Ultrafast high-temperature sintering system capable of realizing electric-thermal-form in-situ measurement

Abstract

The utility model relates to an ultra-fast high-temperature sintering system capable of realizing electricity-heat-shape in-situ measurement. The ultra-fast high-temperature sintering system comprises a furnace body, a heating device, a detection device and a control device, the heating device comprises a heat preservation crucible, a heating medium and a heating unit; the detection device comprises a deformation detection unit, a resistivity monitoring unit and a temperature control unit; the deformation detection unit comprises a displacement sensor, and a probe of the displacement sensor is in contact with a sample in the heat preservation crucible; the temperature control unit comprises an infrared thermometer and a thermocouple; the infrared thermometers are mounted on the left side and the right side of the furnace body; the thermocouples are arranged on the front side and the rear side of the furnace body; the resistivity monitoring unit comprises an ohmmeter; and the ohmmeter, the power supply, the sample or the heating medium form a series loop. According to the ultra-fast high-temperature sintering system disclosed by the utility model, the resistivity of a sample, the resistivity of a heating medium, the heat conductivity, the temperature of the sample and the deformation quantity of the sample in the whole sintering process can be measured and monitored in situ.

Description

Technical Field

[0001] The utility model relates to ultra-fast high-temperature sintering equipment, in particular to an ultra-fast high-temperature sintering system capable of realizing electrical-thermal-morphological in-situ measurement. Background Art

[0002] Ultra-fast high-temperature sintering technology (UHS) is a new green and efficient high-temperature manufacturing method proposed in 2020. It has broad application prospects and can play a role in the preparation of high-performance ceramic materials, functional ceramic structure-performance integrated manufacturing, powder metallurgy, and high-temperature chemical reaction synthesis. The principle is to clamp the sample in layered materials such as graphite paper and carbon felt, and generate Joule heat by electricity, and achieve ultra-fast heating of the sample through heat conduction and heat radiation. However, limited by the layered heating structure, UHS technology can only achieve the preparation of small-sized and simple-structured samples. By changing the structural form of the heating element material, a new ultra-fast high-temperature sintering technology P-UHS based on a powder bed Joule heat source has recently emerged. Although this technology has solved the limitation of sample size to a certain extent, it still does not have the function of real-time monitoring of the physical parameters of the sample and the heating medium "electricity, heat, shape" during the ultra-fast sintering process. Therefore, it is impossible to achieve in-situ measurement and monitoring of important data such as the resistivity of the sample and the resistivity of the heating medium, thermal conductivity, sample temperature, and deformation of the sample during the sintering process. Utility Model Content

[0003] The purpose of the utility model is to overcome the shortcomings of the prior art and provide an ultra-fast high-temperature sintering system that can realize in-situ electrical-thermal-morphological measurement. The ultra-fast high-temperature sintering system can realize in-situ measurement and monitoring of the resistivity of the sample, the resistivity of the heating medium, the thermal conductivity, the sample temperature and the deformation of the sample during the entire sintering process.

[0004] The technical solution of the utility model to solve the above technical problems is:

[0005] An ultra-fast high-temperature sintering system capable of realizing electric-thermal-morphological in-situ measurement comprises a furnace body, a heating device arranged on the furnace body, a detection device and a control device, wherein:

[0006] The heating device is used to heat the sample in the furnace body, and the heating device includes a heat-insulating crucible, a heating medium arranged in the heat-insulating crucible, and a heating unit for heating the heating medium;

[0007] The detection device includes a deformation detection unit, a resistivity monitoring unit and a temperature control unit, wherein:

[0008] The deformation detection unit is used to detect the deformation amount of the sample during the sintering process, and includes a displacement sensor, the displacement sensor is installed on the furnace body, and the probe of the displacement sensor is in contact with the sample in the heat-insulating crucible;

[0009] The temperature control unit is used to detect the temperature of the sample during the sintering process, and includes an infrared thermometer and a thermocouple, wherein the infrared thermometer is installed on the left and right sides of the furnace body; the thermocouple is arranged on the front and rear sides of the furnace body;

[0010] The resistivity monitoring unit comprises an ohmmeter arranged on the upper side of the furnace body, and the ohmmeter forms a series circuit with a power source, a sample or a heating medium.

[0011] Preferably, two air ports are provided on the rear side of the furnace body, one of which serves as an air inlet and the other as an air outlet, and both the air inlet and the air outlet are connected to an atmosphere control system.

[0012] Preferably, the insulating crucible is placed on a bracket in the furnace cavity of the furnace body, and the insulating crucible comprises a main body and a cover plate, wherein openings are arranged on the front, back, left, right, and right sides of the main body and on the cover plate.

[0013] Preferably, a stepper motor is provided between the thermocouple and the furnace body. The stepper motor is mounted on the furnace body, and a main shaft thereof is connected to the thermocouple for driving the thermocouple to perform linear motion in the furnace body.

[0014] Preferably, the heating unit comprises a current input module and a conductive electrode, wherein the current input module is arranged on the left and right sides of the furnace body; the conductive electrodes are also arranged on the left and right sides of the furnace body; one end of the conductive electrode on each side passes through the opening of the insulation crucible and extends into the insulation crucible, and the other end is connected to the current input module.

[0015] Preferably, the heating medium is arranged in the insulating crucible in the form of powder and wraps the sample.

[0016] Preferably, the conductive electrode comprises a hollow electrode rod and an electrode sheet, wherein one end of the electrode rod extends into the insulating crucible and is connected to the electrode sheet, and the other end passes through an opening on the insulating crucible and is connected to the current input module; the electrode sheet is wrapped by the heating medium.

[0017] Preferably, a high temperature resistant insulating observation tube is provided inside the electrode rod; and visualization windows are provided on the left and right sides of the furnace body at positions corresponding to the high temperature resistant insulating observation tube.

[0018] Preferably, a damper is provided inside the displacement sensor, and the probe of the displacement sensor is a low thermal expansion insulating ceramic rod; the piston end of the damper is connected to the low thermal expansion insulating ceramic rod.

[0019] Preferably, the control device comprises a computer, and the computer is connected to the detection device.

[0020] Compared with the prior art, the utility model has the following beneficial effects:

[0021] 1. The ultra-fast high-temperature sintering system of the utility model that can realize in-situ measurement of electricity, heat and shape can realize the collection and recording of the deformation amount of the sample during the whole sintering process by bringing the probe of the displacement sensor into contact with the sample before sintering. During the sintering process, the sample shrinks to different degrees as the temperature rises, and the probe drops or rises as the volume of the sample changes. The displacement sensor then records the data of the probe rising or falling, thereby realizing the collection and recording of the deformation amount of the sample during the whole sintering process.

[0022] 2. The ultra-fast high-temperature sintering system of the utility model that can realize in-situ electrical-thermal-morphological measurement can realize accurate temperature measurement of samples during the sintering process through infrared thermometers and thermocouples, and provide data support for calculating thermal conductivity by collecting corresponding temperature data.

[0023] 3. The ultra-fast high-temperature sintering system of the utility model which can realize the in-situ measurement of electricity, heat and shape can measure the resistance of the sample or heating medium itself by placing an ohmmeter at the upper end of the furnace body and connecting the positive and negative electrodes of the wires corresponding to the power supply to the sample or heating medium; and then calculate the surface resistivity of the sample to be measured through the resistivity formula: ρ = Rx / (L / A), and then convert it into conductivity.

[0024] 4. The ultra-fast high-temperature sintering system of the utility model can realize in-situ measurement and monitoring of the resistivity of the sample, the resistivity of the heating medium, the thermal conductivity, the sample temperature and the deformation of the sample during the sintering process. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 The utility model is a schematic diagram of the overall device of the ultra-fast high-temperature sintering system capable of realizing the in-situ measurement of electricity, heat and shape.

[0026] Figure 2 This is a working principle diagram of the heating device and deformation detection unit.

[0027] Figure 3 It is a structural schematic diagram of the temperature control unit.

[0028] Figure 4 This is a schematic diagram of the thermal conductivity detection principle provided by the utility model.

[0029] Figure 5This is a resistivity detection principle diagram provided by the utility model.

[0030] Figure 6 It is a graph showing the change of resistivity of the heating medium with temperature during the sintering process in a specific implementation case.

[0031] Figure 7 This is a graph showing the change in thermal conductivity of the heating medium with temperature during the sintering process in a specific implementation case.

[0032] Figure 8 This is a graph showing how the sample's own temperature changes over time during the sintering process in a specific implementation case.

[0033] Fig. 9 This is a graph showing the change in sample diameter over time during the sintering process in a specific implementation case. DETAILED DESCRIPTION

[0034] The present invention is further described in detail below in conjunction with embodiments and drawings, but the implementation manner of the present invention is not limited thereto.

[0035] See also Figure 1-Figure 9 The ultra-fast high-temperature sintering system capable of realizing electric-thermal-morphological in-situ measurement of the utility model comprises a furnace body 1, a heating device arranged on the furnace body 1, a detection device and a control device.

[0036] See also Figure 1-Figure 9 The furnace body 1 is provided with a furnace door, and the furnace door can be tightly fitted on the furnace body 1 to ensure that the furnace body 1 is in a closed state.

[0037] See also Figure 1-Figure 9 The heating device is used to heat the sample 13 in the furnace body 1, and the heating device includes a heat-insulating crucible 9, a heating medium 10 arranged in the heat-insulating crucible 9, and a heating unit for heating the heating medium 10; wherein,

[0038] The heat-insulating crucible 9 is placed on a bracket in the furnace chamber of the furnace body 1, and the heat-insulating crucible 9 includes a main body and a cover plate; openings are provided on the front, back, left, right, and right sides of the main body and on the cover plate;

[0039] The heating unit includes a current input module and a conductive electrode 11, wherein the current input module is arranged on the left and right sides of the furnace body 1; the conductive electrode 11 is also arranged on the left and right sides of the furnace body 1; one end of the conductive electrode 11 on each side passes through the opening of the insulating crucible 9 and extends into the insulating crucible 9, and the other end is connected to the current input module; the current applied by the current input module flows through the conductive electrode 11, and then is conducted to the heating medium 10 by the conductive electrode 11. After the current is passed through, the heating medium 10 undergoes a Joule effect, thereby generating a large amount of Joule heat, thereby achieving ultra-fast high-temperature sintering.

[0040] See also Figure 1-Figure 9 The detection device includes a deformation detection unit, a resistivity monitoring unit and a temperature control unit.

[0041] See also Figure 1-Figure 9 The deformation detection unit is used to detect the deformation amount of the sample 13 during the sintering process, and includes a displacement sensor 4. The displacement sensor 4 is installed on the furnace body 1, and the probe of the displacement sensor 4 is in contact with the sample 13 in the insulation crucible 9; by contacting the probe of the displacement sensor 4 with the sample 13 before sintering, the sample 13 shrinks to varying degrees as the temperature rises during the sintering process, and the probe drops or rises as the volume of the sample 13 changes. The displacement sensor 4 then records the data of the probe rising or falling, thereby realizing the recording of the deformation amount of the sample 13 during the entire sintering process.

[0042] In this embodiment, the displacement sensor 4 is fixed on the furnace top. When the experiment starts, the probe of the device is in contact with the sample 13. The part in contact with the heating medium 10 (i.e., the probe part) is a low thermal expansion insulating ceramic rod, commonly used ones are Al2O3, AlN, BeO, BN, Si3N4, etc.; the damper arranged inside the displacement sensor 4 can effectively prevent the weight of the probe itself from affecting the placement of the sample 13. When the sample 13 shrinks during the experiment, the probe slowly descends or rises with the volume change of the sample 13. At the same time, the displacement sensor 4 records the displacement of the probe in real time, thereby reflecting the degree of volume change of the sample 13 during the sintering process.

[0043] See also Figure 1-Figure 9 The temperature control unit is used to detect the temperature of the sample 13 during the sintering process, and includes an infrared thermometer 5 and a thermocouple 2, wherein the infrared thermometer 5 is installed on the fixtures on the left and right sides of the furnace body 1; at the same time, both sides of the furnace body 1 are provided with visualization windows for cooperation; the thermocouple 2 is arranged on the front and rear sides of the furnace body 1, and a stepper motor 14 is arranged between the thermocouple 2 and the furnace body 1, and the stepper motor 14 is installed on the furnace body 1, and its main shaft is connected to the thermocouple 2, and is used to drive the thermocouple 2 to make a linear motion in the furnace body 1; thereby, the temperature of the sample 13 and the heating medium 10 at any position can be accurately measured, and then important parameters such as thermal conductivity can be calculated;

[0044] In addition, the temperature control unit in this embodiment is composed of an infrared thermometer 5 and a thermocouple 2: wherein the infrared thermometer 5 is placed on the fixtures on the left and right sides of the furnace door, and combined with the design of special electrodes, the whole process of visual monitoring and temperature data collection of the sample 13 and the heating medium 10 during the sintering process can be realized;

[0045] Regarding the visual temperature control unit, by adjusting the position of the high temperature resistant insulating observation tube 12 placed in the hollow electrode rod, the infrared thermometer 5 can realize accurate temperature measurement of the sample 13 during the sintering process. As for the temperature measurement of the infrared thermometer 5, by selecting a thermometer with different temperature measurement ranges, the temperature measurement threshold can be between -40℃ and 3200℃. With the development of the technology of the thermometer, the temperature measurement range can be expanded. Its communication interface is connected to the computer for real-time temperature transmission. Because the response time of the infrared thermometer 5 is 2ms, the real-time temperature can be accurately recorded.

[0046] Regarding the collection of thermal conductivity during the sintering process, by selecting thermocouples 2 with various temperature ranges and different functions, such as common types of thermocouples 2, such as J-type, T-type, K-type and B-type, according to different application scenarios, by selecting reasonable types to ensure that the data collected by thermocouple 2 is more accurate. Among them, the K-type thermocouple 2, also known as nickel-chromium-nickel-silicon thermocouple 2, has an operating temperature of -200-1300℃. The J-type thermocouple 2, also known as iron-copper-nickel thermocouple 2, covers a measurement temperature range of -200-1200℃, but the commonly used temperature range is 0-750℃. The T-type thermocouple 2, also known as copper-copper-nickel thermocouple 2, covers a measurement temperature range of -200-350℃. The B-type thermocouple 2, also known as platinum-rhodium 30 - Platinum-rhodium 6 thermocouple 2, which covers a temperature range of 0-1800°C. In addition, there are various types of thermocouples 2 to choose from, which can be freely replaced and flexibly extended by the detachable device and the control of the stepper motor 14 to ensure accurate acquisition of the temperature of the measured position during the sintering process.

[0047] Regarding the measurement of thermal conductivity, by setting the two thermocouples 2 in front and behind the furnace body 1 at different positions (i.e. setting different displacement amounts), the temperature collected by the two thermocouples 2 during the heating process will show a gradient (T1-T2), and at the same time, the cross-sectional area A of the measured object and the distance D between the two thermocouples 2 are recorded. In this way, the thermal conductivity K of the corresponding object can be calculated through Fourier's heat conduction law, that is, the formula: K=Q×D / A×(T1-T2), where the parameter Q is the thermal power. This device is an electric heating device, so Q=U×I.

[0048] See also Figure 1-Figure 9The resistivity monitoring unit includes an ohmmeter 3 arranged on the upper side of the furnace body 1, and the ohmmeter 3, the power supply, and the sample 13 form a series circuit; regarding the measurement of resistivity, the ohmmeter 3 arranged on the upper end of the furnace body 1 is used to contact the positive and negative electrodes of the wires of the ohmmeter 3 corresponding to the power supply with the sample 13 or the heating medium 10, so as to measure the resistance Rx of the sample 13 or the heating medium 10 itself; and then through the resistivity formula: ρ = Rx / (L / A), where L is the thickness of the sample 13, and A is the cross-sectional area of ​​the sample 13, the surface resistivity of the measured sample 13 is calculated, and then converted into conductivity.

[0049] This embodiment also includes a power supply system 6, which is controlled by a computer, wherein the power supply is connected to a current input module, and the input current can be DC, AC, or pulse current input. The heating rate can be adjusted by changing the input current and voltage of the power supply, and the process can be adjusted by controlling the power-on time.

[0050] See also Figure 1-Figure 9 In this embodiment, the sample 13 is placed in a heating medium 10, and the heating medium 10 is placed in a heat-insulating crucible 9 (auxiliary heating chamber) made of refractory material. The material used for the heating medium 10 is an electric heating material; the material has a sufficiently large resistance value so that the electric heating material can generate huge Joule heat when current passes through, and the Joule heat can sinter the sample 13 after heat transfer; therefore, among the electric heating materials that can be used: metal materials with high melting points such as W, Mo, Ta, etc. can be used as electric heating materials; non-metallic materials such as SiC, MoS i2, ZrO2, and graphite materials are all good electric heating materials; and the refractory material needs to have the characteristics of non-conductivity and high temperature resistance, as well as corrosion resistance and good stability. Its role is to minimize the dissipation of heat and make the sample 13 heated more evenly, such as Al2O3, AlN, BeO, BN, Si3N4, etc.

[0051] See also Figure 1-Figure 9 Two air ports are arranged on the rear side of the furnace body 1, one of which serves as an air inlet and the other as an air outlet, and both the air inlet and the air outlet are connected to the atmosphere control system 7; the type of input gas is controlled by connecting various gas pipelines and adjusting valves; and the inside of the furnace cavity can be evacuated to form a vacuum through a vacuum pump.

[0052] See also Figure 1-Figure 9 The conductive electrode 11 includes a hollow electrode rod and an electrode sheet, wherein one end of the electrode rod extends into the heat-insulating crucible 9 and is connected to the electrode sheet, and the other end passes through the opening on the heat-insulating crucible 9 and is connected to the current input module; the electrode sheet is wrapped by the heating medium 10; a high-temperature resistant insulating observation tube 12 is arranged inside the electrode rod;

[0053] The heating medium 10 is composed of an electrothermal material, and is mainly heated in the form of powder wrapping, specifically by the accumulation of powder and wrapping the sample 13; when current is input to the heating medium 10 through the conductive electrode 11, the current flows through the powder to generate a large amount of Joule heat, which is then transferred to the sample 13 wrapped by it to complete sintering. However, there are huge limitations in the visual temperature measurement operation under the condition that the powder is accumulated and buried in the sample 13. Therefore, by designing a conductive electrode 11 with a high-temperature resistant insulating observation tube 12 and adding a movable thermocouple 2, the temperature of each position in the furnace can be accurately obtained.

[0054] Since a movable high-temperature resistant insulating observation tube 12 is arranged in the hollow electrode rod, the high-temperature resistant insulating observation tube 12 can realize smooth movement inside the electrode rod; the electrode rod and the electrode sheet are both composed of conductive materials, commonly used are platinum, palladium, silver, copper, graphite, carbon nanotubes, etc.; the high-temperature resistant insulating observation tube 12 is composed of low thermal expansion insulating ceramic materials, commonly used are Al2O3, AlN, BeO, BN, Si3N4, etc.

[0055] See also Figure 1-Figure 9 , the control device, i.e. the data acquisition unit, analyzes and processes the data after it is transmitted into the computer through the program. A system composed of multiple programs, the system includes: resistivity, thermal conductivity data acquisition calculation, temperature analysis, system current and voltage input control. Regarding resistivity and thermal conductivity data acquisition calculation, the data collected by the above-mentioned ohmmeter 3 and thermocouple 2 are imported into the program, and the resistivity and thermal conductivity of the measured object can be directly calculated and displayed on the program panel; regarding temperature analysis, the infrared thermometer 5 on both sides cooperates with the electrode to achieve accurate acquisition of the sample temperature. In addition, it is also possible to connect the thermocouple 2 that meets the experimental conditions to the set stepper motor 14, and control its forward and backward displacement through the program, so as to achieve accurate measurement of the temperature of the surface of the sample 13 and the surrounding heating medium 10, and the read temperature is converted into a digital signal by the computer in the form of an electrical signal and displayed on the computer panel, so that the temperature can be read more intuitively during the experiment. Regarding the system current and voltage input control, by connecting the power supply system 6 to the computer with a relay, the computer can remotely control the power supply. This not only allows the remote setting of current and voltage, but also records the data of the current and voltage applied by the power supply over time during the entire experiment, and finally exports them into a table for subsequent optimization of the experimental plan.

[0056] See also Figure 1-Figure 9 The specific operation method of the ultra-fast high temperature sintering system of the utility model includes the following steps:

[0057] S1: Install the heat-insulating crucible 9 and place the sample 13:

[0058] First, control the stepper motor 14 to move the thermocouple 2 to a suitable position to ensure that it will not affect the installation of the insulation crucible 9, and then install the insulation crucible 9 corresponding to the electrode position, and then add an appropriate amount of powder (i.e., heating medium 10) to ensure that the height required for the sample 13 is reached. After placing the sample 13, move the observation tube 12 placed inside the conductive electrode 11 to ensure that it is aligned with and close to the sample 13, and then bring the probe of the displacement sensor 4 into contact with the sample 13, and then add subsequent powder to ensure that the sample 13 is fully wrapped.

[0059] S2: Preparation before sintering:

[0060] After the insulation structure is installed, the furnace door is closed, and the atmosphere required for sintering is formed in the furnace through the atmosphere control system 7. Then, the computer is connected to the power supply system 6, the ohmmeter 3, the temperature control unit and the deformation detection unit to ensure real-time monitoring and remote control throughout the experimental process.

[0061] S3: Process Control:

[0062] The power supply system 6 can be remotely controlled by a computer to adjust the input current and voltage, set a suitable sintering process, and move the observation tube 12 on one side to adjust the required temperature measurement area. At the same time, the motor can be adjusted by a computer to move the thermocouple 2 to a suitable position to accurately collect the temperature and thermal conductivity parameters at that position.

[0063] S4: Data Recording:

[0064] During the sintering process, the current and voltage input by the power supply system 6, the resistance data detected by the ohmmeter 3, the temperature change recorded by the infrared thermometer 5, the temperature detected by the thermocouple 2, and the deformation parameters of the sample 13 are all output in the form of line graphs and tables, so as to record all important data during the experiment.

[0065] S5: Cooling and removal:

[0066] After the sintering is completed and the temperature is lowered, the furnace door can be opened, and then the heat-insulating crucible 9 can be opened to take out the sample 13.

[0067] S6: Post-processing:

[0068] According to the mass of the sample 13 taken out, the changes in the output current and voltage during the experiment, the resistivity, thermal conductivity and temperature of the sample 13 or the heating medium 10, and the important data of the size change of the sample 13 itself, the experimental parameters and processes are optimized in combination with simulation to ensure the quality of subsequent experiments.

[0069] The following is a specific implementation case (sintering experiment of material A):

[0070] S1: Preparation of Material A green body: The powder of Material A was dry-pressed (15Mpa) on a uniaxial molding machine, and then maintained at a pressure of 200Mpa for 5 minutes using a cold isostatic press to form a cylindrical green body of Material A with a diameter of 20mm and a height of 3mm. The green body was then cold-isostatically pressed with the process set to 200Mpa for 300s, and then Sample 13 was taken out to complete the preparation of Sample 13.

[0071] S2: Preparation work before sintering: Place the circular green body of material A into the ultra-fast high-temperature sintering system, fill the powder, i.e., the thermoelectric material, to the appropriate position, place the sample 13 stably, and then move the observation tube 12 close to the sample 13 to ensure accurate temperature measurement. Connect the power supply system 6, the temperature control unit, and the deformation detection unit to the computer, and lower the displacement sensor 4 so that its probe contacts the sample 13. At the same time, the computer controls the stepper motor 14 to move the two thermocouples 2 so that they are close to the sample 13 to different degrees to measure the thermal conductivity of the heating medium 10. Then continue to add powder until the sample 13 is completely wrapped. Use a vacuum pump to evacuate the air pressure in the furnace to negative pressure, and then fill the furnace with argon through the atmosphere control system 7 to ensure that the entire experiment is carried out in an argon atmosphere.

[0072] S3: Sintering experiment of sample 13: After ensuring that the computer is connected to the power supply system 6, the input current can be set to 30A through the program. After only 150s, the infrared thermometer 5 measures that the temperature of sample 13 reaches about 1150K. At this time, the control panel shows that the thermal conductivity is 0.33W / (m·K) and the resistivity is 10 -2 s / m, the deformation detection unit detected that the sample 13 had only a displacement of 0.2mm. During the sintering process, the heating rate and the final target temperature were controlled by controlling the input current and voltage. After the sintering was completed, the temperature, thermal conductivity and deformation degree of the sample 13 during the experiment were recorded by the program. After saving, the sample 13 could be cooled naturally and taken out.

[0073] S4: Post-experiment processing and optimization: The resistivity and thermal conductivity of the heating medium 10 monitored during the experiment, as well as the temperature and deformation data of the sample 13 itself, are exported as a line graph through program processing. It can be clearly seen that the sample 13 shrinks significantly at a certain moment, and the temperature of the sample 13 and the resistivity and thermal conductivity of the heating medium 10 are recorded at this time. By comparing each group of data, the optimal sintering temperature of the sample 13 can be obtained. At the same time, the collected data is imported into the simulation software to simulate the subsequent experiments and optimize various process parameters.

[0074] The above is a preferred implementation mode of the present invention, but the implementation mode of the present invention is not limited by the above content. Any other changes, modifications, substitutions, combinations, and simplifications that do not deviate from the spirit and principle of the present invention should be equivalent replacement methods and are included in the protection scope of the present invention.

Claims

1. An ultra-fast high-temperature sintering system capable of realizing in-situ electrical, thermal and structural measurements, characterized in that: It includes a furnace body, a heating device, a detection device and a control device arranged on the furnace body, wherein: The heating device is used to heat the sample in the furnace body, and the heating device includes a heat-insulating crucible, a heating medium arranged in the heat-insulating crucible, and a heating unit for heating the heating medium; The detection device includes a deformation detection unit, a resistivity monitoring unit and a temperature control unit, wherein: The deformation detection unit is used to detect the deformation amount of the sample during the sintering process, and includes a displacement sensor, the displacement sensor is installed on the furnace body, and the probe of the displacement sensor is in contact with the sample in the heat-insulating crucible; The temperature control unit is used to detect the temperature of the sample during the sintering process, and includes an infrared thermometer and a thermocouple, wherein the infrared thermometer is installed on the left and right sides of the furnace body; the thermocouple is arranged on the front and rear sides of the furnace body; The resistivity monitoring unit comprises an ohmmeter arranged on the upper side of the furnace body, and the ohmmeter forms a series loop with a power source, a sample or a heating medium.

2. The ultra-fast high-temperature sintering system capable of realizing in-situ electrical-thermal-morphological measurement according to claim 1, characterized in that: Two air ports are arranged at the rear side of the furnace body, one of which is used as an air inlet and the other is used as an air outlet. Both the air inlet and the air outlet are connected to an atmosphere control system.

3. The ultra-fast high-temperature sintering system capable of realizing in-situ electrical, thermal and structural measurements according to claim 1, characterized in that: The heat-insulating crucible is placed on a bracket in the furnace cavity of the furnace body, and comprises a main body and a cover plate, wherein openings are arranged on the front, back, left, right, and right sides of the main body and on the cover plate.

4. The ultra-fast high-temperature sintering system capable of realizing in-situ electrical-thermal-morphological measurement according to claim 3, characterized in that: A stepper motor is arranged between the thermocouple and the furnace body. The stepper motor is mounted on the furnace body, and a main shaft of the stepper motor is connected to the thermocouple, so as to drive the thermocouple to perform linear motion in the furnace body.

5. The ultra-fast high-temperature sintering system capable of realizing in-situ electrical, thermal and structural measurements according to claim 1, characterized in that: The heating unit includes a current input module and a conductive electrode, wherein the current input module is arranged on the left and right sides of the furnace body; the conductive electrodes are also arranged on the left and right sides of the furnace body; one end of the conductive electrode on each side passes through the opening of the insulation crucible and extends into the insulation crucible, and the other end is connected to the current input module.

6. The ultra-fast high-temperature sintering system capable of realizing in-situ electrical-thermal-morphological measurement according to claim 5, characterized in that: The heating medium is arranged in the heat-insulating crucible in the form of powder and wraps the sample.

7. The ultra-fast high-temperature sintering system capable of realizing in-situ electrical, thermal and structural measurements according to claim 6, characterized in that: The conductive electrode includes a hollow electrode rod and an electrode sheet, wherein one end of the electrode rod extends into the insulating crucible and is connected to the electrode sheet, and the other end passes through the opening on the insulating crucible and is connected to the current input module; the electrode sheet is wrapped by the heating medium.

8. The ultra-fast high-temperature sintering system capable of realizing in-situ electrical-thermal-morphological measurement according to claim 7, characterized in that: A high temperature resistant insulating observation tube is arranged inside the electrode rod; and visualization windows are arranged at positions corresponding to the high temperature resistant insulating observation tube on the left and right sides of the furnace body.

9. The ultra-fast high-temperature sintering system capable of realizing in-situ electrical, thermal and structural measurements according to claim 1, characterized in that: A damper is arranged inside the displacement sensor, and the probe of the displacement sensor is a low thermal expansion insulating ceramic rod; the piston end of the damper is connected to the low thermal expansion insulating ceramic rod.

10. The ultra-fast high-temperature sintering system capable of realizing in-situ electrical, thermal and structural measurements according to claim 1, characterized in that: The control device comprises a computer, and the computer is connected to the detection device.

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