Melt viscosity and density integrated measuring instrument and measuring method thereof

Abstract

The invention discloses a melt viscosity and density integrated measuring instrument and a measuring method thereof. The measuring instrument comprises a vacuum chamber, an oscillation device, a density measuring assembly and a viscosity measuring assembly, wherein the density measuring assembly and the viscosity measuring assembly are arranged in the vacuum chamber; the oscillating device comprises a suspension fiber, a connecting rod and a driving element; two ends of the suspension fiber are respectively connected with the driving element and the density measuring assembly; one end of the connecting rod is hinged with the density measuring assembly, the other end of the connecting rod is fixed with the viscosity measuring assembly, and the density measuring assembly and the viscosity measuring assembly are respectively driven by the suspension wire and the connecting rod to do periodic torsional vibration motion. The measurement method comprises the steps of sample loading, density measurement and viscosity measurement. The density measurement assembly and the viscosity measurement assembly are connected into a whole by arranging the oscillation device, the density of the melt is calculated according to the density measurement assembly, and the viscosity of the melt is calculated according to motion data of the viscosity measurement assembly of the melt. Therefore, the viscosity and density of the melt can be measured at the same time through one device, and the cost and time for measuring the viscosity of the melt are reduced.

Description

Technical Field

[0001] The invention relates to the technical field of viscosity and density detection equipment, and in particular to an integrated measuring instrument for melt viscosity and density and a measuring method thereof. Background Art

[0002] The high-temperature viscosity of the melt directly reflects the fluidity and thermodynamic properties of the melt material at high temperature, and plays a decisive role in improving heat transfer efficiency and reducing flow resistance. The measurement of melt viscosity is indispensable in the development of metal smelting, slag slag, glass ceramics, and new energy high-temperature heat transfer and storage medium materials. Therefore, accurate melt viscosity measurement is very important.

[0003] Melt viscosity is generally measured using a high-temperature viscometer, which has many specifications. The main methods of high-temperature viscometers include: rotary type, capillary type, and oscillating cup method. The oscillating cup method is currently the main method for measuring high-temperature melt viscosity, and has the advantages of high measurement accuracy and easy operation. However, the existing devices that use the oscillating cup method to measure melt viscosity (such as the measuring device disclosed in the patent application document with application publication number CN102879302A or CN105891050A) measure the kinematic viscosity of the melt, and a high-temperature density meter is required to measure the melt density, and then the required dynamic viscosity of the melt can be obtained through calculation. This method of using two devices to measure separately increases the cost and time of high-temperature melt viscosity measurement. Summary of the invention

[0004] In view of the above problems, the present invention provides an integrated measuring instrument for melt viscosity and density and a measuring method thereof.

[0005] The technical solution adopted by the present invention is as follows: The present application provides an integrated melt viscosity and density measuring instrument, comprising a vacuum chamber, an oscillating device, a density measuring component, and a viscosity measuring component; The density measuring component and the viscosity measuring component are respectively arranged in the vacuum chamber; The oscillation device comprises a suspension wire, a connecting rod and a driving element, one end of the suspension wire is connected to the driving element, and the other end is connected to the density measurement component; One end of the connecting rod is hinged to the density measuring component, and the other end is fixed to the viscosity measuring component, and the viscosity measuring component is used to be immersed in the melt; When the driving element drives the suspension wire to rotate, the density measuring component and the viscosity measuring component perform periodic torsional vibration motion driven by the suspension wire and the connecting rod respectively.

[0006] The present application sets an oscillating device, connects the density measuring component and the viscosity measuring component into one body, and places them in a vacuum chamber at the same time. The density measuring component and the viscosity measuring component perform periodic torsional vibration motion under the action of a driving element, so that the density of the melt can be calculated based on the motion data of the density measuring component, and the viscosity of the melt can be calculated based on the motion data of the viscosity measuring component of the melt. That is, the integrated melt viscosity and density measuring instrument provided by the present application can measure the viscosity and density of the melt at the same time through one device, reducing the cost and time of melt viscosity measurement.

[0007] Further, the density measurement assembly includes a fixed body, a sliding block, an elastic element and a sliding resistor; The fixed body is used to be fixed to the suspension wire, and a slide groove is provided in the fixed body; The sliding block is slidably disposed on the sliding groove; One end of the elastic element is fixed to the fixed body, and the other end is fixed to the sliding block, and the elastic element is arranged close to the suspension wire; The sliding resistor is arranged on the sliding block. When the sliding block slides along the sliding groove and is located at different positions of the sliding groove, the sliding resistor has different resistance values.

[0008] Furthermore, the density measurement assembly is coaxially arranged with the suspension wire, and the density measurement assembly further comprises a fixed connection member, the fixed connection member comprises a connection end and a mounting shaft, the connection end is screwed and fixed to the end of the fixed body, and the mounting shaft is used to connect with the suspension wire; A link rod is formed at one end of the sliding block away from the elastic element (ie, away from the side of the suspension wire), and the density measuring component is hinged to the connecting rod through the link rod.

[0009] Furthermore, the fixed body is a columnar structure, the viscosity measuring component is a columnar structure, and in a natural state, the fixed body and the viscosity measuring component are respectively coaxially arranged with the output shaft of the driving element; The oscillation device further comprises a balancing disk and a connecting chuck, wherein the connecting chuck is mounted on the output shaft of the driving element, the suspension wire is mounted on the connecting chuck, the suspension wire is connected to the driving element through the connecting chuck and is arranged coaxially with the output shaft of the driving element; The balancing disk is arranged above the density measuring component, and the balancing disk is passed through the installation shaft and is coaxially arranged with the output shaft of the driving element.

[0010] Furthermore, it also includes a timing device, which includes a timer, a light shielding sheet, a laser emitter and a photosensitive element; The shading sheet is arranged above the viscosity measuring component, the shading sheet is fixed to the viscosity measuring component and is arranged coaxially with the viscosity measuring component; The laser emitter and the photosensitive element are respectively arranged in the vacuum chamber and are respectively located on both sides of the light shielding sheet. The light shielding sheet, the laser emitter and the photosensitive element are located in the same horizontal plane. An angle Φ is formed between a line connecting the laser emitter and the photosensitive element and a line connecting the laser emitter and the light shielding sheet. When the viscosity measuring component performs periodic torsional vibration motion, the value of Φ changes with the periodic torsional vibration motion performed by the viscosity measuring component, and the shading time of the shading sheet also changes when Φ changes; When the viscosity measuring component is stationary, Φ is greater than or equal to 0°, that is, when the viscosity measuring component is stationary, the value of Φ can be greater than 0° or equal to 0°. When Φ is equal to 0°, the laser emitter, the shading sheet and the photosensitive element in the horizontal plane are located in the same straight line.

[0011] The timer is connected to the photosensitive element by electrical signals. When the viscosity measuring component performs periodic torsional vibration motion, the light shielding sheet, the laser transmitter and the photosensitive element cooperate with the timer to measure the time interval between two times when the photosensitive element senses light or the time interval when it does not sense light.

[0012] In actual use, the timer includes two (first timer and second timer). When the photosensitive element receives the light source signal, the first timer starts timing and stops timing when the light source signal is disconnected; when the light source signal is disconnected, the second timer starts timing and stops timing when the light source signal is received again. At this time, the first timer starts timing again and stops timing when the light source signal is disconnected, and repeats in sequence.

[0013] Furthermore, it also includes an inert atmosphere device, a vacuum device, a sealing furnace, a sealing cover and a sealing box; The sealing cover is arranged on the sealing box and forms a first cavity together with the sealing box; The sealed furnace is arranged below the sealed box, a second cavity is formed inside the sealed furnace, a crucible is arranged in the second cavity, the crucible is used to accommodate the melt to be tested, the first cavity and the second cavity are connected to form the vacuum chamber; The density measuring component is arranged in the first cavity, and the viscosity measuring component is arranged in the second cavity; The vacuum device is used to perform vacuum processing on the first cavity and the second cavity, and the inert atmosphere device is used to input inert atmosphere into the first cavity and the second cavity.

[0014] Furthermore, the crucible is a columnar body.

[0015] Furthermore, the driving element is a stepping motor, and the vacuum device is a vacuum pump.

[0016] Furthermore, it also includes a temperature measuring thermocouple wire, a heating device and a cooling device. The temperature measuring thermocouple wire is installed inside the viscosity measuring component; The heating device comprises a high-temperature furnace body, wherein the high-temperature furnace body has a heating element, wherein the high-temperature furnace body is arranged outside the sealed furnace, wherein the heating element is used to heat the sealed furnace, and wherein a heat preservation element is arranged between the high-temperature furnace body and the heating element, wherein the heat preservation element is used to keep the sealed furnace warm; The cooling device includes a first cold pipe and a second cold pipe. The first cold pipe is arranged between the heat preservation element and the high-temperature furnace body and is used to cool the high-temperature furnace body. The second cold pipe is used to cool the sealed box and prevent the heating device from affecting the measured density in the first cavity.

[0017] Furthermore, the temperature measuring thermocouple wire is connected to the heating device signal, and the heating device adjusts the heating power of the heating element according to the signal fed back by the temperature measuring thermocouple wire.

[0018] By implanting the temperature measuring thermocouple wire into the torsion pendulum column and immersing it in the melt sample together with the viscosity measuring component, the actual temperature of the melt can be detected, making the measurement more accurate.

[0019] Furthermore, it also includes a first lifting device, which is used to drive the oscillating device to move in a vertical direction so that the density measuring component is immersed in the melt to be measured.

[0020] Furthermore, the first lifting device is also used to place the light shielding plate, laser transmitter and photosensitive element of the viscosity measuring component at the same horizontal position.

[0021] Furthermore, it also includes a sealing connector, which is arranged between the sealing box and the sealing furnace; It also includes a second lifting device, which is used to control the lifting of the sealing box and control the cooperation between the sealing box and the sealing connector to achieve the sealing of the sealing box and the sealing furnace.

[0022] In actual use, the oscillating device, the viscosity measuring component and the sealing box can be arranged as an integrated structure, in which case only one lifting device is required.

[0023] Furthermore, flanges are respectively provided at the connection ends of the sealing box and the sealing furnace, and the sealing connector is provided between the flanges.

[0024] The present application also provides a method for measuring a melt viscosity and density integrated measuring instrument, wherein the integrated measuring instrument is the above-mentioned integrated measuring instrument for melt viscosity and density, and the measuring method comprises the following steps: S1: Sample loading: placing the melt to be tested in a vacuum chamber and making the melt to be tested in a molten state, and filling the vacuum chamber with protective gas; S2: Density measurement: Control the density measuring component to be immersed in the melt to be measured, and calculate the density of the melt to be measured according to the sliding resistance in the density measuring component; According to Archimedes' principle, if the same viscosity measuring component is immersed in a melt with different densities, the buoyancy of the viscosity measuring component will also be different.

[0025] When the viscosity measuring component is not immersed in the melt and is in a naturally sagging state, the gravity acting on the viscosity measuring component is calculated based on the tension acting on the elastic element; When the viscosity measuring component is immersed in the melt, it will float upwards under the action of the melt buoyancy. The buoyancy of the viscosity measuring component is calculated according to the upward movement of the sliding block, and the melt density is calculated based on the buoyancy. Alternatively, the force balance state is judged according to the floating state (floating or sinking) and the buoyancy of the viscosity measuring component and the density of the melt are calculated.

[0026] Alternatively, when the viscosity measuring component is immersed in the melt, the viscosity measuring component floats under the action of the melt buoyancy, and the sliding block moves freely upward in the sliding groove. The greater the melt density, the greater the buoyancy of the viscosity measuring component, and the greater the upward movement of the sliding block. Since the sliding block is provided with a sliding resistor, the sliding block and the sliding resistor are introduced into a closed circuit, and an electromotive force is passed into the closed circuit, and the melt density can be calculated according to the magnitude of the current in the closed circuit.

[0027] S3: Viscosity measurement: The crucible is fixed, and the driving element is controlled to rotate in the clockwise direction and the counterclockwise direction in turn, so that the oscillation device drives the viscosity measurement component to perform periodic torsional oscillation motion (the amplitude of which will be attenuated due to the effect of the viscous force), and the timing device corresponding to the oscillation device is used to count the shading time, and the viscosity of the melt to be measured is calculated according to the shading time: A timing device is used to count the light shielding time: the light shielding sheet, the laser emitter and the photosensitive element of the timing device are located on the same horizontal line and the light shielding sheet is located between the laser emitter and the photosensitive element. The light shielding sheet includes a light shielding sheet A and a light shielding sheet B. The light shielding sheet A and the light shielding sheet B are symmetrically arranged along the output axis of the driving element; When the light shielding sheet is twisted, the light shielding sheet A and the light shielding sheet B periodically shield the light emitted by the laser transmitter, and the light shielding sheet B rotates counterclockwise. The time from no shielding to shielding is recorded as t BA , the shading piece B twists to the maximum amplitude and then turns back, changing from shading to unshading, and the shading time is t BB Then the light shielding piece A will twist clockwise to block the light, and the time from no blocking to blocking is recorded as t AB , the light-shielding A piece twists to the maximum amplitude and then turns back, changing from blocking to not blocking, and the blocking time is t AA ; When the driving element rotates clockwise and counterclockwise, t BA +t BB =t AB +t AA .

[0028] The motion equation of the oscillation device driving the viscosity measurement component to perform periodic torsional oscillation motion is:

[0029] in: Indicates that the viscosity measurement component is The amplitude of the moment, For The time from the beginning to the i-th moment; Indicates that the viscosity measurement component is Amplitude of moment; represents the attenuation coefficient; Indicates time; Represents angular velocity.

[0030] From the above equation of motion, we can get The value of The viscosity calculation formula is:

[0031] in: , represent the radius of the viscosity measurement assembly and the inner diameter of the crucible, respectively; Indicates the height of the viscosity measuring assembly; The expression coefficient can be obtained by calibration with a standard sample of known viscosity or by blank testing; Represents force resistance, and the calculation formula of force resistance is:

[0032] in: represents the vibration cycle, ; represents the moment of inertia of the viscosity measuring component, Indicates the moment of inertia of the density measurement component. For a solid cylinder, the moment of inertia calculation formula is:

[0033] in: Indicates quality, Indicates the radius.

[0034] The existing measurement method, the capillary method, cannot measure high melting point melts and has very high requirements for sample purity, otherwise it is easy to clog the capillary and cause errors in the measurement results. The rotation method has extremely high requirements for motors and machinery, and the existing torque sensor accuracy is limited when measuring low viscosity melts and cannot meet the requirements well.

[0035] The melt oscillation viscosity measuring instrument proposed in the present invention can measure the melt kinematic viscosity and density simultaneously when in use, and can automatically calculate the melt dynamic viscosity when combined with a computing device. At the same time, a temperature measuring thermocouple wire is implanted inside the torsion pendulum column to detect the actual temperature of the melt in real time, making the measurement more accurate and facilitating the realization of automated precision measurement.

[0036] Further, the sample loading step includes: The melt to be tested is loaded into the crucible, the crucible is sent to a fixed position in the sealing furnace, and the first lifting device and the second lifting device are controlled to make the sealing box and the sealing furnace seal together, the sealing cover and the sealing box seal together, and then seal and lock; Using a vacuum device to evacuate the first cavity, the second cavity and the inside of the sealing cover (i.e., the vacuum chamber), and opening an inert atmosphere device to transport an inert protective atmosphere into the vacuum chamber; Turn on the heating device and the cooling device (circulating cooling water), and set the heating / constant temperature / cooling program of the high-temperature furnace. The heating device makes the melt to be measured in the crucible become or maintain the melt state, and the cooling device is used to prevent the heating device from affecting the density measurement in the first cavity.

[0037] The beneficial effects of the present invention are: (1) The present application sets an oscillating device, connects the density measuring device and the viscosity measuring device together, and places them in a vacuum chamber at the same time. The density measuring device and the viscosity measuring device perform periodic torsional vibration motion under the action of the driving element, so that the density of the melt can be calculated based on the motion data of the density measuring device, and the viscosity of the melt can be calculated based on the motion data of the viscosity measuring device. That is, the integrated melt viscosity and density measuring instrument provided by the present application can measure the viscosity and density of the melt at the same time through one device, reducing the cost and time of melt viscosity measurement.

[0038] (2) This application adopts a lifting mechanism and performs a lifting design on the oscillating device, so that the viscosity measuring component can be immersed in the melt sample. The design in which the crucible does not move and the internal stator drives the movement of the gap fluid is based on the basic principle of viscosity measurement, and the traceability of the measured value is clearer.

[0039] (3) By implanting the temperature measuring thermocouple wire into the torsion pendulum cylinder and immersing it in the melt sample together with the viscosity measuring piece, the actual temperature of the melt can be detected, making the measurement more accurate. BRIEF DESCRIPTION OF THE DRAWINGS

[0040] Figure 1 1 is a schematic structural diagram of an integrated measuring instrument for melt viscosity and density according to an embodiment of the present invention; Figure 2 It is a schematic diagram of the connection structure of the density measurement component and the viscosity measurement component according to an embodiment of the present invention; Figure 3 is a schematic diagram of the structure of a density measurement assembly according to an embodiment of the present invention (some parts are hidden); Figure 4 is a schematic diagram of the structure of a timing device according to an embodiment of the present invention (viewed from above); Figure 5 It is a schematic diagram of the body structure of an integrated measuring instrument for melt viscosity and density according to an embodiment of the present invention.

[0041] The reference numerals in the figures are: 10. Oscillating device; 110. Suspension wire; 120. Connecting rod; 130. Driving element; 140. Balance plate; 150. Connecting chuck; 20. Density measuring assembly; 210. Fixed body; 211. Slideway; 220. Sliding block; 221. Connecting rod; 230. Elastic element; 240. Sliding resistor; 250. Fixed connecting piece; 30. Viscosity measuring assembly; 310. Thermocouple wire for temperature measurement; 40. Timing device; 410. Photosensitive element; 420. Excitation Light emitter; 430, shading sheet; 431, shading sheet A; 432, shading sheet B; 50, vacuum device; 510, inert atmosphere device; 60, sealed furnace; 610, second chamber; 70, sealed box; 710, first chamber; 720, sealed cover; 80, heating device; 810, heating element; 820, insulation element; 830, crucible; 840, high-temperature furnace body; 90, first lifting device; 100, second lifting device; 200, cooling device. DETAILED DESCRIPTION

[0042] The present invention is described in detail below in conjunction with the accompanying drawings.

[0043] like Figure 1~Figure 5 As shown, the present application provides an integrated measuring instrument for melt viscosity and density, including a vacuum chamber, an oscillating device 10, a density measuring component 20, and a viscosity measuring component 30; The density measuring component 20 and the viscosity measuring component 30 are respectively disposed in the vacuum chamber; The oscillating device 10 includes a suspension wire 110, a connecting rod 120 and a driving element 130. One end of the suspension wire 110 is connected to the driving element 130, and the other end is connected to the density measuring component 20. One end of the connecting rod 120 is hinged to the density measuring assembly 20, and the other end is fixed to the viscosity measuring assembly 30, and the viscosity measuring assembly 30 is used to immerse into the melt; When the driving element 130 drives the suspension wire 110 to rotate, the density measuring assembly 20 and the viscosity measuring assembly 30 are driven by the suspension wire 110 and the connecting rod 120 to perform periodic torsional vibration motions, respectively.

[0044] The present application sets an oscillating device 10, connects the density measuring component 20 and the viscosity measuring component 30 into one body, and places them in a vacuum chamber at the same time. The density measuring component 20 and the viscosity measuring component 30 perform periodic torsional vibration motion under the action of the driving element 130, so that the density of the melt can be calculated according to the motion data of the density measuring component 20, and the viscosity of the melt can be calculated according to the motion data of the viscosity measuring component 30. That is, the integrated melt viscosity and density measuring instrument provided by the present application can measure the viscosity and density of the melt at the same time through one device, reducing the cost and time of melt viscosity measurement.

[0045] In this embodiment, the density measuring assembly 20 includes a fixed body 210, a sliding block 220, an elastic element 230 and a sliding resistor 240; The fixing body 210 is used to fix with the suspension wire 110, and a slide groove 211 is provided in the fixing body 210; The sliding block 220 is slidably disposed on the sliding groove 211; One end of the elastic element 230 is fixed to the fixed body 210, and the other end is fixed to the sliding block 220, and the elastic element 230 is arranged on a side close to the suspension wire 110; The sliding resistor 240 is disposed on the sliding block 220 . When the sliding block 220 slides along the sliding groove 211 and is located at different positions of the sliding groove 211 , the sliding resistor 240 has different resistance values.

[0046] In this embodiment, the density measuring assembly 20 is coaxially arranged with the suspension wire 110, and the density measuring assembly 20 further includes a fixed connecting member 250, the fixed connecting member 250 includes a connecting end and a mounting shaft, the connecting end is screwed and fixed to the end of the fixed body 210, and the mounting shaft is used to connect with the suspension wire 110; A link rod 221 is formed at one end of the sliding block 220 away from the elastic element 230 (ie, away from the side of the suspension wire 110 ), and the density measurement assembly 20 is hinged to the connecting rod 120 via the link rod 221 .

[0047] In this embodiment, the fixed body 210 is a columnar structure, and the viscosity measuring component 30 is a columnar structure. In the natural state, the fixed body 210 and the viscosity measuring component 30 are respectively coaxially arranged with the output shaft of the driving element 130; The oscillation device 10 further includes a balancing disk 140 and a connecting chuck 150. The connecting chuck 150 is mounted on the output shaft of the driving element 130. The suspension wire 110 is mounted on the connecting chuck 150. The suspension wire 110 is connected to the driving element 130 through the connecting chuck 150 and is coaxially arranged with the output shaft of the driving element 130. The balancing disk 140 is disposed above the density measuring assembly 20 . The balancing disk 140 is passed through the mounting shaft and is coaxially disposed with the output shaft of the driving element 130 .

[0048] In this embodiment, a timing device 40 is also included, and the timing device 40 includes a timer (not shown in the figure), a light shielding sheet 430, a laser emitter 420 and a photosensitive element 410; The light shielding sheet 430 is disposed above the viscosity measuring assembly 30 , and the light shielding sheet 430 is fixed to the viscosity measuring assembly 30 and is disposed coaxially with the viscosity measuring assembly 30 ; The laser emitter 420 and the photosensitive element 410 are respectively disposed in the vacuum chamber and are respectively located on both sides of the light shielding sheet 430. The light shielding sheet 430, the laser emitter 420 and the photosensitive element 410 are located in the same horizontal plane, and the line connecting the laser emitter 420 and the photosensitive element 410 and the line connecting the laser emitter 420 and the light shielding sheet 430 form an angle Φ; When the viscosity measuring component 30 performs periodic torsional vibration motion, the value of Φ changes with the periodic torsional vibration motion performed by the viscosity measuring component, and the shading time of the shading sheet also changes when Φ changes; When the viscosity measuring component 30 is stationary, Φ is greater than or equal to 0°, that is, when the viscosity measuring component is stationary, the value of Φ can be greater than 0° or equal to 0°. When Φ is equal to 0°, the laser emitter, the shading sheet and the photosensitive element in the horizontal plane are located on the same straight line.

[0049] The timer is connected to the photosensitive element 410 by electrical signals. When the viscosity measuring component 30 performs periodic torsional vibration motion, the light shielding sheet 430, the laser emitter 420 and the photosensitive element 410 cooperate with the timer to measure the time interval between two times when the photosensitive element 410 senses light or the time interval when it does not sense light.

[0050] In actual use, the timers include two (a first timer and a second timer). When the photosensitive element 410 receives a light source signal, the first timer starts timing, and stops timing when the light source signal is disconnected; when the light source signal is disconnected, the second timer starts timing, and stops timing when the light source signal is received again. At this time, the first timer starts timing again, and stops timing when the light source signal is disconnected, and repeats in sequence.

[0051] In this embodiment, an inert atmosphere device 510 (not shown), a vacuum device 50, a sealing furnace 60, a sealing cover 720 and a sealing box 70 are also included; The sealing cover 720 is disposed on the sealing box 70 and forms a first cavity 710 together with the sealing box 70; The sealed furnace 60 is arranged below the sealed box 70. A second cavity 610 is formed inside the sealed furnace 60. A crucible 830 is arranged inside the second cavity 610. The crucible 830 is used to accommodate the melt to be tested. The first cavity 710 and the second cavity 610 are connected to form a vacuum chamber. The density measuring assembly 20 is disposed in the first cavity 710, and the viscosity measuring assembly 30 is disposed in the second cavity 610; The vacuum device 50 is used to evacuate the first cavity 710 and the second cavity 610 , and the inert atmosphere device 510 is used to input an inert atmosphere into the first cavity 710 and the second cavity 610 .

[0052] In this embodiment, the crucible 830 is a columnar body.

[0053] In this embodiment, the driving element 130 is a stepping motor, and the vacuum device 50 is a vacuum pump.

[0054] In this embodiment, it also includes a temperature measuring thermocouple wire 310, a heating device 80 and a cooling device 200. The temperature measuring thermocouple wire 310 is installed inside the viscosity measuring component 30; The heating device 80 includes a high-temperature furnace body 840, and a heating element 810 is provided in the high-temperature furnace body 840. The high-temperature furnace body 840 is arranged outside the sealing furnace 60. The heating element 810 is used to heat the inside of the sealing furnace 60. A heat preservation element 820 is provided between the high-temperature furnace body 840 and the heating element 810. The heat preservation element 820 is used to keep the sealing furnace 60 warm. The cooling device 200 is a water-cooled box, and the cooling device 200 includes a first cold pipe and a second cold pipe. The first cold pipe is arranged between the insulation element 820 and the high-temperature furnace body 840, and is used to cool the high-temperature furnace body 840. The second cold pipe is used to cool the sealing box 70. The second cold pipe is arranged at the connecting flange between the sealing furnace 60 and the sealing box 70 to prevent the heating device 80 from affecting the measured density in the first cavity 710.

[0055] In this embodiment, the temperature measuring thermocouple wire 310 is signal-connected to the heating device 80 , and the heating device 80 adjusts the heating power of the heating element 810 according to the signal fed back by the temperature measuring thermocouple wire 310 .

[0056] By implanting the temperature measuring thermocouple wire 310 into the torsion pendulum column and immersing it in the melt sample together with the viscosity measuring component 30, the actual temperature of the melt can be detected, and the measurement is more accurate.

[0057] In this embodiment, a first lifting device 90 is further included. The first lifting device 90 is used to drive the oscillating device 10 to move in a vertical direction so that the density measuring component 20 is immersed in the melt to be measured.

[0058] In this embodiment, the first lifting device 90 is also used to make the light shielding sheet 430 , the laser emitter 420 and the photosensitive element 410 of the viscosity measuring component 30 be located at the same horizontal position.

[0059] In this embodiment, a sealing connection piece is further included, and the sealing connection piece is arranged between the sealing box 70 and the sealing furnace 60; It also includes a second lifting device 100 , which is used to control the lifting of the sealing box 70 and control the sealing box 70 to cooperate with the sealing connector to achieve sealing between the sealing box 70 and the sealing furnace 60 .

[0060] In actual use, the oscillating device 10, the viscosity measuring assembly 30 and the sealing box 70 can be provided as an integrated structure, in which case only one lifting device is provided.

[0061] The present application also provides a method for measuring a melt viscosity and density integrated measuring instrument, wherein the integrated measuring instrument is the above-mentioned integrated measuring instrument for melt viscosity and density, and the measuring method comprises the following steps: S1: Sample loading: placing the melt to be tested in a vacuum chamber and making the melt to be tested in a molten state, and filling the vacuum chamber with protective gas; S2: Density measurement: Control the density measuring component 20 to be immersed in the melt to be measured, and calculate the density of the melt to be measured according to the sliding resistor 240 in the density measuring component 20; According to Archimedes' principle, when the same viscosity measuring component 30 is immersed in a melt, if the melt densities are different, the buoyancy of the viscosity measuring component 30 will also be different.

[0062] When the viscosity measuring component 30 is not immersed in the melt and is in a naturally drooping state, the gravity exerted on the viscosity measuring component 30 is calculated based on the tension exerted on the elastic element 230; When the viscosity measuring component 30 is immersed in the melt, the viscosity measuring component 30 will float upward under the action of the buoyancy of the melt. The buoyancy of the viscosity measuring component 30 is calculated according to the upward movement of the sliding block 220, and the melt density is calculated according to the buoyancy; or the force balance state is judged according to the floating state (floating or sinking) and the buoyancy of the viscosity measuring component 30 and the density of the melt are calculated.

[0063] Alternatively, when the viscosity measuring assembly 30 is immersed in the melt, the viscosity measuring assembly 30 floats under the action of the melt buoyancy, and the sliding block 220 moves upward freely in the sliding groove. The greater the melt density, the greater the buoyancy of the viscosity measuring assembly 30, and the greater the upward movement of the sliding block 220. Since the sliding block 220 is provided with a sliding resistor 240, the sliding block 220 and the sliding resistor 240 are introduced into a closed circuit, and an electromotive force is passed into the closed circuit, and the melt density can be calculated according to the magnitude of the current in the closed circuit.

[0064] S3: Viscosity measurement: The crucible 830 is fixed, and the driving element 130 is controlled to rotate in the clockwise direction and the counterclockwise direction in sequence, so that the oscillating device 10 drives the viscosity measuring component 30 to perform a periodic torsional oscillation motion (the amplitude of which will be attenuated due to the effect of the viscous force), and the timing device 40 corresponding to the oscillating device 10 is used to count the shading time, and the viscosity of the melt to be measured is calculated according to the shading time: The timing device 40 is used to count the light shielding time: the light shielding sheet 430, the laser emitter 420 and the photosensitive element 410 of the timing device 40 are located on the same horizontal line and the light shielding sheet 430 is located between the laser emitter 420 and the photosensitive element 410. The light shielding sheet 430 includes a light shielding sheet A 431 and a light shielding sheet B 432. The light shielding sheet A 431 and the light shielding sheet B 432 are symmetrically arranged along the output axis of the driving element 130; When the light shielding sheet 430 is twisted, the light shielding sheet A 431 and the light shielding sheet B 432 periodically shield the light emitted by the laser emitter 420, and the light shielding sheet B 432 rotates in a counterclockwise direction. The time from no shielding to shielding is recorded as t BA , the light shielding B sheet 432 twists to the maximum amplitude and then turns back, changing from shielding to non-shielding, and the shielding time is t BB Then the light shielding piece A 431 will twist clockwise to block the light, and the time from no blocking to blocking is recorded as t AB , the light shielding A sheet 431 twists to the maximum amplitude and then turns back, changing from shielding to non-shielding, and the shielding time is t AA ; When the driving element rotates clockwise and counterclockwise, t BA +t BB =t AB +t AA .

[0065] The motion equation of the oscillation device driving the viscosity measurement component to perform periodic torsional oscillation motion is:

[0066] in: Indicates that the viscosity measurement component is The amplitude of the moment, For The time from the beginning to the i-th moment; Indicates that the viscosity measurement component is Amplitude of moment; represents the attenuation coefficient; Indicates time; Represents angular velocity.

[0067] From the above equation of motion, we can get The value of The viscosity calculation formula is:

[0068] in: , represent the radius of the viscosity measurement assembly and the inner diameter of the crucible, respectively; Indicates the height of the viscosity measuring assembly; The expression coefficient can be obtained by calibration with a standard sample of known viscosity or by blank testing; Represents force resistance, and the calculation formula of force resistance is:

[0069] in: represents the vibration cycle, ; represents the moment of inertia of the viscosity measuring component, Indicates the moment of inertia of the density measurement component. For a solid cylinder, the moment of inertia calculation formula is:

[0070] in: Indicates quality, Indicates the radius.

[0071] The existing measurement method, the capillary method, cannot measure high melting point melts and has very high requirements for sample purity, otherwise it is easy to clog the capillary and cause errors in the measurement results. The rotation method has extremely high requirements for motors and machinery, and the existing torque sensor accuracy is limited when measuring low viscosity melts and cannot meet the requirements well.

[0072] The melt oscillation viscosity measuring instrument proposed in the present invention can measure the melt kinematic viscosity and density simultaneously when in use, and can automatically calculate the melt dynamic viscosity in combination with a computing device. At the same time, the temperature measuring thermocouple wire 310 is implanted inside the torsion pendulum column to detect the actual temperature of the melt in real time, making the measurement more accurate and facilitating the realization of automated precision measurement.

[0073] In this embodiment, the sample loading step includes: The melt to be tested is loaded into the crucible 830, and the crucible 830 is sent to a fixed position in the sealing furnace 60, and the first lifting device 90 and the second lifting device 100 are controlled to make the sealing box 70 and the sealing furnace 60 sealed and buckled, and the sealing cover 720 and the sealing box 70 sealed and buckled, and then the sealing and locking are performed; The first cavity 710, the second cavity 610 and the sealing cover 720 (ie, the vacuum chamber) are evacuated by using the vacuum device 50, and the inert atmosphere device 510 is turned on to deliver an inert protective atmosphere into the vacuum chamber; The heating device 80 and the cooling device 200 (circulating cooling water) are turned on, and the heating / constant temperature / cooling program of the high-temperature furnace body 840 is set. The heating device 80 makes the melt to be measured in the crucible 830 become or maintain a melt state, and the cooling device 200 is used to prevent the heating device 80 from affecting the measured density in the first cavity 710.

[0074] The above description is only a preferred embodiment of the present invention, and does not limit the patent protection scope of the present invention. Any equivalent structural transformation made by using the contents of the present invention and the drawings, directly or indirectly used in other related technical fields, is also included in the protection scope of the present invention.

Claims

1. An integrated measuring instrument for melt viscosity and density, characterized in that: It includes a vacuum chamber, an oscillating device, a density measuring component, and a viscosity measuring component; The density measuring component and the viscosity measuring component are respectively arranged in the vacuum chamber; The oscillation device comprises a suspension wire, a connecting rod and a driving element, one end of the suspension wire is connected to the driving element, and the other end is connected to the density measurement component; One end of the connecting rod is hinged to the density measuring component, and the other end is fixed to the viscosity measuring component, and the viscosity measuring component is used to be immersed in the melt; When the driving element drives the suspension wire to rotate, the density measuring component and the viscosity measuring component perform periodic torsional vibration motion driven by the suspension wire and the connecting rod respectively.

2. An integrated melt viscosity and density measuring instrument as claimed in claim 1, characterized in that: The density measurement assembly includes a fixed body, a sliding block, an elastic element and a sliding resistor; The fixed body is used to be fixed to the suspension wire, and a slide groove is provided in the fixed body; The sliding block is slidably disposed on the sliding groove; One end of the elastic element is fixed to the fixed body, and the other end is fixed to the sliding block, and the elastic element is arranged close to the suspension wire; The sliding resistor is arranged on the sliding block. When the sliding block slides along the sliding groove and is located at different positions of the sliding groove, the sliding resistor has different resistance values.

3. An integrated melt viscosity and density measuring instrument as claimed in claim 2, characterized in that: The density measurement assembly is coaxially arranged with the suspension wire, and the density measurement assembly further comprises a fixed connection member, the fixed connection member comprises a connection end and a mounting shaft, the connection end is screwed and fixed to the end of the fixed body, and the mounting shaft is used to connect with the suspension wire; A link rod is formed at one end of the sliding block away from the elastic element, and the density measuring component is hinged to the connecting rod through the link rod.

4. An integrated melt viscosity and density measuring instrument as claimed in claim 1, characterized in that: The fixed body is a columnar structure, the viscosity measuring component is a columnar structure, and in a natural state, the fixed body and the viscosity measuring component are respectively coaxially arranged with the output shaft of the driving element; The oscillation device further comprises a balancing disk and a connecting chuck, wherein the connecting chuck is mounted on the output shaft of the driving element, the suspension wire is mounted on the connecting chuck, the suspension wire is connected to the driving element through the connecting chuck and is arranged coaxially with the output shaft of the driving element; The balancing disk is arranged above the density measuring component, and the balancing disk is passed through the installation shaft and is coaxially arranged with the output shaft of the driving element.

5. An integrated melt viscosity and density measuring instrument as claimed in claim 1, characterized in that: It also includes a timing device, which includes a timer, a light shielding sheet, a laser transmitter and a photosensitive element; The light shielding sheet is arranged above the viscosity measuring component, the light shielding sheet is fixed to the viscosity measuring component and arranged coaxially with the viscosity measuring component, the light shielding sheet includes a light shielding sheet A and a light shielding sheet B, and the light shielding sheet A and the light shielding sheet B are symmetrically arranged along the output axis of the driving element; The laser emitter and the photosensitive element are respectively arranged in the vacuum chamber and are respectively located on both sides of the light shielding sheet. The light shielding sheet, the laser emitter and the photosensitive element are located in the same horizontal plane. An angle Φ is formed between a line connecting the laser emitter and the photosensitive element and a line connecting the laser emitter and the light shielding sheet. When the viscosity measuring component performs periodic torsional vibration motion, the value of Φ changes with the periodic torsional vibration motion of the viscosity measuring component; when the viscosity measuring component is stationary, Φ is greater than or equal to 0°; The timer is connected to the photosensitive element by electrical signals. When the viscosity measuring component performs periodic torsional vibration motion, the timer is used to measure the time interval between two times when the photosensitive element senses light or the time interval when it does not sense light.

6. An integrated melt viscosity and density measuring instrument as claimed in claim 1, characterized in that: It also includes an inert atmosphere device, a vacuum device, a sealed furnace, a sealed cover and a sealed box; The sealing cover is arranged on the sealing box and forms a first cavity together with the sealing box; The sealed furnace is arranged below the sealed box, a second cavity is formed inside the sealed furnace, a crucible is arranged in the second cavity, the crucible is used to accommodate the melt to be tested, the first cavity and the second cavity are connected to form the vacuum chamber; The density measuring component is arranged in the first cavity, and the viscosity measuring component is arranged in the second cavity; The vacuum device is used to perform vacuum processing on the first cavity and the second cavity, and the inert atmosphere device is used to input inert atmosphere into the first cavity and the second cavity.

7. An integrated melt viscosity and density measuring instrument as claimed in claim 6, characterized in that: It also includes a temperature measuring thermocouple wire, a heating device and a cooling device. The temperature measuring thermocouple wire is installed inside the viscosity measuring component; The heating device comprises a high-temperature furnace body, wherein the high-temperature furnace body has a heating element, wherein the high-temperature furnace body is arranged outside the sealed furnace, wherein the heating element is used to heat the sealed furnace, and wherein a heat preservation element is arranged between the high-temperature furnace body and the heating element, wherein the heat preservation element is used to keep the sealed furnace warm; The cooling device includes a first cold pipe and a second cold pipe. The first cold pipe is arranged between the heat preservation element and the high-temperature furnace body and is used to cool the high-temperature furnace body. The second cold pipe is used to cool the sealed box and prevent the heating device from affecting the measured density in the first cavity.

8. An integrated melt viscosity and density measuring instrument as claimed in claim 6, characterized in that: It also includes a first lifting device, which is used to drive the oscillating device to move in a vertical direction so that the density measuring component can be immersed in the melt to be measured.

9. An integrated melt viscosity and density measuring instrument as claimed in claim 8, characterized in that: It also includes a sealing connection piece, which is arranged between the sealing box and the sealing furnace; It also includes a second lifting device, which is used to control the lifting of the sealing box and control the cooperation between the sealing box and the sealing connector to achieve the sealing of the sealing box and the sealing furnace.

10. The method for measuring melt viscosity and density using an integrated measuring instrument according to any one of claims 1 to 9, characterized in that: The following steps are involved: Sample loading: Place the melt to be tested in a vacuum chamber and make it molten, and fill the vacuum chamber with protective gas; Density measurement: Control the density measuring component to be immersed in the melt to be measured, and calculate the density of the melt to be measured according to the sliding resistance in the density measuring component; Viscosity measurement: The driving element is controlled to rotate in a clockwise direction and a counterclockwise direction in sequence, so that the oscillation device drives the viscosity measuring component to perform a periodic torsional oscillation motion, and a timing device corresponding to the oscillation device is used to count the light shielding time, and the viscosity of the melt to be measured is calculated according to the light shielding time; When a timing device is used to count the shading time, the shading sheet, the laser emitter and the photosensitive element of the timing device are located on the same horizontal line and the shading sheet is located between the laser emitter and the photosensitive element. The shading sheet includes a shading sheet A and a shading sheet B. The shading sheet A and the shading sheet B are symmetrically arranged along the output axis of the driving element. When the light shielding sheet is twisted, the light shielding sheet A and the light shielding sheet B periodically shield the light emitted by the laser transmitter, and the light shielding sheet B rotates counterclockwise. The time from no shielding to shielding is recorded as t BA , the shading piece B twists to the maximum amplitude and then turns back, changing from shading to unshading, and the shading time is t BB Then the light shielding piece A will twist clockwise to block the light, and the time from no blocking to blocking is recorded as t AB , the light-shielding A piece twists to the maximum amplitude and then turns back, changing from blocking to not blocking, and the blocking time is t AA ; When the driving element rotates clockwise and counterclockwise, t BA +t BB =t AB +t AA .

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