A magnetic field material processing device under variable atmosphere with a temperature up to 2000 °C

Abstract

The present invention discloses a magnetic field material processing device under variable atmosphere with a temperature up to 2000 °C, comprising: a vacuum furnace body, a heating furnace body, a heat preservation furnace body, a superconducting magnet, a test tube, a heating element and a thermocouple; the vacuum furnace body, the heating furnace body and the heat preservation furnace body are coaxially arranged from top to bottom and detachably connected, the superconducting magnet surrounds the outer periphery of the heating furnace body, an up-and-down driving device is arranged on the mounting rack, and the up-and-down driving device can move the vacuum furnace body and the heating furnace body up and down along the superconducting magnet; a side-end driving device is arranged on the up-and-down driving device, and the side-end driving device can move the vacuum furnace body to one side of the heating furnace body, the lower end of the test tube is inserted into the heating element, and the heating element is used to heat the sample in the test tube; the detection part of the thermocouple is located below the test tube to realize real-time monitoring of the temperature of the sample in the test tube. The present invention couples an atmosphere control system in a conventional heating furnace body, which is closer to the actual working conditions under extreme external fields and provides more technical data for the application of strong magnetic fields.

Description

Technical Field

[0001] The present invention relates to the technical field of melt treatment, heat treatment methods, and test analysis of materials in a wide temperature range (0°C - 2000°C) under extreme external magnetic field conditions, and particularly relates to a magnetic field material treatment device under variable atmosphere with a temperature up to 2000°C. Background Art

[0002] One generation of materials, one generation of equipment. Continuously improving and optimizing the preparation and processing technology of materials to obtain high-quality and high-performance material components is the goal that people have been pursuing tirelessly. With the development bottleneck of conventional preparation technologies and the application development of various external field environments. In recent years, the technology of material preparation under magnetic field has received extensive attention from research scholars, that is, different forms of external magnetic fields, such as static magnetic field, gradient magnetic field, pulsed magnetic field, rotating magnetic field, etc., are applied during the preparation process of materials to achieve the control and improvement of the microstructure and properties of materials. Among them, the strong magnetic field, as an extreme physical field with high energy density, high efficiency, greenness, and non-contact, has rich and strong interaction with matter. Its action spans from the macroscopic to the microscopic levels, and can affect the processes of flow, heat transfer, and mass transfer during the solidification and heat treatment of materials, directly affecting the arrangement, matching, migration, etc. of atoms in the material, and thus affecting the microstructure and service performance of the material. In addition, many interesting phenomena will also be shown after the material is treated under magnetic field, such as magneto-induced phase change, magneto-induced plasticity, magneto-induced supercooling and other effects. Magnetic fields can also be used to prepare magneto-optical materials, gradient functional materials, multi-functional films, etc. with special properties. The nucleation and growth processes of nanomaterials are regulated to obtain highly anisotropic nanomaterials. The above cases all demonstrate the wide potential applications of magnetic fields in controlling the material preparation process, and are regarded as important research fields with foresight and strategy at home and abroad. Therefore, the design and development of related devices for material treatment under magnetic field are essential links.

[0003] In the initial design of material treatment devices under strong magnetic fields, the magnetic field intensity was mostly provided by permanent magnets, and the temperature that the heating furnace body could withstand was relatively low. For such magnetic field heat treatment devices, generally, the demagnetizing magnetic field was provided by combining different forms of permanent magnets, and the magnetic field intensity was far lower than 1T, and the magnetic field treatment temperature was below 800°C. In addition to the function of heat treatment, relevant literature has further designed to form the diversity of material treatment methods under magnetic field, and superconducting strong magnets were used for excitation during the treatment process, but the overall magnetic field intensity was still lower than 1T, the magnetic field treatment temperature was 900°C, and the size of the magnetic field treatment sample was 3mm. When magnetic field treatment was carried out on materials that were insensitive to magnetic fields and had higher treatment temperatures, it would be restricted, and at the same time, it would also limit the performance tests of mechanical properties, electrical properties, magnetic properties, etc. of the materials after magnetic field treatment. This has limited effects on paramagnetic materials that need to be treated with strong magnetic fields and some materials with higher requirements for magnetic field treatment temperatures.

[0004] To overcome the problems of low magnetic field intensity and low temperature range during the processing, many universities and enterprises have targeted magnetic generating devices with higher magnetic field intensity and heat-resistant materials to manufacture heating furnace bodies. However, most of the existing device designs are relatively complex, and the length of the heating furnace body is relatively long. During actual use, the temperature range for material processing is small, and the heat loss in the remaining parts is large, which affects the service life of the heating furnace body and requires irregular replacement. When replacing, many accessories need to be disassembled, which is inconvenient. Manual debugging is required and the position needs to be limited at one time. At the same time, the atmosphere in the furnace is also single and cannot simulate the changes in the atmosphere in the actual working conditions.

[0005] It can be easily seen from the above reports that currently, the material processing devices under extreme magnetic fields are moving towards higher magnetic fields, more complex magnetic field forms, higher temperatures, and larger-sized specimens. However, the actual heating temperature is still limited, often lower than 1700 °C, the magnet aperture is still small, and with the improvement of integration, the device is complex, difficult to maintain, the utilization rate of accessories is low, the service time is short, and the replacement is complex. Therefore, it is necessary to further design and optimize and invent a new magnetic field material processing device. Summary of the Invention

[0006] In order to further increase the material processing temperature of the device, extend the service life of the components, improve the use efficiency, reduce losses, and broaden the working conditions that the device can handle, the present invention proposes a magnetic field material processing device under variable atmosphere with a temperature up to 2000 °C.

[0007] In order to achieve the above objectives, the present invention specifically adopts the following technical solutions:

[0008] The present invention provides a magnetic field material processing device under variable atmosphere with a temperature up to 2000 °C, including: a mounting frame, a vacuum furnace body, a heating furnace body, a heat preservation furnace body, a superconducting magnet, a test tube, a heating element, a thermocouple, and a mechanical pump;

[0009] The vacuum furnace body, the heating furnace body, and the heat preservation furnace body are coaxially arranged from top to bottom and are detachably connected;

[0010] The mechanical pump is externally connected to the vacuum furnace body and is used for evacuating the vacuum furnace body and the heating furnace body;

[0011] The superconducting magnet is fixedly installed at the lower part of the mounting frame, and the superconducting magnet surrounds the outer periphery of the heating furnace body and can move relatively;

[0012] The mounting frame is further provided with an up-and-down driving device which can move the vacuum furnace body and the heating furnace body up and down along the superconducting magnet. A side-end driving device is arranged on the up-and-down driving device. When the vacuum furnace body and the heating furnace body are in a disconnected state, the side-end driving device can move the vacuum furnace body to one side of the heating furnace body.

[0013] The upper end of the test tube is installed in the vacuum furnace body, the lower end is inserted into the heating furnace body and extends into the heating body.

[0014] The heating body is arranged in the heating furnace body and is used to heat the sample in the test tube.

[0015] The thermocouple is installed below the heat preservation furnace body and inserted upward into the heat preservation furnace body and the heating furnace body. The detection part of the thermocouple is located below the test tube to realize real-time monitoring of the temperature of the sample in the test tube and feedback the real-time temperature to the temperature controller. After comparing the received real-time temperature with the set temperature, the temperature controller controls the heating power supply to adjust the heating body.

[0016] Furthermore, the up-and-down driving device includes a lifting motor and a four-axis lead screw; the side-end driving device includes a support plate, a guide rail and a sliding seat.

[0017] The support plate is arranged above the mounting frame. The lifting motor is fixedly installed on the top plate of the mounting frame. The four-axis lead screw is connected to the output shaft of the lifting motor and is threadedly connected to the support plate. The guide rail is fixedly installed on the support plate. The sliding seat is slidably connected to the guide rail. The sliding seat is connected to the side-end mounting plate of the vacuum furnace body. Side U-shaped grooves are opened on both the support plate and the top plate of the mounting frame. When the vacuum furnace body moves to one side, it moves along the inside of the U-shaped groove.

[0018] Furthermore, the test tube is composed of four parts, including a first section, a second section, a third section and a fourth section which are threadedly connected to each other from top to bottom. The first section is assembled in the vacuum furnace body. The first section and the second section are non-heating body heating areas. The third section and the fourth section are core heating areas. The disassembly and assembly of the third section can realize material processing with different intensity gradient magnetic fields.

[0019] Furthermore, the processing materials of the first section and the second section are zirconia materials, and the processing materials of the third section and the fourth section are graphite materials.

[0020] Furthermore, a test tube clamp and an infrared probe are arranged inside the vacuum furnace body, and an electronic precision balance is arranged above the vacuum furnace body; when measuring the magnetic susceptibility of the balance, the top end of the test tube clamp is connected to the electronic precision balance, and the bottom end of the test tube clamp is connected to the test tube through a nylon bolt, so that the test tube is freely suspended, thereby obtaining the change in the total mass of the test tube clamp, the test tube, and the sample located at the bottom inside the test tube through the electronic precision balance; the infrared probe and the precision electronic balance are connected to the main control cabinet through wires and conversion interfaces, thereby displaying the change in the detected real-time temperature and the mass of the object weighed by the balance.

[0021] Furthermore, the infrared probes are a set of symmetrically arranged ones, respectively used for infrared detection in different low-temperature and high-temperature sections. First installation cavities are arranged on both side walls of the vacuum furnace body, and a transverse driving mechanism is connected to the outside of the first installation cavity. The transverse driving mechanism is used to move the corresponding infrared probe into or out of the vacuum furnace body to realize the penetration work of different infrared probes in the low-temperature and high-temperature sections.

[0022] Furthermore, the heating furnace body is provided with a first water-cooled interlayer, and a furnace body heat preservation layer is arranged inside the first water-cooled interlayer. The test tube, the heating element, and the thermocouple are all located inside the furnace body heat preservation layer; a test tube heat preservation layer is arranged outside the test tube, and a thermocouple heat preservation layer is arranged outside the thermocouple. The test tube heat preservation layer and the thermocouple heat preservation layer are both located inside the furnace body heat preservation layer.

[0023] Furthermore, a connecting conductor is arranged inside the heat preservation furnace body. The upper end of the connecting conductor extends into the heating furnace body and is connected to the bottom of the heating element. Water-cooled heating electrodes are arranged on both sides at the lower end of the heat preservation furnace body. The water-cooled heating electrodes extend into the heat preservation furnace body and are connected to the lower end of the connecting conductor; a water-cooling groove is arranged inside the water-cooled heating electrode, a cold water pipe is arranged inside the water-cooling groove, the outer end of the cold water pipe extends out of the water-cooled heating electrode and is connected to a water inlet pipe, and a water outlet pipe is connected to the outer end of the water-cooled heating electrode. The water outlet pipe is communicated with the inside of the water-cooling groove.

[0024] Furthermore, a second installation cavity is arranged on the outer side wall of the heat preservation furnace body. The water-cooled heating electrode enters the heat preservation furnace body through the second installation cavity, and the second installation cavity and the water-cooled heating electrode are connected by a flange; a set of assembly openings for connecting the connecting conductor and the water-cooled heating electrode are also opened on the side wall of the heat preservation furnace body.

[0025] Furthermore, the outer shell of the heat preservation furnace body is a double-layer wall structure inside and outside, forming a second water-cooled interlayer. A lower connecting flange is arranged at the bottom of the heat preservation furnace body. The bottom of the lower connecting flange is connected to a thermocouple fixing plate, and the thermocouple is fixedly installed on the thermocouple fixing plate. A group of symmetrical partitions are arranged in the second water-cooled interlayer. The bottom ends of the partitions are fixed on the lower connecting flange, and the top ends are lower than the top end of the second water-cooled interlayer. The two parts of the cavity formed by the second water-cooled interlayer separated by the partitions are respectively connected with inlet and outlet water pipes at the lower ends.

[0026] Other features and advantages of the present invention will be described in the following specification, and, in part, will be obvious from the specification, or will be understood by implementing the technical solution of the present invention. The objectives and other advantages of the present technical solution can be achieved and obtained through the structures specifically pointed out in the written specification and the drawings.

[0027] The technical solution of the present invention will be further described in detail below through the drawings and embodiments. Description of the Drawings

[0028] The drawings are used to provide a further understanding of the present technical solution, and constitute a part of the specification. Together with the embodiments of the present technical solution, they are used to explain the present technical solution, and do not constitute a limitation to the present technical solution. In the drawings:

[0029] Figure 1 is the overall structure diagram of the variable atmosphere magnetic field material processing device with a temperature up to 2000°C provided by the present invention.

[0030] Figure 2 is the semi-sectional structure diagram of the variable atmosphere magnetic field material processing device with a temperature up to 2000°C provided by the present invention.

[0031] Figure 3 is the structure diagram of the variable atmosphere magnetic field material processing device with a temperature up to 2000°C provided by the present invention.

[0032] Figure 4 is the connection structure diagram of the vacuum furnace body driving device provided by the present invention.

[0033] Figure 5 is the outer side structure diagram of the vacuum furnace body provided by the present invention.

[0034] Figure 6 is the connection structure diagram of the joint between the vacuum furnace body and the heating furnace body provided by the present invention.

[0035] Figure 7 is the structure diagram of the heating furnace body provided by the present invention.

[0036] Figure 8 is the structure diagram of the first water-cooled interlayer provided by the present invention.

[0037] Figure 9 It is a schematic structural diagram of the heating element provided by the present invention.

[0038] Figure 10 It is a schematic structural diagram of the test tube provided by the present invention.

[0039] Figure 11 It is a schematic semi-sectional structural diagram of the heat preservation furnace provided by the present invention.

[0040] Figure 12 It is a schematic structural diagram of the heat preservation furnace with the outer wall removed provided by the present invention.

[0041] Figure 13 It is a schematic semi-sectional structural diagram of the water-cooled heating electrode provided by the present invention.

[0042] Figure 14 It is a magnetic field distribution diagram inside the superconducting magnet when the magnetic field strength is 10T.

[0043] Reference numerals:

[0044] Water cooler 1, compressor 2, excitation power supply 3, superconducting magnet 4, test tube 5, first section 501, second section 502, third section 503, fourth section 504, heating furnace body 6, water inlet 601, water outlet 602, water inlet pipe 603, heating element 7, vertical groove 701, threaded hole 702, sample 8, first water-cooled interlayer 9, connection disk 10, heat preservation furnace body 11, double-layer wall 1101, second water-cooled interlayer 1102, assembly port 1103, lower connection flange 1104, second installation cavity 1105, partition plate 1106, heat preservation layer 12, furnace body heat preservation layer 1201, test tube heat preservation layer 1202, thermocouple heat preservation layer 1203, connection conductor 13, thermocouple 14, water-cooled heating electrode 15, water inlet pipe 1501, water outlet pipe 1502, water-cooled groove 1503, cold water pipe 1504, thermocouple fixing plate 16, vacuum furnace body 17, viewing window 1701, first installation cavity 1702, precision electronic balance 18, infrared probe 19, test tube clamp 20, test tube fastener 21, flange disk 22, mechanical pump 23, heating power supply 24, temperature controller 25, general control cabinet 26, terminal computer 27, U-shaped groove 28, four-axis lead screw 29, lifting motor 30, lateral driving mechanism 31, bracket 3101, screw rod 3102, screw seat 3103, support plate 32, guide rail 3201, sliding seat 3202, mounting frame 33, flange 34, wire connection seat 35. Detailed implementation manners

[0045] To make the objectives, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Apparently, the described embodiments are some, but not all, of the embodiments of the present invention. Components of the embodiments of the present invention generally described and illustrated in the drawings herein can be arranged and designed in a variety of different configurations.

[0046] Therefore, the detailed description of the embodiments of the present invention provided in the drawings below is not intended to limit the scope of the claimed invention, but merely represents selected embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts fall within the scope of protection of the present invention.

[0047] It should be noted that like reference numerals and letters denote like items in the following drawings. Therefore, once an item is defined in one drawing, it does not require further definition and explanation in subsequent drawings.

[0048] In the description of the present invention, it should be noted that the orientation or positional relationship indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. is based on the orientation or positional relationship shown in the drawings, or the orientation or positional relationship in which the inventive product is customarily placed during use. It is only for the convenience of describing the present invention and simplifying the description, and does not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as a limitation of the present invention. In addition, the terms "first", "second", "third", etc. are only used for descriptive distinction and should not be construed as indicating or implying relative importance.

[0049] In addition, terms such as "horizontal" and "vertical" do not mean that the components are required to be absolutely horizontal or hanging, but can be slightly inclined. For example, "horizontal" only means that its direction is more horizontal relative to "vertical", and does not mean that the structure must be completely horizontal, but can be slightly inclined.

[0050] In the description of the present invention, it should also be noted that unless otherwise clearly specified and defined, the terms "set", "installed", "connected", and "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected, or indirectly connected through an intermediate medium, and can be the communication inside two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific situations.

[0051] The technical solutions of the present invention will be explained below with reference to specific embodiments.

[0052] As shown Figure 1-3 in the figure, the present invention provides a magnetic field material processing device under variable atmosphere with a temperature up to 2000 °C, comprising: a mounting frame 33, a vacuum furnace body 17, a heating furnace body 6, a heat preservation furnace body 11, a superconducting magnet 4, a test tube 5, a heating element 7, a thermocouple 14 and a mechanical pump 23;

[0053] The vacuum furnace body 17, the heating furnace body 6 and the heat preservation furnace body 11 are coaxially arranged from top to bottom and detachably connected; the mechanical pump 23 is externally connected to the vacuum furnace body 17 for performing vacuum pumping operations in the vacuum furnace body 17 and the heating furnace body 6; the superconducting magnet 4 is fixedly installed at the lower part of the mounting frame 33, and the superconducting magnet 4 surrounds the outer periphery of the heating furnace body 6 and can move relatively; a vertical driving device is further arranged on the mounting frame 33, and the vertical driving device can realize the vertical movement of the vacuum furnace body 17 and the heating furnace body 6 along the superconducting magnet 4; a side-end driving device is arranged on the vertical driving device, and when the vacuum furnace body 17 and the heating furnace body 6 are in a disconnected state, the side-end driving device can move the vacuum furnace body 17 to one side of the heating furnace body 6; the upper end of the test tube 5 is installed in the vacuum furnace body 17, the lower end is inserted into the heating furnace body 6 and extends into the heating element 7; the heating element 7 is arranged in the heating furnace body 6 for heating the sample 8 in the test tube 5; the thermocouple 14 is installed below the heat preservation furnace body 11 and inserted upward into the heat preservation furnace body 11 and the heating furnace body 6, so that the detection part of the thermocouple 14 is located below the test tube 5 to realize real-time monitoring of the temperature of the sample 8 in the test tube 5, and the real-time temperature is fed back to the temperature controller 25. After comparing the received real-time temperature with the set temperature, the temperature controller 25 controls the heating power supply 24 to realize the regulation of the heating element 7.

[0054] Since the vacuum furnace body 17 is connected to the heating furnace body 6, the vertical driving device can realize the vertical movement of the vacuum furnace body 17 and the heating furnace body 6 along the superconducting magnet 4. With the different moving positions of the heating furnace body 6, the integrated multi-functional function of the device can be realized, that is, at positions 350 mm and 250 mm downward from the upper surface of the superconducting magnet, material processing can be realized under a 0-10 T uniform magnetic field and a 0-75 T 2 / m gradient magnetic field in the temperature range of 0-2000 °C.

[0055] As shown Figure 4As shown, in some embodiments, the up-and-down driving device includes a lifting motor 30 and a four-axis lead screw 29; the side-end driving device includes a support plate 32, a guide rail 3201, and a sliding seat 3202; the support plate 32 is disposed above the mounting frame 33, the lifting motor 30 is fixedly installed on the top plate of the mounting frame 33, the four-axis lead screw 29 is connected to the output shaft of the lifting motor 30, the four-axis lead screw 29 is threadedly connected to the support plate 32, the guide rail 3201 is fixedly installed on the support plate 32, the sliding seat 3202 is slidably connected to the guide rail 3201, the sliding seat 3202 is connected to the side-end mounting plate of the vacuum furnace body 17, and side U-shaped grooves 28 are opened on both the support plate 32 and the top plate of the mounting frame 33. When the vacuum furnace body 17 moves to one side, it moves along the inside of the U-shaped groove 28.

[0056] The lifting motor 30 controlled by the main control cabinet 26 realizes the clockwise / counterclockwise rotation of the four-axis lead screw 29, driving the overall vacuum furnace body 17 to lift. Since the vacuum furnace body 17 is connected to the heating furnace body 6, it can be lifted simultaneously along the Z axis, thereby realizing the automatic adjustment of the position of the heating furnace body and realizing the processing of the test sample 8 under different static magnetic field strengths and gradient magnetic fields of different sizes and directions.

[0057] Since the vacuum furnace body 17 and the heating furnace body 6 adopt a detachable connection method, such as Figure 8 As shown, for example, the two are connected by a flange 34 and bolts. When used in a vacuum and protective atmosphere (an inert gas input device can be connected to the outside of the vacuum furnace body 17), the two parts are connected, which can not only realize the material processing under the atmosphere, but also realize the material processing in the air atmosphere. If the two parts are not connected, the vacuum furnace body 17 can be slid along the x-axis guide rail 3201 to the other end, and only the material processing in the air can be realized.

[0058] The present invention couples an atmosphere control system in a conventional heating furnace body, and can realize the material preparation and processing in various atmospheres such as vacuum, nitrogen, argon, etc. under high-temperature and strong magnetic field conditions, approaching the actual working conditions under extreme external fields more closely, and providing more technical data for the application of strong magnetic fields.

[0059] The structure of the present invention is simple, easy to use and operate, and easy to disassemble. The inner cavity diameter of the superconducting magnet can reach 150 mm, with a large space and a high achievable magnetic field strength, so that the size of the material specimen to be processed can be significantly increased, which is beneficial to various performance tests and assessments of materials in engineering applications, and thus the types of processed materials are increased.

[0060] Among them, the structure of the superconducting magnet 4 is the same as the prior art. The position 350 mm below the upper surface of the superconducting magnet is the position of the uniform magnetic field, where the magnetic field gradient is 0 T 2 / m, and the highest uniform magnetic field strength reaches 10 T. The position 250 mm below the upper surface of the superconducting magnet is the position where the magnetic field gradient is the largest, and the gradient magnetic field at this position reaches up to 75 T2 / m. As shown in the appendix Figure 14 as follows

[0061] As Figure 10 shown, the heating element 7 is a resistance heating element made of high-purity graphite, in the shape of a shell, with vertical grooves 701 spaced on the heating element 7; the openings of the vertical grooves 701 penetrate the lower end surface of the heating element 7, and threaded holes 702 are symmetrically distributed on both sides of the lower end surface of the heating element for connecting the connecting conductor 13 to generate heat. Compared with ordinary induction coil heating, this heating element can, firstly, eliminate the influence of eddy currents generated by induction coil heating, and secondly, the heating temperature can reach up to 2000°C. Compared with the existing heating element structure, it can reduce the volume of the heating element, simplify the structure, improve the heating efficiency, and extend the service life of the heating element.

[0062] The main control cabinet 26 and the computer 27 together constitute the control system of the magnetic field material processing device. The interfaces of the main control cabinet 26 are respectively connected to the interfaces of the computer 27. An LCD panel is built into the main control cabinet, which plays the role of sending commands and displaying data, and transmits the data to the computer 27 in real time for subsequent analysis operations.

[0063] The main control cabinet 26 is connected to the external control interface of the heating power supply 24 through a conversion interface. Set the temperature values of the sample in each stage of heating, heat preservation, and cooling, and send the set temperature values of each stage to the temperature controller 25 through the iTools program.

[0064] Measure the experimental parameters of the sample 8 located in the test tube 5 in the three stages of heating, heat preservation, and cooling in real time, and send the real-time temperature data measured by the thermocouple 14 at the bottom of the test tube 5 in real time to the temperature controller 25. The temperature controller 25 compares the received real-time temperature with the set temperature: when the real-time temperature is greater than the set temperature, the temperature controller 25 controls the heating power supply 24 to reduce the power to lower the heating temperature; when the real-time temperature is less than the set temperature, the temperature controller 25 controls the heating power supply 24 to increase the power to raise the temperature. Adopt PID three-stage regulation to achieve precise temperature control through the feedback regulation.

[0065] As Figure 2 and 3As shown, in some embodiments, a test tube clamp 20 and an infrared probe 19 are provided inside a vacuum furnace body 17, and an electronic precision balance 18 is provided above the vacuum furnace body 17; when measuring the magnetic susceptibility of the balance, the top end of the test tube clamp 20 is connected to the electronic precision balance 18, and the bottom end of the test tube clamp 20 is connected to the test tube 5 through a nylon bolt, so that the test tube 5 is freely suspended, thereby obtaining the change in the total mass of the test tube clamp 20, the test tube 5, and the sample 8 located at the bottom inside the test tube 5 through the electronic precision balance 18; the infrared probe 19 and the precision electronic balance 18 are connected to the total control cabinet 26 through wires and conversion interfaces, so as to display the changes in the detected real-time temperature and the mass of the balance weighing object.

[0066] The infrared probe 19, the test tube clamp 20, and the electronic precision balance 18 constitute the balance magnetic susceptibility measurement system in the present invention. The maximum mass range of the balance in this balance magnetic susceptibility measurement system is 650 g. This system can realize in-situ measurement of the magnetic susceptibility of substances in the temperature range of 0 to 2000 °C under a gradient magnetic field, and can realize in-situ measurement of the density of substances in the temperature range of 0 to 2000 °C under a uniform magnetic field. Experiments and test analysis can be integrated, fully reflecting the versatility of this device.

[0067] When measuring the magnetic susceptibility of the balance, the top end of the test tube clamp 20 is connected to the electronic precision balance 18, and the bottom end of the test tube clamp 20 is connected to the test tube 5 through a nylon bolt, so that the test tube is freely suspended, thereby obtaining the change in the total mass of the test tube clamp, the test tube, and the sample located at the bottom inside the quartz tube through the top balance. The infrared probe 19 and the precision electronic balance 18 are connected to the total control cabinet 26 through wires and conversion interfaces, and the changes in the detected real-time temperature and the balance mass are synchronously displayed through the LabVIEW program. For materials with phases having large magnetic differences, when the material is in a gradient magnetic field, the specimen 8 will be subjected to a magnetization force applied by the gradient magnetic field, and the direction is downward along the axis, thereby causing a change in the mass displayed by the precision electronic balance. Through the formula F Z =(χ / 2μ0) · V · (BdB / dZ)=mM · (dB / dZ) to obtain the change in magnetic susceptibility, and characterize the phase transition of the material at the real-time temperature position where the magnetic susceptibility undergoes a sudden change according to the characteristics of large magnetic differences between different phases, where χ is the magnetic susceptibility of the specimen to be tested; M is the magnetization intensity per unit mass of the specimen to be tested; V and m are the volume and mass of the specimen to be tested respectively; F Z is the sum of the magnetic force exerted on the specimen 8 in the magnetic field and the gravity of the test tube + specimen + test tube clamp.

[0068] Preferably, as Figure 5As shown, a set of infrared probes 19 are symmetrically arranged and are respectively used for infrared detection in different low-temperature and high-temperature sections. First mounting cavities 1702 are provided on both side walls of the vacuum furnace body 17. A lateral driving mechanism 31 is connected to the outside of the first mounting cavity 1702. The lateral driving mechanism 31 is used to move the corresponding infrared probe 19 into or out of the vacuum furnace body 17 to realize the infrared probe penetration operation in different low-temperature and high-temperature sections. In addition, the lateral driving mechanism 31 can also adjust the position of the infrared probe 19 during the experiment so that the infrared light emitted by the probe can irradiate the specimen 8 at the inner bottom of the test tube 5. The temperature of the specimen 8 is monitored in real time through the Infrawin program. When it is necessary to accurately detect the specimen temperature in real time, start the infrared probe to obtain the accurate temperature of the specimen; The lateral driving mechanism 31 includes a bracket 3101 fixed on the first mounting cavity 1702, a screw rod 3102 rotatably connected to the bracket 3101, and a screw seat 3103 threadedly connected to the screw rod 3102. The outer extension rod of the infrared probe 19 is fixedly installed on the screw seat 3103. Limiting slide rods are also slidably connected to both sides of the screw seat 3103. The infrared probe 19 can be sent into the furnace body and its position can be adjusted by screwing the screw rod 3102.

[0069] In some embodiments, as Figure 4 shown, two windows 1701 are also installed on the vacuum furnace body 17 at the same time. Their viewing angles are corresponding to the positions of the infrared probe 19 and the electronic precision balance 18, and the alignment of the infrared thermometer and the normality of the measurement process of the electronic precision balance can be observed in real time.

[0070] In some embodiments, as Figure 9 shown, the test tube 5 is composed of four parts, which successively include a first section 501, a second section 502, a third section 503, and a fourth section 504 that are threadedly connected to each other from top to bottom; the first section 501 is assembled in the vacuum furnace body 17; the first section 501 and the second section 502 are non-heating body heating areas; the third section 503 and the fourth section 504 are core heating areas, and the disassembly and assembly of the third section 503 can realize the material treatment of materials with different intensity gradient magnetic fields; when installing, it is also necessary to ensure that there is a distance of 5 mm to 25 mm between the lower end surface of the test tube and the upper end surface of the thermocouple. The test tube 5 is preferably a quartz tube, and the size of the accommodated specimen can be selected from 5 mm to 30 mm.

[0071] As Figure 8As shown, the first section 501 at the uppermost position of the test tube 5 mainly functions as central calibration and fixation. Its top is connected to the specimen clamp 20, and the test tube fastener 21 at its upper end is in a vertically movable limiting fit with the flange disc 22 in the vacuum furnace body 17. The two ends of the second section 502 are tapped with threads. The upper part can be in threaded fit with the first section 501, the lower part is in fit with the upper threaded part of the third section 503, and the lower threaded part of the third section 503 is in fit with the upper threaded part of the fourth section 504. The crucible containing the sample 8 to be tested is placed at the bottom of the fourth section 504. In the experiment, if the third section 503 is removed and the second and fourth sections are directly connected, the material treatment with the strongest gradient magnetic field can be achieved. Among them, the first and second sections are non-heating body heating areas, and zirconia material is selected as the processing material, while the third and fourth sections are the core heating areas, and graphite material is selected. To prevent the reaction and infiltration of the sample and graphite at the high-temperature stage, the crucible used is made of heat-resistant zirconia material to separate the sample 8 from the graphite tube.

[0072] The above test tube system adopts a uniquely designed four-section structure and is interconnected by threads. Some sections of the structure can be reused multiple times, which is convenient for disassembly and replacement, prolongs the service life of the test tube, and can be flexibly assembled according to actual heating requirements to achieve the length change of the test tube.

[0073] Specifically, the first section 501 is connected to the test tube clamp 20 (the upper frame of the test tube clamp is omitted in some figures) by nylon bolts, and the lower convex surface of the first section 501 contacts the inner wall of the test tube clamp 20 and is inserted vertically downward into the central hole of the flange disc 22.

[0074] In some embodiments, test tubes 5 with different inner diameters (10 - 25 mm) can be selected according to the size of the test tube clamp 20 and the inner diameter (50 mm) of the heating body 7, so the width dimension of the specimen inside can vary within the range of 0 - 25 mm. Since the heating area is completely uniform, the specimen height can vary from 0 to 150 mm (the distance from the bottom of the test tube 5 to the upper end face of the heating body 7).

[0075] In some embodiments, such as Figure 6As shown, the heating furnace body 6 is provided with a first water-cooled interlayer 9. Inside the first water-cooled interlayer 9, a furnace body heat-insulating layer 1201 is provided. The test tube 5, the heating element 7, and the thermocouple 14 are all located inside the furnace body heat-insulating layer 1201, and there is a spacing of 10 - 20 mm between the outer circumferential surface of the heating element 7 and the inner circumferential surface of the furnace body heat-insulating layer 1201. In addition, a test tube heat-insulating layer 1202 is provided outside the test tube 5, and a thermocouple heat-insulating layer 1203 is provided outside the thermocouple 14. The test tube heat-insulating layer 1202 and the thermocouple heat-insulating layer 1203 are both located inside the furnace body heat-insulating layer 1201. The thermocouple heat-insulating layer 1203 can prevent the problem of inaccurate heat transfer of the thermocouple caused by the heat dissipation of the thermocouple 14 during the heat transfer process into the heating furnace body 6. On the other hand, the test tube heat-insulating layer 1202 and the thermocouple heat-insulating layer 1203 can also fix the positions of the thermocouple 14 and the test tube 5.

[0076] Specifically, as Figure 6 and 7 shown, the outer shell of the heating furnace body 6 is a hollow structure, thus forming the first water-cooled interlayer 9. A group of water inlet pipes 603 are symmetrically arranged inside the first water-cooled interlayer 9. The lower ends of the water inlet pipes 603 are higher than the bottom end of the first water-cooled interlayer 9. Two water inlets 601 and two water outlets 602 are provided at the upper end of the outer shell of the heating furnace body 6. The two water inlets 601 are respectively connected to the corresponding side water inlet pipes 603, and the two water outlets 602 are communicated with the inside of the first water-cooled interlayer 9. The water inlets 601 and the water outlets 602 are respectively connected to the water cooler 1. Specifically, the water cooler 1 has two sets of water inlets / water outlets. One set of water inlets / water outlets are respectively connected to the water inlet and the water outlet of the compressor 2 through water pipes, and the other set of water inlets / water outlets are respectively connected to the water inlet 601 and the water outlet 602 through water pipes. The water temperature of this water cooler is 10 - 20 °C, providing a water cycle for the compressor 2 to take away a large amount of heat generated during the operation of cooling the superconducting magnet 4 by the compressor 2; providing a water cycle for the water-cooled layer 9 to take away the heat generated by the heating element 7 to protect the magnet in the low-temperature superconducting state from being damaged.

[0077] In addition, the output end and the input end of the liquid nitrogen cooling pipe orifice of the compressor 2 are respectively connected to the input end and the output end of the liquid nitrogen cooling pipe orifice of the superconducting magnet 4 through liquid helium pipes. The positive pole and the negative pole of the excitation power supply 3 are respectively connected to the positive pole and the negative pole of the superconducting magnet 4 through wires. When the superconducting magnet 4 works, after the superconducting magnet 4 is cooled to below the liquid nitrogen temperature by the compressor 2, the excitation power supply 3 is turned on to provide voltage and current to the coil of the superconducting magnet 4 to reach the required magnetic field strength.

[0078] In some embodiments, as Figure 12 and 13As shown in the figure, a connecting conductor 13 is arranged inside the heat preservation furnace body 11. The upper end of the connecting conductor 13 extends into the heating furnace body and is connected to the bottom of the heating element 7. Water-cooled heating electrodes 15 are arranged on both sides of the lower end of the heat preservation furnace body 11. The water-cooled heating electrodes 15 extend into the heat preservation furnace body 11 and are connected to the lower end of the connecting conductor 13. A water-cooled groove 1503 is arranged inside the water-cooled heating electrode 15. A cold water pipe 1504 is arranged inside the water-cooled groove 1503. The outer end of the cold water pipe 1504 extends out of the water-cooled heating electrode 15 and is connected with a water inlet pipe 1501. The outer end of the water-cooled heating electrode 15 is connected with a water outlet pipe 1502. The water outlet pipe 1502 is communicated with the inside of the water-cooled groove 1503.

[0079] The setting of the heat preservation furnace body 11 can not only install and connect the water-cooled heating electrode 15 for the heating element 7, but also realize the heat preservation of the thermocouple. More importantly, the original long heating furnace body is divided into the heat preservation furnace body 11 and the heating furnace body in this application. On the one hand, when the components inside the furnace body are damaged, the heat preservation furnace body 11 can be removed separately, making the internal components exposed, and it is better to replace and repair the internal components; on the other hand, the heating furnace body is made more miniaturized, the heating section can be effectively utilized, and the heat loss and life damage outside the effective heating section caused by the increase in the length of the furnace body can be avoided. The corresponding matching design of the heating electrode and the heat preservation furnace body also significantly shortens the length of the heating element 7, avoiding the heat loss and life damage outside the effective heating section. In addition, the water-cooled structure design inside the water-cooled heating electrode 15 can also greatly delay the service life of the water-cooled heating electrode 15.

[0080] Furthermore, as Figure 11 and 12 shown in the figure, a second installation cavity 1105 is arranged on the outer side wall of the heat preservation furnace body 11. The water-cooled heating electrode 15 enters the heat preservation furnace body 11 through the second installation cavity 1105, and the second installation cavity 1105 is connected with the water-cooled heating electrode 15 through a flange; a set of assembly ports 1103 for connecting the connecting conductor 13 and the water-cooled heating electrode 15 are also arranged on the side wall of the heat preservation furnace body 11. The setting of the assembly ports 1103 can facilitate the assembly between the connecting conductor 13 and the water-cooled heating electrode 15.

[0081] Even further, as Figure 11 and 12As shown, the outer shell of the heat-insulating furnace body 11 is a double-layer wall 1101 structure inside and outside, forming a second water-cooling interlayer 1102. A lower connecting flange 1104 is arranged at the bottom of the heat-insulating furnace body 11. A thermocouple fixing plate 16 is connected to the bottom of the lower connecting flange 1104. The thermocouple 14 is fixedly installed on the thermocouple fixing plate 16. A group of symmetrical partition plates 1106 are arranged in the second water-cooling interlayer 1102. The bottom end of the partition plate 1106 is fixed on the lower connecting flange 1104, and the top end is lower than the top end of the second water-cooling interlayer 1102. The two parts of the cavity formed by the second water-cooling interlayer 1102 separated by the partition plate 1106 are respectively connected with water inlet and outlet pipes at the lower ends. The design of the second water-cooling interlayer 1102 can facilitate the cooling of the outer wall of the heat-insulating furnace body 11. The design of the partition plate 1106 therein divides the second water-cooling interlayer 1102 into two cavities, which is convenient to separate the water inlet side and the water outlet side. After the cooling water enters, it first fills one cavity and then overflows to the other cavity and is discharged from the lower side.

[0082] Among them, the bottom end of the thermocouple 14 is fixed by the thermocouple fixing plate 16, and the upper end is fixed by the thermocouple heat-insulating layer 1203, realizing the regional clamping of the thermocouple 14, which is more fixed and reliable, ensuring the accurate measurement of temperature, and avoiding the problem of reduced service life caused by the inclination and deflection of the thermocouple due to the fluctuation of the atmosphere in the high-temperature furnace body.

[0083] In addition, as Figure 3 shown, connection plates 10 are integrally formed at the top end of the heat-insulating furnace body 11 and the bottom end of the heating furnace body 6. The setting of the connection plates 10 can cooperate with bolts to realize the detachable connection between the heat-insulating furnace body 11 and the heating furnace body 6.

[0084] In actual use, the lifting electrode can also be controlled, that is, the connection between the heating furnace body and the heat-insulating furnace body is disconnected, and then through the integrated automation lifting of the vacuum furnace body - heating furnace body, the heating furnace body can be freely moved within a longitudinal stroke of 100 mm. At this time, since the heating element 7 is connected to the heat-insulating furnace body with the connecting conductor 13 (the connecting conductor 13 is preferably a graphite electrode) below it, the heating position at the lower end of the test tube 5 will move along the heating element 7, and there is no need to disassemble the lead wire to manually adjust the heating position, effectively increasing the heating efficiency and the service life of the heating element.

[0085] The above-given embodiments are the better examples to implement the present invention, and the present invention is not limited to the above embodiments. Any non-essential addition or replacement made by those skilled in the art according to the technical features of the technical solution of the present invention belongs to the protection scope of the present invention.

Claims

1. A magnetic field material processing device under variable atmosphere with a temperature up to 2000 °C, characterized in that, Including: Mounting frame (33), vacuum furnace body (17), heating furnace body (6), heat preservation furnace body (11), superconducting magnet (4), test tube (5), heating element (7), thermocouple (14) and mechanical pump (23); The vacuum furnace body (17), the heating furnace body (6) and the heat preservation furnace body (11) are coaxially arranged from top to bottom and detachably connected; when the vacuum furnace body (17) is connected to the heating furnace body (6), material processing under vacuum or protective atmosphere can be realized, and when the vacuum furnace body (17) is not connected to the heating furnace body (6), material processing under atmosphere can be realized; The mechanical pump (23) is externally connected to the vacuum furnace body (17) and is used for performing vacuum pumping operations in the vacuum furnace body (17) and the heating furnace body (6); The superconducting magnet (4) is fixedly installed at the lower part of the mounting frame (33), and the superconducting magnet (4) surrounds the outer periphery of the heating furnace body (6) and can move relatively; A vertical driving device is further arranged on the mounting frame (33), and the vertical driving device can realize the vertical movement of the vacuum furnace body (17) and the heating furnace body (6) along the superconducting magnet (4); a side-end driving device is arranged on the vertical driving device, and when the vacuum furnace body (17) and the heating furnace body (6) are in a disconnected state, the side-end driving device can move the vacuum furnace body (17) to one side of the heating furnace body (6); The upper end of the test tube (5) is installed in the vacuum furnace body (17), and the lower end is inserted into the heating furnace body (6) and extends into the heating element (7); The heating element (7) is arranged in the heating furnace body (6) and is used for heating the sample (8) in the test tube (5); The thermocouple (14) is installed below the heat preservation furnace body (11) and is inserted upward into the heat preservation furnace body (11) and the heating furnace body (6), so that the detection part of the thermocouple (14) is located below the test tube (5) to realize real-time monitoring of the temperature of the sample (8) in the test tube (5), and the real-time temperature is fed back to the temperature controller (25). After comparing the received real-time temperature with the set temperature, the temperature controller (25) controls the heating power supply (24) to realize the regulation of the heating element (7).

2. The variable atmosphere magnetic field material processing device with a temperature up to 2000 °C as claimed in claim 1, characterized in that, The vertical driving device includes a lifting motor (30) and a four-axis lead screw (29); the side-end driving device includes a support plate (32), a guide rail (3201) and a sliding seat (3202); The support plate (32) is arranged above the mounting frame (33). The lifting motor (30) is fixedly installed on the top plate of the mounting frame (33). The four-axis lead screw (29) is connected to the output shaft of the lifting motor (30). The four-axis lead screw (29) is threadedly connected to the support plate (32). The guide rail (3201) is fixedly installed on the support plate (32). The sliding seat (3202) is slidably connected to the guide rail (3201). The sliding seat (3202) is connected to the side mounting plate of the vacuum furnace body (17). Side U-shaped grooves (28) are formed on both the support plate (32) and the top plate of the mounting frame (33). When the vacuum furnace body (17) moves to one side, it moves along the inside of the U-shaped groove (28).

3. The variable atmosphere magnetic field material processing device with a temperature up to 2000 °C as claimed in claim 1, wherein The test tube (5) consists of four parts, including a first section (501), a second section (502), a third section (503), and a fourth section (504) that are threadedly connected to each other from top to bottom. The first section (501) is assembled inside the vacuum furnace body (17). The first section (501) and the second section (502) are non-heating body heating areas. The third section (503) and the fourth section (504) are core heating areas. The disassembly and assembly of the third section (503) can achieve material processing with different intensity gradient magnetic fields.

4. The variable atmosphere magnetic field material processing device with a temperature up to 2000 °C as described in claim 1, characterized in that, The processing materials of the first section (501) and the second section (502) are zirconia materials, and the processing materials of the third section (503) and the fourth section (504) are graphite materials.

5. The variable atmosphere magnetic field material processing device with a temperature up to 2000 °C as described in claim 1, characterized in that, A test tube clamp (20) and an infrared probe (19) are arranged inside the vacuum furnace body (17). An electronic precision balance (18) is arranged above the vacuum furnace body (17). When measuring the magnetic susceptibility of the balance, the top end of the test tube clamp (20) is connected to the electronic precision balance (18), and the bottom end of the test tube clamp (20) is connected to the test tube (5) through a nylon bolt, so that the test tube (5) is freely suspended. Thus, the change in the total mass of the test tube clamp (20), the test tube (5), and the sample (8) at the bottom inside the test tube (5) is obtained through the electronic precision balance (18). The infrared probe (19) and the precision electronic balance (18) are connected to the total control cabinet (26) through wires and conversion interfaces, so as to display the detected real-time temperature and the change in the balance mass.

6. The variable atmosphere magnetic field material processing device with a temperature up to 2000 °C as described in claim 5, characterized in that The infrared probes (19) are a set of symmetrically arranged ones, which are respectively used for different infrared detections in the low-temperature section and the high-temperature section. First mounting cavities (1702) are arranged on both side walls of the vacuum furnace body (17). A lateral driving mechanism (31) is connected to the outside of the first mounting cavity (1702). The lateral driving mechanism (31) is used to move the corresponding infrared probe (19) into or out of the vacuum furnace body (17) to realize the infrared probe penetration work in the low-temperature section and the high-temperature section.

7. The variable atmosphere magnetic field material processing device with a temperature reachable up to 2000 °C as described in claim 1, characterized in that, The heating furnace body (6) is provided with a first water-cooled interlayer (9). Inside the first water-cooled interlayer (9), a furnace body heat preservation layer (1201) is provided. The test tube (5), the heating element (7), and the thermocouple (14) are all located inside the furnace body heat preservation layer (1201). Outside the test tube (5), a test tube heat preservation layer (1202) is provided. Outside the thermocouple (14), a thermocouple heat preservation layer (1203) is provided. Both the test tube heat preservation layer (1202) and the thermocouple heat preservation layer (1203) are located inside the furnace body heat preservation layer (1201).

8. The variable atmosphere magnetic field material processing device with a temperature up to 2000 °C as described in claim 1, characterized in that, A connecting conductor (13) is provided inside the heat preservation furnace body (11). The upper end of the connecting conductor (13) extends into the heating furnace body and is connected to the bottom of the heating element (7). On both sides of the lower end of the heat preservation furnace body (11), water-cooled heating electrodes (15) are provided. The water-cooled heating electrodes (15) extend into the heat preservation furnace body (11) and are connected to the lower end of the connecting conductor (13). Inside the water-cooled heating electrode (15), a water-cooled groove (1503) is provided. Inside the water-cooled groove (1503), a cold water pipe (1504) is provided. The outer end of the cold water pipe (1504) extends out of the water-cooled heating electrode (15) and is connected to a water inlet pipe (1501). The outer end part of the water-cooled heating electrode (15) is connected to a water outlet pipe (1502). The water outlet pipe (1502) is communicated with the inside of the water-cooled groove (1503).

9. The variable atmosphere magnetic field material processing device with a temperature up to 2000 °C as described in claim 8, characterized in that, On the outer side wall of the heat preservation furnace body (11), a second installation cavity (1105) is provided. The water-cooled heating electrode (15) enters the heat preservation furnace body (11) through the second installation cavity (1105). The second installation cavity (1105) and the water-cooled heating electrode (15) are connected by a flange. On the side wall of the heat preservation furnace body (11), a set of assembly openings (1103) for connecting the connecting conductor (13) and the water-cooled heating electrode (15) are also provided.

10. The variable atmosphere magnetic field material processing device with a temperature up to 2000 °C as described in claim 9, characterized in that, The outer shell of the heat preservation furnace body (11) has a double-layer wall (1101) structure inside and outside, forming a second water-cooled interlayer (1102). At the bottom of the heat preservation furnace body (11), a lower connecting flange (1104) is provided. The bottom of the lower connecting flange (1104) is connected to a thermocouple fixing plate (16). The thermocouple (14) is fixedly installed on the thermocouple fixing plate (16). Inside the second water-cooled interlayer (1102), a set of symmetric partitions (1106) are provided. The bottom ends of the partitions (1106) are fixed on the lower connecting flange (1104), and the top ends are lower than the top end of the second water-cooled interlayer (1102). The lower ends of the two part cavities formed by the second water-cooled interlayer (1102) separated by the partitions (1106) are respectively connected with water inlet and outlet pipes.

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