Method and system for measuring gas-liquid ratio of fluid inclusion

Abstract

The invention relates to a method for measuring the gas-liquid ratio of a fluid inclusion, which comprises the following steps: sample preparation: cutting a rock sample into temperature measuring sheets, polishing, and positioning a target fluid inclusion; sound tweezers are locked, wherein a standing wave sound field is generated by combining high-frequency sound waves with a piezoelectric transducer array and a holographic acoustic lens or phased array technology, and bubbles in the inclusion are locked; raman spectrum verification: before and after the acoustic tweezers are locked, scanning the inclusion by adopting a Raman spectrum technology, and verifying that the sound field operation does not cause phase change or component loss by comparing peak position offset; performing Raman three-dimensional CT scanning and deformation correction: performing layer-by-layer scanning on the inclusion by utilizing a Raman microscope, constructing three-dimensional component distribution information of the inclusion, analyzing and simulating the influence of sound radiation pressure on the bubble form through a finite element, establishing a relation model of bubble deformation and sound field intensity, and correcting an initial volume calculation result; and gas-liquid ratio calculation: calculating a gas phase volume, a liquid phase volume and a sub-mineral volume in combination with the corrected three-dimensional model.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of geological research, and particularly relates to a method and system for measuring gas-liquid ratio of fluid inclusions. BACKGROUND

[0002] The measurement of the gas-liquid ratio of fluid inclusions is a crucial link in geological research. As ancient fluid samples captured during mineral growth, the original physical and chemical information carried by fluid inclusions is irreplaceable in revealing the process of rock and mineral formation. The gas-liquid ratio, which is the volume ratio of gas phase to liquid phase, is a key indicator for classifying inclusion types (such as liquid-rich or gas-rich) and has a wide range of applications in the fields of deposit genesis analysis and paleofluid temperature and pressure recovery. Accurate measurement of the gas-liquid ratio of fluid inclusions is crucial to understanding the process of rock and mineral formation. For example, in the study of ore deposits, the gas-liquid ratio data can reveal the evolution of ore-forming fluids, classify inclusion types, and differentiate the temperature and pressure of different ore-forming stages. It can also be used to estimate the ore-forming pressure and depth, providing direct evidence for deposit genesis analysis, resource evaluation, and ore exploration. At the same time, these studies deepen the understanding of ore-forming fluid behavior, paleogeological environment, and resource potential, and promote the development of geological science, with significant scientific and application value.

[0003] In the prior art, the traditional freezing process can cause the liquid water to solidify into ice (gas-liquid ratio -> gas-solid ratio), and the growth of ice crystals can squeeze the gas bubbles, which will fundamentally destroy the physical meaning of the original gas-liquid ratio. Therefore, it is particularly important to propose a method and system for measuring the gas-liquid ratio of fluid inclusions. SUMMARY

[0004] The purpose of the present application is to solve the problems existing in the prior art and provide a method and system for measuring the gas-liquid ratio of fluid inclusions.

[0005] To achieve the above purpose, the present application adopts the following technical solutions: A method for measuring the gas-liquid ratio of fluid inclusions, comprising the following steps: Sample preparation: cutting rock samples into temperature measurement pieces and polishing, and positioning target fluid inclusions; Acoustic tweezer locking: using high-frequency sound waves combined with piezoelectric transducer array and holographic acoustic lens or phased array technology to generate standing wave field to lock the gas bubbles in the inclusions; Raman spectrum verification: before and after acoustic tweezer locking, Raman spectrum technology is used to scan the inclusions, and the initial and locked peak positions of the gas-liquid phase composition are recorded. The phase change or composition loss caused by the acoustic field operation is verified by comparing the peak position shift; Raman 3D CT scanning and deformation correction: Use Raman microscope to scan the inclusion layer by layer, obtain Raman spectrum data at different depths, distinguish the signal characteristics of gas and liquid phases, construct the three-dimensional composition distribution information of the inclusion, simulate the influence of acoustic radiation pressure on the shape of the bubble based on the acoustic tweezers parameters through finite element analysis, establish the relationship model between bubble deformation and acoustic field intensity, and correct the calculation results of the initial volume; Gas-liquid ratio calculation: Calculate the gas volume, liquid volume and sub-mineral volume based on the corrected three-dimensional model, and then obtain the gas-liquid ratio, and confirm the sub-mineral composition combined with Raman composition analysis.

[0006] The above scheme further comprises: Further, in sample preparation, an automatic polishing machine is used, and 120 mesh, 600 mesh, 1200 mesh and 2400 mesh silicon carbide sandpaper are used in turn for rough polishing, and 4000 mesh diamond suspension is used for fine polishing, to obtain a smooth surface with a surface roughness of less than 10 nm.

[0007] Further, in the acoustic tweezers locking, the specific steps of locking the bubble in the inclusion are: Step 1: Device initialization and parameter presetting: Use a combination of acoustic transducers and piezoelectric transducer arrays, connect a holographic acoustic lens or phased array control system, set the frequency to 10 MHz, the sound pressure level to 150 dB-180 dB, and the action time to 5 seconds-10 seconds according to the size of the inclusion; Step 2: Target bubble positioning and acoustic field focusing: Position the inclusion through an optical microscope or confirm the position of the inclusion, adjust the sample stage to make the center of the bubble coincide with the focus of the acoustic tweezers, use a laser Doppler vibrometer to monitor the acoustic field distribution in real time, and make the standing wave node match the position of the bubble to form a three-dimensional trapping potential well; Step 3: Acoustic field activation and bubble locking: Increase the sound pressure step by step at an interval of 0.1 seconds, record the bubble motion trajectory through a high-speed camera, and reach a stable locking state.

[0008] Further, in the Raman spectrum verification, the specific steps of comparing the peak positions before and after acoustic tweezers locking to ensure that the acoustic field operation does not cause phase transition or composition loss are: Initial scanning sample positioning before acoustic tweezers locking: Place the prepared thin section on the Raman sample stage, adjust the sample position through an optical microscope to focus the laser on the center of the bubble, scan the area without inclusion first, obtain the background spectrum and subtract it, and perform full spectrum scanning on the inclusion, focusing on recording the gas-liquid phase characteristic peaks, scan the same position 3 times, and calculate the average value of the peak position; Acoustic tweezers locking and maintaining: Start the acoustic tweezers, lock the bubble and maintain the acoustic field parameters; Post-sonoporation verification scan: Before turning off the acoustic field, confirm that the laser focus point is still at the center of the bubble through the microscope, keep the same parameters as the initial scan, and perform a full-spectrum scan on the same inclusion, focusing on comparing the characteristic peak position changes, and scanning the full spectrum to confirm that there are no new peaks; Data analysis and verification standard: Set the peak position offset tolerance range to be <1 , and if the threshold is exceeded, it is considered that the acoustic field triggers phase transition or component loss. If no ex situ peak is found in the scanning full spectrum, it is confirmed that the composition has not changed. Through t-test comparison of peak position data before and after locking, if the difference is not significant, it proves that the acoustic field operation has no significant effect on the properties of the inclusion; Abnormal processing and rescan: If the peak position offset is greater than 1 , adjust the acoustic field parameters, re-lock and scan.

[0009] Further, in the Raman three-dimensional CT scanning and deformation correction, the specific steps of constructing the three-dimensional component distribution information of the inclusion are as follows: Parameterized scanning: Start from the top of the inclusion, and after each layer scan, move down along the Z axis until the entire depth of the inclusion is covered. Before each layer scan, adjust the laser focus point to the center of the layer through the automatic focusing system; Characteristic peak identification: Identify the gas phase, liquid phase and daughter mineral through the characteristic peak intensity. Save each layer scan result as a two-dimensional Raman spectrum, label the depth information, and form a three-dimensional data stack: Three-dimensional reconstruction: Subtract the glass slide background from each layer spectrum, smooth the spectrum data, set the threshold according to the characteristic peak intensity, and distinguish the gas phase, liquid phase and daughter mineral. Import the segmented two-dimensional spectrum into three-dimensional reconstruction software, fill the interlayer data through interpolation algorithm, and generate a three-dimensional component distribution model of the inclusion.

[0010] Further, in the Raman three-dimensional CT scanning and deformation correction, the specific steps of correcting the initial volume calculation results are as follows: Acoustic field parameterized modeling: Based on the actual sonoporation operation parameters, a two-dimensional axisymmetric model is established and the fluid properties are set. The linear acoustic equation is used to calculate the acoustic radiation pressure, where is the reference pressure in acoustic measurement, is the mass of the fluid per unit volume, is the speed of sound in the fluid; Deformation quantitative simulation: The elastic mechanics equilibrium equation is used to simulate the bubble long axis elongation rate and surface curvature change , where is the long axis elongation rate, is the initial radius of the fluid inclusion or bubble, is the shear modulus, For surface curvature change, and then establish the relationship model of volume change rate and long axis extension rate , For volume change rate, wherein, For total volume change caused by acoustic radiation pressure or temperature change, For the total volume of the inclusion.

[0011] Further, in the gas-liquid ratio calculation, the corrected three-dimensional model is combined to calculate the gas volume, liquid volume and sub-mineral volume, and then the gas-liquid ratio is obtained: Gas volume correction: adjust the total volume change rate To the initial gas volume Corrected, expressed as ; Liquid volume correction: adjust the liquid volume by the total volume change rate, expressed as , wherein, The initial volume of the liquid phase measured before the sound field is locked; Based on the corrected gas volume And the corrected liquid volume Calculate the gas-liquid ratio .

[0012] A measuring system used in a method for measuring the gas-liquid ratio of a fluid inclusion, comprising: Sample preparation module: cut the rock sample into a thin slice and polish it with chemical mechanical polishing technology, while positioning the fluid inclusion containing sub-mineral or specific phase state with an optical microscope; Acoustic tweezers locking module: generate adjustable frequency and focus standing wave sound field by combining piezoelectric transducer array with holographic acoustic lens, and dynamically adjust the sound field parameters through real-time control by FPGA and PID feedback control algorithm, while integrating temperature sensor and sound pressure gauge to monitor safety parameters; Raman spectrum module: use confocal Raman spectrometer to scan the whole spectrum of the inclusion before and after acoustic tweezers locking, focus on collecting the characteristic peaks of gas and liquid phases, and calculate the composition ratio of gas and liquid phases and identify the type of sub-mineral through peak comparison and peak area integration; Three-dimensional CT scanning module: control the vertical step of the sample stage to scan layer by layer, combine acoustic tweezers locking to ensure the stable position of each layer of gas bubbles, synchronize the spectral data and bright field image collected by Raman microscope to generate a composite data set, extract the gas, liquid and sub-mineral regions through threshold segmentation and region growing algorithm, obtain the morphology data of the inclusion at different depths and construct a three-dimensional model; Data analysis module: based on the acoustic tweezers parameters, the finite element analysis is simulated to simulate the influence of acoustic radiation pressure on the bubble shape, and a deformation-volume correction model is established, then a geometric correction algorithm is used to adjust the volume calculation result, and finally the gas phase volume, liquid phase volume, sub-mineral volume and gas-liquid ratio and composition analysis report are output.

[0013] The present application has the following advantages: 8、In the present application, the standing wave sound field is generated by the high-frequency sound wave, the bubble position is accurately locked, the fluid inclusion can be fixed without freezing, the problem of solidification of liquid water into ice is completely avoided, and the physical meaning of the original gas-liquid phase state is preserved. The Raman peak position before and after locking is compared to confirm that the acoustic field operation does not cause phase change or composition change, proving that the fluid properties are not disturbed by the acoustic field, and improving the data reliability.

[0014] 9、In the present application, based on the acoustic tweezers parameters, the influence of acoustic radiation pressure on the bubble shape is simulated, a relationship model between bubble deformation and sound field intensity is established, deformation indicators such as bubble long axis elongation rate and surface curvature change are quantified, and the initial volume calculation result is corrected to reduce the volume error. BRIEF DESCRIPTION OF DRAWINGS

[0015] Fig. 1 A method step diagram of a fluid inclusion gas-liquid ratio determination method is provided for the present application; Fig. 2 A system block diagram of a fluid inclusion gas-liquid ratio determination system is provided for the present application. DETAILED DESCRIPTION

[0016] The technical solutions in the embodiments of the present application will be described clearly and completely below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor belong to the scope of protection of the present application.

[0017] Please refer to Figs. 1-2 The present application is a fluid inclusion gas-liquid ratio determination method, which comprises the following steps: Sample preparation: cut the rock sample into a temperature measuring sheet with a thickness of 50-100 μm and polish it, position the target fluid inclusion, and ensure that the inclusion is located at the center and close to the upper surface; Acoustic tweezers locking: use high-frequency sound waves (such as GHz-level body sound wave transducers) combined with piezoelectric transducer arrays and holographic acoustic lenses or phased array technology to generate a standing wave sound field, lock the bubbles in the inclusion, prevent them from moving, and ensure the in-situ stability of the inclusion during subsequent scanning; Raman spectrum verification: before and after acoustic tweezers locking, respectively, use Raman spectrum technology to scan the inclusion, record the gas-liquid phase composition (such as of peaks, 3410 initial and post-locking peak positions, by comparing the peak shift (less than 1 and no new peaks are generated) to verify that the acoustic field operation does not cause phase transition or component loss, ensuring data reliability; Raman three-dimensional CT scanning and deformation correction: using a Raman microscope to scan the inclusion layer by layer, obtaining Raman spectrum data at different depths, distinguishing the signal characteristics of gas and liquid phases, constructing the three-dimensional composition distribution information of the inclusion, based on the sonoporation parameters (frequency, power, array configuration), through finite element analysis (FEA) to simulate the influence of acoustic radiation pressure on the shape of the bubble, to establish the relationship model between the bubble deformation (such as the elongation rate of the long axis, the change of surface curvature) and the intensity of the acoustic field, to correct the initial volume calculation results (if the mineral composition affects the fluid density or shear modulus (such as the high density of quartz increases the overall density), the corrected ρ and G values need to be substituted into the total volume change rate calculation), to eliminate the deformation error caused by the acoustic field; Gas-liquid ratio calculation: combined with the corrected three-dimensional model to calculate the gas volume, liquid volume and mineral volume (assuming that the mineral is a rigid solid, its volume change in the acoustic field or thermal field can be ignored, and the initial measured value is directly retained), and then the gas-liquid ratio is obtained, combined with the Raman composition analysis (comparing the measured Raman spectrum with the standard mineral database (such as RRUFF, Mineral Raman Library) to identify the mineral composition), to confirm the mineral composition and ensure the accuracy of the volume calculation.

[0018] In one embodiment, in sample preparation, an automatic polisher is used, and 120-mesh, 600-mesh, 1200-mesh, and 2400-mesh silicon carbide sandpaper is used in sequence for rough polishing, and 4000-mesh diamond suspension is used for fine polishing, to finally obtain a smooth plane with a surface roughness of less than 10 nm: The inclusions are identified by image comparison, and isolated, intact, and 5-50 μm in diameter inclusions are preferentially selected to avoid interference from adjacent inclusions. For inclusions containing minerals, the interface between the mineral (such as halite) and the liquid and gas phases should be clear. A nanometer-precision laser marking system (such as a femtosecond laser) is used to mark the inclusion position on the sample surface to ensure accurate positioning during subsequent cutting; An ultrathin sectioning machine or a focused ion beam cutting system is used, and the cutting thickness is accurately controlled to 50-100 μm by a feedback control system. The polished sample is embedded in an epoxy resin on a glass slide, and the resin provides mechanical support during cutting to prevent the sample from moving. After cutting, the thin section is solidified by low-temperature (4°C) resin to enhance stability; The surface of the thin slice was polished with an argon ion polishing instrument for 10-30 minutes at a voltage of 5 kV and a current of 1 mA, to remove the surface damage layer (about 1-5 μm thick) caused by cutting. The thin slice was then ultrasonically cleaned with ultrapure water, anhydrous ethanol, and acetone for 5 minutes each time, to remove residual resin and polishing debris and avoid contamination of subsequent acoustic tweezers and Raman analysis. The cut thin slice was rechecked under an optical microscope or a scanning electron microscope to confirm that the inclusion was located at the center and close to the upper surface (distance from the surface ≤5 μm), and to ensure that the bubble was in the focal point area of the acoustic field when the acoustic tweezers were locked. If the position of the inclusion deviated, the position of the glass slide was adjusted or the local area was re-cut until the position of the inclusion met the requirements.

[0019] In one embodiment, in the acoustic tweezers locking, the specific steps of locking the bubble in the inclusion are as follows: Step 1: Device initialization and parameter presetting: a GHz-level bulk acoustic wave transducer (such as Murata MA40S4S resonator) and a piezoelectric transducer array (16 channels, spacing 50 μm) were combined, connected to a holographic acoustic lens (focusing accuracy ±1 μm) or a phased array control system (such as Verasonics Vantage), and the frequency was set to 10 MHz, the sound pressure level was set to 150 dB-180 dB, and the action time was set to 5 seconds-10 seconds according to the size of the inclusion (assuming the bubble diameter is 20 μm), to ensure that the acoustic radiation force (about 50 nN) was sufficient to overcome the fluid viscous resistance (about 10 nN when the water-based fluid viscosity is 1 mPa·s), while avoiding nonlinear effects (such as acoustic flow velocity <1 μm / s); Step 2: Target bubble positioning and acoustic field focusing: the position of the inclusion was confirmed by an optical microscope or a scanning electron microscope, the sample stage was adjusted to make the center of the bubble coincide with the focus of the acoustic tweezers (error <2 μm), and a laser Doppler vibrometer (Polytec PSV-500) was used to monitor the acoustic field distribution in real time, so that the standing wave node (sound pressure minimum point) matched the position of the bubble, forming a three-dimensional trapping potential well (depth about 10 kBT, kBT is the thermal energy unit); Step 3: Acoustic field activation and bubble locking: the sound pressure was gradually increased at an interval of 0.1 seconds to avoid sudden application of sound pressure causing bubble deformation or displacement, the bubble motion trajectory was recorded by a high-speed camera (Phantom v2640, frame rate 10,000 fps), and it was confirmed that the displacement was <0.5 μm within 2 seconds after the acoustic field was activated, reaching a stable locking state.

[0020] In one embodiment, in the Raman spectrum verification, the specific steps of ensuring that the acoustic field operation did not cause phase transition or composition loss by comparing the peak positions before and after the acoustic tweezers locking are as follows: Initial scanning before sonoporation: A confocal Raman spectrometer (e.g. Horiba LabRAM HR Evolution) equipped with a 532 nm or 785 nm laser (532 nm for inorganic, 785 nm for fluorescence suppression), 1800 g / mm grating, Peltier-cooled CCD detector, is used to set the scanning range (e.g. 100-4000 cm-1) and laser power (1-5 mW for 532 nm, 10-20 mW for 785 nm), integration time (5-10 s per point), step size (1-2 ) according to the composition of the inclusion. The prepared thin section is placed on the Raman stage, and the sample position is adjusted by optical microscopy to focus the laser on the bubble center. The background spectrum is obtained by scanning the non-inclusion area (e.g. the surface of the glass slide) and subtracting it to eliminate the interference of fluorescence or stray light. The full spectrum of the inclusion is scanned (100 -4000 cm-1), and the gas-liquid characteristic peaks are recorded. The same position is scanned three times, and the average peak position is calculated to ensure the stability of the initial data. Sonoporation locking and maintaining: Start the sonoporation, lock the bubble, and maintain the sonication field parameters. Verification scanning after sonoporation locking: Before turning off the sonication field, confirm by microscopy that the laser focus point is still located at the bubble center to avoid scanning position deviation due to sample movement. Keep the same parameters as the initial scanning, and perform full spectrum scanning on the same inclusion. Focus on comparing the characteristic peak position changes, and scan the full spectrum (100 -4000 cm-1) to confirm that there are no new peaks, and exclude the possibility of chemical reactions induced by the sonication field. Data analysis and verification standards: Set the peak position tolerance range to be <1 , or the characteristic peak position of ethane in the gas and liquid phases is 2912 -2920 and 2908 -2916 , and the characteristic peak position of propane is 2887 -2896 and 2884 -2892 . The characteristic peak position of bicarbonate in the salt solution is 1064 -1072 These data can be used to calculate the allowed range of peak shift, beyond the threshold is considered to be sound field induced phase transition or component loss, if the scan full spectrum did not find non-in situ peak, confirm the composition is not changed, by t test (p>0.05) comparison before and after locking peak position data, if the difference is not significant, then prove that the sound field operation has no significant effect on the properties of the inclusion;

[0021] Abnormal processing and rescan: if the peak shift is greater than 1 , adjust the sound field parameters, re-lock and scan.

[0022] In one embodiment, in the Raman three-dimensional CT scanning and deformation correction, the specific steps of constructing the three-dimensional component distribution information of the inclusion are as follows: Parametric scanning: starting from the top of the inclusion (0 μm from the surface), after each layer scanning, descending along the Z axis, until covering the whole depth of the inclusion, before each layer scanning, adjusting the laser focus to the center of the layer through the autofocus system, ensuring that the spatial positioning error is less than 1 μm. Using a confocal Raman spectrometer (such as Horiba LabRAM HR Evolution or WITec alpha300 R), equipped with near-infrared laser (785 nm, to suppress fluorescence interference), 1800 g / mm grating, Peltier refrigeration CCD detector, according to the composition of the inclusion, the 785 nm laser is recommended to be 10-20 mW (to avoid overheating the sample).

[0023] Integration time: 8-10 seconds per point (balance signal-to-noise ratio and scanning efficiency).

[0024] Step size: 0.5-1 μm (along X / Y axis), ensuring that the spatial resolution is less than or equal to 1 μm.

[0025] Scanning layer thickness: 1 μm (along Z axis, consistent with the cutting depth of the acoustic tweezers).

[0026] Scanning range: 100-4000 cm⁻¹ (covering gas phase, liquid phase and sub-mineral characteristic peaks).

[0027] Characteristic peak identification: identify gas phase, liquid phase and sub-mineral by characteristic peak intensity, save each layer scanning result as a two-dimensional Raman spectrum (pixel size 0.5 μm x 0.5 μm), mark the depth information, form a three-dimensional data stack: Gas phase: 1386 -1390 (F2g symmetric stretching vibration), 2913 -2919 (C-H stretching vibration).

[0028] Liquid phase: 3310 -3610 (O-H symmetric stretching vibration), 2987 (-2994 ( bending vibration superposition).

[0029] Submineral: 1085 (T2g vibration mode).

[0030] Three-dimensional reconstruction: Subtract the slide background (no inclusion area scanning results) for each layer spectrum, eliminate the interference of fluorescence or stray light, smooth the spectral data with Savitzky-Golay filter (window size 5 points) to improve the peak identification accuracy, set threshold according to the intensity of characteristic peaks, distinguish gas phase, liquid phase and submineral, import the segmented two-dimensional spectrum into three-dimensional reconstruction software (such as Amira or Dragonfly), fill the interlayer data by interpolation algorithm (such as cubic spline interpolation), and generate three-dimensional composition distribution model of inclusion.

[0031] Threshold: Gas phase area: peak intensity > 1000 counts and peak intensity < 500 counts.

[0032] Liquid phase area: peak intensity > 800 counts and peak intensity < 300 counts.

[0033] Submineral area: NaCl peak intensity > 1200 counts and peak intensity < 400 counts.

[0034] In one embodiment, in the Raman three-dimensional CT scanning and deformation correction, the specific steps of correcting the initial volume calculation results are as follows: Acoustic field parameterized modeling: Based on the actual acoustic tweezers operation parameters (frequency f = 10 MHz, acoustic pressure P = 160 dB, 16 channel ring array configuration), a two-dimensional axisymmetric model is established in COMSOL Multiphysics or ANSYS and the fluid properties (density p = 1000 , acoustic velocity c = 1500 m / s, shear modulus G = 0.1 Pa\cdot ps) are set, and the linear acoustic equation is used to calculate the acoustic radiation pressure, where is the reference pressure in acoustic measurement, is the mass of the fluid in a unit volume, the speed of sound wave propagating in the fluid; Deformation quantitative simulation: through the elastic mechanics equilibrium equation Simulate the bubble long axis elongation and surface curvature change , wherein, is the long axis elongation, is the initial radius of the fluid inclusion or bubble, is the shear modulus, is the surface curvature change, and then the relationship model of the volume change rate and the long axis elongation is established , is the volume change rate, wherein, is the total volume change amount caused by the acoustic radiation pressure or the temperature change, is the total volume of the inclusion (gas phase + liquid phase + daughter mineral); In one embodiment, in the gas-liquid ratio calculation, the gas phase volume, the liquid phase volume and the daughter mineral volume (assuming that the daughter mineral is a rigid solid, the volume change in the acoustic field or the thermal field can be ignored, and the initial measured value is directly retained) are calculated by combining the corrected three-dimensional model, and then the gas-liquid ratio is obtained: Gas phase volume correction: through the total volume change rate The initial gas phase volume is corrected and expressed as ; Liquid phase volume correction: adjust the liquid phase volume by the total volume change rate to eliminate the deformation effect, expressed as , wherein, is the initial volume of the liquid phase measured before the acoustic field is locked; Based on the corrected gas phase volume and the corrected liquid phase volume , the gas-liquid ratio is calculated .

[0035] A determination system used by a determination method of a fluid inclusion gas-liquid ratio, comprising: Sample preparation module: cut the rock sample into a thickness of 50-100 μm by a laser cutting machine or an ion beam cutting system and polish it by combining a chemical mechanical polishing technology to reduce the surface roughness to nanometer level (<10 nm), and use an optical microscope to locate the fluid inclusion containing a daughter mineral or a specific phase state; Acoustic tweezers locking module: generate a tunable and focus standing wave acoustic field by using a piezoelectric transducer array combined with a holographic acoustic lens, dynamically adjust the acoustic field parameters by real-time control of FPGA and PID feedback control algorithm, and integrate temperature sensors and acoustic pressure meters to monitor safety parameters, lock the bubble in the inclusion and prevent it from moving by acoustic field control; Raman spectrum module: Use confocal Raman spectrometer to scan the inclusion before and after the sonotrode locking, focus on collecting the characteristic peaks of gas and liquid phase, and through peak comparison and peak area integration, calculate the composition ratio of gas and liquid phase and identify the types of sub-minerals, verify the influence of acoustic field operation on fluid properties (no phase change or composition loss), and provide composition basis for volume calculation; Three-dimensional CT scanning module: Through the step motor control sample table vertical step length scanning layer by layer, combined with the sonotrode locking to ensure the position of each layer of bubble stable, at the same time Raman microscope synchronous acquisition spectrum data and bright field image generation composite data set, and using ImageJ / Fiji or Avizo software through threshold segmentation and region growing algorithm to extract gas phase, liquid phase and sub-mineral area, get the different depth of inclusion morphology data and build three-dimensional model; Data analysis module: Based on the sonotrode parameters, use COMSOL Multiphysics or ANSYS to analyze the influence of acoustic radiation pressure on bubble shape and establish a deformation-volume correction model, then use geometric correction algorithm to adjust the volume calculation results, finally output the gas volume, liquid volume, sub-mineral volume, gas-liquid ratio and composition analysis report.

[0036] The sample preparation module outputs the wafer to the sonotrode locking module, the sonotrode locking module triggers the Raman spectrum module to scan and feedback the safety verification result, the Raman spectrum module transmits the composition data to the three-dimensional CT scanning module, the three-dimensional CT scanning module transmits the morphology data to the data analysis module, and the data analysis module outputs the final determination result.

[0037] Although the embodiments of the present application have been shown and described, it can be understood by those skilled in the art that various changes, modifications, replacements and deformations can be made to the embodiments without departing from the principles and spirits of the present application, and the scope of the present application is defined by the appended claims and their equivalents.

Claims

1. A method for determining the gas-liquid ratio of fluid inclusions, characterized in that, Includes the following steps: Sample preparation: The rock sample was cut into thermometers and polished to locate the target fluid inclusions; Acoustic tweezers locking: High-frequency sound waves are used in combination with piezoelectric transducer arrays and holographic acoustic lenses or phased array technology to generate a standing wave sound field to lock the bubbles in the inclusion. Raman spectroscopy verification: Before and after the acoustic tweezers were locked, the inclusions were scanned using Raman spectroscopy. The initial and locked peak positions of the gas and liquid phases were recorded. The peak position shift was compared to verify that the acoustic field operation did not induce a phase change or loss of components. Raman 3D CT Scanning and Deformation Correction: The inclusions were scanned layer by layer using a Raman microscope to obtain Raman spectral data at different depths, distinguishing the signal characteristics of the gas phase and the liquid phase, constructing the three-dimensional composition distribution information of the inclusions, and simulating the influence of acoustic radiation pressure on bubble morphology through finite element analysis based on acoustic tweezers parameters. A model of the relationship between bubble deformation and sound field intensity was established, and the initial volume calculation results were corrected. Gas-liquid ratio calculation: The gas phase volume, liquid phase volume and daughter mineral volume are calculated by combining the corrected three-dimensional model, and then the gas-liquid ratio is obtained. The daughter mineral composition is confirmed by Raman composition analysis.

2. The method for determining the gas-liquid ratio of fluid inclusions according to claim 1, characterized in that, In sample preparation, an automatic polishing machine was used to perform coarse polishing with 120-mesh, 600-mesh, 1200-mesh, and 2400-mesh silicon carbide sandpaper in sequence, followed by fine polishing with 4000-mesh diamond suspension, ultimately obtaining a smooth surface with a surface roughness of less than 10 nm.

3. The method for determining the gas-liquid ratio of fluid inclusions according to claim 1, characterized in that, The specific steps for locking air bubbles within an inclusion in acoustic tweezers locking are as follows: Step 1: Equipment initialization and parameter preset: Use a combination of acoustic transducer and piezoelectric transducer array, connect to holographic acoustic lens or phased array control system, and set the frequency to 10 MHz, sound pressure level to 150dB-180dB, and action time to 5-10 seconds according to the size of the package. Step 2: Target bubble localization and acoustic field focusing: By using an optical microscope or confirming the position of the inclusion, adjust the sample stage so that the center of the bubble coincides with the focal point of the acoustic tweezers. Use a laser Doppler vibrometer to monitor the acoustic field distribution in real time, so that the standing wave nodes match the position of the bubble, forming a three-dimensional trapping potential well. Step 3: Sound field activation and bubble locking: The sound pressure is gradually increased at 0.1-second intervals, and the bubble movement trajectory is recorded by a high-speed camera to achieve a stable locking state.

4. The method for determining the gas-liquid ratio of fluid inclusions according to claim 1, characterized in that, In Raman spectroscopy verification, the specific steps for locking the peak positions before and after using acoustic tweezers to ensure that the acoustic field operation did not induce a phase transition or component loss are as follows: Initial scanning sample positioning before acoustic tweezers locking: The prepared thin slice is placed on the Raman stage, and the sample position is adjusted by optical microscope so that the laser is focused on the center of the bubble. First, the region without inclusions is scanned to obtain the background spectrum and subtract it. The inclusions are scanned in full spectrum, and the characteristic peaks of the gas and liquid phases are recorded. The same position is scanned 3 times and the average value of the peak position is calculated. Acoustic tweezers locking and holding: Activate the acoustic tweezers to lock the bubble and maintain the acoustic field parameters; After locking with acoustic tweezers, the verification scan was performed: Before turning off the acoustic field, the laser focus point was confirmed to be still located in the center of the bubble by using a microscope. The same parameters as the initial scan were maintained, and a full spectrum scan was performed on the same inclusion. The changes in the position of characteristic peaks were compared in the key area. The full spectrum scan was confirmed to have no new peaks. Data analysis and validation standards: Set the peak offset tolerance range to <1. If the threshold is exceeded, it is considered that the sound field has induced a phase transition or component loss. If no non-in-situ peaks are found when scanning the full spectrum, it is confirmed that the composition has not changed. The peak position data before and after are locked by comparing the t test. If the difference is not significant, it proves that the sound field operation has no significant effect on the properties of the inclusions. Anomaly handling and rescanning: If the peak offset is greater than 1 Adjust the sound field parameters, re-lock and scan.

5. The method for determining the gas-liquid ratio of fluid inclusions according to claim 1, characterized in that, Specific steps for constructing three-dimensional compositional distribution information of inclusions in Raman 3D CT scanning and deformation correction; Parametric scanning: Starting from the top of the package, the laser descends along the Z-axis after each layer is scanned until the entire depth of the package is covered. Before each layer is scanned, the laser focus is adjusted to the center of the layer using an autofocus system. Characteristic peak identification: The gas phase, liquid phase, and daughter minerals are identified by the intensity of characteristic peaks. The scanning results of each layer are saved as two-dimensional Raman spectra, with depth information annotated to form a three-dimensional data stack. 3D Reconstruction: The background of the slide is removed from each layer of the spectrum, the spectral data is smoothed, a threshold is set according to the intensity of the characteristic peaks to distinguish between the gas phase, liquid phase and daughter minerals, the segmented 2D spectrum is imported into the 3D reconstruction software, and the interlayer data is filled by the interpolation algorithm to generate a 3D composition distribution model of the inclusions.

6. The method for determining the gas-liquid ratio of fluid inclusions according to claim 5, characterized in that, The specific steps for correcting the initial volume calculation results in Raman 3D CT scanning and deformation correction are as follows: Sound field parametric modeling: A two-dimensional axisymmetric model is established based on actual acoustic tweezers operating parameters, and fluid properties are defined. Linear acoustic equations are then used. Calculate the sound radiation pressure, where, The reference pressure in acoustic measurements The mass of the fluid per unit volume. The speed at which sound waves propagate in a fluid; Quantitative simulation of deformation: using the equilibrium equations of elasticity Simulated changes in the long axis elongation and surface curvature of bubbles ,in, For the long axis elongation, The initial radius of the fluid inclusion or bubble. Shear modulus To account for changes in surface curvature, a model is established to show the relationship between the rate of volume change and the elongation of the major axis. , Let be the rate of change of volume, where This represents the total volume change, caused by changes in sound radiation pressure or temperature. This represents the total volume of the inclusion.

7. The method for determining the gas-liquid ratio of fluid inclusions according to claim 6, characterized in that, In the calculation of the gas-liquid ratio, the gas phase volume, liquid phase volume, and daughter mineral volume are calculated using the corrected three-dimensional model, and then the gas-liquid ratio is obtained: Gas phase volume correction: via total volume change rate For the initial gas phase volume To perform correction, as shown in the following diagram. ; Liquid phase volume correction: Adjusting the liquid phase volume by the rate of change of total volume, expressed as... ,in, The initial volume of the liquid phase measured before acoustic field locking; Based on the corrected gas volume With the corrected liquid volume Calculate the gas-liquid ratio .

8. The measuring system used in the method for determining the gas-liquid ratio of fluid inclusions according to claim 1, characterized in that, include: Sample preparation module: The rock sample is cut into thin sections and polished using chemical mechanical polishing technology. At the same time, an optical microscope is used to locate the daughter minerals or fluid inclusions in a specific phase. Acoustic tweezers locking module: It uses a piezoelectric transducer array combined with a holographic acoustic lens to generate a frequency-tunable and focusable standing wave sound field, and dynamically adjusts the sound field parameters through FPGA real-time control and PID feedback control algorithm. At the same time, it integrates a temperature sensor and a sound pressure meter to monitor safety parameters. Raman spectroscopy module: Using a confocal Raman spectrometer, the inclusions are scanned in their entirety before and after being locked by acoustic tweezers. The key features of the gas and liquid phases are collected. The proportion of gas and liquid phase components is quantitatively calculated and the sub-mineral types are identified by comparing peak positions and integrating peak areas. 3D CT scanning module: Controls the vertical step size of the sample stage to scan layer by layer, and combines acoustic tweezers to lock and ensure the stability of the bubble position in each layer. At the same time, Raman microscopy simultaneously acquires spectral data and bright field images to generate a composite dataset. Through threshold segmentation and region growth algorithms, gas phase, liquid phase and daughter mineral regions are extracted to obtain morphological data of inclusions at different depths and construct a 3D model. Data Analysis Module: Based on acoustic tweezers parameters, finite element analysis is performed to simulate the influence of acoustic radiation pressure on bubble morphology and a deformation-volume correction model is established. Then, a geometric correction algorithm is used to adjust the volume calculation results, and finally, gas phase volume, liquid phase volume, daughter mineral volume, gas-liquid ratio and composition analysis report are output.

Images