CN113687283B - Device and method for quantitatively detecting material very weak magnetism - Google Patents

Device and method for quantitatively detecting material very weak magnetism Download PDF

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Publication number
CN113687283B
CN113687283B CN202110960548.0A CN202110960548A CN113687283B CN 113687283 B CN113687283 B CN 113687283B CN 202110960548 A CN202110960548 A CN 202110960548A CN 113687283 B CN113687283 B CN 113687283B
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sample
magnetic
magnetic field
support
detected
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CN113687283A (en
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王晓飞
***
姜永亮
武春风
胡金萌
吕亮
庹文波
成红
蓝学楷
张璐
任杰
王耀东
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Wuhan Optical Valley Aerospace Sanjiang Laser Industry Technology Research Institute Co Ltd
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Wuhan Optical Valley Aerospace Sanjiang Laser Industry Technology Research Institute Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01RMEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00Arrangements or instruments for measuring magnetic variables
    • G01R33/12Measuring magnetic properties of articles or specimens of solids or fluids
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01RMEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00Arrangements or instruments for measuring magnetic variables
    • G01R33/02Measuring direction or magnitude of magnetic fields or magnetic flux
    • G01R33/032Measuring direction or magnitude of magnetic fields or magnetic flux using magneto-optic devices, e.g. Faraday or Cotton-Mouton effect

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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Measuring Magnetic Variables (AREA)

Abstract

The invention belongs to the technical field of weak magnetic field measurement, and particularly discloses a device and a method for quantitatively detecting the very weak magnetic property of a material. The device comprises an internal magnetic shielding, an external magnetic shielding, a non-magnetic sample introduction guide pipe, a sample rotating carrier, a pneumatic turbofan, a rotating support module, a magnetic field calibration coil and a vector atom magnetometer, wherein the magnetic field is detected in the magnetic shielding of a magnetic silence space, and the magnetic field is measured by matching with the rotating sample introduction device. The method comprises the steps that a sample to be detected is sent into a magnetic silence detection space after being silence for a certain time, so that the sample to be detected generates magnetic field disturbance in the magnetic sensitivity direction of a vector atom magnetometer, the vector atom magnetometer detects and collects magnetic signals of the detection space, and the material very weak magnetic quantitative detection of the sample to be detected is realized according to the magnetic signals of the sample to be detected and the calibrated magnetic field. The invention can be effectively applied to quantitative detection of extremely weak magnetism of materials, can realize extremely weak magnetism measurement of fT magnitude, and has wide application field and strong applicability.

Description

Device and method for quantitatively detecting material very weak magnetism
Technical Field
The invention belongs to the technical field of weak magnetic field measurement, and particularly relates to a device and a method for quantitatively detecting the very weak magnetic property of a material.
Background
With the development of atomic sensor technology, the sensors such as atomic clocks, atomic magnetometers, nuclear magnetic resonance gyroscopes and the like are developed towards the directions of small volume, low power consumption, light weight, high precision and the like, so that the manufactured more excellent tiny components are important to the performance influence of the atomic sensors, the influence of devices can be effectively eliminated by the quantitative detection of the extremely weak magnetism of the materials, and the influence of necessary devices on the high-precision sensors is evaluated. The performance of the geological rock material is rapidly tested through the quantitative detection of the very weak magnetism of the material, and geomagnetic evolution characteristics are researched through the quantitative measurement of a magnetic field generated by geological rock. The magnetic quantitative measurement of the material can also be used for developing a high-field magnetic resonance spectrometer, and can be used for discriminating the material, so that the influence of the magnetic material on a high-precision performance instrument is avoided.
Currently, there are various methods for detecting magnetism of materials such as magnetometers with different principles, and for extremely weak magnetic field measurement, fluxgate magnetometers, superconducting quantum interference (SQUID) magnetometers, atomic magnetometers and the like are mainly used for measurement. The magnetic detection of materials such as ancient rocks can detect the remanence of the materials through a fluxgate magnetometer and the like, and the sensitivity is relatively high, but the magnetism lower than nT cannot be detected, so that the method is not suitable for the extremely weak magnetic detection of the materials. SQUIDs are expensive to manufacture and not portable, limiting their range of use.
In the Chinese patent No. 106405457B, a device and a method for detecting the ferromagnetism and the magnetization property of a material are disclosed, the detection of the ferromagnetism and the magnetization property of the material is obtained through nonlinear magneto-optical resonance dispersion signals, the device and the method have the characteristic of ultra-high sensitivity magnetic measurement and practical value, but the device and the method do not realize the quantitative detection of the magnetism of the material. Currently, atomic magnetometers are comparable in sensitivity to SQUIDs, can detect the magnetic field of fT, and can be miniaturized. The miniaturized atomic magnetometer can quantitatively measure the magnetic field generated by the components required by the miniaturization and the chip-level atomic frequency standard, atomic magnetometer, nuclear magnetic resonance gyroscope and other sensors, and the nonmagnetic components are selected so as to eliminate the magnetic field non-uniformity in the sensor caused by the magnetism generated by the components. It is important to detect the magnetic properties of the material more simply, rapidly and accurately, and quantitatively measure the magnetic field, for example, quantitatively measure the magnetic field generated by materials such as geological rock, and the like, so that the magnetic properties of the material can be conveniently researched. Therefore, there is an urgent need to develop a new method and new technology for quantitative detection of very weak magnetism of materials.
Disclosure of Invention
Aiming at the defects or improvement demands of the prior art, the invention provides a device and a method for quantitatively detecting the extremely weak magnetism of a material, wherein the characteristics of the magnetic material and the magnetic performance detection process characteristics of the magnetic material are combined, a vector atomic magnetometer is used as an ultra-high sensitive magnetic field probe, and magnetic field measurement is carried out in a magnetic shielding space by detecting and matching with a rotary sample injection device, so that the device can be effectively applied to quantitatively detecting the extremely weak magnetism of the material, can realize the extremely weak magnetism measurement of fT magnitude, can be applied to quantitatively measuring the magnetic field generated by components required by miniaturized chip-scale atomic clocks, atomic magnetometers, nuclear magnetic resonance gyroscopes and other sensors, and can select non-magnetic components so as to eliminate the non-uniformity of the magnetic field in the sensor caused by the magnetism generated by the components, and can also be applied to quantitatively measuring the magnetic field generated by the materials such as geological rock research. Thus, the invention has wider application fields.
To achieve the above object, according to one aspect of the present invention, there is provided an apparatus for quantitative detection of very weak magnetism of a material, comprising:
an internal magnetic shielding for providing a detection space for the silence of a magnetic field of the sample to be detected;
an external magnetic shield arranged on the periphery of the internal magnetic shield and used for realizing demagnetizing of the silence magnetic field;
the non-magnetic sample injection guide pipe penetrates through the inner magnetic shielding and the outer magnetic shielding, and is arranged in a non-contact manner with the inner magnetic shielding and the outer magnetic shielding, and one end of the non-magnetic sample injection guide pipe is connected with an air inlet module;
the sample rotating carrier is arranged in the detection space and is arranged in the non-magnetic sample injection catheter, and a sample filling bin is arranged in the sample rotating carrier and is used for placing a sample to be detected;
the pneumatic turbofan is arranged at one end of the sample rotating carrier, which is close to the air inlet module, and is used for driving the sample rotating carrier to rotate along the axis of the non-magnetic sample introduction guide pipe under the action of air flow provided by the air inlet module;
the rotating support module is arranged at the other end of the sample rotating carrier and is movably connected with the sample rotating carrier;
the magnetic field calibration coil is arranged in the detection space and corresponds to the sample filling bin and is used for calibrating the magnetic field of the sample to be detected; and
the vector atom magnetometer is arranged in the detection space and corresponds to the sample filling bin, and is used for detecting magnetic signals in the rotation process of the sample to be detected.
As a further preferable mode, the rotation support module comprises a slide block support stator, the connecting surface of the slide block support stator and the sample rotation carrier is a spherical curved surface, and a plurality of ventilation grooves are formed in the spherical curved surface.
As a further preference, the connecting surface of the slide support stator and the sample rotary carrier is also coated with a lubricant.
As a further preferable mode, the rotary support module further comprises a first support, a second support and a stator support, wherein the first support and the second support are fixedly connected with the non-magnetic sample injection guide pipe, the first support is arranged between the air inlet module and the external magnetic shielding, the second support is provided with the stator support which is fixedly connected with the sliding block support stator, and an air outlet pipe communicated with the air vent groove is arranged inside the stator support;
the stator support is carved with scales for conveying and positioning samples to be tested.
As a further preferable mode, the air inlet module comprises a gas compressor, a flow controller and an air inlet conduit which are sequentially connected, and the air inlet conduit is communicated with the non-magnetic sample injection conduit.
As a further preferred aspect, the magnetic field calibration device further comprises a precision power supply, wherein the precision power supply is electrically connected with the magnetic field calibration coil;
the magnetic field calibration coil generates a precise magnetic field with the same frequency as the rotating speed of the sample to be measured.
The system is used for acquiring magnetic signals obtained by detection and acquisition of a vector atom magnetometer, and the controller is used for realizing quantitative detection of the material very weak magnetism of the sample to be detected according to the magnetic signals and the calibrated magnetic field of the sample to be detected.
As a further preferred aspect, the sample filling bin is a square sample filling bin;
the sample rotating carrier is also provided with a sample bin cover;
the inner magnetic shielding and the outer magnetic shielding are both made of multi-layer permalloy.
According to another aspect of the present invention, there is also provided a method for quantitative detection of very weak magnetism of a material, comprising the steps of:
s1, providing a magnetically silent detection space, and feeding a sample to be detected into the detection space after the sample to be detected is silent for a certain time;
s2, driving the sample to be tested to rotate in a pneumatic mode, so that the sample to be tested generates magnetic field disturbance in the magnetic sensitivity direction of the vector atom magnetometer, and at the moment, the vector atom magnetometer detects and acquires magnetic signals of a detection space;
s3, adjusting the placing direction of the sample to be measured, and repeating the step S and the step S, so as to obtain magnetic signals of the sample to be measured in other directions;
s4, starting a magnetic field calibration coil, and completing calibration of the magnetic field of the sample to be tested by adopting the magnetic field calibration coil;
s5, realizing the quantitative detection of the material very weak magnetism of the sample to be detected according to the magnetic signal of the sample to be detected and the calibrated magnetic field.
As a further preferred aspect, step S1 specifically includes the steps of: after a sample to be measured is placed in a sample filling bin, pushing the sample rotating carrier into an external magnetic shielding for silence for a certain time, and then sending the sample rotating carrier into an internal magnetic shielding;
in step S2, the method for driving the sample to be tested to rotate in a pneumatic manner is as follows: controlling an air inlet module to input air flow into the nonmagnetic sample introduction guide pipe so as to blow the pneumatic turbofan to rotate by the air flow and drive a sample rotary carrier loaded with a sample to be tested to rotate; wherein the temperature within the sample rotating carrier can be controlled by controlling the temperature of the gas stream;
in step S3, the magnetic field calibration coil generates a precise magnetic field with the same frequency as the rotation speed of the sample to be measured, so as to calibrate the magnetic field.
In general, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
1. the vector atom magnetometer is used as an ultra-high-sensitivity magnetic field probe, and the magnetic field is measured in a magnetic shielding way in a magnetic silence space by matching with the rotary sample injection device; using a rotary sample feeding device to drive a sample to be measured to rotate, wherein the sample to be measured generates magnetic field disturbance in the magnetic sensitivity direction of the vector atom magnetometer; the vector atom magnetometer quantitatively detects the magnetic signal generated by the sample, so that the extremely weak magnetic quantitative detection of the material is realized.
2. The invention utilizes the vector atom magnetometer to cooperate with the rotary sample injection device to detect the magnetic field disturbance generated in the magnetic sensitive direction of the vector atom magnetometer by driving the sample to rotate in the rotating square sample filling bin in the magnetic shielding of the magnetic silence space, thereby realizing the quantitative detection of the material with very weak magnetism.
3. According to the invention, the air flow of the air inlet duct and the non-magnetic sample injection duct blows the pneumatic turbofan to drive the sample rotary carrier to rotate, the rotating speed of the sample rotary carrier is controlled by precisely controlled air flow, the rotation of the sample to be tested is realized, and the temperature of the sample in the square sample filling bin can be controlled by controlling the temperature of the air flow, so that a temperature change experiment is facilitated.
4. The stator supporting material is quartz glass with scales for sample transmission and positioning, the sliding block supporting stator can rotate to adapt to the rotation of the sample rotating carrier, and the rotating part uses materials with excellent lubricating performance, such as boron nitride, talcum powder with small granularity or silicone oil, and the like, as a lubricant, so that the friction force among parts is reduced, and the control precision of the rotating speed of the sample rotating carrier can be improved.
5. The inner magnetic shielding provides a detection space with silent magnetic field for the sample to be detected by using the atomic magnetometer, and the outer magnetic shielding provides a space with silent magnetic field for the sample to be detected before using the atomic magnetometer to demagnetize, so that the real magnetism of the material in the magnetic shielding can be accurately acquired.
6. The magnetic field calibration coil provided by the invention generates a precise magnetic field with the same frequency as the rotating speed of the sample, so that the magnetic field generated by the sample to be measured can be calibrated conveniently.
7. The non-magnetic sample injection guide pipe passes through the external magnetic shielding and the internal magnetic shielding and has no direct contact, so that the influence of mechanical vibration of the rotary sample injection device module on the magnetic field control module can be avoided.
8. The sample to be measured in the sample filling bin is solid material, can be square material or can be fixed by using a regular non-magnetic clamp and then placed in the square sample filling bin, so that the samples in various shapes can be conveniently measured.
9. The square sample filling bin can also be fixed on the nonmagnetic sampling guide pipe, and the sample rotation is realized by rotating the nonmagnetic sampling guide pipe, so that the magnetic field disturbance measurement of the rotating sample is realized.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for quantitative determination of very weak magnetism of a material according to a preferred embodiment of the present invention;
FIG. 2 is a schematic diagram of the working principle of the method related to the quantitative detection of the extremely weak magnetism of the material in the embodiment of the invention;
FIG. 3 is a schematic structural diagram of an apparatus for quantitative determination of very weak magnetism of a material according to another preferred embodiment of the present invention.
Like reference numerals denote like technical features throughout the drawings, in particular: 01-air inlet guide pipe, 02-air inlet sealing cover, 03-first support, 04-nonmagnetic sample injection guide pipe, 05-pneumatic turbofan, 06-sample bin cover, 07-sample filling bin, 08-sample rotating carrier, 09-second support, 10-slider support stator, 11-air outlet pipe, 12-stator support, 21-magnetic field calibration coil, 22-internal magnetic shielding, 23-external magnetic shielding, 24-vector atom magnetometer, 31-precise power supply, 32-signal acquisition system, 33-gas compressor, 34-flow controller, 41-sample to be tested and 42-rotational symmetry axis.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
As shown in fig. 1, the device for quantitatively detecting the very weak magnetism of a material provided by the embodiment of the invention comprises an internal magnetic shielding 22, an external magnetic shielding 23, a non-magnetic sample introduction conduit 04, a sample rotating carrier 08, a pneumatic turbofan 05, a rotating support module, a magnetic field calibration coil 21 and a vector atom magnetometer 24. The internal magnetic shield 22 provides a detection space for the sample to be tested to be subjected to magnetic field silence by using atomic magnetometer. The outer magnetic shield 23 is provided on the outer periphery of the inner magnetic shield 22, and is used for demagnetizing the magnetic field. The external magnetic shield 23 provides a space demagnetizing with a silent magnetic field for the sample to be measured before using the atomic magnetometer, so that the real magnetism of the material in the magnetic shield can be accurately obtained. In the present invention, both the inner magnetic shield 22 and the outer magnetic shield 23 are multi-layered permalloy. During operation of the device, the sample 41 to be measured first enters the external magnetic shield 23 and is silenced for a certain period of time, which can be set as required, typically for a few minutes. And then into the internal magnetic shield 22 for corresponding rotation and detection.
The non-magnetic sample introduction guide pipe 04 passes through the inner magnetic shielding 22 and the outer magnetic shielding 23, and the non-magnetic sample introduction guide pipe 04 is arranged in a non-contact manner with the inner magnetic shielding 22 and the outer magnetic shielding 23, and one end of the non-magnetic sample introduction guide pipe 04 is connected with an air inlet module. More specifically, the middle part of the nonmagnetic sample introduction guide pipe 04 is positioned in the outer magnetic shielding 23, and when the nonmagnetic sample introduction guide pipe 04 passes through the inner magnetic shielding 22 and the outer magnetic shielding 23, the nonmagnetic sample introduction guide pipe 04 is not contacted with the inner magnetic shielding 22 and the outer magnetic shielding 23. In one embodiment of the present invention, the internal magnetic shield 22 and the external magnetic shield 23 are provided with a rotation hole through which the nonmagnetic sample introduction pipe 04 is received, and the nonmagnetic sample introduction pipe 04 can rotate along its own axis in the rotation hole, as shown in fig. 2, in this embodiment of the present invention, the axis of the nonmagnetic sample introduction pipe 04 is collinear with the rotation symmetry axis 42, in such a way that the nonmagnetic sample introduction pipe 04 does not touch the internal magnetic shield 22 and the external magnetic shield 23 when corresponding mechanical vibration is generated.
The sample rotating carrier 08 is arranged in the detection space, the sample rotating carrier 08 is arranged in the non-magnetic sample introduction conduit 04, and a sample filling bin 07 is arranged in the sample rotating carrier 08 and used for placing a sample 41 to be detected. In general, sample filling bin 07 is a square sample filling bin. Of course, in some embodiments of the present invention, if the sample 41 to be measured is in a regular square shape, the sample 41 to be measured may be directly placed in the sample rotary carrier 08 instead of the sample filling bin 07, and the sample 41 to be measured may be rotated along with the rotation of the sample rotary carrier 08. In one embodiment of the present invention, the axial end of the sample rotary carrier 08 is further provided with a sample bin cover 06, and the rotating shaft of the pneumatic turbofan 05 is fixedly connected with the sample bin cover 06, so as to drive the sample rotary carrier 08 to rotate. Specifically, the pneumatic turbofan 05 is disposed at one end of the sample rotating carrier 08 near the air inlet module, and the pneumatic turbofan 05 is configured to drive the sample rotating carrier 08 to rotate along the axis of the non-magnetic sample injection conduit 04 under the action of the air flow provided by the air inlet module. In the present invention, in order to ensure the normal rotation of the pneumatic turbofan 05, a gap is provided between the outer wall of the sample rotating carrier 08 and the inner wall of the non-magnetic sample introduction pipe 04, and the gap can allow the air flow input by the air inlet module to pass through. In the invention, the air inlet module comprises a gas compressor 33, a flow controller 34 and an air inlet conduit 01 which are sequentially connected, wherein the air inlet conduit 01 is communicated with a non-magnetic sample introduction conduit 04.
The rotary support module is arranged at the other end of the sample rotary carrier 08 and is movably connected with the sample rotary carrier 08. More specifically, as shown in fig. 1 and 3, the rotation support module includes a slider support stator 10, a connection surface between the slider support stator 10 and the sample rotation carrier 08 is a spherical curved surface, and correspondingly, an end of the sample rotation carrier 08 is also a spherical curved surface corresponding to the spherical curved surface of the slider support stator 10. Specifically, the connection surface between the slider supporting stator 10 and the sample rotating carrier 08 is a concave spherical surface, the connection surface between the sample rotating carrier 08 and the slider supporting stator 10 is a convex spherical surface, and the spherical centers of the concave spherical surface and the convex spherical surface are the same, so that the sample rotating carrier 08 can rotate relative to the slider supporting stator 10 under the condition that the slider supporting stator 10 is fixed. In addition, in order to reduce the sliding friction between the sample rotary carrier 08 and the slider support stator 10, the connecting surface of the slider support stator 10 and the sample rotary carrier 08 is also coated with a lubricant. Meanwhile, a plurality of thread ventilation grooves are formed in the concave spherical curved surface and are used for enabling air flow of the air inlet module to pass through. In one real-time example of the invention, the plurality of vent grooves are symmetrically arranged about the axis of the sample rotary carrier 08.
In the preferred embodiment of the present invention, the rotary support module further includes a first support 03, a second support 09, and a stator support 12, where the first support 03 and the second support 09 are fixedly connected with the nonmagnetic sample injection conduit 04, the first support 03 is disposed between the air intake module and the external magnetic shielding 23, the second support 09 is provided with a stator support 12, the stator support 12 is fixedly connected with the slider support stator 10, and an air outlet pipe 11 communicating with the air vent groove is disposed inside the stator support 12. The stator support 12 is engraved with graduations for the transport positioning of the sample 41 to be measured.
In the present invention, the vector atom magnetometer 24 is disposed in the detection space and is disposed corresponding to the sample filling bin 07, for detecting the magnetic signal during the rotation of the sample 41 to be detected. The magnetic field calibration coil 21 is disposed in the detection space and corresponds to the sample filling bin 07, and is used for calibrating the magnetic field of the sample 41 to be detected. In general, the vector atom magnetometer 24 and the magnetic field calibration coil 21 are provided on both radial sides of the sample filling chamber 07, respectively. In the invention, the vector atom magnetometer 24 is adopted to detect in the magnetic shielding of the magnetic silence space, the rotary sample feeding device is matched for magnetic field measurement, then, the magnetic field calibration coil 21 is adopted to calibrate the magnetic field generated by the sample to be measured in the magnetic shielding of the magnetic silence space, the magnetic field calibration coil 21 generates a precise magnetic field with the same frequency as the rotating speed of the sample to be measured 41, and the precise magnetic field is used as magnetic field calibration to calibrate the magnetic field. The device comprises a signal acquisition system 32 and a controller, wherein the signal acquisition system 32 is used for acquiring magnetic signals obtained by detection and acquisition of the vector atom magnetometer 24, and the controller is used for realizing the quantitative detection of the extremely weak magnetism of the material of the sample 41 to be detected according to the magnetic signals and the calibrated magnetic field of the sample 41 to be detected.
According to another aspect of the present invention, there is also provided a method for quantitative detection of very weak magnetism of a material, comprising the steps of:
step one, providing a magnetic silence detection space, and feeding a sample to be detected into the detection space after silence for a certain time. More specifically, after the sample 41 to be measured is placed in the sample filling bin 07, the sample rotary carrier 08 is pushed into the external magnetic shield 23 to be silenced for a certain period of time, and then the sample rotary carrier 08 is sent into the internal magnetic shield 22.
And secondly, driving the sample 41 to be tested to rotate in a pneumatic mode, so that the sample 41 to be tested generates magnetic field disturbance in the magnetic sensitivity direction of the vector atom magnetometer 24, and at the moment, the vector atom magnetometer 24 detects and acquires magnetic signals of a detection space. More specifically, the air inlet module is controlled to input air flow into the non-magnetic sample introduction conduit 04, so that the air flow blows the pneumatic turbofan 05 to rotate to drive the sample rotary carrier 08 to rotate, so that the sample 41 to be measured generates magnetic field disturbance in the magnetic sensitivity direction of the vector atom magnetometer 24, and at this time, the vector atom magnetometer 24 detects and collects magnetic signals of the detection space. Wherein the temperature within the sample rotating carrier 08 can be controlled by controlling the temperature of the gas stream during the introduction of the gas stream. At the same time, vector atom magnetometer 24 communicates its magnetic signals that detect and acquire the detection space to signal acquisition system 32.
Step three, the placing direction of the sample 41 to be measured is adjusted, and the steps S1 and S2 are repeated, so as to obtain magnetic signals of other directions of the sample 41 to be measured. In the present invention, in the process of adjusting the placement direction of the sample 41 to be measured, the placement direction of the sample 41 to be measured can be adjusted along the axis direction of the sample 41 to be measured.
And step four, starting a magnetic field calibration coil 21, and completing the calibration of the magnetic field of the sample 41 to be tested by adopting the magnetic field calibration coil 21.
And fifthly, realizing the quantitative detection of the extremely weak magnetism of the material of the sample 41 to be detected according to the magnetic signal of the sample 41 to be detected and the calibrated magnetic field. In the invention, the controller is used for receiving the magnetic signal and the calibrated magnetic field size, and realizing the quantitative detection of the material very weak magnetism of the sample to be detected according to the magnetic signal and the calibrated magnetic field size of the sample to be detected.
The device and the method for quantitatively detecting the material in the extremely weak magnetism are particularly suitable for quantitatively measuring the magnetic field generated by components required by miniaturized chip of sensors such as chip-level atomic clocks, atomic magnetometers, nuclear magnetic resonance gyroscopes and the like, and selecting nonmagnetic components so as to eliminate the non-uniformity of the magnetic field in the sensor caused by magnetism generated by the components, and can also be used for quantitatively measuring the magnetic field generated by materials such as geological rock research and the like. The vector atom magnetometer is used as an ultra-high sensitive magnetic field probe, and the rotary sample feeding device is used for driving the sample to be tested to rotate in the magnetic shielding of the magnetic silence space during detection, so that the magnetic field disturbance of the sample to be tested in the magnetic sensitivity direction of the vector atom magnetometer is generated, the vector atom magnetometer detects the magnetic signal of the sample, and the ultra-weak magnetic quantitative detection of the material is realized. The invention is particularly suitable for quantitative measurement of magnetic fields generated by components required by miniaturized chips of sensors such as chip-level atomic clocks, atomic magnetometers, nuclear magnetic resonance gyroscopes and the like, and non-magnetic components are selected so as to eliminate non-uniformity of the magnetic fields in the sensors caused by magnetism generated by the components, and can also be used for quantitative measurement of the magnetic fields generated by materials such as geological rock research and the like.
Example 1
In this embodiment, the device for quantitatively detecting the very weak magnetism of the material comprises a rotary sample injection device module and a magnetic field control module, wherein the rotary sample injection device part comprises an air inlet guide pipe 01, an air inlet sealing cover 02, a first support 03, a non-magnetic sample injection guide pipe 04, a pneumatic turbofan 05, a sample bin cover 06, a square sample filling bin 07, a sample rotary carrier 08, a second support 09, a sliding block support stator 10, an air outlet pipe 11 and a stator support 12, and the magnetic field control part comprises a magnetic field calibration coil 21, an internal magnetic shielding 22, an external magnetic shielding 23 and a vector atomic magnetometer 24. In this embodiment, the vector atom magnetometer 24 is used in combination with the rotary sample injection device to detect the magnetic field disturbance generated in the magnetic sensitive direction of the vector atom magnetometer 24 by the rotation of the sample in the square sample filling bin 07 in the magnetic shielding 22 of the magnetic silence space, and the ultra-high sensitivity of the vector atom magnetometer 24 is used to quantitatively detect the magnetic field component of the rotary sample, so as to realize the quantitative detection of the ultra-weak magnetism of the material. The sample rotating carrier 08 blows the air-driven turbofan 05 through the air flow of the air inlet duct 01 and the non-magnetic sample injection duct 04 to drive the sample rotating carrier 08 to rotate, the rotating speed of the sample rotating carrier 08 is controlled through the air flow which is precisely controlled, so that magnetic field information with stable rotating frequency of the rotating sample is obtained, and the temperature of the sample in the square sample filling bin 07 can be controlled through controlling the temperature of the air flow. The slide block supporting stator 10 and the sample rotating carrier 08 are made of hard nonmetallic materials such as zirconia, the stator supporting 12 is made of quartz glass, scales are arranged on the quartz glass and used for sample transmission and positioning, the slide block supporting stator 10 can rotate to adapt to the rotation of the sample rotating carrier 08, boron nitride can be used as a lubricant in a rotating part, friction force among parts can be reduced, and the control precision of the rotating speed of the sample rotating carrier 08 is improved. The inner magnetic shielding 22 and the outer magnetic shielding 23 are both made of multi-layer permalloy, the inner magnetic shielding 22 provides a magnetic field silencing detection space for a sample to be detected by using an atomic magnetometer, and the outer magnetic shielding 23 provides a magnetic field silencing space for the sample to be detected before using the atomic magnetometer so as to accurately acquire the real magnetism of the material in the magnetic shielding.
The magnetic field calibration coil 21 generates a precise magnetic field with the same frequency as the rotation speed of the sample to calibrate the magnetic field generated by the sample to be measured. The nonmagnetic sample injection guide pipe 04 is made of a quartz glass tube, and is supported by the first support 03 and the second support 09, and the nonmagnetic sample injection guide pipe 04 passes through the outer magnetic shielding 23 and the inner magnetic shielding 22 without direct contact, so that the influence of mechanical vibration of the rotary sample injection device module on the magnetic field control module can be avoided.
The sample to be measured in the sample filling bin 07 is solid material, and can be square material or fixed by using a regular non-magnetic clamp and then placed in the sample filling bin 07 so as to measure samples with various shapes. The sample filling bin 07 can also be fixed on the non-magnetic sample introduction guide pipe 04, and the sample rotation is realized by rotating the non-magnetic sample introduction guide pipe 04, so that the magnetic field disturbance measurement of the rotating sample is realized.
In operation, a sample to be measured is placed in the square sample filling bin 07, and the sample bin cover 06 is tightly covered. The sample-loaded sample rotary carrier 08 is then pushed into the external magnetic shield 23 by the stator support 12 and silenced for a few minutes before being fed into the internal magnetic shield 22 for measurement. The precisely controlled air flow blows the pneumatic turbofan 05 through the air inlet duct 01 and the non-magnetic sample injection duct 04 to drive the sample rotary carrier 08 to rotate, the rotating speed of the sample rotary carrier 08 is controlled through the precisely controlled air flow, the vector atomic magnetometer 24 detects and obtains magnetic signals and collects the magnetic signals, and the temperature of samples in the square sample filling bin 07 can be controlled by controlling the temperature of the air flow if temperature control is needed. And (3) placing the sample to be measured into a square sample filling bin 07 after adjusting the direction, covering a sample bin cover 06, repeating the step (1) and the step (2), and measuring magnetic fields of the sample in other directions. Finally, the magnetic field calibration coil 21 is used for calibrating the magnetic field of the sample, so that the material extremely weak magnetism quantitative detection of the sample is realized.
As shown in fig. 3, some devices including a precise power supply 31, a signal acquisition system 32, a gas compressor 33 and a flow controller 34 are added, so that the method is more practical to be applied to the quantitative detection of the extremely weak magnetism of the material. In an embodiment, the precision power supply 31 provides the precision current required by the magnetic field calibration coil 21. The signal acquisition system 32 acquires magnetic signals acquired by the vector atom magnetometer 24. The air compressor 33 and the flow controller 34 are matched to provide precisely controlled air flow so as to control the rotation speed of the sample rotary carrier 08 and realize the rotation of the sample to be tested.
It will be readily appreciated by those skilled in the art that the foregoing description is merely a preferred embodiment of the invention and is not intended to limit the invention, but any modifications, equivalents, improvements or alternatives falling within the spirit and principles of the invention are intended to be included within the scope of the invention.

Claims (10)

1. A device for quantitative detection of very weak magnetism of a material, comprising:
an internal magnetic shield (22) for providing a detection space for the silence of the magnetic field of the sample (41) to be detected;
an external magnetic shield (23), wherein the external magnetic shield (23) is arranged on the periphery of the internal magnetic shield (22) and is used for realizing demagnetizing of the silence magnetic field;
the non-magnetic sample injection guide pipe (04), the non-magnetic sample injection guide pipe (04) passes through the inner magnetic shielding (22) and the outer magnetic shielding (23), the non-magnetic sample injection guide pipe (04) is arranged in a non-contact manner with the inner magnetic shielding (22) and the outer magnetic shielding (23), and one end of the non-magnetic sample injection guide pipe (04) is connected with an air inlet module;
the sample rotary carrier (08), the said sample rotary carrier (08) is said to detect in the space, and this sample rotary carrier (08) locates in the said non-magnetic sample introduction conduit (04), there are sample filling bins (07) in this sample rotary carrier (08), is used for placing the sample (41) to be measured;
the pneumatic turbofan (05) is arranged at one end of the sample rotating carrier (08) close to the air inlet module, the pneumatic turbofan (05) is used for driving the sample rotating carrier (08) to rotate along the axis of the non-magnetic sample injection conduit (04) under the action of air flow provided by the air inlet module, and the temperature in the sample rotating carrier (08) is controlled by controlling the temperature of the air flow in the air flow introducing process;
the rotary support module is arranged at the other end of the sample rotary carrier (08) and is movably connected with the sample rotary carrier (08);
the magnetic field calibration coil (21) is arranged in the detection space and corresponds to the sample filling bin (07) for calibrating the magnetic field of the sample (41) to be detected; and
and the vector atom magnetometer (24) is arranged in the detection space and corresponds to the sample filling bin (07) and is used for detecting magnetic signals in the rotation process of the sample (41) to be detected.
2. The device for quantitative detection of material very weak magnetism according to claim 1, wherein the rotation support module comprises a slide support stator (10), a connection surface of the slide support stator (10) and the sample rotation carrier (08) is a spherical curved surface, and a plurality of ventilation grooves are arranged on the spherical curved surface.
3. A device for quantitative detection of very weak magnetism of a material according to claim 2, characterized in that the interface of the slider support stator (10) and the sample rotation carrier (08) is further coated with a lubricant.
4. The device for quantitative detection of material very weak magnetism according to claim 2, wherein the rotary support module further comprises a first support (03), a second support (09) and a stator support (12), the first support (03) and the second support (09) are fixedly connected with the non-magnetic sample introduction guide tube (04), the first support (03) is arranged between the air inlet module and the external magnetic shielding (23), the second support (09) is provided with the stator support (12), the stator support (12) is fixedly connected with the sliding block support stator (10), and an air outlet tube (11) communicated with the air vent groove is arranged inside the stator support (12); the stator support (12) is carved with scales for conveying and positioning the sample (41) to be tested.
5. The device for quantitative detection of material very weak magnetism according to claim 1, wherein the air inlet module comprises a gas compressor (33), a flow controller (34) and an air inlet conduit (01) which are sequentially connected, and the air inlet conduit (01) is communicated with a non-magnetic sample introduction conduit (04).
6. The device for quantitative detection of very weak magnetism of material according to claim 1, further comprising a precision power supply (31), said precision power supply (31) being electrically connected to the magnetic field calibration coil (21); the magnetic field calibration coil (21) generates a precise magnetic field with the same frequency as the rotating speed of the sample (41) to be measured as magnetic field calibration.
7. The device for quantitative detection of material very weak magnetism according to claim 1, further comprising a signal acquisition system (32) and a controller, wherein the signal acquisition system (32) is used for acquiring a magnetic signal obtained by detection and acquisition of a vector atomic magnetometer (24), and the controller is used for realizing quantitative detection of material very weak magnetism of the sample (41) to be detected according to the magnetic signal and the calibrated magnetic field size of the sample (41) to be detected.
8. The device for quantitative detection of very weak magnetism of materials according to claim 1, characterized in that the sample filling bin (07) is a square sample filling bin; a sample bin cover (06) is further arranged on the sample rotary carrier (08); the inner magnetic shielding (22) and the outer magnetic shielding (23) are both made of multi-layer permalloy.
9. A method for quantitatively detecting the very weak magnetism of a material, which is characterized by comprising the following steps:
s1, providing a magnetically silent detection space, and feeding a sample to be detected into the detection space after the sample to be detected is silent for a certain time;
s2, driving the sample (41) to be tested to rotate in a pneumatic mode, so that the sample (41) to be tested generates magnetic field disturbance in the magnetic sensitivity direction of the vector atom magnetometer (24), and at the moment, the vector atom magnetometer (24) detects and acquires magnetic signals of a detection space;
s3, adjusting the placement direction of the sample (41) to be measured, and repeating the step S1 and the step S2, so as to obtain magnetic signals of the sample (41) to be measured in other directions;
s4, starting a magnetic field calibration coil (21), and completing the calibration of the magnetic field of the sample (41) to be tested by adopting the magnetic field calibration coil (21);
s5, realizing the quantitative detection of the extremely weak magnetism of the material of the sample (41) to be detected according to the magnetic signal of the sample (41) to be detected and the calibrated magnetic field.
10. The method for quantitative detection of very weak magnetism of a material according to claim 9, wherein step S1 specifically comprises the steps of: after a sample (41) to be tested is placed into a sample filling bin (07), pushing a sample rotating carrier (08) into an external magnetic shielding (23) for silence for a certain time, and then sending the sample rotating carrier (08) into an internal magnetic shielding (22);
in step S2, the method for driving the sample (41) to be tested to rotate in a pneumatic manner is as follows: controlling an air inlet module to input air flow into the nonmagnetic sample introduction conduit (04) so as to blow the pneumatic turbofan (05) to rotate by the air flow and drive the sample rotary carrier (08) loaded with the sample (41) to be tested to rotate; wherein the temperature within the sample rotating carrier (08) can be controlled by controlling the temperature of the air flow;
in step S4, the magnetic field calibration coil (21) generates a precision magnetic field with the same frequency as the rotation speed of the sample (41) to be measured, so as to calibrate the magnetic field.
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