Material rheological behavior visual measurement device and application method thereof

Abstract

The invention provides a material rheological behavior visual measurement device and an application method thereof. The visual measuring device comprises a transparent measuring cell, a cylinder measuring rotor embedded in the center of the interior of the transparent measuring cell in a matched mode, a laser light source arranged on the outer side of the transparent measuring cell in a matched mode, a high-speed camera system, a constant-temperature liquid bath tank, an online refractometer, an online densimeter and a rotational rheometer. The device can realize simultaneous measurement of macroscopic rheology and shear deformation of the non-Newtonian fluid, can be directly applied to research of a medium rheology mechanism, and provides reliable data basis and image analysis materials for establishment of rheology models such as a constitutive relationship of a complex system; a multi-phase dispersion system and a high-molecular polymer rheological measurement theory and technology are established, an existing rheometer measurement technology is reconstructed, and high-precision visuality information for measuring rheological characteristics of a non-uniform or anisotropic medium is increased.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of measuring devices, in particular to a material flow behavior visualized measuring device and application method thereof. BACKGROUND

[0002] Rheometers are mainly used for measuring the macro rheological characteristics of non-Newtonian fluids. For single-phase media, the rheometer can well describe the correspondence between fluid deformation flow and shear force, and further establish reliable constitutive relationship and other rheological theories. However, for multi-phase dispersion systems or polymer materials, which are generally heterogeneous media, especially for multi-phase dispersion systems, the dispersed phase may deform, break or coalesce under shear, which will bring great difficulties to the measurement theory, method and accuracy of rheological parameters.

[0003] Generally, the rheological experiment of multi-phase dispersion does not perform visualized measurement, and the detection cell used is generally a cup-shaped stainless steel product, without considering the influence of image data on rheological detection. Individual experiments seeking visualization use a radioactive source to irradiate the container (similar to CT), which not only needs to add some absorption or reflection X-ray band tracer particles in the sample to be tested, but also the imaging quality is the 2D projection of the ion passing path, and the experimental analysis depends on experienced staff and advanced algorithms. At the same time, the use of radioactive sources faces great regulatory pressure and increases the risk of physical and mental health damage to experimental personnel.

[0004] At present, for the measurement of rheological characteristics of the above-mentioned multi-phase dispersion system or polymer material, the existing rheometer cannot meet the requirement of accurate measurement. On the other hand, the measurement theory of the rheometer is based on laminar flow, while the deformation, breakage or coalescence of the dispersed phase droplets in the suspension may cause the shear flow in the rheometer measurement process to reach the state of turbulent flow or transition, resulting in increased error of rheological measurement data and lack of data analysis basis. Therefore, the material rheological behavior measurement process urgently needs a visualized measuring device to judge the reliability of rheological measurement data in real time and provide support for data analysis.

[0005] In specific rheological experiments, particularly in the study of liquids with special components such as polymer solutions, it has been found that data during the smooth operation of the testing instrument is generally uniform and stable, representing the general average properties of the measured liquid. However, at specific moments such as the initial and final moments of detection, the data feedback from the testing instrument often exhibits significant unique characteristics. Visualization devices aim to provide corresponding visualized data in real time, based on the data stream from the testing instrument, thereby analyzing the primary driving force and viscoelastic behavior in rheological testing under spatiotemporal synchronization. However, in the imaging process of existing experimental methods, the refraction phenomenon of the "liquid film" in ordinary circulating liquids causes optical imaging problems such as image blurring and distortion. This results in the visualization measurement data not being well corroborated with the testing instrument data, necessitating improvements to mitigate these effects and enhance image quality.

[0006] In conclusion, it is necessary to further innovate existing technologies. Summary of the Invention

[0007] To address the technical problems existing in the background art, this invention proposes a material rheological behavior visualization measurement device and its application method. Its concept is reasonable and can realize the visualization of flow field characteristics such as shear band, flow instability, and initiation flow during the rheological behavior measurement process, as well as the online and in-situ measurement of rheological parameters and micro-deformation characteristics of non-Newtonian fluids. It is convenient to combine with a rheometer to analyze the accuracy and reliability of rheological measurement data, and provide a technical solution for theoretical research on rheology of multiphase dispersion systems.

[0008] To solve the above-mentioned technical problems, the present invention provides a material rheological behavior visualization measurement device, which includes a transparent measuring cell, a cylindrical measuring rotor that is matched and embedded in the center of the transparent measuring cell (and a laser light source, a high-speed camera system, a constant temperature liquid bath, an online refractometer, an online density meter and a rotational rheometer matched and disposed on the outside of the transparent measuring cell).

[0009] The cylindrical measuring rotor includes a cylindrical rotor body and a connecting rod that is vertically fixed to the center of the top of the cylindrical rotor body; the top end of the connecting rod is matched and connected to the power output end of the rotary rheometer.

[0010] The transparent liquid bath measuring cell includes a transparent measuring cell body and a cylinder that is fitted into the center of the transparent measuring cell body; during the experiment, the cylindrical measuring rotor is entirely embedded in the cylinder.

[0011] The upper side of the transparent measuring pool body is matched with an upper circulating liquid port, and the lower side is matched with a lower circulating liquid port; the upper circulating liquid port is connected to the liquid inlet of the constant temperature liquid bath through a pipeline, and the lower circulating liquid port is connected to the liquid outlet of the online density instrument through a pipeline; the liquid outlet of the constant temperature liquid bath is connected to the liquid inlet of the online refractometer through a pipeline, and the liquid outlet of the online refractometer is connected to the liquid inlet of the online density instrument through a pipeline;

[0012] The lower chamber of the transparent measuring pool body is also matched with evenly arranged flow straightening plates below the cylindrical rotor body; and a cross laser collimator is arranged in the gap of the flow straightening plate located at the front of the bottom of the cylindrical rotor body; before the experiment, the cross laser collimator emits laser from the bottom of the transparent measuring pool body upwards to calibrate the center point mark at the bottom of the cylindrical rotor body, and the cross laser collimator is turned off during the experiment;

[0013] The laser light source is a high-frequency low-energy light source for providing a visual measurement light source.

[0014] The high-speed camera system is located below the laser light source to realize flow field visualization.

[0015] The material rheological behavior visualization measurement device, wherein the outer side wall of the cylindrical rotor body is uniformly provided with a through notch.

[0016] The material rheological behavior visualization measurement device, wherein the top and bottom of the cylindrical rotor body are provided with a guard slot along the circumferential edge.

[0017] The material rheological behavior visualization measurement device, wherein the cylindrical measuring rotor is made of anodized black aluminum material.

[0018] The material rheological behavior visualization measurement device, wherein the upper inside of the transparent measuring pool body is matched with a horizontally installed upper limiting flow plate, and the lower inside is matched with a horizontally installed lower limiting flow plate.

[0019] The central part of the upper limiting flow plate is provided with an upper through hole through which the cylindrical rotor can pass in the vertical direction; the central part of the lower limiting flow plate is provided with a lower through hole through which the cylindrical rotor can pass in the vertical direction.

[0020] The inner cavity of the transparent measuring pool body is divided into upper, middle and lower chambers by the upper limiting flow plate and the lower limiting flow plate; the cylindrical rotor passes through the upper through hole and the lower through hole in turn from top to bottom, and the upper end of the cylindrical rotor extends into the upper chamber of the transparent measuring pool body.

[0021] The material flow behavior visual measurement device, wherein: the lower chamber of the transparent measurement pool body is located below the lower through hole, and a flow buffering and rectifying area is formed by matching and arranging the rectifying plates vertically and spaced apart from each other; and the cross laser collimator is arranged in the gap between the rectifying plates directly below the lower through hole.

[0022] The material flow behavior visual measurement device, wherein: the liquid bath transparent measurement pool is made of pure quartz glass.

[0023] The material flow behavior visual measurement device, wherein: the high-speed camera system comprises an optical lens, a high-speed camera, and an image processing device.

[0024] An application method of a material flow behavior visual measurement device, comprising the following steps:

[0025] 1) Select the liquid bath transparent measurement pool to be used. Before first use, the refractive index adjustment test is performed according to the material of the liquid bath transparent measurement pool (2) using the two circulating liquids, so as to find the appropriate refractive index composition and ratio.

[0026] 2) Turn on the rotating rheometer and preheat it according to the requirements, then install the selected cylindrical measurement rotor on the rotor seat of the rotating rheometer, and perform self-checking of the rotating rheometer, the constant temperature liquid bath, the online refractometer, the online densitometer, the laser light source, and the high-speed camera.

[0027] 3) Connect the visual measurement device, and use the cross laser collimator to adjust and fix the liquid bath transparent measurement pool with the center of the rotor bottom on the rotating rheometer as the centering point.

[0028] 4) Use the calibrated refractive circulating liquid, set the experimental temperature, adjust the circulating flow, slowly fill the interlayer between the transparent measurement pool body and the inner pool of the measurement pool, and pay attention to bubble removal during the process.

[0029] 5) Carefully move the sample to be tested into the inner pool of the measurement pool, and adjust the rotating rheometer to slowly descend to the appropriate position. Wait for the experimental constant temperature for about 1-2 hours.

[0030] 6) Turn on the laser light source and the high-speed camera system, adjust the related parameters to the focal point required by the experiment, and make sure that the side surface of the cylindrical measurement rotor in the liquid bath transparent measurement pool is clear.

[0031] 7) Turn on the high-speed camera recording and determine that there is no error, then the experimenter starts the pre-set rotating rheometer to perform measurement.

[0032] 8) Before the rotation rheometer runs, the sample is placed in the selected sample cup, and the sample is sheared to produce deformation by applying a preset torque or rotational speed to the cylinder measuring rotor, to obtain the relationship between the deformation and stress of the measured fluid under shearing; wherein for the coaxial cylinder measuring rotor, the conversion between torque and shear stress, and the conversion between rotational speed and shear rate are shown in equations (1) and (2) respectively:

[0033]

[0034] In the above equations (1)-(2), τ is the shear stress; Ft is the torque; Rb is the outer diameter of the rotor; l is the height of the rotor; γ' is the shear rate; Rc is the inner diameter of the sample cup; and ω is the angular velocity of rotation;

[0035] Through the above steps 1)-8), the required rheological visualization information can be obtained.

[0036] With the above technical solution, the present application has the following beneficial effects:

[0037] The material rheological behavior visualization measurement device and the application method thereof have reasonable concepts, can realize the visualization of the shear band, flow instability, initial flow and other flow field characteristics in the rheological behavior measurement process, and can realize the online and in-situ measurement of the rheological parameters and micro deformation characteristics of the non-Newtonian fluid, thereby facilitating the analysis of the precision and reliability of the rheological measurement data in combination with the rheometer, and providing a technical solution for the rheological theory research of the multiphase dispersion system.

[0038] The present application can realize the simultaneous measurement of the macro rheological behavior and shear deformation of the non-Newtonian fluid, can be directly applied to the research of the medium rheological mechanism, and provides reliable data basis and image analysis materials for the establishment of the rheological model of the constitutive relationship of the complex system; the rheological measurement theory and technology of the multiphase dispersion system and the polymer are established, the existing rheometer measurement technology is reconstructed, and the high-precision visual information of the rheological characteristics measurement of the non-uniform or anisotropic medium is increased.

[0039] The present application can avoid the image blurring and distortion caused by the ordinary circulating liquid "liquid film" refraction phenomenon in the shooting process of the existing experimental method, can maximize the guarantee of the mutual verification of the rheological detection data and the fine image data under the condition of time and space synchronization, and can simultaneously realize the modular design of the measurement device, and help to increase or decrease according to the experimental requirements. BRIEF DESCRIPTION OF DRAWINGS

[0040] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0041] Figure 1 This is a schematic diagram of the overall structure of the material rheological behavior visualization measurement device of the present invention;

[0042] Figure 2 This is a cross-sectional view of the transparent measuring cell of the material rheological behavior visualization measuring device of the present invention;

[0043] Figure 3 This is a schematic diagram of the cylindrical measuring rotor of the material rheological behavior visualization measuring device of the present invention. Detailed Implementation

[0044] The technical solution of the present invention will now be clearly and completely described with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0045] The present invention will be further explained below with reference to specific embodiments.

[0046] like Figure 1 As shown, this embodiment provides a material rheological behavior visualization measurement device, including a cylindrical measuring rotor 1, a transparent measuring pool 2, a laser light source 3, a high-speed camera system 4, a constant temperature liquid bath 5, an online refractometer 6, an online density meter 7, and a rotational rheometer.

[0047] The cylinder measuring rotor 1 is an anodized black aluminum material, and when the light curtain of the laser light source 3 is used, the light path reflection can be prevented, and the surface is uniformly provided with a notch to prevent the rotor wall from slipping. The cylinder measuring rotor 1 includes a cylinder rotor body 11 and a connecting rod 12. The outer side wall of the cylinder rotor body 11 is uniformly provided with a through notch 13, which can prevent the cylinder rotor body 11 wall from slipping. The top and bottom of the cylinder rotor body 11 are provided with a height of about 5mm edge groove along the circumferential edge, which is integrally formed with the cylinder rotor body 11, and the main function is to isolate the interference of the test sample liquid on the top and bottom of the cylinder rotor body 11 caused by viscous friction. The material of the cylinder rotor body 11 is generally anodized black magnesium-silicon-aluminum alloy. For special applications, a titanium-magnesium alloy can be used to make the cylinder body, which is coated with a carbon nanotube coating to minimize its surface reflectivity. When the laser light curtain is irradiated, the light path reflection can be prevented, and the high-speed camera can be prevented from rotating and failing to shoot. The connecting rod 12 is vertically fixed to the top center of the cylinder rotor body 11 and connected to the power output end of the rotary rheometer.

[0048] The liquid bath transparent measuring pool 2 forms a coaxial cylinder measuring system with the cylinder measuring rotor 1, which is made of pure quartz glass material, which is convenient for laser penetration and realizes the visualization of the flow field in the rheological measurement process. The liquid bath transparent measuring pool 2 includes a transparent measuring pool body 21 and a measuring pool inner pool 22 matched and embedded in the central inside of the transparent measuring pool body 21. The cylinder measuring rotor 1 is embedded in the measuring pool inner pool 22.

[0049] The transparent measuring pool body 21 has an accommodation space inside, and the upper inside is matched with a horizontal installation of an upper limiting flow plate 211, and the lower inside is matched with a horizontal installation of a lower limiting flow plate 212. The central of the upper limiting flow plate 211 is vertically provided with an upper through hole 2111 through which the measuring pool inner pool 22 can pass, and the central of the lower limiting flow plate 212 is vertically provided with a lower through hole 2121 through which the measuring pool inner pool 22 can pass. The inner cavity of the transparent measuring pool body 21 is divided into three chambers by the upper limiting flow plate 211 and the lower limiting flow plate 212. The measuring pool inner pool 22 passes through the upper through hole 2111 and the lower through hole 2121 of the transparent measuring pool body 21 in turn from top to bottom, and the upper end of the measuring pool inner pool 22 extends into the upper chamber of the transparent measuring pool body 21.

[0050] The side wall of the upper chamber of the transparent measuring cell body 21 is matched with an upper circulating liquid port 213, and the side wall of the lower chamber is matched with a lower circulating liquid port 214; when self-checking, the upper circulating liquid port 213 is connected to the liquid inlet of the constant-temperature liquid bath tank 5 through a pipeline, and the lower circulating liquid port 214 is connected to the liquid outlet of the online density meter 7 through a pipeline; the liquid outlet of the constant-temperature liquid bath tank 5 is connected to the liquid inlet of the online refractometer 6 through a pipeline, and the liquid outlet of the online refractometer 6 is connected to the liquid inlet of the online density meter 7 through a pipeline; specifically, the constant-temperature liquid bath tank 5 pumps the constant-temperature circulating liquid bath into the online refractometer 6 through a pipeline to detect the refractive index, and after the detection of the refractive index, the online refractometer 6 passes the circulating liquid bath into the online density meter 7 through a pipeline to detect the density of the liquid bath, and after the detection of the density of the liquid bath, the liquid is passed into the interlayer between the transparent measuring cell body 21 and the measuring cell inner cell 22 through a pipeline, so that the temperature of the sample to be tested in the measuring cell inner cell 22 tends to be constant-temperature, and finally the liquid bath flowing out of the upper circulating liquid port 213 returns to the constant-temperature liquid bath tank 5 for recycling.

[0051] Meanwhile, the lower chamber of the transparent measuring cell body 21 is matched with a plurality of spaced rectifier plates 23 arranged vertically below the lower through hole 2121 and forms a flow buffering and rectifying area through the rectifier plates 23; a cross laser collimator 24 is arranged in the gap of the rectifier plate 23 directly below the lower through hole 2121 of the transparent measuring cell body 21, and before the experiment, the cross laser collimator 24 emits laser upward from the bottom of the transparent measuring cell body 21 to calibrate the center point mark at the bottom of the cylindrical rotor body 11, and the cross laser collimator 24 is closed during the experiment.

[0052] The liquid bath transparent measuring cell 2 and the cylindrical measuring rotor 1 form a coaxial cylindrical measuring system; the liquid bath transparent measuring cell 2 is made of pure quartz glass material, which is convenient for laser penetration and realizes the visualization of the flow field in the rheological measurement process.

[0053] After the liquid flow enters the lower chamber of the transparent measuring cell body 21, due to the action of the lower limiting plate 212, the circulating fluid is constrained to vertically upward annular jetting along the inner wall, and cooperating with the action of the upper limiting plate 211, the circulating fluid flows vertically upward in the detection field, and the flow layer closely adheres to the inner wall for heat exchange, so that the heat exchange efficiency is high, which is helpful to quickly constant-temperature the measuring cell inner cell 22 and shorten the experimental waiting time. In order to ensure the jetting intensity of the circulating fluid, the interlayer between the transparent measuring cell body 21 and the measuring cell inner cell 22 is made of quartz glass by fusion welding, and the upper circulating liquid port 213 and the lower circulating liquid port 214 are GL18 external thread structures, so as to be connected to the constant-temperature liquid bath tank 5; during the experiment, the cylindrical measuring rotor 1 rotates horizontally, and the controlled vertical flow of the circulating fluid will not interfere with the camera light path, avoiding the interference of the turbulent flow in the general water bath jacket beaker (the jacket water flow in the general jacket beaker used at present is turbulent, which will affect the refractometer) on the experimental results.

[0054] The transparent measuring pool body 21 is made of quartz glass, including a square shell, a circulating water inlet and an outlet, and a cavity between the transparent measuring pool body 21 and the measuring pool inner pool 22 is used for visualizing the correction of the measuring light path.

[0055] The laser light source 3 is matched and arranged outside the liquid bath transparent measuring pool 2, and is a high-frequency low-energy light source for providing a visual measuring light source.

[0056] The high-speed camera system 4 is also matched and arranged outside the liquid bath transparent measuring pool 2 and below the laser light source 3, and is used for realizing flow field visualization. The high-speed camera system 4 includes a high-speed camera, an optical lens mounted on the high-speed camera, and an image processing device. Generally, according to the experimental requirements, the laser light source 3 is arranged at an angle of 30-60° with the liquid bath transparent measuring pool 2, the laser light source 3 is aligned with the side wall of the cylindrical measuring rotor 1, and the high-speed camera is arranged opposite to the illuminated side wall of the cylindrical measuring rotor 1 to shoot the image of the laser illuminated part. The material flow behavior visualization measuring device composed of the cylindrical measuring rotor 1, the transparent measuring pool 2, the laser light source 3, the high-speed camera system 4, the rotary rheometer, and the instrument control operation computer can realize the visualization of the shear band, flow instability, and initial flow in the rheological behavior measurement process, and is convenient for analyzing the rheological measurement data.

[0057] The power output end of the rotary rheometer is connected with the cylindrical measuring rotor 1 through a rotor seat, and the connected cylindrical measuring rotor 1 is slowly lowered by the rotary rheometer to be immersed in the sample to be tested in the measuring pool inner pool 22 of the liquid bath transparent measuring pool 2. The rotary rheometer is integrated with a torque measuring instrument, a rotational speed detector, and a temperature sensor socket. The rotary rheometer provides a temperature sensor socket which can be connected to the inner wall of the measuring pool inner pool 22 as required. Generally, in the presence of the constant temperature liquid bath 5, the constant temperature after circulating the liquid bath in the jacket for 1-2 hours is used as the reference, and the material temperature is not detected alone to reduce the interference on the detection of the rotary rheometer.

[0058] The refractive index of the quartz glass to light decreases with the increase of the wavelength of light, and the refractive index is

[0059] In order to mask the texture of the optical glass in the laser imaging, the refractive index of the circulating liquid in the liquid bath transparent measuring pool 2 should be consistent with that of the quartz glass. The refractive index of the liquid is determined by the online detector 5 and fed back to the experimental personnel for adjustment.

[0060] At present, the two preferred circulating liquids are:

[0061] ① Zinc bromide (ZnBr2)-ethanol (CH3CH2OH) aqueous solution

[0062] The solution is based on saturated zinc bromide aqueous solution, and the refractive index is adjusted by adding 75% anhydrous ethanol dropwise. The adjustment range is 1.33-1.48.

[0063] ②XS275, XS255-150 mixed oil solution

[0064] XS275 and XS255-150 are two phenyl silicone oils, and the chemical nature is polymethylphenylsiloxane with different polymerization degrees. The refractive index of the oil solution is adjusted by mixing a certain proportion of XS255-150 based on XS275 in a circulating liquid bath. The adjustment range is 1.48-1.58.

[0065] Compared with the currently commonly used several optical solvents: THF (tetrahydrofuran, flammable and explosive, dangerous goods); DMF (N, N-dimethylformamide, multiple toxicities); DMSO (dimethyl sulfoxide, multiple toxicities); NMP: N-methyl pyrrolidone, colorless liquid, potential reproductive toxicity) The two circulating liquids prepared in this patent not only have low cost, but also are non-toxic and harmless. The low-refractive zinc bromide aqueous solution can be used for a long time under the storage condition of normal temperature and light avoidance, and the aqueous solution is stable when used within 80 DEG C; the mixed oil solution with high refractive index is a chemically inert polymethylphenylsiloxane, which can be stably used within 200 DEG C. The two circulating liquids are used in relay, and can provide a wide refractive correction range 1.33-1.58. This greatly expands the material selection range of future various types of liquid bath transparent measuring cells.

[0066] The transparent materials whose refractive index can be adjusted and corrected by the above-mentioned solutions at present include but are not limited to: PMMA (polymethyl methacrylate, organic glass), PC (polycarbonate), quartz glass (SiO2), boron glass, etc.

[0067] The application method of the material rheological behavior visual measurement device is as follows:

[0068] 1) Select the liquid bath transparent measuring cell 2 to be used. Before first use, the refractive index of the liquid bath transparent measuring cell 2 should be adjusted and tested according to the material of the liquid bath transparent measuring cell 2 using the two circulating liquids, and the appropriate refractive index and the proportion of the components are found.

[0069] 2) Turn on the rotational rheometer and preheat it according to the requirements, then install the selected cylinder measuring rotor 1 on the rotor seat of the rotational rheometer, and pass the self-checking of the rotational rheometer, the constant-temperature liquid bath tank 5, the online refractometer 6, the online densitometer 7, the laser light source 3 and the high-speed camera 4. During the self-checking process, that is, during the refractive index detection process of the online refractometer 6 and the liquid bath density detection process of the online densitometer 7, whether the refractive index of the liquid bath is appropriate is observed by the naked eye and the high-speed camera image, whether there is a clear "light refraction phenomenon" between the quartz glass wall of the transparent measuring pool body 21 and the transparent liquid bath, if there is, the proportion of different components in the formula is adjusted to improve the light refraction phenomenon of the liquid bath transparent measuring pool 2 at the set temperature, until such phenomenon disappears or is negligible. The density value is an important reference for refractive index adjustment, and the whole adjustment process needs to be carried out after the temperature fluctuation of the constant-temperature tank is less than ±0.5℃. Among them, the wavelength of the laser light source and the material of the liquid bath transparent measuring ruler determine the refractive index value, for example, when using a green laser light source with a wavelength of 527 nm, the measured value of the refractive index of the quartz glass material used at 527 nm is 1.4632, and the calculated value is 1.460, so the liquid bath refractive index should be adjusted according to the measured value. Select zinc bromide (ZnBr2)-ethanol (CH3CH2OH) aqueous solution as the liquid bath: after the saturated zinc bromide solution reaches the set temperature of the experiment, according to the refractive index value and the density value provided by the aforementioned instruments, anhydrous ethanol is added to the constant-temperature liquid bath tank to change the refractive index of the liquid bath to the approximate value mentioned above, and the instrument reading is observed, combined with the naked eye and camera image. All medium adjustments should be carried out after the temperature tends to be constant to avoid the influence of temperature changes on the refractive index caused by changes in the density of the liquid bath medium. The refractive index of more materials or wavelength light sources can be calculated by the Sellmeier dispersion equation to obtain the approximate value. And debug according to the foregoing steps.

[0070] 3) Connect the material flow behavior visualization measurement device of the application, and use the cross laser collimator 24 to adjust and fix the liquid bath transparent measuring pool 2 with the rotor bottom center on the rotational rheometer as the centering point.

[0071] 4) Use the calibrated refractive cycle liquid, set the experimental temperature, adjust the circulation flow rate through the ball valve at the outlet of the constant-temperature liquid bath tank 5, slowly fill the interlayer between the transparent measuring pool body 21 and the measuring pool inner pool 22, and pay attention to the bubble removal during the process.

[0072] 5) Carefully move the sample to be tested into the measuring pool inner pool 22, and adjust the rotational rheometer to slowly descend to the appropriate position, and wait for the experimental constant temperature for about 1-2 hours.

[0073] 6) After the above process is completed, the laser light source 3 and the high-speed camera are turned on, and the related parameters are adjusted to the focus required by the experiment, generally, the side of the cylindrical measuring rotor 1 in the transparent measuring bath 2 of the liquid bath is clearly visible; if it is a particle suspension, the particle is focused.

[0074] 7) After starting the video and confirming that there is no error, the experimenter starts the pre-set rotational rheometer program to measure.

[0075] 8) Before the rotational rheometer runs, the sample is placed in the selected measuring bath 22, and the sample is sheared to produce deformation by applying a pre-set torque or rotational speed to the cylindrical measuring rotor 1, and the relationship between the deformation of the measured fluid under shear and the force is obtained. Among them, for the coaxial cylinder rotor, the conversion between torque and shear stress, and the conversion between rotational speed and shear rate are shown in equations (1) and (2) respectively:

[0076]

[0077] In equations (1)-(2), τ is the shear stress; Ft is the torque; Rb is the outer diameter of the rotor; l is the height of the rotor; γ' is the shear rate; Rc is the inner diameter of the sample cup; and ω is the angular velocity of rotation.

[0078] By this method, the required rheological visualization information can be conveniently obtained.

[0079] The present application has reasonable concept, and can realize the visualization of shear band, flow instability, initial flow and other flow field characteristics in the rheological behavior measurement process, and the online and in-situ measurement of rheological parameters and micro deformation characteristics of non-Newtonian fluid, which is convenient for analyzing the precision and reliability of rheological measurement data by matching the rheometer, and provides a technical solution for the theoretical research of multiphase dispersion system rheology.

[0080] Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present application, and not to limit them; although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the foregoing embodiments, or make equivalent substitutions for part or all of the technical features; and these modifications or substitutions do not make the essence of the corresponding technical solution deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A material flow behavior visual measurement device, characterized by: The visual measurement device comprises a transparent measurement pool (2), a cylindrical measurement rotor (1) matched and embedded in the center inside the transparent measurement pool (2), and a laser light source (3), a high-speed camera system (4), a constant-temperature liquid bath (5), an online refractometer (6), an online density meter (7) and a rotary rheometer matched and arranged outside the transparent measurement pool (2). The cylindrical measurement rotor (1) comprises a cylindrical rotor body (11) and a connecting rod (12) matched and vertically fixed to the top center of the cylindrical rotor body (11); the top end of the connecting rod (12) is matched and connected with the power output end of the rotary rheometer. The liquid-bath transparent measurement pool (2) comprises a transparent measurement pool body (21) and a cylinder (22) matched and embedded in the center inside the transparent measurement pool body (21); during the experiment, the cylindrical measurement rotor (1) is embedded in the cylinder (22) as a whole. An upper circulating liquid port (213) is matched and arranged on one side of the upper part of the transparent measurement pool body (21), and a lower circulating liquid port (214) is matched and arranged on one side of the lower part of the transparent measurement pool body (21); the upper circulating liquid port (213) is connected to the liquid inlet of the constant-temperature liquid bath (5) through a pipeline, and the lower circulating liquid port (214) is connected to the liquid outlet of the online density meter (7) through a pipeline; the liquid outlet of the constant-temperature liquid bath (5) is connected to the liquid inlet of the online refractometer (6) through a pipeline, and the liquid outlet of the online refractometer (6) is connected to the liquid inlet of the online density meter (7) through a pipeline. The lower chamber of the transparent measurement pool body (21) is further matched and uniformly provided with a flow straightener (23) below the cylindrical rotor body (11); and a cross laser collimator (24) is arranged in the gap of the flow straightener (23) at the bottom of the cylindrical rotor body (11); before the experiment, the cross laser collimator (24) emits laser from the bottom of the transparent measurement pool body (21) upwards to calibrate the center point mark at the bottom of the cylindrical rotor body (11), and the cross laser collimator (24) is turned off during the experiment. The laser light source (3) is a high-frequency low-energy light source for providing a visual measurement light source. The high-speed camera system (4) is located below the laser light source (3) and is used for realizing flow field visualization.

2. The material flow behavior visualizing measuring device according to claim 1, characterized in that The outer side wall of the cylindrical rotor body (11) is uniformly provided with a through notch (13).

3. The material flow behavior visualizing measuring device according to claim 1, characterized in that The top and bottom of the cylindrical rotor body (11) are provided with edge protection grooves along the circumferential edge.

4. The material flow behavior visualizing measuring device according to claim 1, characterized in that: The cylindrical measurement rotor (1) is made of anodized black aluminum material.

5. The material flow behavior visualizing measuring device according to claim 1, characterized in that An upper flow limiting plate (211) is matched and horizontally mounted on the inner side of the upper part of the transparent measurement pool body (21), and a lower flow limiting plate (212) is matched and horizontally mounted on the inner side of the lower part of the transparent measurement pool body (21). An upper through hole (2111) is vertically and throughly provided in the center of the upper flow limiting plate (211) and can be passed through by the cylinder (22); a lower through hole (2121) is vertically and throughly provided in the center of the lower flow limiting plate (212) and can be passed through by the cylinder (22) in the axial direction. The inner cavity of the transparent measuring pool body (21) is divided into upper, middle and lower chambers by the upper and lower flow limiting plates (211) and (212); the cylinder (22) passes through the upper and lower through holes (2111) and (2121) in sequence from top to bottom, and the upper end thereof extends into the upper chamber of the transparent measuring pool body (21).

6. The material flow behavior visualizing measuring device according to claim 1, characterized in that The lower chamber of the transparent measuring pool body (21) is located below the lower through hole (2121) and matches the rectifier plate (23) arranged vertically and spaced apart from each other and forms a flow buffering rectification area through the rectifier plate (23); the cross laser collimator (24) is arranged in the gap between the rectifier plates (23) directly below the lower through hole (2121).

7. The material flow behavior visualizing measuring device according to claim 1, characterized in that The liquid bath transparent measuring pool (2) is made of pure quartz glass.

8. The material flow behavior visualizing measuring device according to claim 1, characterized in that The high-speed camera system (4) comprises an optical lens, a high-speed camera and an image processing device.

9. Use of a device for visual measurement of flow behavior of a material according to any one of claims 1 to 8, characterized in that The method comprises the following steps: 1) Select the liquid bath transparent measuring pool (2) to be used, and before first use, the refractive index adjustment test is performed on the liquid bath transparent measuring pool (2) according to the two kinds of circulating liquids mentioned above according to the material of the liquid bath transparent measuring pool (2) to find the appropriate refractive index coefficient composition and proportion; 2) Start the rotating rheometer according to the requirements, then install the selected cylinder measuring rotor (1) on the rotor seat of the rotating rheometer, and perform self-checking on the rotating rheometer, the constant temperature liquid bath (5), the online refractometer (6), the online density meter (7), the laser light source (3) and the high-speed camera (4); 3) Connect the visual measurement device, and use the cross laser collimator (24) to take the center of the rotor bottom of the rotating rheometer as the centering point, adjust and fix the liquid bath transparent measuring pool (2); 4) Use the calibrated refractive circulating liquid, set the experimental temperature, adjust the circulating flow, slowly fill the interlayer between the transparent measuring pool body (21) and the measuring pool inner pool (22), and pay attention to bubble removal during the process; 5) Carefully move the sample to be tested into the measuring pool inner pool (22), adjust the rotating rheometer to slowly descend to the appropriate position, and wait for the experimental constant temperature for about 1-2 hours; 6) Turn on the laser light source (3) and the high-speed camera system (4), adjust the related parameters to the focus point required by the experiment, and clearly see the side of the cylinder measuring rotor (1) in the liquid bath transparent measuring pool (2) as the criterion; 7) After starting the high-speed camera recording and determining that there is no error, the experimenter starts the pre-set rotating rheometer to measure; 8) Before the rotating rheometer runs, place the sample in the selected sample cup, apply a preset torque or rotating speed to the cylinder measuring rotor (1) to shear the sample to produce deformation, and obtain the relationship between the deformation and the stress of the measured fluid under shearing; wherein for the coaxial cylinder measuring rotor (1), the conversion between the torque and the shear stress, and the conversion between the rotating speed and the shear rate are respectively shown in formulas (1) and (2): In the above formulas (1)-(2), τ is the shear stress; Ft is the torque; Rb is the outer diameter of the rotor; l is the height of the rotor; γ' is the shear rate; Rc is the inner diameter of the sample cup; ω is the angular velocity of rotation; The rheological visual information required can be obtained through the above steps 1)-8).

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