Disclosure of Invention
Aiming at the problems that the existing two working mode combination modes cannot be characterized in situ and cannot objectively reflect the real relationship of interaction between physical fields at the same moment, the invention provides an atomic force microscope control method for cooperative work of a non-contact mode and a contact mode.
The invention relates to an atomic force microscope control method for cooperative work of a non-contact mode and a contact mode, wherein a cantilever beam of an atomic force microscope drives a probe to be above a sample, and the method comprises the following steps:
S1, a cantilever beam of an atomic force microscope drives a probe to be at a set distance above a sample, an excitation sensor excites the cantilever beam to drive the probe to resonate, and long-range performance is tested; the method can also be switched from one non-contact mode to another non-contact mode, so that the other non-contact mode sensor is excited to test the long-range performance.
S2, the excitation sensor stops excitation, the sample is driven to move upwards or the probe is driven to move downwards so that the surface of the sample is closely attached to the probe above the sample, the excitation sensor generates an excitation signal to act on the sample and/or the probe, and the physicochemical characteristics of the sample are tested; it is also possible to switch from one contact mode to another, so that the excitation sensor of the other contact mode generates an excitation signal to test the physicochemical properties of the sample.
S3, the excitation sensor stops generating an excitation signal, and simultaneously the sample or the probe returns to the original position, and the sample or the probe is driven to move so that the cantilever beam of the atomic force microscope drives the probe to move to the next test position point, and the S1 is shifted.
The invention can also be in a contact mode and then in a non-contact mode, and specifically comprises the following steps:
S1, a cantilever beam of an atomic force microscope drives a probe to be at a set distance above a sample, the sample is driven to move upwards or the probe is driven to move downwards so as to enable the surface of the sample to be closely attached to the probe above, an excitation sensor generates an excitation signal to act on the sample and/or the probe, and the physicochemical characteristics of the sample are tested; it is also possible to switch from one contact mode to another, so that the excitation sensor of the other contact mode generates an excitation signal to test the physicochemical properties of the sample.
S2, the excitation sensor stops generating excitation signals, and simultaneously the sample or the probe returns to the original position, the excitation sensor excites the cantilever beam to drive the probe to resonate, and the long-range performance is tested; it is also possible to switch from one non-contact mode to another non-contact mode, causing the other non-contact mode sensor to excite, imaging the sample surface.
S3, the excitation sensor stops excitation, the sample or the probe is driven to move, so that the cantilever beam of the atomic force microscope drives the probe to move to the next test position point, and S1 is carried out.
Preferably, the physicochemical properties include the morphology, mechanical properties, thermal properties, electrical properties, optical properties, magnetic properties, piezoelectric properties, and electrochemical properties of the sample.
Preferably, the excitation signal includes an electrical signal, a magnetic signal, a thermal signal, an optical signal, and a mechanical signal.
Preferably, the testing long-range performance includes: imaging the morphology of the sample, magnetic field force imaging and electrostatic force imaging.
The invention has the beneficial effects that the in-situ rapid switching method is adopted, and the vertical distance between the probe and the sample is adjusted on the same position point to sequentially realize in-situ measurement of short-range and long-range performances, so that the atomic force microscope can use a contact mode to measure the physicochemical characteristics of the sample while scanning in a non-contact mode. The invention has instantaneity for representing various physical and chemical properties, and the obtained test performance can objectively reflect the real relationship of interaction between physical fields at the same moment. The invention can solve the problem that the non-contact mode and the contact mode of the atomic force microscope are incompatible.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
The invention is further described below with reference to the drawings and specific examples, which are not intended to be limiting.
The application relates to an atomic force microscope control method for cooperative work of a non-contact mode and a contact mode, wherein a cantilever beam of an atomic force microscope drives a probe to be above a sample, and the atomic force microscope control method comprises the following steps:
step 1, a cantilever beam of an atomic force microscope drives a probe to be at a set distance above a sample, and an excitation sensor excites the cantilever beam to drive the probe to resonate, so that the long-range performance is tested;
Step 2, the excitation sensor stops excitation, the sample is driven to move upwards or the probe is driven to move downwards so that the surface of the sample is closely attached to the probe above, the excitation sensor generates an excitation signal to act on the sample and/or the probe, and the physicochemical characteristics of the sample are tested;
And 3, stopping generating an excitation signal by the excitation sensor, returning the sample or the probe to the original position, driving the sample or the probe to move so that the cantilever beam of the atomic force microscope drives the probe to move to the next test position point, and turning to the step 1.
In the application, when testing the same test position point, the non-contact mode test is firstly carried out by utilizing the time-sharing excitation control method, then the contact mode test is carried out, then the non-contact mode test is carried out by moving to the next test position point, and the in-situ measurement of the long-distance and short-distance performance is sequentially realized by adjusting the vertical distance between the probe and the sample at the same test position point, so that the atomic force microscope can use the contact mode to measure the physicochemical characteristics of the sample while scanning in the non-contact mode. The non-contact mode and the contact mode parameters are collected and performance is characterized on the determined test position point, so that the performance of the sample such as force, heat, electricity, light and magnetism at the same test position point can be truly characterized.
In the application, when testing the same test position point, the contact mode test is executed firstly, then the non-contact mode test is executed, then the contact mode test is executed after moving to the next test position point, and the normal distance between the probe and the sample is adjusted on the same test position point to sequentially realize the in-situ measurement of the process and the remote performance, so that the atomic force microscope can use the non-contact mode to measure the physicochemical characteristics of the sample while scanning in the contact mode.
The switching of the operation mode in the present application includes switching from the non-contact mode to the contact mode, switching from the contact mode to the non-contact mode, and also switching from the non-contact mode to another non-contact mode or switching from the contact mode to another contact mode. The combined application of the two scanning techniques of non-contact mode and contact mode is any permutation and combination of any number of non-contact modes and any number of contact modes. For example, a non-contact mode-non-contact mode, or a contact mode-non-contact mode, or the like. After specific functions are assigned to the atomic force microscope operating mode, specific switching schemes are illustrated: imaging mode (non-contact mode) -conductive force mode (contact mode) -electrostatic force mode (non-contact mode) -imaging mode (non-contact mode).
Physicochemical properties in the present application include morphology, mechanical properties, thermal properties, electrical properties, optical properties, magnetic properties, piezoelectric properties, and electrochemical properties of the sample.
The excitation signal in the present application includes an electrical signal, a magnetic signal, a thermal signal, an optical signal, and a mechanical signal.
The application tests long-range performance including: imaging the morphology of the sample, magnetic field force imaging and electrostatic force imaging.
The first embodiment is as follows:
The hardware structure of this embodiment is shown in fig. 2, and the cantilever beam of the atomic force microscope drives the probe to be above the sample 3, and the sample 3 is placed on the piezoelectric scanning tube 4; the hardware structure of the embodiment also comprises an excitation sensor for exciting the cantilever beam to drive the probe to resonate, a position sensor for driving the piezoelectric scanning tube to move upwards, an excitation sensor in a contact mode, an excitation sensor in a non-contact mode and a sensor for driving the piezoelectric scanning tube to move in the horizontal plane;
The specific control process comprises the following steps: firstly, parameters to be set are transmitted to a time-sharing excitation control system through an upper computer, and the time-sharing excitation control system generates corresponding signals and loads the corresponding signals into corresponding sensors through digital-to-analog conversion. Meanwhile, the hardware structure transmits feedback signals back to the time-sharing excitation control system through the analog-digital conversion module during operation, and then the time-sharing collaborative excitation technology of the non-contact mode and the contact mode is realized under the action of control methods such as a phase-locked loop, negative feedback and the like.
When the working mode is set as a non-contact mode, a contact mode and a non-contact mode, and when excitation signals sent by the time-sharing excitation control system through the sensors are subjected to digital-to-analog conversion and then act on a hardware structure, taking fig. 2 as an example, when the atomic force microscope is in a non-contact mode state, the cantilever beam drives the probe to keep a certain distance from the sample 3 at the position 1, the excitation sensor excites the cantilever beam to resonate, the probe and the sample keep a non-contact state in cooperation with the negative feedback loop, the feedback parameter signals can be respectively set as various physical parameters such as frequency, amplitude, phase and current according to physical and chemical characteristics to be specifically represented, the imaging of the surface of the sample is realized by the atomic force microscope in an amplitude modulation mode, and the long-range performance of the sample is represented by the non-contact mode, for example: sample morphology imaging, magnetic field force imaging and electrostatic force imaging; after the operation step of the non-contact mode is completed, when the atomic force microscope is switched to the contact mode, the piezoelectric scanning tube 4 is driven by a driving signal of the position signal sensor to displace so as to enable the sample to move upwards, and the cantilever beam drives the probe to be in contact with the sample 3 at the position 2, so that the excitation sensor can perform corresponding contact mode characterization on the sample 3, and a negative feedback loop taking the amplitude as a set parameter is in a closed state at the moment;
Finally, when the atomic force microscope is switched to the non-contact mode after the testing task in the contact mode is executed, the piezoelectric scanning tube 4 generates reverse displacement, the sample 3 is moved downwards, the cantilever beam recovery position 1 is returned to the original position, and the cantilever beam recovery position 1 is far away from the sample 3 so as to keep the non-contact mode to operate, and at the moment, the negative feedback loop is restarted to maintain the dynamic non-contact state between the probe and the sample.
In the above mode of operation, it is assumed that the additionally determined property is characterized as a conductive property. When the clock signal reaches the switching time set by the time-sharing excitation control system, the excitation signal for driving the cantilever beam to resonate in a non-contact mode is immediately closed, and at the moment, the system drives the piezoelectric scanning tube to advance so that the probe is in contact with the sample, so that an obvious current signal can be seen. After the current signal is tested, the atomic force microscope is switched to a non-contact mode, the probe leaves the surface of the sample to enable the current to disappear, and the excitation signal of the excitation sensor is recovered to excite the cantilever beam to keep a resonance state. At the two mode switches, the excitation signal and the change in the current signal may correspond exactly.
The signal timing diagram of the time-sharing excitation control system is shown in fig. 1, the atomic force microscope operates in a non-contact mode before the time t 0, the excitation signal of the excitation sensor is closed at the time t 0, meanwhile, the position sensor sends a driving signal to the piezoelectric scanning tube 4 to drive the sample to move upwards, so that the probe and the sample are in a contact state, the excitation sensor is adopted to apply an additional excitation signal to the probe and/or the sample to start to detect specific parameters, after the relevant detection instruction of the contact mode is completed, the excitation signal of the excitation sensor is restarted at the time t 1, meanwhile, the driving signal of the position sensor is adjusted to the piezoelectric scanning tube 4, the piezoelectric scanning tube 4 drives the sample to move downwards, the surface of the sample returns to the original position, and the excitation signal of the excitation sensor in the contact mode is closed. Namely, the atomic force microscope completes switching from the non-contact mode to the contact mode at the time t 0, maintains the contact state in the period from t 0 to t 1, and then returns to the non-contact mode at the time t 1.
The second embodiment is as follows: the hardware structure of this embodiment differs from that of fig. 2 in that the sample is fixed, the cantilever beam of the atomic force microscope drives the probe to move vertically and horizontally above the sample 3, and the piezoelectric scanning tube is fixed to the cantilever beam, so that the cantilever beam drives the probe to move vertically and horizontally above the sample 3 by driving the piezoelectric scanning tube. The sensor in the hardware structure comprises an excitation sensor for exciting the cantilever beam to drive the probe to resonate, a position sensor for driving the piezoelectric scanning tube to move downwards, an excitation sensor in a contact mode, an excitation sensor in a non-contact mode and a sensor for driving the piezoelectric scanning tube to move horizontally;
The specific process comprises the following steps: firstly, parameters to be set are transmitted to a time-sharing excitation control system through an upper computer, and the time-sharing excitation control system generates corresponding signals and loads the corresponding signals into corresponding sensors through digital-to-analog conversion. Meanwhile, the hardware structure transmits feedback signals back to the time-sharing excitation control system through the analog-digital conversion module during operation, and then the time-sharing collaborative excitation technology of the non-contact mode and the contact mode is realized under the action of control methods such as a phase-locked loop, negative feedback and the like.
When the working mode is set as a non-contact mode, a contact mode and a non-contact mode, the time-sharing excitation control system acts on a hardware structure after digital-to-analog conversion of excitation signals sent by the sensors, when the atomic force microscope is in the non-contact mode state, the cantilever beam drives the probe to keep a certain distance from the sample, the excitation sensors excite the cantilever beam to resonate, the probe and the sample keep the non-contact state in cooperation with the negative feedback loop, the feedback parameter signals can be respectively set as various physical parameters such as frequency, amplitude, phase and current according to physical and chemical characteristics to be specifically represented, the imaging of the surface of the sample is realized by the atomic force microscope in an amplitude modulation mode, and the long-range performance of the sample is represented by the non-contact mode, for example: sample morphology imaging, magnetic field force imaging and electrostatic force imaging; when the atomic force microscope is switched to the contact mode after the operation step of the non-contact mode is completed, the piezoelectric scanning tube is driven by a driving signal of the position signal sensor to displace so that the cantilever beam drives the probe to move downwards, the probe is contacted with the sample, the excitation sensor can perform corresponding contact mode characterization on the sample, and a negative feedback loop taking amplitude as a set parameter is in a closed state at the moment;
Finally, when the atomic force microscope is switched to the non-contact mode after the testing task in the contact mode is executed, the piezoelectric scanning tube 4 can generate reverse displacement, so that the cantilever beam recovery position 1 is far away from the sample 3 and returns to the original position, the non-contact mode operation is kept, and the negative feedback loop is restarted at the moment to maintain the dynamic non-contact state between the probe and the sample.
The signal timing of the time-sharing excitation control system is the same as that of fig. 1, the atomic force microscope operates in a non-contact mode before the time t 0, the excitation signal of the excitation sensor is closed at the time t 0, meanwhile, the position sensor sends a driving signal to the piezoelectric scanning tube 4 to enable the probe to move downwards to be in a contact state with the sample, the excitation sensor is adopted to apply an additional excitation signal to the probe and/or the sample to start to detect specific parameters, after the relevant detection instruction of the contact mode is completed, the excitation signal of the excitation sensor is restarted at the time t 1, the driving signal of the position sensor is adjusted to enable the probe to leave the surface of the sample and return to the original position, and the excitation signal of the excitation sensor in the contact mode is closed. Namely, the atomic force microscope completes switching from the non-contact mode to the contact mode at the time t 0, maintains the contact state in the period from t 0 to t 1, and then returns to the non-contact mode at the time t 1. Specific examples are given below:
Example 1:
an atomic force microscope performs a design of non-contact mode-non-contact mode switching at a test location on the HOPG sample. The morphology of the sample is characterized in the non-contact mode and the conductivity of the sample is characterized in the contact mode.
As shown in fig. 3, the signal 1 is a real-time position signal of the cantilever beam under the control of the time-sharing excitation control system, the position sensor sends out a driving signal, and the signal 2 is a current signal of contact conduction between the probe and the sample.
The front end of the signal 1 corresponds to a vibration signal of the cantilever beam in a resonance state maintained in a non-contact mode, and when t=0, the piezoelectric scanning tube drives the cantilever beam to press down the surface of the sample, and at the moment, the amplitude of the signal 1 is greatly reduced, namely, the resonance actively excited by the probe in a contact mode is stopped. In addition, the horizontal position of signal 1 translates upward by an increase in voltage, reflecting the change in Z-axis position of the piezo scanner tube. At time t=0, a significant contact current was generated between the probe and the sample, with a signal intensity of 40 millivolts.
After about 3 milliseconds of contact current between the acquisition probe and the sample, the system executes a switch command from contact mode to non-contact mode. At this time, the initial position of the voltage drop of the Z axis of the piezoelectric scanning tube enables the probe to be far away from the surface of the HOPG sample, and the excitation signal of the excitation sensor restarts to maintain the cantilever resonance state. At the same time, the contact current signal disappears.
To this end, the command to measure the contact current using the non-contact mode-non-contact mode switching at a test location takes about 4 milliseconds to complete.
Example 2:
an atomic force microscope performs a design of non-contact mode-non-contact mode switching at a test location on the HOPG sample. The morphology of the sample is characterized in a non-contact mode, and the stress-strain performance of the sample is characterized in a contact mode.
The non-contact mode switching procedure was essentially the same as in example 1 above, except that the performance characterization function turned on was stress strain testing when switching to contact mode.
As shown in fig. 4, the curve formed by square data points is a contact stress curve of the probe and the sample switched from a non-contact state to a contact state, and the curve formed by circular data points is a desorption stress curve of the probe and the sample switched from the contact state to the non-contact state. According to international convention, the contact stress curve is symmetrically processed about the Y-axis at the zero point in the figure, so that two stress strain curves can be observed and compared in the figure at the same time.
After the system is switched to a contact mode, the piezoelectric scanning tube pushes the sample to be continuously close to the probe. As can be seen from the contact stress curve in FIG. 4, the maximum attractive force of about 8N is generated between the sample and the probe when the distance between the sample and the probe is within 3 nanometers, the repulsive force starts to be obviously increased when the distance between the sample and the probe is smaller than 2.5 nanometers, and the repulsive force and the attractive force between the probe and the sample reach an equilibrium state when the distance between the sample and the probe is 2 nanometers. Thereafter, as the probe is brought closer to the sample, a repulsive force of about 50 newtons can be generated at maximum between the two.
When the system switches to a non-contact mode, the piezoelectric scanning tube drives the sample away from the probe. At this time, the repulsive force between the probe and the sample gradually decreases, and the desorption stress curve is observed, so that the maximum attractive force of 18 newtons is generated during desorption and is significantly larger than the maximum attractive force during contact because the probe is pressed into the sample. In addition, the equilibrium point of attraction and repulsion between the sample and the probe and the initial point of attraction in the desorption stage are moved backward by about 2 nm and 7 nm, respectively.
Example 3:
an atomic force microscope performs a non-contact mode-non-contact mode switching design on a1 micron by 1 micron area of the HOPG sample. The morphology of the sample is characterized in the non-contact mode and the conductivity of the sample is characterized in the contact mode.
This embodiment is a set after the single test site operation in embodiment 1 is performed on the X-axis 512 by Y-axis 512 points within the scan area, respectively, and the control command at each test site is the same as that in embodiment 1. In addition, basic parameters of the operation of the scanning probe microscope, that is, scanning position, scanning point number, scanning speed, scanning slope, etc., need to be additionally set.
Fig. 5 is a topography diagram of an atomic force microscope scanning a particular region of an HOPG sample, and fig. 6 is a contact current diagram of an atomic force microscope scanning the same region of the HOPG sample. By comparing the two images, the appearance image of the sample and the contact current image have an accurate corresponding relation, and the contact current of the sample and the probe corresponding to the height fluctuation position of the appearance also has a change in size according with the appearance rule.
Therefore, the non-contact mode and contact mode cooperative work technology can truly realize multi-field coupling in-situ characterization of materials, and solves the problem that the topography map and the current map cannot be accurately corresponding due to intrinsic defects of mechanical equipment in the traditional secondary scanning technology.
Although the invention herein has been described with reference to particular embodiments, it is to be understood that these embodiments are merely illustrative of the principles and applications of the present invention. It is therefore to be understood that numerous modifications may be made to the illustrative embodiments and that other arrangements may be devised without departing from the spirit and scope of the present invention as defined by the appended claims. It should be understood that the different dependent claims and the features described herein may be combined in ways other than as described in the original claims. It is also to be understood that features described in connection with separate embodiments may be used in other described embodiments.