A high-temperature melt viscosity measurement method, device and storage medium

Abstract

The present application relates to the technical field of metallurgy, and particularly relates to a high-temperature melt viscosity determination method, device and storage medium, comprising the following steps: vacuumizing a cavity of a viscosity determination equipment, heating a blank crucible to make the crucible heat up to 1450-1600 DEG C and keep warm, the crucible entering a free oscillation state, recording an oscillation period and corresponding logarithmic decay rate average value; cooling the suspension system to below 1350 DEG C; setting a temperature determination point, recording corresponding oscillation data after constant temperature; fitting the collected oscillation period and logarithmic decay rate data, establishing a temperature-oscillation period curve and a temperature-logarithmic decay rate curve; when determining a melt to be measured, repeating the above steps, completing full-process determination and data recording of the melt to be measured, and then performing viscosity determination calculation; the present application constructs a temperature-oscillation parameter dynamic correction relationship, and realizes intelligent adjustment of melt system viscosity determination in a 1200 DEG C to 1600 DEG C interval.

Description

Technical Field

[0001] This invention relates to the field of metallurgical technology, and in particular to a method, apparatus and storage medium for measuring the viscosity of high-temperature melts. Background Technology

[0002] Existing measurement methods generally rely on system reference parameters obtained at room temperature or under fixed conditions (such as the logarithmic decay rate of an empty crucible, oscillation period, etc.), failing to fully consider the dynamic changes of these parameters with temperature in high-temperature environments. Especially in melt systems above 1350℃, ignoring the influence of temperature on system damping characteristics and sample physical properties can easily introduce systematic errors, thereby limiting the accuracy and stability of viscosity measurement results and making it difficult to meet the refined requirements of high-temperature process control and material performance analysis.

[0003] In the prior art, Chinese patent CN105891050B discloses a variable magnetic field high-temperature melt oscillating viscometer and its rapid measurement method, including a central plate, the upper part of which supports a measuring container, and the lower part of which is connected to a heating device; the measuring container is equipped with an oscillation system, which includes a rotating power device, the bottom of which is connected to a measuring rod via a suspension wire, and the bottom of the measuring rod is connected to a sample holding device inside the heating device; the suspension wire is equipped with an optical measurement system for measuring logarithmic decay rate; the heating device is fitted with a magnetic field system with adjustable magnetic field direction and intensity to keep the heating device in a variable magnetic field; however, this patent ignores the influence of temperature on the system damping characteristics and sample physical parameters.

[0004] In the prior art, Chinese patent CN101923032B discloses a device and method for rapidly determining the viscosity of high-temperature melts using a spring oscillator free vibration method. The device includes: a blade oscillator connected to one end of a connecting rod; a spring fitted into the connecting rod to form a single unit; a permanent magnet connected to the other end of the connecting rod; a coil fitted around the outer ring of the permanent magnet; the size of the coil being larger than the outer ring size of the permanent magnet; the coil being connected to a signal amplifier processor; the signal amplifier processor being connected to a computer; and the blade oscillator extending into a crucible. However, this patent does not consider the influence of temperature on the physical properties of the sample, which can easily introduce systematic errors during viscosity determination. Summary of the Invention

[0005] This invention provides a method, apparatus, and storage medium for measuring the viscosity of high-temperature melts. It establishes a dynamic correction relationship between temperature and oscillation parameters, enabling intelligent adjustment of the viscosity measurement of melt systems in the range of 1200℃ to 1600℃. It is particularly suitable for high-temperature metallurgical media such as molten iron and molten steel, effectively avoiding systematic errors, thereby significantly improving the accuracy of viscosity measurement. It has stronger industrial adaptability and meets the refined requirements of viscosity measurement in high-temperature processes.

[0006] To achieve the above objectives, the present invention employs the following technical solution: A method for determining the viscosity of a high-temperature melt includes the following steps: S1. Place the empty crucible in the suspension system inside the viscosity measuring device cavity, and start the vacuum system to evacuate the viscosity measuring device cavity to a vacuum level higher than 10. -5 Pa; S2. Maintain the thermal balance of the suspension system through a cooling medium; S3. Inert gas is introduced into the cavity of the viscosity measuring device as a protective atmosphere, and the pressure inside the crucible is restored to normal. S4. Heat the empty crucible at a rate of 10-20℃ / min until it reaches 1450-1600℃, then hold the temperature for 0.5-1h to ensure the thermal stability of the suspension system. S5. Put the empty crucible into a free oscillation state. At the target temperature, record at least 5 sets of oscillation period and corresponding logarithmic decay rate data continuously through the laser measurement system, and take the average value of each as the oscillation parameter of the empty crucible at that temperature point. S6. Cool the suspension system with a cooling medium at a rate of 10-15℃ / min, gradually cooling it from 1450℃ to 1600℃ to below 1350℃; set a temperature measurement point every 20-50℃, and record the corresponding oscillation data after holding the temperature for 0.5-1h. S7. Fit the collected oscillation period and logarithmic decay rate data to establish the relationship curves between temperature and oscillation period, and between temperature and logarithmic decay rate; S8. When measuring the melt to be tested, place the crucible containing the melt into the suspension system inside the viscosity measuring device cavity, and start the vacuum system to evacuate the viscosity measuring device cavity to a vacuum level higher than 10. -5 Pa, return to execute steps S2 to S7 to complete the full process measurement and data recording of the melt to be tested, and then execute step S9; S9. Viscosity calculation is as follows: ; ; ; Where η is the viscosity of the melt to be tested, Pa·s; I is the moment of inertia of the suspended part, kg·m²; and ρ is the density of the melt to be tested, g·cm³. -3δ is the logarithmic decay rate of the melt to be tested, dimensionless; t is the oscillation period of the melt to be tested, s; ​​δ0(T) is the logarithmic decay rate of the oscillation of the empty crucible at different temperatures, dimensionless; t0(T) is the oscillation period of the empty crucible at different temperatures, s; W is the correction coefficient, dimensionless; a, b, and c are instrument correlation constants, dimensionless; p is the number of horizontal planes in contact with the sample and the crucible, p=1 when the melt is not full; p=2 when the melt is fully filled with the crucible and in contact with the crucible lid, dimensionless; m is the mass of the melt, kg; r is the inner diameter of the crucible, m; h is the height of the melt, m; The damping ratio is dimensionless.

[0007] Furthermore, the cooling medium is cooling water.

[0008] A system for determining the viscosity of high-temperature melts, employing a viscometer; the viscometer includes a laser measurement system and a suspension system. The viscometer is used to heat the sample and provide a controlled atmosphere protection. The laser measurement system includes a laser source, a reflector, an image sensor, and a timing module. The reflector is mounted on a rotating suspension system, and all laser beams emitted by the laser source are reflected onto the reflector. The image sensor is positioned to receive the beam reflected by the reflector, and its signal line is connected to the timing module. The timing module is used to obtain the time difference between the beam received by the image sensor and the time difference, thereby calculating the oscillation period. The suspension system includes a stepper motor, a molybdenum wire, an inertia disk, and a molybdenum rod. The upper end of the molybdenum wire is connected to the output shaft of the stepper motor, and the lower end of the molybdenum wire is connected to a reflector. The reflector is connected to the molybdenum rod, the inertia disk is connected through the molybdenum rod and can rotate, and the crucible is connected to the bottom of the molybdenum rod and can rotate and oscillate.

[0009] Furthermore, the crucible has a double-layer structure, with the outer layer being a graphite-protected crucible connected to a molybdenum rod for rotational suspension and oscillation; the inner layer is a corundum crucible with a lid.

[0010] Furthermore, the inner diameter of the corundum crucible is 30-50 mm.

[0011] Furthermore, the reflector reflects at least three beams.

[0012] A computer-readable storage medium storing a computer program that, when executed by a processor, implements the method for determining the viscosity of a high-temperature melt.

[0013] Compared with the prior art, the beneficial effects of the present invention are: 1) Improve measurement accuracy: By introducing the relationship between oscillation parameters and temperature, the dynamic viscosity of molten metal measured by the oscillating cup viscometer is dynamically corrected, which significantly reduces the systematic error caused by using room temperature constant values, and the viscosity calculation results are closer to the actual value; 2) Adaptable to high-temperature and complex environments: Suitable for melt systems in the range of 1200℃ to 1600℃, especially suitable for high-temperature metallurgical media such as molten iron and molten steel, with stronger industrial adaptability; 3) High testing efficiency: The single-point viscosity measurement time is controlled within 5 minutes, which can quickly obtain the viscosity values ​​at multiple temperature points, making it suitable for dynamic process monitoring and process optimization feedback; 4) Strong repeatability and stability: It exhibits good consistency in results across multiple rounds of sample determination, possesses strong repeatability and experimental controllability, and meets the dual needs of scientific research and industry. 5) The model has strong scalability: the constructed temperature-oscillation period and temperature-logarithmic decay rate relationship curves can be adapted to different material systems and experimental platforms, and have good reusability and scalability. 6) Applicable to multiple scenarios: It can be widely used for viscosity determination of various high-temperature liquid systems such as blast furnace iron, converter steel, continuous casting melt, and glass melt, and has high industrialization value. Attached Figure Description

[0014] Figure 1 This is a schematic diagram of the suspension system described in this invention.

[0015] Figure 2 This is a schematic diagram of the structure of the crucible described in this invention.

[0016] Figure 3 This relates the oscillation period, logarithmic decay rate, and temperature of the empty crucible described in this invention.

[0017] Figure 4 This is the viscosity-temperature relationship curve of the Fe-C binary alloy melt in an embodiment of the present invention.

[0018] Figure 5 This is a comparison chart of the measured viscosity values ​​of the Fe-C binary alloy melt in the embodiments of the present invention with the values ​​in the literature.

[0019] In the diagram: 1. Image sensor; 2. Laser source; 3. Molybdenum wire; 4. Reflector; 5. Inertial disk; 6. Molybdenum rod; 7. Crucible. Detailed Implementation

[0020] The specific embodiments of the present invention will be further described below with reference to the accompanying drawings: This invention discloses a method for determining the viscosity of high-temperature melts, comprising the following steps: S1: Place the empty crucible 7 into the suspension system of the viscometer; S2: Ensure the device is airtight, start the vacuum system, and evacuate the viscometer chamber to a vacuum level higher than 10. -5 Pa; S3: Turn on the cooling medium to maintain system thermal balance; S4: Introduce a high-purity argon protective atmosphere into the viscometer chamber to restore it to normal pressure. S5: Set the heating program to heat up at a rate of 10-20℃ / min; S6: After heating to 1450-1600℃, maintain the temperature for 0.5-1 hour to ensure system thermal stability; S7: Turn on the laser measurement system; S8: Adjust the angle and position of the reflector to ensure that the laser acquisition point is consistent with the preset position; S9: Start the suspension system to allow the empty crucible 7 to enter a free oscillation state. Record 5 sets of oscillation periods and corresponding logarithmic decay rate data continuously at the target temperature, perform statistical processing on them, and take the average value as the oscillation parameter of the empty crucible 7 at that temperature point. S10: Cool down at a rate of 10-15℃ / min, gradually cooling from 1600℃ to 1350℃. 1350℃ is the solidification point of common iron-based alloys. Set a temperature measurement point every 50℃, and record the corresponding oscillation data after holding the temperature for 0.5-1h. S11: Finally, the experimental data of crucible 7 were measured, and the collected oscillation period and logarithmic decay rate data were fitted to establish the relationship curves between temperature and oscillation period, and temperature and logarithmic decay rate. S12. When measuring the melt to be tested, place the crucible containing the melt into the suspension system inside the viscosity measuring device cavity, and start the vacuum system to evacuate the viscosity measuring device cavity to a vacuum level higher than 10. -5 Pa, return to execute steps S2 to S11 to complete the full process measurement and data recording of the melt to be tested, and then execute step S13; S13. Viscosity calculation is as follows: ; ; ; Where η is the viscosity of the melt to be tested, Pa·s; I is the moment of inertia of the suspended part, kg·m²; and ρ is the density of the melt to be tested, g·cm³. -3δ is the logarithmic decay rate of the melt to be tested, dimensionless; t is the oscillation period of the melt to be tested, s; ​​δ0(T) is the logarithmic decay rate of the oscillation of the empty crucible at different temperatures, dimensionless; t0(T) is the oscillation period of the empty crucible at different temperatures, s; W is the correction coefficient, dimensionless; a, b, and c are instrument correlation constants, dimensionless; p is the number of horizontal planes in contact with the sample and the crucible, p=1 when the melt is not full; p=2 when the melt is fully filled with the crucible and in contact with the crucible lid, dimensionless; m is the mass of the melt, kg; r is the inner diameter of the crucible, m; h is the height of the melt, m; The damping ratio is dimensionless.

[0021] This invention utilizes an oscillating cup method for measuring the viscosity of high-temperature melts. By applying minute angular vibrations and measuring the oscillation decay behavior of the system, combined with the classical Shvidkovskiy viscosity calculation formula, a quantitative solution for melt viscosity is achieved. Furthermore, a temperature-oscillation parameter relationship is constructed to intelligently adjust viscosity measurements at different temperatures, avoiding systematic errors and significantly improving the accuracy and adaptability of viscosity measurements, thus meeting the refined viscosity measurement requirements of high-temperature processes.

[0022] The viscosity measurement formula of this invention is based on the oscillation method. In the melt-crucible system, there is a one-to-one correspondence between the oscillation decay characteristics and the fluid damping force, and the damping force is closely related to the viscosity of the melt. By introducing temperature to correct the decay rate and oscillation period of the empty crucible 7, accurate measurement of melt viscosity is achieved under high-temperature conditions. The specific approach includes: The dynamic relationship of the oscillating system is established: the suspended crucible 7 and the melt system are regarded as a damped torsional pendulum system, whose equation of motion includes the moment of inertia I, fluid damping and the inherent restoring force; the degree of oscillation decay can be characterized by the logarithmic decay rate δ, and the speed of oscillation is determined by the period t; the combination of the two can be used to deduce the viscous damping contribution of the fluid to the system.

[0023] Correction for temperature relationship of empty crucible: In actual testing, the empty crucible itself will have differences in thermal expansion, atmosphere disturbance and material damping at different temperatures, which will cause the decay rate δ0 and period t0 to change with temperature. If no correction is made, these deviations can easily be mistaken for the true viscosity effect of the melt. Therefore, the formula of this invention specifically introduces two temperature relationships, δ0(T) and t0(T), as reference benchmarks, so as to automatically eliminate the influence of the crucible itself changing with temperature in the calculation.

[0024] The parameters and geometric factors are reflected in the formula: ρ (melt density) and p (number of contact horizontal surfaces) are included in the formula, which reflect the influence of melt volume filling and flow field distribution on damping force; W, a, b, and c are instrument-related constants obtained through experimental calibration, which are used to match the theoretical model with the characteristics of the actual device. This ensures the universality of the formula of this invention while taking into account the differences of the device.

[0025] Data processing logic: By comparing the differences in oscillation parameters (δ-δ0(T), t-t0(T)) between the sample and the empty crucible, and combining the density and geometric correction coefficient, the viscosity η of the melt to be tested can be directly obtained. This processing method simplifies the complex fluid dynamics calculation, allowing the experimenter to complete the viscosity solution simply by obtaining measurable physical quantities (period, decay rate, density).

[0026] A high-temperature melt viscosity measurement system, employing a viscometer; see [link / reference]. Figure 1 The viscometer is equipped with a laser measurement system and a suspension system; The viscometer is used to heat the sample and provide a controlled atmosphere protection. The laser measurement system includes a laser source 2, a reflector 4, an image sensor 1, and a timing module. The reflector 4 is mounted on a rotating suspension system, and all laser beams emitted by the laser source 2 are reflected onto the reflector 4. The image sensor 1 is positioned to receive the beam reflected by the reflector 4, and is captured by three photosensitive elements (A, B, and O) positioned at different angles. The signal line of the image sensor 1 is connected to the timing module. The timing module is used to obtain the time difference between the beam received by the image sensor 1, thereby calculating the oscillation period, and finally calculating the viscosity value using the method described above. The suspension system enables the oscillation of the sample system and includes a stepper motor, a molybdenum wire 3, an inertial disk 5, and a molybdenum rod 6. The upper end of the molybdenum wire 3 is connected to the output shaft of the stepper motor, and the lower end of the molybdenum wire 3 is connected to a reflector 4. The reflector 4 is connected to the molybdenum rod 6. The inertial disk 5 passes through the molybdenum rod 6 and can rotate. The crucible 7 is connected to the bottom of the molybdenum rod 6 and can rotate and oscillate, ensuring the symmetry and stability of the rotation process.

[0027] See Figure 2 The crucible 7 has a double-layer structure. The outer layer is a graphite-protected crucible connected to a molybdenum rod 6, enabling rotational suspension and oscillation. The inner layer is a covered corundum crucible with an inner diameter of 28 mm, specifically designed to hold samples and ensure physical stability and chemical inertness at high temperatures. The entire system can achieve high vacuum (better than 10⁻⁶) during the experiment. -5 Protect the system with a Pa or an inert atmosphere (such as argon) to prevent oxidation interference.

[0028] When used for viscosity determination of Fe-C binary high-temperature melts, the following steps are included: S1. Sample preparation: Fe-C binary alloy iron samples were prepared by chemically reducing iron powder (AR, purity > 98%) and graphite powder (CP, purity > 99%). The powdered samples were mixed thoroughly and placed in a container with a volume of 400–700 mm². 3 The corundum crucible was placed in the furnace tube of a high-temperature energy-saving tube furnace and heated to above 1550℃ at a heating rate greater than 5℃ / min for a holding time greater than 2 hours. During this time, the sample was stirred using a quartz tube to ensure uniform dissolution. Before cooling, the iron-based melt at high temperature was water-quenched and sampled using a pipette and a quartz tube for subsequent compositional confirmation and analysis. The cooling rate was greater than 5℃ / min, and the sample mass was approximately 10–30 g for subsequent analysis. The entire pre-melting experiment was conducted under a protective atmosphere (such as argon) (gas purity greater than 99.99%, gas filling rate greater than 3 L / min). The pre-melted sample was surface-treated to remove the surface oxide layer and impurities, and the sample mass was recorded using an electronic balance.

[0029] S2. Measurement process: Place the weighed sample into an empty crucible 7 and then place it inside the equipment's suspended crucible 7; after ensuring the equipment is sealed, evacuate the device until the vacuum level reaches 10. -5 Above Pa, argon protective gas is introduced. When the gas pressure inside the furnace returns to atmospheric pressure, the temperature is raised at a rate of 10-15℃ / min. The viscosity is measured during the cooling process, starting from 1450℃. Each temperature is held for 20-30 minutes, and a measurement point is set every 50℃ until solidification. The cooling rate is 10-15℃ / min. Before measurement, the mirror position needs to be adjusted to ensure that the laser acquisition process meets the position requirements of the formula.

[0030] S3, Viscosity Calculation: Based on the curve relationship obtained from the oscillation period and logarithmic decay rate parameters of the crucible containing the sample, the oscillation period and logarithmic decay rate at the corresponding temperature are obtained, and the viscosity value of the Fe-C binary alloy iron sample is obtained according to the formula.

[0031] A computer-readable storage medium storing a computer program that, when executed by a processor, implements the method for determining the viscosity of a high-temperature melt.

[0032] The following embodiments are implemented based on the technical solution of the present invention, providing detailed implementation methods and specific operation processes. However, the scope of protection of the present invention is not limited to the following embodiments. Unless otherwise specified, the methods used in the following embodiments are conventional methods.

[0033] Example: This invention discloses a method for determining the viscosity of high-temperature melts, comprising the following steps: S1: Place the empty crucible 7 into the suspension system of the viscometer; S2: Ensure the apparatus is airtight, activate the vacuum system, and evacuate crucible 7 chamber to a vacuum level higher than 10. -5 Pa; S3: Turn on the cooling medium to maintain system thermal balance; S4: Introduce high-purity argon gas to create a protective atmosphere and restore the pressure to normal. S5: Set the heating program to heat up at a rate of 10-20℃ / min; S6: After heating to 1450-1600℃, maintain the temperature for 0.5-1 hour to ensure system thermal stability; S7: Turn on the laser measurement system; S8: Adjust the angle and position of the reflector to ensure that the laser acquisition point is consistent with the preset position; S9: Start the suspension system to allow the empty crucible 7 to enter a free oscillation state. Record 5 sets of oscillation periods and corresponding logarithmic decay rate data continuously at the target temperature, perform statistical processing on them, and take the average value as the oscillation parameter of the empty crucible 7 at that temperature point. S10: Cool down at a rate of 10-15℃ / min, gradually cooling from 1600℃ to 1350℃. 1350℃ is the solidification point of common iron-based alloys. Set a temperature measurement point every 50℃, and record the corresponding oscillation data after holding the temperature for 0.5-1h. S11: The final experimental data for crucible 7 are shown in Tables 1 and 2. The collected oscillation period and logarithmic decay rate data were fitted to establish the relationship curves between temperature and oscillation period, and between temperature and logarithmic decay rate. (See...) Figure 3 ; S12. When measuring the melt to be tested, place the crucible containing the melt into the suspension system inside the viscosity measuring device cavity, and start the vacuum system to evacuate the viscosity measuring device cavity to a vacuum level higher than 10. -5 Pa, return to execute steps S2 to S11 to complete the full process measurement and data recording of the melt to be tested, and then execute step S13; S13. Viscosity calculation is as follows: ; ; ; Where η is the viscosity of the melt to be tested, Pa·s; I is the moment of inertia of the suspended part, kg·m²; and ρ is the density of the melt to be tested, g·cm³. -3δ is the logarithmic decay rate of the melt to be tested, dimensionless; t is the oscillation period of the melt to be tested, s; ​​δ0(T) is the logarithmic decay rate of the oscillation of the empty crucible at different temperatures, dimensionless; t0(T) is the oscillation period of the empty crucible at different temperatures, s; W is the correction coefficient, dimensionless; a, b, and c are instrument correlation constants, dimensionless; p is the number of horizontal planes in contact with the sample and the crucible, p=1 when the melt is not full; p=2 when the melt is fully filled with the crucible and in contact with the crucible lid, dimensionless; m is the mass of the melt, kg; r is the inner diameter of the crucible, m; h is the height of the melt, m; The damping ratio is dimensionless.

[0034] Table 1 Oscillation period of empty crucible at different temperatures Table 2 Logarithmic decay rate of empty crucible at different temperatures Currently used for viscosity determination of Fe-C binary high-temperature melts, including the following steps: S1. Sample Preparation Process: Iron powder (AR, purity greater than 98%) and graphite powder (CP, purity greater than 99.95%) were reduced using chemical reagents. 200g of experimental Fe-C binary alloy iron samples were prepared according to carbon mass percentages of 3.9wt%, 4.1wt%, 4.3wt%, 4.5wt%, and 4.7wt%. After preparing the iron samples according to the designed composition, the powdered samples were mixed thoroughly and placed in a corundum crucible with a diameter of ϕ30mm × h200mm. The corundum crucible containing the iron samples was then placed in the furnace tube of a high-temperature energy-saving tube furnace, and the temperature was programmed to rise to 1550℃. After reaching the set temperature of 1550℃, the samples were kept at this temperature for 2 hours, during which time the samples were stirred using a quartz tube to ensure uniform dissolution. Before cooling, the iron-based melt at high temperature was water-quenched and sampled using a pipette and a quartz tube. The sample mass was approximately 20g, for subsequent testing and analysis. The entire pre-melting experiment was conducted in a high-purity argon atmosphere (99.99%, 3 L / min), with a temperature change rate of 5 °C / min during both heating and cooling processes. The pre-melted samples underwent surface treatment to remove the surface oxide layer and impurities. The sample mass was then weighed and recorded using an electronic balance, as shown in Table 3.

[0035] Table 3. Sample Information for Fe-C Binary Viscosity Tests S2. Measurement Procedure: Place the weighed sample into the corundum crucible, then place it inside the graphite crucible of the equipment to assemble the shaking crucible. After ensuring the equipment is sealed, evacuate the device until the vacuum level reaches 10. -5Pa, then argon protective gas is introduced. When the gas pressure inside the furnace returns to atmospheric pressure, the temperature is raised at a rate of 10℃ / min. The viscosity is measured during the cooling process, starting from 1450℃, each temperature is held for 20 minutes, and a measurement point is set every 50℃ until solidification. The cooling rate is 10℃ / min. Before the measurement, the mirror position needs to be adjusted to ensure that the laser acquisition process meets the position in the formula.

[0036] S3. Viscosity Calculation: The oscillation period and logarithmic decay rate of the crucible containing the sample, obtained from the tests, are imported into the temperature-oscillation parameter relationship to obtain the viscosity value of the Fe-C binary alloy iron sample. The experimentally determined viscosity-temperature relationship curve is shown below. Figure 4 As shown in the figure, it can be seen that the viscosity of Fe-C binary alloy melts with different compositions increases monotonically as the temperature decreases. Figure 5 The variation of Fe-C binary alloy melt viscosity with carbon content is described. The figure shows that under high-temperature liquid conditions, the melt viscosity gradually increases with increasing carbon content. The viscosity variation trend obtained by this invention closely matches the actual viscosity composition relationship curve, demonstrating the accuracy of the measurement method described in this invention.

Claims

1. A method for determining the viscosity of a high-temperature melt, characterized in that, Includes the following steps: S1. Place the empty crucible in the suspension system inside the viscosity measuring device cavity, and start the vacuum system to evacuate the viscosity measuring device cavity to a vacuum level higher than 10. -5 Pa; S2. Maintain the thermal balance of the suspension system through a cooling medium; S3. Inert gas is introduced into the cavity of the viscosity measuring device as a protective atmosphere, and the pressure inside the crucible is restored to normal. S4. Heat the empty crucible at a rate of 10-20℃ / min until it reaches 1450-1600℃, then hold the temperature for 0.5-1h to ensure the thermal stability of the suspension system. S5. Put the empty crucible into a free oscillation state. At the target temperature, record at least 5 sets of oscillation period and corresponding logarithmic decay rate data continuously through the laser measurement system, and take the average value of each as the oscillation parameter of the empty crucible at that temperature point. S6. Cool the suspension system with a cooling medium at a rate of 10-15℃ / min, gradually cooling it from 1450℃ to 1600℃ to below 1350℃; set a temperature measurement point every 20-50℃, and record the corresponding oscillation data after holding the temperature for 0.5-1h. S7. Fit the collected oscillation period and logarithmic decay rate data to establish the relationship curves between temperature and oscillation period, and between temperature and logarithmic decay rate; S8. When measuring the melt to be tested, place the crucible containing the melt into the suspension system inside the viscosity measuring device cavity, and start the vacuum system to evacuate the viscosity measuring device cavity to a vacuum level higher than 10. -5 Pa, return to execute steps S2 to S7 to complete the full process measurement and data recording of the melt to be tested, and then execute step S9; S9. Viscosity measurement calculation is as follows: ； ； ； Where η is the viscosity of the melt to be tested, Pa·s; I is the moment of inertia of the suspended part, kg·m²; and ρ is the density of the melt to be tested, g·cm³. -3 δ is the logarithmic decay rate of the melt to be tested, dimensionless; t is the oscillation period of the melt to be tested, s; ​​δ0(T) is the logarithmic decay rate of the oscillation of the empty crucible at different temperatures, dimensionless; t0(T) is the oscillation period of the empty crucible at different temperatures, s; W is the correction coefficient, dimensionless; a, b, and c are instrument correlation constants, dimensionless; p is the number of horizontal planes in contact with the sample and the crucible, p=1 when the melt is not full; p=2 when the melt is fully filled with the crucible and in contact with the crucible lid, dimensionless; m is the mass of the melt, kg; r is the inner diameter of the crucible, m; h is the height of the melt, m; The damping ratio is dimensionless.

2. The method for determining the viscosity of a high-temperature melt according to claim 1, characterized in that, The cooling medium is cooling water.

3. A system employing the high-temperature melt viscosity determination method as described in any one of claims 1 to 2, characterized in that, A viscometer is used; the viscometer is equipped with a laser measurement system and a suspension system; The viscometer is used to heat the sample and provide a controlled atmosphere protection. The laser measurement system includes a laser source, a reflector, an image sensor, and a timing module. The reflector is mounted on a rotating suspension system, and all laser beams emitted by the laser source are reflected onto the reflector. The image sensor is positioned to receive the beam reflected by the reflector, and its signal line is connected to the timing module. The timing module is used to obtain the time difference between the beam received by the image sensor and the time difference, thereby calculating the oscillation period. The suspension system includes a stepper motor, a molybdenum wire, an inertia disk, and a molybdenum rod. The upper end of the molybdenum wire is connected to the output shaft of the stepper motor, and the lower end of the molybdenum wire is connected to a reflector. The reflector is connected to the molybdenum rod, the inertia disk is connected through the molybdenum rod and can rotate, and the crucible is connected to the bottom of the molybdenum rod and can rotate and oscillate.

4. The high-temperature melt viscosity measuring device according to claim 3, characterized in that, The crucible has a double-layer structure. The outer layer is a graphite-protected crucible connected to a molybdenum rod, which allows for rotational suspension and oscillation. The inner layer is a corundum crucible with a lid.

5. The high-temperature melt viscosity measuring device according to claim 4, characterized in that, The inner diameter of the corundum crucible is 30-50 mm.

6. The high-temperature melt viscosity measuring device according to claim 3, characterized in that, The reflector reflects at least three beams.

7. A computer-readable storage medium storing a computer program, characterized in that, When the computer program is executed by the processor, it implements the method for measuring the viscosity of high-temperature melts.

Images