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CN110567814B - Neutron imaging method for triaxial mechanical test of natural gas hydrate sediment - Google Patents

Neutron imaging method for triaxial mechanical test of natural gas hydrate sediment Download PDF

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CN110567814B
CN110567814B CN201910790243.2A CN201910790243A CN110567814B CN 110567814 B CN110567814 B CN 110567814B CN 201910790243 A CN201910790243 A CN 201910790243A CN 110567814 B CN110567814 B CN 110567814B
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neutron
natural gas
data wire
pressure
self
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CN110567814A (en
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李守定
陈卫昌
李晓
孙一鸣
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Institute of Geology and Geophysics of CAS
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Institute of Geology and Geophysics of CAS
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/203Measuring back scattering
    • G01N23/204Measuring back scattering using neutrons
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/08Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
    • G01N3/10Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces generated by pneumatic or hydraulic pressure
    • G01N3/12Pressure testing
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02Details not specific for a particular testing method
    • G01N2203/025Geometry of the test
    • G01N2203/0256Triaxial, i.e. the forces being applied along three normal axes of the specimen

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Abstract

The invention provides a method capable of carrying out high-precision imaging on an internal structure of a triaxial mechanical test of a natural gas hydrate sediment. The method is characterized in that by utilizing the characteristic that the molecular structure size of the hydrate is similar to the wavelength of cold neutrons, the mass attenuation coefficient of the neutron beams is improved by reducing the energy of the neutron beams, so that the distinguishing degree of natural gas hydrate, natural gas and water molecules is enhanced, the imaging resolution of the internal structure of the natural gas hydrate sediment is improved, and the high-precision imaging of the structure of the natural gas hydrate in the triaxial mechanical test process is realized. The creep and relaxation rules in the formation and decomposition processes of the natural gas hydrate sample can be obtained by the method, and the method is favorable for understanding the dynamic response process of the stability of the reservoir after the development of the natural gas hydrate. The method is characterized in that by utilizing the characteristic that the molecular structure size of the hydrate is similar to the wavelength of cold neutrons, the mass attenuation coefficient of the neutron beam is improved by reducing the energy of the neutron beam, so that the distinguishing degree of the natural gas hydrate, the natural gas and the water molecules is enhanced, the imaging resolution is improved, and the high-precision imaging of the dynamic gathering and dispersing process of the natural gas hydrate is realized.

Description

Neutron imaging method for triaxial mechanical test of natural gas hydrate sediment
Technical Field
The invention designs a neutron imaging method for a triaxial mechanical test of a natural gas hydrate sediment, and belongs to the technical field of natural gas hydrate exploitation.
Background
The investigation and development of natural gas hydrate have certain effects, but the formation, decomposition and secondary generation processes of natural gas hydrate in sediment, the existence form and behavior of the natural gas hydrate in sediment pores, the influence of hydrate formation decomposition on sediment physical properties (permeability, sonic velocity, heat conduction, electric conduction and the like), gas-liquid multiphase flow in a production system, the secondary generation of hydrate in reservoir sediment stability and a production string and other key basic scientific problems are unclear, so that the commercialization development of the natural gas hydrate is limited. The microscopic mechanisms of the formation and decomposition and structural stability of natural gas hydrates within reservoir pores are poorly understood, and the main difficulty is that the formation and decomposition and structural high-precision imaging of natural gas hydrates under temperature and pressure environments are limited by current technical means. Current natural gas hydrate microscopic imaging mainly depends on electron imaging techniques such as X-ray diffraction (XRD) and X-ray CT (X-ray CT). The X-ray diffraction can determine the crystal structure type of the natural gas hydrate through diffraction peaks, but cannot realize imaging of the dynamic aggregation and dispersion process of the natural gas hydrate; the X-ray CT imaging technology relies on density difference of an object to be detected, and the hydrate mainly comprises natural gas (mainly methane molecules) and water molecules, the molecular weight of the natural gas hydrate and the water molecules are close, and the natural gas hydrate is difficult to distinguish by the X-ray CT, so that the phase state imaging precision of the natural gas hydrate is extremely limited. Indoor triaxial mechanical tests are an important means for researching the structural stability of natural gas hydrate sediment, but the X-ray has limited capability of penetrating through a high-pressure cavity, and is difficult to be applied to detecting the dynamic process and thermodynamic process of hydrate formation and decomposition. Therefore, the current technology of X-ray diffraction and X-ray CT technology cannot meet the imaging requirement of triaxial mechanical test of natural gas hydrate sediment.
Neutrons are uncharged and can penetrate the material without being destructive, thereby giving internal force field information of the material phase; the effect of neutrons and atomic nuclei does not change regularly with atomic numbers, so that light elements and adjacent elements can be better distinguished through neutron scattering or imaging technology; the neutron diffraction has high penetrability, can be tested and researched in special experimental environments such as high pressure, low temperature, strong field and different environments, can be used for exploring the static microstructure of a substance, can be used for researching the material dynamics process, and provides possibility for imaging the internal structure of the triaxial mechanical test of the natural gas hydrate sediment.
Disclosure of Invention
The invention provides a method capable of carrying out high-precision imaging on an internal structure of a triaxial mechanical test of a natural gas hydrate sediment. The method is characterized in that by utilizing the characteristic that the molecular structure size of the hydrate is similar to the wavelength of cold neutrons, the mass attenuation coefficient of the neutron beams is improved by reducing the energy of the neutron beams, so that the distinguishing degree of natural gas hydrate, natural gas and water molecules is enhanced, the imaging resolution of the internal structure of the natural gas hydrate sediment is improved, and the high-precision imaging of the structure of the natural gas hydrate in the triaxial mechanical test process is realized.
The main technical scheme of the neutron imaging method for the triaxial mechanical test of the natural gas hydrate deposit consists of six parts: the device consists of a self-balancing pressure chamber part, a triaxial host loading part, a closed-loop servo control part, an air source power part, a turntable part and a neutron ray part. The self-balancing pressure chamber is characterized by comprising the following parts: the device comprises a rock sample, an upper cushion block, a lower cushion block, a spherical seat, a triaxial cylinder, a high-pressure oil pipe, a self-balancing piston upper cavity and a self-balancing piston, wherein the rock sample is arranged between the upper cushion block and the lower cushion block, the maximum diameter of the rock sample is 100mm, the spherical seat is arranged below the lower cushion block, the full-angle adjustment of the spherical seat avoids the stress concentration of the end face in the rock sample loading process, the high-pressure oil pipe is connected with the triaxial cylinder, so that the triaxial cylinder is filled with methane gas to load confining pressure, the self-balancing piston upper cavity is connected with the self-balancing piston upper cavity, the air pressure is ensured to be equal, and the self-balancing piston can keep balance when moving up and down for loading; the triaxial host loading part consists of a fixed frame, an actuator lower cavity and an actuator piston, wherein the actuator lower cavity is connected with the air source power part, and the actuator piston moves up and down through air source power loading to realize loading of a rock sample; the closed-loop servo control part consists of a data wire, a confining pressure servo valve, a multichannel digital closed-loop servo controller, an axle pressure servo valve, a deformation data wire, a data line table, a stress data wire, a temperature data wire, a displacement data wire and a control computer, wherein the data line table leads out the deformation data wire, the stress data wire, the temperature data wire, the displacement data wire, the deformation data wire, the stress data wire, the temperature data wire and the displacement data wire from the self-balancing pressure chamber part, the multichannel digital closed-loop servo controller is respectively connected with the multichannel digital closed-loop servo controller, the multichannel digital closed-loop servo controller takes sensor data as a servo variable, and is communicated with the control computer through the data wire and performs data interaction, and the multichannel digital closed-loop servo controller controls the confining pressure servo valve and the axle pressure servo valve through control parameters, so that closed-loop servo control of an air source power part is realized; the air source power part consists of a confining pressure booster, methane gas, an air pump, an overflow valve and a Freon cooler, the air pump presses the methane gas into the overflow valve through a three-way high-pressure oil pipe, and when the output pressure is greater than the pressure value of the overflow valve, the methane gas returns redundant pressure to the methane gas tank through the overflow valve, so that the output pressure of the air pump is adjustable and stable, the power loading of the axial pressure is ensured, and the power loading of the confining pressure is realized through the confining pressure booster; the turntable part consists of a high-precision digital turntable and a turntable bracket, wherein the high-precision digital turntable adopts a high-precision turntable with a load of 20kN and a rotation stability of 5 seconds, and the self-balancing pressure chamber part, the triaxial host loading part, the closed-loop servo control part and the air source power part are arranged on the high-precision digital turntable, so that the host is ensured to rotate in high precision, and the high-precision digital turntable is arranged on the turntable bracket; the neutron ray part comprises a neutron ray source, a rotary collimator, a liquid hydrogen cooling box, a speed selector, a neutron flight tube, cold neutron rays, a detector column and a neutron catcher, wherein the cold neutron ray source and the detector are respectively arranged on the detector column, the neutron ray source excites the neutron rays to pass through the rotary collimator and the liquid hydrogen cooling box, the temperature reduction of the neutron source is realized, the speed of a neutron beam is controlled by the neutron beam speed selector, a neutron beam with a neutron wavelength lower than the hydrate molecular Bragg limit is obtained, the neutron rays are transmitted through a triaxial cylinder and a rock sample through the neutron flight tube and are received by the detector, and redundant neutron beams are received by the neutron catcher.
Description of the drawings: FIG. 1 is a schematic diagram of a neutron imaging method for triaxial mechanical testing of natural gas hydrate deposits.
1: a rock sample; 2: an upper cushion block; 3: a lower cushion block; 4: a spherical seat; 5: a triaxial cylinder; 6: a data wire; 7: a high pressure oil pipe; 8: self-balancing piston upper chamber; 9: a self-balancing piston lower chamber; 10: a self-balancing piston; 11: a fixed frame; 12: an actuator lower chamber; 13: an actuator piston; 14: a confining pressure electrohydraulic servo valve; 15: a confining pressure booster; 16: a multichannel digital closed loop servo controller; 17: a servo valve; 18: methane gas; 19: a high pressure air pump; 20: an overflow valve; 22: freon refrigerator; 23: a control computer; 24: a deformed data line; 25: a data hub station; 26: stress data line; 27: a temperature data line; 28: a displacement data line; 29: a high-precision digital turntable; 30: a turntable support; 31: a neutron source; 32: rotating the collimator; 33: a liquid hydrogen cooling tank; 34: a speed selector; 35: a neutron flight tube; 36: cold neutron rays; 37: a detector; 38: a detector column; 39: a neutron trap.
Basic principle and technique
The neutron beam can transmit different materials to generate different attenuation characteristics, and the attenuation effect is related to elements, density and the like of the materials, so that the composition and structural information inside the materials can be analyzed through the transmitted neutron beam. The spatial distribution of the transmitted neutron fluence rate is displayed by a detection technology and an image display technology, so that the spatial distribution, the density change and various defect information of the sample to be detected can be obtained. Cold neutrons are neutrons with kinetic energy of millielectron volt magnitude or lower, generally ranging from neutron kinetic energy less than 0.005eV, and having longer de broglie wavelength than thermal neutron wavelength, and scattering characteristics suitable for studying the substructure and excitation of condensed substances, in particular high molecular compounds and biological macromolecules. The closer the wavelength of neutrons is to the structural size of the polymer in the condensed state to be detected, the stronger the attenuation effect of neutron beams is, so that the larger the contrast of neutron imaging is, the higher the resolution is. The neutron source of the reactor active area or the reflecting layer is cooled by utilizing liquid hydrogen to improve the cold neutron content in the neutron beam, the speed of the neutron beam is controlled by a speed selector, the cold neutron beam with the wavelength lower than the Bragg limit of the hydrate molecule is obtained, the cold neutron beam transmits the hydrate to be detected through a neutron flight tube, the light intensity distribution of the intensity space distribution of the neutron beam is converted by utilizing a converter, the light intensity distribution of the neutron beam is converted into an electric signal by utilizing an imaging plate, and the digital image output is realized.
Detailed Description
1. The rock sample 1 is placed between the upper cushion block 2 and the lower cushion block 3, the centering is carried out, the length and the position of a sample are recorded, and the triaxial cylinder 5 is packaged;
2. the positions of the cold neutron ray source on the detector column 38 are adjusted, and the positions of the detector 37 and the detector column 38 are adjusted, so that the cold neutron ray 36 can completely cover the rock sample 1 and reach the detector 37;
3. opening a control computer 23, opening the multi-channel digital closed-loop servo controller 16, and connecting the control computer 23 with the multi-channel digital closed-loop servo controller 16 to keep data communication;
4. setting the sampling parameters of each sensor of the physical quantity measuring part on the control computer 23, setting the force loading or displacement loading parameter waveforms in the test process, and starting high-precision
A digital turntable starts a rock mechanics neutron imaging test;
5. after the test is completed, the values of the sensors of the dynamic measurement part of the test are stored in the control computer 23, the actuator piston 13 is displaced downwards, the rock sample 1 is unloaded, and the test is completed.

Claims (1)

1. The neutron imaging method for the natural gas hydrate sediment triaxial mechanical test comprises a self-balancing pressure chamber part, a triaxial host loading part, a closed-loop servo control part, an air source power part, a turntable part and a neutron ray part, wherein the self-balancing pressure chamber part comprises a rock sample (1), an upper cushion block (2), a lower cushion block (3), a spherical seat (4), a triaxial cylinder (5), a high-pressure oil pipe (7), a self-balancing piston upper cavity (8), a self-balancing piston lower cavity (9) and a self-balancing piston (10), the rock sample (1) is arranged between the upper cushion block (2) and the lower cushion block (3), the maximum diameter of a sample is 100mm, the spherical seat (4) is arranged below the lower cushion block (3), the full-angle adjustment of the spherical seat (4) avoids stress concentration of the end face in the sample loading process, the high-pressure oil pipe (7) is connected with the triaxial cylinder (5), so that the triaxial cylinder (5) is filled with methane gas loading confining pressure, the self-balancing piston upper cavity (8) is connected with the self-balancing piston lower cavity (9), and the self-balancing piston lower cavity (9) is ensured to be balanced when the self-balancing piston (10) moves up and down for loading; the triaxial host loading part consists of a fixed frame (11), an actuator lower cavity (12) and an actuator piston (13), wherein the actuator lower cavity (12) is connected with the air source power part, and the actuator piston (13) moves up and down through air source power loading to realize loading of a rock sample (1); the closed-loop servo control part consists of a data wire (6), a confining pressure servo valve (14), a multi-channel digital closed-loop servo controller (16), a shaft pressure servo valve (17), a deformation data wire (24), a data line collecting table (25), a stress data wire (26), a temperature data wire (27), a displacement data wire (28) and a control computer (23), wherein the data line collecting table (25) is used for leading out the deformation data wire (24), the stress data wire (26), the temperature data wire (27), the displacement data wire (28), the deformation data wire (24), the stress data wire (26), the temperature data wire (27) and the displacement data wire (28) are respectively connected into the multi-channel digital closed-loop servo controller (16), and the multi-channel digital closed-loop servo controller (16) is communicated with the control computer (23) through the data wire (6) and performs data interaction, so that the multi-channel digital closed-loop servo controller (16) controls the confining pressure servo valve (14) and the shaft pressure servo valve (17) through control parameters, thereby realizing closed-loop servo control of an air source power part; the air source power part consists of a confining pressure booster (15), methane gas (18), an air pump (19), an overflow valve (20) and a Freon cooler (22), wherein the air pump (19) presses the methane gas (18) into the overflow valve (20) through a high-pressure oil pipe (7), and when the output pressure is greater than the pressure value of the overflow valve, the methane gas (18) returns redundant pressure to the methane gas tank through the overflow valve (20), so that the output pressure of the air pump is adjustable and stable, the power loading of axial pressure is ensured, and the power loading of confining pressure is realized through the confining pressure booster (15); the turntable part consists of a high-precision digital turntable (29) and a turntable bracket, wherein the high-precision digital turntable (29) adopts a high-precision turntable with a load of 20kN and a rotation stability of 5 seconds, a self-balancing pressure chamber part, a triaxial host loading part, a closed-loop servo control part and an air source power part are arranged on the high-precision digital turntable (29), so that the host is ensured to rotate with high precision, and the high-precision digital turntable (29) is arranged on the turntable bracket (30); the neutron ray part comprises a neutron source (31), a rotary collimator (32), a liquid hydrogen cooling tank (33), a speed selector (34), a neutron flight tube (35), cold neutron rays (36), a detector (37), a detector upright post (38) and a neutron catcher (39), wherein the cold neutron ray source and the detector (37) are respectively arranged on the detector upright post (38), the neutron source (31) excites neutron rays to pass through the rotary collimator (32) and the liquid hydrogen cooling tank (33), the temperature reduction of the neutron source is realized, the speed of a neutron beam is controlled by the neutron beam speed selector (34), a neutron beam with a neutron wavelength lower than the molecular Bragg limit of the hydrate is obtained, the neutron rays (36) penetrate through the neutron flight tube (35) and the triaxial cylinder (5) and the rock sample (1), the redundant neutron beam is received by the detector (37), and the redundant neutron beam is received by the neutron catcher (39).
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PCT/CN2019/103964 WO2021035765A1 (en) 2019-08-26 2019-09-02 Method for neutron imaging during triaxial mechanical test of sediment of natural gas hydrate

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