CN106771376B - Method for preparing atomic force microscope needle point - Google Patents
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- CN106771376B CN106771376B CN201710127121.6A CN201710127121A CN106771376B CN 106771376 B CN106771376 B CN 106771376B CN 201710127121 A CN201710127121 A CN 201710127121A CN 106771376 B CN106771376 B CN 106771376B
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- 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 relates to the field of atomic force microscopes, in particular to a method for preparing an atomic force microscope needle tip, which is characterized in that a device for realizing the method mainly comprises a resistor, a cantilever, a needle tip, a sample, a gap between the sample and the needle tip, a thorn-shaped object, a current feedback system, a photoelectric feedback system, a piezoelectric driver and a power supply U, wherein the current feedback loop is formed by connecting the power supply U, the resistor, the current feedback system, the cantilever, the needle tip, the gap and the sample, the photoelectric feedback system is connected between the cantilever and the sample, the piezoelectric driver is connected with the cantilever, the needle tip is fixed below the cantilever, the sample is positioned below the needle tip, the gap is arranged between the sample and the needle tip, and when the needle tip approaches the surface of the sample, the power supply U is started to form a high electric field at the gap, so that the thorn-shaped object with the length of hundreds of nanometers grows from the front end of the needle tip by using the first sample and the second sample successively, and the thorn-shaped object which is perpendicular to the surface of the sample and meets the experimental requirements is grown.
Description
Technical Field
The invention relates to the field of preparation of atomic force microscope needlepoints with a nano structure, in particular to a method for preparing an atomic force microscope needlepoint, which can directly prepare the needlepoint meeting the experimental requirement on the original needlepoint under the condition of normal temperature and atmosphere and is simple and effective.
Background
An atomic force microscope (Atomic Force Microscope, AFM) is an instrument for observing the microscopic morphology of the surface of an object by utilizing the interaction force between atoms and molecules, and the basic principle is as follows: by fixing a nanoscale probe on a micron-sized elastic cantilever which can be flexibly controlled, when the needle point is very close to a sample, the acting force between the atom at the tip of the needle point and the atom on the surface of the sample can bend the micron-sized elastic cantilever and deviate from the original position; at the same time, a beam of laser irradiates the cantilever and is reflected to the laser monitor, the bending of the elastic cantilever causes the deflection of the laser, so as to obtain the offset of the light spot, the offset and the vibration frequency are used as feedback signals, and the feedback signals are input into a computer through a specific feedback system, so that the computer can reconstruct a three-dimensional image, and the morphology and the composition information of the sample surface are obtained.
Atomic force microscopes can operate in different modes, mainly contact mode, tap mode, lateral force mode, etc. In the contact mode, the tip of the needle is stroked across the sample surface and the deflection from the cantilever can directly analyze the surface elevation. In the tapping mode or the lateral force mode, a signal source drives the cantilever to vibrate at an external reference frequency, the frequency of the cantilever vibration changes during the scanning of the sample, parameters such as amplitude, phase and resonance are related to the acting force between the probe and the sample, and the change of the parameters relative to the vibration of the external reference provided by the signal source can reflect the properties of the sample. Among them, as an extension technique of the tapping mode, the phase shift mode images by detecting a change in a difference between a phase angle of a signal source driving vibration of the cantilever probe and a phase angle of actual vibration of the cantilever probe (i.e., a phase shift of the signal source and the actual vibration).
Atomic Force Microscopy (AFM) offers significant advantages over scanning electron microscopy, first, atomic force microscopy can provide true three-dimensional surface maps, whereas scanning electron microscopy can only provide two-dimensional images; second, atomic force microscopy does not require any special treatment of the sample, such as copper plating or carbon, which can cause irreversible damage to the sample; thirdly, the atomic force microscope can work well under normal pressure and even under liquid environment, can be used for researching biological macro molecules and even living biological tissues, and can visually express the shape of atoms by slowly stroking on the surface of an object like a blind person. While electron microscopes need to operate under high vacuum conditions.
The tip of an atomic force microscope is usually a silicon material Si or Si 3 N 4 Is made by plating different metal layers on the outer part according to different requirements. When the traditional atomic force microscope probe tip is worn, the curvature radius of the probe tip is increased, the image resolution of a sample obtained by scanning is reduced, so that the imaging of the atomic force microscope is greatly influenced by the probe, the atomic force microscope probe tip is a consumable, the probe tip is extremely easy to consume in the use process, particularly after a high-precision experiment, the replacement of the probe tip is time-consuming and labor-consuming, the experiment progress is delayed, and the current method for growing a spike at the tip of the silicon probe tip comprises the following steps: ion or electron beam deposition, focused ion beam etching, chemical vapor depositionCarbon nanotubes or metal nanotubes, etc. However, these methods have the following drawbacks: firstly, the cost is higher, secondly, the method needs to be carried out in a vacuum cavity and has high requirement on vacuum, thirdly, the method can not be carried out in situ, and the experimental process needs to be interrupted, so that a new needle point can not be replaced conveniently and timely, the experimental process is delayed, and the problem can be solved by the method for preparing the atomic force microscope needle point.
Disclosure of Invention
In order to solve the problems, the invention controls the distance between the needle point and the sample by adding the current feedback system, uses the first sample and the second sample successively, grows the thorn-shaped object which is vertical to the surface of the sample and meets the experimental requirements, can directly operate under the atmospheric condition and obviously improve the sharpness of the needle point of the atomic force microscope, can prepare the needle point which meets the experimental requirements in situ without replacing the needle point, does not need a closed cavity filled with certain protective gas, does not need to use more complex preparation tools, and is effective.
The technical scheme adopted by the invention is as follows:
the device for realizing the method mainly comprises a resistor, a cantilever, a needle point, a sample, a gap between the sample and the needle point, a thorn-shaped object, a current feedback system, a photoelectric feedback system, a piezoelectric driver and a power supply U, wherein the power supply U, the resistor, the current feedback system, the cantilever, the needle point, the gap and the sample are connected to form a current feedback loop; when the current feedback system is started, weak current between the needle point and the sample can be detected and compared with a preset current value, a feedback signal of the current feedback system is input into the piezoelectric driver and can control the distance between the needle point and the sample, the needle point is made of a semiconductor material or provided with a metal coating, the sample is made of a thin film of conductive metal nickel or cobalt or gold or platinum, and the semiconductor material Si or GaAs,
the sample comprises a first sample and a second sample, wherein the surface of the first sample is provided with inverted cone concave pits which are arranged in an array, every 100nm is provided with a concave pit with the diameter of 100nm and the depth of 30nm, and the surface of the second sample is provided with protrusions which are arranged in an array, every 20nm is provided with a protrusion with the height of 20nm and the diameter of 10 nm;
a method of making an atomic force microscope tip comprising: a method of growing a spike for the first time, a method of growing a spike longer, a method of growing a spike perpendicular to the surface of a sample, and a method of checking whether the tip of a needle is sharp,
the method of primary growth of the thorns is as follows: selecting a first sample, horizontally moving a needle point to a position above a pit by using an atomic force microscope tapping mode, closing a photoelectric feedback system, starting a current feedback system, setting a current set value to be 1pA, starting a power supply U, and increasing the output voltage of the power supply U from 0 to V in 2 seconds 1 Wherein 20V < V 1 The power supply U is turned off after the voltage is less than 90V for 2 seconds, the primary growth process of the thorn is completed, and if the output voltage value is reduced to 0 from the original set value within 5 seconds before the power supply U is turned off, the thorn and the needle point can be combined more firmly;
the method of growing the thorns longer is as follows: after the primary growth process of the thorns is completed, the tip of the needle is horizontally moved to the position above the other concave pit by using an atomic force microscope tapping mode, and then the primary growth process is repeated, so that the thorns can be grown longer;
the method of growing the thorns perpendicular to the surface of the sample is as follows: after the primary growth process of the thorns is finished, the first sample is changed into a second sample, the atomic force microscope works in a tapping mode, the photoelectric feedback system is started, the current feedback system is closed, the power supply U is started again, the output voltage of the power supply U is kept at a value between 10V and 20V, then the needle tip starts to scan the samples, and as the needle tip is slightly contacted with the protrusions on the surface of the second sample, the thorns with larger random directions originally grown can slightly change direction, and thorns which are vertical to the surface of the samples and meet the experimental requirements are grown;
the method for checking whether the needle tip is sharp is as follows: using another sample with a relatively flat surface, operating an atomic force microscope in a phase shift mode, setting an initial amplitude to be A0, a scanning distance to be 15nm and a setting value to be 0.6A0, and if the phase shift on the flat surface is negative, considering the sample as a sharp needle point, so that the experimental requirement can be met; if the phase shift is not negative, the process of applying the power supply U to create a high electric field at the gap is repeated until an experimentally satisfactory spike is grown perpendicular to the sample surface.
If the protrusions on the surface of the second sample incline towards the same direction, the second sample is adopted to perform single-direction line scanning, and better effect can be obtained when the scanning direction is opposite to the inclined direction of the protrusions, after one line scanning is finished, the needle tip is lifted away from the second sample, and the needle tip returns to the line starting point to perform next line scanning, and the scanning is repeated in sequence.
The principle of thorn formation: the electric field can maintain a large value in a relatively confined area near the surface of the sample, and the sample and the needle tip can form nano structure growth, and the nano structure growth is spatially formed on the needle tip because one electrode is the tip of the needle tip, the electric field is uneven, adsorbates on the surface of the sample are transferred in the uneven electric field and decomposed, and then self-assembled, so that thorns are formed on the needle tip. The source of the spike constituent material is an adsorbate of hydrocarbons adsorbed in the atmosphere of the needle tip and sample surface, the decomposition of hydrocarbons that constitute the adsorbate forming carbon nanostructures on the needle tip and sample surface. By applying a power supply, there will be a deposit on both the sample and the tip, in most cases the deposited material will be carbon, which will be decomposed from the adsorbed hydrocarbons.
The beneficial effects of the invention are as follows:
according to the invention, the distance between the needle point and the sample is controlled by adding the current feedback system, the first sample and the second sample are used successively, the spike-shaped object which is vertical to the surface of the sample and meets the experimental requirement is grown, the needle point can be directly prepared under the atmospheric condition and the sharpness of the needle point of the atomic force microscope is obviously improved by adding a high electric field at the gap between the sample and the needle point, the needle point does not need to be carried out in a vacuum cavity, and a more complex preparation tool is not needed.
Drawings
The following is further described in connection with the figures of the present invention:
FIG. 1 is a schematic illustration of the present invention;
FIG. 2 is an enlarged schematic view of the gap between the sample and the tip;
FIG. 3 is an enlarged schematic view of a first sample;
FIG. 4 is an enlarged schematic view of a second sample;
FIG. 5 is a two-dimensional enlarged schematic of the second sample.
In the figure, 1, resistor, 2, cantilever, 3, needle tip, 4, sample, 5, gap, 6, spike, 7, current feedback system, 8, photoelectric feedback system, 9, piezoelectric driver.
Detailed Description
As shown in fig. 1, the device for realizing the method mainly comprises a resistor (1), a cantilever (2), a needle point (3), a sample (4), a gap (5) between the sample and the needle point, a thorn (6), a current feedback system (7), a photoelectric feedback system (8), a piezoelectric driver (9) and a power supply U, wherein the power supply U, the resistor (1), the current feedback system (7), the cantilever (2), the needle point (3), the gap (5) and the sample (4) are connected to form a current feedback loop, the negative electrode of the power supply U is connected with the resistor (1), the positive electrode is connected with the sample (4), the resistor (1) is a 20G ohm ballast resistor so as to prevent overlarge current in the current feedback loop, the photoelectric feedback system (8) is connected between the cantilever (2) and the sample (4), the current feedback system (7) is electrically connected with the piezoelectric driver (9), the piezoelectric driver (9) is connected with the cantilever (2), the needle point (3) is fixed below the cantilever (2), and the sample (4) is positioned below the needle point (3), and the gap (5) is arranged between the sample (4) and the needle point (3). When the current feedback system (7) is started, weak current between the needle point (3) and the sample (4) can be detected and compared with a preset current value, a feedback signal of the current feedback system (7) is input into the piezoelectric driver (9) and can control the distance between the needle point (3) and the sample (4), the needle point (3) is made of a semiconductor material or is provided with a metal coating, the sample (4) is made of a thin film of conductive metal nickel or cobalt or gold or platinum, the semiconductor material Si or GaAs, and the sample (4) is provided with a first sample and a second sample.
As shown in fig. 2, which is an enlarged schematic diagram of the gap between the sample and the needle tip, when the needle tip (3) approaches the surface of the sample (4), the power supply U is turned on to form a high electric field at the gap (5), so that a spike (6) with a length of hundreds of nanometers is grown at the front end of the needle tip (3).
As shown in FIG. 3, which is an enlarged schematic view of the first sample, the surface of the first sample has inverted cone pits arranged in an array, and every 100nm, there is a pit with a diameter of 100nm and a depth of 30 nm.
FIG. 4 is an enlarged schematic view of a second sample having protrusions arranged in an array on the surface thereof, each having protrusions with a height of 20nm and a diameter of 10nm at intervals of 20 nm.
As shown in fig. 5, which is a two-dimensional enlarged schematic view of the second sample, if the protrusions on the surface of the second sample are inclined in the same direction, the second sample is adopted to perform a single-direction line scanning, and when the scanning direction is opposite to the inclined direction of the protrusions, a better effect can be obtained, and after the line scanning is finished, the needle tip (3) is lifted away from the second sample, and the second sample is returned to the line starting point to perform the next line scanning, and the scanning is repeated in turn.
A method for preparing an atomic force microscope tip, comprising a method for growing a spike (6) for the first time, a method for growing a spike (6) longer, a method for growing a spike (6) perpendicular to the surface of a sample (4), and a method for checking whether the tip (3) is sharp,
the method of primary growth of the thorns (6) is as follows: selecting a first sample, horizontally moving the needle point (3) to a position above the pit by using an atomic force microscope tapping mode, closing a photoelectric feedback system (8), starting a current feedback system (7), setting the current to be 1pA, starting a power supply U, and increasing the output voltage of the power supply U from 0 to V in 2 seconds 1 Wherein 20V < V 1 < 90V for 2 secondsAfter the power supply U is turned off, the process of growing the thorn (6) for the first time is completed, if the output voltage value is reduced to 0 from the original set value within 5 seconds before the power supply U is turned off, the thorn (6) and the needle point (3) can be firmly combined, compared with the surface of a flat sample (4), the focusing electric field is stronger when the needle point (3) is positioned at a concave pit position, and the thorn (6) is easier to generate;
the method for growing the thorns (6) longer is as follows: after the primary growth of the thorn (6) is finished, the tip (3) is horizontally moved to the position above the other concave pit by using an atomic force microscope tapping mode, and then the primary growth of the thorn (6) is repeated, so that the thorn (6) can be grown longer;
the method of growing the lances (6) perpendicular to the surface of the sample (4) is as follows: after the process of growing the thorns (6) for the first time is finished, the first sample is changed into a second sample, the atomic force microscope works in a tapping mode, a photoelectric feedback system (8) is started, a current feedback system (7) is closed, a power supply U is started again, the output voltage of the power supply U is kept at a value between 10V and 20V, then a needle point (3) starts to scan the sample (4), and as the needle point (3) is slightly contacted with the protrusions on the surface of the second sample, the thorns (6) with larger random directions originally growing can slightly change the directions, and the thorns (6) which are perpendicular to the surface of the sample (4) and meet the experimental requirements are grown;
the method for checking whether the needle tip (3) is sharp is as follows: using another sample with a relatively flat surface, operating an atomic force microscope in a phase shift mode, setting an initial amplitude to be A0, a scanning distance to be 15nm and a setting value to be 0.6A0, and if the phase shift on the flat surface is negative, considering the sample as a sharp needle point (3), so that the experimental requirement can be met; if the phase shift is not negative, the process of applying the power supply U to form a high electric field at the gap (5) is repeated until an experimentally satisfactory spike (6) is grown perpendicular to the surface of the sample (4).
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and various modifications can be made to the above-described embodiment of the present invention. All simple, equivalent changes and modifications made in accordance with the claims and the specification of the present application fall within the scope of the patent claims.
The present invention is not described in detail in the conventional art.
Claims (2)
1. The device for realizing the method mainly comprises a resistor (1), a cantilever (2), a needle point (3), a sample (4), a gap (5) between the sample and the needle point, a thorn-shaped object (6), a current feedback system (7), a photoelectric feedback system (8), a piezoelectric driver (9) and a power supply U, wherein the power supply U, the resistor (1), the current feedback system (7), the cantilever (2), the needle point (3), the gap (5) and the sample (4) are connected to form a current feedback loop, the negative electrode of the power supply U is connected with the resistor (1), the positive electrode is connected with the sample (4), the resistor (1) is a 20G ohm ballast resistor, the photoelectric feedback system (8) is connected between the cantilever (2) and the sample (4), the current feedback system (7) is electrically connected with the piezoelectric driver (9), the piezoelectric driver (9) is connected with the cantilever (2), the needle point (3) is fixed below the cantilever (2), the sample (4) is positioned below the needle point (3), the gap (5) is formed between the sample (4) and the needle point (3), when the surface of the sample (3) is stopped at the surface of the needle point (4) and a high electric field can be formed at the gap (5), thereby leading the front end of the needle point (3) to grow a spike (6) with the length of hundreds of nanometers; when the current feedback system (7) is started, weak current between the needle point (3) and the sample (4) can be detected and compared with a preset current value, a feedback signal of the current feedback system (7) is input into the piezoelectric driver (9) and can control the distance between the needle point (3) and the sample (4), the needle point (3) is made of a semiconductor material or is provided with a metal coating, the sample (4) is made of a thin film of conductive metal nickel or cobalt or gold or platinum, a semiconductor material Si or GaAs,
the sample (4) is provided with a first sample and a second sample, wherein the surface of the first sample is provided with inverted cone concave pits which are arranged in an array, every 100nm is provided with a concave pit with the diameter of 100nm and the depth of 30nm, and the surface of the second sample is provided with a protrusion which is arranged in an array, every 20nm is provided with a protrusion with the height of 20nm and the diameter of 10 nm;
the method is characterized by comprising the following steps: a method for initially growing the spike (6), a method for growing the spike (6) longer, a method for growing the spike (6) perpendicular to the surface of the sample (4), and a method for checking if the needle tip (3) is sharp,
the method of primary growth of the thorns (6) is as follows: selecting a first sample, horizontally moving the needle point (3) to a position above the pit by using an atomic force microscope tapping mode, closing a photoelectric feedback system (8), starting a current feedback system (7), setting the current to be 1pA, starting a power supply U, and increasing the output voltage of the power supply U from 0 to V in 2 seconds 1 Wherein 20V < V 1 The power supply U is turned off after the power supply U is kept for 2 seconds less than 90V, the process of growing the thorn (6) for the first time is completed, and if the output voltage value is reduced to 0 from the original set value within 5 seconds before the power supply U is turned off, the thorn (6) and the needle point (3) can be combined more firmly;
the method for growing the thorns (6) longer is as follows: after the primary growth of the thorn (6) is finished, the tip (3) is horizontally moved to the position above the other concave pit by using an atomic force microscope tapping mode, and then the primary growth of the thorn (6) is repeated, so that the thorn (6) can be grown longer;
the method of growing the lances (6) perpendicular to the surface of the sample (4) is as follows: after the process of growing the thorns (6) for the first time is finished, the first sample is changed into a second sample, the atomic force microscope works in a tapping mode, a photoelectric feedback system (8) is started, a current feedback system (7) is closed, a power supply U is started again, the output voltage of the power supply U is kept at a value between 10V and 20V, then a needle point (3) starts to scan the sample (4), and as the needle point (3) is slightly contacted with the protrusions on the surface of the second sample, the thorns (6) with larger random directions originally growing can change directions, and the thorns (6) which are perpendicular to the surface of the sample (4) and meet the experimental requirements can be grown;
the method for checking whether the needle tip (3) is sharp is as follows: using another sample with a relatively flat surface, operating an atomic force microscope in a phase shift mode, setting an initial amplitude to be A0, a scanning distance to be 15nm and a setting value to be 0.6A0, and if the phase shift on the flat surface is negative, considering the sample as a sharp needle point (3), so that the experimental requirement can be met; if the phase shift is not negative, the process of applying the power supply U to form a high electric field at the gap (5) is repeated until an experimentally satisfactory spike (6) is grown perpendicular to the surface of the sample (4).
2. A method of preparing an atomic force microscope tip according to claim 1, characterized by: if the protrusions on the surface of the second sample incline towards the same direction, the second sample is adopted to perform single-direction line scanning, and better effect can be obtained when the scanning direction is opposite to the inclined direction of the protrusions, after one line scanning is finished, the needle tip (3) is lifted away from the second sample, and the second sample returns to the line starting point to perform the scanning of the next line, and the scanning is repeated in sequence.
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| CN110967527A (en) * | 2018-09-30 | 2020-04-07 | 中国计量科学研究院 | Preparation device for scanning probe tip |
| CN109507454A (en) * | 2018-11-07 | 2019-03-22 | 中北大学 | A kind of preparation method measuring crystal face active force atomic-force microscope needle-tip |
| CN110658360B (en) * | 2019-09-16 | 2020-08-18 | 浙江大学 | Method and device for preparing superfine atomic force microscope metal probe |
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