CN114764078A - High-temperature nuclear magnetic resonance probe and high-temperature nuclear magnetic resonance device - Google Patents

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

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Publication number
CN114764078A
CN114764078A CN202110048411.8A CN202110048411A CN114764078A CN 114764078 A CN114764078 A CN 114764078A CN 202110048411 A CN202110048411 A CN 202110048411A CN 114764078 A CN114764078 A CN 114764078A
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flange
radio frequency
atmosphere
sample
chamber
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许巍
李傲
王军强
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Ningbo Institute of Material Technology and Engineering of CAS
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Ningbo Institute of Material Technology and Engineering of CAS
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
    • G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00—Arrangements or instruments for measuring magnetic variables
    • G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
    • G01R33/28—Details of apparatus provided for in groups G01R33/44 - G01R33/64
    • G01R33/30—Sample handling arrangements, e.g. sample cells, spinning mechanisms
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00—Arrangements or instruments for measuring magnetic variables
    • G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
    • G01R33/28—Details of apparatus provided for in groups G01R33/44 - G01R33/64
    • G01R33/30—Sample handling arrangements, e.g. sample cells, spinning mechanisms
    • G01R33/31—Temperature control thereof
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00—Arrangements or instruments for measuring magnetic variables
    • G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
    • G01R33/28—Details of apparatus provided for in groups G01R33/44 - G01R33/64
    • G01R33/32—Excitation or detection systems, e.g. using radio frequency signals
    • G01R33/34—Constructional details, e.g. resonators, specially adapted to MR
    • G01R33/34007—Manufacture of RF coils, e.g. using printed circuit board technology; additional hardware for providing mechanical support to the RF coil assembly or to part thereof, e.g. a support for moving the coil assembly relative to the remainder of the MR system
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00—Arrangements or instruments for measuring magnetic variables
    • G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
    • G01R33/28—Details of apparatus provided for in groups G01R33/44 - G01R33/64
    • G01R33/32—Excitation or detection systems, e.g. using radio frequency signals
    • G01R33/34—Constructional details, e.g. resonators, specially adapted to MR
    • G01R33/34015—Temperature-controlled RF coils
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00—Arrangements or instruments for measuring magnetic variables
    • G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
    • G01R33/28—Details of apparatus provided for in groups G01R33/44 - G01R33/64
    • G01R33/32—Excitation or detection systems, e.g. using radio frequency signals
    • G01R33/34—Constructional details, e.g. resonators, specially adapted to MR
    • G01R33/34015—Temperature-controlled RF coils
    • G01R33/3403—Means for cooling of the RF coils, e.g. a refrigerator or a cooling vessel specially adapted for housing an RF coil

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Thermal Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
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  • Magnetic Resonance Imaging Apparatus (AREA)

Abstract

The application discloses a high-temperature nuclear magnetic resonance probe and a device. The 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; or, the radio frequency coil is located in the atmosphere chamber; the atmosphere chamber is provided with an air inlet and an air outlet and is used for introducing air into the atmosphere chamber. The probe comprises a radio frequency coil and an atmosphere chamber, different atmosphere environments can be provided in a high-temperature environment by using the atmosphere chamber, and the pressure and the flow of the atmosphere can be accurately regulated and controlled.

Description

High-temperature nuclear magnetic resonance probe and high-temperature nuclear magnetic resonance device
Technical Field
The application relates to a high-temperature nuclear magnetic resonance probe and a high-temperature nuclear magnetic resonance device, and belongs to the technical field of nuclear magnetic resonance devices.
Background
Nuclear Magnetic Resonance (NMR) technology is an important research tool for probing the microstructure and dynamics of various materials. The NMR platform comprises three main components, namely a superconducting magnet, a control cabinet and a probe. The superconducting magnet provides a high-uniformity high-stability magnetic field in the vertical direction, and the control cabinet integrates functional components such as radio frequency transmitting and receiving, radio frequency power amplification and the like; the NMR probe integrates important instruments of a radio frequency receiving and transmitting coil, a tuning and impedance matching circuit and a sample chamber and is arranged in a high-uniformity magnetic field space generated by a superconducting magnet. In the high-temperature NMR probe, the most core part is a harmonic oscillator composed of a sample and a radio frequency coil, and the harmonic oscillator and other circuit devices in the probe form a radio frequency resonance circuit, so that the functions of transmitting and receiving radio frequency signals are finally realized.
In recent years, the research on the structures and dynamics of various materials under different atmospheres in a high temperature environment (e.g., oxidation and reduction processes of a metal material, a high temperature heat treatment process of a material, a corrosion process at a high temperature, etc.) has been required, and these demands have led to the development of NMR probes capable of providing both a high temperature environment and different atmosphere environments for a sample to be measured. At present, the existing high-temperature NMR probes mainly comprise two types, wherein the first type adopts a resistance heating device to heat a sample through the heat conduction of a gas medium, but the sample and a radio frequency coil are simultaneously positioned in a high-temperature environment, and the radio frequency coil is made of a metal material, so that the radio frequency coil cannot be suitable for high-temperature oxidizing and corrosive atmosphere, and the slow oxidation phenomenon can also occur in a high-temperature inert gas environment; the second high-temperature NMR probe adopts a laser heating mode, and is characterized in that a sample is directly irradiated or a crucible for containing the sample is used for heating the sample, the temperature of a radio frequency coil is reduced by isolating the sample from the heat conduction of the radio frequency coil or (and) actively cooling the radio frequency coil, but the current laser heating NMR probe cannot provide different atmosphere (oxidation, reduction, inertia, corrosiveness and the like) environments while providing a high-temperature environment, and cannot accurately regulate and control the pressure and the flow of the atmosphere according to actual needs.
Disclosure of Invention
According to one aspect of the application, a high-temperature nuclear magnetic resonance probe is provided, wherein the probe comprises a solenoid-shaped radio frequency coil and an atmosphere chamber, different atmosphere environments can be provided in the high-temperature environment by using the atmosphere chamber, and the pressure and the flow of the atmosphere can be accurately regulated and controlled.
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; or, the radio frequency coil is located in the atmosphere chamber; the atmosphere chamber is provided with an air inlet and an air outlet and is used for introducing air into the atmosphere chamber.
Specifically, an inlet and an outlet for respectively passing gas into or out of the atmosphere chamber.
The problems still exist in the current laser heating type high-temperature NMR probe: in the prior art, laser directly irradiates a sample or a crucible for holding the sample to further heat the sample, in order to improve the signal-to-noise ratio, the temperature of a radio frequency coil needs to be reduced, generally, a heat insulation material is adopted to isolate heat conduction between the sample and the radio frequency coil, meanwhile, air is blown to the outside of the radio frequency coil, so that the heat of the radio frequency coil is taken away by flowing low-temperature gas medium, the low-temperature gas medium for cooling is inert or reducing gas, and oxidizing or corrosive gas cannot be used; since the space around the sample communicates with the space around the radio frequency coil, in this case, it is impossible to freely select the kind of gas in the space around the sample, and it is impossible to use an oxidizing or corrosive gas, and it is also difficult to precisely control the pressure and flow rate of the gas.
In this application, utilize the atmosphere cavity, let in the atmosphere cavity with the gas of required atmosphere, can provide the atmosphere environment or the flowing atmosphere environment of stewing, realize carrying out the accurate control to the pressure and the flow of gas.
In the application, the atmosphere chamber is at least partially located in the radio frequency coil, so that the separation of the space around the sample and the space around the radio frequency coil is realized, in this case, the required test environment atmosphere (such as oxidation, reduction, inertia, corrosiveness and the like) can be freely selected, and meanwhile, the pressure and the flow of gas can be precisely controlled.
Specifically, the gas introduced into the atmosphere chamber in the present application includes one or more of oxygen, hydrogen, and inert gas. The present application is not limited strictly, and those skilled in the art can select a suitable atmosphere according to actual needs.
In the present application, the number of the air inlets may be one, two, or more.
When the air inlet is arranged on one path, the air inlet can be connected with an external vacuum obtaining system or an air source, the pressure of the atmosphere cavity can be controlled (from vacuum to positive pressure), and various gases of different types can be selected.
During two way air inlets, can connect the vacuum acquisition system all the way, the air supply can be connected to another way, can carry out pressure control (vacuum to malleation) to the atmosphere cavity, can select different kinds of gas to can carry out accurate control to the gas flow who lets in the cavity.
During the multichannel air inlet, one way or multichannel can connect the vacuum and obtain the system, and different kinds of air supplies can be connected to other gas circuits, can carry out pressure control (vacuum to malleation) to the atmosphere cavity, can select different kinds of gas, mixes different kinds of gas, controls the partial pressure of different gases to can carry out accurate control to every kind of gas flow that lets in the cavity.
Optionally, the shape of the radio frequency coil is selected from any one of a solenoid shape, a saddle shape, and a profile shape.
In particular, the solenoid-shaped radio frequency coil may be circular, square, or elliptical in cross-section; other shapes are of course possible and are not strictly limited in this application.
Optionally, the radio frequency coil is horizontally disposed; or, the radio frequency coil is vertically placed; alternatively, the radio frequency coil is placed obliquely.
Optionally, when the radio frequency coil is placed in an inclined manner, an included angle between the axis of the radio frequency coil and the vertical direction is α, and a value range of α is as follows: alpha is more than 0 degree and less than 90 degrees.
Optionally, the atmospheric chamber is at least partially located within the radio frequency coil;
the atmosphere chamber comprises a sample cavity and a flange end; the sample cavity is provided with at least one opening end along the axial direction of the sample cavity; the flange end closure is arranged at the opening end; the flange end closure comprises a first flange piece and a second flange piece which are matched with each other, the first flange piece is fixed at the opening end, and the second flange piece is provided with a laser transmission window mirror; the radio frequency coil is sleeved on the periphery of the sample cavity.
Specifically, the axial direction of the atmosphere chamber may coincide with the axial direction of the radio frequency coil; or the axial direction of the atmosphere chamber is vertical to the axial direction of the radio frequency coil; or the axial direction of the atmosphere chamber and the axial direction of the radio frequency coil are perpendicular to each other at an angle smaller than 90 degrees and larger than 0 degree, and the specific angle can be selected by a person skilled in the art according to actual needs.
Optionally, the sample cavity is provided with an open end along the axial direction thereof, which is an open end a; the flange end closure is arranged at the opening end a.
Optionally, the sample cavity is provided with two open ends along the axial direction thereof, namely an open end b1 and an open end b 2; the flange end closures are arranged at the opening end b1 and the opening end b 2.
Optionally, the gas inlet is disposed on the sample chamber; alternatively, the air inlet is provided on the flange seal end.
Optionally, the vent is disposed on the sample chamber; alternatively, the vent is disposed on the flange seal end.
Optionally, the gas inlet and gas outlet are both provided on the sample chamber.
Optionally, the gas inlet and the gas outlet are respectively arranged on the flange sealing ends at two ends of the sample cavity.
Optionally, the air inlet and the air outlet are the same opening I;
the opening I is positioned on the sample cavity; or,
the opening I is located on the sealing end of the flange.
Optionally, a hollow first pipeline is arranged in the sheet layer of the first flange sheet, and/or a hollow second pipeline is arranged in the sheet layer of the second flange sheet; the first pipeline and the second pipeline are used for introducing cooling liquid.
Optionally, the radio frequency coil is positioned within the atmospheric chamber; an air inlet and an air outlet are arranged on the cavity wall of the atmosphere cavity;
the top wall and/or the bottom wall of the atmosphere chamber are/is provided with a laser transmission window mirror; or, a through hole is formed in the wall of the atmosphere chamber, and the through hole is used for enabling the optical fiber to penetrate into the atmosphere chamber.
Optionally, the bottom wall of the atmosphere chamber is provided with the gas inlet and the gas outlet.
Optionally, the radio frequency coil is formed by winding a hollow metal tube; the hollow structure is used for introducing cooling liquid.
According to the second aspect of the application, a high-temperature nuclear magnetic resonance device is further provided, and comprises a laser transmission assembly, a magnet and the high-temperature nuclear magnetic resonance probe;
a room temperature hole is arranged between the magnets;
the high-temperature nuclear magnetic resonance probe is arranged in the room-temperature hole,
the laser beam generated by the laser transmission assembly is reflected to 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 assembly is emitted to the sample through the optical fiber.
Possible implementations are described below:
a high-temperature nuclear magnetic resonance probe comprises a solenoid-shaped radio frequency coil and an atmosphere chamber; the radio frequency coil is horizontally arranged; the atmosphere chamber is at least partially located within the radio frequency coil; or, the radio frequency coil is located in the atmosphere chamber; the atmosphere cavity is provided with an air inlet and an air outlet and is used for introducing gas into the atmosphere cavity.
In the application, the radio frequency transceiving coil in the solenoid configuration can be adopted in the probe, so that laser beams can be incident to the surface of a sample, the radio frequency transceiving efficiency of the radio frequency coil is greatly improved, the detection time of the probe is shortened, and the detection sensitivity is improved.
Optionally, the atmospheric chamber is at least partially located within the radio frequency coil;
the atmosphere chamber comprises a sample cavity and a flange end;
the sample cavity is provided with at least one opening end along the horizontal direction;
the flange end closure is arranged at the opening end;
the flange end closure comprises a first flange piece and a second flange piece which are matched with each other, the first flange piece is fixed at the opening end, and the second flange piece is provided with a laser transmission window mirror;
the radio frequency coil is sleeved on the periphery of the sample cavity.
Optionally, the sample cavity is provided with an open end in the horizontal direction, which is an open end a; the flange end closure is arranged at the opening end a.
Optionally, the sample cavity is provided with two open ends along the horizontal direction, namely an open end b1 and an open end b 2; the flange end closures are arranged at the opening end b1 and the opening end b 2.
Optionally, the gas inlet is disposed on the sample chamber; alternatively, the air inlet is provided on the flange seal end.
Optionally, the vent is disposed on the sample chamber; alternatively, the exhaust port is provided on the flange seal end
Optionally, the gas inlet and the gas outlet are both disposed on the sample chamber; and the air inlet and the air outlet are respectively positioned at two sides of the radio frequency coil.
Optionally, the gas inlet and the gas outlet are respectively arranged on the flange sealing ends at two ends of the sample cavity.
Optionally, the air inlet and the air outlet are the same opening I; the opening I is positioned on the sample cavity; or the opening I is positioned on the sealing end of the flange.
Optionally, a hollow first pipeline is arranged in the sheet layer of the first flange sheet, and/or a hollow second pipeline is arranged in the sheet layer of the second flange sheet; the first pipeline and the second pipeline are used for introducing cooling liquid.
Optionally, the radio frequency coil is located within the atmospheric chamber; the top wall of the atmosphere chamber is provided with a laser transmission window mirror; and the wall of the atmosphere cavity is provided with an air inlet and an air outlet.
Optionally, the bottom wall of the atmosphere chamber is provided with the air inlet and the air outlet.
Optionally, the radio frequency coil is formed by winding a hollow metal tube; the hollow structure is used for introducing cooling liquid.
The application also provides a high-temperature nuclear magnetic resonance device, which comprises a laser transmission assembly, a magnet and any one of the high-temperature nuclear magnetic resonance probes;
a room temperature hole is arranged between the magnets;
the high-temperature nuclear magnetic resonance probe is arranged in the room-temperature hole,
and the laser beam generated by the laser transmission assembly is reflected to the sample through the laser transmission window mirror in the high-temperature nuclear magnetic resonance probe.
The beneficial effect that this application can produce includes:
1) in this application, utilize the atmosphere cavity, let in the atmosphere cavity with the gas of required atmosphere, can provide the atmosphere environment or the flowing atmosphere environment of stewing, realize carrying out the accurate control to the pressure and the flow of gas.
2) In this application, the atmosphere chamber is located in the radio frequency coil, has realized the separation of sample surrounding space and radio frequency coil surrounding space, under this condition, can freely select required test environment atmosphere (for example oxidation, reduction, inertia, corrosivity etc.) simultaneously can also realize carrying out fine control to the pressure and the flow of gas.
3) In this application, through set up hollow cooling structure in solenoid's radio frequency coil, under high temperature test environment, reduced radio frequency coil's temperature, improved the SNR.
4) In this application, be equipped with hollow cooling pipeline on the flange piece of flange end sealing, can reduce the temperature of flange piece, guaranteed the sealed effect of the sealing washer between the flange piece, and then guaranteed the accurate control of pressure, the flow of atmosphere in the atmosphere cavity.
5) In the application, the radio frequency transceiving coil is made into a solenoid shape, so that the radio frequency transceiving efficiency is improved, the detection time of the probe is shortened, and the detection sensitivity is improved.
6) For samples of the same material and the same shape, under the conditions of the same sample filling factor and the same external environment, the radio frequency transceiving coil of the solenoid configuration has the highest radio frequency transceiving efficiency at the sample position, and is at least 3 times higher than that of a saddle-shaped ring under the same condition; in addition, compared with other configurations of radio frequency transceiver coils, the solenoid coil has the highest spatial uniformity of the radio frequency field at the sample, so the detection time and the detection sensitivity of the static NMR probe composed of the solenoid type coil are far higher than those of the static NMR probe composed of the saddle type coil in the prior art.
7) The application provides a laser heating high temperature nuclear magnetic resonance probe has carried out the innovation to the mode that laser incided to the sample to make in the vertical direction external magnetic field that the magnet produced, adopt the radio frequency coil of horizontal direction open-ended solenoid configuration in nuclear magnetic probe, can make the laser beam pass through final level incidence to the sample surface behind the multistage reflection. The radio frequency receiving and transmitting efficiency of the radio frequency coil is greatly improved, the detection sensitivity is improved, and the detection time is shortened.
Drawings
FIG. 1 is a schematic structural view of a high temperature NMR probe in example 1 of the present application;
FIG. 2 is a schematic structural view of a high temperature NMR probe in example 2 of the present application;
FIG. 3 is a schematic structural view of a high temperature NMR probe in example 3 of the present application;
FIG. 4 is a schematic structural view of a high temperature NMR probe in example 4 of the present application;
FIG. 5 is a schematic view of the structure of a high temperature NMR probe in example 5 of the present application;
fig. 6 is a schematic structural view of a high-temperature nmr probe in example 6 of the present application.
List of components and reference numbers:
100 atmosphere chamber; 101 a sample chamber; 1011 air inlet;
1012 exhaust port; 102, flange end sealing; 1021 a first flange segment;
1022 a second flange sheet; 1023 sealing rings; 1024 laser transmission window mirror;
103 a first conduit; 104 a second pipeline;
200 radio frequency coils; 201 a hollow structure;
300 samples.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples. Some possible embodiments are presented below.
For the case when the radio frequency coil is located within the atmospheric chamber: the atmosphere chamber 100 is composed of a housing (which may be a whole or may be composed of a plurality of hermetically connected parts), a laser transmission window lens 1024 fixed on the housing, a resonance subsystem composed of the sample 300 and the rf coil 200, and an air path interface of the atmosphere chamber. The laser transmission window and the shell are connected in a vacuum airtight mode, and can be connected in a welding or bonding mode, or the laser transmission window and the shell are connected in a transition mode through a third sealing medium such as a rubber ring. Laser beams emitted by the laser are incident into the atmosphere chamber through a laser transmission window mirror 1024 fixed on the shell, and are directly incident or finally incident to the sample or the surface of the crucible for containing the sample through other optical systems in the chamber. The radio frequency coil is formed by winding a hollow thin metal tube, and cooling fluid is introduced to refrigerate the radio frequency coil. The two ends of the radio frequency coil penetrate through the atmosphere chamber shell, but the outer wall of the coil is connected with the atmosphere chamber shell in a vacuum airtight mode, and the radio frequency coil and the atmosphere chamber shell can be in a welding or bonding mode, or the radio frequency coil and the atmosphere chamber shell are in transition connection through a third sealing medium such as a rubber ring. The atmosphere cavity shell is also connected with a gas circuit interface which can be one interface or two-way or multi-way interfaces. When the interface all the way, can connect outside vacuum acquisition system or air supply, can carry out pressure control (vacuum to malleation) to the atmosphere cavity, can select different kinds of multiple gas. During two way interfaces, can connect the vacuum acquisition system all the way, the air supply can be connected in another way, can carry out pressure control (vacuum to malleation) to the atmosphere cavity, can select different kinds of gas to can carry out accurate control to the gas flow who lets in the cavity. During the multichannel interface, one way or multichannel can connect the vacuum and obtain the system, and different kinds of air supplies can be connected to other gas circuits, can carry out pressure control (vacuum to malleation) to the atmosphere cavity, can select different kinds of gas, mixes different kinds of gas, controls the partial pressure of different gases to can carry out accurate control to every kind of gas flow that lets in the cavity.
For the case when the atmospheric chamber is located within the radio frequency coil: the atmosphere cavity shell is connected with a gas circuit interface which can be one interface or two-way or multi-way interfaces. When the interface all the way, can connect outside vacuum and obtain system or air supply, can carry out pressure control (vacuum to malleation) to the atmosphere cavity, can select the multiple gas of different kinds. During two way interfaces, can connect the vacuum acquisition system all the way, the air supply can be connected in another way, can carry out pressure control (vacuum to malleation) to the atmosphere cavity, can select different kinds of gas to can carry out accurate control to the gas flow who lets in the cavity. During the multichannel interface, one way or multichannel can connect the vacuum and obtain the system, and different types of air supplies can be connected to other gas circuits, can carry out pressure control (vacuum to malleation) to the atmosphere cavity, can select different types of gas, mixes different types of gas, controls the partial pressure of different gases to can carry out accurate control to every kind of gas flow who lets in the cavity.
Regarding the materials of the components of the device:
the atmosphere chamber can be made of high-temperature-resistant non-conductive airtight materials such as ceramics (alumina, zirconia, boron nitride and the like), quartz glass, silicate glass and the like;
the flange may be ceramic, quartz glass, silicate glass, or a metallic material;
when the flange connected with the atmosphere cavity and the atmosphere cavity are made of the same material, the flange can be processed by adopting a single material, and when the flange is made of a different material, the flange and the atmosphere cavity can be connected in an airtight manner by welding, bonding and the like; the other half of the flange is tightly connected with the flange of the connecting atmosphere chamber in a vacuum mode through an O ring or a gasket.
The material of the laser transmission window mirror can be selected according to the wavelength of an incident laser beam, a ZnSe window can be selected for 1.06um carbon dioxide laser, and the transmission window and the flange can be tightly connected through an O ring or a gasket or in a bonding mode.
Example 1
Fig. 1 is a schematic structural diagram of the high-temperature nmr probe provided in this embodiment.
In fig. 1, the high-temperature nmr probe includes an atmosphere chamber 100 and a radio frequency coil 200 (the radio frequency coil may be in a solenoid shape or a saddle shape), and the axial direction of the atmosphere chamber 100 is coincident with the axial direction of the radio frequency coil 200; the atmosphere chamber 100 comprises a sample chamber body 101, the radio frequency coil 200 is sleeved on the periphery of the sample chamber body 101 along the axial direction, two axial ends of the sample chamber body 101 are open ends, namely an open end b1 and an open end b2, and flange end caps 102 are arranged on the open end b1 and the open end b2, namely a first flange end cap and a second flange end cap.
The first flange termination includes two flange pieces: a sealing ring 1023 is arranged between the first flange piece 1021 and the second flange piece 1022; the first flange piece 1021 is fixed at the opening end of the sample cavity 101, and the second flange piece 1022 is provided with a laser transmission window mirror 1024; the second flange terminates similarly and will not be described further herein.
An air inlet 1011 is formed in one side, close to the first flange end seal, of the sample cavity 101; a vent 1012 is provided in the sample chamber 101 near the end of the second flange. A sample 300 is placed in the sample chamber 101.
The laser beam is incident on the sample 300 in the sample chamber 101 from both sides, and is a dual light path.
The high-temperature nuclear magnetic resonance probe provided by the embodiment can provide a static atmosphere environment and can also provide a flowing atmosphere environment.
Example 2
Fig. 2 is a schematic structural diagram of the high-temperature nmr probe provided in this embodiment.
As shown in fig. 2, in the present embodiment, similarly to embodiment 1, the difference is that: the air inlet 1011 is arranged on the first flange part 1021 of the left flange termination 102 and the air outlet 1012 is arranged on the first flange part 1021 of the right flange termination 102.
The high-temperature nuclear magnetic resonance probe provided by the embodiment can provide a static atmosphere environment and can also provide a flowing atmosphere environment.
Example 3
Fig. 3 is a schematic structural diagram of the high-temperature nmr probe provided in this embodiment.
As shown in fig. 3, in the present embodiment, similarly to embodiment 2, the difference is that: a hollow first pipeline 103 is arranged in the sheet layer of the first flange piece 1021, and a hollow second pipeline 104 is arranged in the sheet layer of the second flange piece 1022; the first pipeline and the second pipeline are used for introducing cooling liquid, and the cooling liquid is water.
The high-temperature nuclear magnetic resonance probe provided by the embodiment can provide a static atmosphere environment and can also provide a flowing atmosphere environment.
Example 4
Fig. 4 is a schematic structural diagram of the high-temperature nmr probe provided in this embodiment.
As shown in fig. 4, in this embodiment, the high-temperature nmr probe includes an atmosphere chamber 100 and a solenoid-shaped rf coil 200, the atmosphere chamber 100 includes a sample cavity 101, the rf coil 200 is sleeved on the periphery of the sample cavity 101 along the horizontal direction, one end of the sample cavity 101 along the horizontal direction is an open end (e.g., the right end shown in fig. 4), and a flange end 102 is provided, where the flange end 102 includes two flange pieces: a sealing ring 1023 is arranged between the first flange piece 1021 and the second flange piece 1022; the first flange plate 1021 is fixed at the open end of the sample chamber 101, and the second flange plate 1022 is provided with a laser transmission window mirror 1024. The other end of the sample chamber 101 in the horizontal direction is of a closed design. An air inlet 1011 is formed in one side, close to the closed end, of the sample cavity 101; a vent 1012 is provided near the side of the flange termination 102. A sample 300 is placed in the sample chamber 101.
The laser light is incident on the sample 300 in the sample chamber 101 from the laser of the flange 102 through the window mirror 1024 as a single-sided light path.
The high-temperature nuclear magnetic resonance probe provided by the embodiment can provide a static atmosphere environment and can also provide a flowing atmosphere environment.
Example 5
Fig. 5 is a schematic structural diagram of the high-temperature nmr probe provided in this embodiment.
As shown in fig. 5, in this embodiment, the high-temperature nmr probe includes an atmosphere chamber 100 and a solenoid-shaped rf coil 200, the atmosphere chamber 100 includes a sample cavity 101, the rf 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 (e.g., the right end shown in fig. 5), and is provided with a flange terminating end 102, and the flange terminating end 102 includes two flange pieces: a sealing ring 1023 is arranged between the first flange piece 1021 and the second flange piece 1022; the first flange plate 1021 is fixed at the open end of the sample chamber 101, and the second flange plate 1022 is provided with a laser transmission window mirror 1024. The other end of the sample chamber 101 in the horizontal direction is of a closed design. A sample 300 is placed in the sample chamber 101. The laser light is incident on the sample 300 in the sample chamber 101 from the laser of the flange 102 through the window mirror 1024 as a single-sided light path.
The solenoid-shaped rf coil 200 is formed by winding a hollow metal tube having a hollow structure 201 for passing a cooling fluid, such as water.
The side of the sample chamber 101 near the flange end 102 is provided with an opening i, which is both an air inlet 1011 and an air outlet 1012.
The high-temperature nuclear magnetic resonance probe of the present embodiment can provide a static atmosphere.
Example 6
Fig. 6 is a schematic structural diagram of the high-temperature nmr probe provided in this embodiment.
As shown in fig. 6, in the present embodiment, the rf coil 200 is located in the atmosphere chamber 100, a laser transmission window mirror 1024 is installed on the top wall of the atmosphere chamber 100 for absorbing laser light onto the sample 300, and an air inlet 1011 and an air outlet 1012 are installed on the bottom wall of the atmosphere chamber 100.
The rf coil 200 is a metal tube with a hollow structure, and both ends of the rf coil 200 penetrate through the bottom wall of the atmosphere chamber 100 to communicate with the coolant loop pipe.
The high temperature nuclear magnetic resonance probe is located in the room temperature hole between the magnets.
Although the present invention has been described with reference to a few preferred embodiments, it should be understood that various changes and modifications can be made without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (9)

1. A high-temperature nuclear magnetic resonance probe is characterized by comprising a radio frequency coil and an atmosphere chamber;
the atmospheric chamber is at least partially located within the radio frequency coil; or, the radio frequency coil is located in the atmosphere chamber;
the atmosphere chamber is provided with an air inlet and an air outlet and is used for introducing air into the atmosphere chamber.
2. A high temperature nmr probe according to claim 1, wherein the shape of the rf coil is selected from any of a solenoid shape, a saddle shape, and a profile shape.
3. The high temperature nuclear magnetic resonance probe according to claim 1, wherein the radio frequency coil is horizontally disposed; or,
the radio frequency coil is vertically arranged; or,
the radio frequency coil is placed obliquely.
4. A high temperature NMR probe according to claim 3, wherein the RF coil is tilted such that the axis of the RF coil forms an angle α with the vertical,
the value range of alpha is as follows: alpha is more than 0 degree and less than 90 degrees.
5. The high temperature nmr probe of claim 1, wherein the atmospheric chamber is at least partially within the rf coil;
the atmosphere chamber comprises a sample cavity and a flange end;
the sample cavity is provided with at least one opening end along the axial direction of the sample cavity; the flange end closure is arranged at the opening end;
the flange end closure comprises a first flange piece and a second flange piece which are matched with each other, the first flange piece is fixed at the opening end, and the second flange piece is provided with a laser transmission window mirror;
the radio frequency coil is sleeved on the periphery of the sample cavity;
preferably, the sample cavity is provided with an open end along the axial direction, namely an open end a;
the flange end closure is arranged at the opening end a;
preferably, the sample chamber is provided with two open ends along the axial direction thereof, namely an open end b1 and an open end b 2;
the flange end closures are arranged at the opening end b1 and the opening end b 2;
preferably, the gas inlet is provided on the sample chamber; or,
the air inlet is arranged on the flange sealing end;
preferably, the vent is provided on the sample chamber; or,
the exhaust port is arranged on the flange sealing end;
preferably, the gas inlet and the gas outlet are both arranged on the sample chamber;
preferably, the gas inlet and the gas outlet are respectively arranged on the flange sealing ends at two ends of the sample cavity;
preferably, the air inlet and the air outlet are the same opening I;
the opening I is positioned on the sample cavity; or,
the opening I is positioned on the sealing end of the flange;
preferably, a hollow first pipeline is arranged in the sheet layer of the first flange sheet, and/or a hollow second pipeline is arranged in the sheet layer of the second flange sheet;
the first pipeline and the second pipeline are used for introducing cooling liquid.
6. The high temperature nmr probe of claim 1, wherein the rf coil is positioned within the atmospheric chamber;
an air inlet and an air outlet are arranged on the cavity wall of the atmosphere cavity;
the top wall and/or the bottom wall of the atmosphere chamber are/is provided with a laser transmission window mirror; or,
and a through hole is formed in the wall of the atmosphere cavity and is used for enabling the optical fiber to penetrate into the atmosphere cavity.
7. A high temperature NMR probe according to claim 6, wherein the gas inlet and outlet are provided in the bottom wall of the atmosphere chamber.
8. The high-temperature nuclear magnetic resonance probe according to claim 1, wherein the radio frequency coil is formed by winding a hollow metal tube;
the hollow structure is used for introducing cooling liquid.
9. A high temperature nmr apparatus comprising a laser transmission assembly, a magnet, and the high temperature nmr probe of any of claims 1-8;
a room temperature hole is arranged between the magnets;
the high-temperature nuclear magnetic resonance probe is arranged in the room-temperature hole,
the laser beam generated by the laser transmission assembly is reflected to 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 assembly is emitted to the sample through the optical fiber.
CN202110048411.8A 2021-01-14 2021-01-14 High-temperature nuclear magnetic resonance probe and high-temperature nuclear magnetic resonance device Pending CN114764078A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110048411.8A CN114764078A (en) 2021-01-14 2021-01-14 High-temperature nuclear magnetic resonance probe and high-temperature nuclear magnetic resonance device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110048411.8A CN114764078A (en) 2021-01-14 2021-01-14 High-temperature nuclear magnetic resonance probe and high-temperature nuclear magnetic resonance device

Publications (1)

Publication Number Publication Date
CN114764078A true CN114764078A (en) 2022-07-19

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Family Applications (1)

Application Number Title Priority Date Filing Date
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Country Status (1)

Country Link
CN (1) CN114764078A (en)

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