CN111579569A - Neutron scattering experimental system for simulating high-temperature and high-pressure sample environment - Google Patents
Neutron scattering experimental system for simulating high-temperature and high-pressure sample environment Download PDFInfo
- Publication number
- CN111579569A CN111579569A CN202010469270.2A CN202010469270A CN111579569A CN 111579569 A CN111579569 A CN 111579569A CN 202010469270 A CN202010469270 A CN 202010469270A CN 111579569 A CN111579569 A CN 111579569A
- Authority
- CN
- China
- Prior art keywords
- shell
- window
- heating
- unit
- neutron scattering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating 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
- G01N23/20—Investigating 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating 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
- G01N23/20—Investigating 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
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating 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
- G01N23/20—Investigating 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
- G01N23/201—Investigating 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 by measuring small-angle scattering
- G01N23/202—Investigating 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 by measuring small-angle scattering using neutrons
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention belongs to the technical field of emerging unconventional oil and gas experiments, and particularly relates to a neutron scattering experiment system for simulating a high-temperature and high-pressure sample environment. The utility model provides a neutron scattering experimental system of simulation high temperature high pressure sample environment, includes air supply, neutron scattering device and heating pressure boost unit, the third of air supply give vent to anger the end with the third inlet end of heating pressure boost unit is connected, the fourth of heating pressure boost unit give vent to anger the end with first inlet end intercommunication, the air supply be used for to heating pressure boost unit conveying gas, heating pressure boost unit is used for carrying on gas after the heating pressure boost handles again to the casing. The neutron scattering experiment system can realize the simulation of the in-situ high-temperature and high-pressure sample environment of the stratum in the neutron scattering experiment, and further enables the application of the neutron scattering technology in the characterization of the nano-pore structure of the shale gas reservoir under the in-situ gas pressure conditions of overpressure, normal pressure and the like to be possible.
Description
Technical Field
The invention belongs to the technical field of emerging unconventional oil and gas experiments, and particularly relates to a neutron scattering experiment system for simulating a high-temperature and high-pressure sample environment.
Background
Shale gas has become an important component of global energy over the past decades, but there is great uncertainty in its long-term growth potential and sustainability. Oil and gas recovery from shale and other tight formations is low, with shale gas recovery rates below 20%. The phenomena of low recovery of shale oil and gas reservoirs and obvious reduction of gas well yield are related to the nano-scale pores and low permeability of shale matrix. Therefore, in order to improve the oil and gas recovery efficiency of the shale matrix, it is necessary to research the nano-pore structure and the restriction fluid behavior.
In recent years, small and ultra-small angle neutron scattering (SANS and USANS) have significant advantages over other characterization methods such as fluid invasion, gas adsorption, nuclear magnetic resonance, etc., and have become one of the most powerful methods for characterizing the structure of shale nanopores and confining fluid behavior. However, the research on the structure of the shale nanopore and the behavior of the restriction beam is limited in the normal-temperature and normal-pressure sample environment provided by the neutron scattering station. Therefore, neutron scattering experimental devices capable of applying hydrostatic pressure and uniaxial stress have been developed to study the behavior of shale pore fluid under reservoir pressure and hydraulic fracturing conditions. However, no corresponding solution is available for an experimental device which can provide a high-temperature and high-pressure gas environment and is used for characterization research on the nano-pore structure of the overpressure and normal-pressure shale gas reservoir.
Disclosure of Invention
In view of this, the invention provides a neutron scattering experimental system for simulating a high-temperature and high-pressure sample environment.
The invention provides a neutron scattering experimental system for simulating a high-temperature and high-pressure sample environment, which comprises a gas source, a neutron scattering device and a heating and pressurizing unit, wherein the gas source is connected with the neutron scattering device;
the neutron scattering device comprises a shell, a lofting unit and a heating unit, wherein the shell is of a cylindrical structure and is horizontally arranged, an incident channel penetrating through the shell along the axial direction of the shell is arranged in the middle of the shell, the lofting unit is arranged in the incident channel and detachably connected with the shell through a fastener, the lofting unit is used for placing a sample, the heating unit is arranged in the shell and is used for heating the lofting unit, a first air inlet end and a first air outlet end are arranged on the shell, a second air inlet end and a second air outlet end are arranged on the lofting unit, the second air inlet end is communicated with the first air inlet end, and the second air outlet end is communicated with the first air outlet end;
the third of air supply give vent to anger the end with the third inlet end of heating pressure boost unit is connected, the fourth of heating pressure boost unit give vent to anger the end with first inlet end intercommunication, the air supply be used for to heating pressure boost unit carries gas, heating pressure boost unit is used for carrying on the heating pressure boost to gas after and carries to in the casing again.
Further, the air supply with be equipped with first pressure sensor and first evacuation interface in proper order along gas conveying direction on the return circuit that the heating and pressurizing unit is connected, the heating and pressurizing unit with be equipped with first rupture disk, pressure release valve, second pressure sensor, second evacuation interface, isolation valve and second rupture disk in proper order along gas conveying direction on the return circuit that the casing is connected, first evacuation interface with second evacuation interface all is used for external vacuum pump.
Furthermore, the shell comprises an outer shell and an inner shell which are both cylindrical structures, a first incident channel which penetrates through the outer shell along the axial direction of the outer shell is arranged in the middle of the outer shell, the inner shell is coaxially arranged in the first incident channel, a first cavity is formed between the outer wall of the inner shell and the inner wall of the outer shell, the heating unit is arranged in the first cavity, a second incident channel which penetrates through the inner shell along the axial direction of the inner shell is arranged in the middle of the inner shell, the second incident channel is communicated with the first incident channel, the lofting unit and the fastening piece are both arranged in the first incident channel, a first sub air inlet and a first sub air outlet are respectively arranged on the outer shell, a second sub air inlet and a second sub air outlet are respectively arranged on the outer side wall of the inner shell, and the second sub air inlet and the second sub air outlet are respectively communicated with the first sub air inlet and the first sub air outlet, the heating and pressurizing unit is communicated with the first sub-air inlet.
Furthermore, the shell is hollow, and a cooling unit is arranged in the shell and used for cooling the shell.
Furthermore, the cooling unit is water, and the shell is provided with a water inlet and a water outlet which are communicated with the inside of the shell.
Further, the first incident channel is composed of a first channel, a first accommodating through groove and a second channel which are arranged along the axial direction of the outer shell and sequentially communicated, the inner shell is coaxially arranged in the first accommodating through groove, the outer wall of the first incident channel and the inner wall of the first accommodating through groove form a first cavity, the heating unit is a heating pipe of an annular structure, the heating pipe is coaxially sleeved outside the inner shell, a heat insulation piece is filled between the first accommodating through groove and the outer shell, a fourth sub air inlet and a fourth sub air outlet which are respectively communicated with the first sub air inlet and the first sub air outlet are arranged on the heat insulation piece, and the second incident channel is respectively communicated with the first channel and the second channel.
Furthermore, the lofting unit comprises a window body and two window body supporting pieces, wherein the window body and the two window body supporting pieces are both of a cylindrical structure, each window body supporting piece is provided with a third incident channel which penetrates through the window body supporting piece along the axial direction of the window body supporting piece, the two window body supporting pieces are coaxially and alternately arranged in the second incident channel, an air inlet channel which is respectively communicated with the second sub air inlet and the second sub air outlet is formed between the two window body supporting pieces, one opposite ends of the two window body supporting pieces are coaxially provided with object placing through grooves which are communicated with the corresponding second incident channels, the two object placing through grooves jointly enclose an object placing cavity matched with the window body, the window body is detachably arranged in the object placing cavity, the window body is respectively provided with a third sub air inlet and a third sub air outlet which are communicated with the air inlet channel, and the window body is used for placing a, the fastener is arranged at the rear end of the window body supporting piece positioned at the rear and is detachably connected with the window body supporting piece.
Furthermore, the second incident channel comprises a third channel, a second accommodating through groove and a third accommodating through groove which are arranged along the axial direction of the inner shell and are sequentially communicated, the second accommodating through groove is matched with the window body supporting part, the aperture of the second accommodating through groove is larger than that of the third channel, the two window body supporting parts are coaxially arranged in the second accommodating through groove, the front end of the window body supporting part in front is abutted against the side wall of the corresponding side of the second accommodating through groove, and the fastening part and the third accommodating through groove are matched with each other to form a sleeve which is arranged in the third accommodating through groove and detachably connected with the rear end of the window body supporting part in the rear.
Further, the window body comprises a window frame of a cylindrical structure and two sapphire circular lenses matched with the window frame, the window frame is coaxially and detachably mounted in the object placing cavity, the sapphire circular lenses are coaxially and detachably mounted in the window frame and are respectively distributed along the axial direction of the window frame at intervals, a second cavity used for placing a sample is jointly limited by the sapphire circular lenses and the inner wall of the window frame, and the third sub air inlet and the third sub air outlet are both formed in the window frame and are communicated with the second cavity.
Further, the heating and pressurizing unit is a supercharger.
The technical scheme provided by the invention has the beneficial effects that: the neutron scattering experiment system for simulating the high-temperature and high-pressure sample environment can realize the simulation of the in-situ high-temperature and high-pressure sample environment of the stratum in the neutron scattering experiment, further enables the application of the neutron scattering technology to the characterization of the nano pore structure of the shale gas reservoir under the in-situ gas pressure conditions of overpressure, normal pressure and the like to be possible, further expands the application range of the neutron scattering technology to the shale reservoir research, and has the advantages of convenience in operation and the like. In addition, the system can realize the repeated utilization of experimental gas, and has good economic performance.
Drawings
FIG. 1 is a schematic structural diagram of a neutron scattering experimental system for simulating a high-temperature high-pressure sample environment according to the present invention;
fig. 2 is a cross-sectional view of a neutron scattering device of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
Referring to fig. 1-2, a neutron scattering experimental system for simulating a high-temperature and high-pressure sample environment includes an air source 10, a neutron scattering device 100, and a heating and pressurizing unit 20, where the neutron scattering device 100 includes a casing, a lofting unit, and a heating unit 30, the casing includes an outer casing 31 and an inner casing 32 both having a cylindrical structure, the outer casing 31 is horizontally disposed, a first incident channel axially penetrating the outer casing is disposed in the middle of the outer casing 31, a first sub air inlet 311 and a first sub air outlet communicated with the first incident channel are respectively disposed on the outer side wall of the outer casing, the first sub air inlet 311 and the first sub air outlet are uniformly distributed at intervals along the circumferential direction of the outer casing 31, the inner casing 32 is coaxially disposed in the first incident channel, a first cavity 313 is formed between the outer wall of the inner casing 32 and the inner wall of the outer casing 31, the heating unit 30 is disposed in the first cavity 313, the middle part of the inner shell 32 is provided with a second incident channel which penetrates through the inner shell in the axial direction, the second incident channel is communicated with the first incident channel, the outer side wall of the inner shell 32 is respectively provided with a second sub air inlet and a second sub air outlet which are communicated with the second incident channel, the second sub air inlet is communicated with the first sub air inlet 311, the second sub air outlet is communicated with the first sub air outlet, the lofting unit comprises a window body 34 which is of a cylindrical structure and two window body supporting pieces 33, each window body supporting piece 33 is provided with a third incident channel 331 which penetrates through the window body supporting piece in the axial direction, the two window body supporting pieces 33 are coaxially and alternately arranged in the second incident channel, the two third incident channels 331 are communicated with the second incident channel, and an air inlet channel which is respectively communicated with the second sub air inlet and the second sub air outlet is formed between the two window body supporting pieces 33, two opposite ends of the window body supporting member 33 are coaxially provided with storage through grooves of a cylindrical structure, the storage through grooves are communicated with the corresponding second incident channels, the two storage through grooves jointly enclose a storage cavity matched with the window body 34, the window body 34 is a sapphire observation window, and mainly comprises a window frame of a cylindrical structure and two sapphire circular lenses, the window frame is coaxially and detachably installed in the storage cavity, the two sapphire circular lenses are coaxially and detachably installed in the window frame and are distributed at intervals along the axial direction of the window frame, the two sapphire circular lenses and the inner wall of the window frame jointly define a second chamber 341 for placing a sample, the window frame is respectively provided with a third sub air inlet and a third sub air outlet communicated with the second chamber 341, and the third sub air inlet and the third sub air outlet are communicated with the air inlet channel, a third air outlet end of the air source 10 is connected with a third air inlet end of the heating and pressurizing unit 20 through a first pipeline, the fourth air outlet end of the heating and pressurizing unit 20 is communicated with the first sub-air inlet 311 through a second pipeline, and a first pressure sensor 40 and a first vacuum pumping interface 41 are sequentially arranged on the first pipeline along the gas conveying direction, a first rupture disk 42, a pressure release valve 43, a second pressure sensor 44, a second vacuum-pumping interface 45, an isolation valve 46 and a second rupture disk 47 are sequentially arranged on the second pipeline along the gas conveying direction, wherein the heating unit 30 is used for heating the inner shell 32, the gas source 10 is used for delivering gas to the heating and pressurizing unit 20, the heating and pressurizing unit 20 is configured to heat and pressurize gas, and the first vacuum pumping interface 41 and the second vacuum pumping interface 45 are both configured to be externally connected to a vacuum pump.
In the present invention, the heating and pressurizing unit 20 heats and pressurizes the gas, and the high-temperature and high-pressure gas is input into the second chamber 341 to achieve the purpose of simulating the high-temperature and high-pressure environment in the second chamber 341, and the heating unit 30 heats the inner shell 32 to keep the temperature of the high-temperature and high-pressure gas entering the second chamber 341 constant, thereby achieving the purpose of maintaining the gas pressure. In addition, the neutron scattering experiment system of the invention further comprises a control system and a temperature sensor, wherein the temperature sensor is arranged on the second pipeline and used for detecting the temperature value of the gas output from the fourth gas outlet end of the heating and pressurizing unit 20, the temperature sensor, the heating and pressurizing unit 20, the first pressure sensor 40 and the second pressure sensor 44 are all electrically connected with the control system, when the vacuum pump vacuumizes the system, the first pressure sensor 40 and the second pressure sensor 44 are used for detecting the pressure values in the first pipeline and the second pipeline and sending the detection signals to the control system so as to monitor whether the system reaches a vacuum state in real time, and the purpose of vacuumizing the system is to ensure the purity of the gas entering the second chamber 341. And after the pressurized and pressurized gas is output from the fourth gas outlet end of the heating and pressurizing unit 20, the temperature sensor and the second pressure sensor 44 respectively detect the temperature value and the pressure value of the pressurized and pressurized gas, and send the corresponding temperature value and pressure value to the control system, and the control system, the temperature sensor and the second pressure sensor 44 can achieve the purpose of controlling the temperature and the pressure of the gas input into the shell 31 in real time. The first rupture disk 42 and the second rupture disk 47 are used for respectively carrying out timely pressure relief treatment on the air pressure in the supercharger and the lofting unit after the air pressure in the supercharger and the lofting unit exceeds the calibrated maximum bearing pressure so as to ensure that the internal pressure of the supercharger and the lofting unit is in a safe pressure range. The isolation valve 46 is used for connecting and disconnecting the air path between the housing 31 and the heating and pressurizing unit 20. When the sample is loaded, only one of the sapphire circular lenses needs to be taken down, and after the sample is placed in the second chamber 341, the sapphire circular lens is installed in the window frame. It should be noted that, in the present invention, the connections between the outer shell 31 and the inner shell 32, the heating unit 30 and the inner shell 32, the window support 33 and the inner shell 32 and the fastener 50, the window 34 and the window support 33, and the sapphire circular lens and the window frame are all detachable connection structures, which can be detached and assembled according to experimental needs, but the present invention is not limited to the specific embodiment of detachable connection, and the structures that can realize detachable connection between the outer shell 31 and the inner shell 32, between the heating unit 30 and the inner shell 32, between the window support 33 and the inner shell 32 and the fastener 50, between the window 34 and the window support 33, and between the sapphire circular lens and the window frame can be all used as specific embodiments of corresponding detachable connection in the present invention, such as a snap connection and a threaded connection.
When a neutron scattering experiment is performed, the neutron scattering research experiment of the shale sample can be performed in different high-temperature and high-pressure environments only by placing the shale sample to be researched into the second chamber 341 and simulating different high-temperature and high-pressure environments in the second chamber 341.
In the above embodiment, the first incident channel and the second incident channel form an incident channel of the housing, the first sub air inlet 311 and the second sub air inlet form a first air inlet end of the housing, the first sub air outlet and the second sub air outlet form a first air outlet end of the housing, and the first sub air inlet 311, the second sub air inlet, the air inlet channel, the third sub air inlet, the third sub air outlet, the second sub air outlet and the first sub air outlet are all located on the same vertical plane and are communicated with each other, so as to achieve the purpose of inputting high-pressure air into the second chamber 341. In addition, for the convenience of gas entering the second chamber 341, the second sub-gas inlet and the second sub-gas outlet are both connected with gas tubes 38, and the two gas tubes respectively and correspondingly penetrate through the first sub-gas inlet 311 and the first sub-gas outlet and extend out of the housing 31,
the gas source 10 is a gas storage cylinder, nitrogen is stored in the gas storage cylinder, and the specification is 40L. And the gas storage cylinder is respectively provided with a first gas inlet valve 11 and a pressure reducing valve 12. The heating and pressurizing unit 20 is a supercharger, the capacity of the supercharger is within 20ml, and the supercharger heats the received gas to be less than or equal to 200 ℃ and pressurizes the gas to ensure that the pressurized gas reaches the high pressure of not less than 70 Mpa. And the supercharger is distributed with a second air inlet valve. The second chamber 341 has a volume of about 1ml and the lofting unit of the invention can withstand high temperature of 150 ℃ and high pressure of 70 Mpa. The pressurized gas may sequentially enter the second chamber 341 through the first sub-inlet 311, the second sub-inlet, the inlet passage, and the third sub-inlet.
In the above embodiment, the first incident channel includes a first channel 315, a first accommodating through groove and a second channel 316 that are arranged along the axial direction of the outer shell 31 and sequentially communicated with each other, the aperture of the first accommodating through groove is larger than the apertures of the first channel 315 and the second channel 316, the inner shell 32 is coaxially arranged in the first accommodating through groove, the first cavity 313 is formed between the outer wall of the inner shell and the inner wall of the first accommodating through groove, the heating unit 30 is a heating pipe with an annular structure, the heating pipe is coaxially sleeved outside the inner shell 32, a heat insulating member 35 is filled between the first accommodating through groove and the outer shell 31, and the heat insulating member 35 is provided with a fourth sub air inlet and a fourth sub air outlet that are respectively communicated with the first sub air inlet 311 and the first sub air outlet.
In the present invention, the thermal insulation member 35 is a thermal insulation asbestos pad filled on the inner wall of the first receiving through groove, and the thermal insulation member 35 serves to preserve heat of the inner shell 32 and prevent dissipation of gas heat in the second chamber 341, and on the other hand, to prevent the outer shell 31 from overheating, so as to ensure the temperature safety of the outer shell 31 and prevent hazards such as fire or scald. And in order to realize the compactness of the structure of the neutron scattering device 100 and improve the sealing performance thereof, the upper part and the lower part of the front and rear ends of the upper part and the lower part of the two ends of the inner shell 32 are respectively closely attached to the heat insulating member 35, and the outer periphery of the heating pipe extends to be attached to the heat insulating member 35. In order to prevent the heating pipe from affecting the operation of the second sub-inlet and the second sub-outlet, the heating pipe is disposed behind the second sub-inlet and the second sub-outlet, and the rear side of the heating pipe is flush with the rear end of the inner shell 32. The inner casing 32 and the outer casing 31 are both provided with through holes (not shown) for the electric wires of the heating tube to extend out, so that the heating tube can be conveniently connected with an external power supply, and in addition, the heating tube is electrically connected with a control system, and the control system automatically controls the opening and closing of the heating tube, the heating time and the heating temperature. The heating pipe has the advantages of high heating speed, low implementation cost and the like.
In the above embodiment, the casing 31 is hollow, a cooling unit is disposed in the casing, the cooling unit is water, and the casing 31 is provided with a water inlet and a water outlet communicated with the inside of the casing.
In the present invention, the cooling unit is used to cool the inner casing 32 and the second chamber 341, and is used together with the heating unit 30 to maintain the inner casing 32 and the second chamber 341 in a constant temperature and pressure state. In addition, as other embodiments of the cooling unit in the invention, the cooling unit can also be a semiconductor refrigeration sheet, and the cooling mode adopting water cooling has the advantages of low implementation cost, economy, environmental protection and the like.
In the above embodiment, the second incident passage includes the third passage 325, the second accommodating through groove, and the third accommodating through groove, which are provided in the axial direction of the inner casing 32 and communicate in this order, the second accommodating through groove is fitted to the window support 33, and the aperture thereof is larger than that of the third channel 325, two window supports 33 are coaxially disposed in the second receiving through groove, and the front end of the window support member 33 positioned at the front abuts against the side wall of the corresponding side of the second accommodating through groove, the fastening member 50 is a sleeve having an aperture larger than that of the third incident passage 331, the third receiving channel is adapted to the fastener 50, the fastener 50 is disposed in the third receiving channel, and coaxially sleeved at the rear end of the window support member 33 located at the rear, and the fastener 50 is detachably connected with the window support member 33.
In the present invention, the third channel 325 communicates with the first channel 315 to constitute a neutron scattering end, and the third accommodating through groove communicates with the second channel 316 to constitute a neutron incidence end. The installation mode of window 34 and two window support members 33 is that, after installing window 34 in putting the thing intracavity, will two window support members 33 all place the second and hold logical inslot back, establish the sleeve cover in the rear end of the window support member 33 that is located the rear again to with two window support members 33 centre gripping in inner shell 32. When the window 34 and the window supporting member 33 need to be removed, the fastener 50 is removed, and then the window supporting member 33 is ejected out together with the window 34 from the neutron scattering end. The detachable connection structure between the fastener 50 and the window support member 33 is not limited in the present invention, and any structure capable of realizing detachable connection between the fastener 50 and the window support member 33 in the prior art can be used as a specific embodiment of detachable connection between the fastener 50 and the window support member 33 in the present invention. Specifically, the fastener 50 is threadably engaged with the window support member 33.
The neutron scattering experiment system comprises the following operation steps:
1. sample loading: loosening the fasteners 50, removing the window supports 33 and the window 34, placing the sample into the second chamber 341 of the window 34, then installing the window 34 between the two window supports 33, installing the two window supports 33 back into the inner housing 32, and fixing the window supports 33 using the fasteners 50;
2. ensuring that all valves are in a closed state, externally connecting vacuum pumps at the first vacuumizing interface 41 and the second vacuumizing interface 45, and simultaneously starting the two vacuum pumps to vacuumize the supercharger and the shell;
3. after the vacuumizing treatment is finished, closing the first vacuumizing interface 41 and the second vacuumizing interface 45, opening the first air inlet valve 11 of the gas storage bottle and the second air inlet valve of the supercharger, conveying gas into the supercharger, after the supercharger is filled with the gas, closing the first air inlet valve 11 of the gas storage bottle and the second air inlet valve of the supercharger, and performing temperature and pressure increasing treatment on the gas by the supercharger;
4. opening a pressure release valve 43 and an isolation valve 46 of the supercharger to allow the gas subjected to temperature and pressure increasing treatment to pass through the housing and enter the second chamber 341, and simultaneously, starting the heating unit 30 and the water cooling unit to maintain the constant temperature and pressure state in the second chamber 341 and the safe temperature of the shell 31;
5. performing a neutron scattering experiment;
6. after the experiment is finished, closing the heating unit 30 and the water cooling unit, closing the supercharger, opening the pressure release valve 43 and the second vacuumizing interface 45 for pressure release, and standing until the shell is cooled;
7. cleaning: fastener 50 is loosened, window support 33 and window 34 are tooled out from the neutron scattering side, the sample is removed, and window 34 is wiped clean.
In addition, the neutron scattering experiment system can also realize the reutilization of the experiment gas, and the specific operation method comprises the following steps:
1. after the neutron scattering experiment is finished, the isolation valve 46 is opened to enable the shell to be communicated with the supercharger;
2. performing liquid nitrogen cooling bath treatment on the supercharger to enable the inside of the supercharger to be in a negative pressure state so as to enable the experimental gas in the shell to flow into the supercharger, closing the isolation valve 46 after the air pressure is balanced, and performing temperature and pressure increasing treatment on the returned gas by the supercharger again;
3. the sample in the second chamber 341 is replaced, and the operations 4-6 are repeated to perform the neutron scattering experiment on the new sample to be tested.
Because some experimental gases (such as deuterated methane) are expensive, the experimental gases can be recycled through the steps, the economic performance of the system is improved, in addition, the operation frequency of vacuumizing or pressure releasing of the system can be reduced through the method, and the method also has the advantages of simplifying the experimental steps, being convenient to operate and the like.
In this document, the terms front, back, upper and lower are used to define the components in the drawings and the positions of the components relative to each other, and are used for clarity and convenience of the technical solution. It is to be understood that the use of the directional terms should not be taken to limit the scope of the claims.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A neutron scattering experiment system for simulating a high-temperature and high-pressure sample environment is characterized by comprising a gas source (10), a neutron scattering device (100) and a heating and pressurizing unit (20);
the neutron scattering device (100) comprises a shell, a lofting unit and a heating unit (30), wherein the shell is of a cylindrical structure and is horizontally arranged, an incident channel penetrating through the shell along the axial direction of the shell is arranged in the middle of the shell, the lofting unit is arranged in the incident channel and detachably connected with the shell through a fastener (50), the lofting unit is used for placing a sample, the heating unit (30) is arranged in the shell and is used for heating the lofting unit, a first air inlet end and a first air outlet end are arranged on the shell, a second air inlet end and a second air outlet end are arranged on the lofting unit, the second air inlet end is communicated with the first air inlet end, and the second air outlet end is communicated with the first air outlet end;
the third of air supply (10) is given vent to anger the end with the third inlet end of heating pressure boost unit (20) is connected, the fourth of heating pressure boost unit (20) is given vent to anger the end with first inlet end intercommunication, air supply (10) be used for to heating pressure boost unit (20) conveying gas, heating pressure boost unit (20) are used for carrying on heating pressure boost to gas and carry to again in the casing after handling.
2. The neutron scattering experiment system for simulating the high-temperature and high-pressure sample environment according to claim 1, wherein a first pressure sensor (40) and a first vacuumizing interface (41) are sequentially arranged on a loop connected with the gas source (10) and the heating and pressurizing unit (20) along a gas conveying direction, a first rupture disk (42), a pressure release valve (43), a second pressure sensor (44), a second vacuumizing interface (45), an isolation valve (46) and a second rupture disk (47) are sequentially arranged on a loop connected with the heating and pressurizing unit (20) and the shell along the gas conveying direction, and the first vacuumizing interface (41) and the second vacuumizing interface (45) are both used for an external vacuum pump.
3. The neutron scattering experimental system for simulating the high-temperature and high-pressure sample environment according to claim 1, wherein the shell comprises an outer shell (31) and an inner shell (32) which are both cylindrical structures, a first incident channel axially penetrating the outer shell (31) is arranged in the middle of the outer shell, the inner shell (32) is coaxially arranged in the first incident channel, a first cavity (313) is formed between the outer wall of the inner shell (32) and the inner wall of the outer shell (31), the heating unit (30) is arranged in the first cavity (313), a second incident channel axially penetrating the inner shell (32) is arranged in the middle of the inner shell (32) and is communicated with the first incident channel, the lofting unit and the fastening member (50) are arranged in the first incident channel, and a first sub air inlet (311) and a first sub air outlet are respectively arranged on the outer shell (31), the outer side wall of the inner shell (32) is respectively provided with a second sub air inlet and a second sub air outlet, the second sub air inlet and the second sub air outlet are respectively communicated with the first sub air inlet (311) and the first sub air outlet, and the heating and pressurizing unit (20) is communicated with the first sub air inlet (311).
4. The neutron scattering experiment system for simulating the high-temperature and high-pressure sample environment according to claim 3, characterized in that the inside of the shell (31) is hollow, and a cooling unit is arranged in the shell and used for cooling the shell (31).
5. The neutron scattering experiment system for simulating the high-temperature and high-pressure sample environment according to claim 4, wherein the cooling unit is water, and the shell (31) is provided with a water inlet and a water outlet communicated with the inside of the shell.
6. The neutron scattering experimental system for simulating the environment of the high-temperature and high-pressure sample according to claim 3, characterized in that the first incident channel consists of a first channel (315), a first accommodating through groove and a second channel (316) which are arranged along the axial direction of the outer shell (31) and are communicated in sequence, the inner shell (32) is coaxially arranged in the first accommodating through groove, the first cavity (313) is formed between the outer wall of the heating unit and the inner wall of the first accommodating through groove, the heating unit (30) is a heating pipe with an annular structure, which is coaxially sleeved outside the inner shell (32), a heat insulation piece (35) is filled between the first containing through groove and the outer shell (31), the heat insulation piece (35) is provided with a fourth sub air inlet and a fourth sub air outlet which are respectively communicated with the first sub air inlet (311) and the first sub air outlet, the second incident channel communicates with the first channel (315) and the second channel (316), respectively.
7. The neutron scattering experimental system for simulating the high-temperature and high-pressure sample environment according to claim 3, wherein the lofting unit comprises a window (34) and two window supports (33) which are both of a cylindrical structure, each window support (33) is provided with a third incident channel (331) which axially penetrates through the window support, the two window supports (33) are coaxially and intermittently arranged in the second incident channel, an air inlet channel which is respectively communicated with the second sub air inlet and the second sub air outlet is formed between the two window supports (33), opposite ends of the two window supports (33) are coaxially provided with article placing through grooves which are communicated with the corresponding second incident channels, and the two article placing through grooves jointly enclose an article placing cavity matched with the window (34), window body (34) detachable install put the thing intracavity, be equipped with respectively on window body (34) with air inlet channel communicates's third sub-air inlet and third sub-gas outlet, window body (34) are used for placing the sample, fastener (50) set up be located the rear in the rear end of window body support piece (33) to with window body support piece (33) detachable connection.
8. The neutron scattering experimental system for simulating the environment of the high-temperature and high-pressure sample according to claim 7, characterized in that the second incident channel comprises a third channel (325), a second accommodating through groove and a third accommodating through groove which are arranged along the axial direction of the inner shell (32) and are communicated in sequence, the second accommodating through groove is matched with the window support member (33), and the aperture of which is larger than that of the third channel (325), two window supports (33) are coaxially arranged in the second accommodating through groove, the front end of the window support member (33) positioned in front is abutted against the side wall of the corresponding side of the second accommodating through groove, the fastener (50) is matched with the sleeve of the third accommodating through groove, which is arranged in the third accommodating through groove and detachably connected with the rear end of the window support member (33) located at the rear.
9. The neutron scattering experiment system for simulating the high-temperature and high-pressure sample environment according to claim 7, wherein the window (34) comprises a window frame with a cylindrical structure and two sapphire circular lenses matched with the window frame, the window frame is coaxially and detachably mounted in the object placing cavity, the two sapphire circular lenses are coaxially and detachably mounted in the window frame and are respectively distributed at intervals along the axial direction of the window frame, the two sapphire circular lenses and the inner wall of the window frame jointly define a second chamber (341) for placing a sample, and the third sub air inlet and the third sub air outlet are both arranged on the window frame and are both communicated with the second chamber (341).
10. The neutron scattering experimental system for simulating the high-temperature and high-pressure sample environment according to claim 1, wherein the heating and pressurizing unit (20) is a pressure booster.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010469270.2A CN111579569A (en) | 2020-05-28 | 2020-05-28 | Neutron scattering experimental system for simulating high-temperature and high-pressure sample environment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010469270.2A CN111579569A (en) | 2020-05-28 | 2020-05-28 | Neutron scattering experimental system for simulating high-temperature and high-pressure sample environment |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111579569A true CN111579569A (en) | 2020-08-25 |
Family
ID=72115839
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010469270.2A Pending CN111579569A (en) | 2020-05-28 | 2020-05-28 | Neutron scattering experimental system for simulating high-temperature and high-pressure sample environment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111579569A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113418944A (en) * | 2021-07-06 | 2021-09-21 | 散裂中子源科学中心 | Small-angle scattering temperature jump system |
| CN113960083A (en) * | 2021-09-14 | 2022-01-21 | 散裂中子源科学中心 | Experimental device for small-angle scattering experiment and gas mixing pressurization system |
-
2020
- 2020-05-28 CN CN202010469270.2A patent/CN111579569A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113418944A (en) * | 2021-07-06 | 2021-09-21 | 散裂中子源科学中心 | Small-angle scattering temperature jump system |
| CN113960083A (en) * | 2021-09-14 | 2022-01-21 | 散裂中子源科学中心 | Experimental device for small-angle scattering experiment and gas mixing pressurization system |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN212845119U (en) | Neutron scattering device for simulating high-temperature and high-pressure sample environment | |
| CN111579569A (en) | Neutron scattering experimental system for simulating high-temperature and high-pressure sample environment | |
| US11812732B2 (en) | Suction sampler system for in situ collection of deep-sea floor organisms and method of using same | |
| CN203940962U (en) | Lithium battery casing leakage detection apparatus | |
| CN103322857B (en) | Small two-stage light-gas gun | |
| CN212845118U (en) | High-temperature high-pressure gas source system for neutron scattering experiment | |
| CN110221640A (en) | A kind of controllable temperature pressure control air seal test platform auxiliary system | |
| CN106525687B (en) | Supercritical carbon dioxide soaks shale experimental apparatus | |
| CN205826237U (en) | The outer device for detecting leakage of a kind of heat exchanger internal hemorrhage due to trauma | |
| CN212568548U (en) | Neutron scattering experimental system for simulating high-temperature and high-pressure sample environment | |
| CN115487887B (en) | Temperature and pressure control method for high-temperature high-pressure micro-nano flow control chip holder | |
| CN111089746A (en) | Pressure-maintaining and heat-preserving sampling and transferring system and sampling and transferring method for benthos | |
| CN111076986A (en) | Full-sea deep macro-organism pump suction type fidelity acquisition and storage system and acquisition and storage method | |
| KR100717391B1 (en) | Apparatus for supplying underground water geotherm heat-exchanger | |
| CN109724835B (en) | Device and method for rapidly collecting sediment pore water containing natural gas hydrate on site | |
| CN112631178A (en) | Deep sea macro-organism fidelity sampling control system and control method | |
| CN217765379U (en) | High-temperature high-pressure helium leakage detection device | |
| CN101275806A (en) | Carbon dioxide supercritical drying device | |
| CN207894750U (en) | A kind of cladding tubes internal pressure explosion bulge test device | |
| CN106654373A (en) | Device for infiltrating electric core | |
| CN211904766U (en) | Full-sea deep macro-organism pump suction type fidelity acquisition and storage system | |
| CN210923608U (en) | Gas analysis device | |
| CN111855308B (en) | Air cabin compression type active pressure-maintaining in-situ seawater sampler and sampling method thereof | |
| CN1614384A (en) | Submarine volcano hot liquid sampler | |
| CN211952244U (en) | Welding heat insulation gas cylinder interlayer vacuumizing device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |