CN113049853A - Method for preparing tilting AFM probe tip with size and tilt angle controllable and ultra-large height-to-width ratio - Google Patents
Method for preparing tilting AFM probe tip with size and tilt angle controllable and ultra-large height-to-width ratio Download PDFInfo
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- CN113049853A CN113049853A CN202110273278.6A CN202110273278A CN113049853A CN 113049853 A CN113049853 A CN 113049853A CN 202110273278 A CN202110273278 A CN 202110273278A CN 113049853 A CN113049853 A CN 113049853A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention provides a method for preparing a tilting AFM probe tip with a size and a tilting angle controllable and an ultra-large height-width ratio. According to the technical scheme, the focused ion beam is utilized to irradiate the suspended micro-nano metal structure to enable the micro-nano metal structure to be folded upwards, the characteristics of angle and irradiation energy correlation are adopted, a metal film is deposited on the top end of the cantilever beam, different focused ion beam parameters are selected to irradiate the suspended part of the metal structure outside the cantilever beam, and the ultra-large aspect ratio inclined AFM probe tip with the controllable inclination angle is prepared. As a brand-new manufacturing method of the AFM probe with the large height-width ratio, the method is controllable in consistency, suitable for various materials, simple and suitable for mass production. As a core component of the atomic force microscope, the product has higher detection precision.
Description
Technical Field
The invention relates to the technical field of micro-nano processing, in particular to a method for preparing a tilting AFM probe tip with a controllable size and a controllable tilting angle and an ultra-large height-width ratio.
Background
An Atomic Force Microscope (AFM) is a common detection device, and the basic principle is that the surface appearance of a sample is detected by utilizing the acting force between a probe tip and atoms on the surface of the sample, so that not only can three-dimensional surface imaging with nanoscale resolution be realized, but also the sample does not need to be conductive, can work in complex environments such as atmosphere, liquid, low temperature and the like, and can image active samples such as single cells, single molecules and the like. Atomic force microscope probes are classified into contact probes, non-contact/tapping mode probes, conductive probes, magnetic probes, high aspect ratio probes, diamond-like atomic force microscope probes, and the like, according to the use. The shape of the needle tip has great influence on the detection precision, and the sharper the needle tip is, the higher the detection precision is. Especially for the sample surface with large fluctuation and narrow and deep groove, the detection result of the common probe is easy to deviate from the actual appearance of the sample, as shown in fig. 1. The aspect ratio of the probe is extremely important, and the research of the high aspect ratio probe becomes a hot spot in the current research field of the AFM probe.
The method for preparing the probe with the large height-to-width ratio mainly comprises a carbon nano tube adhesion method, a focused ion beam etching method, a focused ion beam deposition method, a metal particle catalyst induced silicon nanowire growth method and the like. The carbon nanotube adhering method is to put AFM probe into carbon nanotube dispersing liquid and to adhere carbon nanotube to AFM probe with electric field force. In the method, the size and the direction randomness of the carbon nano tube attached to the probe tip is large, so that the size and the inclination angle of the obtained tip with the large aspect ratio cannot be accurately controlled. The focused ion beam etching method is to bombard the tip of a common probe with focused ion beams to sharpen the tip, and the method has higher cost and longer time consumption and is not suitable for batch production. The focused ion beam deposition method is to deposit a nanowire on a common probe tip as a new tip by using a focused ion beam. The method is also high in cost, long in time consumption and not suitable for mass production. The metal particle catalyst induced silicon nanowire growth method is that gold or other metal particles are used as a catalyst and attached to the surface of silicon, and then the chemical vapor deposition silicon nanowire is used as a probe tip. The method has poor controllability for the size of the needle tip due to the inherent disadvantages of chemical vapor deposition.
Disclosure of Invention
The invention aims to provide a method for preparing a tilting AFM probe tip with a size and a tilting angle controllable and an ultra-large height-to-width ratio, aiming at overcoming the technical problems of high cost, poor consistency and the like of the conventional preparation process of the AFM probe with the large height-to-width ratio at present.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
the preparation method of the tilted AFM probe tip with the ultra-large height-width ratio and the controllable tilt angle comprises the following steps:
1) spin-coating 200-400 nanometer PMMA photoresist on the surface of the cleaned SOI wafer, and baking for 1-2 minutes at 180 ℃;
2) exposing the sample wafer obtained in the step 1) by using an electron beam exposure machine, wherein the exposure dose is 500-2(ii) a After exposure, the sample wafer is put into a developing solution for development for 30-50s, and then is put into a fixing solution for fixation for 30-50 s;
3) directly depositing 20-30 nm Cr or Ti metal film on the sample wafer obtained in the step 2) by using thermal evaporation coating equipment, electron beam evaporation coating equipment or magnetron sputtering coating equipment;
4) immersing the sample wafer obtained in the step 3) in acetone, and immersing for 10-30 minutes at room temperature (so that the photoresist naturally falls off and a metal structure is left);
5) respectively etching the front and back sides of the sample obtained in the step 4) to prepare an AFM probe cantilever beam part and a base part (at the moment, the metal structure part is in a suspended state);
6) and 5) irradiating the metal nanowire structure by using a focused ion beam to fold the sample wafer obtained in the step 5).
Preferably, the SOI wafer in the step 1) is composed of a device Si layer and an insulating SiO layer2Layer and substrate Si layer, wherein the device Si layer, insulating SiO2The thickness of the layer and the substrate Si layer are respectively 1-5 microns, 0.5-2 microns and 350-500 microns.
Preferably, step 3) is replaced by the following step 3 a): depositing a 3-5 nanometer Cr or Ti adhesion layer on the sample wafer obtained in the step 2) by using thermal evaporation coating equipment, electron beam evaporation coating equipment or magnetron sputtering coating equipment, and then depositing a 20-30 nanometer metal film.
Preferably, the metal of the metal film is selected from one or several of the following components: w, Pt, Au.
Preferably, step 4) is carried out using a liftoff process.
Preferably, in step 5), the front and back sides of the sample are etched respectively by using photolithography and deep silicon etching Bosch process (the Bosch process has a horizontal etching of tens of nanometers, so silicon under the metal nanowire structure is etched away).
Preferably, in the step 6), the AFM probe tips in a vertical state or different inclination angles are obtained by adjusting the ion beam irradiation parameters.
Preferably, in the step 1), the SOI wafer is cleaned by RCA standard process, so that the surface of the UV lamp is clean and free of impurities under microscopic examination.
Preferably, the spin coating conditions in step 1) are as follows: the forward rotation speed is 500r/min and the time is 5s, and the rear rotation speed is 4000r/min and the time is 40 s.
Preferably, in step 2), the acceleration voltage of the electron beam exposure apparatus is 100KeV and the beam current is 100 pA.
The invention provides a method for preparing a tilting AFM probe tip with a size and a tilting angle controllable and an ultra-large height-width ratio. According to the technical scheme, the focused ion beam is utilized to irradiate the suspended micro-nano metal structure to enable the micro-nano metal structure to be folded upwards, the characteristics of angle and irradiation energy correlation are adopted, a metal film is deposited on the top end of the cantilever beam, different focused ion beam parameters are selected to irradiate the suspended part of the metal structure outside the cantilever beam, and the ultra-large aspect ratio inclined AFM probe tip with the controllable inclination angle is prepared. As a brand-new manufacturing method of the AFM probe with the large height-width ratio, the method is controllable in consistency, suitable for various materials, simple and suitable for mass production. As a core component of the atomic force microscope, the product has higher detection precision.
Drawings
FIG. 1 is a graph of the difference in measurements for different types of probes;
FIG. 2 is a flow chart of the method of the present invention;
FIG. 3 is a top view of the metal nanowire structure of FIG. 2, 2 e;
in the figure:
1. SOI silicon chip 2, photoresist 3, metal film 4 and probe substrate
5. A probe cantilever 6 and a probe tip.
Detailed Description
Hereinafter, specific embodiments of the present invention will be described in detail. Well-known structures or functions may not be described in detail in the following embodiments in order to avoid unnecessarily obscuring the details. Approximating language, as used herein in the following examples, may be applied to identify quantitative representations that could permissibly vary in number without resulting in a change in the basic function. Unless defined otherwise, technical and scientific terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Example 1
The preparation method of the tilted AFM probe tip with the ultra-large height-width ratio and the controllable tilt angle comprises the following steps:
1. the double-side polished SOI wafer is selected as a raw material and comprises a device silicon layer, a silicon dioxide layer and a substrate silicon layer, wherein the thicknesses of the device silicon layer, the silicon dioxide layer and the substrate silicon layer are respectively 2.5 micrometers, 0.5 micrometer and 350 micrometer. (as shown in FIG. 2 a)
2. And cleaning the sample wafer by the RCA standard process to achieve the cleanness and no impurities of the surface of the ultraviolet lamp under microscopic examination.
3. And spin-coating a layer of PMMA photoresist with the thickness of 200 nanometers on the surface of the sample wafer by using the forward rotation speed of 500r/min for 5s and the backward rotation speed of 4000r/min for 40 s. Placing on a hot plate, and heating and baking at 180 deg.C for 1 min. (as shown in FIG. 2 b)
4. Performing electron beam lithography on the photoresist with an accelerating voltage of 100KeV and a beam current of 100pA at a dose of 900mJ/cm2。
5. The sample piece is placed in MIBK 1:3IPA for development at room temperature for 40s, then placed in IPA solution for fixation for 30s, taken out and dried by blowing. A long stripe groove pattern with triangular tips was obtained with a length of 5 microns and a width of 20 nm. (as shown in FIG. 2 c)
6. And (3) evaporating and plating a 5 nanometer Cr +15n nanometer W metal film on the sample wafer by using thermal evaporation coating equipment. (as shown in FIG. 2 d)
7. And (3) placing the sample wafer in an acetone solution, soaking for 10min at room temperature, and naturally stripping the photoresist to leave a metal structure. (as shown in FIGS. 2e and 3)
8. Firstly, coating 10 microns of AZ4620 photoresist on the front surface of a sample wafer as a protective layer, then coating 10 microns of AZ4620 photoresist on the back surface of the sample wafer, and using the coating rate of 500r/min for 10s before and 2000r/min for 40s after. Placing on a hot plate, and baking the sample wafer at 100 deg.C for 3 min.
9. The sample was photo-etched using 405 nm light at an exposure dose of 1000mJ/cm2。
10. Developing with AZ positive photoresist developer for 5min at room temperature, and then rinsing with deionized water and drying.
11. And etching the back surface to the silicon oxide layer in the middle of the SOI silicon wafer by a dry method, and removing residual glue.
12. And (3) uniformly coating 1.6-micron AZ5214 photoresist on the front surface of the sample wafer, wherein the coating rate is 500r/min before 5s and 2000r/min after 40 s. Placing on a hot plate, and baking the sample wafer at 100 deg.C for 1 min.
13. The sample was photo-etched using 405 nm light at an exposure dose of 100mJ/cm2。
14. Developing with AZ positive photoresist developer for 3min at room temperature, and then rinsing with deionized water and drying.
15. And dry etching the back surface to the intermediate silicon oxide layer of the SOI silicon wafer.
16. And soaking the BOE solution for 5min to obtain the probe substrate and the cantilever structure. (as shown in FIG. 2 g)
17. And scanning the metal suspension part by using a focused ion beam to enable the metal suspension part to be folded upwards. A gallium ion source is adopted, the accelerating voltage is 30kV, and the beam current is 150 pA. The obtained metal probe is vertical at an angle of 80 degrees with the horizontal direction, and the preparation of the probe is finished. (as shown in FIG. 2 j)
The key point of the invention is that ion beams with different energies are utilized to irradiate the suspended metal nanowire structure to obtain the needle tip with high aspect ratio and different angles of inclination. It will be apparent to those skilled in the art that various changes and adjustments can be made in the parameters of the steps according to the embodiments of the present invention, and such changes and adjustments should not be excluded from the scope of the present invention.
Example 2
The preparation method of the tilted AFM probe tip with the ultra-large height-width ratio and the controllable tilt angle comprises the following steps:
1. cleaning the SOI wafer, spin-coating 200-400 nanometer PMMA photoresist on the surface of the cleaned SOI wafer, and baking the cleaned SOI wafer for 1-2 minutes at 180 ℃. Wherein the SOI wafer is composed of a device Si layer, an insulating SiO2 layer and a substrate Si layer. The thicknesses of the device Si layer, SiO2 layer, and substrate Si layer were 1-5 microns, 0.5-2 microns, and 350-500 microns, respectively.
2. Exposing the sample coated with the glue by an electron beam exposure machine with the exposure dose of 500-1000mJ/cm2. After exposure, the sample wafer is put into a developing solution for development for 30-50s, and then is put into a fixing solution for fixation for 30-50 s.
3. Directly depositing 20-30 nm Cr or Ti metal film by thermal evaporation, electron beam evaporation or magnetron sputtering equipment. Or depositing a 3-5 nm Cr or Ti adhesion layer, and then depositing 20-30 nm W, Pt, Au and other metal films.
4. And (3) soaking the exposed and developed sample in acetone by a liftoff process for 10-30 minutes at room temperature, and naturally dropping the photoresist to leave a metal structure.
5. And respectively etching the front side and the back side of the sample by utilizing photoetching and deep silicon etching Bosch processes to prepare the cantilever beam part and the base part of the AFM probe, wherein the metal structure part is in a suspended state. (since this step is not a core step of the present invention, it is not described in detail, it should be noted that the Bosch process has a lateral etch of tens of nanometers, and thus the silicon under the metal nanowire structure is etched away.)
6. And (3) irradiating the metal nanowire structure by using a focused ion beam to fold the metal nanowire structure, and adjusting the ion beam irradiation parameters to obtain the AFM probe tips in a vertical state or different inclination angles.
The embodiments of the present invention have been described in detail, but the description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. Any modification, equivalent replacement, and improvement made within the scope of the application of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the tilted AFM probe tip with the ultra-large height-width ratio and the controllable tilt angle is characterized by comprising the following steps of:
1) spin-coating 200-400 nanometer PMMA photoresist on the surface of the cleaned SOI wafer, and baking for 1-2 minutes at 180 ℃;
2) exposing the sample wafer obtained in the step 1) by using an electron beam exposure machine, wherein the exposure dose is 500-2(ii) a After exposure, the sample wafer is put into a developing solution for development for 30-50s, and then is put into a fixing solution for fixation for 30-50 s;
3) directly depositing 20-30 nm Cr or Ti metal film on the sample wafer obtained in the step 2) by using thermal evaporation coating equipment, electron beam evaporation coating equipment or magnetron sputtering coating equipment;
4) immersing the sample wafer obtained in the step 3) in acetone for 10-30 minutes at room temperature;
5) respectively etching the front and back surfaces of the sample wafer obtained in the step 4) to prepare an AFM probe cantilever beam part and a base part;
6) and 5) irradiating the metal nanowire structure by using a focused ion beam to fold the sample wafer obtained in the step 5).
2. The method for preparing the tilted AFM probe tip with the ultra-large aspect ratio and the controllable size and the tilt angle as claimed in claim 1, wherein the SOI wafer in the step 1) is composed of a device Si layer and an insulating SiO2Layer and substrate Si layer, wherein the device Si layer, insulating SiO2The thickness of the layer and the substrate Si layer are respectively 1-5 microns, 0.5-2 microns and 350-500 microns.
3. The method for preparing the tilted AFM probe tip with the ultra-large aspect ratio and the controllable size and the tilt angle of claim 1, wherein the step 3) is replaced by the following step 3 a): depositing a 3-5 nanometer Cr or Ti adhesion layer on the sample wafer obtained in the step 2) by using thermal evaporation coating equipment, electron beam evaporation coating equipment or magnetron sputtering coating equipment, and then depositing a 20-30 nanometer metal film.
4. The method for preparing the tilted AFM probe tip with the ultra-large aspect ratio and the controllable size and the tilt angle as claimed in claim 3, wherein the metal of the metal thin film is selected from one or more of the following components: w, Pt, Au.
5. The method for preparing the tilted AFM probe tip with the ultra-large aspect ratio and the controllable size and the tilt angle of the claim 1, wherein the step 4) is performed by a liftoff process.
6. The method for preparing the tilted AFM probe tip with the ultra-large aspect ratio and the controllable size and the tilt angle as recited in claim 1, wherein in the step 5), the front and the back of the sample are respectively etched by utilizing photolithography and deep silicon etching Bosch processes.
7. The method for preparing the tilted AFM probe tip with the ultra-large aspect ratio and the controllable size and the tilt angle according to claim 1, wherein in the step 6), the AFM probe tip in a vertical state or at different tilt angles is obtained by adjusting ion beam irradiation parameters.
8. The method for preparing the AFM probe tip with the size and the inclination angle controllable and the ultra-large aspect ratio, according to claim 1, is characterized in that in the step 1), the SOI sheet is cleaned by an RCA standard process, so that the surface of an ultraviolet lamp for microscopic examination is clean and free of impurities.
9. The method for preparing the tilted AFM probe tip with the ultra-large aspect ratio and the controllable size and the tilt angle according to claim 1, wherein the spin coating conditions in the step 1) are as follows: the forward rotation speed is 500r/min and the time is 5s, and the rear rotation speed is 4000r/min and the time is 40 s.
10. The method for preparing the tilted AFM probe tip with the ultra-large aspect ratio and the controllable size and the tilt angle as claimed in claim 1, wherein in the step 2), the acceleration voltage of the electron beam exposure machine is 100KeV, and the beam current is 100 pA.
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Cited By (2)
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| CN113582129A (en) * | 2021-07-27 | 2021-11-02 | 浙江大学 | Large-aspect-ratio probe based on metal-assisted chemical etching and manufacturing method thereof |
| CN113917190A (en) * | 2021-10-08 | 2022-01-11 | 中国科学院上海微系统与信息技术研究所 | Method for customizing AFM probe based on FIB equipment and atomic force microscope |
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