CN103336151A - Magnetic microscope and measurement method thereof - Google Patents
Magnetic microscope and measurement method thereof Download PDFInfo
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Abstract
The invention discloses a magnetic microscope and a measurement method thereof. The magnetic microscope comprises a microscope support, a probe, a detector, an excitation coil, a scanner, a first signal generator, a first signal detector, a controller and a display, wherein the probe, the detector and the scanner are all mounted on the microscope support; a tested sample is located above the scanner; the probe is located above the tested sample; the first signal generator is used for generating an excitation signal, sends the excitation signal to the excitation coil via the first output end of the first signal generator, and sends the excitation signal to the first signal detector via the second output end of the first signal generator; the controller outputs a voltage control signal to the scanner via the first output end of the controller, as a result, the movement of the scanner is controlled via the voltage control signal. The magnetic microscope is high in detection sensitivity, and good in resolution ratio and imaging effect, can better reflect the surface magnetic field distribution of the tested sample, and can be widely applied to measurement of magnetic material.
Description
Technical Field
The invention relates to the field of microscopes, in particular to a magnetic force microscope and a measuring method thereof.
Background
Magnetic Force Microscopy (MFM) is based on atomic force microscopy, and uses a Magnetic probe to detect the Magnetic interaction between the probe and a sample, and reflects the Magnetic flux leakage and the two-dimensional distribution of the sample surface, which has become an important characterization means for the microstructure and properties of Magnetic materials. At present, imaging by magnetic force microscopy usually takes a two-pass, probe-lift mode of operation (so-called "lift-up mode"): the first scanning step includes measuring interatomic force to obtain surface topography, and the second scanning step includes raising the probe to certain height to make the probe and the sample have no contact and scanning while maintaining the probe-sample interval constant based on the obtained topographic relief information; at this time, the main factor affecting the vibration of the probe is the magnetic force to which the probe is subjected, and thus the second pass reflects the two-dimensional distribution of the remote magnetic force, i.e., the magnetic force microscope image. Due to the large probe-sample spacing for magnetic imaging, the lateral resolution is typically lower than that of atomic force microscopy, which typically achieves a lateral resolution of 30-100 nm. Therefore, the resolution and sensitivity of magnetic force microscopy do not meet the requirements for characterization of materials on the nanometer scale, and are generally not capable of magnetically imaging nanomagnetic particles. In addition, for weak magnetic materials such as superparamagnetic materials, because the magnetic force generated between the materials and the probe is weak, the existing magnetic force microscope is adopted to image the weak magnetic materials, so that the sensitivity is low, and the imaging effect is not ideal.
Disclosure of Invention
In order to solve the above-mentioned technical problems, it is an object of the present invention to provide a magnetic force microscope with high sensitivity and good imaging effect, and it is another object of the present invention to provide a measuring method of a magnetic force microscope with high measuring sensitivity and good imaging effect.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a magnetic force microscope comprises a microscope support, a probe, a detector, an exciting coil, a scanner, a first signal generator, a first signal detector, a controller and a display;
the probe, the detector and the scanner are all arranged on a microscope bracket, the sample to be measured is positioned above the scanner, the probe is positioned above the sample to be measured, and the surface of the probe close to the needle point on one side of the sample to be measured is plated with a layer of magnetic film;
the first signal generator is used for generating an excitation signal and sending the excitation signal to the excitation coil through a first output end of the first signal generator, and sending the excitation signal to the first signal detector through a second output end of the first signal generator;
the controller outputs a voltage control signal to the scanner through a first output end of the controller, so that the movement of the scanner is controlled through the voltage control signal;
the exciting coil generates an alternating magnetic field under the action of an exciting signal so as to modulate the probe and a sample to be detected, the probe is subjected to magnetic force, the probe vibrates under the action of the magnetic force, the detector detects the vibration information of the probe and sends the vibration information to the first signal detector, the first signal detector demodulates the received vibration information of the probe to obtain a position change signal of the probe and sends the position change signal to the controller, and the controller obtains a magnetic image of the sample to be detected according to the received position change signal and outputs the magnetic image to the display through the second output end of the controller.
The probe comprises a probe body, a probe head and a controller, and is characterized by further comprising a vibration exciter, a second signal generator and a second signal detector, wherein the second signal generator is used for generating an alternating excitation electric signal and respectively sending the alternating excitation electric signal to the vibration exciter and the second signal detector, the vibration exciter is used for driving the probe to vibrate according to the received alternating excitation electric signal, the detector is also used for sending detected vibration information of the probe to the second signal detector, and the second signal detector is used for demodulating the received vibration information of the probe, obtaining a position change signal of the probe and sending the position change signal to the controller.
Further, the exciting coil is positioned above, below or on the side surface of the tested sample.
The invention also provides a measuring method of the magnetic microscope, which solves the technical problem, and adopts a first technical scheme that:
a measurement method of a magnetic force microscope, comprising:
carrying out three-dimensional scanning, simultaneously enabling the three-dimensional position change between the detected sample and the probe to occur, further detecting the position change information of the probe and demodulating to obtain a position change signal of the probe, further processing the position change signal of the probe in the three-dimensional scanning process to obtain a surface topography of the detected sample;
and carrying out three-dimensional scanning, simultaneously generating an alternating magnetic field to modulate the detected sample and the probe, so that the probe is subjected to magnetic force, further exciting the probe to enter a local oscillation mode, simultaneously detecting position change information brought by the probe under the action of the alternating magnetic field, demodulating the position change information to obtain a position change signal of the probe, and further processing the position change signal of the probe in the three-dimensional scanning process to obtain a magnetic image of the detected sample.
Further, the position change signal is at least one of a vibration amplitude signal, a phase signal and a frequency signal.
The second technical scheme adopted by the method is as follows:
a measurement method of a magnetic force microscope, comprising:
s1, fixing the tested sample above the scanner, enabling the probe to contact the surface of the tested sample, outputting a voltage control signal by the controller to control the scanner to carry out three-dimensional scanning, driving the tested sample to generate three-dimensional position change under the action of the voltage control signal output by the controller by the scanner during scanning, so as to drive the probe to generate three-dimensional position change, detecting the three-dimensional position change information of the probe by the detector, sending the three-dimensional position change information to the first signal detector for demodulation, obtaining the position change signal of the probe and sending the position change signal to the controller, and processing the position change signal of the probe in the three-dimensional scanning process by the controller to obtain the surface topography of the tested sample;
and S2, outputting a voltage control signal by the controller to control the scanner to enable the probe to withdraw from the surface of the detected sample by a certain distance and control the scanner to perform three-dimensional scanning along the scanning track of the step S1, wherein during scanning, the first signal generator generates an excitation signal and applies the excitation signal to the excitation coil, the excitation coil generates an alternating magnetic field under the action of the excitation signal so as to modulate the probe and the detected sample, the probe is subjected to magnetic force, the probe is further excited to enter a first intrinsic vibration mode, the detector detects vibration information of the probe and sends the vibration information to the first signal detector, the first signal detector demodulates the received vibration information of the probe to obtain a position change signal of the probe and sends the position change signal to the controller, and the controller processes the position change signal of the probe in the three-dimensional scanning process to obtain a magnetic image of the detected sample.
The third technical scheme adopted by the method is as follows:
a measurement method of a magnetic force microscope, comprising:
fixing a sample to be detected above a scanner, enabling a probe to be in contact with the surface of the sample to be detected, outputting a voltage control signal by a controller to control the scanner to carry out three-dimensional scanning, driving the sample to be detected to generate three-dimensional position change under the action of the voltage control signal output by the controller by the scanner during scanning, and driving the probe to generate the three-dimensional position change, and simultaneously generating an excitation signal by a first signal generator and applying the excitation signal to an excitation coil;
the detector detects the three-dimensional position change information of the probe and sends the three-dimensional position change information to the first signal detector for demodulation, the position change signal of the probe is obtained and sent to the controller, and the controller processes the position change signal of the probe in the three-dimensional scanning process to obtain a surface topography of the detected sample;
the exciting coil generates an alternating magnetic field under the action of an exciting signal so as to modulate the probe and a detected sample, the probe is subjected to magnetic force, the probe is further excited to enter a first intrinsic vibration mode, the detector detects vibration information of the probe and sends the vibration information to the first signal detector, the first signal detector demodulates the received vibration information of the probe to obtain a position change signal of the probe and sends the position change signal to the controller, and the controller processes the position change signal of the probe in the three-dimensional scanning process to obtain a magnetic image of the detected sample.
The fourth technical scheme adopted by the method is as follows:
a measurement method of a magnetic force microscope, comprising:
s1, fixing the tested sample above a scanner, outputting a voltage control signal by a controller to control the scanner to carry out three-dimensional scanning, generating an alternating excitation electric signal by a second signal generator and applying the alternating excitation electric signal to a vibration exciter during scanning, exciting the probe to enter an intrinsic vibration mode A by the vibration exciter under the action of the alternating excitation electric signal, detecting vibration information of the probe by a detector, sending the vibration information to a second signal detector for demodulation, obtaining a position change signal of the probe and sending the position change signal to the controller, and processing the position change signal of the probe in the three-dimensional scanning process by the controller to obtain a surface topography map of the tested sample;
and S2, outputting a voltage control signal by the controller to control the scanner to enable the probe to withdraw from the surface of the detected sample by a certain distance and control the scanner to perform three-dimensional scanning along the scanning track of the step S1, wherein during scanning, the first signal generator generates an excitation signal and applies the excitation signal to the excitation coil, the excitation coil generates an alternating magnetic field under the action of the excitation signal so as to modulate the probe and the detected sample, the probe is subjected to magnetic force, the probe is further excited to enter an intrinsic vibration mode B, the detector detects vibration information of the probe and sends the vibration information to the first signal detector, the first signal detector demodulates the received vibration information of the probe to obtain a position change signal of the probe and sends the position change signal to the controller, and the controller processes the position change signal of the probe in the scanning process to obtain a magnetic image of the detected sample.
Further, the eigen-vibration mode a and the eigen-vibration mode B are any one of a plurality of eigen-vibration modes of the probe.
The fifth technical scheme adopted by the method is as follows:
a measurement method of a magnetic force microscope, comprising:
fixing a sample to be detected above a scanner, outputting a voltage control signal by a controller to control the scanner to carry out three-dimensional scanning, wherein during scanning, a second signal generator generates an alternating excitation electric signal and applies the alternating excitation electric signal to a vibration exciter, and meanwhile, a first signal generator generates an excitation signal and applies the excitation signal to an excitation coil;
the vibration exciter excites the probe to enter an intrinsic vibration mode A under the action of an alternating excitation electric signal, the detector detects vibration information of the probe and sends the vibration information to the second signal detector for demodulation, a position change signal of the probe is obtained and sent to the controller, and the controller processes the position change signal of the probe in the three-dimensional scanning process to obtain a surface topography of a detected sample;
the exciting coil generates an alternating magnetic field under the action of an exciting signal so as to modulate the probe and a sample to be detected, the probe is subjected to magnetic force, the probe is further excited to enter an intrinsic vibration mode B, the detector detects vibration information of the probe and sends the vibration information to the first signal detector, the first signal detector demodulates the received vibration information of the probe to obtain a position change signal of the probe and sends the position change signal to the controller, and the controller processes the position change signal of the probe in the scanning process to obtain a magnetic force image of the sample to be detected;
the eigen-vibration mode A is any one of a plurality of eigen-vibration modes of the probe, and the eigen-vibration mode B is any one of a plurality of eigen-vibration modes of the probe except the eigen-vibration mode A.
The invention has the beneficial effects that: the invention relates to a magnetic force microscope, wherein an exciting coil is arranged near a probe and a tested sample, the exciting coil generates an alternating magnetic field under the action of an exciting signal sent by a first signal generator so as to modulate the probe and the tested sample, the probe is subjected to magnetic force, the probe vibrates under the action of the magnetic force, then a detector of the magnetic force microscope can be used for detecting vibration information of the probe and sending the vibration information to a first signal detector, the first signal detector demodulates the received vibration information of the probe to obtain a position change signal of the probe and sends the position change signal to a controller, the controller obtains a magnetic force image of the tested sample according to the received position change signal, the detection sensitivity is high, the resolution is high, the imaging effect is good, and the surface magnetic field distribution of the tested sample can be better measured.
The invention has the following beneficial effects: the invention relates to a measuring method of a magnetic microscope, which leads the three-dimensional position change between a measured sample and a probe, then processes the position change signal of the probe in the three-dimensional scanning process to obtain the surface appearance picture of the measured sample, generates an alternating magnetic field to modulate the measured sample and the probe, leads the probe to be subject to magnetic force, further stimulates the probe to enter a local oscillation mode, then detects the position change information brought by the probe under the action of the alternating magnetic field and processes the position change information to obtain the magnetic image of the measured sample.
Drawings
The invention is further illustrated by the following figures and examples.
FIG. 1 is a block diagram of a first embodiment of a magnetic force microscope of the present invention;
FIG. 2 is a block diagram of a second embodiment of a magnetic force microscope of the present invention;
FIG. 3 is an image obtained by measuring a superparamagnetic nanoparticle sample using a magnetic microscope of the present invention;
FIG. 4 is an image obtained by measuring a ferromagnetic particle sample using the magnetic microscope of the present invention;
FIG. 5 is a graph of the relationship between the excitation signal amplitude versus the probe vibration amplitude when a superparamagnetic nanoparticle sample is measured using a magnetic microscope of the present invention;
FIG. 6 is a graph of the relationship between probe-to-sample spacing versus probe vibration amplitude for superparamagnetic nanoparticle samples measured using a magnetic microscope of the present invention.
Detailed Description
Magnetic force microscope example 1:
referring to fig. 1, a magnetic force microscope includes a microscope stand 1, a probe 2, a probe 3, an exciting coil 5, a scanner 6, a first signal generator 7, a first signal detector 8, a controller 9, and a display 10;
the probe 2, the detector 3 and the scanner 6 are all arranged on the microscope bracket 1, the tested sample 4 is positioned above the scanner 6, the probe 2 is positioned above the tested sample 4, and the surface of the probe 2 close to the needle point of one side of the tested sample 4 is plated with a layer of magnetic film;
a first signal generator 7 for generating an excitation signal and sending the excitation signal to the excitation coil 5 through a first output thereof, while sending the excitation signal to a first signal detector 8 through a second output thereof;
the controller 9 outputs a voltage control signal to the scanner 6 through a first output terminal thereof, thereby controlling the movement of the scanner 6 by the voltage control signal;
the exciting coil 5 generates an alternating magnetic field under the action of an exciting signal to modulate the probe 2 and the sample 4 to be detected, so that the probe 2 is subjected to magnetic force, the probe 2 vibrates under the action of the magnetic force, the detector 3 detects vibration information of the probe 2 and sends the vibration information to the first signal detector 8, the first signal detector 8 demodulates the received vibration information of the probe 2 to obtain a position change signal of the probe 2 and sends the position change signal to the controller 9, and the controller 9 obtains a magnetic image of the sample 4 to be detected according to the received position change signal and outputs the magnetic image to the display 10 through a second output end of the controller 9.
The exciting coil 5 is located above, below or at the side of the measured sample 4, and the direction of the alternating magnetic field generated by the exciting coil can be perpendicular or parallel to the measured sample 4, or form other angles with the measured sample 4.
The tested sample 4 is usually installed on the scanner 6, and the scanner drives the tested sample 4 to generate X, Y, Z three-dimensional position changes for scanning; the sample 4 to be measured may be fixed on the microscope stand 1, the scanner 6 may be installed between the microscope stand 1 and the base of the probe 2, and the probe 2 may be driven by the scanner 6 to generate X, Y, Z three-dimensional position changes for scanning.
The detector 3 adopts a four-quadrant photoelectric converter, and can detect the change of the light spot position caused by the deformation of the probe 2 after being stressed, so as to obtain the position change information of the probe 2.
The excitation signal generated by the first signal generator 7 may be one or more sinusoidal alternating signals, but may also be one or more sinusoidal alternating signals comprising a direct current signal. If the excitation signal generated by the first signal generator 7 comprises a plurality of signals, the first signal detector 8 correspondingly comprises a plurality of detecting units for respectively detecting the vibration amplitude, phase or frequency of the position change information of the probe 2 finally obtained under the action of each signal. When the first signal detector 8 performs demodulation, an effective value detection method or a lock-in amplification method may be used.
To increase the strength of the mechanical vibration response signal of probe 2, the excitation signal is selected to be appropriate so that probe 2 vibrates under the influence of magnetic force at or near the multiple eigen-vibration frequencies of probe 2.
The magnetic force microscope can be used for measuring various magnetic materials, particularly various weak magnetic materials, and after an alternating magnetic field is applied, the magnetic field of a measured sample 4 is increased, so that the magnetic force received by the probe 2 is enhanced, the vibration signal of the probe is changed, and the magnetic force microscope can be used for imaging, so that the microscopic characteristics of the magnetic materials are represented.
Magnetic force microscope example 2:
referring to fig. 2, the magnetic force microscope includes a microscope support 1, a probe 2, a detector 3, an exciting coil 5, a scanner 6, a first signal generator 7, a first signal detector 8, a controller 9, a display 10, a vibration exciter 11, a second signal generator 12, and a second signal detector 13;
the probe 2, the detector 3 and the scanner 6 are all arranged on the microscope bracket 1, the tested sample 4 is positioned above the scanner 6, the probe 2 is positioned above the tested sample 4, and the surface of the probe 2 close to the needle point of one side of the tested sample 4 is plated with a layer of magnetic film;
a first signal generator 7 for generating an excitation signal and sending the excitation signal to the excitation coil 5 through a first output thereof, while sending the excitation signal to a first signal detector 8 through a second output thereof;
the controller 9 outputs a voltage control signal to the scanner 6 through a first output terminal thereof, thereby controlling the movement of the scanner 6 by the voltage control signal;
the second signal generator 12 is configured to generate an alternating excitation electrical signal and send the alternating excitation electrical signal to the vibration exciter 11 and the second signal detector 13, the vibration exciter 11 is configured to drive the probe 2 to vibrate according to the received alternating excitation electrical signal, the detector 3 further sends the detected vibration information of the probe 2 to the second signal detector 13, the second signal detector 13 is configured to demodulate the received vibration information of the probe 2 to obtain a position change signal of the probe 2 and send the position change signal to the controller 9, and the controller 9 obtains a magnetic image of the sample 4 to be detected according to the received position change signal and outputs the magnetic image to the display 10 through a second output end of the magnetic image;
the exciting coil 5 generates an alternating magnetic field under the action of an exciting signal to modulate the probe 2 and the sample 4 to be detected, so that the probe 2 is subjected to magnetic force, the probe 2 vibrates under the action of the magnetic force, the detector 3 detects vibration information of the probe 2 and sends the vibration information to the first signal detector 8, the first signal detector 8 demodulates the received vibration information of the probe 2 to obtain a position change signal of the probe 2 and sends the position change signal to the controller 9, and the controller 9 obtains a magnetic image of the sample 4 to be detected according to the received position change signal and outputs the magnetic image to the display 10 through a second output end of the controller 9.
Because the frequency of the position change signal of the probe 2 under the action of the alternating magnetic field is high, and can be clearly distinguished from the position change signal of the probe 2 under the action of the alternating excitation electric signal, the controller 9 processes the position change signals sent by the first signal detector 8 and the second signal detector 13 respectively in the data processing process, and further obtains the surface topography map and the magnetic force image of the detected sample 4 respectively.
The exciting coil 5 is located above, below or at the side of the measured sample 4, and the direction of the alternating magnetic field generated by the exciting coil can be perpendicular or parallel to the measured sample 4, or form other angles with the measured sample 4.
The tested sample 4 is usually installed on the scanner 6, and the scanner drives the tested sample 4 to generate X, Y, Z three-dimensional position changes for scanning; the sample 4 to be measured may be fixed on the microscope stand 1, the scanner 6 may be installed between the microscope stand 1 and the base of the probe 2, and the probe 2 may be driven by the scanner 6 to generate X, Y, Z three-dimensional position changes for scanning.
The detector 3 adopts a four-quadrant photoelectric converter, and can detect the change of the light spot position caused by the deformation of the probe 2 after being stressed, so as to obtain the position change information of the probe 2.
The excitation signal generated by the first signal generator 7 may be one or more sinusoidal alternating signals, but may also be one or more sinusoidal alternating signals comprising a direct current signal. If the excitation signal generated by the first signal generator 7 comprises a plurality of signals, the first signal detector 8 correspondingly comprises a plurality of detecting units for respectively detecting the vibration amplitude, phase or frequency of the position change information of the probe 2 finally obtained under the action of each signal. When the first signal detector 8 performs demodulation, an effective value detection method or a lock-in amplification method may be used.
To increase the strength of the mechanical vibration response signal of probe 2, the excitation signal is selected to be appropriate so that probe 2 vibrates under the influence of magnetic force at or near the multiple eigen-vibration frequencies of probe 2.
The magnetic force microscope can be used for measuring various magnetic materials, particularly various weak magnetic materials, and after an alternating magnetic field is applied, the magnetic field of a measured sample 4 is increased, so that the magnetic force received by the probe 2 is enhanced, the vibration signal of the probe is changed, and the magnetic force microscope can be used for imaging, so that the microscopic characteristics of the magnetic materials are represented.
The magnetic microscopes in embodiment 1 and embodiment 2 each include an exciting coil 5 for generating an alternating magnetic field, and when the magnetic microscope is in operation, the magnetic field strength of the sample 4 to be measured can be increased, thereby realizing two-dimensional imaging.
The invention also provides a measuring method of the magnetic microscope, which comprises the following steps:
a morphology imaging step: three-dimensional scanning is carried out, meanwhile, three-dimensional position change occurs between the detected sample 4 and the probe 2, further, position change information of the probe 2 is detected and demodulated, then, a position change signal of the probe 2 is obtained, further, the position change signal of the probe 2 in the three-dimensional scanning process is processed, and then, a surface topography of the detected sample 4 is obtained;
magnetic imaging: and carrying out three-dimensional scanning, simultaneously generating an alternating magnetic field to modulate the detected sample 4 and the probe 2, so that the probe 2 is subjected to magnetic force, further exciting the probe 2 to enter a local oscillation mode, simultaneously detecting position change information brought by the probe 2 under the action of the alternating magnetic field, demodulating the position change information to obtain a position change signal of the probe 2, further processing the position change signal of the probe 2 in the three-dimensional scanning process, and then obtaining a magnetic image of the detected sample 4.
The position change signal is at least one of a vibration amplitude signal, a phase signal and a frequency signal.
In all embodiments of the present invention, the three-dimensional position change refers to X, Y, Z three-dimensional position change in three directions.
Measurement method example 1:
a measurement method of a magnetic force microscope, comprising:
s1, fixing the tested sample 4 above the scanner 6, and making the probe 2 contact with the surface of the tested sample 4, the controller 9 outputting a voltage control signal to control the scanner 6 to perform three-dimensional scanning, during scanning, the scanner 6 driving the tested sample 4 to generate three-dimensional position change under the action of the voltage control signal output by the controller 9, so as to drive the probe 2 to generate three-dimensional position change, the detector 3 detecting the three-dimensional position change information of the probe 2 and sending the information to the first signal detector 8 for demodulation to obtain the position change signal of the probe 2 and sending the signal to the controller 9, the controller 9 processing the position change signal of the probe 2 in the three-dimensional scanning process to obtain the surface topography map of the tested sample 4;
s2, the controller 9 outputs voltage control signal to control the scanner 6 to make the probe 2 withdraw from the surface of the tested sample 4 for a certain distance and control the scanner 6 to carry out three-dimensional scanning along the scanning track of the step S1, the first signal generator 7 generates an excitation signal and applies the excitation signal to the excitation coil 5, the excitation coil 5 generates an alternating magnetic field under the action of the excitation signal so as to modulate the probe 2 and the tested sample 4, the probe 2 is subjected to magnetic force, and then the probe 2 is excited to enter a first eigen-vibration mode, the detector 3 detects the vibration information of the probe 2 and sends the vibration information to the first signal detector 8, after the first signal detector 8 demodulates the received vibration information of the probe 2, and obtaining a position change signal of the probe 2 and sending the position change signal to the controller 9, wherein the controller 9 processes the position change signal of the probe 2 in the three-dimensional scanning process to obtain a magnetic image of the detected sample 4. In this step, the scanner 6 is controlled to make the probe 2 leave a certain distance from the surface of the sample 4 to be measured, that is, the scanner 6 is controlled to raise a certain height in the Z direction to make the probe 2 not contact with the sample 4 to be measured.
Step S1 is a topography imaging step, and step S2 is a magnetomechanical imaging step. In step S1, topography imaging is performed in the contact mode, and in step S2, magnetic force imaging is performed in the lift-off mode. In this embodiment, the measurement is performed by two scanning passes.
Measurement method example 2:
a measurement method of a magnetic force microscope, comprising:
fixing a sample 4 to be detected above a scanner 6, enabling a probe 2 to be in contact with the surface of the sample 4 to be detected, outputting a voltage control signal by a controller 9 to control the scanner 6 to carry out three-dimensional scanning, wherein during scanning, the scanner 6 drives the sample 4 to be detected to generate three-dimensional position change under the action of the voltage control signal output by the controller 9, so as to drive the probe 2 to generate three-dimensional position change, and meanwhile, a first signal generator 7 generates an excitation signal and applies the excitation signal to an excitation coil 5;
the detector 3 detects the three-dimensional position change information of the probe 2 and sends the three-dimensional position change information to the first signal detector 8 for demodulation, so that a position change signal of the probe 2 is obtained and sent to the controller 9, and the controller 9 processes the position change signal of the probe 2 in the three-dimensional scanning process to obtain a surface topography of the detected sample 4;
the exciting coil 5 generates an alternating magnetic field under the action of an exciting signal to modulate the probe 2 and the sample 4 to be detected, so that the probe 2 is subjected to magnetic force, the probe 2 is further excited to enter a first eigen-vibration mode, the detector 3 detects vibration information of the probe 2 and sends the vibration information to the first signal detector 8, the first signal detector 8 demodulates the received vibration information of the probe 2 to obtain a position change signal of the probe 2 and sends the position change signal to the controller 9, and the controller 9 processes the position change signal of the probe 2 in the three-dimensional scanning process to obtain a magnetic force image of the sample 4 to be detected.
The difference between this embodiment and the measurement method embodiment 1 is that this embodiment adopts a one-pass scanning mode for measurement, and the topography imaging step and the magnetometric imaging step are performed simultaneously.
Measurement method example 3:
a measurement method of a magnetic force microscope, comprising:
s1, fixing the sample 4 to be measured above the scanner 6, outputting a voltage control signal by the controller 9 to control the scanner 6 to perform three-dimensional scanning, generating an alternating excitation electric signal by the second signal generator 12 and applying the alternating excitation electric signal to the vibration exciter 11 during scanning, exciting the probe 2 into an intrinsic vibration mode A by the vibration exciter 11 under the action of the alternating excitation electric signal, detecting vibration information of the probe 2 by the detector 3 and sending the vibration information to the second signal detector 13 for demodulation to obtain a position change signal of the probe 2 and sending the position change signal to the controller 9, and processing the position change signal of the probe 2 in the three-dimensional scanning process by the controller 9 to obtain a surface topography map of the sample 4 to be measured;
s2, the controller 9 outputs voltage control signal to control the scanner 6 to make the probe 2 withdraw from the surface of the tested sample 4 for a certain distance and control the scanner 6 to carry out three-dimensional scanning along the scanning track of the step S1, the first signal generator 7 generates an excitation signal and applies the excitation signal to the excitation coil 5, the excitation coil 5 generates an alternating magnetic field under the action of the excitation signal so as to modulate the probe 2 and the tested sample 4, the probe 2 is subjected to magnetic force, and then the probe 2 is excited to enter the eigen-vibration mode B, the detector 3 detects the vibration information of the probe 2 and sends the vibration information to the first signal detector 8, after the first signal detector 8 demodulates the received vibration information of the probe 2, and obtaining a position change signal of the probe 2 and sending the position change signal to the controller 9, wherein the controller 9 processes the position change signal of the probe 2 in the scanning process to obtain a magnetic image of the tested sample 4. In this step, the scanner 6 is controlled to make the probe 2 leave a certain distance from the surface of the sample 4 to be measured, that is, the scanner 6 is controlled to raise a certain height in the Z direction to make the probe 2 not contact with the sample 4 to be measured.
Step S1 is a topography imaging step, and step S2 is a magnetomechanical imaging step. In this embodiment, the measurement is performed by using two scanning passes, the eigen-vibration mode a and the eigen-vibration mode B are both any one of the multiple eigen-vibration modes of the probe 2, and the frequency of the eigen-vibration mode a may be the same as or different from the frequency of the eigen-vibration mode B. During the measurement, the probe 2 and the sample 4 may not be in contact at all, or may be in contact intermittently, and in step S2, the second signal generator 12 may or may not continue to apply the alternating excitation electrical signal to the vibration exciter 11.
Specifically, the eigen-vibration mode a adopts a first eigen-vibration mode of the probe 2, and the eigen-vibration mode B adopts a second eigen-vibration mode of the probe 2, that is, the first eigen-vibration mode of the probe 2 is adopted for topographic imaging, that is, the second eigen-vibration mode of the probe 2 is adopted for magnetic imaging.
(A) Fig. 3 shows a surface topography and a magnetic topography obtained by measuring a superparamagnetic nanoparticle sample by using the method of the present embodiment, where fig. 3 (a) is a surface topography of a superparamagnetic nanoparticle sample, fig. 3 (b) is a magnetic image of the superparamagnetic nanoparticle sample expressed by a phase signal, fig. 3 (c) is a magnetic image of the superparamagnetic nanoparticle sample expressed by an amplitude signal, and the superparamagnetic nanoparticle sample is a biological protein containing superparamagnetic nanoparticles having a diameter of about 50 nm. From the comparison of the obtained surface topography map and the magnetic force image, it can be seen that the magnetic force image obtained by the second eigen-vibration mode (including the magnetic force image represented by the phase signal and the magnetic force image represented by the vibration amplitude signal) has different characteristics from the surface topography map and has a higher resolution, reflecting the distribution of superparamagnetic nanoparticles. Fig. 5 is a graph of the relationship between the amplitude of the excitation signal and the amplitude of the vibration of the probe during the measurement, and it can be seen from the graph of fig. 5 that the amplitude signal of the vibration of the probe 2 is enhanced with the enhancement of the excitation signal, and from the comparison of the obtained graphs, when the tip of the probe 2 is located near the position of the superparamagnetic particle (i.e., in the case of a superparamagnetic nanoparticle sample), the amplitude signal of the probe 2 in the second eigenmode of vibration is enhanced, indicating that the presence of the superparamagnetic nanoparticle sample enhances the magnetic induction. Therefore, the magnetic force microscope of the invention can accurately obtain the distribution diagram of the superparamagnetic nano-particle sample, which can not be realized by the existing magnetic force microscope. Fig. 6 is a curve of the relationship between the distance between the probe and the sample and the vibration amplitude of the probe in the measuring process, and it can be seen from the curve in fig. 6 that the force applied to the probe 2 is reduced along with the increase of the distance between the probe and the sample, and the consistent magnetic force is a characteristic of long-range acting force, and the correctness of the measuring method is also verified.
The working principle of the method for measuring superparamagnetic nanoparticles (sample 4) is as follows:
the exciting coil 5 continuously generates an alternating magnetic field (the alternating magnetic field is approximately uniformly distributed and does not influence magnetic imaging), and the probe 2 is acted by a magnetic force Fm under the action of the continuous alternating magnetic field of the exciting coil 5, so that mechanical vibration with a vibration amplitude A is generated; meanwhile, the superparamagnetic nanoparticles generate an induced magnetic field Hs under the action of the alternating magnetic field sustained by the exciting coil 5, and the induced magnetic field Hs exerts a force on the probe 2, so that the probe 2 is caused to generate vibration amplitude change and phase change. Therefore, the superparamagnetic nanoparticle sample can be imaged separately with the vibration amplitude signal and the phase signal of the vibration of the probe 2.
The magnetic tip of the probe 2 is approximated to point magnetic charge, and the expression of the magnetic force applied to the tip of the probe 2 is as follows:
wherein,the tip of the probe 2 is subjected to a magnetic force,
is the tip local magnetic moment of the probe 2,
a magnetic field generated by superparamagnetic nanoparticles.
In the absence of an applied magnetic field, the magnetic field generated by the superparamagnetic nanoparticles at the experimental temperature
Substantially zero and thus the magnetic probe cannot detect the magnetic force. Moreover, due to the particularity of the magnetization process of superparamagnetic nanoparticlesIt is also impossible to generate an effective magnetic field by using the conventional magnetic microscope imaging method after magnetization by an external magnetic field.
When the magnetic force microscope is used for measurement, under the action of a continuous alternating magnetic field, the expression of the magnetic force borne by the needle point of the probe 2 is as follows:
wherein,
the tip of the probe 2 is subjected to a magnetic force,
is the tip local magnetic moment of the probe 2,the magnetic field generated by the superparamagnetic nanoparticles,
is an induction magnetic field generated by the superparamagnetic nano-particles under the action of an alternating magnetic field.
The probe 2 vibrates under the excitation of magnetic force, and the vibration amplitude thereof is expressed as:
wherein,A 0is the amplitude of the microcantilever of probe 2,Qk is the coefficient of elasticity of the cantilever, mpThe magnetic moment of the superparamagnetic nanoparticle.
In the present invention, although the tip of the probe 2 is actually subjected to the magnetic force to vibrate the entire probe 2, the probe 2 may be considered to be subjected to the magnetic force in a general way, and thus, in the description, the two are not distinguished in detail except for the principle description.
(B) Fig. 4 shows a surface topography map and a magnetometric map obtained by measuring a ferromagnetic nanoparticle sample by using the method of the present embodiment, where fig. 4 (a) is the surface topography map of the ferromagnetic nanoparticle sample, fig. 4 (b) is a magnetic force image of the ferromagnetic nanoparticle sample represented by a phase signal, and fig. 4 (c) is a magnetic force image of the ferromagnetic nanoparticle sample represented by an amplitude signal. From the comparison of the obtained surface topography map and the magnetic force image, it can be seen that the magnetic force image obtained by the second eigen-vibration mode (including the magnetic force image represented by the phase signal and the magnetic force image represented by the vibration amplitude signal) has different characteristics from the surface topography map and has a higher resolution, reflecting the distribution of the ferromagnetic nanoparticle sample.
The principle of the method for measuring the ferromagnetic nanoparticle sample is as follows: the exciting coil 5 continuously generates an alternating magnetic field (the alternating magnetic field is approximately uniformly distributed and does not influence magnetic imaging), and the probe 2 is acted by a magnetic force F under the action of the continuous alternating magnetic field of the exciting coil 5, so that mechanical vibration with a vibration amplitude A is generated; meanwhile, the ferromagnetic nanoparticle sample subjects the probe 2 to an additional magnetic force F 'under the action of the alternating magnetic field sustained by the exciting coil 5, so that the vibration amplitude of the probe 2 is changed to a'. Therefore, the ferromagnetic nanoparticle sample can be imaged with the vibration amplitude signal and the phase signal of the vibration of the probe 2, respectively. As can be seen from fig. 4, the method can improve the resolution of the magnetic image of the ferromagnetic nanoparticle sample, and solve the problem of insufficient sensitivity when the conventional magnetic microscope images the ferromagnetic nanoparticle sample.
Measurement method example 4:
a measurement method of a magnetic force microscope, comprising:
fixing the tested sample 4 above the scanner 6, outputting a voltage control signal by the controller 9 to control the scanner 6 to perform three-dimensional scanning, wherein during scanning, the second signal generator 12 generates an alternating excitation electric signal and applies the alternating excitation electric signal to the vibration exciter 11, and the first signal generator 7 generates an excitation signal and applies the excitation signal to the excitation coil 5;
the vibration exciter 11 excites the probe 2 to enter an intrinsic vibration mode A under the action of an alternating excitation electric signal, the detector 3 detects vibration information of the probe 2 and sends the vibration information to the second signal detector 13 for demodulation, a position change signal of the probe 2 is obtained and sent to the controller 9, and the controller 9 processes the position change signal of the probe 2 in the three-dimensional scanning process to obtain a surface topography of the sample 4 to be detected;
the exciting coil 5 generates an alternating magnetic field under the action of an exciting signal so as to modulate the probe 2 and the sample 4 to be detected, so that the probe 2 is subjected to magnetic force, the probe 2 is further excited to enter an intrinsic vibration mode B, the detector 3 detects vibration information of the probe 2 and sends the vibration information to the first signal detector 8, the first signal detector 8 demodulates the received vibration information of the probe 2 to obtain a position change signal of the probe 2 and sends the position change signal to the controller 9, and the controller 9 processes the position change signal of the probe 2 in the scanning process to obtain a magnetic force image of the sample 4 to be detected;
eigenmode a is any one of a plurality of eigenmodes of probe 2, and eigenmode B is any one of a plurality of eigenmodes of probe 2 other than eigenmode a.
The embodiment is different from the measurement method embodiment 3 in that the measurement is performed by one-pass scanning, and the topography imaging step and the magnetometric imaging step are performed simultaneously. The eigen-vibration mode a and the eigen-vibration mode B are each any one of a plurality of eigen-vibration modes of the probe 2, and the frequency of the eigen-vibration mode a may be the same as or different from the frequency of the eigen-vibration mode B. During measurement, the probe 2 and the sample 4 to be measured may not be in contact at all, or may be in contact intermittently.
In all embodiments of the present invention, the exciting coil 5 continuously generates an alternating magnetic field, which acts on the sample 4 and the probe 2 to be measured, and finally vibrates the probe 2, so that the vibration amplitude, phase or frequency changes, therefore, it can be regarded as that the exciting coil 5 modulates the sample 4 and the probe 2 to be measured, and therefore, the vibration amplitude signal, phase signal or frequency signal when the probe 2 vibrates can be detected and obtained through demodulation by the first signal detector 8, and the signals are used for magnetic force imaging. In the magnetic microscope of fig. 2, the probe 2 is vibrated by the exciter 11, so that the amplitude, phase or frequency of the vibration is changed, and it can also be regarded as modulation, so that the modulation can be performed by the second signal detector 13, so as to obtain a vibration amplitude signal, a phase signal or a frequency signal when the probe 2 is vibrated, and use these signals for topography imaging.
While the preferred embodiments of the present invention have been illustrated and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A magnetic force microscope is characterized by comprising a microscope support (1), a probe (2), a detector (3), an exciting coil (5), a scanner (6), a first signal generator (7), a first signal detector (8), a controller (9) and a display (10);
the probe (2), the detector (3) and the scanner (6) are all arranged on the microscope support (1), the sample (4) to be detected is positioned above the scanner (6), the probe (2) is positioned above the sample (4) to be detected, and a magnetic film is plated on the surface of the probe tip, close to one side of the sample (4) to be detected, of the probe (2);
the first signal generator (7) is used for generating an excitation signal and sending the excitation signal to the excitation coil (5) through a first output end of the first signal generator, and sending the excitation signal to the first signal detector (8) through a second output end of the first signal generator;
the controller (9) outputs a voltage control signal to the scanner (6) through a first output terminal thereof, so that the movement of the scanner (6) is controlled by the voltage control signal;
the excitation coil (5) generates an alternating magnetic field under the action of an excitation signal so as to modulate the probe (2) and the sample (4) to be detected, the probe (2) is subjected to magnetic force, the probe (2) vibrates under the action of the magnetic force, the detector (3) detects vibration information of the probe (2) and sends the vibration information to the first signal detector (8), the first signal detector (8) demodulates the received vibration information of the probe (2) to obtain a position change signal of the probe (2) and sends the position change signal to the controller (9), and the controller (9) obtains a magnetic image of the sample (4) to be detected according to the received position change signal and outputs the magnetic image to the display (10) through a second output end of the controller.
2. A magnetic force microscope according to claim 1, characterized by further comprising an exciter (11), a second signal generator (12) and a second signal detector (13), wherein the second signal generator (12) is configured to generate an alternating excitation electrical signal and send the alternating excitation electrical signal to the exciter (11) and the second signal detector (13), the exciter (11) is configured to drive the probe (2) to vibrate according to the received alternating excitation electrical signal, the probe (3) further sends the detected vibration information of the probe (2) to the second signal detector (13), and the second signal detector (13) is configured to demodulate the received vibration information of the probe (2) to obtain a position change signal of the probe (2) and send the position change signal to the controller (9).
3. A magnetic force microscope according to claim 1, characterized in that the excitation coil (5) is located above, below or to the side of the sample (4) to be measured.
4. A method of measurement in a magnetic force microscope, comprising:
three-dimensional scanning is carried out, meanwhile, three-dimensional position change is carried out between a sample (4) to be detected and the probe (2), further, position change information of the probe (2) is detected and demodulated, then, a position change signal of the probe (2) is obtained, further, the position change signal of the probe (2) in the three-dimensional scanning process is processed, and then, a surface topography of the sample (4) to be detected is obtained;
the method comprises the steps of carrying out three-dimensional scanning, simultaneously generating an alternating magnetic field to modulate a detected sample (4) and a probe (2), enabling the probe (2) to be subjected to magnetic force, further exciting the probe (2) to enter a local oscillation mode, simultaneously detecting position change information brought by the probe (2) under the action of the alternating magnetic field, demodulating the position change information to obtain a position change signal of the probe (2), further processing the position change signal of the probe (2) in the three-dimensional scanning process, and then obtaining a magnetic force image of the detected sample (4).
5. The method of claim 4, wherein the position variation signal is at least one of a vibration amplitude signal, a phase signal and a frequency signal.
6. A method of measurement in a magnetic force microscope, comprising:
s1, fixing a detected sample (4) above a scanner (6), enabling a probe (2) to be in contact with the surface of the detected sample (4), outputting a voltage control signal by a controller (9) to control the scanner (6) to perform three-dimensional scanning, driving the detected sample (4) to generate three-dimensional position change under the action of the voltage control signal output by the controller (9) by the scanner (6) during scanning, so as to drive the probe (2) to generate three-dimensional position change, detecting the three-dimensional position change information of the probe (2) by a detector (3) and sending the three-dimensional position change information to a first signal detector (8) for demodulation, obtaining a position change signal of the probe (2) and sending the position change signal to the controller (9), and processing the position change signal of the probe (2) in the three-dimensional scanning process by the controller (9) to obtain a surface topography map of the detected sample (4);
s2, a controller (9) outputs a voltage control signal to control a scanner (6) to enable a probe (2) to withdraw from the surface of a detected sample (4) for a certain distance and control the scanner (6) to conduct three-dimensional scanning along the scanning track of the step S1, during scanning, a first signal generator (7) generates an excitation signal and applies the excitation signal to an excitation coil (5), the excitation coil (5) generates an alternating magnetic field under the action of the excitation signal to modulate the probe (2) and the detected sample (4), the probe (2) is subjected to magnetic force, the probe (2) is further excited to enter a first intrinsic vibration mode, a detector (3) detects vibration information of the probe (2) and sends the vibration information to a first signal detector (8), the first signal detector (8) demodulates the received vibration information of the probe (2) to obtain a position change signal of the probe (2) and sends the position change signal to the controller (9), the controller (9) processes the position change signal of the probe (2) in the three-dimensional scanning process to obtain a magnetic image of the detected sample (4).
7. A method of measurement in a magnetic force microscope, comprising:
fixing a tested sample (4) above a scanner (6), enabling a probe (2) to be in contact with the surface of the tested sample (4), outputting a voltage control signal by a controller (9) to control the scanner (6) to carry out three-dimensional scanning, and during scanning, driving the tested sample (4) to generate three-dimensional position change by the scanner (6) under the action of the voltage control signal output by the controller (9), so as to drive the probe (2) to generate the three-dimensional position change, and meanwhile, generating an excitation signal by a first signal generator (7) and applying the excitation signal to an excitation coil (5);
the detector (3) detects the three-dimensional position change information of the probe (2) and sends the three-dimensional position change information to the first signal detector (8) for demodulation, then the position change signal of the probe (2) is obtained and sent to the controller (9), and the controller (9) processes the position change signal of the probe (2) in the three-dimensional scanning process to obtain a surface topography map of the detected sample (4);
the exciting coil (5) generates an alternating magnetic field under the action of an exciting signal so as to modulate the probe (2) and the detected sample (4), the probe (2) is subjected to magnetic force, the probe (2) is further excited to enter a first eigen-vibration mode, the detector (3) detects vibration information of the probe (2) and sends the vibration information to the first signal detector (8), the first signal detector (8) demodulates the received vibration information of the probe (2) to obtain a position change signal of the probe (2) and sends the position change signal to the controller (9), and the controller (9) processes the position change signal of the probe (2) in the three-dimensional scanning process to obtain a magnetic force image of the detected sample (4).
8. A method of measurement in a magnetic force microscope, comprising:
s1, fixing a sample to be detected (4) above a scanner (6), outputting a voltage control signal by a controller (9) to control the scanner (6) to perform three-dimensional scanning, wherein during scanning, a second signal generator (12) generates an alternating excitation electric signal and applies the alternating excitation electric signal to a vibration exciter (11), the vibration exciter (11) excites a probe (2) to enter an intrinsic vibration mode A under the action of the alternating excitation electric signal, a detector (3) detects vibration information of the probe (2) and sends the vibration information to a second signal detector (13) for demodulation to obtain a position change signal of the probe (2) and send the position change signal to the controller (9), and the controller (9) processes the position change signal of the probe (2) in the three-dimensional scanning process to obtain a surface topography map of the sample to be detected (4);
s2, a controller (9) outputs a voltage control signal to control a scanner (6) to enable a probe (2) to withdraw from the surface of a detected sample (4) for a certain distance and control the scanner (6) to conduct three-dimensional scanning along the scanning track of the step S1, during scanning, a first signal generator (7) generates an excitation signal and applies the excitation signal to an excitation coil (5), the excitation coil (5) generates an alternating magnetic field under the action of the excitation signal to modulate the probe (2) and the detected sample (4), the probe (2) is subjected to magnetic force, the probe (2) is further excited to enter an intrinsic vibration mode B, a detector (3) detects vibration information of the probe (2) and sends the vibration information to a first signal detector (8), the first signal detector (8) demodulates the received vibration information of the probe (2) to obtain a position change signal of the probe (2) and sends the position change signal to the controller (9), the controller (9) processes the position change signal of the probe (2) in the scanning process to obtain a magnetic image of the tested sample (4).
9. A method of measurement for a magnetic force microscope according to claim 8 wherein the eigenmode A and eigenmode B are each any of a plurality of eigenmodes of the probe (2).
10. A method of measurement in a magnetic force microscope, comprising:
fixing a sample (4) to be detected above a scanner (6), outputting a voltage control signal by a controller (9) to control the scanner (6) to carry out three-dimensional scanning, wherein during scanning, a second signal generator (12) generates an alternating excitation electric signal and applies the alternating excitation electric signal to a vibration exciter (11), and simultaneously a first signal generator (7) generates an excitation signal and applies the excitation signal to an excitation coil (5);
the vibration exciter (11) excites the probe (2) to enter an intrinsic vibration mode A under the action of an alternating excitation electric signal, the detector (3) detects vibration information of the probe (2) and sends the vibration information to the second signal detector (13) for demodulation, a position change signal of the probe (2) is obtained and sent to the controller (9), and the controller (9) processes the position change signal of the probe (2) in the three-dimensional scanning process to obtain a surface topography map of the detected sample (4);
the exciting coil (5) generates an alternating magnetic field under the action of an exciting signal so as to modulate the probe (2) and the detected sample (4), the probe (2) is subjected to magnetic force, the probe (2) is further excited to enter an intrinsic vibration mode B, the detector (3) detects vibration information of the probe (2) and sends the vibration information to the first signal detector (8), the first signal detector (8) demodulates the received vibration information of the probe (2) to obtain a position change signal of the probe (2) and sends the position change signal to the controller (9), and the controller (9) processes the position change signal of the probe (2) in the scanning process to obtain a magnetic force image of the detected sample (4);
the eigen-vibration mode A is any one of a plurality of eigen-vibration modes of the probe (2), and the eigen-vibration mode B is any one of a plurality of eigen-vibration modes of the probe (2) except the eigen-vibration mode A.
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Application publication date: 20131002 |