CN109765407B - Preparation method of large length-diameter ratio probe based on one-dimensional nano material - Google Patents
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Abstract
The invention discloses a preparation method of a large length-diameter ratio probe based on a one-dimensional nano material, the probe comprises an atomic force microscope common silicon probe and a tip nano structure, and the preparation method of the probe comprises the following steps: firstly, installing an atomic force microscope silicon probe on a measuring head of atomic force microscope equipment which is provided with a liquid groove capable of being used as a tapping mode; then, injecting a small amount of solution prepared by mixing the two solutions, namely growth solution, into the liquid pool, and manually controlling needle insertion to pick up the growth solution; and finally, after the growth liquid is picked up, synthesizing a one-dimensional nano material at the tip of the prefabricated silicon needle tip to prepare the needle tip with a large length-diameter ratio. The invention overcomes the problem that the imaging false image is easy to generate when the atomic force common silicon probe is used for imaging the fine structure with the high depth-to-width ratio at present, the length-diameter ratio of the probe obtained by the method is larger, and the structure can be measured with better resolution.
Description
Technical Field
The invention belongs to the technical field of micro-nano manufacturing and measurement, and particularly relates to a preparation method of a probe with a large length-diameter ratio based on a one-dimensional nano material.
Background
In recent years, fields such as large-scale integrated circuits, micro-spacecraft control, carrier stealth and the like are rapidly developed, and the emerging technologies depend on complex and precise fine structures to a great extent, particularly high-aspect-ratio fine structures with high complexity, so that the method has very wide application prospects in the fields. Compared with a planar structure, a three-dimensional structure with a high aspect ratio (the aspect ratio is the ratio of the maximum depth to the width of a fine structure) has a larger specific surface area, which means that a larger available space can be obtained in a vertical dimension under the condition of keeping the same substrate area, and a new idea and a wider application field are developed for the upgrading of micro-nano devices. However, due to the size of the high aspect ratio microstructure, it is difficult to perform accurate measurement and characterization in the depth direction, and it is difficult to develop more intensive research on the function, the application, and the novel manufacturing process of the structure. At present, the measurement methods for the fine structure with high depth-to-width ratio at home and abroad are mainly divided into two major types, one is an optical non-contact measurement method represented by various laser interferometers, but the measurement is limited by small depth of field and small focusing range of a lens; a contact measurement method of scanning probe microscopy represented by an atomic force microscope has high resolution, but the length-diameter ratio (length/diameter ratio) of a common probe is small, the resolution is limited by the curvature radius of a needle point, and the measurement requirement of a high-aspect-ratio structure is difficult to meet.
The probe of the atomic force microscope is one of the most central components and plays a decisive role in the imaging performance. One-dimensional nanomaterials, such as nanowires, nanotubes, nanobelts, nanorods, etc., have been widely studied due to their excellent electrical, mechanical, optical, and other properties. Compared with a two-dimensional nano film and a zero-dimensional nano particle, the one-dimensional nano material has the following advantages: firstly, the one-dimensional nano material can be prepared by a chemical method under a simpler growth condition, and almost has no requirement on the material and the shape of a substrate, the growth conditions required by the nano film and the particles obtained by the atomic layer deposition method are extremely strict, and the equipment is very expensive; and secondly, because the size of the one-dimensional nano material is in a nano scale in two dimensions, the mechanical elasticity, yield limit and initial property of the one-dimensional nano material are far beyond those of a block material, the one-dimensional nano material is not easy to break and strain in structure even if large mechanical deformation such as bending occurs, and can bear large acting force and strain, the nano film is easy to crack under small strain, and the nano particles almost have no mechanical elasticity. The one-dimensional nano material with larger major diameter is combined with the atomic force microscope, so that the imaging performance of the atomic force microscope can be greatly improved. At present, methods for preparing carbon nanotube probes, such as conductive adhesive bonding, pore growth, and manual assembly, are available. The conductive adhesive bonding method uses an optical microscope, and when the carbon nanotubes are bonded, thicker carbon nanotube bundles are easy to select, but the finest carbon nanotubes are easy to select, so that the imaging resolution is influenced. The core problems restricting the application at present are low preparation efficiency, high cost and easy generation of imaging false images.
Disclosure of Invention
In view of the defects and shortcomings in the prior art, one of the purposes of the present invention is to provide a method for preparing a probe with a large length-diameter ratio based on a one-dimensional nano material, which meets the requirements of high aspect ratio structure measurement, stability, reliability, high precision, etc.
The invention is realized by adopting the following technical scheme:
a method for preparing a probe with large length-diameter ratio based on a one-dimensional nano material comprises an atomic force microscope common silicon probe and a tip nanostructure, and the method for preparing the probe comprises the following steps:
firstly, installing an atomic force microscope silicon probe on a measuring head of atomic force microscope equipment which is provided with a liquid groove capable of being used as a tapping mode; then, injecting a small amount of solution prepared by mixing the two solutions, namely growth solution, into the liquid pool, and manually controlling needle insertion to pick up the growth solution; and finally, after the growth liquid is picked up, synthesizing a one-dimensional nano material at the tip of the prefabricated silicon needle tip to prepare the needle tip with a large length-diameter ratio.
A further improvement of the invention is that the method comprises in particular the steps of:
1) cleaning of substrates
The method comprises the following steps of (1) cleaning a newly dissociated mica sheet serving as a substrate, using a culture dish as a liquid pool for containing liquid, and sequentially using acetone, ethanol and deionized water;
2) preparation of growth liquid
First, a first solution is prepared: dissolving aluminum trichloride hexahydrate in an ethanol solution, slowly injecting a silicon tetrachloride solution by using a liquid transfer device, and placing the prepared solution in a constant-temperature magnetic heating stirrer for uniformly mixing; preparing a second solution: dissolving ferric trichloride hexahydrate in an ethanol solution, mixing the two solutions, placing the two solutions in a constant-temperature magnetic heating stirrer for stirring, and then standing the solution at room temperature for 12-24 hours;
3) picking up growth liquid
Firstly, calibrating the sensitivity of a needle tip; after calibration is finished, fixing the substrate material on the bottom surface of the liquid pool by using glue which is insoluble in the growth liquid, and mounting the prefabricated silicon probe on the measuring head of the atomic force microscope after the glue is completely cured; adjusting the position of laser, wherein the needle point is most sensitive to force, the laser is adjusted to be shot at the needle point, the contact between the needle point and the growth liquid level is adjusted through the detection of a feedback system, and the amplitude of the micro-cantilever is further controlled, so that the growth liquid is picked up;
4) synthesis of the tip of a needle
And carrying out chemical reaction on the needle tip by adopting a chemical vapor deposition method to prepare probes with different types of tips.
The further improvement of the invention is that in the step 1), the time for cleaning the mica sheets by adopting acetone, ethanol and deionized water is 5-10min in sequence.
The further improvement of the invention is that in the step 2), the mass of aluminum trichloride hexahydrate in the first solution in the growth solution is 2.4-4.8g, the volume of ethanol is 15-30mL, and the volume of silicon tetrachloride solution is 1.2-2.4 mL.
The further improvement of the invention is that in the step 2), the mass of ferric trichloride hexahydrate in the second solution in the growth solution is 2-4g, and the volume of ethanol is 5-10 mL.
The invention further improves that in the step 3), a method of making a force curve on a rigid silicon sample is adopted to calibrate the sensitivity.
The invention further improves that in the step 3), the growth liquid is picked up by adopting a peak force tapping mode of an atomic force microscope.
The invention is further improved in that in the step 4), the nano-materials synthesized by the probe tip comprise nanowires, nanorods, nanotubes and nanofibers.
The invention has the following beneficial technical effects:
according to the step implementation of the preparation method, the prefabricated needle point is used for picking up the growth liquid and then synthesizing the tip with the large length-diameter ratio at the needle point. The invention overcomes the problem that the imaging false image is easy to generate when the atomic force common silicon probe is used for imaging the fine structure with high depth-to-width ratio at present, the length-diameter ratio of the probe obtained by the method is larger and is more than or equal to 10: 1, measurement of the structure can lead to better resolution.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is a schematic diagram of the operation of picking up growth liquid using a preformed needle tip in an embodiment of the present invention.
FIG. 2 is a schematic diagram of the force variation with time during the operation of picking up growth liquid in an embodiment of the present invention.
FIG. 3 is a double heating zone vacuum tube furnace used to prepare the tips in an embodiment of the present invention.
FIG. 4 is a scanning electron microscope photograph of the probe prepared in the example of the present invention.
FIG. 5 is a scanning electron microscope image of a high aspect ratio sample in accordance with an embodiment of the present invention.
FIG. 6 is a photograph of topography measurements of a high aspect ratio sample with probes prepared in an embodiment of the present invention.
Detailed Description
The invention is further explained below with reference to the drawings and the detailed description.
The invention provides a method for preparing a probe for measuring a high-length-diameter ratio fine structure, the probe comprises an atomic force microscope common silicon probe and a tip nanostructure, and the method for preparing the probe comprises the following steps: firstly, installing an atomic force microscope silicon probe on a measuring head of atomic force microscope equipment (Bruker Dimension Icon) which is provided with a tapping mode liquid tank, then injecting a small amount of growth liquid into the liquid tank, manually controlling the needle insertion to pick up the growth liquid, and finally synthesizing a nano material at the tip of a prefabricated silicon needle tip after the growth liquid is picked up to prepare the needle tip with a large length-diameter ratio.
The method comprises the following specific steps:
1) cleaning of substrates
The newly dissociated mica sheet is used as a substrate, a culture dish is used as a liquid pool for containing liquid, and the mica sheet is washed by acetone, ethanol and deionized water in sequence. Wherein the time for cleaning the mica sheet by using acetone, ethanol and deionized water is 5-10min in sequence.
2) Preparation of growth liquid
First, a first solution is prepared: dissolving aluminum trichloride hexahydrate in an ethanol solution, slowly injecting a silicon tetrachloride solution by using a liquid transfer device, and placing the prepared solution in a constant-temperature magnetic heating stirrer for uniformly mixing; preparing a second solution: ferric chloride hexahydrate is dissolved in ethanol solution. Mixing the two solutions, placing in a constant-temperature magnetic heating stirrer, stirring, and standing at room temperature for 12-24 h. Wherein the mass of aluminum trichloride hexahydrate in the first solution used for preparing the growth solution is 2.4-4.8g, the volume of ethanol is 15-30mL, the volume of silicon tetrachloride solution is 1.2-2.4mL, the mass of ferric trichloride hexahydrate in the first solution used for preparing the growth solution is 2-4g, and the volume of ethanol is 5-10 mL.
3) Picking up growth liquid
Firstly, the sensitivity of the needle point needs to be calibrated, and the method of making a force curve on a rigid silicon sample is adopted to calibrate the sensitivity. And after calibration is finished, fixing the substrate material on the bottom surface of the liquid pool by using glue insoluble in the growth liquid, and mounting the prefabricated silicon probe on the measuring head of the atomic force microscope after the glue is completely cured. The position of the laser is adjusted, and the laser is adjusted to be hit at the needle point because the needle point is most sensitive to force. The contact between the needle tip and the growth liquid level is adjusted through the detection of a feedback system, and then the amplitude of the micro-cantilever is controlled, so that the growth liquid is picked up.
4) Synthesis of the tip of a needle
And (3) carrying out chemical reaction on the needle tip by adopting a chemical vapor deposition method to prepare probes with different types of tips, wherein the nano materials synthesized by the probe tip comprise nanowires, nanorods, nanotubes and nano fibers.
Example 1
(1) Cleaning of substrates
The newly dissociated mica sheet is used as a substrate, the culture dish is used as a liquid pool for containing liquid, and in order to ensure the purity of the liquid and avoid introducing impurities, the needle point is polluted, and the cleanliness of the surface of a sample needs to be ensured. Immersing mica sheets in acetone for 10min, clamping the mica sheets by using tweezers, soaking the mica sheets in ethanol, clamping the mica sheets by using the tweezers after 10min, washing the mica sheets by using deionized water for 5min, immediately blowing the mica sheets by using nitrogen, and storing the cleaned mica sheet substrate in a closed container to prevent excessive water vapor in the air from being adsorbed.
(2) Preparation of growth liquid
First, a first solution is prepared: dissolving 2.4g of aluminum trichloride hexahydrate in 15mL of ethanol solution, slowly injecting 1.2mL of silicon tetrachloride solution by using a liquid transfer device, and placing the prepared solution in a constant-temperature magnetic heating stirrer for uniformly mixing; preparing a second solution: 2.0g of ferric chloride hexahydrate was dissolved in 5mL of an ethanol solution. Mixing the two solutions, placing the two solutions in a constant-temperature magnetic heating stirrer for stirring, and standing the mixture for 12 to 24 hours at room temperature. The two solutions are prepared without any sequence relation.
(3) Picking up growth liquid
Firstly, the sensitivity of a needle point needs to be calibrated, and the sensitivity is calibrated by a method of making a force curve on a rigid silicon sample in an experiment. And obtaining a curve of the deformation quantity of the cantilever beam and the height of the piezoelectric ceramic relative to the surface of the sample through sensitivity. The experimental process adopts atomic force microscope's peak force mode of tapping, drives little cantilever vibration during scanning promptly and makes needle point and growth liquid level intermittent contact, and the amplitude reduces when the needle point receives the basement effort, and feedback system adjusts the contact of needle point and growth liquid level through detecting this change, and then control little cantilever amplitude to pick up growth liquid. The operation diagram of the growth liquid pickup is shown in fig. 1, wherein 1 is a substrate, 2 is a liquid pool, 3 is position sensitive detection, 4 is a laser, 5 is a cantilever beam, 6 is a growth liquid level, and 7 is a needle point. The picking process is divided into five states which respectively correspond to points A-E in the figure 2, wherein the point A is a state that the probe is close to the growth liquid level and is not contacted; in the section B-C, the force borne by the needle tip is gradually increased, and the needle tip at the point C is contacted with the liquid level; due to the repulsion between the needle tip and the growth liquid sample, after the needle tip is separated from the liquid surface, the growth liquid can generate adhesion force with the needle tip to be adhered to the tip; as the tip is moved further away, the force experienced by the tip decreases progressively as shown at point E in figure 2.
(4) Synthesis of the tip of a needle
After the growth liquid is picked up, the carbon nanotubes are synthesized at the tip of the prefabricated needle tip, and the specific process is realized in a double-heating-zone vacuum tube furnace as shown in fig. 3, wherein 8 is a tube furnace, 9 is a quartz tube, and 10 is a quartz boat. Placing the prefabricated needle tip on a quartz boat, introducing methane with the flow of 1000sccm by taking the methane as a carbon source, wherein the temperature is 950 ℃, and the time is 10 min; then introducing 130sccm hydrogen for 10 min; finally, the temperature in the furnace is cooled to room temperature in a hydrogen atmosphere. The resulting tip was prepared as shown in FIG. 4.
A groove-like structure with a high aspect ratio was selected as a sample, and a scanning electron microscope photograph of the structure is shown in FIG. 5. FIG. 6 shows the result of imaging a sample with a high aspect ratio structure using the prepared probe, which is consistent with the actual topography. The result proves that the probe manufactured by the invention can obtain a high-quality morphology image of a fine structure with a high depth-width ratio.
Example 2
The steps of cleaning the substrate and picking up the growth liquid are the same as those of the embodiment 1; the difference between the embodiment and the embodiment 1 is that the first solution prepared in the step (2) contains 4.8g of aluminum trichloride hexahydrate, 30mL of ethanol and 2.4mL of silicon tetrachloride; and (3) after the ferric trichloride hexahydrate in the second solution is 4g and the ethanol capacity is 10mL, and the growth solution is picked up in the step (4), synthesizing the silicon oxide nanowire at the tip of the prefabricated needle tip, taking silane gas as a silicon source, controlling the flow to be 10sccm, simultaneously introducing 100sccm high-purity helium as a carrier gas, reacting for 2 hours, and rapidly cooling the sample to room temperature under the protection of the high-purity helium after the reaction.
Claims (7)
1. A method for preparing a probe with large length-diameter ratio based on a one-dimensional nano material is characterized in that the probe comprises an atomic force microscope common silicon probe and a tip nanostructure, and the method for preparing the probe comprises the following steps:
firstly, installing an atomic force microscope silicon probe on a measuring head of atomic force microscope equipment which is provided with a liquid groove capable of being used as a tapping mode; then, injecting a small amount of solution prepared by mixing the two solutions, namely growth solution, into the liquid pool, and manually controlling needle insertion to pick up the growth solution; finally, after the growth liquid is picked up, synthesizing a one-dimensional nano material at the tip of the prefabricated silicon needle tip to prepare the needle tip with a large length-diameter ratio;
the method specifically comprises the following steps:
1) cleaning of substrates
The method comprises the following steps of (1) cleaning a newly dissociated mica sheet serving as a substrate, using a culture dish as a liquid pool for containing liquid, and sequentially using acetone, ethanol and deionized water;
2) preparation of growth liquid
First, a first solution is prepared: dissolving aluminum trichloride hexahydrate in an ethanol solution, slowly injecting a silicon tetrachloride solution by using a liquid transfer device, and placing the prepared solution in a constant-temperature magnetic heating stirrer for uniformly mixing; preparing a second solution: dissolving ferric trichloride hexahydrate in an ethanol solution, mixing the two solutions, placing the two solutions in a constant-temperature magnetic heating stirrer for stirring, and then standing the solution at room temperature for 12-24 hours;
3) picking up growth liquid
Firstly, calibrating the sensitivity of a needle tip; after calibration is finished, fixing the substrate material on the bottom surface of the liquid pool by using glue which is insoluble in the growth liquid, and mounting the prefabricated silicon probe on the measuring head of the atomic force microscope after the glue is completely cured; adjusting the position of laser, wherein the needle point is most sensitive to force, the laser is adjusted to be shot at the needle point, the contact between the needle point and the growth liquid level is adjusted through the detection of a feedback system, and the amplitude of the micro-cantilever is further controlled, so that the growth liquid is picked up;
4) synthesis of the tip of a needle
And carrying out chemical reaction on the needle tip by adopting a chemical vapor deposition method to prepare probes with different types of tips.
2. The method for preparing the probe with the large length-diameter ratio based on the one-dimensional nano material as claimed in claim 1, wherein in the step 1), the time for cleaning the mica sheet by using acetone, ethanol and deionized water is 5-10 min.
3. The method for preparing the probe with the large length-diameter ratio based on the one-dimensional nano material as claimed in claim 1, wherein in the step 2), the mass of aluminum trichloride hexahydrate in the first solution in the growth solution is 2.4-4.8g, the amount of ethanol is 15-30mL, and the amount of silicon tetrachloride solution is 1.2-2.4 mL.
4. The method for preparing a probe with a large length-diameter ratio based on a one-dimensional nano material as claimed in claim 1, wherein in the step 2), the mass of ferric trichloride hexahydrate in the second solution in the growth solution is 2-4g, and the amount of ethanol is 5-10 mL.
5. The method for preparing the probe with the large length-diameter ratio based on the one-dimensional nanometer material as claimed in claim 1, wherein in the step 3), the sensitivity is calibrated by a method of making a force curve for a rigid silicon sample.
6. The method for preparing the probe with the large length-diameter ratio based on the one-dimensional nanometer material as claimed in claim 1, wherein in the step 3), the growth solution is picked up by adopting a peak force tapping mode of an atomic force microscope.
7. The method for preparing a probe with a large length-to-diameter ratio based on one-dimensional nano-materials as claimed in claim 1, wherein the nano-materials synthesized by the probe tip in step 4) comprise nanowires, nanorods, nanotubes and nanofibers.
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| CN110658360B (en) * | 2019-09-16 | 2020-08-18 | 浙江大学 | Method and device for preparing superfine atomic force microscope metal probe |
| CN111693737B (en) * | 2020-06-18 | 2021-05-07 | 中国科学院力学研究所 | Method for manufacturing nanofiber probe tip for sample surface topography measurement |
| GB2611841A (en) * | 2021-04-28 | 2023-04-19 | Univ Xi An Jiaotong | Method for preparing nanoprobe |
| CN113219211B (en) * | 2021-04-28 | 2022-02-22 | 西安交通大学 | Preparation method of nano probe |
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