CN110470442B - Normal elastic constant needle point nondestructive calibration device of atomic force microscope probe and use method - Google Patents

Normal elastic constant needle point nondestructive calibration device of atomic force microscope probe and use method Download PDF

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CN110470442B
CN110470442B CN201910744619.6A CN201910744619A CN110470442B CN 110470442 B CN110470442 B CN 110470442B CN 201910744619 A CN201910744619 A CN 201910744619A CN 110470442 B CN110470442 B CN 110470442B
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镐东越
吴森
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Tianjin University
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M5/00—Investigating the elasticity of structures, e.g. deflection of bridges or air-craft wings
    • G01M5/0041—Investigating the elasticity of structures, e.g. deflection of bridges or air-craft wings by determining deflection or stress
    • G01M5/005—Investigating the elasticity of structures, e.g. deflection of bridges or air-craft wings by determining deflection or stress by means of external apparatus, e.g. test benches or portable test systems
    • G01M5/0058—Investigating the elasticity of structures, e.g. deflection of bridges or air-craft wings by determining deflection or stress by means of external apparatus, e.g. test benches or portable test systems of elongated objects, e.g. pipes, masts, towers or railways
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/20—Investigating strength properties of solid materials by application of mechanical stress by applying steady bending forces
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
    • G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
    • G01Q60/38—Probes, their manufacture, or their related instrumentation, e.g. holders

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Abstract

The invention discloses a normal elastic constant needle point nondestructive calibration device of an atomic force microscope probe and a use method thereof, wherein the normal elastic constant needle point nondestructive calibration device comprises: little platform is markd to sensitivity, bending force and little platform and two-dimentional electric displacement platform, and little platform is markd to sensitivity and little platform is markd to bending force respectively installs on a two-dimentional electric displacement bench or installs on same two-dimentional electric displacement bench, and wherein, little platform is markd to sensitivity includes a first slope silicon chip base, and little platform is markd to bending force includes: the top ends of the first inclined silicon wafer substrate and the second inclined silicon wafer substrate are respectively provided with a ridge. Compared with the prior system for calibrating the normal elastic constant of the atomic force microscope probe by adopting a bending method, the nondestructive calibration device for the normal elastic constant needle tip cannot damage and pollute the needle tip of the micro-cantilever probe.

Description

Normal elastic constant needle point nondestructive calibration device of atomic force microscope probe and use method
Technical Field
The invention belongs to the technical field of precision instruments, and particularly relates to a normal elastic constant needle point nondestructive calibration device of an atomic force microscope probe and a using method thereof.
Background
An Atomic Force Microscope (AFM) has wide application in surface topography measurement and characterization of micro-nano scale structures or materials. In the mechanical test based on the atomic force microscope, the micro-cantilever probe plays a crucial role. The normal elastic constant calibration of the micro-cantilever probe is necessary work before the surface topography of a micro-nano scale structure or material is measured and characterized. In the measurement and characterization of the surface topography of a micro-nano scale structure or material, the tip of the probe tip directly interacts with the surface of a sample, and the radius of the tip determines the imaging quality and resolution. The needle point and the sample interact in the measuring process, after multiple times of measurement, the needle point is possibly abraded or polluted, subsequent imaging quality is poor, the measured micro-nano scale structure or the material surface is inaccurate in appearance, a new probe needs to be replaced at the moment, and the original probe is discarded and recycled. In addition, the micro-cantilever probe has complex manufacturing process and high price, the cost of one needle is from hundreds to thousands of yuan, and the cost of some probes with special purposes is even more than ten thousand yuan. When the probe is calibrated, on the premise of not influencing the calibration accuracy, the smaller the damage of the probe tip is, the better the damage is, and the use of the subsequent formal test on the sample is not influenced as much as possible. Over the last two decades, a variety of methods have emerged to calibrate the elastic constants of microcantilever probes. These methods can be classified in principle into a dimensional parameter method, a resonance method, a bending method, and the like. The above methods have their own advantages and disadvantages. When the normal elastic constant of the probe is measured and calculated by using a dimension method and a resonance method, the probe tip cannot be damaged or polluted at all, but the two methods have respective limitations, and have larger uncertainty which is generally between 10 and 25 percent and even larger. The Hooke's law in the bending method is the basic principle, the cantilever beam is bent under the action of external force, and the bending amount of the cantilever beam is measured according to a formula
K is F/delta X type (1)
Wherein K is the normal elastic constant of the probe, F is the external force, and Delta X is the bending amount of the cantilever beam
And calculating to obtain the normal elastic constant of the cantilever beam. The calibration uncertainty of the method can reach below 2 percent, and the method can carry out relatively accurate normal elastic constant calibration on micro-cantilevers with various shapes and sizes. But in this method the probe tip acts as the point of stress. The tip of the atomic force microscope probe is generally conical, the height of the tip is about 5-20 μm, and the radius of the tip is about 5-40 nm. In the actual calibration process, the probe tip faces downwards, and the probe tip is used as a main stress point to drive the micro-cantilever to bend. Meanwhile, in order to obtain data with high signal-to-noise ratio, improve the accuracy of measurement and reduce the uncertainty of measurement, the bending amount of the micro-cantilever beam can reach several microns sometimes, the acting force at the needle tip of the micro-cantilever beam can reach several to dozens of micro-newtons, and the tip of the needle tip of the probe is easy to wear and break. And the micro-cantilever needle tip is directly contacted with the calibration substrate, and particles on the substrate can be adhered to the needle tip to pollute the needle tip.
Disclosure of Invention
The invention aims to provide a normal elastic constant needle point nondestructive calibration device of an atomic force microscope probe, which enables the back surface of a micro-cantilever of the probe (micro-cantilever probe) to bear force, the needle point is not contacted with any object, the stressed position of the back surface of the micro-cantilever is approximately the same as the position of the needle point, and the normal elastic constant needle point nondestructive calibration device can carry out large-bending-amount repeated in-situ calibration on any micro-cantilever probe for multiple times without any damage and pollution to the needle point of the probe.
The invention also aims to provide a using method of the normal elastic constant needle point nondestructive calibration device, the using method obtains the bending amount and the bending force of the cantilever beam of the micro-cantilever probe through the normal elastic constant needle point nondestructive calibration device, and the normal elastic constant of the micro-cantilever is worked out according to Hooke's law.
The purpose of the invention is realized by the following technical scheme.
A normal elastic constant needle point nondestructive calibration device of an atomic force microscope probe comprises: the bending force calibration device comprises a sensitivity calibration micro-platform, a bending force calibration micro-platform and a two-dimensional electric displacement platform, wherein the sensitivity calibration micro-platform and the bending force calibration micro-platform are respectively arranged on one two-dimensional electric displacement platform or the same two-dimensional electric displacement platform and used for moving on a horizontal plane, the sensitivity calibration micro-platform comprises a first inclined silicon chip substrate, and the bending force calibration micro-platform comprises: the silicon chip comprises a balance and a second inclined silicon chip substrate, wherein the top ends of the first inclined silicon chip substrate and the second inclined silicon chip substrate are respectively provided with a ridge.
In the above technical solution, the method further comprises: an optical structure, the optical structure comprising: the laser device comprises a laser source, a polarization spectroscope, a thin film beam splitter, an objective lens, a three-dimensional electric displacement table, a piezoelectric ceramic piece and a photoelectric detector, wherein an aperture diaphragm is arranged on a light path of laser emitted by the laser source and used for constraining the laser into parallel light, the polarization spectroscope is arranged on the light path of the parallel light so that the parallel light penetrates through the polarization spectroscope to form P light, a quarter glass slide is arranged on the light path of the P light so that the P light is changed into elliptical polarized light after passing through the quarter glass slide, and the thin film beam splitter is arranged on the light path of the elliptical polarized light so that the elliptical polarized light is reflected by the thin film beam splitter to form a first light beam; the micro-cantilever probe is installed in a probe holder, the probe holder and the three-dimensional electric displacement platform are fixedly installed on two opposite sides of the piezoelectric ceramic plate respectively, the micro-cantilever probe is located at a focal plane of the objective lens, the first light beam penetrates through the objective lens and is reflected by the micro-cantilever probe to form a second light beam, the second light beam penetrates through the objective lens and forms a third light beam, the third light beam is reflected by the film beam splitter to form linearly polarized light behind the quarter glass plate, and the linearly polarized light is reflected by the polarization beam splitter to the photoelectric detector.
In the above technical solution, the method further comprises: the laser light source, the aperture diaphragm, the polarizing beam splitter, the quarter glass, the thin film beam splitter, the objective lens, the three-dimensional electric displacement table and the photoelectric detector are fixedly mounted with a fixing piece, and the fixing piece is fixedly mounted with the longitudinal displacer.
In the above technical solution, the method further comprises: an observation system, the observation system comprising: the white light source, the tube lens, the beam splitter prism and the CCD camera are arranged on the white light beam emitted by the white light source, so that the white light reflected by the beam splitter prism sequentially penetrates through the film beam splitter and the objective lens to form a fourth light beam, the fourth light beam irradiates the micro-cantilever probe and is reflected by the micro-cantilever probe to sequentially penetrate through the objective lens, the film beam splitter, the beam splitter prism and the tube lens to form a fifth light beam, and the fifth light beam is acquired by the CCD camera.
In the above technical scheme, the white light source, the tube lens, the beam splitter prism and the CCD camera are all fixedly mounted with the fixing member.
The using method of the normal elastic constant needle point nondestructive calibration device comprises the following steps:
1) the needle point of the micro-cantilever probe is enabled to face upwards, the two-dimensional electric displacement platform is moved, so that the edge of the first inclined silicon chip substrate is positioned at the position of 400-600nm right below the needle point, the edge of the first inclined silicon chip substrate is pressed down by the micro-cantilever probe according to the downward displacement delta Z', and the normal voltage output delta U of the micro-cantilever probe is obtained through the photoelectric detectory', output of normal voltage Δ Uy' and amount of Down-Shift Δ ZSubstituting into formula (1) to obtain the optical lever sensitivity S of the micro-cantilever probey；
Sy＝ΔUy'/ΔZ' (1)
2) The needle point of the micro-cantilever probe is enabled to face upwards, the two-dimensional electric displacement platform is moved to enable the edge of the second inclined silicon chip substrate to be located at the position of 400-plus-600 nm right below the needle point, the micro-cantilever probe is pressed downwards, the edge of the second inclined silicon chip substrate is pressed downwards by the micro-cantilever probe according to the downward displacement delta Z', and the normal voltage output delta U of the micro-cantilever probe is obtained through the photoelectric detectory"and obtaining the index change Δ M of the balance before and after pressing down by the balance to output the normal voltage Δ Uy"and optical lever sensitivity SySubstituting the formula (2) to obtain the bending quantity delta Z' of the micro cantilever;
ΔZ″＝ΔUy″/Sy(2)
3) substituting the index change delta M and the bending quantity delta Z' of the micro cantilever into a formula (3) to obtain a normal elastic constant KnWherein G is the acceleration of gravity;
Kn＝ΔM·G/ΔZ″ (3)。
compared with the prior system for calibrating the normal elastic constant of the atomic force microscope probe by adopting a bending method, the nondestructive calibration device for the normal elastic constant needle tip cannot damage and pollute the needle tip of the micro-cantilever probe. The probe can be calibrated accurately and nondestructively from a common probe to a special cantilever probe or a micro-cantilever probe with a special needle tip, so that the integrity of the needle tip of the probe is ensured.
Drawings
FIG. 1 is a schematic structural diagram of a needle point nondestructive calibration apparatus with normal elastic constant in embodiment 3;
FIG. 2 is an SEM image of the needle tip after being stressed and subjected to normal elastic constant calibration;
FIG. 3 is an SEM image of the tip after normal spring constant calibration using the method of example 3 (cantilever back force).
1: longitudinal displacer, 2: CCD camera, 3: tube lens, 4: beam splitter prism, 5: white light source, 6: pellicle beam splitter, 7: three-dimensional electric displacement table, 8: piezoelectric ceramic sheet, 9: probe holder, 10: micro-cantilever probe, 11: first inclined silicon wafer substrate, 12: two-dimensional electric displacement table, 13: fixing member, 14: photodetector, 15: quarter slide, 16: polarizing beam splitter, 17: aperture stop, 18: laser light source, 19: objective lens, 20: loading column, 21: balance, 22: and a second inclined silicon wafer substrate.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
Example 1
As shown in FIG. 1, the nondestructive normal elastic constant tip calibration device for an atomic force microscope probe comprises: little platform is markd to sensitivity, bending force and little platform and two-dimentional electric displacement platform 12 are markd to sensitivity, and little platform is markd to sensitivity and bending force is markd respectively installs on a two-dimentional electric displacement platform 12 or installs on same two-dimentional electric displacement platform 12 for move at the horizontal plane, wherein, little platform is markd to sensitivity includes a first slope silicon chip base 11, and little platform is markd to bending force includes: a balance 21 and a second inclined silicon substrate 22, wherein the top ends of the first inclined silicon substrate 11 and the second inclined silicon substrate 22 are respectively formed with a rib.
The using method of the normal elastic constant needle point nondestructive calibration device comprises the following steps:
1) the radius of the bottom surface of the tip of the micro-cantilever probe 10 is 5-8 μm, the tip of the micro-cantilever probe 10 is made to face upwards, the two-dimensional electric displacement table 12 is moved to make the edge of the first inclined silicon substrate 11 be located at the position of 400 nm and 600nm right below the tip, the edge of the first inclined silicon substrate 11 is pressed down by the micro-cantilever probe 10 with the downward displacement delta Z', and the normal voltage output delta U of the micro-cantilever probe 10 is obtained by the photoelectric detector 14y', output of normal voltage Δ Uy'and the amount of downshifting DeltaZ' are substituted into the formula (1) to obtain the optical lever sensitivity S of the micro-cantilever probe 10y；
Sy＝ΔUy'/ΔZ' (1)
2) Making a micro-cantilever probe 10The tip of the probe is upward, the two-dimensional electric displacement table 12 is moved to enable the edge of the second inclined silicon chip substrate 22 to be positioned at the position of 400-plus 600nm right below the tip, the micro-cantilever probe 10 is pressed downwards, the micro-cantilever probe 10 is enabled to press the edge of the second inclined silicon chip substrate 22 downwards by the downward movement amount delta Z', and the normal voltage output amount delta U of the micro-cantilever probe 10 is obtained through the photoelectric detectory"and obtaining the indication change Δ M of the balance 21 before and after pressing by the balance 21 to output the normal voltage Δ Uy"and optical lever sensitivity SySubstituting the formula (2) to obtain the bending quantity delta Z' of the micro cantilever;
ΔZ″＝ΔUy″/Sy(2)
3) substituting the index change Delta M and the bending quantity Delta Z' of the micro cantilever into a formula (3) to obtain a normal elastic constant KnWherein G is the acceleration of gravity;
Kn＝ΔM·G/ΔZ″ (3)。
example 2
In order to more conveniently realize the measurement of the normal elastic constant, on the basis of embodiment 1, the method further comprises: an optical structure, the optical structure comprising: the laser device comprises a laser source 18, a polarization spectroscope 16, a film beam splitter 6, an objective lens 19, a three-dimensional electric displacement table 7, a piezoelectric ceramic piece 8 and a photoelectric detector 14, wherein an aperture diaphragm 17 is arranged on a light path of laser emitted by the laser source 18 and used for restricting the laser into parallel light, the polarization spectroscope 16 is arranged on the light path of the parallel light so that the parallel light forms P light after penetrating through the polarization spectroscope 16, a quarter glass slide 15 is arranged on the light path of the P light so that the P light becomes elliptically polarized light after passing through the quarter glass slide 15, and the film beam splitter 6 is arranged on the light path of the elliptically polarized light so that the elliptically polarized light is reflected by the film beam splitter 6 to form first light beams; the micro-cantilever probe 10 is arranged in a probe holder 9, the probe holder 9 and the three-dimensional electric displacement platform 7 are fixedly arranged on two opposite sides of the piezoelectric ceramic plate 8 respectively, the micro-cantilever probe 10 is positioned at a focal plane of the objective lens 19, the first light beam penetrates through the objective lens 19 and is reflected by the micro-cantilever probe 10 to form a second light beam, the second light beam penetrates through the objective lens 19 to form a third light beam, the third light beam is reflected to the quarter glass slide 15 by the thin film beam splitter 6 to form linearly polarized light, and the linearly polarized light is reflected to the photoelectric detector 14 by the polarized beam splitter 16.
Preferably, a loading column 20 is fixed to the second inclined silicon wafer base 22 and the balance 21.
Example 3
In order to more conveniently realize the measurement of the normal elastic constant, on the basis of embodiment 2, the method further comprises: the longitudinal shifter 1, the laser light source 18, the aperture diaphragm 17, the polarization beam splitter 16, the quarter glass 15, the thin film beam splitter 6, the objective lens 19, the three-dimensional electric displacement table 7 and the photoelectric detector 14 are fixedly mounted with a fixing piece 13, and the fixing piece 13 is fixedly mounted with the longitudinal shifter 1.
Example 3
In order to more conveniently realize the measurement of the normal elastic constant, on the basis of embodiment 2, the method further comprises: an observation system, the observation system comprising: the white light source 5, the tube lens 3, the beam splitter prism 4 and the CCD camera 2, the beam splitter prism 4 is arranged on a white light beam emitted by the white light source 5, so that the white light reflected by the beam splitter prism 4 sequentially penetrates through the film beam splitter 6 and the objective lens 19 to form a fourth light beam, the fourth light beam irradiates the micro-cantilever probe 10 and is reflected by the micro-cantilever probe 10 to sequentially penetrate through the objective lens 19, the film beam splitter 6, the beam splitter prism 4 and the tube lens 3 to form a fifth light beam, and the fifth light beam is acquired by the CCD camera 2. The white light source 5, the tube lens 3, the beam splitter prism 4 and the CCD camera 2 are fixedly arranged with the fixing piece 13.
The use method of the normal elastic constant needle point nondestructive calibration device comprises the following steps:
1) the micro-cantilever probe 10 is mounted on the probe holder 9 in a reversed manner with the tip of the micro-cantilever probe 10 facing upwards. The three-dimensional motorized displacement stage 7 is adjusted so that the micro-cantilever probe 10 can be clearly seen from the CCD camera 2 and so that the first light beam impinges on the micro-cantilever probe 10. Moving the two-dimensional electric displacement table 12 to enable the first inclined silicon chip substrate 11 to be positioned below the micro-cantilever beam probe 10, controlling the longitudinal displacement device 1 to enable the micro-cantilever beam probe 10 to slowly approach to the edge of the first inclined silicon chip substrate 11 positioned right below the micro-cantilever beam probe 10, observing the CCD camera 2, and enabling the two-dimensional electric displacement table 12 to carry out water operation when the light gradually changes from dark to lightAnd (3) flat micro displacement, wherein the visual field of the CCD camera 2 is roughly divided into a light part and a dark part, and then the longitudinal shifter 1 is controlled until the edge of the first inclined silicon chip substrate 11 and the micro cantilever probe 10 are clearly seen at the same time. Controlling the two-dimensional electric displacement platform 12 and the piezoelectric ceramic plate 8 to enable the edge of the first inclined silicon chip substrate 11 to be positioned at the position of 400-plus-600 nm right below the needle tip, enabling the micro-cantilever probe 10 to press the edge of the first inclined silicon chip substrate 11 with the downward displacement delta Z' through the three-dimensional electric displacement platform 7, and acquiring the normal voltage output delta U of the micro-cantilever probe 10 through the photoelectric detectory', output of normal voltage Δ Uy'and the amount of downshifting DeltaZ' are substituted into the formula (1) to obtain the optical lever sensitivity S of the micro-cantilever probe 10y；
Sy＝ΔUy'/ΔZ' (1)
2) And controlling the longitudinal shifter 1 to drive the micro-cantilever probe 10 to move upwards by about 5mm and keep away from the first inclined silicon chip substrate 11. And (3) finely adjusting the three-dimensional electric displacement table 7 to ensure that the position of the first light beam irradiated on the micro-cantilever probe 10 is unchanged. And moving the two-dimensional electric displacement platform 12 to enable the second inclined silicon wafer substrate 22 to be positioned below the micro-cantilever beam probe 10, controlling the longitudinal displacement device 1 to enable the micro-cantilever beam probe 10 to slowly approach to the edge of the second inclined silicon wafer substrate 22 positioned right below the micro-cantilever beam probe 10, observing the CCD camera 2 at the same time, enabling the two-dimensional electric displacement platform 12 to carry out horizontal micro-displacement when the light gradually changes from dark to bright, observing that the visual field of the CCD camera 2 is roughly divided into a light part and a dark part, and then controlling the longitudinal displacement device 1 until the edge of the second inclined silicon wafer substrate 22 and the micro-cantilever beam probe 10 are clearly seen at the same time. Controlling the two-dimensional electric displacement platform 12 and the piezoelectric ceramic plate 8 to enable the edge of the second inclined silicon wafer substrate 22 to be positioned at the position of 400-plus-600 nm right below the needle tip, pressing down the micro-cantilever probe 10 through the three-dimensional electric displacement platform 7 to enable the micro-cantilever probe 10 to press down the edge of the second inclined silicon wafer substrate 22 by the downward displacement delta Z', and acquiring the normal voltage output delta U of the micro-cantilever probe 10 through the photoelectric detectory"and obtaining the indication change Δ M of the balance 21 before and after pressing by the balance 21 to output the normal voltage Δ Uy"and optical lever sensitivity SySubstituting the formula (2) to obtain the bending quantity delta Z' of the micro cantilever;
ΔZ″＝ΔUy″/Sy(2)
3) substituting the index change Delta M and the bending quantity Delta Z' of the micro cantilever into a formula (3) to obtain a normal elastic constant KnWherein G is the acceleration of gravity;
Kn＝ΔM·G/ΔZ″ (3)。
in the above embodiment, the resolution of a CCD camera, a CMOS camera model DCC1545M manufactured by Thorlabs corporation, usa, is 1280 × 1024 pixels, and the individual pixel size is 5.6 × 5.6 μm;
the objective lens is an objective lens with model number of 0.42 and model number of M Plan Apo 20X and NA manufactured by Sanfeng corporation of Japan, the working distance is 20mm, and the diameter of the objective lens is 29.2 mm;
the longitudinal shifter 1 uses a PSA100-11-Z model precision electric lifting table produced by Touhuang optical company, the central load is 5kg, and the open-loop resolution is subdivided by 8 μm;
the probe holder is a probe holder which is produced by Bruker and used on Dimension ICON, and the included angle between the groove and the horizontal plane is 12 degrees;
the first inclined silicon wafer substrate is obliquely fixed on the glass slide by a rectangular polished silicon wafer, and the included angle between the inclined angle of the rectangular polished silicon wafer and the horizontal plane is about 15 degrees. The size of the silicon chip is 10 multiplied by 10mm, the thickness is about 1mm, and the edge angles are all 90 degrees;
the loading column is about 30mm long and about 1g in weight, the top end of the loading column is an oblique plane, and the included angle between the oblique plane and the horizontal plane is about 15 degrees. And the top end of the loading column is adhered with a polished small silicon wafer, the edge angle is upward, and the edge angle is 90 degrees to form an edge of a second inclined silicon wafer substrate.
TABLE 1 comparison of the results of the probe elastic constant calibration of the stress on the tip and the stress on the back of the micro-cantilever
Figure BDA0002165141720000071
Figure BDA0002165141720000081
As can be seen from Table 1, the probe tips and the back of the micro-cantilever of the probes are respectively used for calibrating the probes with three different models for multiple times, the calibrated elastic constants are almost consistent, and the uncertainty is small. Therefore, the method for calibrating the normal elastic constant of the probe by the force method on the back surface of the micro-cantilever beam of the probe is feasible and has accurate result.
As shown in FIG. 2, it can be seen that after ten times of tip force calibration of the universal atomic force microscope probe OTESPA-R3, the diameter of the tip reaches 126.3nm, and the tip of the tip is obviously worn and broken. The universal atomic force microscope probe OTESPA-R3 was calibrated for the back force of the micro-cantilever ten times according to the method used in example 3, and as shown in FIG. 3, the diameter of the tip after the back force calibration of the micro-cantilever was about 38.96nm, and no damage or contamination was caused to the tip.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.

Claims (5)

1. A use method of a normal elastic constant needle point nondestructive calibration device of an atomic force microscope probe comprises the following steps: the device comprises a sensitivity calibration micro-platform, a bending force calibration micro-platform and a two-dimensional electric displacement platform (12), wherein the sensitivity calibration micro-platform and the bending force calibration micro-platform are respectively installed on the two-dimensional electric displacement platform (12) or the same two-dimensional electric displacement platform (12) and used for moving on a horizontal plane, the sensitivity calibration micro-platform comprises a first inclined silicon chip substrate (11), and the bending force calibration micro-platform comprises: the silicon wafer scale comprises a balance (21) and a second inclined silicon wafer substrate (22), wherein the top ends of the first inclined silicon wafer substrate (11) and the second inclined silicon wafer substrate (22) are respectively provided with a ridge; the method is characterized in that the using method of the normal elastic constant needle point nondestructive calibration device comprises the following steps:
1) the needle point of a micro-cantilever probe (10) is enabled to face upwards, the two-dimensional electric displacement table (12) is moved, and the edge of the first inclined silicon chip substrate (11) is located at the needle pointAt the position of 400-600nm right below the micro-cantilever probe (10), the edge of the first inclined silicon wafer substrate (11) is pressed down by the micro-cantilever probe (10) with a downward displacement delta Z', and the normal voltage output delta U of the micro-cantilever probe (10) is obtained through the photoelectric detector (14)y', output of normal voltage Δ Uy'and the amount of downward shift DeltaZ' are substituted into the formula (1) to obtain the optical lever sensitivity S of the micro-cantilever probe (10)y；
Sy＝ΔUy'/ΔZ' (1)
2) Enabling the needle point of a micro-cantilever probe (10) to face upwards, moving the two-dimensional electric displacement table (12) to enable the edge of the second inclined silicon chip substrate (22) to be located at a position of 400-plus 600nm right below the needle point, pressing down the micro-cantilever probe (10), enabling the micro-cantilever probe (10) to press down the edge of the second inclined silicon chip substrate (22) by a downward displacement delta Z', and acquiring the normal voltage output delta U of the micro-cantilever probe (10) through a photoelectric detector (14)yAnd obtaining the indication change delta M of the balance (21) before and after pressing through the balance (21) to output the normal voltage delta Uy"and optical lever sensitivity SySubstituting the formula (2) to obtain the bending quantity delta Z of the micro cantilever;
ΔZ”＝ΔUy”/Sy(2)
3) substituting the index change delta M and the bending quantity delta Z' of the micro cantilever into a formula (3) to obtain a normal elastic constant KnWherein G is the acceleration of gravity;
Kn＝ΔM·G/ΔZ” (3)。
2. the method of use of claim 1, further comprising: an optical structure, the optical structure comprising: the device comprises a laser light source (18), a polarization spectroscope (16), a thin film beam splitter (6), an objective lens (19), a three-dimensional electric displacement table (7), a piezoelectric ceramic piece (8) and a photoelectric detector (14), wherein an aperture diaphragm (17) is arranged on a light path of laser light emitted by the laser light source (18) and used for constraining the laser light into parallel light, the polarization spectroscope (16) is arranged on the light path of the parallel light so that the parallel light penetrates through the polarization spectroscope (16) to form P light, a quarter glass (15) is arranged on the light path of the P light so that the P light is changed into elliptically polarized light after passing through the quarter glass (15), and the thin film beam splitter (6) is arranged on the light path of the elliptically polarized light so that the elliptically polarized light is reflected by the thin film beam splitter (6) to form a first light beam; micro-cantilever probe (10) are installed in a probe holder (9), probe holder (9) and three-dimensional electronic displacement platform (7) are adorned admittedly respectively the relative both sides of piezoceramics piece (8), micro-cantilever probe (10) are located the focal plane department of objective (19), first light beam passes through objective (19) and by micro-cantilever probe (10) reflection forms the second light beam, the second light beam passes through objective (19) and forms the third light beam, the third light beam by thin film beam splitter (6) reflect extremely form the line polarization behind quarter slide (15), the line polarization quilt polarization spectroscope (16) reflect extremely photodetector (14).
3. The method of use of claim 2, further comprising: the device comprises a longitudinal shifter (1), wherein a laser light source (18), an aperture diaphragm (17), a polarizing beam splitter (16), a quarter glass (15), a thin film beam splitter (6), an objective lens (19), a three-dimensional electric displacement table (7) and a photoelectric detector (14) are fixedly mounted on a fixing piece (13), and the fixing piece (13) is fixedly mounted on the longitudinal shifter (1).
4. The method of use of claim 3, further comprising: an observation system, the observation system comprising: the white light source (5), the tube lens (3), the beam splitter prism (4) and the CCD camera (2), wherein the beam splitter prism (4) is arranged on a white light beam emitted by the white light source (5), so that white light reflected by the beam splitter prism (4) sequentially penetrates through the film beam splitter (6) and the objective lens (19) to form a fourth light beam, the fourth light beam irradiates on the micro cantilever probe (10) and is reflected by the micro cantilever probe (10) to sequentially penetrate through the objective lens (19), the film beam splitter (6), the beam splitter prism (4) and the tube lens (3) to form a fifth light beam, and the fifth light beam is obtained by the CCD camera (2).
5. The use method according to claim 4, characterized in that the white light source (5), the tube mirror (3), the beam splitter prism (4) and the CCD camera (2) are all fixedly mounted with the fixing member (13).
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