A multi-dimensional visual micro-force measuring device and measuring method

Abstract

The application relates to a multi-dimensional visual micro-force measuring device and a measuring method, and relates to the technical field of experimental measuring devices.The device comprises a high-pressure reaction cavity, a three-dimensional moving table, a moving-end glass fiber, a fixed-end glass fiber and an image and data acquisition system; the moving-end glass fiber is fixed on the three-dimensional moving table, and the fixed glass fiber is fixed on the inner wall of the high-pressure reaction cavity; a first observation window is arranged at the top of the high-pressure reaction cavity, a second observation window is arranged on one side of the high-pressure reaction cavity, and the image and data acquisition system is used to realize the measurement of two forms of micro-forces between hydrate particles-hydrate particles, hydrate particles-droplets-wall surfaces. The application can accurately measure the micro-forces between hydrate particles-hydrate particles, hydrate particles-droplets-wall surfaces in a high-pressure gas main system through multi-dimensional and multi-angle observation, and further evaluate the effect of a "double-effect" inhibitor in "preventing particle aggregation and preventing particle wall adhesion".

Description

Technical Field

[0001] This invention relates to the field of experimental measurement device technology, specifically to a multidimensional visualization microscopic force measurement device and method. Background Technology

[0002] Natural gas hydrates are non-stoichiometric cage-like crystals formed from small-molecule gases and water. Their resources are vast, generally found in shallow deep-sea strata or permafrost, and are considered an important alternative energy source for the 21st century. However, in deep-sea oil and gas development and subsea pipeline transportation, natural gas and water produced from the formation can also form hydrates under the low-temperature, high-pressure environment of the seabed. These hydrates are carried by fluids in pipelines, migrate, deposit, and adhere to the pipe walls, reducing the pipeline's flow area and even completely clogging wells or pipelines, causing serious economic losses. The issue of hydrate flow assurance has become a major challenge restricting the safe and efficient development and transportation of deep-sea oil and gas.

[0003] Currently, the most common method for preventing hydrate formation is to inject excessive amounts of thermodynamic inhibitors to completely remove the wellbore or gathering pipeline from the hydrate formation zone. However, this method requires large amounts of inhibitors, generally above 50 wt%, resulting in high costs. Furthermore, methanol-based chemicals are highly toxic and can easily cause serious environmental problems. Kinetic inhibitors, which are more widely studied, are difficult to apply in deep-sea environments due to their inability to withstand high supercooling conditions. In recent years, hydrate risk management strategies have gradually gained acceptance in the field. This strategy uses low-dose inhibitors (0.5~2 wt%) such as polymerization inhibitors to allow hydrate formation while preventing interparticle aggregation and pipe wall adhesion, dispersing them in a continuous phase. This method prevents hydrates from agglomerating and clogging pipelines, and also improves pipeline transport capacity through hydrate formation, making it a hot research topic. However, the evaluation methods for this "dual-effect" hydrate inhibitor are limited. Macroscopic evaluation can only be performed through high-pressure reactors or flow loop experiments, and the "dual-effect" performance of the inhibitor in "inhibiting particle aggregation and preventing particle adhesion" cannot be evaluated microscopically.

[0004] Currently, researchers have proposed using micro-force measurement devices (MMF) to measure the forces between hydrate particles, thereby directly characterizing the performance of polymerization inhibitors. However, this method has several drawbacks: Firstly, it only allows for one-dimensional observation, which can easily lead to the particles being misaligned during measurement. Adjustments can only be made by ensuring both particles are in sharp focus simultaneously. Secondly, it cannot observe the morphology of hydrate particles from opposite perspectives. If hydrate particles are crushed during formation, resulting in uneven surfaces, this cannot be observed in one-dimensional measurements, leading to insufficient contact between the measured objects. Thirdly, simply applying existing methods for measuring particle-particle forces to measuring particle-droplet-wall forces can easily result in issues such as droplet deformation due to gravity. All these problems contribute to significant measurement errors.

[0005] In view of this, there is an urgent need for a microscopic force measurement device that can be visualized in multiple dimensions, and to improve existing measurement devices to meet the microscopic evaluation and testing functions of "dual-effect" inhibitors. Summary of the Invention

[0006] The purpose of this invention is to provide a multidimensional visualization microscopic force measurement device and method, which can accurately measure the microscopic forces between hydrate particles and between hydrate particles, droplets and walls in a high-pressure gas-dominated system through multidimensional and multi-view observation, thereby evaluating the effectiveness of the "dual-effect" inhibitor in "preventing particle aggregation and preventing particle adhesion to the tube wall".

[0007] To achieve the above objectives, this invention provides a multidimensional visualization microscopic force measurement device, comprising: a high-pressure reaction chamber, a three-dimensional moving stage, a moving end glass fiber, a fixed end glass fiber, and an image and data acquisition system; the three-dimensional moving stage is disposed within the high-pressure reaction chamber and is capable of three-dimensional movement in xyz; the moving end glass fiber is fixed to the three-dimensional moving stage, and the fixed end glass fiber is fixed to the inner wall of the high-pressure reaction chamber, corresponding to the position of the moving end glass fiber; a first observation window is provided at the top of the high-pressure reaction chamber, and a second observation window is provided on one side of the high-pressure reaction chamber; the image and data acquisition system is used to determine whether the research object is located on the same horizontal or vertical line, and to accurately observe the hydrate formation morphology in the blind spot of the field of view and determine whether the current particle can meet the experimental requirements, ultimately realizing the measurement of two forms of microscopic forces: hydrate particle-hydrate particle and hydrate particle-droplet-wall interaction.

[0008] Furthermore, the image and data acquisition system includes a first microscopic observation mirror, a second microscopic observation mirror, a pressure sensor, a temperature sensor, and a data acquisition terminal. The first microscopic observation mirror is vertically aligned with a first observation window to observe the measurement process from a top-down perspective, and the second microscopic observation mirror is vertically aligned with a second observation window to observe the measurement process from a side perspective, thereby achieving multi-dimensional visualization measurement during the experiment. Both the pressure sensor and the temperature sensor are connected to the high-pressure reaction chamber to monitor temperature and pressure changes in real time. The first microscopic observation mirror, the second microscopic observation mirror, the pressure sensor, and the temperature sensor are all connected to the data acquisition terminal via high-definition signal cables.

[0009] Furthermore, three-dimensional shifting linkages are respectively installed on the three sides of the high-pressure reaction chamber. One end of the three-dimensional shifting linkage extends into the high-pressure reaction chamber and is connected to the three-dimensional moving stage, which is used to drive the three-dimensional moving stage to achieve three-dimensional movement in xyz.

[0010] Furthermore, the fixed form of the movable glass fiber is divided into horizontal fixed and vertical fixed according to the different measurement objects. The horizontally fixed is the movable glass fiber one, which is mainly used to measure the interaction force between hydrate particles and hydrate particles. The vertically fixed is the movable glass fiber two, which is mainly used to measure the interaction force between hydrate particles, droplets and wall.

[0011] Furthermore, both the first and second observation windows are composed of two layers of glass, with the inner glass layer made of sapphire and the outer glass layer made of acrylic glass.

[0012] Furthermore, it also includes an air intake system, which includes a high-pressure air source and an air cooling coil. The high-pressure air source is connected to the high-pressure reaction chamber through the air cooling coil, and a pressure gauge is installed on the pipeline connecting the high-pressure air source and the air cooling coil.

[0013] Furthermore, it also includes a low-temperature water bath system, which includes a low-temperature water bath tank filled with ethylene glycol antifreeze. The tank is connected to the outer jacket of the high-pressure reaction chamber via a hose. A circulating pump is used to circulate the antifreeze between the low-temperature water bath tank and the outer jacket to maintain the experimental temperature inside the high-pressure reaction chamber.

[0014] A multidimensional visualization method for measuring microscopic forces includes the following steps:

[0015] (1) Experimental preparation stage: The temperature of the high pressure reaction chamber was reduced to -7~-10℃ using a low temperature water bath system. Two glass fiber elastic coefficients were selected and measured. Ice particles containing "dual-effect" inhibitors were prepared at the tip of the fixed glass fiber using liquid nitrogen. Ice particles or carbon steel with droplets were prepared at the tip of the moving glass fiber. The fixed glass fiber with ice particles was fixed at the fixed end of the reactor body. The moving glass fiber with ice particles / carbon steel was fixed on the three-dimensional moving stage in the high pressure reaction chamber and the reactor body was quickly sealed.

[0016] (2) Hydrate particle induction stage: Open the vent valve to evacuate the high-pressure reaction chamber. The high-pressure gas source slowly adds methane into the high-pressure reaction chamber through the gas cooling coil. After reaching the predetermined experimental pressure, close the high-pressure gas source and the gas cooling coil, raise the temperature of the high-pressure reaction chamber to -1℃, and then raise the temperature of the high-pressure reaction chamber to 1.7℃. During this process, the ice particles melt and generate hydrate particles under the action of high-pressure methane gas.

[0017] (3) Adhesion test stage: The three-dimensional moving stage is controlled by three three-dimensional shifting linkages to move along the xyz three-dimensional axis so that the center of the test object at the moving end and the center of the hydrate particle at the fixed end are on the same horizontal line or the same vertical line. Then, the three three-dimensional shifting linkages are manipulated to make the test object at the moving end approach the hydrate particle at the fixed end at a uniform speed. After the two objects come into contact, the moving end is pressed to displace the fixed end by 0.3 mm. After the two objects come into contact for 10 seconds, they are slowly pulled apart at a uniform speed. The separation process of the two objects is captured in real time using the image and data acquisition system. The displacement of the fixed end is converted into the actual displacement. The micro force is solved using Hooke's law and corrected using the harmonic radius. The average value of the measured results is taken.

[0018] (4) After the experiment, release the pressure using the vent valve.

[0019] Further, in the experimental preparation stage, the vent valve is opened and a vacuum pump is used to evacuate the inside of the high-pressure reaction chamber. The pressure inside the high-pressure reaction chamber is read by a pressure sensor. When the pressure stabilizes above -0.008MPa for 10 minutes, it indicates that the chamber is well sealed. The vent valve is then closed and the formal experiment begins.

[0020] Furthermore, the method for determining whether the center of the object under test is located on the same horizontal or vertical line is as follows:

[0021] If the moving end is a hydrate particle, the moving end and the fixed end will be displaced in the x direction, thus making the centers of the hydrate particles at the moving end and the hydrate particles at the fixed end located on the same horizontal line. This process is judged by the side view of the second observation window, and the judgment criterion is whether the glass fibers at the moving end and the glass fibers at the fixed end are completely overlapped.

[0022] If the moving end is a droplet-wall, the moving end and the fixed end will be displaced in the z direction, thus making the center of the droplet-wall at the moving end and the center of the hydrate particle at the fixed end on the same vertical line. This process is judged by the top view of the first observation window, and the judgment criterion is whether the glass fiber at the moving end and the glass fiber at the fixed end are completely overlapped.

[0023] Furthermore, the force between hydrate particles is measured mainly by recording the displacement between the measured objects from a top-down perspective using a first microscope and a first observation window, while the displacement between the hydrate particles, droplets, and the wall is measured mainly by recording the displacement between the measured objects from a side-view perspective using a second microscope and a second observation window.

[0024] The beneficial effects of this invention are as follows:

[0025] 1. Overcoming the limitations of the original device in measuring the micro-force between hydrate particles, droplets and the wall surface due to the severe deformation of droplets caused by gravity, the device innovatively adopts a vertical fixing method for the moving end, providing a new method for measuring the micro-force between hydrate particles, droplets and the wall surface;

[0026] 2. Existing single-viewing-window observation systems cannot observe mobile devices in a vertically fixed manner. Furthermore, a single viewing window cannot accurately determine whether two research objects are located on the same horizontal or vertical line; it can only vaguely judge by whether both objects are simultaneously in focus. This invention innovatively sets up a first and a second observation window and employs an image and data acquisition system for multi-dimensional observation. This ensures the measurement of two forms of microscopic forces: hydrate particle-hydrate particle and hydrate particle-droplet-wall, enabling a comprehensive evaluation of the inhibitor's dual-effect performance in "inhibiting particle aggregation and preventing particle adhesion." It also provides an accurate criterion for determining whether research objects are located on the same horizontal or vertical line by observing whether the glass fibers overlap.

[0027] 3. Existing single-viewing-window observation systems cannot accurately observe the formation morphology of hydrates in blind spots and determine whether the current particles meet experimental requirements. This invention innovatively sets up a first observation window and a second observation window, and uses an image and data acquisition system to observe the formation morphology of hydrate particles in multiple dimensions, ensuring the smoothness of the measured object surface, improving experimental standards and greatly reducing experimental errors. Attached Figure Description

[0028] Figure 1 This is a schematic diagram of the structure of the present invention.

[0029] In the figure:

[0030] 1-High-pressure gas source, 2-Pressure gauge, 3-First microscopic observation mirror, 4-Second microscopic observation mirror, 5-Pressure sensor, 6-Temperature sensor, 7-Gas cooling coil, 8-Data acquisition terminal, 9-Low-temperature water bath, 10-First observation window, 11-Second observation window, 12-High-pressure reaction chamber, 13-Three-dimensional shifting linkage, 14-Three-dimensional moving stage, 15-Moving end glass fiber one, 16-Fixed end glass fiber, 17-Glass fiber fixed support, 18-Moving end glass fiber two, V1-Pressure reducing valve, V2-Inlet valve, V3-Vent valve. Detailed Implementation

[0031] To achieve the above objectives and effects, the technical means and structure adopted by the present invention will be described in detail with reference to the accompanying drawings, focusing on the features and functions of the preferred embodiments of the present invention.

[0032] like Figure 1 As shown, this invention provides a multidimensional visualization microscopic force measurement device, comprising: a high-pressure reaction chamber 12, a three-dimensional moving stage 14, a moving glass fiber, a fixed glass fiber 16, and an image and data acquisition system. The three-dimensional moving stage 14 is disposed within the high-pressure reaction chamber 12 and can achieve three-dimensional movement (x, y, z). The moving glass fiber is fixed to the three-dimensional moving stage 14, and the fixed glass fiber is fixed to the inner wall of the high-pressure reaction chamber 12 by a glass fiber fixing support 17, corresponding to the position of the moving glass fiber. A first observation window 10 is provided at the top of the high-pressure reaction chamber 12, and a second observation window 11 is provided on one side of the high-pressure reaction chamber 12. The image and data acquisition system is used to determine whether the research object is located on the same horizontal or vertical line, and to accurately observe the hydrate formation morphology in the blind spot of the field of view and determine whether the current particle can meet the experimental requirements. Ultimately, it realizes the measurement of two forms of microscopic forces: hydrate particle-hydrate particle and hydrate particle-droplet-wall. The high-pressure reaction chamber 12 can withstand a pressure of 25 MPa. The inner wall of the vessel is equipped with glass fiber slots for placing the fixed-end research object; similarly, glass fiber slots are installed on the three-dimensional moving platform inside the vessel for placing the moving-end research object. During the measurement process, the glass fiber 16 at the fixed end should be thinner than the glass fiber at the moving end, so that the glass fiber 16 at the fixed end will undergo a larger displacement under force, resulting in a larger measured microscopic force and reducing experimental error.

[0033] The image and data acquisition system includes a first microscopic observation mirror 3, a second microscopic observation mirror 4, a pressure sensor 5, a temperature sensor 6, and a data acquisition terminal 8. The first microscopic observation mirror 3 is vertically aligned with the first observation window 10 to observe the measurement process from a top-down perspective, and the second microscopic observation mirror 4 is vertically aligned with the second observation window 11 to observe the measurement process from a side perspective, thereby achieving multi-dimensional visualization measurement during the experiment. The pressure sensor 5 and the temperature sensor 6 are both connected to the high-pressure reaction chamber 12 to monitor temperature and pressure changes in real time. The first microscopic observation mirror 3, the second microscopic observation mirror 4, the pressure sensor 5, and the temperature sensor 6 are all connected to the data acquisition terminal 8 via high-definition signal cables. Temperature and pressure data and image data are collected by the acquisition system for subsequent data processing.

[0034] In this embodiment, three-dimensional shifting rods 13 are respectively installed on the three sides of the high-pressure reaction chamber 12. One end of the three-dimensional shifting rod 13 extends into the high-pressure reaction chamber 12 and is connected to the three-dimensional moving stage 14 to drive the three-dimensional moving stage 14 to achieve xyz three-dimensional movement.

[0035] In this embodiment, the fixed form of the movable glass fiber is divided into horizontal fixing and vertical fixing depending on the measurement object. The horizontally fixed movable glass fiber 15 is mainly used to measure the interaction force between hydrate particles, while the vertically fixed movable glass fiber 18 is mainly used to measure the interaction force between hydrate particles, droplets, and the wall. This solves the problem that current methods for measuring the microscopic interaction force between hydrate particles, droplets, and the wall simply use the method of measuring the interaction force between hydrate particles, which all use the method of horizontal fixing of the movable glass fiber. However, this method is prone to large deformation of the wall particles due to gravity, resulting in large errors. The tip of the fixed glass fiber 16 can be made and placed with hydrate particles by ice particle induction. The movable glass fiber can adopt two fixing methods depending on the research object. If the research object is hydrate particles, the horizontally fixed movable glass fiber 15 is used; if the research object is droplets and the wall, the vertically fixed movable glass fiber 18 is used.

[0036] In this embodiment, both the first observation window 10 and the second observation window 11 are composed of two layers of glass. The inner glass layer is made of sapphire, and the outer glass layer is made of acrylic. The purpose of the double-layered glass windows is to prevent water vapor from forming due to temperature differences. Two optical microscopes are installed, one perpendicular to the first observation window 10 and the other perpendicular to the second observation window 11, respectively, to observe the position and shape of the object under test in real time. The two microscopes are named the first observation system and the second observation system, respectively. The first observation system is perpendicular to the first observation window 10 in the z-direction of the top of the high-pressure reaction chamber 12, and observes the measurement process from a top-down perspective. The second observation system is perpendicular to the second observation window 11 in the negative x-direction of the high-pressure reaction chamber 12, and observes the measurement process from a side-view perspective.

[0037] The first observation system has two practical uses for top-down observation: First, when measuring the force between hydrate particles, the direction of particle motion is the x-direction, and this angle is perpendicular to the direction of particle motion, which allows for the observation of the displacement of particles at the fixed end and the calculation of the microscopic force between particles; Second, when measuring the force between hydrate particles, droplets, and the wall, the direction of wall motion is the z-direction, and the top-down angle is parallel to the direction of wall motion, which allows for the determination of whether the center point of the hydrate particle and the wall is located on the same vertical line by checking whether the two glass fibers overlap.

[0038] The second observation system has two practical functions in side-view observation. First, when measuring the force between hydrate particles, the direction of particle motion is the x-direction. This viewing angle is parallel to the direction of particle motion, and it is possible to determine whether the center points of hydrate particles are located on the same horizontal line by whether the two glass fibers overlap. Second, when measuring the force between hydrate particles, droplets, and the wall, the direction of wall motion is the z-direction. The side-view is perpendicular to the direction of wall motion, and it is possible to observe the displacement of the fixed-end particles and then calculate the microscopic force between hydrate particles, droplets, and the wall.

[0039] The simultaneous use of two observation systems allows for multi-dimensional observation of the morphology of generated hydrate particles, avoiding blind observation due to blind spots and preventing experiments from being conducted blindly.

[0040] The present invention also includes an intake system comprising a high-pressure gas source 1 and a gas path cooling coil 7. The high-pressure gas source 11 is connected to the high-pressure reaction chamber 12 via a pressure reducing valve V1, a pressure gauge 2, the gas path cooling coil 7, and an intake valve V2. A pressure gauge 2 is installed on the pipeline connecting the high-pressure gas source 1 and the gas path cooling coil 7. High-pressure methane gas in the high-pressure gas source 1 enters the high-pressure reaction chamber 12 through the gas path cooling coil 7, providing a high-pressure environment and gas source for hydrate formation.

[0041] The present invention also includes a low-temperature water bath system, comprising a low-temperature water bath tank 9 filled with ethylene glycol antifreeze, which is connected to the outer jacket of the high-pressure reaction chamber 12 via a hose. A circulation pump circulates the antifreeze between the low-temperature water bath tank 9 and the outer jacket to maintain the experimental temperature inside the high-pressure reaction chamber 12. The outer jacket is connected to the low-temperature water bath tank 9 via an inlet and an outlet, and the water bath temperature can be lowered to as low as -20°C, providing low-temperature conditions for the formation of hydrates within the high-pressure reaction chamber 12.

[0042] A multidimensional visualization method for measuring microscopic forces includes an experimental preparation stage, a hydrate formation stage, an adhesion force testing stage, and an experimental conclusion stage, specifically comprising the following steps:

[0043] (1) Experimental preparation stage: The temperature of the high pressure reaction chamber was reduced to -7~-10℃ and stabilized for half an hour using a low temperature water bath system. Two glass fiber elastic coefficients were selected and measured. Ice particles containing "dual-effect" inhibitors were prepared at the tip of the fixed glass fiber using liquid nitrogen. Ice particles or carbon steel with droplets were prepared at the tip of the moving glass fiber using the same method. The fixed glass fiber with ice particles was fixed at the fixed end of the reactor body. The moving glass fiber with ice particles / carbon steel was fixed on the three-dimensional moving stage in the high pressure reaction chamber and the reactor body was quickly sealed.

[0044] (2) Hydrate particle induction stage: Open the vent valve to evacuate the high-pressure reaction chamber. The high-pressure gas source slowly adds methane into the high-pressure reaction chamber through the gas cooling coil. The experimental pressure is generally controlled at 7-10 MPa. After reaching the predetermined experimental pressure, the high-pressure gas source and the gas cooling coil are turned off. The temperature inside the high-pressure reaction chamber is raised to -1℃ and stabilized for half an hour. The purpose of this is to ensure that the surface of the ice particles is smooth. Then the temperature of the high-pressure reaction chamber is raised to 1.7℃ and stabilized for two hours. During this process, the ice particles melt and generate hydrate particles under the action of high-pressure methane gas. The purpose of stabilizing for two hours is to ensure that the outer shell of the hydrate particles is hard enough.

[0045] (3) Adhesion test stage: The three-dimensional moving stage is controlled by three three-dimensional shifting linkages to move along the xyz three-dimensional axis so that the center of the test object at the moving end and the hydrate particle at the fixed end are on the same horizontal line or the same vertical line. At the same time, the surface of the test object is observed in multiple dimensions through the first observation system and the second observation system to see if it is smooth. If the experimental conditions are met, the three three-dimensional shifting linkages are then manipulated to make the test object at the moving end approach the hydrate particle at the fixed end at a uniform speed. After the two objects come into contact, the moving end is pressed to displace the fixed end by 0.3 mm. After the two objects come into contact for 10 seconds, they are slowly pulled apart at a uniform speed. The separation process of the two objects is captured in real time using the image and data acquisition system, and the displacement of the fixed end is converted into the actual displacement. The Hooke's law is used to solve the micro force and the harmonic radius is used for correction. The experiment is repeated 40 times and the average value of the measured results is taken.

[0046] (4) After the experiment, release the pressure using the vent valve.

[0047] In this embodiment, during the experimental preparation stage, the vent valve V3 is first opened to evacuate the high-pressure reaction chamber using a vacuum pump. The pressure inside the high-pressure reaction chamber is read by a pressure sensor. When the pressure stabilizes above -0.008MPa for 10 minutes, it indicates that the chamber is well sealed. The vent valve V3 is then closed, and the formal experiment begins.

[0048] In this embodiment, the method for determining whether the center of the object to be tested is located on the same horizontal or vertical line is as follows:

[0049] If the moving end is a hydrate particle, the moving end and the fixed end will be displaced in the x direction, thus making the centers of the hydrate particles at the moving end and the hydrate particles at the fixed end located on the same horizontal line. This process is judged by the side view of the second observation window, and the judgment criterion is whether the glass fibers at the moving end and the glass fibers at the fixed end are completely overlapped.

[0050] If the moving end is a droplet-carbon steel wall, the moving end and the fixed end will be displaced in the z direction, thus making the droplet-carbon steel wall of the moving end and the center of the hydrate particle of the fixed end located on the same vertical line. This process is judged by the top view of the first observation window, and the judgment criterion is whether the glass fiber of the moving end and the glass fiber of the fixed end are completely overlapped.

[0051] This invention overcomes the limitations of existing devices in measuring the micro-forces between hydrate particles, droplets, and the wall surface, where droplets are severely deformed due to gravity. It innovatively employs a vertically fixed moving end, providing a new method for measuring these micro-forces. Existing single-viewing-window observation systems cannot observe vertically fixed moving ends, and a single viewing window cannot accurately determine whether two objects are on the same horizontal or vertical line; it can only vaguely judge by whether both objects are simultaneously in focus. This invention innovatively sets up a first and a second observation window and uses an image and data acquisition system for multi-dimensional observation, ensuring both accurate measurement of the micro-forces between hydrate particles and the water-droplet interaction. This invention measures two forms of microscopic forces between hydrate particles, droplets, and the wall surface to comprehensively evaluate the "dual-effect" performance of the inhibitor in "inhibiting particle aggregation and preventing particle adhesion." It also provides an accurate criterion for determining whether the research objects are located on the same horizontal or vertical line by observing whether the glass fibers overlap. Existing single-viewing-window observation systems cannot accurately observe the hydrate formation morphology in blind spots and determine whether the current particles meet experimental requirements. This invention innovatively sets up a first and a second observation window and uses an image and data acquisition system to observe the hydrate particle formation morphology in multiple dimensions, ensuring the smoothness of the measured object's surface, improving experimental standards, and greatly reducing experimental errors.

[0052] The above description is merely a preferred embodiment of the present invention and does not constitute any limitation on the technical scope of the present invention. Therefore, any minor modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of the present invention shall still fall within the scope of the technical solution of the present invention.

Claims

1. A multidimensional visualization microscopic force measurement device, characterized in that, include: High-pressure reaction chamber, three-dimensional moving stage, moving end glass fiber, fixed end glass fiber and image and data acquisition system; The three-dimensional moving stage is set inside the high-pressure reaction chamber and can realize three-dimensional movement in xyz. The moving end glass fiber is fixed on the three-dimensional moving stage, and the fixed end glass fiber is fixed on the inner wall of the high-pressure reaction chamber and corresponds to the position of the moving end glass fiber. A first observation window is set on the top of the high-pressure reaction chamber, and a second observation window is set on one side of the high-pressure reaction chamber. The image and data acquisition system is used to determine whether the research object is located on the same horizontal or vertical line, and to realize accurate observation of the hydrate formation morphology in the blind spot of the field of view and to determine whether the current particle can meet the experimental requirements. Finally, it realizes the measurement of two forms of microscopic interaction forces between hydrate particles and hydrate particles, and between hydrate particles, droplets and walls. The image and data acquisition system includes a first microscope, a second microscope, a pressure sensor, a temperature sensor, and a data acquisition terminal. The first microscope is vertically aligned with a first observation window to observe the measurement process from a top-down perspective, and the second microscope is vertically aligned with a second observation window to observe the measurement process from a side perspective, thereby achieving multi-dimensional visualization measurement during the experiment. Both the pressure sensor and the temperature sensor are connected to the high-pressure reaction chamber to monitor temperature and pressure changes in real time. The first microscope, the second microscope, the pressure sensor, and the temperature sensor are all connected to the data acquisition terminal via high-definition signal cables. The fixed form of the movable end glass fiber is divided into horizontal fixed and vertical fixed according to the different measurement objects. The horizontal fixed is the movable end glass fiber one, which is mainly used to measure the interaction force between hydrate particles; the vertical fixed is the movable end glass fiber two, which is mainly used to measure the interaction force between hydrate particles, droplets and wall. The wall movement direction is the z direction, and the side viewing angle is perpendicular to the wall movement direction, which can observe the displacement of the fixed end particles and then calculate the microscopic interaction force between hydrate particles, droplets and wall.

2. The multidimensional visualization microscopic force measurement device as described in claim 1, characterized in that, Three-dimensional shifting rods are respectively installed on three sides of the high-pressure reaction chamber. One end of the three-dimensional shifting rod extends into the high-pressure reaction chamber and is connected to the three-dimensional moving stage, which is used to drive the three-dimensional moving stage to achieve three-dimensional movement in xyz.

3. The multidimensional visualization microscopic force measurement device as described in claim 1, characterized in that, Both the first observation window and the second observation window are composed of two layers of glass windows. The inner glass window is made of sapphire plate, and the outer glass window is made of plexiglass.

4. The multidimensional visualization microscopic force measurement device as described in claim 1, characterized in that, It also includes an air intake system, which includes a high-pressure air source and an air cooling coil. The high-pressure air source is connected to the high-pressure reaction chamber through the air cooling coil, and a pressure gauge is installed on the pipeline connecting the high-pressure air source and the air cooling coil.

5. The multidimensional visualization microscopic force measurement device as described in claim 1, characterized in that, It also includes a low-temperature water bath system, which includes a low-temperature water bath tank filled with ethylene glycol antifreeze. The tank is connected to the outer jacket of the high-pressure reaction chamber via a hose. A circulating pump is used to circulate the antifreeze between the low-temperature water bath tank and the outer jacket to maintain the experimental temperature inside the high-pressure reaction chamber.

6. A method for measuring multidimensional visualized microscopic forces, characterized in that, This is achieved using the multidimensional visualization microscopic force measurement device according to any one of claims 1-5, comprising the following steps: (1) Experimental preparation stage: The temperature of the high pressure reaction chamber was reduced to -7~-10℃ using a low temperature water bath system. Two glass fiber elastic coefficients were selected and measured. Ice particles containing "dual-effect" inhibitors were prepared at the tip of the fixed glass fiber using liquid nitrogen. Ice particles or carbon steel with droplets were prepared at the tip of the moving glass fiber. The fixed glass fiber with ice particles was fixed at the fixed end of the reactor body. The moving glass fiber with ice particles / carbon steel was fixed on the three-dimensional moving stage in the high pressure reaction chamber and the reactor body was quickly sealed. (2) Hydrate particle induction stage: Open the vent valve to evacuate the high-pressure reaction chamber. The high-pressure gas source slowly adds methane into the high-pressure reaction chamber through the gas cooling coil. After reaching the predetermined experimental pressure, close the high-pressure gas source and the gas cooling coil, raise the temperature of the high-pressure reaction chamber to -1℃, and then raise the temperature of the high-pressure reaction chamber to 1.7℃. During this process, the ice particles melt and generate hydrate particles under the action of high-pressure methane gas. (3) Adhesion test stage: The three-dimensional moving stage is controlled by three three-dimensional shifting linkages to move along the xyz three-dimensional axis so that the center of the test object at the moving end and the center of the hydrate particle at the fixed end are on the same horizontal line or the same vertical line. Then, the three three-dimensional shifting linkages are manipulated to make the test object at the moving end approach the hydrate particle at the fixed end at a uniform speed. After the two objects come into contact, the moving end is pressed to displace the fixed end by 0.3 mm. After the two objects come into contact for 10 seconds, they are slowly pulled apart at a uniform speed. The separation process of the two objects is captured in real time using the image and data acquisition system. The displacement of the fixed end is converted into the actual displacement. The micro force is solved using Hooke's law and corrected using the harmonic radius. The average value of the measured results is taken. (4) After the experiment, release the pressure using the vent valve.

7. The multidimensional visualization microscopic force measurement method as described in claim 6, characterized in that, In the experimental preparation stage, the vent valve is first opened and a vacuum pump is used to evacuate the high-pressure reaction chamber. The pressure inside the high-pressure reaction chamber is read by a pressure sensor. When the pressure stabilizes above -0.008MPa for 10 minutes, it indicates that the chamber is well sealed. The vent valve is then closed and the formal experiment begins.

8. The method for measuring multidimensional visual microscopic forces as described in claim 6, characterized in that, The method for determining whether the center of the object to be measured is located on the same horizontal or vertical line is as follows: If the moving end is a hydrate particle, the moving end and the fixed end will be displaced in the x direction, thus making the centers of the hydrate particles at the moving end and the hydrate particles at the fixed end located on the same horizontal line. This process is judged by the side view of the second observation window, and the judgment criterion is whether the glass fibers at the moving end and the glass fibers at the fixed end are completely overlapped. If the moving end is a droplet-wall, the moving end and the fixed end will be displaced in the z direction, thus making the center of the droplet-wall at the moving end and the center of the hydrate particle at the fixed end on the same vertical line. This process is judged by the top view of the first observation window, and the judgment criterion is whether the glass fiber at the moving end and the glass fiber at the fixed end are completely overlapped.

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