CN109444476B - Preparation method of submicron probe for atomic force microscope - Google Patents
Preparation method of submicron probe for atomic force microscope Download PDFInfo
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- CN109444476B CN109444476B CN201811195404.5A CN201811195404A CN109444476B CN 109444476 B CN109444476 B CN 109444476B CN 201811195404 A CN201811195404 A CN 201811195404A CN 109444476 B CN109444476 B CN 109444476B
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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
Abstract
The invention discloses a preparation method of a submicron probe for an atomic force microscope, which comprises the following steps: firstly, cutting the front end of a micro-cantilever probe into a platform by an FIB technology; dispersing the microspherical particles for preparing the probe on the silicon wafer template marked with the position, and recording the position of the microspherical particles according to the mark; thirdly, replacing the commercial probe with the probe prepared in the first step; fourthly, fully sticking epoxy glue on the platform obtained in the first step; and fifthly, searching the position of the microsphere particles recorded in the step two by using a high-resolution optical microscope and a position control system which are carried by the atomic force microscope, and accurately positioning the needle to ensure that the microsphere particles can be bonded on the probe to obtain the submicron probe for the atomic force microscope. The method can adhere submicron particles on the needle tip in the air, can be used for detecting the interaction force, friction and other mechanical properties between particle materials and other materials under different environmental conditions, and can be used in the fields of life science, material science and the like.
Description
Technical Field
The invention belongs to the technical field of modification and processing of atomic force microscope probes, and particularly relates to a preparation method of a submicron probe for an atomic force microscope.
Background
An Atomic Force Microscope (AFM), which was invented since 1986, has been widely used in the fields of chemistry, biology, physics, and materials science, as well as in the industrial fields of semiconductors, integrated circuits, etc. The material surface micro-topography and the electromagnetic property of the material surface micro-topography can be represented mainly because the material has atomic-level spatial resolution and multiple imaging modes; in addition, the interaction force between the needle tip and the sample can be used for representing the mechanical properties of the surface of the material, such as elastic modulus, viscous force and friction property; meanwhile, the device can work in air, liquid and vacuum environments.
One of the key components of AFM to achieve high resolution detection is the probe. The probe mainly comprises a substrate, a micro-cantilever and a needle tip, wherein in the testing process, the needle tip is contacted with the surface of a sample to generate an interaction force, so that the micro-cantilever of the probe is bent, and various information is obtained by detecting the bending size of the micro-cantilever. The parameters and precision of the probe have an important influence on the test result, and the conventional commercial probe is a substrate-micro cantilever-tip integrated structure which is processed by using semiconductor materials through etching, deposition and other technologies. The sharp needle tip is positioned at the free end of the micro-cantilever, the needle tip is generally in a shape of a four-cone or a cone, and the curvature radius is from several nanometers to dozens of nanometers. The main tip materials are silicon, silicon nitride and certain metals.
There has been a great deal of interest in the study of mechanical properties between specific materials, such as the interaction between drug particles and cells, and the desired results cannot be directly obtained using conventional commercial probes and colloidal probes.
Thus, there will also be some spherical colloidal probes. The used small ball is generally in the size of several microns to tens of microns, and is adhered to the cantilever without the needle tip through glue under an optical microscope. The prepared needle tip has a large contact area with a sample. For such micron-sized colloidal particles with larger size, it is easier to bond to the cantilever under an optical microscope (CN 107796958A).
However, for submicron particles, the optical microscope is not sufficiently magnified to directly observe the position of the particle, and if the thickness of the glue on the microcantilever is large, the extra glue will cover the submicron particles, resulting in a change in the surface material properties of the particles.
Disclosure of Invention
In view of the defects in the prior art, the technical problem to be solved by the invention is how to accurately position the submicron particles, so as to develop a method for preparing a good submicron probe for an atomic force microscope.
The specific technical scheme is as follows: a method for preparing a submicron probe for an atomic force microscope comprises the following steps:
firstly, cutting the front end of a micro-cantilever probe into a platform through a focused ion beam time-of-flight secondary ion mass spectrometer (FIB);
dispersing microspherical particles for preparing the probe on a silicon wafer template marked with positions, and recording the positions of the microspherical particles according to the marks through an atomic force microscope;
step three, replacing the commercial probe on the atomic force microscope with the probe prepared in the step one;
fixing a glass slide or a silicon wafer with an epoxy glue layer on a sample platform of the atomic force microscope, moving the glass slide or the silicon wafer to a relatively thin area of the epoxy glue layer by using a high-resolution optical microscope and a position control system which are carried by the atomic force microscope, adjusting needle insertion under the contact mode of the atomic force microscope, fully sticking the epoxy glue on the platform obtained in the step one after the probe is contacted with the surface of the epoxy glue, and withdrawing the needle;
replacing the glass slide or the silicon wafer with the epoxy glue water layer with the silicon wafer template which is obtained in the second step and is dispersed with the microsphere particles and marked with the positions, searching the positions of the microsphere particles recorded in the second step by using a high-resolution optical microscope and a position control system which are carried by the atomic force microscope, accurately positioning the probe, and bonding the microsphere particles on the probe after the microsphere particles contact the surface of the epoxy glue on the probe to obtain the submicron probe for the atomic force microscope; the submicron probe for the atomic force microscope is a microcantilever probe with a submicron particle at the tip.
And further, in the fourth step, the probe is kept still for 30 seconds after contacting the surface of the epoxy glue.
And further, in the fifth step, standing for 60 seconds after the probe is contacted with the surface of the epoxy glue.
Further, the micro-cantilever of the micro-cantilever probe in the step one is a micro-cantilever with a needle tip, a triangular micro-cantilever or a rectangular micro-cantilever; the width of the plateaus is 0.5-1.5 microns. Preferably around 1 micron.
Further, the specific operation of dispersing the microspherical particles for preparing the probe on the silicon chip template marked with the position in the second step comprises the following steps:
2.1, sequentially placing the microspherical particles for preparing the probe in acetone and ethanol for ultrasonic cleaning, and placing the cleaned microspherical particles in ethanol or aqueous dispersion for storage for later use to obtain dispersion with the microspherical particles;
2.2, sequentially placing the silicon wafer template marked with the position in an acetone and isopropanol solution for ultrasonic cleaning, and finally blowing the cleaned template for later use by using pure nitrogen;
and 2.3, dripping a drop of the dispersion liquid with the microsphere particles obtained in the step two on the silicon wafer template marked with the position after the treatment in the step 2.2, and drying for later use.
Further, the specific operation of recording the position of the microspheroidal particle according to the mark by the atomic force microscope in the step two is as follows: sequentially opening a controller and supporting software of the atomic force microscope, selecting a commercial probe, scanning and imaging the silicon wafer template dispersed with the microsphere particles, and recording the positions of the microsphere particles with better dispersibility according to the marks; the curvature radius of the needle point of the commercial probe is 2-50nm, preferably 9-11 nm; better dispersion means that the microspheroidal particles are positioned far enough apart to avoid interaction between the microspheroidal particles when they are bonded to the probe.
Furthermore, after the probe is replaced in the third step, the position and the reflection value of the laser are readjusted, and the effective needle insertion of the atomic force microscope is guaranteed.
Further, the preparation operation of the glass slide or the silicon wafer with the epoxy glue water layer in the fourth step is specifically as follows: and dripping the two-component epoxy glue on the cleaned glass slide or silicon wafer, uniformly stirring, and scraping redundant two-component epoxy glue from the side surface of the other cleaned glass slide, or spin-coating at high speed by using a spin-coating instrument to ensure that the epoxy glue on the surface of the glass slide or silicon wafer is as thin as possible, thereby obtaining the glass slide or silicon wafer with an epoxy glue water layer.
Further, the curing time of the two-component epoxy adhesive is 30 minutes or more. The two-part epoxy glue is UHU and/or endest 300.
And furthermore, the fifth step also comprises the step of taking down the prepared probe from the micro cantilever frame of the atomic force microscope after the microsphere particles are bonded on the probe, and placing the probe in a clean environment for 24 hours to completely cure the epoxy glue.
Further, the microspheroidal particles are spherical or lamellar particles of 200-1000nm size.
Further, the microsphere particles are silicon dioxide spheres or organic drug particles.
The invention also relates to the submicron probe for the atomic force microscope, which is obtained by the preparation method.
The beneficial effects are as follows:
1. the invention utilizes the high-precision optical imaging system and the high-precision motion control system which are arranged on the atomic force instrument, and the operation is convenient and visual.
2. The existing cantilever with the needle point is adopted, glue is adhered to the needle point through the needle inserting mode of the atomic force instrument, and the particles are prevented from being influenced by excessive glue.
3. The sharp needlepoint is partially cut by FIB, so that the phenomenon that the glue is excessively coated on the micro-cantilever is avoided.
4. The template is used as a carrier of the particles, so that the submicron particles can be accurately positioned.
The method provided by the invention can adhere submicron particles on the tip (or needle point) of the micro-cantilever in air, can be used for detecting the interaction force between the particle material and other materials and the mechanical properties such as friction under different environmental conditions, and can be used in various fields such as life science and material science.
Drawings
FIG. 1 is a schematic diagram of the cleavage of a probe.
FIG. 2 is a view of the probe tip before cutting.
FIG. 3 is a view of the probe tip after FIB cutting.
FIG. 4 is a schematic diagram of the scanning of an atomic force microscope to locate the position of microspheroidal particles.
FIG. 5 is a schematic view of a tip of a contact glue under an atomic force microscope.
FIG. 6 is a schematic illustration of a particle positioned by tip bonding under an atomic force microscope.
FIG. 7 is a front view of a submicron probe for an atomic force microscope.
FIG. 8 is a side view of a submicron probe for an atomic force microscope.
Detailed Description
The present invention is described in further detail below with reference to specific examples and with reference to the data. It will be understood that these examples are intended to illustrate the invention and are not intended to limit the scope of the invention in any way. The experimental procedures used in the following examples are all conventional procedures unless otherwise specified. Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
1. A commercial microcantilever probe with a tip (with a tip, a triangular or rectangular microcantilever) with appropriate parameters was selected, and the sharp front end of the tip was cut into a platform with a width of about 1 μm by a focused ion beam time-of-flight secondary ion mass spectrometer (FIB) instrument, as shown in fig. 1-3.
2. And (3) placing the microsphere particles for preparing the probe in an acetone and ethanol solution for ultrasonic cleaning, and placing the cleaned particles in well-sealed ethanol or water dispersion for storage for later use.
3. And (3) placing the silicon wafer template marked with the position in an acetone and isopropanol solution for ultrasonic cleaning, and finally blowing the cleaned template by using pure nitrogen for later use.
4. Taking a drop of ethanol or deionized water dispersion of microsphere particles (200-1000 nm spherical or lamellar particles such as silicon dioxide spheres or organic drug particles are selected as required), dropping the ethanol or deionized water dispersion on the silicon wafer template marked with the position after the treatment (as shown in figure 4), and drying for later use.
5. And dripping the two-component epoxy glue (which is prepared according to a certain proportion, has the curing time of more than 30min, is dripped on a glass slide or a silicon wafer cleaned by acetone or ethanol, stirring uniformly, and then forcibly scraping off redundant glue for many times by using the side surface of the other cleaned glass slide, or performing high-speed spin coating by using a spin coater to ensure that the glue on the glass slide or the silicon wafer is as thin as possible.
6. Sequentially opening a controller and supporting software (optical and position control accessories with higher precision, such as Bruker division Icon) of the atomic force microscope, selecting a commercial sharp probe (the curvature radius is about 2-50 nm), and scanning and imaging the silicon wafer template marked with the position prepared in the step 4, as shown in FIG. 4; a well-dispersed position of the particles is obtained and this position is recorded on the basis of the label (the position between the particles is far enough to avoid interference when adhering to the probe).
7. And (3) replacing the probe with the probe prepared in the step 1, and readjusting the position and the reflection value of the laser to ensure the effective needle insertion of the atomic force microscope.
8. Fixing the prepared glass slide or silicon wafer with the epoxy glue layer in the step 5 on a sample table, moving the glass slide or silicon wafer to a relatively thin epoxy glue layer area by using a high-resolution optical microscope and a position control system which are carried by the instrument, adjusting the automatic needle insertion under the atomic force microscope contact mode, standing for 30 seconds after a probe is contacted with the epoxy glue surface, fully sticking the epoxy glue on the platform obtained in the step 1 (as shown in figure 5), and then automatically withdrawing the needle.
9. And replacing the glass slide or the silicon wafer with the epoxy glue water layer with the prepared silicon wafer template with the microsphere particles dispersed in the silicon wafer template with the positions marked in the step 4, searching the positions of the microsphere particles recorded in the step 6 by using a high-resolution optical microscope and a position control system which are arranged on the instrument, accurately positioning the needle (as shown in figure 6), and standing for 60 seconds after the probe is contacted with the surface of the epoxy glue, so that the microsphere particles can be bonded on the probe.
10. The prepared probe in 9 was removed from the cantilever holder of the atomic force microscope and placed in a clean environment for 24 hours to completely cure the epoxy glue, and a cantilever probe with submicron particles at the tip was obtained (see fig. 7 and 8).
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (9)
1. A method for preparing a submicron probe for an atomic force microscope is characterized by comprising the following steps:
firstly, cutting the front end of a micro-cantilever probe into a platform through a focused ion beam flight time secondary ion mass spectrometer;
step two, placing the microspherical particles for preparing the probe in acetone and ethanol solution for ultrasonic cleaning in sequence, placing the cleaned microspherical particles in ethanol or water dispersion for storage for later use, and obtaining dispersion liquid with the microspherical particles; sequentially placing the silicon wafer template marked with the position in acetone and isopropanol solution for ultrasonic cleaning, and finally blowing the cleaned template by using pure nitrogen for later use; taking a drop of the dispersion liquid with the microspherical particles obtained in the second step, dropping the dispersion liquid on the silicon wafer template marked with the position, drying the dispersion liquid for later use, and recording the position of the microspherical particles according to the mark through an atomic force microscope;
step three, replacing the commercial probe on the atomic force microscope with the probe prepared in the step one;
fixing a glass slide or a silicon wafer with an epoxy glue layer on a sample stage of the atomic force microscope, moving the glass slide or the silicon wafer to a relatively thin area of the epoxy glue layer by using a high-resolution optical microscope and a position control system which are carried by the atomic force microscope, adjusting needle insertion under the contact mode of the atomic force microscope, and after a probe is contacted with the surface of the epoxy glue, fully sticking the epoxy glue on the platform obtained in the step one, and withdrawing the needle;
replacing the glass slide or the silicon wafer with the epoxy glue water layer with the silicon wafer template which is obtained in the second step and is dispersed with the microsphere particles and marked with the positions, searching the positions of the microsphere particles recorded in the second step by using a high-resolution optical microscope and a position control system which are carried by the atomic force microscope, accurately positioning the probe, and bonding the microsphere particles to the probe after the microsphere particles contact the surface of the epoxy glue on the probe to obtain the submicron probe for the atomic force microscope; the submicron probe for the atomic force microscope is a micro-cantilever probe with a submicron particle at the tip.
2. The method for preparing a submicron probe for an atomic force microscope according to claim 1, wherein the micro-cantilever of the micro-cantilever probe in the first step is a micro-cantilever with a tip, a triangular micro-cantilever or a rectangular micro-cantilever; the width of the platform is 0.5-1.5 microns.
3. The method for preparing a submicron probe for an atomic force microscope according to claim 1, wherein the step two of recording the position of the microspheroidal particle according to the mark by the atomic force microscope comprises the following specific operations: sequentially opening a controller and supporting software of the atomic force microscope, selecting a commercial probe, scanning and imaging the silicon wafer template dispersed with the microsphere particles, and recording the positions of the microsphere particles with better dispersibility according to the marks; the curvature radius of the needle point of the commercial probe is 2-50 nm; the better dispersibility means that the positions of the microspheroidal particles are far enough to avoid the microspheroidal particles from influencing each other when the microspheroidal particles are adhered to the probe.
4. The method for preparing a submicron probe for an atomic force microscope according to claim 1, wherein after the probe is replaced in the third step, the position and the reflection value of the laser are readjusted to ensure the effective insertion of the atomic force microscope.
5. The method for preparing a submicron probe for an atomic force microscope according to claim 1, wherein the preparation operation of the slide glass or the silicon wafer with the epoxy glue layer in the fourth step is specifically: and dripping the two-component epoxy glue on the cleaned glass slide or silicon wafer, uniformly stirring, and scraping the redundant two-component epoxy glue from the side surface of the other cleaned glass slide, or spin-coating at high speed by using a spin-coating instrument to ensure that the epoxy glue on the surface of the glass slide or silicon wafer is as thin as possible, thereby obtaining the glass slide or silicon wafer with the epoxy glue water layer.
6. The method for preparing a submicron probe for an atomic force microscope according to claim 5, wherein the curing time of the two-component epoxy glue is 30 minutes or more.
7. The method for preparing a submicron probe for an atomic force microscope according to claim 1, wherein the fifth step further comprises removing the prepared probe from the cantilever mount of the atomic force microscope after the bonding of the microsphere particles to the probe, and placing the probe in a clean environment for 24 hours to completely cure the epoxy glue.
8. The method for preparing a submicron probe for an atomic force microscope as set forth in claim 1, wherein the microspheroidal particle is a spherical or lamellar particle having a size of 200-1000nm, and further wherein the microspheroidal particle is a silica microsphere or an organic drug particle.
9. A submicron probe for an atomic force microscope obtained by the production method according to claim 1.
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| CN110155938B (en) * | 2019-06-11 | 2022-01-28 | 西南交通大学 | Method for preparing microsphere probe based on micro-cantilever transfer |
| CN110542768A (en) * | 2019-08-07 | 2019-12-06 | 合肥学院 | method for processing micro-cantilever probe for measuring ultralow friction coefficient |
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| CN112180124A (en) * | 2020-08-31 | 2021-01-05 | 上海交通大学 | Preparation method of submicron probe for atomic force microscope |
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| CN116553475B (en) * | 2023-03-23 | 2024-01-30 | 清华大学 | Laser-based single-particle microelectrode preparation method |
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| CN107430148A (en) * | 2015-02-03 | 2017-12-01 | Fei Efa有限公司 | Method using scanning probe microscopy to characteristic imaging |
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