CN109655771A - Ac magnetic susceptibility measuring device and its measurement method - Google Patents
Ac magnetic susceptibility measuring device and its measurement method Download PDFInfo
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- CN109655771A CN109655771A CN201710941542.2A CN201710941542A CN109655771A CN 109655771 A CN109655771 A CN 109655771A CN 201710941542 A CN201710941542 A CN 201710941542A CN 109655771 A CN109655771 A CN 109655771A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R33/00—Arrangements or instruments for measuring magnetic variables
- G01R33/12—Measuring magnetic properties of articles or specimens of solids or fluids
- G01R33/16—Measuring susceptibility
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Abstract
The present invention provides a kind of ac magnetic susceptibility measuring devices, comprising: excitation coil is used to generate excitation field in the energized state；Hall sensor inside the excitation coil, the Hall sensor include two current input terminals and two voltage output ends, the direction for the excitation field of the bias current in described two current input terminals being oriented parallel to inside the excitation coil；First signal generator, for providing the ac-excited of first frequency to the excitation coil；Second signal generator, output end are connected to two current input terminals of the Hall sensor, for providing the ac-excited of second frequency to the Hall sensor；Lock-in amplifier measures the voltage output signal of the Hall sensor；And third signal generator provides third frequency reference signal for the lock-in amplifier.Ac magnetic susceptibility measuring device of the invention has the excellent properties such as measurement accuracy height, signal-to-noise ratio height at low frequency.
Description
Technical field
The present invention relates to magnetic susceptibility measurement fields, and in particular to a kind of ac magnetic susceptibility measuring device and its measurement method.
Background technique
When applying an alternating magnetic field in magnetic sample, magnetic sample itself, which can induce, generates an alternation magnetic moment,
The ratio of the magnetic moment and alternating magnetic field is exactly the ac magnetic susceptibility of magnetic sample.It is induced under alternating magnetic field due to magnetic sample
Magnetic moment shakes at any time, therefore from the magnetization dynamics information of the available sample of ac magnetic susceptibility.Ac magnetic susceptibility is characterization
The important parameter of physical property has in fields such as spin glass, superparamagnetic, magnetic phase transition and superconductions and is widely applied very much.
Fig. 1 is a kind of schematic diagram of ac magnetic susceptibility measuring device in the prior art, as shown in Figure 1, ac magnetic susceptibility
Measuring device 1 includes primary excitation coil 11 and secondary induction coil 12,13.Secondary induction coil 12 and 13 is located at primary excitation
In coil 11, the two the number of turns is identical, winding direction is opposite.The both ends of primary excitation coil 11 are connected to AC power source 14, secondary
Induction coil 12,13 is connected to voltmeter 15.By [Mn12O12(CH3COO)16(H2O)4] (0.2 millimeter × 0.2 millimeter ×
0.4 millimeter) made of magnetism sample to be tested 16 (black block shown in Fig. 1) be placed on the inside of secondary induction coil 12, it is primary
The alternating magnetic field induced samples 16 generated in excitation coil 11 generate alternation magnetic moment, and the alternation magnetic moment is in secondary induction coil 12
Induction generates induced electromotive force, and the magnetic field that primary coil 11 generates induces the induced electromotive force of generation anti-in secondary coil 12
The reverse induction electromotive force generated to the secondary coil 13 of coiling is offset.Therefore, both ends is total after secondary coil 12,13 is connected
Induced electromotive force is only generated by sample 16, obtains the ac magnetic susceptibility information of magnetic sample 16 by measuring the induced electromotive force.
Fig. 2 and Fig. 3 is that ac magnetic susceptibility measuring device measurement magnetic sample frequency shown in FIG. 1 is under 13 hertz respectively
The real and imaginary parts of ac magnetic susceptibility vary with temperature curve graph.From Fig. 2 and 3 as can be seen that the real part and void of ac magnetic susceptibility
Portion can not learn magnetic sample ac magnetic susceptibility with the changing rule of external environment with the random variation of temperature.
Since the principle of the above-mentioned ac magnetic susceptibility using search coil measurement magnetic sample is based on the sense of faraday's electromagnetism
Law is answered, therefore induced electromotive force is proportional to the change rate of magnetic flux in coil.In high frequency measurement area, due to 12 He of secondary coil
13 high frequency magnetic field that primary excitation coil 11 full symmetric will not be made to generate in practical winding process is in secondary induction line
The induced electromotive force generated in circle 12,13 can not be completely counterbalanced by and generate biggish measurement background signal.Importantly, low
Frequency measurement zone low frequency ac makes the electromotive force inducted on search coil 12 and 13 lower, therefore signal-to-noise ratio is very poor.In addition, new
It was found that sample of magnetic material the usual very little of volume, magnetic moment also very little, this puts forward higher requirements measurement accuracy.Cause
This is unable to satisfy using the ac magnetic susceptibility measuring device 1 of search coil in low frequency range currently based on Faraday's electromagnetic induction law
Measure the demand of the sample ac magnetic susceptibility of small magnetic moment.
Summary of the invention
For above-mentioned technical problem of the existing technology, the embodiment provides a kind of measurements of ac magnetic susceptibility
Device, comprising:
Excitation coil is used to generate excitation field in the energized state；
Hall sensor inside the excitation coil, the Hall sensor include two current input terminals and two
A voltage output end, the excitation of the bias current in described two current input terminals being oriented parallel to inside the excitation coil
The direction in magnetic field；
First signal generator, output end are connected to the both ends of the excitation coil, for mentioning to the excitation coil
For the ac-excited of first frequency；
Second signal generator, output end are connected to two current input terminals of the Hall sensor, for institute
It states Hall sensor and the ac-excited of second frequency is provided；
Lock-in amplifier, signal input part are connected to two voltage output ends of the Hall sensor；And
Third signal generator exports the reference signal input of the lock-in amplifier of third frequency
End.
Preferably, the Hall sensor is in cross, two current input terminals of the Hall sensor are oppositely arranged,
And it is parallel to the direction of the excitation field.
Preferably, two voltage output ends of the Hall sensor be disposed in in described two current input terminals
On the vertical same straight line of bias current.
Preferably, there is the adhesive for fixed magnetic sample at the right-angled intersection of the Hall sensor.
Preferably, the excitation coil is in solenoidal structure.
It preferably, further include bracket made of non-magnetic material, the bracket is located inside the excitation coil, the branch
Frame has the positioning plane parallel with the direction of the excitation field, and the Hall sensor is arranged on the positioning plane
On.
Preferably, the third frequency be equal to the first frequency and second frequency difference or the sum of.
Preferably, the frequency of first signal generator, second signal generator and the output of third signal generator connects
Continue adjustable and is triggered with common clock.
The present invention also provides a kind of measurement methods based on above-mentioned ac magnetic susceptibility measuring device, including the following steps:
Sample to be tested is adhered to the induction region of the Hall sensor by step 1)；
The Hall sensor is placed on inside the excitation coil by step 2), so that the Hall sensor is inclined
Set the direction for the excitation field that sense of current is parallel to inside the excitation coil；
Step 3), the temperature for controlling the sample to be tested is scheduled temperature value；
Step 4) adjusts the output frequency of first signal generator to provide first frequency to the excitation coil
It is ac-excited, the output frequency of the second signal generator is adjusted to provide the exchange of second frequency to the Hall sensor
Excitation adjusts the third signal generator output frequency to provide third to the reference signal input terminal of the lock-in amplifier
Frequency it is ac-excited；
Step 5) measures the voltage of the voltage output end of the Hall sensor using the lock-in amplifier.
It is excellent that ac magnetic susceptibility measuring device of the invention has that measurement accuracy is high, signal-to-noise performance is excellent etc. at low frequency
Performance.
Detailed description of the invention
Embodiments of the present invention is further illustrated referring to the drawings, in which:
Fig. 1 is a kind of schematic diagram of ac magnetic susceptibility measuring device in the prior art.
Fig. 2 is ac magnetic susceptibility measuring device measurement [Mn shown in FIG. 112O12(CH3COO)16(H2O)4] (0.2 millimeter ×
0.2 millimeter × 0.4 millimeter) magnetic sample frequency is that the real part of ac magnetic susceptibility under 13 hertz varies with temperature curve graph.
Fig. 3 is ac magnetic susceptibility measuring device measurement [Mn shown in FIG. 112O12(CH3COO)16(H2O)4] (0.2 millimeter ×
0.2 millimeter × 0.4 millimeter) magnetic sample frequency is that the imaginary part of ac magnetic susceptibility under 13 hertz varies with temperature curve graph.
Fig. 4 is the schematic diagram of the ac magnetic susceptibility measuring device of preferred embodiment according to the present invention.
Fig. 5 is to measure [Mn using ac magnetic susceptibility measuring device shown in Fig. 412O12(CH3COO)16(H2O)4] (0.2 milli
Rice × 0.2 millimeter × 0.4 millimeter) magnetic sample frequency is respectively ac magnetization under 3Hz, 13Hz, 33Hz, 77Hz and 133Hz
Rate real part varies with temperature curve graph.
Fig. 6 is ac magnetic susceptibility measuring device measurement [Mn shown in Fig. 412O12(CH3COO)16(H2O)4] (0.2 millimeter ×
0.2 millimeter × 0.4 millimeter) magnetic sample frequency is respectively that ac magnetic susceptibility under 3Hz, 13Hz, 33Hz, 77Hz and 133Hz is empty
Portion varies with temperature curve graph.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, pass through below in conjunction with attached drawing specific real
Applying example, the present invention is described in more detail.
Fig. 4 is the schematic diagram of the ac magnetic susceptibility measuring device of preferred embodiment according to the present invention.As shown in figure 4, exchange
Magnetic susceptibility measurement device 2 includes bracket 25, solenoidal structure excitation coil 21.Bracket 25 is made of non-magnetic material, is in semicolumn
Shape, have with a part of compatible arc surface 251 of the inner sidewall of excitation coil 21 (in Fig. 4 shown in dotted line) and with swash
Encourage the parallel positioning plane 252 of the axial direction of coil 21.Ac magnetic susceptibility measuring device 2 further includes by GaAs/AlGaAs hetero-junctions
Manufactured sheet Hall sensor 22, Hall sensor 22 are adhered in the positioning plane 252 of bracket 25 and are parallel to the positioning
Plane 252.Hall sensor 22 is in cross, has the current input terminal 221,222 being oppositely arranged, and be oppositely arranged
Voltage output end 223,224.The axis for being parallel to excitation coil 21 since current input terminal 221,222 on the same line is arranged
To, therefore when the current input terminal of Hall sensor 22 221,222 is powered, the bias current direction in Hall sensor 22 is flat
Magnetic direction of the row inside excitation coil 21, so that excitation field will not induce on Hall sensor 22 generates Hall
Voltage.
Ac magnetic susceptibility measuring device 2 further includes the locking phase being connected with the voltage output end 223,224 of Hall sensor 22
Amplifier 23, frequency continuously adjustable signal generator 2a, 2b and 2c trigger clock 2d and the computer for data acquisition
26。
The output end of signal generator 2a is connected to the both ends of excitation coil 21, and the output end of signal generator 2b is connected to
The current input terminal 221,222 of Hall sensor 22, the output end of signal generator 2c is connected to the reference of lock-in amplifier 23
Signal input part 231, wherein signal generator 2c and lock-in amplifier 23 constitute voltage measuring apparatus.Trigger clock 2d output end
The input end of clock of signal generator 2a, 2b and 2c are connected to so that three's clock triggering having the same.
The measuring principle of the ac magnetic susceptibility measuring device 2 of the present embodiment is as follows:
Signal generator 2a output frequency is the ac-excited into excitation coil 21 of f, and excitation is generated in excitation coil 21
Magnetic fieldWherein H0For the magnetic field amplitude in excitation coil 21, f is field frequency,For magnetic phase.
Signal generator 2b exports alternating currentWherein I0For the bias current width in Hall sensor 22
Value, f ' are power frequency,' it is current phase.Sample to be tested induces the magnetic for generating identical frequency under the action of excitation field H
Square M=χ H, wherein χ is sample magnetic susceptibility.The magnetic fields that the magnetic moment generates generate Hall voltage on Hall sensor.Hall
Voltage VHallIt is as follows with the relationship of the electric current I on sample magnetic susceptibility χ, excitation field H and Hall sensor:
Signal generator 2c output frequency be f-f ' (or f+f ') alternating signal to lock-in amplifier 23 reference signal
Input terminal, thus lock-in amplifier 23 measures Hall voltage VHallIn f-f ' difference frequency component (or f+f ' sum of fundamental frequencies component), just
Than in sample magnetic susceptibility χ.
Hall sensor 22 of the invention can detect magnetic field caused by small magnetic moment sample, and then improve measurement accuracy；
The Hall voltage that Hall sensor 22 exports is directly proportional to the magnetic field that sample magnetic moment generates, unrelated with measurement frequency, therefore even if
The ac magnetic susceptibility data of high s/n ratio can be also obtained in low frequency region；Hall sensor is equivalent to a mixing in the measurements
Device, relevant double cross flow measuring method use so that lock-in amplifier frequency measured directly is excitation coil alternating magnetic field and suddenly
The difference frequency or sum of fundamental frequencies of your sensor current, avoid excitation coil alternating magnetic field frequency, efficiently solve based on faraday's electricity
The larger back that the search coil ac magnetic susceptibility device medium-high frequency region alternating magnetic field of law of magnetic induction is inducted in measuring circuit
This problem of bottom signal.More importantly due to Hall sensor electric current, the electric current of generation alternating current magnetic field and lock-in amplifier ginseng
Signal is examined from same clock, lock-in amplifier carries out relevant detection to electric current and magnetic field signal, and noncoherent noise is filtered out, and believes
It makes an uproar than further increasing.
Based on above-mentioned measuring principle, in order to improve precision, the voltage output end 223,224 of Hall sensor 22 is disposed in
On the same straight line vertical with the bias current direction in current input terminal 221,222, reduce or avoid Hall sensor 22
Electric resistance partial pressure on bias current direction impacts measurement Hall voltage.
The ac magnetic susceptibility of the measurement magnetic sample of ac magnetic susceptibility measuring device 2 using the present embodiment is summarized below
Method.
Prepare 0.2 millimeter × 0.2 millimeter × 0.4 millimeter of single molecular magnets [Mn first12O12(CH3COO)16(H2O)4]
(Mn12Ac) single crystal samples 24.Single crystal samples 24 to be measured are adhered on the surface of Hall sensor 22 by cryogenic vacuum silicone grease,
Wherein one end of single crystal samples 24 is fixed at the Hall sensor right-angled intersection made using GaAs/AlGaAs hetero-junctions.It will
Single crystal samples 24 and Hall sensor 22 are fixed on together in the positioning plane 252 of bracket 25, then bracket 25 is placed on excitation
Inside coil 21, the property of can choose between the contact surface of the two filling adhesive to avoid excitation coil 21 with respect to bracket 25
Sliding, further ensures that the magnetic direction that the bias current in Hall sensor 22 is oriented parallel to inside excitation coil 21, most
Ac magnetic susceptibility measuring device 2 is placed on to the measurement that sample to be tested 24 is controlled in physical measurement instrument (PPMS) sample cavity afterwards
Temperature.
The same clock triggering 2d that wherein signal generator 2a, 2b, 2c is selected is signal generator 2a internal clocking, frequency
For 10MHz.The voltage peak-to-peak value of signal generator 2a output is 10 volts, and frequency f is 13 hertz, at this time swashing in excitation coil 21
Encouraging electric current is 3.6mA, and excitation field is about 12 Gausses.The voltage peak-to-peak value of signal generator 2b output is 10 volts, frequency f'=
8.125Hz, the current offset in Hall sensor 22 is 3.6 μ A at this time.The voltage peak-to-peak value of signal generator 2c output is 2
Volt, frequency are 4.875Hz (i.e. f-f').The parameter setting of lock-in amplifier 23 is as follows: time constant is 3 seconds, and range is 20 μ V,
Signal behavior XY mode, reference signal selection external reference signal source.
The real and imaginary parts numerical value of the output signal of lock-in amplifier 23 is recorded using computer 26, frequency, which can be obtained, is
The information of the real and imaginary parts of the ac magnetic susceptibility of institute's sample under 13Hz.By changing the temperature in PPMS sample cavity, thus
Obtain the information of the ac magnetic susceptibility real and imaginary parts of sample to be tested 24 at different temperatures.
Fig. 5 and Fig. 6 show respectively using ac magnetic susceptibility measuring device 2 measure above-mentioned sample frequency be respectively 3Hz,
Ac magnetic susceptibility real and imaginary parts under 13Hz, 33Hz, 77Hz and 133Hz vary with temperature curve graph.With adopt in the prior art
It is compared, the exchange of the present embodiment with based on Faraday's electromagnetic induction law using coil measurement ac magnetic susceptibility (Fig. 2,3 shown in)
Magnetic susceptibility measurement device 2 effectively improves measurement accuracy and signal-to-noise ratio, obtains the excellent low-frequency ac magnetic susceptibility number of signal-to-noise ratio
According to.
The present invention is not limited to measure the ac magnetic susceptibility of single molecular magnets, the exchange of other magnetic materials can also be measured
Magnetic susceptibility.
In other embodiments of the invention, other any materials with significant Hall effect can be used in Hall sensor
Preparation.
In other embodiments of the invention, excitation coil 21 is not limited to winding in solenoidal structure, as long as making in it
The magnetic field distribution in portion is uniform.Similarly, bracket 25 of the invention is not limited to semi-cylindrical, is also possible to other shapes
Shape is configured to have the positioning plane parallel with the direction of excitation field.
In other embodiments of the invention, the clock output of any of signal generator 2a, 2b, 2c signal generator
End is connected to the input end of clock of other two signal generators.
In other embodiments of the invention, the ac-excited frequency of signal generator 2c output is signal generator 2a
With the sum of the ac-excited frequency of signal generator 2b output.
Although the present invention has been described by means of preferred embodiments, the present invention is not limited to described here
Embodiment, without departing from the present invention further include made various changes and variation.
Claims (9)
1. a kind of ac magnetic susceptibility measuring device characterized by comprising
Excitation coil is used to generate excitation field in the energized state；
Hall sensor inside the excitation coil, the Hall sensor include two current input terminals and two electricity
Press output end, the excitation field of the bias current in described two current input terminals being oriented parallel to inside the excitation coil
Direction；
First signal generator, output end are connected to the both ends of the excitation coil, for providing the to the excitation coil
One frequency it is ac-excited；
Second signal generator, output end are connected to two current input terminals of the Hall sensor, are used for described in suddenly
You provide the ac-excited of second frequency by sensor；
Lock-in amplifier, signal input part are connected to two voltage output ends of the Hall sensor；And
Third signal generator exports the reference signal input terminal of the lock-in amplifier of third frequency.
2. ac magnetic susceptibility measuring device according to claim 1, which is characterized in that the Hall sensor is in cross
Two current input terminals of shape, the Hall sensor are oppositely arranged and are parallel to the direction of the excitation field.
3. ac magnetic susceptibility measuring device according to claim 2, which is characterized in that two electricity of the Hall sensor
Pressure output end is disposed on the same straight line vertical with the bias current in described two current input terminals.
4. ac magnetic susceptibility measuring device according to claim 2, which is characterized in that the cross of the Hall sensor is handed over
There is the adhesive for fixed magnetic sample at fork.
5. ac magnetic susceptibility measuring device according to claim 1, which is characterized in that the excitation coil is in solenoid
Shape.
6. ac magnetic susceptibility measuring device according to claim 5, which is characterized in that further include made of non-magnetic material
Bracket, the bracket are located inside the excitation coil, and the bracket has the positioning parallel with the direction of the excitation field
Plane, the Hall sensor are arranged in the positioning plane.
7. ac magnetic susceptibility measuring device according to claim 1, which is characterized in that the third frequency is equal to described the
The difference of one frequency and second frequency or the sum of.
8. ac magnetic susceptibility measuring device according to claim 1, which is characterized in that first signal generator,
Binary signal generator and the frequency of third signal generator output are continuously adjusted and trigger with common clock.
9. a kind of measurement method based on ac magnetic susceptibility measuring device described in any item of the claim 1 to 8, feature exist
In, including the following steps:
Sample to be tested is adhered to the Hall sensor induction region by step 1)；
The Hall sensor is placed on inside the excitation coil by step 2), so that the biased electrical of the Hall sensor
The direction for the excitation field of stream being oriented parallel to inside the excitation coil；
Step 3), the temperature for controlling the sample to be tested is scheduled temperature value；
Step 4) adjusts the output frequency of first signal generator to provide the exchange of first frequency to the excitation coil
Excitation adjusts the output frequency of the second signal generator to provide the exchange of second frequency to the Hall sensor and swash
It encourages, adjusts the third signal generator output frequency to provide third frequency to the reference signal input terminal of the lock-in amplifier
Rate it is ac-excited；
Step 5) measures the voltage of the voltage output end of the Hall sensor using the lock-in amplifier.
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| CN110579729A (en) * | 2019-10-10 | 2019-12-17 | 北京飞斯科科技有限公司 | alternating current magnetic susceptibility measuring device and method |
| CN114264555A (en) * | 2021-12-29 | 2022-04-01 | 中国科学院合肥物质科学研究院 | Device and method for measuring strain distribution state of superconducting wire |
| CN115718273A (en) * | 2022-11-18 | 2023-02-28 | 华中科技大学 | Device and method for measuring object magnetic susceptibility based on magnetic induction intensity |
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| CN114264555A (en) * | 2021-12-29 | 2022-04-01 | 中国科学院合肥物质科学研究院 | Device and method for measuring strain distribution state of superconducting wire |
| CN114264555B (en) * | 2021-12-29 | 2023-09-12 | 中国科学院合肥物质科学研究院 | Device and method for measuring strain distribution state of superconducting wire |
| CN115718273A (en) * | 2022-11-18 | 2023-02-28 | 华中科技大学 | Device and method for measuring object magnetic susceptibility based on magnetic induction intensity |
| CN115718273B (en) * | 2022-11-18 | 2024-04-19 | 华中科技大学 | Device for measuring object magnetic susceptibility based on magnetic induction intensity and measuring method thereof |
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| CN109655771B (en) | 2020-05-12 |
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