An imaging device and an imaging method

Abstract

The present invention provides an imaging device and an imaging method, belonging to the technical field of microscopic characterization of hydrates. The imaging device includes a gas injection component, a temperature control device, a reaction kettle, and a Raman spectroscopy test component; the gas injection component includes a gas storage cylinder and a pressure regulating valve, the gas storage cylinder is communicated with the reaction kettle through a pipeline, and the pressure regulating valve is arranged between the gas storage cylinder and the reaction kettle to adjust the internal pressure of the reaction kettle to a preset pressure value; the Raman spectroscopy test component includes a Raman spectrometer, a laser, and a stage; the temperature control device is connected to the side wall of the reaction kettle to adjust the internal temperature of the reaction kettle to a preset temperature value; visual windows are arranged on both opposite sides of the reaction kettle, and the lens of the Raman spectrometer and the output end of the laser are respectively oriented towards the visual window on the side away from the stage. By controlling the stability of the temperature and pressure of the reaction kettle and adjusting the distance between the stage and the Raman spectrometer, the efficiency and accuracy of 3D imaging of hydrates are improved.

Description

Technical Field

[0001] The present invention relates to the technical field of microscopic characterization of hydrates, and in particular to an imaging device and an imaging method. Background Art

[0002] In the initial stage of hydrate research, the kinetic and thermodynamic processes during the formation and decomposition of hydrates were mostly analyzed from a macroscopic perspective, and thick-walled blind reactors were mostly used in the experimental system. With the progress of modern testing means, especially the development of in-situ testing means, the research on hydrate characterization has been pushed into a new stage.

[0003] The change of hydrate structure requires the use of microscopic characterization instruments to characterize the structural characteristics of hydrates. Laser Raman spectroscopy is widely used in the research of hydrates due to its fast testing speed, non-damage to samples, and ability to accurately judge the hydrate structure. Usually, an atmospheric pressure low-temperature hot and cold stage is mostly used to maintain the stability of the sample structure at extremely low temperatures. However, the release of pressure and the change of temperature during the sampling process will both cause partial decomposition of the hydrate, resulting in poor imaging effect of the hydrate. Summary of the Invention

[0004] In view of this, the purpose of the present invention is to overcome the deficiencies in the prior art and provide an imaging device and an imaging method.

[0005] The present invention provides the following technical solutions: An imaging device includes a gas injection component, a temperature control device, a reaction kettle, and a Raman spectroscopy test component;

[0006] The gas injection component includes a gas storage cylinder and a pressure regulating valve. The gas storage cylinder is connected to the reaction kettle through a pipeline, and the pressure regulating valve is arranged between the gas storage cylinder and the reaction kettle to adjust the internal pressure of the reaction kettle to a preset pressure range;

[0007] The Raman spectroscopy test component includes a Raman spectrometer, a laser, and a stage;

[0008] The reaction kettle is arranged on the stage, and the Raman spectrometer is arranged on the side of the reaction kettle away from the stage;

[0009] The temperature control device is connected to the side wall of the reaction kettle to adjust the internal temperature of the reaction kettle to a preset temperature range;

[0010] Visual windows are provided on both opposite sides of the reaction kettle, and the lens of the Raman spectrometer and the output end of the laser are respectively oriented towards the visual window on the side away from the stage.

[0011] In some embodiments of the present invention, the gas injection component further includes an air compressor, a booster pump, and a gas storage tank;

[0012] The air compressor is connected to the booster pump through a pipeline;

[0013] The intake port of the booster pump is communicated with the gas storage cylinder through a first connecting pipe, and the outlet port of the booster pump is communicated with the reaction kettle through a second connecting pipe;

[0014] The gas storage tank is arranged between the booster pump and the reaction kettle, and the outlet port of the gas storage tank is communicated with the second connecting pipe through a pipeline;

[0015] The pressure regulating valve is arranged on the second connecting pipe.

[0016] Further, the preset temperature value is 2 to 4 °C;

[0017] The preset pressure value is 8 to 15 MPa.

[0018] Further, the reaction kettle includes a flange, two groups of visual windows and a support ring;

[0019] The two groups of visual windows are respectively stacked on both sides of the support ring in the axial direction to form a sample chamber, and the flange is sleeved on the support ring and the visual windows;

[0020] The side wall of the flange is provided with a gas inlet and a gas outlet which are spaced apart, the gas inlet and the gas outlet are respectively communicated with the sample chamber, and the second connecting pipe is communicated with the gas inlet;

[0021] Further, a liquid circulation channel is arranged inside the support ring, and the liquid circulation channel is coaxially arranged with the support ring;

[0022] The side wall of the support ring is provided with a liquid inlet and a liquid outlet which are spaced apart, and the liquid inlet and the liquid outlet are respectively communicated with the liquid circulation channel.

[0023] Further, the temperature control device includes a constant temperature water bath and a cold circulation pump;

[0024] The cold circulation pump is arranged inside the constant temperature water bath, and the output end of the cold circulation pump is communicated with the liquid inlet;

[0025] The water inlet of the constant temperature water bath is communicated with the liquid outlet through a pipeline.

[0026] Further, it further includes a data acquisition module and a background processor, and the data acquisition module is electrically connected to the background processor;

[0027] The Raman spectrometer is electrically connected to the background processor.

[0028] Further, the support ring is made of stainless steel.

[0029] Further, it also includes a pressure sensor and a temperature sensor;

[0030] The pressure sensor is arranged at the gas inlet of the reaction kettle, and one end of the temperature sensor penetrates through the side wall of the reaction kettle and is placed in the sample chamber;

[0031] The temperature sensor and the pressure sensor are respectively electrically connected to the data acquisition module.

[0032] Some embodiments of the present invention also provide an imaging method, using the imaging device described above, including:

[0033] Step S1, obtaining a sample and placing the sample into the reaction kettle;

[0034] Step S2, evacuating the reaction kettle and adjusting the stage to make the scanning lens of the Raman spectrometer close to the viewing window;

[0035] Step S3, adjusting the temperature of the reaction kettle to a preset temperature value through the temperature control device;

[0036] Step S4, introducing a test gas into the reaction kettle to a preset pressure value;

[0037] Step S5, adjusting the focusing position of the lens of the Raman spectrometer through the stage, and scanning and analyzing the structures and distributions of hydrates at different depths to obtain a 3D image of the hydrate.

[0038] The embodiments of the present invention have the following advantages: continuously supplying gas to the reaction kettle through the gas storage cylinder, and adjusting the pressure inside the reaction kettle through the pressure regulating valve to improve the pressure stability in the reaction kettle. At the same time, a temperature control device is arranged on the side wall of the reaction kettle to control the temperature inside the reaction kettle through the temperature control device to improve the temperature stability inside the reaction kettle. At the same time, by adjusting the distance between the stage and the Raman spectrometer, a 3D image of the hydrate in the reaction kettle is realized, thereby improving the efficiency and accuracy of the 3D imaging of the hydrate.

[0039] In order to make the above objects, features, and advantages of the present invention more obvious and understandable, the following specifically gives preferred embodiments and, in conjunction with the accompanying drawings, makes a detailed description as follows. Description of the Drawings

[0040] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following will briefly introduce the drawings required to be used in the embodiments. It should be understood that the following drawings only show some embodiments of the present invention, and therefore should not be regarded as limiting the scope. For those of ordinary skill in the art, without creative efforts, other related drawings can also be obtained based on these drawings.

[0041] Figure 1A schematic structural diagram of a perspective view of an imaging device provided by some embodiments of the present invention is shown;

[0042] Figure 2 A schematic structural diagram of a perspective view of a reactor in an imaging device provided by some embodiments of the present invention is shown;

[0043] Figure 3 Shows Figure 2 A cross-sectional view of part A-A in;

[0044] Figure 4 Shows Figure 2 A cross-sectional view of part B-B in;

[0045] Figure 5 Shows Figure 4 A cross-sectional view of part C-C in;

[0046] Figure 6 A schematic structural diagram of a perspective view inside a temperature control device in an imaging device provided by some embodiments of the present invention is shown;

[0047] Figure 7 A microscopic image of methane hydrate in a reactor in an imaging device provided by some embodiments of the present invention is shown;

[0048] Figure 8 Shows Figure 7 Raman spectra of methane hydrate in parts A and B in;

[0049] Figure 9 Shows the Raman intensity distribution diagram corresponding to methane hydrate in the large cage at 2904 cm -1 in a reactor in an imaging device provided by some embodiments of the present invention;

[0050] Figure 10 Shows the Raman intensity distribution diagram corresponding to methane hydrate in the small cage at 2915 cm -1 in a reactor in an imaging device provided by some embodiments of the present invention;

[0051] Figure 11 A flowchart of an imaging method provided by some embodiments of the present invention is shown.

[0052] Description of main element symbols:

[0053] 100 - Gas injection assembly; 200 - Temperature control device; 300 - Reactor; 400 - Raman spectroscopy test assembly; 110 - Gas cylinder; 120 - Pressure regulating valve; 410 - Raman spectrometer; 430 - Stage; 310 - Visual window; 130 - Air compressor; 140 - Booster pump; 150 - Gas storage tank; 500 - First connecting pipe; 600 - Second connecting pipe; 320 - Flange; 330 - Support ring; 340 - Sample chamber; 321 - Gas inlet; 322 - Gas outlet; 331 - Liquid circulation channel; 332 - Liquid inlet; 333 - Liquid outlet; 210 - Constant temperature water bath; 220 - Cold circulation pump; 700 - Data acquisition module; 800 - Background processor; 350 - Pressure sensor; 360 - Temperature sensor; 900 - Safety valve. Detailed implementation manners

[0054] The embodiments of the present invention will be described in detail below. The examples of the embodiments are shown in the accompanying drawings, where the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below by referring to the accompanying drawings are exemplary and are only used to explain the present invention and should not be construed as a limitation to the present invention.

[0055] It should be noted that when an element is referred to as being "fixed to" another element, it can be directly on the other element or there may also be a middle element. When an element is considered to be "connected" to another element, it can be directly connected to the other element or there may be a middle element at the same time. On the contrary, when an element is referred to as being "directly on" another element, there is no middle element. The terms "vertical", "horizontal", "left", "right" and similar expressions used herein are only for the purpose of illustration.

[0056] In the present invention, unless otherwise clearly defined and limited, the terms "installed", "connected", "connected", "fixed" and other terms should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or integrated; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the communication inside two elements or the interaction relationship between two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific situations.

[0057] In addition, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly indicating the quantity of the indicated technical features. Thus, the features defined with "first" and "second" may explicitly or implicitly include one or more of such features. In the description of the present invention, "a plurality of" means two or more unless otherwise clearly and specifically defined.

[0058] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the technical field to which this application belongs. The terms used in the specification of the template herein are for the purpose of describing specific embodiments only and are not intended to limit the present invention. The term "and / or" used herein includes any and all combinations of one or more of the related listed items.

[0059] As Figures 1 to 3 shown, some embodiments of the present invention provide an imaging device, which is mainly applied to 3D imaging of hydrates. The imaging device includes a gas injection assembly 100, a temperature control device 200, a reaction kettle 300, and a Raman spectroscopy test assembly 400.

[0060] It can be understood that gas is injected into the reaction kettle 300 through the gas injection assembly 100, and at the same time, the temperature in the reaction kettle 300 is controlled through the temperature control assembly, and the sample in the reaction kettle 300 is tested through the Raman spectroscopy test assembly 400.

[0061] Specifically, the gas injection assembly 100 includes a gas storage cylinder 110 and a pressure regulating valve 120. The gas storage cylinder 110 is communicated with the reaction kettle 300 through a pipeline, and gas is injected into the reaction kettle 300 through the gas storage cylinder 110. At the same time, the pressure regulating valve 120 is arranged between the gas storage cylinder 110 and the reaction kettle 300 to adjust the internal pressure of the reaction kettle 300 to a preset pressure value through the pressure regulating valve 120.

[0062] Specifically, the preset pressure value is 8 - 15 MPa.

[0063] Among them, the gas in the gas storage cylinder 110 can be specifically set according to the actual situation. In some embodiments of the present invention, the gas in the gas storage cylinder 110 can be any one of methane or ethane.

[0064] Among them, the Raman spectroscopy test assembly 400 includes a Raman spectrometer 410, a laser (not shown in the figure), and a stage 430.

[0065] It should be noted that the Raman spectrometer 410 is mainly applicable to optical aspects such as scientific research institutions, physics and chemistry laboratories of universities and colleges, and biological and medical fields, for the determination and confirmation of the composition of substances. This instrument is known for its simple structure, easy operation, fast, efficient, and accurate measurement, and low wavenumber measurement ability; it adopts a confocal optical path design to obtain higher resolution, can perform μm-level microarea detection on the sample surface, and can also be used for microscopic image measurement. In some embodiments of the present invention, the model of the Raman spectrometer 410 can be any one of LRS-5 or HM-LMSP.

[0066] A laser, as the name suggests, is a device that can emit lasers. The light emitted by a laser is pure in quality and has a stable spectrum, and can be used in many aspects.

[0067] In addition, it should be noted that in some embodiments of the present invention, the stage 430 is also called a mirror stage, which is located below or above the objective lens and is used to place the specimen to be observed. The shape is square or round, with a light hole in the center. A specimen pusher (film pusher) is installed on the stage 430. A spring clip is provided on the left side of the pusher to clamp the specimen. A pusher adjustment wheel is provided under the stage 430 to move the specimen left and right and front and back. The design of the stage 430 should have super durability and be convenient for specimen observation, that is, the operation of the microscope is more stable and more durable.

[0068] Specifically, the reactor 300 is disposed on the stage 430. It should be noted that the shape of the reactor 300 can be any one of a hollow cuboid, a cube, a cylinder, a polygonal prism, a sphere or an ellipsoid, and can be specifically set according to actual conditions. In some embodiments of the present invention, the shape of the reactor 300 is a cylinder.

[0069] It can be understood that one side of the reaction kettle 300 in the axial direction is in contact with the stage 430 to improve the stability of the reaction kettle 300 on the stage 430 .

[0070] Meanwhile, the Raman spectrometer 410 is disposed on a side of the reaction kettle 300 away from the stage 430 , and the Raman spectrometer 410 and the reaction kettle 300 are spaced apart from each other.

[0071] In addition, visual windows 310 are respectively provided on two opposite sides of the reactor 300. Specifically, two groups of visual windows 310 are respectively provided on two sides of the axis direction of the reactor 300.

[0072] At the same time, the lens of the Raman spectrometer 410 and the output end of the laser are respectively directed toward the visible window 310 on the side away from the stage 430, and the laser emitted by the laser passes through the visible window 310 to irradiate the surface of the test sample inside the reactor 300, and the test sample in the reactor 300 is detected by the Raman spectrometer 410.

[0073] It should be noted that the laser is disposed on a side of the reaction vessel 300 away from the stage 430 , and the laser is spaced apart from the Raman spectrometer 410 .

[0074] Specifically, the laser emitted by the laser can directly penetrate the sapphire to perform in-situ Raman testing on the hydrate sample inside the sample chamber 340 of the reactor 300, so as to accurately obtain the crystal form characteristics of the hydrate (such as sI, sII, etc.) and the structural characteristics during the formation and decomposition of the hydrate (such as the Raman peak positions and intensities of gas molecules in the large and small cages and the proportion of large and small cages, etc.).

[0075] It should be noted that the Raman spectrometer 410 can accurately measure the Raman vibration intensities of gas molecules in different cages of the hydrate, and the Raman intensity is proportional to the number of molecules. Since the sizes of different types of cages in the hydrate are different and the interaction forces between gas molecules and water molecules forming the cages are different, the Raman shifts of molecules in different cages are different. Since the number of large cages (5 12 6 2 ) in the sI-type hydrate is 3 times that of the small cages (5 12 ) and the number of large cages (5 12 6 4 ) in the sII-type hydrate is 0.5 times that of the small cages (5 12 ), for hydrates, the type of hydrate can be judged according to the peak values of the large and small cages on the measured Raman spectrum.

[0076] In addition, the temperature control device 200 is communicated with the reactor 300, and the temperature of the reactor 300 is controlled by the temperature control device 200 to make the temperature inside the reactor 300 reach the preset temperature value. Specifically, the preset temperature value is 2 - 4°C.

[0077] It should be noted that in some embodiments of the present invention, the temperature control device 200 is a constant temperature water bath 210, and a circulating water pump is provided inside the constant temperature water bath 210, and the output end of the circulating water pump is communicated with the reactor 300 through a pipeline.

[0078] The internal temperature of the reactor 300 is controlled by the temperature control device 200 to keep the temperature inside the reactor 300 stable. At the same time, the gas pressure in the reactor 300 is adjusted by a regulating valve to keep the gas pressure in the reactor 300 stable, thereby improving the accuracy of the Raman spectrometer 410 in detecting the sample in the reactor 300.

[0079] In some embodiments of the present invention, the material of the viewing window 310 is sapphire. Since sapphire has better light transmission effect, it can not only be used to observe the morphological changes of the hydrate during the formation and decomposition of the hydrate, but also be suitable for analyzing the structural information of the hydrate sample during the formation and decomposition of the hydrate.

[0080] Specifically, by adjusting the height of the stage 430, the distance between the viewing window 310 on the reactor 300 and the lens of the Raman spectrometer 410 is controlled to obtain a better spatial resolution effect.

[0081] Among them, the stage 430 can move freely along the XY plane and the Z axis. It can be understood that the XY plane is the horizontal plane and the Z axis is the direction perpendicular to the horizontal plane.

[0082] It should be noted that the Raman 3D full-automatic imaging process of hydrates is to focus point by point at a certain interval distance, test the Raman spectrum of the sample, analyze the intensity of the hydrate characteristic peaks in the spectrum of the hydrate sample, and display the distribution of hydrates on the sediment surface in the form of a two-dimensional image (as shown in the figure). Then, by moving the stage 430 in the Z-axis height, the hydrate samples within a certain range are scanned layer by layer to obtain the 3D full-automatic imaging during the formation and decomposition process of hydrates.

[0083] It should be noted that in some embodiments of the present invention, the hydrate is methane hydrate.

[0084] As Figure 1 、 Figure 4 and Figure 5 shown, in some embodiments of the present invention, the gas injection assembly 100 further includes an air compressor 130, a booster pump 140, and a gas storage tank 150.

[0085] Among them, the air compressor 130 is connected to the booster pump 140 through a pipeline to adjust the gas pressure in the pipeline through the air compressor 130 and the booster pump 140.

[0086] It can be understood that the air compressor 130 provides power to related equipment by compressing air. Since mechanical or hydraulic power transmission is not suitable in some places, gas power transmission can be used.

[0087] Among them, as the name implies, the booster pump 140 is a pump used for boosting pressure. In some embodiments of the present invention, the booster pump 140 is an air booster pump 140. The principle of the air booster pump 140 is to use the low air pressure of a large-area piston to generate the high hydraulic pressure of a small-area piston. The air booster pump 140 can increase the air pressure of the working system by 2-5 times, and only the compressed air in the working system needs to be used as the gas source. This pump is suitable for single-gas-source boosting. No power supply is required (it can be used in explosion-proof fields). Within the pressure range of the pump, adjust the regulating valve to adjust the intake pressure, and the output hydraulic pressure can be adjusted infinitely accordingly.

[0088] In addition, the intake port of the booster pump 140 is communicated with the outlet port of the gas storage cylinder 110 through a first connecting pipe 500, and the outlet port of the booster pump 140 is communicated with the reaction kettle 300 through a second connecting pipe 600. Meanwhile, the gas storage tank 150 is arranged between the booster pump 140 and the reaction kettle 300, and the outlet port of the gas storage tank 150 is communicated with the second connecting pipe 600 through a pipeline, and the pressure regulating valve 120 is arranged on the second connecting pipe 600.

[0089] Specifically, the pressure regulating valve 120 is arranged at one end of the second connecting pipe 600 close to the reaction kettle 300 to adjust the gas pressure entering the reaction kettle 300 through the pressure regulating valve 120, so as to maintain the stability of the pressure in the reaction kettle 300.

[0090] Among them, the gas storage tank 150 can be used as a backup for the gas storage cylinder 110. When the gas pressure in the gas storage cylinder 110 is insufficient, the gas storage tank 150 can also supply gas to the reaction kettle 300, so as to maintain the stability of the pressure in the reaction kettle 300.

[0091] Specifically, when the internal gas pressure of the gas storage cylinder 110 and the gas storage tank 150 is not less than 8 MPa, the gas in the gas storage cylinder 110 and / or the gas storage tank 150 enters the reaction kettle 300 through the second connecting pipe 600 to reach the required pressure value for the test. It should be noted that in some embodiments of the present invention, the range of the required pressure for the test is 8 - 15 MPa.

[0092] When the internal gas pressure of the gas storage cylinder 110 is between 2 MPa and 4 MPa, the gas storage tank 150 can be started, and the gas storage tank 150 supplies gas to the reaction kettle 300 to maintain the stability of the pressure in the reaction kettle 300. Or when the internal gas pressure of the gas storage tank 150 is between 2 MPa and 4 MPa, the gas storage cylinder 110 can be started, and the gas storage cylinder 110 supplies gas to the reaction kettle 300 to maintain the stability of the pressure in the reaction kettle 300.

[0093] Or when the internal gas pressures of both the gas storage cylinder 110 and the gas storage tank 150 are between 2 MPa and 4 MPa, the air compressor 130 and the booster pump 140 can be started to adjust the gas pressure in the second connecting pipe 600 to achieve the stability of the pressure in the reaction kettle 300, thereby improving the accuracy of the test data.

[0094] Such as Figure 1 、 Figure 3 、 Figure 4 and Figure 6 As shown, in some embodiments of the present invention, the reaction kettle 300 includes a flange 320, two groups of visual windows 310 and a support ring 330.

[0095] It should be noted that the support ring 330, the viewing window 310, and the support ring 330 are coaxially arranged.

[0096] Among them, two groups of the viewing windows 310 are respectively stacked on both sides of the support ring 330 in the axial direction to form a sample chamber 340, and the flange 320 is sleeved on the support ring 330 and the viewing window 310. The flange 320 is in interference fit with the support ring 330 to improve the stability between the support ring 330 and the flange 320.

[0097] Specifically, the two groups of the viewing windows 310 are respectively transparent disc structures, and the diameter of the viewing window 310 is equal to the outer diameter of the support ring 330. In addition, the support ring 330 and the flange 320 are coaxially arranged, and the height of the support ring 330 in its axial direction and the sum of the thicknesses of the two groups of the viewing windows 310 are less than the height of the flange 320 in its axial direction.

[0098] Meanwhile, a gas inlet 321 and a gas outlet 322 are provided at intervals on the side wall of the flange 320. The gas inlet 321 and the gas outlet 322 are respectively communicated with the sample chamber 340 so that gas can enter the sample chamber 340 through the gas inlet 321. By connecting the second connecting pipe 600 with the gas inlet 321, the gas in the gas storage cylinder 110 and the gas storage tank 150 enters the sample chamber 340 through the second connecting ring and the gas inlet 321, and at the same time, the gas entering the sample chamber 340 can be discharged through the gas outlet 322.

[0099] It should be noted that the gas inlet 321 and the gas outlet 322 can be arranged at any position on the side wall of the flange 320, and can be specifically defined according to the actual situation. In some embodiments of the present invention, the gas outlet 322 and the gas inlet 321 are respectively arranged on opposite sides of the flange 320, that is, the gas outlet 322 and the gas inlet 321 are symmetric about the axis of the flange 320.

[0100] As Figures 2 to 5 shown, in some embodiments of the present invention, a liquid circulation channel 331 is provided inside the support ring 330, and the liquid circulation channel 331 is coaxially arranged with the support ring 330.

[0101] It can be understood that the liquid circulation channel 331 is a ring-shaped structure.

[0102] It should be noted that there is a gap between the liquid circulation channel 331 and the sample chamber 340, and the liquid circulation channel 331 is arranged circumferentially of the sample chamber 340.

[0103] Meanwhile, spaced liquid inlets 332 and liquid outlets 333 are provided on the side wall of the support ring 330. The liquid inlets 332 and the liquid outlets 333 are respectively communicated with the liquid circulation channel 331, so that external liquid can enter the liquid circulation channel 331 through the liquid inlets 332 and be discharged from the liquid outlets 333. It can be understood that by adjusting the temperature of the liquid entering the liquid circulation channel 331, the temperature in the sample chamber 340 can be adjusted.

[0104] Specifically, in some embodiments of the present invention, the support ring 330 is made of stainless steel to improve the corrosion resistance of the support ring 330.

[0105] It should be noted that the liquid inlets 332 and the liquid outlets 333 can be arranged at any position on the side wall of the support ring 330, and can be specifically defined according to the actual situation. In some embodiments of the present invention, the liquid outlets 333 and the liquid inlets 332 are respectively arranged on opposite sides of the support ring 330, that is, the liquid outlets 333 and the liquid inlets 332 are symmetric about the axis of the support ring 330.

[0106] Such as Figure 1 、 Figure 4 and Figure 6 As shown in

[0107] Among them, the cold circulation pump 220 is arranged inside the constant temperature water bath 210. The output end of the cold circulation pump 220 is communicated with the liquid inlet 332, so that the liquid in the constant temperature water bath 210 is pumped into the liquid circulation channel 331 through the cold circulation pump 220 via the liquid inlet 332, and the temperature of the sample chamber 340 is adjusted through the heat conduction of the support ring 330.

[0108] Meanwhile, the water inlet of the constant temperature water bath 210 is communicated with the liquid outlet 333 through a pipeline, so that the liquid flowing through the liquid circulation channel 331 flows back to the constant temperature water bath 210 through the pipeline via the liquid outlet, so as to form a liquid circulation, thereby improving the stability of the temperature in the sample chamber 340.

[0109] Such as Figure 1 As shown in

[0110] Among them, the Raman spectrometer 410 is electrically connected to the background processor 800. The Raman spectrometer 410 sends the measured microscopic images to the background processor 800 through signals, and the background processor 800 presents the microscopic images measured by the Raman spectrometer 410. In some embodiments of the present invention, the background processor 800 is a computer.

[0111] The data acquisition module 700 and the background processor 800 are used to collect, save, and analyze the temperature and pressure change results of the sample chamber 340 in the reaction kettle 300 during the formation and decomposition of hydrates, and control the pressure and temperature in the high-pressure visible reaction kettle 300.

[0112] In some embodiments of the present invention, the data acquisition module 700 is a data acquisition card. Among them, the model of the data acquisition card can be any one of PCL-10168 or PCI-1712.

[0113] It should be noted that data acquisition refers to automatically collecting the analog or digital signals measured by the device and sending them to the upper computer for analysis and processing. A data acquisition card, that is, a computer expansion card that realizes the data acquisition function, can be connected to a computer through buses such as USB, PXI, PCI, PCI Express, PCMCIA, ISA, Compact Flash, Ethernet, and various wireless networks.

[0114] In some embodiments of the present invention, the hydrate can be a natural gas hydrate. Among them, natural gas hydrate (Natural Gas Hydrate / Gas Hydrate), also known as combustible ice, is an ice-like crystalline substance formed by natural gas and water under high pressure and low temperature conditions. Because of its ice-like appearance and the fact that it burns when encountering fire, it is called "combustible ice", "solid gas", and "gas ice".

[0115] Specifically, when the temperature is between 2 and 4 °C, natural gas hydrates are formed. When the temperature is not less than 20 °C, the natural gas hydrates decompose to form gas.

[0116] As Figure 1 and Figure 3 shown, in some embodiments of the present invention, the imaging device further includes a pressure sensor 350 and a temperature sensor 360.

[0117] Among them, the pressure sensor 350 is arranged at the gas inlet 321 of the reaction kettle 300, and the gas pressure entering the reaction kettle 300 is monitored in real time through the pressure sensor 350. At the same time, the pressure sensor 350 is electrically connected to the data acquisition module 700, and the received data is sent to the background processor 800 through the data acquisition module 700 by signals.

[0118] In addition, one end of the temperature sensor 360 is inserted through the side wall of the reaction kettle 300 and placed in the sample chamber 340, so as to monitor the temperature of the sample chamber 340 in real time through the temperature sensor 360.

[0119] It should be noted that the test end of the temperature sensor 360 is placed in the sample chamber 340.

[0120] Meanwhile, the temperature sensor 360 is electrically connected to the data acquisition module 700, and the monitored temperature data is sent to the data acquisition module 700 through a signal by the temperature sensor 360, and the received temperature data is sent to the background processor 800 through a signal by the data acquisition module 700, so as to realize the real-time monitoring of the changes in temperature and pressure in the reaction kettle 300.

[0121] Optionally, a pressure sensor 350 is provided in the sample chamber 340, and the pressure in the sample chamber 340 is monitored in real time through the pressure sensor 350 provided in the sample chamber 340. Meanwhile, the pressure sensor 350 is electrically connected to the data acquisition module 700, and the monitored data is sent to the data acquisition module 700 through a signal.

[0122] As Figure 1 shown, in some embodiments of the present invention, a safety valve 900 is further provided between the booster pump 140 and the pressure regulating valve 120. The safety valve 900 is arranged on the second connecting pipe 600, provides a protection function through the safety valve 900, and disconnects the reaction kettle 300 from the gas storage tank 150 and the gas cylinder 110 through the safety valve 900 when the gas pressure in the second connecting pipe 600 exceeds the specified value, so as to avoid excessive pressure in the reaction kettle 300.

[0123] It should be noted that the safety valve 900 is a special valve in which the opening and closing member is in a normally closed state under the action of external force. When the medium pressure in the equipment or pipeline rises and exceeds the specified value, the medium is discharged to the outside of the system to prevent the medium pressure in the pipeline or equipment from exceeding the specified value.

[0124] Optionally, in some embodiments of the present invention, the imaging device further includes a cold nitrogen purging device. The cold nitrogen purging device is arranged on one side of the stage 430, and the gas storage and outlet end of the cold nitrogen purging device faces the viewing window 310. During the test, the viewing window 310 is purged through the cold nitrogen purging device to prevent water vapor from condensing above the viewing window 310 during the cooling process from affecting the accuracy of the test, and at the same time keep the surface of the viewing window 310 dry, so as to improve the measurement accuracy.

[0125] As Figures 6 to 11As shown, some embodiments of the present invention also provide an imaging method, using the imaging device described in any of the above embodiments, including:

[0126] Step S1, obtain a sample and place the sample into the reaction kettle 300.

[0127] Specifically, before placing the sample into the reaction kettle 300, check the experimental equipment, calibrate the temperature control device 200, the temperature sensor 360, and the pressure sensor 350. At the same time, conduct leak detection on the reaction kettle 300, the pressure regulating valve 120, the safety valve 900, the first connection ring, and the second connecting pipe 600 to ensure that the entire experimental system is airtight without leakage, so as to improve the reliability and accuracy of the test data.

[0128] Secondly, open the high-pressure visible reaction kettle 300, and clean the reaction kettle 300 with deionized water to improve the cleaning efficiency and quality of the reaction kettle 300. After the reaction kettle 300 is dried, prepare the configuration for the experimental sample, that is, obtain the test sample.

[0129] Step S2, adjust the temperature of the reaction kettle 300 to a preset temperature value through the temperature control device 200.

[0130] Specifically, the liquid in the constant temperature water bath 210 is pumped into the liquid circulation channel 331 through the liquid inlet 332 by the cold circulation pump 220, and the liquid returns to the constant temperature water bath 210 through the pipeline from the liquid outlet 333 through the liquid circulation channel 331. Through continuous circulation, the reaction kettle 300 and the sample chamber 340 reach the preset temperature value.

[0131] It can be understood that the temperature of the reaction kettle 300 and the sample chamber 340 can be controlled by adjusting the temperature of the liquid in the constant temperature water bath 210.

[0132] Specifically, the range of the preset temperature value is 2 - 4°C. It should be noted that when methane gas is at 2 - 4°C, methane hydrate is formed.

[0133] Step S3, evacuate the reaction kettle 300, and adjust the stage 430 so that the scanning lens of the Raman spectrometer 410 is close to the viewing window 310.

[0134] Specifically, evacuate the reaction kettle 300 to discharge the impurity gas in it to improve the accuracy of the measurement data during the test process.

[0135] By adjusting the height of the stage 430 in the vertical direction, the distance between the viewing window 310 and the scanning lens of the Raman spectrometer 410 is adjusted, so that the scanning lens of the Raman spectrometer 410 is close to the viewing window 310 of the reaction kettle 300 to improve the accuracy of the Raman spectrometer 410 during the measurement process.

[0136] Optionally, test gas can also be injected into the sample chamber 340 of the reactor 300, then emptied, and this step can be repeated at least twice to ensure that the air in the sample chamber 340 of the reactor 300 is exhausted, so as to prevent the air in the reactor 300 from affecting the experimental results.

[0137] Step S4: Introduce test gas into the reactor 300 until the preset pressure value is reached.

[0138] It should be noted that in some embodiments of the present invention, the test gas is methane gas.

[0139] Among them, the range of the preset pressure value is 8 - 15 MPa.

[0140] Step S5: Adjust the focusing position of the lens of the Raman spectrometer 410 through the stage 430, and scan and analyze the structures and distributions of methane hydrates at different depths to obtain a 3D image of methane hydrates.

[0141] Specifically, by adjusting the position of the stage 430 in the vertical direction, the focusing position of the lens of the Raman spectrometer 410 is adjusted, and the structures and distributions of hydrates at different depth positions are scanned and analyzed by the Raman spectrometer 410.

[0142] Meanwhile, by adjusting the position of the stage 430 in the horizontal direction, rough imaging is performed to determine the area of the hydrate sample that needs to be focused on, improving the measurement efficiency.

[0143] In all the examples shown and described here, any specific value should be construed as merely exemplary, not as a limitation. Therefore, other examples of the exemplary embodiments may have different values.

[0144] It should be noted that similar reference numerals and letters denote similar items in the following drawings. Therefore, once an item is defined in one drawing, it does not need to be further defined and explained in subsequent drawings.

[0145] The above-described embodiments merely represent several implementation manners of the present invention. Their descriptions are relatively specific and detailed, but should not be construed as limiting the scope of the present invention. It should be pointed out that for those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can still be made, and these all belong to the protection scope of the present invention.

Claims

1. An imaging device, characterized in that, It includes a gas injection component, a temperature control device, a reaction kettle, and a Raman spectroscopy test component; The gas injection component includes a gas cylinder and a pressure regulating valve. The gas cylinder is connected to the reaction kettle through a pipeline, and the pressure regulating valve is arranged between the gas cylinder and the reaction kettle to adjust the internal pressure of the reaction kettle to a preset pressure value; The Raman spectroscopy test component includes a Raman spectrometer, a laser, and a stage; The reaction kettle is arranged on the stage, and the Raman spectrometer is arranged on one side of the reaction kettle away from the stage; The temperature control device is connected to the side wall of the reaction kettle to adjust the internal temperature of the reaction kettle to a preset temperature value; Visual windows are provided on both opposite sides of the reaction kettle, and the lens of the Raman spectrometer and the output end of the laser are respectively oriented towards the visual window on the side away from the stage; The reaction kettle includes a flange, two groups of visual windows, and a support ring; The two groups of visual windows are respectively stacked on both sides in the axial direction of the support ring to form a sample chamber, and the flange is sleeved on the support ring and the visual windows; The side wall of the flange is provided with a gas inlet and a gas outlet spaced apart from each other, and the gas inlet and the gas outlet are respectively communicated with the sample chamber; A liquid circulation channel is arranged inside the support ring, and the liquid circulation channel is coaxially arranged with the support ring; The side wall of the support ring is provided with a liquid inlet and a liquid outlet spaced apart from each other, and the liquid inlet and the liquid outlet are respectively communicated with the liquid circulation channel.

2. The imaging device according to claim 1, characterized in that, The gas injection component further includes an air compressor, a booster pump, and a gas storage tank; The air compressor is connected to the booster pump through a pipeline; The air inlet of the booster pump is communicated with the gas cylinder through a first connecting pipe, and the air outlet of the booster pump is communicated with the reaction kettle through a second connecting pipe; The gas storage tank is arranged between the booster pump and the reaction kettle, and the air outlet of the gas storage tank is communicated with the second connecting pipe through a pipeline; The pressure regulating valve is arranged on the second connecting pipe.

3. The imaging device according to claim 1, wherein The preset temperature value is 2 - 4 °C; The preset pressure value is 8 - 15 MPa.

4. The imaging device according to claim 2, characterized in that, The second connecting pipe is communicated with the gas inlet.

5. The imaging device according to claim 1, characterized in that, The temperature control device includes a constant temperature water bath and a cold circulation pump; The cold circulation pump is arranged inside the constant temperature water bath, and the output end of the cold circulation pump is communicated with the liquid inlet; The water inlet of the constant temperature water bath is communicated with the liquid outlet through a pipeline.

6. The imaging device according to claim 1, wherein It further includes a data acquisition module and a background processor, and the data acquisition module is electrically connected to the background processor; The Raman spectrometer is electrically connected to the background processor.

7. The imaging device according to claim 1, wherein The support ring is made of stainless steel.

8. The imaging device according to claim 6, characterized in that, It further includes a pressure sensor and a temperature sensor; The pressure sensor is arranged at the gas inlet of the reaction kettle, and one end of the temperature sensor penetrates through the side wall of the reaction kettle and is placed inside the sample chamber; The temperature sensor and the pressure sensor are respectively electrically connected to the data acquisition module.

9. An imaging method, using the imaging device according to any one of claims 1 to 8, characterized in that, It includes: Step S1, obtaining a sample and putting the sample into the reaction kettle; Step S2, evacuating the reaction kettle and adjusting the stage to make the scanning lens of the Raman spectrometer close to the visual window; Step S3, adjust the temperature of the reactor to the preset temperature value through a temperature control device; Step S4, introduce the test gas into the reactor until the preset pressure value is reached; Step S5, adjust the focusing position of the lens of the Raman spectrometer through the stage, and scan and analyze the structures and their distributions of hydrates at different depths to obtain a 3D image of the hydrates.

Images