple operation, low cost, small occupied space, stable and reliable operation, can perform multiple function tests on samples, has good versatility, can greatly save test time and improve test efficiency.

Description

A platform device for testing electrical properties of multifunctional solid oxides

technical field

The invention relates to the technical field of equipment for testing material properties, in particular to a platform device for testing the electrical characteristics of a multifunctional solid oxide.

Background technique

At present, the research on solid oxide materials at home and abroad mainly focuses on testing its conductivity and AC impedance characteristics, ion or electron transfer number of solid oxide electrolyte materials, Seebeck coefficient (Seebeck effect) of solid materials, and oxygen permeability of solid oxides. Oxygen permeability test of membrane, charge and discharge performance test of solid oxide fuel cell single cell, and electrolysis experiment of solid oxide electrolytic cell, etc. Basically, it adopts an independent self-made test platform system, which is usually temporarily produced from local materials for the implementation of a specific performance test, or the platform produced by it can only provide a very small number of functional test purposes, and the function is single. Not well promoted and applied.

The reasons are as follows: 1. When the purpose or method of the experiment is changed, this kind of self-made platform device often involves the modification and reconstruction of the device platform, which is time-consuming and laborious, which is not conducive to the development of normal experiments and reduces the efficiency of scientific research; 2. Such self-made platform devices can usually only achieve a single performance test, that is, different performance tests of the same material need to use different platform systems, which can easily cause certain resources to be idle. 3. The test platform devices built by different researchers usually have different shapes and structures due to their different ideas, and there are also differences in the level of test environment control. It is easy to cause problems when testing the same performance of the same material under the same conditions The difference in data cannot provide experimental results based on the same reference standard, and even draw diametrically opposite conclusions.

At present, there is no test platform with independent intellectual property rights in China that integrates various basic solid oxide electrical and electrochemical performance test environments. Although a few platform devices with similar functions have entered the market abroad, their prices are high.

Contents of the invention

The purpose of the present invention is to overcome the deficiencies of the prior art, to provide a platform device for testing the electrical properties of a multifunctional solid oxide, which can meet the requirements of the above-mentioned testing of the electrical and electrochemical properties of various solid oxides, Improve the efficiency of scientific research, and the cost is low, with strong market competitiveness.

The technical solution of the present invention is: a platform device for testing the electrical characteristics of a multifunctional solid oxide, including a heating unit, a support table, an external box, a test base, a sample support assembly, a protective sleeve and test accessories; the heating unit is fixed Installed on a support platform, an external box is connected to the bottom of the test base, and the external box is provided with a plurality of electrodes and thermocouple interfaces connected to external testing instruments and equipment, and an air inlet interface and an air outlet interface for testing atmosphere control; One end of the sample support assembly, the protective sleeve and the test fitting is respectively sealed and connected to the corresponding interface of the test base, and the test fitting and the sample support assembly are all located in the protective sleeve; the protective sleeve, the test fitting and the sample support The other end of the assembly where the test sample is placed is inside the heating unit.

Further, the heating unit is a vertical tube furnace; further, it is an open vertical tube furnace.

Further, the test base includes a base body and an outer protection sleeve nut; the protection sleeve is sealed and connected to the base body through the outer protection sleeve nut and the sealing coil; the base body is provided with a protective sleeve for connecting The positioning groove of the protective sleeve and the sample support component interface sealed with the sample support component, and at least 2 pairs of air inlet/outlet channels, 3 pairs of thermocouple channels and 4 pairs of electrode channels, and each channel is independent of each other and does not communicate with each other ; The air inlet/outlet passage includes an outer pipe air inlet, an outer pipe air outlet, an inner pipe air inlet and an inner pipe air outlet; the thermocouple passage is equipped with thermocouple pins and lead wires, and the electrode passage is equipped with Electrode pins and leads.

Further, the electrodes and thermocouple interfaces on the external box are correspondingly connected to the thermocouple channels and electrode channels of the test base; the internal and external air inlet interfaces are respectively connected to the air inlets of the outer tube and the air inlets of the inner tube; The inner and outer air outlet ports are respectively connected to the air outlet of the outer pipe and the air outlet of the inner pipe correspondingly.

Further, the test base is also provided with a constant temperature/cooling circulating water inlet, a constant temperature/cooling circulating water outlet and a constant temperature water groove; the cooling water enters the constant temperature water groove through the constant temperature/cooling circulating water inlet, and then flows from the constant temperature/cooling The circulating water is discharged from the outlet to avoid the overheating of the test base from interfering with the experimental test.

Further, the sample support assembly includes a sample support rod, a sample support rod connector, a spring rod, a spring rod fixing pin, a spring and a sample fixing top sheet; the sample support rod and the sample support rod connector are hermetically connected by a sealing coil , the connecting piece of the sample support rod is provided with a spring hook screw, one end of the spring is connected to the spring hook screw, and the other end is connected to the spring pull rod; the test sample is placed on the sample support rod, and the spring pull rod is fixed by the spring pull rod fixing pin and The cooperating action of the sample holding top sheet holds the test sample in place.

Further, the shape of the sample support rod includes a complete cylinder, a cylinder with several notched grooves at one end, or a hollow cylinder in the middle, which are selected according to different test purposes.

Further, the test accessories include electrode wires equipped with electrode wire sleeves, electrode wire plugs, thermocouple wires equipped with thermocouple wire sleeves, thermocouple wire plugs, outer air intake pipes, outer air intake pipe adapters, inner Air intake pipe and inner air intake pipe adapter; the electrode lead is connected to the test sample; the electrode wire plug, thermocouple wire plug, outer air intake pipe adapter and inner air intake pipe adapter are respectively connected to the electrode pins in the test base, The thermocouple pin, the air inlet of the outer tube and the air inlet of the inner tube are connected correspondingly.

Further, the external box, the test base and the sample support rod connector are all made of metal materials with good electromagnetic shielding effect; the material of the protective sleeve is made of high-purity corundum or high-purity quartz; the The sample support rod, spring pull rod and spring pull rod fixing pin in the sample support assembly are all made of high-purity corundum; the electrode lead sleeve and thermocouple wire sleeve are made of high-purity corundum; The outer air intake pipe is made of high-purity quartz tube; the inner air intake pipe is made of high-purity corundum or high-purity quartz.

Further, the shape of the test sample includes a disc sample or a columnar sample; the diameter of the disc sample is no more than 25mm, and the length of the columnar sample is no more than 50mm.

The beneficial effects of the present invention are:

1. Integrating various performance tests: the device can be used to test various electrical and electrochemical properties of new energy solid oxide functional materials, which can significantly save equipment investment costs;

2. Multi-sample testing capability: the device provides multiple electrical interfaces, allowing multiple samples to be tested under the same test conditions in one test. Compared with a single-sample test platform, it can greatly save test time and improve test efficiency. ;

3. Small operating space: For experimental environments with compact space or small site area, this device can effectively improve the utilization efficiency of scientific research resources and demonstrate the scientific research strength of scientific research institutions;

4. Functional scalability: This device allows experimental researchers to design and replace the internal sample support frame for other specific test requirements, expand existing test functions, and realize new test technology innovations. It can also be used for non-solid oxide high-temperature materials electrical performance test;

5. At present, the platform devices used in the material performance test corresponding to the functions provided by the device platform in China are of different styles, and are usually temporarily produced by local teachers of various colleges and universities, or the platforms produced by them are often only It provides a very small number of functional testing purposes, and the function is single, which cannot be well promoted and applied in teaching and research. Especially when the experimental purpose or experimental method is changed, it often involves the rebuilding of the device platform, which is time-consuming and laborious. It is conducive to the development of normal experimental teaching, and there are still problems such as the difference in the results of the same test of the same material in different research institutes; the platform device can be used as a basic platform, which can greatly improve the standard uniformity of the test, thereby improving the scientificity of the test results sex.

Description of drawings

Fig. 1 is a schematic structural diagram of a platform device for testing electrical properties of multifunctional solid oxides according to the present invention.

Fig. 2 is a schematic diagram of the connection between the external box, the test base and the protective sleeve.

Figure 3 is a schematic diagram of the enlarged structure of the test base.

Figure 4 is a schematic structural view of the sample support assembly.

Figure 5 is a schematic diagram of sample support rods in different styles.

Fig. 6 is a schematic structural diagram of a test accessory.

Reference numerals: heating unit 101, support platform 201, external box 301, internal and external air inlet interface 311, internal and external air outlet interface 312, electrode and thermocouple interface 313, test base 401, constant temperature/cooling circulating water inlet 411, constant temperature/cooling cycle Water outlet 412, outer pipe air inlet 413, outer pipe air outlet 414, inner pipe air inlet 415, inner pipe air outlet 416, protective sleeve positioning groove 417, outer protective sleeve nut 418, electrode pin 419, thermoelectric Couple pin 420, sample support assembly interface 421, sample support assembly 501, sample support rod 511, sample support rod connector 512, spring pull rod 513, spring pull rod fixing pin 514, spring 515, spring hook screw 516, sample fixing top piece 517, protective sleeve 601, test accessories 701, electrode lead 711, pole line sleeve 712, electrode lead plug 713, thermocouple wire 721, thermocouple line sleeve 722, thermocouple line plug 723, outer air intake pipe 731, outer Air intake pipe adapter 732 , inner air intake pipe 741 , inner air intake pipe adapter 742 , sealing coil 801 .

Detailed ways

The implementation structure of the present invention will be described below in conjunction with the accompanying drawings.

As shown in Figures 1 to 6, the platform device for testing the electrical characteristics of multifunctional solid oxides of the present invention includes a heating unit 101, a support table 201, an external box 301, a test base 401, a sample support assembly 501, and a protective cover Tube 601 and test accessories 701; the heating unit 101 is fixedly installed on the support platform 201, and an external box 301 is connected to the bottom of the test base 401, and the external box 301 is provided with several electrodes connected to external testing instruments and equipment. A thermocouple interface 313 and an air inlet interface 311 and an air outlet interface 312 for controlling the test atmosphere; one end of the sample support assembly 501, the protective sleeve 601 and the test accessory 701 are respectively sealed and connected to the corresponding interface of the test base 401, and the The test accessories 701 and the sample support assembly 501 are located in the protective sleeve 601 ;

The external testing instruments and equipment are special testing instruments for electrical and electrochemical performance testing, including digital multimeters, potentiostats/current meters, electronic loads, oxygen analyzers, or electrochemical workstations.

Further, the heating unit 101 is a vertical tube furnace, preferably an open vertical tube furnace; the design of the open vertical tube furnace can eliminate the influence of the magnetoelectric effect produced by the coiled heating wire on the electrical and mechanical properties of the sample as much as possible. influence on electrochemical performance.

Further, the test base 401 includes a base body and an outer protection sleeve nut 418; the protection sleeve 601 is sealed and connected to the base body through the outer protection sleeve nut 418 and the sealing coil 801; The protective sleeve positioning groove 417 that is connected with the protective sleeve 601 and the sample support assembly interface 421 that is sealingly connected with the sample support assembly 501 are also provided with at least 2 pairs of air inlet/outlet channels, 3 pairs of thermocouple channels and 4 pairs of electrode channels, It can meet the test requirements for the existing performance of the test sample, and each channel is independent of each other and does not communicate with each other; the air inlet/outlet channel includes an outer tube air inlet 413, an outer tube air outlet 414, an inner tube air inlet 415 and an inner pipe air inlet. Tube air outlet 416; the thermocouple channel is equipped with a thermocouple pin 419 and a lead wire, and the electrode channel is equipped with an electrode pin 420 and a lead wire.

Further, the electrodes and the thermocouple interface 313 on the external box 301 are connected to the thermocouple channel and the electrode channel of the test base 401; The air inlet 415 of the inner pipe corresponds to a sealed connection; the inner and outer air outlets 312 are respectively connected to the air outlet 414 of the outer pipe and the air outlet 416 of the inner pipe through quick-twist joints; this type of air circuit connection can provide sufficiently small air leakage The rate can meet the airtightness requirements of the platform device.

Further, the test base 401 is also provided with a constant temperature/cooling circulating water inlet 411, a constant temperature/cooling circulating water outlet 412 and a constant temperature water groove; the cooling water enters the constant temperature water groove through the constant temperature/cooling circulating water inlet 411, and then It is discharged from the constant temperature/cooling circulating water outlet 412 to prevent the overheating of the test base 401 from interfering with the experimental test.

Further, the sample support assembly 501 includes a sample support rod 511, a sample support rod connector 512, a spring pull rod 513, a spring pull rod fixing pin 514, a spring 515 and a sample fixing top sheet 517; the sample support rod 511 and the sample support The rod connector 512 is sealed and connected through the sealing coil 801. The sample support rod connector 512 is provided with a spring hook screw 516. One end of the spring 515 is connected to the spring hook screw 516, and the other end is connected to the spring pull rod 513; the sample support rod Place the test sample on 511, and the spring pull rod 513 fixes the test sample through the cooperation of the spring pull rod fixing pin 514 and the sample fixing top sheet 517.

The sealing coil 801 mentioned above is made of rubber sealing ring with high temperature resistance, oxidation resistance and chemical corrosion resistance, such as silicon rubber, fluorine rubber, ethylene propylene rubber, etc.; the purpose of sealing the connection with the sealing coil 801 is to ensure the test process The airtightness of the inner and outer sides makes the test effect more accurate; in this embodiment, the O-shaped sealing coil made of fluororubber is preferably used, which can operate well for a long time within the experimental operation range, and it is easy to operate even if it needs to be replaced, and the cost is low. low.

Further, the shape of the sample support rod 511 includes a complete cylinder, a cylinder with several notched grooves at one end, or a hollow cylinder in the middle, which can be selected according to different test purposes.

Further, the test accessory 701 includes an electrode wire 711 equipped with an electrode wire sleeve 712, an electrode wire plug 713, a thermocouple wire 721 equipped with a thermocouple wire sleeve 722, a thermocouple wire plug 723, and an outer air intake pipe 731 , the outside air intake pipe adapter 732, the inside air intake pipe 741 and the inside air intake pipe adapter 742; the electrode wires 711 are respectively connected to the test sample; the electrode wire plug 713, the thermocouple wire plug 723, the outside air intake pipe adapter 732 and the inner air inlet pipe adapter 742 are respectively connected with the electrode pin 420 in the test base 401, the thermocouple pin 419, the outer pipe air inlet 413 and the inner pipe air inlet 415; wherein, the thermocouple wire 721 and The thermocouple composed of the thermocouple wire plug 723 is preferably an S-type thermocouple, and the S-type thermocouple is suitable for accurate temperature measurement in different non-reducing atmospheres; the electrode wire 711 is made of an inert conductive material, including platinum , gold or silver metal, the user can choose other inert metals as the electrode wire according to the actual use temperature and atmosphere requirements; this embodiment uses platinum metal as the electrode wire, which can maintain high signal stability, minimize the measurement error, and achieve measurement The results are highly accurate. .

Further, the external box 301, the test base 401 and the sample support rod connector 512 are all made of a metal material with good electromagnetic shielding effect, preferably 316L stainless steel; the material of the protective sleeve 601 is high-purity corundum or Made of high-purity quartz; the sample support rod 511, spring pull rod 513 and spring pull rod fixing pin 514 in the sample support assembly 501 are made of high-purity corundum material; the electrode lead sleeve electrode lead sleeve 712 and thermocouple The line sleeve 722 is made of high-purity corundum; the outer air intake pipe 731 is made of high-purity quartz; the inner air intake 741 is made of high-purity corundum or high-purity quartz. During the performance test, the heating unit 101 is heated, and the heat will be transferred. The selected metal material should not be easily oxidized to ensure that the atmospheric conditions in the test space will not be affected. Considering the price factor, 316L stainless steel is the preferred material. ; High-purity corundum or high-purity quartz can withstand high temperature and corrosion resistance.

Further, the shape of the test sample includes a disc sample or a columnar sample; the diameter of the disc sample is no more than 25mm, and the length of the columnar sample is no more than 50mm; in addition, other shapes or specifications can be appropriately used according to actual conditions. sample.

The present invention is used for the multifunctional solid oxide electrical characteristic testing platform device, comprises the following steps: the prepared test sample is installed on the sample support rod 511 in the sample support assembly 501, and the spring pull rod 513 passes the spring pull rod fixing pin 514 Cooperate with the sample fixing top sheet 517 to fix the test sample; correctly connect the electrode wires and thermocouple wires in the test fitting 701 to the corresponding wire pins of the test base 401; correctly connect the inner air intake pipe 741 in the test fitting 701 Connect the outer air intake pipe 731 to the corresponding air intake hole of the test base 401; correctly connect the sample support assembly 501 and the protective sleeve 601 to the corresponding interface of the test base 401; connect the electrodes of the external box 301 to the thermocouple interface 313 External test equipment, the air inlet port 311 is connected to the gas source supply system for atmosphere control, which can be equipped according to the flow and humidity requirements; the gas used for the test is from a gas source, such as a gas cylinder, through a pressure reducing valve, a flow meter, etc. The inner pipe air inlet 415 enters the inner air inlet pipe 741, or enters the outer air inlet pipe 731 through the outer pipe air inlet 413; when ready, turn on the power supply of the open-type vertical tube furnace, and heat up according to a certain heating program until the temperature reaches After testing the temperature, perform the performance test on the test sample.

If the external test equipment is an electrochemical workstation, the conductivity properties of the solid oxide material, the surface oxygen exchange reaction and the transfer properties of oxygen diffusion inside the dense material can be obtained according to the measured AC impedance spectrum; it can be realized in the solid oxide The separation of electrolyte resistance and electrode resistance during fuel cell discharge can be used to study the effect of electrolyte or electrode material on battery performance. In addition, different testing instruments and equipment can be connected according to the actual situation to test the conductivity and AC impedance characteristics of solid oxides, the ion or electron transfer number of solid oxide electrolyte materials, the Seebeck coefficient and Seebeck effect of solid materials, solid Oxygen transmission rate of oxide oxygen permeable membrane, charge and discharge performance of solid oxide fuel cell, electrolysis performance of solid oxide electrolytic cell, etc.

The above is only a specific implementation of the present invention, but the scope of protection of the present invention is not limited thereto, and any changes or simple replacements that do not go through creative work should be covered within the scope of protection of the present invention.

Claims (5)

1. A platform device for testing the electrical characteristics of a multifunctional solid oxide, characterized in that it includes a heating unit (101), a support table (201), an external box (301), a test base (401), and a sample support assembly (501 ), protective sleeve (601) and test accessories (701); the heating unit (101) is fixedly installed on the support platform (201), and an external box (301) is connected under the test base (401), the The external box (301) is provided with several electrodes and thermocouple interfaces (313) connected to external testing instruments and equipment, internal and external air inlet interfaces (311) and internal and external air outlet interfaces (312) for testing atmosphere control; the sample supports One end of the component (501), the protective sleeve (601) and the test fitting (701) is respectively sealed and connected to the corresponding interface of the test base (401), and the test fitting (701) and the sample support component (501) are located in the protective Inside the sleeve (601); the other end of the protective sleeve (601), the test fitting (701) and the sample support assembly (501) where the test sample is placed is located in the heating unit (101), and the test base (401) It includes a base body and an outer protection sleeve nut (418); the protection sleeve (601) is sealed and connected to the base body through an outer protection sleeve nut (418) and a sealing coil (801); the base body is provided with a The protective sleeve positioning groove (417) connected with the protective sleeve (601) and the sample support assembly interface (421) sealingly connected with the sample support assembly (501) are also equipped with at least 2 pairs of air inlet/outlet channels, 3 pairs of thermoelectric Dual channels and 4 pairs of electrode channels, and each channel is independent of each other and does not communicate with each other; the air inlet/outlet channels include outer tube air inlet (413), outer tube air outlet (414), inner tube air inlet (415) and the inner tube air outlet (416); the thermocouple channel is equipped with thermocouple pins (419) and lead wires, the electrode channel is equipped with electrode pins (420) and lead wires, and the external box (301) The electrode and thermocouple interface (313) are connected to the thermocouple channel and electrode channel of the test base (401); 415) are connected correspondingly; the internal and external air outlet ports (312) are respectively connected with the outer pipe air outlet (414) and the inner pipe air outlet (416), and the test base (401) is also provided with a constant temperature/cooling circulating water inlet ( 411), constant temperature/cooling circulating water outlet (412) and constant temperature water groove; the cooling water enters the constant temperature water groove through the constant temperature/cooling circulating water inlet (411), and then is discharged from the constant temperature/cooling circulating water outlet (412), To prevent the overheating of the test base (401) from interfering with the experimental test, the sample support assembly (501) includes a sample support rod (511), a sample support rod connector (512), a spring pull rod (513), a spring pull rod fixing pin ( 514), spring (51 5) and the sample fixing top sheet (517); the sample support rod (511) and the sample support rod connector (512) are sealed and connected through the sealing coil (801), and the sample support rod connector (512) is provided with Spring hook screw (516), one end of the spring (515) is connected to the spring hook screw (516), and the other end is connected to the spring pull rod (513); the test sample is placed on the sample support rod (511), and the spring pull rod (513 ) to fix the test sample through the cooperation of the spring pull rod fixing pin (514) and the sample fixing top piece (517), the test accessory (701) includes the electrode lead (711) equipped with the electrode lead sleeve (712), Electrode lead plug (713), thermocouple wire with thermocouple sleeve (722) (721), thermocouple wire plug (723), outer air inlet tube (731), outer air inlet tube adapter (732), inner The air intake pipe (741) and the inner air intake pipe adapter (742); the electrode wire (711) is connected to the test sample; the electrode wire plug (713), the thermocouple wire plug (723), the outer air intake pipe adapter ( 732) and the inner air inlet pipe adapter (742) are respectively connected with the electrode pin (420), thermocouple pin (419), outer pipe air inlet (413) and inner pipe air inlet ( 415) corresponds to the connection. 2. The multifunctional platform device for testing electrical properties of solid oxides according to claim 1, characterized in that: the heating unit (101) is a vertical tube furnace. 3. The platform device for testing the electrical properties of multifunctional solid oxides according to claim 1, characterized in that: the shape of the sample support rod (511) includes a complete cylinder and a cylinder with several notched grooves at one end Or a hollow cylinder in the middle. 4. The platform device for testing the electrical characteristics of multifunctional solid oxides according to claim 1, characterized in that: the external box (301), the test base (401) and the sample support rod connector (512) are all made of Made of metal material with good electromagnetic shielding effect; the protective sleeve (601) is made of high-purity corundum or high-purity quartz; the sample support rod (511) and spring pull rod in the sample support assembly (501) (513) and spring rod fixing pin (514) are made of high-purity corundum; the electrode wire sleeve (712) and thermocouple wire sleeve (722) are made of high-purity corundum; The trachea (731) is made of high-purity quartz tube; the inner air intake pipe (741) is made of high-purity corundum or high-purity quartz. 5. The platform device for testing the electrical characteristics of multifunctional solid oxides according to claim 1, wherein the shape of the test sample includes a disc sample or a columnar sample; the diameter of the disc sample is no more than 25mm, and the The length of the columnar sample shall not exceed 50mm.