A non-contact high-temperature melt basic physical property measurement device and measurement method

Abstract

The present invention relates to a non-contact high-temperature melt basic physical property measurement device and method, the device includes a temperature control and suspension system, a temperature measurement system, a melt movement and morphology optical measurement system, a fixed-point negative pressure delivery system, and a device frame body platform; the temperature control and suspension system suspends the sample and reaches a preset temperature condition; the temperature measurement system measures the temperature data of the sample; the melt movement and morphology optical measurement system is used for contour imaging of the high-temperature melt, and the density, viscosity coefficient and surface tension coefficient of the sample in the high-temperature melt state are calculated based on the contour imaging; the fixed-point negative pressure delivery system is used to deliver the sample to a predetermined suspension position. The method mainly includes the steps of sample pretreatment, program compilation, system adjustment setting, sample suspension, sample temperature control, excitation loading, sensor measurement, data analysis, sample post-processing, etc. The present invention can measure physical quantities such as high-temperature melt density, viscosity coefficient, surface tension coefficient, etc. through non-contact control and signal acquisition.

Description

Technical Field

[0001] The invention belongs to the field of material research, and in particular relates to a non-contact high-temperature melt basic physical property measuring device. Background Art

[0002] High-temperature melt basic physical property measurement technology is of great significance in the fields of basic material research and nuclear power safety research. In addition, in the production technology fields of steel, metallurgy, petrochemicals, etc., high-temperature melt basic physical property measurement technology can also play a role in determining the physical properties of molten steel and measuring the viscosity change of blast furnace slag.

[0003] The viscosity coefficient of high-temperature fluid is usually measured using the principle of rotation method, and the viscosity of the fluid is determined by measuring the viscous torque of the fluid acting on the rotor or the rotation speed of the rotor. The existing viscometer based on the principle of rotation method mainly includes a testing device and a heating device: the testing device is connected to the rotor, and a crucible is set in the heating device, and the fluid is carried in the crucible. When one or both of the fluid and the rotor immersed therein rotate, the rotor will be affected by the viscous torque of the fluid and change the original speed and torque, so that the viscosity of the fluid can be directly measured by the viscometer (see CN201285366Y, CN201540238Y, CN101685058A). The existing surface tension coefficient can be measured by the cylinder pulling method, and the density parameter can be measured by the Archimedean method (CN105716997).

[0004] The existing rotational viscometer has certain limitations in the hanging wire or torque method measuring device. For example, the hanging wire assembly process is complicated, and the hanging wire position is difficult to coincide with the motor axis, making it difficult to accurately control, resulting in large errors; for example, when the heating device and the test device are close, the temperature range is limited, generally only to about 300°C; for example, when the temperature measurement range is between 100-1000°C, the heating device and the test device are far apart. In order to avoid collision between the rotor and the crucible wall during the test, a large distance must be kept between the rotor and the crucible, thereby limiting the lower limit of the viscosity test (see CN105300842A). The existing pulling tube method for measuring surface tension and the Archimedes method for measuring density both involve certain parts of the device in contact with the high-temperature melt, which is easy to be contaminated and melted (CN105716997). At the same time, temperature monitoring generally uses contact measurement methods such as thermocouples, and it is difficult for temperature-sensitive elements to withstand the corrosion of high temperatures or salt substances for a long time.

[0005] In view of this, the present invention is proposed. Summary of the invention

[0006] The purpose of the present invention is to provide a non-contact high-temperature melt basic physical property measuring device, which can measure physical quantities such as high-temperature melt density, viscosity coefficient, surface tension coefficient, etc. through non-contact control and signal acquisition methods.

[0007] To achieve this purpose, the technical solution of the present invention is as follows:

[0008] A non-contact high-temperature melt basic physical property measurement device, including a temperature adjustment and suspension system, a temperature measurement system, a melt movement and morphology optical measurement system, a fixed-point negative pressure delivery system and a device frame body platform;

[0009] The temperature control and suspension system, temperature measurement system, melt movement and morphology optical measurement system and fixed-point negative pressure delivery system are all installed on the device frame body platform;

[0010] The temperature adjustment and suspension system is used to suspend the sample and keep it in a preset temperature environment;

[0011] The temperature measurement system is used to measure the temperature data of the sample;

[0012] The melt motion and morphology optical measurement system is used to measure the high-temperature melt density, viscosity coefficient and surface tension coefficient of the sample;

[0013] The fixed-point negative pressure delivery system is used to deliver the sample to a predetermined suspension position.

[0014] Furthermore, in the above-mentioned high-temperature melt basic physical property measurement device, the temperature adjustment and suspension system includes a three-axis acoustically stabilized suspension system, a temperature-adjustable inert gas suspension system and a laser heating system;

[0015] The three-axis orthogonal points of the three-axis acoustically stable suspension system coincide with the sample suspension point of the temperature-adjustable inert gas suspension system;

[0016] The horizontal line of the optical path of the laser heating system passes through the sample suspension point and is perpendicular to the outlet gas path of the temperature-adjustable inert gas suspension system.

[0017] Furthermore, in the above-mentioned high-temperature melt basic physical property measurement device, the three-axis acoustic stable suspension system includes three groups of spatially orthogonal and two-to-two opposing acoustic wave transducers; each pair of transducers is orthogonal to each other at the midpoint of the connecting line and is fixed to the device frame body platform at an angle of 45° to the vertical plane.

[0018] Furthermore, in the above-mentioned high-temperature melt basic physical property measuring device, the adjustable temperature inert gas suspension system includes a gas source, a heating structure and a gas heating device body; the gas source is connected to the inlet of the gas heating device body to provide inert gas; the heating structure is arranged in the gas heating device body to adjust the inert gas temperature at the outlet.

[0019] Furthermore, in the above-mentioned high-temperature melt basic physical property measurement device, the laser heating system includes a laser, a light guide arm, an anti-reflection mirror, a circular polarizer, a total reflector and an adjustable converging lens;

[0020] The laser emitted by the laser passes through an anti-reflection mirror, a circular polarizer and a total reflection mirror in the optical guide arm and is focused by a converging lens so that the light spots are projected toward each other onto the sample surface.

[0021] Furthermore, in the above-mentioned high-temperature melt basic physical property measurement device, the temperature measurement system includes two high-precision infrared two-color temperature sensors arranged at a small angle and with adaptive high and low range splicing. The high-precision infrared two-color temperature sensors are used to collect the temperature of the sample surface and are installed obliquely above the sample.

[0022] Furthermore, in the above-mentioned high-temperature melt basic physical property measuring device, the fixed-point negative pressure delivery system includes an automatically retractable negative pressure delivery device;

[0023] The automatic telescopic negative pressure delivery device is a negative pressure rod type device, which can absorb the sample and move the sample to a predetermined suspension position along a specified path, deliver and withdraw after cutting off the negative pressure.

[0024] Furthermore, in the above-mentioned high-temperature melt basic physical property measurement device, the melt movement and morphology optical measurement system includes a laser positioning and sample surface point / line deformation subsystem, an optical image acquisition subsystem and a related data analysis subsystem;

[0025] The laser positioning and sample surface point / line / surface deformation subsystem includes three point / line / surface laser displacement sensors orthogonal to the test planes, which are used to measure the movement trajectory of the sample and the surface deformation of the liquid sample;

[0026] The optical image acquisition subsystem is used to record the periodic / non-periodic morphological changes of the sample.

[0027] The related data analysis subsystem is used to analyze the data of the optical image acquisition subsystem and the laser positioning and sample surface point / line deformation subsystem.

[0028] Furthermore, in the above-mentioned high-temperature melt basic physical property measurement device, the optical image acquisition subsystem includes a high-speed camera, a monochromatic laser lighting device, a narrow-band filter and a macro lens;

[0029] The monochromatic laser lighting device is located on one side of the sample, the laser axis passes through the sample center and remains horizontal with it, and the light spot completely covers the sample; the narrow-band filter, macro lens and high-speed camera are located on the other side of the sample and remain horizontal and coaxial with the sample; the narrow-band filter is mounted on one side of the macro lens and only allows the light emitted by the monochromatic laser lighting device to pass through; the other side of the macro lens is connected to the high-speed camera, and the laser emitted by the monochromatic laser lighting device passes through the sample and is finally captured by the high-speed camera, finally presenting the outline of the sample.

[0030] A method for measuring basic physical properties of high temperature melt using the above device comprises the following steps:

[0031] 1) Sample suspension: Open the inert gas valve of the adjustable temperature inert gas suspension system in the temperature control and suspension system, adjust the gas flow controller to 2-3L / min, run the gas temperature control program to heat the inert gas to above 500°C, use the fixed-point negative pressure delivery system to place the spherical sample 2-3cm above the nozzle to keep it basically balanced in the vertical direction, and start the three-axis acoustic stabilization suspension system in the temperature control and suspension system to keep the spherical sample stable in three-dimensional space;

[0032] 2) Sample temperature control and heating: Turn on the power supply of the laser heating system and the cooling system of the supporting equipment in the temperature control and suspension system, adjust the distance between the two sets of converging lenses and the sample so that the diameter of the laser spot projected onto the surface of the spherical sample is 3-6mm, run the laser power control input card program, heat and melt the sample according to the predetermined program, and keep it at the temperature to be measured;

[0033] 3) Excitation loading: During the sample density measurement process, no excitation loading is required; during the surface tension measurement process, one pair of transducers in the three-axis acoustic stable suspension system is controlled, and a series of sine waves are loaded on the basis of the original stable suspension control waveform, and the frequency scanning range, frequency step, scanning speed and amplitude value are set (such as setting the frequency scanning range to 100-300Hz, the frequency step to 1Hz, and the dwell time at each frequency to 2s) to make the sample surface stimulated to oscillate until resonance occurs and reaches the maximum amplitude; during the viscosity coefficient measurement process, the sample surface is excited to resonate as above, and the excitation signal loading is stopped after 10-20s, so that the sample surface is damped and vibrated until it recovers stability;

[0034] 4) Measurements by various sensors: During the experiment, the temperature measurement system continuously monitors the temperature data of the sample in real time and provides feedback signals to the laser heating system. The high-speed camera continuously records the contour changes of the sample in real time. The melt movement and morphology optical measurement system continuously monitors the position of the sample in real time and records the changes in the surface contour and compares them with the high-speed camera data.

[0035] Furthermore, the above method for measuring the basic physical properties of high temperature melt also includes a preparation step before the measurement experiment, which is as follows:

[0036] Sample pretreatment: weigh the powders of each component of the sample according to the stoichiometric ratio, weigh the powders after uniform mixing, press them into spheres with a diameter of 4-8 mm, sinter them at a high temperature of 900-1500℃ to make the porosity of the sample reach 5-15%, weigh the spherical samples, and record the mass of each sample;

[0037] Laser power output control program compilation: edit the laser power control input card, set the initial output control parameters, process temperature control curve and corresponding duration; the laser power control input card takes effect when the laser is heating the sample. Its heating power and time make the sample heat up and melt at the expected speed. When the temperature required for the experiment is reached, this program is coupled with the pyrometer to obtain the real-time temperature of the sample, which is convenient for fine adjustment of the laser power, so that the temperature of the sample is stabilized at the set temperature;

[0038] Adjustment and setting of high-temperature imaging system: prepare a standard steel ball with a diameter of 2 mm to calibrate the pixels of the high-speed camera, adjust the relative positions of the high-speed camera, macro lens, background laser and sample to focus the image and make the spherical sample occupy 1 / 2-2 / 3 of the field of view, and set the frame rate of the high-speed camera to 800-1500 Hz.

[0039] Furthermore, the above method for measuring the basic physical properties of high temperature melt further includes a post-measurement experiment processing step, which is as follows:

[0040] Data analysis: After all experimental data are transferred to the hard disk, the photos taken are analyzed and data fitted to obtain the semi-major axis, angle and position information of the ellipse corresponding to each frame of the picture. Then, the density, surface tension and viscosity of the tested sample are obtained according to the algorithm and a database is compiled;

[0041] Sample post-processing: After the experiment, samples are stored centrally. If toxic or hazardous substances are present, they must be packaged separately and labeled with warnings. If national controlled materials are involved, they must be weighed after the experiment, and detailed records must be kept for standardized storage.

[0042] The beneficial effects of the present invention are:

[0043] 1. The high-temperature melt basic physical property measuring device of the present invention can measure physical quantities such as high-temperature melt density, viscosity coefficient, surface tension coefficient, etc. through non-contact control and signal acquisition methods.

[0044] 2. The laser heating technology can make the measured material reach above 3000℃, with a wide measurable temperature range. The laser heating design that covers the surface of the spherical sample in opposite directions can make the sample heated more evenly;

[0045] 3. Use acoustically assisted gas suspension to suspend the sample in space to achieve the purpose of non-contact;

[0046] 4. The temperature measurement method adopts high-precision infrared two-color sensor. The overall temperature measurement range of the two ranges can be 1000-3500℃, and it can ensure an accuracy of 0.25% in the relatively low temperature section and 0.5% in the high temperature section. It has a more flexible and reliable accuracy configuration than the general single-range sensor, and it is far beyond the temperature range that can be measured by thermocouples. It is a non-contact measurement, which can effectively avoid high temperature damage to the temperature measuring element;

[0047] 5. The measurement principle is classic and clear. The surface displacement signal analysis method is used to obtain the resonance frequency of the sample when it is deformed by external excitation and the attenuation factor of deformation recovery after the excitation is removed to deduce the surface tension coefficient and viscosity coefficient of the melt sample at a certain temperature. The Young-Laplace curve of the sample under a small deformation due to gravity is obtained through image analysis, and the density of the melt sample is derived from it.

[0048] 6. The present invention has no restrictions on materials, and the heating efficiency is higher than that of conventional electric heating and electromagnetic induction heating. The non-contact measurement can well avoid interference with the sample and contamination and melting of sensitive components. The device can measure multiple physical parameters and has good integration. BRIEF DESCRIPTION OF THE DRAWINGS

[0049] Figure 1 It is a structural diagram of an exemplary high-temperature melt basic physical property measurement device of the present invention.

[0050] Figure 2 The figure is a schematic diagram of the structure of the laser heating system in the high-temperature melt basic physical property measurement device of the present invention.

[0051] Figure 3 The figure is a schematic structural cross-sectional diagram of an exemplary temperature-adjustable inert gas suspension system in a high-temperature melt basic physical property measurement device of the present invention.

[0052] Figure 4 It is a schematic diagram of the structure of the optical image acquisition subsystem in the high-temperature melt basic physical property measurement device of the present invention.

[0053] In the above drawings, 01, laser; 02, laser; 03, acoustic transducer; 04, acoustic transducer; 05, acoustic transducer; 06, acoustic transducer; 07, acoustic transducer; 08, acoustic transducer; 09, adjustable temperature inert gas suspension system; 10, temperature measurement system; 11-14, melt movement and morphology optical measurement system; 15, fixed-point negative pressure delivery system; 16, sample; 17, converging lens; 18, converging Lens; 19. Totally reflective mirror; 20. Totally reflective mirror; 21. Anti-reflective mirror; 22. Anti-reflective mirror; 23. Circular polarizer; 24. Circular polarizer; 25. Laser; 26. Laser; 27. Gas heating device body; 28. Inlet; 29. ​​Outlet; 30. Heating rod; 31. Heating rod; 32. Heating rod; 33. Heating rod; 34. Monochromatic laser lighting equipment; 35. Narrow-band filter; 36. Macro lens; 37. High-speed camera. DETAILED DESCRIPTION

[0054] The specific implementation of the present invention is further described below in conjunction with the accompanying drawings.

[0055] like Figure 1 As shown, the high-temperature melt basic physical property measuring device of the present invention includes a temperature control and suspension system, a temperature measurement system, a melt movement and morphology optical measurement system, a fixed-point negative pressure delivery system and a device frame body platform; the temperature control and suspension system, the temperature measurement system, the melt movement and morphology optical measurement system and the fixed-point negative pressure delivery system are all installed on the device frame body platform; the temperature control and suspension system is used to suspend the sample and place it in a preset temperature environment; the temperature measurement system is used to measure the temperature data of the sample; the melt movement and morphology optical measurement system is used to measure the high-temperature melt density, viscosity coefficient and surface tension coefficient of the sample; the fixed-point negative pressure delivery system is used to deliver the sample to a predetermined suspension position.

[0056] The high-temperature melt basic physical property measuring device of the present invention suspends the sample through a suspension system to achieve the purpose of non-contact, can avoid the influence between the hanging wire and the motor in the prior art, can greatly improve the control accuracy, and can effectively reduce errors.

[0057] The temperature control and suspension system includes a three-axis acoustically stable suspension system, a temperature-adjustable inert gas suspension system and a laser heating system; the three-axis orthogonal point of the three-axis acoustically stable suspension system coincides with the sample suspension point of the temperature-adjustable inert gas suspension system; the horizontal optical path line of the laser heating system passes through the sample suspension point and is perpendicular to the outlet gas path of the temperature-adjustable inert gas suspension system. In one embodiment of the present invention, the three-axis acoustically stable suspension system and the temperature-adjustable inert gas suspension system 09 are three-dimensionally intersected, the three-axis orthogonal point of the former coincides with the sample 16 suspension point of the latter, the horizontal line of any pair of transducers of the former is at an angle of 45° with the vertical or horizontal line, and the inert gas of the latter is ejected from the vertical direction from bottom to top; the horizontal optical path line of the laser heating system passes through the sample 16 and is perpendicular to the temperature-adjustable inert gas suspension system 09; the melt movement and morphology optical measurement system 11-14 is horizontally placed on one side of the sample 16 and is perpendicular to the temperature-adjustable inert gas suspension system 09.

[0058] like Figure 2 As shown, the laser heating system includes two lasers (25, 26), a light guide arm and two groups of circular polarizers (23, 24), two groups of anti-reflection mirrors (21, 22), two groups of 90-degree full-reflection mirrors (19, 20), and two groups of adjustable convergent lenses (17, 18), which can heat the sample 16 to a molten state, and the maximum temperature can reach above 3000°C. In the embodiment of the present invention, the laser is a continuous or pulsed laser, with a spot diameter of 3-10mm and a parallel light, a power of 50-400W, and the light outlets are all vertically upward; the light guide arm is a right-angled hollow cylinder with a diameter of 3-6cm, and a full-reflection mirror (19, 20) is installed at the right angle, and the length of the light guide arm can be adjusted within a certain range; the adjustable convergent lens (17, 18) is a convex lens with a focal length of 10-30mm, and the position of the lens can be adjusted within a certain range, so that the spot of the laser (01, 02) is projected onto the surface of the sample 16. The present invention utilizes laser heating technology to make the measured material reach above 3000°C, and the measurable temperature range is wide.

[0059] The fixed-point negative pressure delivery system includes an automatically retractable negative pressure delivery device 15; the sample 16 in this embodiment is spherical, with a diameter of 2-5mm, and a density of no more than 10000kg / m 3 The automatic telescopic negative pressure delivery device 15 is a negative pressure rod type device, which can absorb the spherical sample 16, move the sample to the sample suspension point along a specified path, deliver and withdraw after cutting off the negative pressure.

[0060] In this embodiment, the three-axis acoustically stable suspension system includes three groups of spatially orthogonal and two-to-two opposite acoustic transducers (03, 04, 05, 06, 07, 08), which can achieve a diameter of 2-5 mm and a density of 0-10000 kg / m 3The spatial stable suspension of any material and the application of liquid deformation force, the distance between each pair of acoustic transducers is 10-20cm, the operating frequency is 2-3WHz, the sound pressure level is 100-150dB, the bandwidth is 20-50Hz, and the modulation signal of 0-200Hz can be input; each pair of transducers are orthogonal to each other at the midpoint of the connecting line and are fixed to the device frame body platform at an angle of 45° with the vertical plane.

[0061] The temperature-adjustable inert gas suspension system 09 includes a gas source, a heating structure (30, 31, 32, 33) and a gas heating device body 27; the gas source is connected to the inlet 28 of the gas heating device body 27 to provide inert gas; the heating structure (30, 31, 32, 33) is arranged in the gas heating device body 27 to adjust the inert gas temperature at the outlet 29. The gas source can be a gas cylinder, which is connected to the gas heating device body 27 through a gas flow pipeline and is provided with a pressure gauge, a pressure reducing valve and a gas flow meter. In this embodiment, the gas outlet 29 of the gas heating device body 27 has a flow rate of 10-30 m / s, a gas temperature range of 300-600°C, and an inner diameter of the gas outlet 29 of 2-8 mm.

[0062] In one embodiment of the present invention, the gas cylinder is a pressure-resistant container that can withstand 8-15 MPa, and the gas inside can be an inert gas such as nitrogen or argon;

[0063] The gas heater adopts a ceramic electric heating method. Accordingly, the heating structure (26, 27, 28, 29) is a ceramic electric heating tube. The length of the heating straight tube section is 30-100 mm, the inner diameter is 6-12 mm, the power is 100-200 W, the thermal efficiency is more than 90%, and the ceramic material is Al 2 O 3 Or SiC, etc. In addition, the gas heating device body 23 may also be provided with a gas thermometer to monitor the outlet gas temperature.

[0064] The high-temperature melt temperature measurement system 10 includes two high-precision infrared two-color sensors and their controllers arranged at a small angle and with adaptive range splicing. The temperature measurement range is 1000-3500℃, the accuracy is 0.25-0.5%, the spot diameter is 0.8-2mm, and the working distance is 120-250mm. It is set up obliquely above the sample 16 and does not interfere with all the above systems; the high-precision infrared two-color sensor is used to collect the temperature of the surface of the sample 16. The system is equipped with a visible laser spot and a video display, and an acquisition card is used for temperature measurement position adjustment and operation process monitoring. The present invention uses a high-precision infrared two-color sensor, the range can be 1000-3500℃, which is far beyond the temperature range that can be measured by thermocouples, and it is a non-contact measurement, which can effectively avoid high-temperature damage to the temperature measuring element.

[0065] The melt movement and morphology optical measurement system 11-14 includes a laser positioning and sample surface point / line deformation subsystem, an optical image acquisition subsystem and a related data analysis subsystem; the laser positioning and sample surface point / line deformation subsystem includes three point / line laser displacement sensors orthogonal to the test planes, the measurement target is the above-mentioned spherical sample 16, and the measured physical quantities are the movement trajectory of the sample 16 and the surface deformation of the liquid sample 16;

[0066] The sample surface point / line deformation subsystem and the three-axis acoustic stable suspension system are set up on the platform of the device frame body at a certain spatial angle without interfering with each other, and the spherical sample 16 is taken as the center point;

[0067] The working distance of the laser displacement sensor is 50-300mm, and the sampling frequency is adjustable within 100-10KHz as required;

[0068] like Figure 4 As shown, the optical image acquisition subsystem includes a high-speed camera 37, a monochromatic laser lighting device 34, a narrow-band filter 35 and a macro lens 36; the monochromatic laser lighting device 34 is located on one side of the sample 16, the laser axis passes through the sample sphere center and keeps it horizontal, and the light spot completely covers the sample, the narrow-band filter 35, the macro lens 36 and the high-speed camera 37 are located on the other side of the sample 16 and keep it horizontal and coaxial with the sample 16, the narrow-band filter 35 is set on one side of the macro lens 36, and only allows the light emitted by the monochromatic laser lighting device 34 to pass through, the other side of the macro lens 36 is connected to the high-speed camera 37, the high-speed camera 37 is set on the horizontal side 20-40cm away from the sample, the sample 16 is located in the center of the visible field of view, and occupies 1 / 2-1 / 4 of the field of view, and the image acquisition frequency is sufficient to record the periodic / non-periodic morphological changes of the sample 16 under the joint action of the laser heating system 01-02, the three-axis acoustically stable suspension system 03-08 and the adjustable temperature inert gas suspension system 09;

[0069] The laser emitted by the monochromatic laser illumination device passes through the sample and is finally captured by the high-speed camera, thereby finally presenting the outline of the sample;

[0070] A narrow-band filter is mounted in front of the high-speed camera lens, and only allows the light emitted by the monochromatic laser lighting device to pass through;

[0071] The relevant data analysis subsystem includes laser displacement data analysis program and optical image analysis program.

[0072] The device frame body platform includes the main equipment position and height adjustment frame, the inert gas emission angle adjustment frame, the supporting hydropower equipment integration frame and the signal acquisition and control equipment integration frame, which are used for the installation and positioning of each system.

[0073] The method for measuring the basic physical properties of high-temperature melts using the device provided in the above embodiment mainly includes pre-experimental preparation, experimental process and post-experimental processing, specifically involving sample pretreatment, laser power output control program compilation, high-temperature imaging system adjustment and setting, sample suspension, sample temperature control and heating, excitation loading, sensor measurement, data analysis, sample post-processing and other steps.

[0074] The preparation steps before the measurement experiment mainly include the following:

[0075] Sample pretreatment: weigh the powders of each component of the sample according to the stoichiometric ratio, weigh the powders after uniform mixing, press them into spheres with a diameter of 4-8 mm, sinter them at a high temperature of 900-1500℃ to make the porosity of the sample reach 5-15%, weigh the spherical samples, and record the mass of each sample;

[0076] Laser power output control program compilation: edit the laser power control input card, set the initial output control parameters, process temperature control curve and corresponding duration. The laser power control input card takes effect when the laser is heating the sample. Its heating power and time make the sample heat up and melt at the expected speed. When the temperature required for the experiment is reached, this program is coupled with the pyrometer to obtain the real-time temperature of the sample, which is convenient for fine adjustment of the laser power, so that the temperature of the sample is stabilized at the set temperature;

[0077] Adjustment and setting of high-temperature imaging system: prepare a standard steel ball with a diameter of 2 mm to calibrate the pixels of the high-speed camera, adjust the relative positions of the high-speed camera, macro lens, background laser and sample to focus the image and make the spherical sample occupy 1 / 2-2 / 3 of the field of view, and set the frame rate of the high-speed camera to 800-1500 Hz.

[0078] The specific measurement experiment process includes the following steps:

[0079] 1) Sample suspension: Open the inert gas valve of the adjustable temperature inert gas suspension system, adjust the gas flow controller to 2-3L / min, run the gas temperature control program to heat the inert gas to above 500°C, use the fixed-point negative pressure delivery system to place the spherical sample 2-3cm above the nozzle to keep it basically balanced in the vertical direction, and start the three-axis acoustic stabilization suspension system to keep the spherical sample stable in three-dimensional space;

[0080] 2) Sample temperature control and heating: Turn on the power of the laser heating system and the cooling system of the supporting equipment, adjust the distance between the two sets of converging lenses and the sample so that the diameter of the laser spot projected onto the surface of the spherical sample is 3-6mm, run the laser power control input card program, heat and melt the sample according to the predetermined program, and keep it at the temperature to be measured;

[0081] 3) Excitation loading: During the sample density measurement process, no excitation loading is required; during the surface tension measurement process, one pair of transducers in the three-axis acoustic stable suspension system is controlled, and a series of sine waves are loaded on the basis of the original stable suspension control waveform, and the frequency scanning range, frequency step, scanning speed and amplitude value are set (such as setting the frequency scanning range to 100-300Hz, the frequency step to 1Hz, and the dwell time at each frequency to 2s) to make the sample surface stimulated to oscillate until resonance occurs and reaches the maximum amplitude; during the viscosity coefficient measurement process, the sample surface is excited to resonate as above, and the excitation signal loading is stopped after 10-20s, so that the sample surface is damped and vibrated until it recovers stability;

[0082] 4) Measurements of various sensors: During the experiment, the two-color pyrometer continuously monitors the temperature data of the sample in real time and provides feedback signals to the laser heating system. The high-speed camera continuously records the contour changes of the sample in real time. The laser positioning system continuously monitors the position of the sample in real time and records the changes in the surface contour for comparison and verification with the high-speed camera data.

[0083] The post-processing steps of the measurement experiment mainly include the following:

[0084] Data analysis: After all experimental data are transferred to the hard disk, the photos taken are analyzed and data fitted to obtain the semi-major axis, angle and position information of the ellipse corresponding to each frame of the picture. Then, the density, surface tension and viscosity of the tested sample are obtained according to the algorithm and a database is compiled;

[0085] Sample post-processing: After the experiment, samples are stored centrally. If toxic or hazardous substances are present, they must be packaged separately and labeled with warnings. If national controlled materials are involved, they must be weighed after the experiment, and detailed records must be kept for standardized storage.

[0086] Obviously, those skilled in the art can make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if these modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include these changes and variations. The above-mentioned embodiments are merely illustrative of the present invention, and the present invention may also be implemented in other specific ways or other specific forms without departing from the gist or essential features of the present invention. Therefore, the described embodiments should be considered illustrative rather than restrictive in any respect. The scope of the present invention shall be described by the appended claims, and any changes equivalent to the intent and scope of the claims shall also be included within the scope of the present invention.

Claims

1. A non-contact high-temperature melt basic physical property measurement device, characterized in that: It includes temperature control and suspension system, temperature measurement system, melt movement and morphology optical measurement system, fixed-point negative pressure delivery system and device frame platform; The temperature control and suspension system, temperature measurement system, melt movement and morphology optical measurement system and fixed-point negative pressure delivery system are all installed on the device frame body platform; The temperature adjustment and suspension system is used to suspend the sample and reach a preset temperature condition; The temperature measurement system is used to measure the temperature data of the sample; The melt motion and morphology optical measurement system is used for contour imaging of high-temperature melts, and based on this, the density, viscosity coefficient and surface tension coefficient of the sample in the high-temperature melt state are deduced; The fixed-point negative pressure delivery system is used to deliver the sample to a predetermined suspension position; The temperature control and suspension system includes a three-axis acoustically stable suspension system, a temperature-adjustable inert gas suspension system and a laser heating system; The three-axis orthogonal points of the three-axis acoustically stable suspension system coincide with the sample suspension points of the temperature-adjustable inert gas suspension system; the three-axis acoustically stable suspension system includes three groups of spatially orthogonal and two-to-two opposing acoustic wave transducers, each pair of transducers is orthogonal to each other at the midpoint of the connecting line, and is fixed to the device frame body platform at an angle of 45° to the vertical plane, achieving a diameter of 2-5mm and a density of 0-10000kg / m 3 The invention relates to a spatially stable suspension of any material and the application of liquid deformation force; the temperature-adjustable inert gas suspension system comprises a gas source, a heating structure and a gas heating device body; the gas source is connected to the inlet of the gas heating device body to provide inert gas; the heating structure is arranged in the gas heating device body to adjust the inert gas temperature at the outlet; The horizontal line of the optical path of the laser heating system passes through the sample suspension point and is perpendicular to the outlet gas path of the temperature-adjustable inert gas suspension system; The melt movement and morphology optical measurement system includes a laser positioning and sample surface point / line deformation subsystem, an optical image acquisition subsystem and a related data analysis subsystem; the laser positioning and sample surface point / line deformation subsystem includes three point / line laser displacement sensors orthogonal to the test planes, which are used to measure the movement trajectory of the sample and the surface deformation of the liquid sample; The optical image acquisition subsystem is used to record the periodic / non-periodic morphological changes of the sample; the related data analysis subsystem is used to analyze the data of the optical image acquisition subsystem and the laser positioning and sample surface point / line deformation subsystem.

2. The measuring device according to claim 1, characterized in that: The laser heating system comprises a laser, a light guide arm, an anti-reflection mirror, a circular polarizer, a total reflection mirror and an adjustable converging lens; The laser emitted by the laser passes through an anti-reflection mirror, a circular polarizer and a total reflection mirror in the optical guide arm and is focused by a converging lens so that the light spots are projected toward each other onto the sample surface.

3. The high temperature melt basic physical property measuring device according to claim 1, characterized in that: The temperature measurement system includes two high-precision infrared two-color temperature sensors arranged at a small angle and with adaptive high and low range splicing. The high-precision infrared two-color temperature sensors are used to collect the temperature of the sample surface and are installed obliquely above the sample.

4. The high temperature melt basic physical property measuring device according to claim 1, characterized in that: The fixed-point negative pressure delivery system includes an automatically retractable negative pressure delivery device; The automatic telescopic negative pressure delivery device is a negative pressure rod type device, which can absorb the sample and move the sample to a predetermined suspension position along a specified path, deliver and withdraw after cutting off the negative pressure.

5. The high temperature melt basic physical property measuring device according to claim 1, characterized in that: The optical image acquisition subsystem includes a high-speed camera, a monochromatic laser lighting device, a narrow-band filter and a macro lens; The monochromatic laser lighting device is located on one side of the sample, the laser axis passes through the sample center and remains horizontal with it, and the light spot completely covers the sample; the narrow-band filter, macro lens and high-speed camera are located on the other side of the sample and remain horizontal and coaxial with the sample; the narrow-band filter is mounted on one side of the macro lens and only allows the light emitted by the monochromatic laser lighting device to pass through; the other side of the macro lens is connected to the high-speed camera, and the laser emitted by the monochromatic laser lighting device passes through the sample and is finally captured by the high-speed camera, finally presenting the outline of the sample.

6. A method for measuring basic physical properties of high temperature melt using the device described in any one of claims 1 to 5, characterized in that: The steps include: 1) Sample suspension: Open the inert gas valve of the adjustable temperature inert gas suspension system in the temperature control and suspension system, adjust the gas flow controller to 2-3L / min, run the gas temperature control program to heat the inert gas to above 500°C, use the fixed-point negative pressure delivery system to place the spherical sample 2-3cm above the nozzle to keep it basically balanced in the vertical direction, and start the three-axis acoustic stabilization suspension system in the temperature control and suspension system to keep the spherical sample stable in three-dimensional space; 2) Sample temperature control and heating: Turn on the power supply of the laser heating system and the cooling system of the supporting equipment in the temperature control and suspension system, adjust the distance between the two sets of converging lenses and the sample so that the diameter of the laser spot projected onto the surface of the spherical sample is 3-6mm, run the laser power control input card program, heat and melt the sample according to the predetermined program, and keep it at the temperature to be measured; 3) Excitation loading: During the sample density measurement process, no excitation loading is required; during the surface tension measurement process, one pair of transducers in the three-axis acoustic stable suspension system is controlled, and a sine wave is loaded on the basis of the original stable suspension control waveform. The frequency scanning range, frequency step, scanning speed and amplitude are set to make the sample surface stimulated to oscillate until resonance occurs and reaches the maximum amplitude; During the viscosity coefficient measurement process, the sample surface is subjected to excitation as described above to make it resonate. After 10-20 seconds, the excitation signal loading is stopped to allow the sample surface to vibrate with damping until it recovers to stability. 4) Measurements by various sensors: During the experiment, the temperature measurement system continuously monitors the temperature data of the sample in real time and provides feedback signals to the laser heating system. The high-speed camera continuously records the contour changes of the sample in real time. The melt movement and morphology optical measurement system continuously monitors the position of the sample in real time and records the changes in the surface contour and compares them with the high-speed camera data.

7. The method for measuring basic physical properties of high temperature melt according to claim 6, characterized in that: It also includes the preparation steps before the measurement experiment, as follows: Sample pretreatment: weigh the powders of each component of the sample according to the stoichiometric ratio, weigh out the powder after uniform stirring, press it into a sphere with a diameter of 4-5mm, sinter it at a high temperature of 900-1500℃ to make the porosity of the sample reach 5-15%, weigh the spherical sample, and record the mass of each sample; Laser power output control program compilation: edit the laser power control input card, set the initial output control parameters, process temperature control curve and corresponding duration; the laser power control input card takes effect when the laser is heating the sample. Its heating power and time make the sample heat up and melt at the expected speed. When the temperature required for the experiment is reached, this program is coupled with the pyrometer to obtain the real-time temperature of the sample, which is convenient for fine adjustment of the laser power, so that the temperature of the sample is stabilized at the set temperature; Adjustment and setting of high-temperature imaging system: prepare a standard steel ball with a diameter of 2 mm to calibrate the pixels of the high-speed camera, adjust the relative positions of the high-speed camera, macro lens, background laser and sample to focus the image and make the spherical sample occupy 1 / 2-2 / 3 of the field of view, and set the frame rate of the high-speed camera to 800-1500 Hz.

8. The method for measuring basic physical properties of a high temperature melt according to claim 6 or 7, characterized in that: It also includes the measurement experiment post-processing steps, which are as follows: Data analysis: After all experimental data are transferred to the hard disk, the photos taken are analyzed and data fitted to obtain the semi-major axis, angle and position information of the ellipse corresponding to each frame of the picture. Then, the density, surface tension and viscosity of the tested sample are obtained according to the algorithm and a database is compiled; Sample post-processing: After the experiment, samples are stored centrally. If toxic or hazardous substances are present, they must be packaged separately and labeled with warnings. If national controlled materials are involved, they must be weighed after the experiment, and detailed records must be kept for standardized storage.

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