High-temperature nuclear magnetic resonance probe and high-temperature nuclear magnetic resonance device

By introducing an atmosphere chamber and a multi-channel gas circuit system into the high-temperature NMR probe, the problem of not being able to provide multiple atmosphere environments and precisely controlling the gas pressure flow rate in the prior art is solved, and the precise control and detection sensitivity of multiple atmospheres at high temperatures is achieved.

CN114764078BActive Publication Date: 2025-08-15NINGBO INST OF MATERIALS TECH & ENG CHINESE ACAD OF SCI
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Patent Information

Application Number
CN202110048411.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2021-01-14
Publication Date
2025-08-15
Estimated Expiration
2041-01-14

AI Technical Summary

Technical Problem

Existing high-temperature NMR probes cannot provide different atmospheres (oxidation, reduction, inertness, corrosiveness, etc.) environments under high temperature environments, and it is difficult to accurately control the pressure and flow of the atmosphere, and the radio frequency coils are susceptible to oxidation or corrosion.

Method used

A high-temperature nuclear magnetic resonance probe is designed, including a solenoid radio frequency coil and an atmosphere chamber. The atmosphere chamber is located in or around the radio frequency coil and is equipped with an air inlet and exhaust port, which can provide different atmosphere environments and accurately control the pressure and flow of the gas through a multiple-channel gas system.

Benefits of technology

It realizes the barrier between the space around the sample and the space around the radio frequency coil under high temperature environment, can freely select the test atmosphere, and accurately control the pressure and flow of the gas, improving the signal-to-noise ratio and detection sensitivity.

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Abstract

This application discloses a high-temperature nuclear magnetic resonance (NMR) probe and device. The high-temperature NMR probe includes a radio frequency (RF) coil and an atmosphere chamber; the atmosphere chamber is at least partially located within the RF coil; alternatively, the RF coil is located within the atmosphere chamber; the atmosphere chamber is provided with an air inlet and an exhaust port for introducing gas into the atmosphere chamber. The probe contains the RF coil and the atmosphere chamber, and the atmosphere chamber can provide different atmospheres in a high-temperature environment, while also enabling precise control of the pressure and flow of the atmosphere.
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Description

Technical Field

[0001] The present application relates to a high-temperature nuclear magnetic resonance probe and a high-temperature nuclear magnetic resonance device, belonging to the technical field of nuclear magnetic resonance devices. Background Art

[0002] Nuclear magnetic resonance (NMR) technology is an important research method for probing the microstructure and dynamics of various materials. The NMR platform consists of three main components: a superconducting magnet, a control cabinet, and a probe. The superconducting magnet provides a highly uniform and stable magnetic field in the vertical direction. The control cabinet integrates functional components such as RF transmission and reception, and RF power amplification. The NMR probe integrates important instruments such as RF transceiver coils, tuning and impedance matching circuits, and a sample chamber, and is placed in the highly uniform magnetic field space generated by the superconducting magnet. In a high-temperature NMR probe, the most core part is the resonator composed of the sample and the RF coil. The resonator and other circuit devices in the probe form an RF resonant circuit, ultimately realizing the transmission and reception of RF signals.

[0003] In recent years, the need to study the structure and dynamics of various materials in high-temperature environments and under different atmospheres has grown rapidly (e.g., oxidation and reduction processes of metals, high-temperature heat treatment processes of materials, and corrosion processes at high temperatures). This demand has driven the development of NMR probes that can simultaneously provide high-temperature environments and different atmospheres for the samples being tested. Currently, there are two main types of high-temperature NMR probes. The first type uses a resistive heating element to heat the sample through heat conduction through a gas medium. However, both the sample and the radio frequency coil are exposed to high temperatures. Because the radio frequency coil is made of metal, it is not suitable for high-temperature oxidizing and corrosive atmospheres and will also experience slow oxidation in high-temperature inert gas environments. The second type of high-temperature NMR probe uses laser heating. Laser heating directly irradiates the sample or its crucible, heating it. The temperature of the radio frequency coil is then reduced by heat conduction through isolation between the sample and the radio frequency coil or by actively cooling the coil. However, current laser-heated NMR probes cannot simultaneously provide a high temperature environment with different atmospheres (oxidizing, reducing, inert, corrosive, etc.), nor can they precisely control the pressure and flow of the atmosphere according to actual needs. Summary of the Invention

[0004] According to one aspect of the present application, a high-temperature nuclear magnetic resonance probe is provided, which contains a solenoid-shaped radio frequency coil and an atmosphere chamber. The atmosphere chamber can provide different atmospheres in a high-temperature environment, and can also accurately control the pressure and flow of the atmosphere.

[0005] A high-temperature nuclear magnetic resonance probe comprises a radio frequency coil and an atmosphere chamber; the atmosphere chamber is at least partially located within the radio frequency coil; alternatively, the radio frequency coil is located within the atmosphere chamber; the atmosphere chamber is provided with an air inlet and an exhaust port for passing gas into the atmosphere chamber.

[0006] Specifically, the air inlet and the air outlet are used to respectively allow gas to enter or exhaust the atmosphere chamber.

[0007] Currently, there are still problems with laser-heated high-temperature NMR probes: In the existing technology, the laser directly irradiates the sample or the crucible containing the sample, thereby heating the sample. In order to improve the signal-to-noise ratio, the temperature of the RF coil needs to be reduced. Generally, thermal insulation materials are used to isolate the heat conduction between the sample and the RF coil. At the same time, air is blown to the outside of the RF coil to allow the flowing low-temperature gas medium to take away the heat of the RF coil. The low-temperature gas medium used for cooling is an inert or reducing gas, and oxidizing or corrosive gases cannot be used. Since the space around the sample is connected to the space around the RF coil, in this case, the type of gas in the space around the sample cannot be freely selected, and oxidizing or corrosive gases cannot be used. At the same time, it is also difficult to precisely control the pressure and flow of the gas.

[0008] In the present application, an atmosphere chamber is utilized to introduce gas of a desired atmosphere into the atmosphere chamber, thereby providing a static atmosphere environment or a flowing atmosphere environment, thereby achieving precise control over the pressure and flow of the gas.

[0009] In the present application, the atmosphere chamber is at least partially located within the RF coil, thereby isolating the space surrounding the sample from the space surrounding the RF coil. In this case, the required test environment atmosphere (e.g., oxidizing, reducing, inert, corrosive, etc.) can be freely selected, while also achieving precise control of the gas pressure and flow.

[0010] Specifically, the gas introduced into the atmosphere chamber in the present application includes one or more of oxygen, hydrogen, and inert gas. This application does not impose strict restrictions, and those skilled in the art can select a suitable atmosphere according to actual needs.

[0011] In the present application, there may be one, two, or more air inlets.

[0012] When there is one air inlet, it can be connected to an external vacuum system or gas source, the pressure of the atmosphere chamber can be controlled (vacuum to positive pressure), and a variety of different gases can be selected.

[0013] When there are two air inlets, one can be connected to the vacuum acquisition system and the other can be connected to the gas source, which can control the pressure of the atmosphere chamber (vacuum to positive pressure), select different types of gases, and accurately control the gas flow into the chamber.

[0014] When there are multiple gas inlets, one or more of them can be connected to the vacuum acquisition system, and the other gas lines can be connected to different types of gas sources, which can control the pressure of the atmosphere chamber (vacuum to positive pressure), select different types of gases, mix different types of gases, control the partial pressure of different gases, and accurately control the flow of each gas entering the chamber.

[0015] Optionally, the shape of the radio frequency coil is selected from any one of a solenoid shape, a saddle shape, and a special shape.

[0016] Specifically, the cross section of the solenoid-shaped radio frequency coil may be circular, square, or elliptical; of course, other shapes are also possible, and this application does not impose strict limitations thereto.

[0017] Optionally, the radio frequency coil is placed horizontally; or, the radio frequency coil is placed vertically; or, the radio frequency coil is placed obliquely.

[0018] Optionally, when the radio frequency coil is placed at an angle, the angle between the axis of the radio frequency coil and the vertical direction is α, and the value range of α is: 0°<α<90°.

[0019] Optionally, when the atmosphere chamber is at least partially located within the radio frequency coil;

[0020] The atmosphere chamber includes a sample cavity and a flange seal; the sample cavity is provided with at least one open end along its axial direction; the flange seal is arranged at the open end; the flange seal includes a first flange piece and a second flange piece that cooperate with each other, the first flange piece is fixed at the open end, and the second flange piece is provided with a laser transmission window mirror; the radio frequency coil is arranged on the periphery of the sample cavity.

[0021] Specifically, the axial direction of the atmosphere chamber may be consistent with the axial direction of the RF coil; or the axial direction of the atmosphere chamber may be perpendicular to the axial direction of the RF coil; or the axial direction of the atmosphere chamber may form an angle with the axial direction of the RF coil, and the angle is less than 90° and greater than 0°. The specific angle can be selected by those skilled in the art according to actual needs.

[0022] Optionally, the sample cavity is provided with an open end along its axial direction, which is the open end a; and the flange sealing end is provided at the open end a.

[0023] Optionally, the sample chamber is provided with two open ends along its axial direction, namely, an open end b1 and an open end b2; and the flange sealing end is provided at both the open end b1 and the open end b2.

[0024] Optionally, the air inlet is provided on the sample cavity; or, the air inlet is provided on the flange sealing end.

[0025] Optionally, the exhaust port is provided on the sample cavity; or, the exhaust port is provided on the flange sealing end.

[0026] Optionally, the air inlet and the air outlet are both provided on the sample cavity.

[0027] Optionally, the air inlet and the air outlet are respectively provided on flange sealing ends at both ends of the sample chamber.

[0028] Optionally, the air inlet and the exhaust port are the same opening I;

[0029] The opening I is located on the sample cavity; or,

[0030] The opening I is located on the flange sealing end.

[0031] Optionally, a hollow first pipeline is provided in the sheet layer of the first flange sheet, and / or a hollow second pipeline is provided in the sheet layer of the second flange sheet; the first pipeline and the second pipeline are used for passing coolant.

[0032] Optionally, when the radio frequency coil is located in the atmosphere chamber, an air inlet and an air outlet are provided on the wall of the atmosphere chamber;

[0033] A laser transmission window mirror is provided on the top wall and / or bottom wall of the atmosphere chamber; or a through hole is opened on the cavity wall of the atmosphere chamber, and the through hole is used to allow the optical fiber to pass into the atmosphere chamber.

[0034] Optionally, the air inlet and the air outlet are provided on the bottom wall of the atmosphere chamber.

[0035] Optionally, the radio frequency coil is wound from a hollow metal tube; the hollow structure is used for passing a coolant.

[0036] According to a second aspect of the present application, a high-temperature nuclear magnetic resonance apparatus is also provided, comprising a laser transmission assembly, a magnet, and the high-temperature nuclear magnetic resonance probe described in any one of the above items;

[0037] Room temperature holes are provided between the magnets;

[0038] The high temperature nuclear magnetic resonance probe is installed in the room temperature hole,

[0039] The laser beam generated by the laser transmission component is directed toward the sample through the laser transmission window mirror in the high-temperature nuclear magnetic resonance probe; or

[0040] The laser beam generated by the laser transmission component is directed toward the sample through an optical fiber.

[0041] Here are some possible implementations:

[0042] A high-temperature nuclear magnetic resonance probe comprises a solenoid-shaped radio frequency coil and an atmosphere chamber; the radio frequency coil is placed horizontally; the atmosphere chamber is at least partially located within the radio frequency coil; alternatively, the radio frequency coil is located within the atmosphere chamber; the atmosphere chamber is provided with an air inlet and an exhaust port for passing gas into the atmosphere chamber.

[0043] In this application, a solenoid-shaped RF transceiver coil can be used in the probe, which can enable the laser beam to be incident on the sample surface, greatly improving the RF transceiver efficiency of the RF coil, shortening the detection time of the probe, and improving the detection sensitivity.

[0044] Optionally, when the atmosphere chamber is at least partially located within the radio frequency coil;

[0045] The atmosphere chamber includes a sample cavity and a flange seal;

[0046] The sample cavity is provided with at least one open end along the horizontal direction;

[0047] The flange sealing end is arranged at the open end;

[0048] The flange end seal comprises a first flange piece and a second flange piece used in conjunction with each other, the first flange piece is fixed to the open end, and the second flange piece is provided with a laser transmission window mirror;

[0049] The radio frequency coil is arranged on the periphery of the sample cavity.

[0050] Optionally, the sample cavity is provided with an open end in the horizontal direction, which is the open end a; and the flange sealing end is provided at the open end a.

[0051] Optionally, the sample chamber is provided with two open ends along the horizontal direction, namely, an open end b1 and an open end b2; and the flange sealing end is provided at both the open end b1 and the open end b2.

[0052] Optionally, the air inlet is provided on the sample cavity; or, the air inlet is provided on the flange sealing end.

[0053] Optionally, the exhaust port is provided on the sample chamber; or, the exhaust port is provided on the flange end.

[0054] Optionally, the air inlet and the air exhaust are both provided on the sample chamber; and the air inlet and the air exhaust are respectively located on both sides of the radio frequency coil.

[0055] Optionally, the air inlet and the air outlet are respectively provided on flange sealing ends at both ends of the sample chamber.

[0056] Optionally, the air inlet and the air outlet are the same opening I; the opening I is located on the sample chamber; or, the opening I is located on the flange sealing end.

[0057] Optionally, a hollow first pipeline is provided in the sheet layer of the first flange sheet, and / or a hollow second pipeline is provided in the sheet layer of the second flange sheet; the first pipeline and the second pipeline are used for passing coolant.

[0058] Optionally, the radio frequency coil is located in the atmosphere chamber; a laser transmission window mirror is provided on the top wall of the atmosphere chamber; and an air inlet and an exhaust port are provided on the cavity wall of the atmosphere chamber.

[0059] Optionally, the air inlet and the air outlet are provided on the bottom wall of the atmosphere chamber.

[0060] Optionally, the radio frequency coil is wound from a hollow metal tube; the hollow structure is used for passing a coolant.

[0061] The present application also provides a high-temperature nuclear magnetic resonance device, comprising a laser transmission assembly, a magnet, and the high-temperature nuclear magnetic resonance probe described in any one of the above items;

[0062] Room temperature holes are provided between the magnets;

[0063] The high temperature nuclear magnetic resonance probe is installed in the room temperature hole,

[0064] The laser beam generated by the laser transmission component is directed toward the sample through a laser transmission window mirror in the high-temperature nuclear magnetic resonance probe.

[0065] The beneficial effects of this application include:

[0066] 1) In the present application, an atmosphere chamber is used to introduce gas of the desired atmosphere into the atmosphere chamber, thereby providing a static atmosphere environment or a flowing atmosphere environment, thereby achieving precise control of the pressure and flow of the gas.

[0067] 2) In the present application, the atmosphere chamber is located within the RF coil, which achieves the isolation between the space around the sample and the space around the RF coil. In this case, the required test environment atmosphere (such as oxidizing, reducing, inert, corrosive, etc.) can be freely selected, and the pressure and flow of the gas can also be precisely controlled.

[0068] 3) In the present application, by providing a hollow cooling structure in the solenoid-shaped radio frequency coil, the temperature of the radio frequency coil is reduced and the signal-to-noise ratio is improved in a high-temperature test environment.

[0069] 4) In this application, a hollow cooling pipe is provided on the flange of the flange end, which can reduce the temperature of the flange, ensure the sealing effect of the sealing ring between the flanges, and further ensure the precise control of the pressure and flow of the atmosphere in the atmosphere chamber.

[0070] 5) In this application, the RF transceiver coil is made into a solenoid shape, which improves the RF transceiver efficiency, shortens the detection time of the probe, and improves the detection sensitivity.

[0071] 6) For samples of the same material and shape, under the same sample fill factor and external environment, the solenoid-configured RF transceiver coil has the highest RF transceiver efficiency at the sample, at least three times higher than the saddle-shaped coil under the same conditions. In addition, compared with RF transceiver coils of other configurations, the solenoid coil has the highest RF field spatial uniformity at the sample. Therefore, the detection time and detection sensitivity of the static NMR probe composed of the solenoid coil are much higher than those of the static NMR probe composed of the saddle coil in the prior art.

[0072] 7) The laser-heated high-temperature NMR probe provided in this application innovates the way the laser is incident on the sample. This allows the laser beam to be incident horizontally on the sample surface after multiple reflections within the vertical external magnetic field generated by the magnet, using a horizontally open solenoid-shaped RF coil in the NMR probe. This significantly improves the RF coil's radio frequency transmission and reception efficiency, enhances detection sensitivity, and reduces detection time. BRIEF DESCRIPTION OF THE DRAWINGS

[0073] Figure 1 This is a schematic structural diagram of the high-temperature nuclear magnetic resonance probe in Example 1 of the present application;

[0074] Figure 2 This is a schematic structural diagram of the high-temperature nuclear magnetic resonance probe in Example 2 of the present application;

[0075] Figure 3 This is a schematic structural diagram of the high-temperature nuclear magnetic resonance probe in Example 3 of the present application;

[0076] Figure 4 This is a schematic structural diagram of the high-temperature nuclear magnetic resonance probe in Example 4 of the present application;

[0077] Figure 5 This is a schematic structural diagram of the high-temperature nuclear magnetic resonance probe in Example 5 of the present application;

[0078] Figure 6 This is a schematic structural diagram of the high-temperature nuclear magnetic resonance probe in Example 6 of the present application.

[0079] List of parts and reference numerals:

[0080] 100 atmosphere chamber; 101 sample chamber; 1011 air inlet;

[0081] 1012 exhaust port; 102 flange end cap; 1021 first flange;

[0082] 1022 second flange; 1023 sealing ring; 1024 laser transmission window mirror;

[0083] 103 first pipeline; 104 second pipeline;

[0084] 200 radio frequency coil; 201 hollow structure;

[0085] 300 samples. DETAILED DESCRIPTION

[0086] The present invention is described in detail below with reference to the following examples, but the present invention is not limited to these examples.

[0087] For the case where the RF coil is located within an atmosphere chamber: the atmosphere chamber 100 comprises a housing (which can be a single piece or comprised of multiple airtightly connected parts), a laser transmission window lens 1024 fixed to the housing, a resonant subsystem consisting of the sample 300 and RF coil 200, and an air interface within the atmosphere chamber. The laser transmission window and the housing are connected in a vacuum-tight manner, which can be achieved by welding, gluing, or by using a third sealing medium such as a rubber ring as a transitional connection between the two. The laser beam emitted by the laser enters the atmosphere chamber through the laser transmission window lens 1024 fixed to the housing, and ultimately impacts the sample or the crucible containing the sample, either directly or through other optical systems within the chamber. The RF coil is wound from a hollow, thin metal tube, and a cooling fluid is passed through it to cool the RF coil. Both ends of the RF coil pass through the atmosphere chamber housing, but the outer wall of the coil is vacuum-tightly connected to the housing, which can be achieved by welding, gluing, or by using a third sealing medium such as a rubber ring as a transitional connection between the two. The atmosphere chamber shell is also connected to a gas path interface, which can be a single interface or two or more interfaces. When there is a single interface, it can be connected to an external vacuum acquisition system or gas source, and the atmosphere chamber pressure can be controlled (vacuum to positive pressure), and a variety of different types of gases can be selected. When there are two interfaces, one can be connected to the vacuum acquisition system, and the other can be connected to the gas source, which can control the atmosphere chamber pressure (vacuum to positive pressure), select different types of gases, and accurately control the gas flow into the chamber. When there are multiple interfaces, one or more can be connected to the vacuum acquisition system, and the other gas paths can be connected to different types of gas sources, which can control the atmosphere chamber pressure (vacuum to positive pressure), select different types of gases, mix different types of gases, control the partial pressure of different gases, and accurately control the flow of each gas into the chamber.

[0088] For the case where the atmosphere chamber is located inside the RF coil: a gas path interface is connected to the shell of the atmosphere chamber, which can be one interface or two or more interfaces. When there is only one interface, it can be connected to an external vacuum acquisition system or gas source, and the atmosphere chamber can be pressure-controlled (from vacuum to positive pressure), and a variety of different types of gases can be selected. When there are two interfaces, one can be connected to the vacuum acquisition system, and the other can be connected to the gas source, and the atmosphere chamber can be pressure-controlled (from vacuum to positive pressure), and different types of gases can be selected, and the gas flow rate entering the chamber can be precisely controlled. When there are multiple interfaces, one or more can be connected to the vacuum acquisition system, and the other gas paths can be connected to different types of gas sources, and the atmosphere chamber can be pressure-controlled (from vacuum to positive pressure), and different types of gases can be selected, mixed, and the partial pressures of different gases can be controlled, and the flow rate of each gas entering the chamber can be precisely controlled.

[0089] About the materials of each component of the device:

[0090] The atmosphere chamber can be made of high temperature resistant non-conductive airtight materials such as ceramics (alumina, zirconia, boron nitride, etc.), quartz glass, silicate glass, etc.

[0091] The flange can be made of ceramic, quartz glass, silicate glass, or metal;

[0092] When the flange connected to the atmosphere chamber is made of the same material as the atmosphere chamber, it can be processed from a single piece of material. When it is made of different materials, it can be airtightly connected by welding, bonding, etc. The other half of the flange is vacuum-tightly connected to the flange connected to the atmosphere chamber through an O-ring or gasket.

[0093] The laser transmission window material can be selected according to the wavelength of the incident laser beam. For 1.06um carbon dioxide laser, a ZnSe window can be selected. The transmission window and the flange can be tightly connected by an O-ring or gasket, or by bonding.

[0094] Example 1

[0095] Figure 1 This is a schematic structural diagram of the high-temperature nuclear magnetic resonance probe provided in this embodiment.

[0096] Figure 1 In the embodiment, the high-temperature nuclear magnetic resonance probe includes an atmosphere chamber 100 and a radio frequency coil 200 (the radio frequency coil can be solenoid-shaped or saddle-shaped). The axial direction of the atmosphere chamber 100 is consistent with the axial direction of the radio frequency coil 200. The atmosphere chamber 100 includes a sample cavity 101. The radio frequency coil 200 is axially sleeved on the outer periphery of the sample cavity 101. The two axial ends of the sample cavity 101 are open ends, namely, the open end b1 and the open end b2. The open ends b1 and b2 are both provided with flange seals 102, namely, the first flange seal and the second flange seal.

[0097] The first flange seal includes two flanges: a first flange 1021 and a second flange 1022, with a sealing ring 1023 provided between the first flange 1021 and the second flange 1022; the first flange 1021 is fixed at the open end of the sample chamber 101, and the second flange 1022 is provided with a laser transmission window mirror 1024; the second flange seal is similar and will not be repeated here.

[0098] An air inlet 1011 is provided on one side of the sample chamber 101 close to the first flange end, and an air outlet 1012 is provided on one side of the sample chamber 101 close to the second flange end. A sample 300 is placed in the sample chamber 101 .

[0099] The laser is incident on the sample 300 in the sample chamber 101 from both sides, forming a dual light path.

[0100] The high-temperature nuclear magnetic resonance probe provided in this embodiment can provide both a static atmosphere and a flowing atmosphere.

[0101] Example 2

[0102] Figure 2 This is a schematic structural diagram of the high-temperature nuclear magnetic resonance probe provided in this embodiment.

[0103] like Figure 2 As shown, this embodiment is similar to embodiment 1, except that the air inlet 1011 is arranged on the first flange piece 1021 of the left flange sealing end 102, and the air outlet 1012 is arranged on the first flange piece 1021 of the right flange sealing end 102.

[0104] The high-temperature nuclear magnetic resonance probe provided in this embodiment can provide both a static atmosphere and a flowing atmosphere.

[0105] Example 3

[0106] Figure 3 This is a schematic structural diagram of the high-temperature nuclear magnetic resonance probe provided in this embodiment.

[0107] like Figure 3 As shown, this embodiment is similar to Example 2, except that: a hollow first pipe 103 is provided in the sheet layer of the first flange 1021, and a hollow second pipe 104 is provided in the sheet layer of the second flange 1022; the first pipe and the second pipe are used to pass the coolant, and the coolant is water.

[0108] The high-temperature nuclear magnetic resonance probe provided in this embodiment can provide both a static atmosphere and a flowing atmosphere.

[0109] Example 4

[0110] Figure 4 Schematic diagram of the structure of the high-temperature nuclear magnetic resonance probe provided in this embodiment.

[0111] like Figure 4 As shown in the embodiment, the high temperature nuclear magnetic resonance probe includes an atmosphere chamber 100 and a solenoid-shaped radio frequency coil 200. The atmosphere chamber 100 includes a sample cavity 101. The radio frequency coil 200 is horizontally sleeved on the periphery of the sample cavity 101. One end of the sample cavity 101 in the horizontal direction is an open end (such as Figure 4The sample chamber 101 is provided with a flange seal 102 (see the right end shown in FIG). The flange seal 102 comprises two flanges: a first flange 1021 and a second flange 1022, with a sealing ring 1023 positioned between the first and second flanges 1021 and 1022. The first flange 1021 is secured to the open end of the sample chamber 101, while the second flange 1022 is provided with a laser transmission window 1024. The other horizontal end of the sample chamber 101 is closed. An air inlet 1011 is provided on the side of the sample chamber 101 near the closed end, and an exhaust port 1012 is provided on the side of the flange seal 102. The sample 300 is placed within the sample chamber 101.

[0112] The laser light from the flange sealing end 102 is incident on the sample 300 in the sample chamber 101 through the window mirror 1024 , which is a single-sided light path.

[0113] The high-temperature nuclear magnetic resonance probe provided in this embodiment can provide both a static atmosphere and a flowing atmosphere.

[0114] Example 5

[0115] Figure 5 Schematic diagram of the structure of the high-temperature nuclear magnetic resonance probe provided in this embodiment.

[0116] like Figure 5 As shown in the embodiment, the high temperature nuclear magnetic resonance probe includes an atmosphere chamber 100 and a solenoid-shaped radio frequency coil 200. The atmosphere chamber 100 includes a sample cavity 101. The radio frequency coil 200 is horizontally sleeved on the periphery of the sample cavity 101. One end of the sample cavity 101 in the horizontal direction is an open end (such as Figure 5 The sample chamber 101 is sealed with a flange 102 (see the right end shown in the figure). The flange 102 comprises two flanges: a first flange 1021 and a second flange 1022, with a sealing ring 1023 positioned between them. The first flange 1021 is secured to the open end of the sample chamber 101, while the second flange 1022 is provided with a laser transmission window 1024. The other horizontal end of the sample chamber 101 is closed. A sample 300 is placed within the sample chamber 101. Laser light from the flange 102 passes through the laser window 1024 and enters the sample 300 within the sample chamber 101, creating a single-sided optical path.

[0117] The solenoid-shaped radio frequency coil 200 is wound from a hollow metal tube. The metal tube has a hollow structure 201 for passing a cooling liquid, such as water.

[0118] An opening I is provided on one side of the sample chamber 101 close to the flange sealing end 102 . The opening I serves as both an air inlet 1011 and an air outlet 1012 .

[0119] The high-temperature nuclear magnetic resonance probe of this embodiment can provide a static atmosphere environment.

[0120] Example 6

[0121] Figure 6 Schematic diagram of the structure of the high-temperature nuclear magnetic resonance probe provided in this embodiment.

[0122] like Figure 6 As shown, in this embodiment, the RF coil 200 is located in the atmosphere chamber 100, and a laser transmission window mirror 1024 is installed on the top wall of the atmosphere chamber 100 for allowing the laser to enter the sample 300. An air inlet 1011 and an exhaust port 1012 are provided on the bottom wall of the atmosphere chamber 100.

[0123] The RF coil 200 is a metal tube with a hollow structure. Both ends of the RF coil 200 pass through the bottom wall of the atmosphere chamber 100 and communicate with the cooling liquid loop pipe.

[0124] The high-temperature NMR probe is located in the room-temperature bore between the magnets.

[0125] The above descriptions are merely a few embodiments of the present application and do not constitute any form of limitation to the present application. Although the present application discloses the preferred embodiments as above, they are not intended to limit the present application. Any technical personnel familiar with the present profession, without departing from the scope of the technical solution of the present application, using the technical content disclosed above to make slight changes or modifications are equivalent to equivalent implementation cases and fall within the scope of the technical solution.

Claims

1. A high-temperature nuclear magnetic resonance probe, characterized in that: including a radio frequency coil and an atmosphere chamber; The atmosphere chamber is used to provide a static atmosphere environment or a flowing atmosphere environment; The atmosphere chamber is at least partially located within the radio frequency coil, for isolating the space surrounding the sample from the space surrounding the radio frequency coil; or, the radio frequency coil is located within the atmosphere chamber; The atmosphere chamber is provided with an air inlet and an air outlet for introducing the test environment atmosphere selected by the user into the atmosphere chamber; The atmosphere chamber includes a sample cavity and a flange seal; a laser beam is irradiated into the sample cavity to generate high temperature; The radio frequency coil is wound from a hollow metal tube; the hollow structure is used to allow cooling liquid to flow into it.

2. The high temperature nuclear magnetic resonance probe according to claim 1, characterized in that The radio frequency coil has an irregular shape.

3. The high temperature nuclear magnetic resonance probe according to claim 2, characterized in that: The shape of the radio frequency coil is selected from any one of a solenoid shape and a saddle shape.

4. The high temperature nuclear magnetic resonance probe according to claim 1, characterized in that The radio frequency coil is placed horizontally; or, The radio frequency coil is placed vertically; or, The radio frequency coil is placed obliquely.

5. The high temperature nuclear magnetic resonance probe according to claim 4, characterized in that: When the RF coil is tilted, the angle between the axis of the RF coil and the vertical direction is α. The value range of α is: 0°<α<90°.

6. The high temperature nuclear magnetic resonance probe according to claim 1, characterized in that: The atmosphere chamber is at least partially located within the radio frequency coil; The sample cavity is provided with at least one open end along its axial direction; the flange sealing end is provided at the open end; The flange end seal comprises a first flange piece and a second flange piece used in conjunction with each other, the first flange piece is fixed to the open end, and the second flange piece is provided with a laser transmission window mirror; The radio frequency coil is arranged on the periphery of the sample cavity.

7. The high temperature nuclear magnetic resonance probe according to claim 6, characterized in that: The sample cavity has an open end along its axial direction, which is the open end a; The flange sealing end is provided at the opening end a.

8. The high temperature nuclear magnetic resonance probe according to claim 6, characterized in that: The sample cavity is provided with two opening ends along its axial direction, namely, opening end b1 and opening end b2; The flange sealing ends are provided at both the opening end b1 and the opening end b2.

9. The high temperature nuclear magnetic resonance probe according to claim 6, characterized in that: The air inlet is arranged on the sample cavity; or, The air inlet is arranged on the flange sealing end.

10. The high temperature nuclear magnetic resonance probe according to claim 6, characterized in that: The exhaust port is provided on the sample cavity; or, The exhaust port is arranged on the flange sealing end.

11. The high temperature nuclear magnetic resonance probe according to claim 6, characterized in that: The air inlet and the air outlet are both arranged on the sample cavity.

12. The high temperature nuclear magnetic resonance probe according to claim 6, characterized in that: The air inlet and the air outlet are respectively arranged on the flange sealing ends at both ends of the sample cavity.

13. The high temperature nuclear magnetic resonance probe according to claim 11 or 12, characterized in that: The air inlet and the exhaust port are the same opening I; The opening I is located on the sample cavity; or, The opening I is located on the flange sealing end.

14. The high temperature nuclear magnetic resonance probe according to claim 6, characterized in that: A hollow first pipeline is provided in the sheet layer of the first flange sheet, and / or a hollow second pipeline is provided in the sheet layer of the second flange sheet; The first pipeline and the second pipeline are used for introducing cooling liquid.

15. The high temperature nuclear magnetic resonance probe according to claim 1, characterized in that: When the radio frequency coil is located in the atmosphere chamber; An air inlet and an air outlet are provided on the wall of the atmosphere chamber; The top wall and / or bottom wall of the atmosphere chamber is provided with a laser transmission window mirror; or, A through hole is provided on the cavity wall of the atmosphere chamber, and the through hole is used for allowing the optical fiber to pass into the atmosphere chamber.

16. The high temperature nuclear magnetic resonance probe according to claim 15, characterized in that: The air inlet and the air outlet are provided on the bottom wall of the atmosphere chamber.

17. A high temperature nuclear magnetic resonance device, characterized in that: A method comprising a laser transmission assembly, a magnet, and a high-temperature nuclear magnetic resonance probe according to any one of claims 1 to 16; Room temperature holes are provided between the magnets; The high temperature nuclear magnetic resonance probe is installed in the room temperature hole, The laser beam generated by the laser transmission component is directed toward the sample through the laser transmission window mirror in the high-temperature nuclear magnetic resonance probe; or The laser beam generated by the laser transmission component is directed toward the sample through an optical fiber.

Citation Information

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