CN109765407A - A kind of big L/D ratio probe preparation method based on monodimension nanometer material - Google Patents
A kind of big L/D ratio probe preparation method based on monodimension nanometer material Download PDFInfo
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Abstract
The big L/D ratio probe preparation method based on monodimension nanometer material that the invention discloses a kind of, the probe includes the nanostructure at the common silicon probe of atomic force microscope and tip, the probe the preparation method comprises the following steps: Atomic Force Microscopy Silicon probe is mounted on equipped on the gauge head of atomic force microscopy mirror device that can make tapping-mode liquid tank first；Then injected into liquid pool on a small quantity by two kinds of solution mixing systems at solution i.e. growth-promoting media, hand-guided inserting needle picks up growth-promoting media；Last liquid to be grown, which picks up, to be completed, and in prefabricated silicon needle point tip synthesizing one-dimensional nano material, prepares the needle point of big L/D ratio.The problem of being also easy to produce image artifacts to suitable to fine structure with high depth-width ratio imaging the present invention overcomes the common silicon probe of currently used atomic force, the probe major diameter that this method obtains is bigger, better resolution ratio available to the measurement of structure.
Description
Technical field
The invention belongs to micro-nano manufacture field of measuring technique, and in particular to a kind of big major diameter based on monodimension nanometer material
Compare probe preparation method.
Background technique
In recent years, the fields rapid developments such as large scale integrated circuit, minitype spacecraft control, carrier is stealthy, these are emerging
Technology is largely dependent upon complicated, accurate fine structure, especially with the high depth-to-width ratio micro knot of high complexity
Structure has very wide application prospect in these fields.In contrast to planar structure, high-aspect-ratio (depth-to-width ratio, that is, fine structure
Depth capacity/width ratio) three-dimensional structure has bigger specific surface area, it is meant that same substrate area can kept
In the case of obtain bigger available space in the vertical dimension, for micro-nano device upgrading open new thinking and wider array of application
Field.But suitable to fine structure with high depth-width ratio in the depth direction, is difficult accurately to be measured due to own dimensions
With characterization, it is difficult to the function, purposes, novel manufacturing process of its structure carry out deeper into research.Currently, both at home and abroad for height
The measurement method of depth-to-width ratio fine structure mainly divides two major classes, and one kind is using various laser interferometer as the optical touchless of representative
Measurement method, but while measuring, will receive the depth of field and the small limitation of focus lens region；One kind is using atomic force microscope as representative
Scanning Probe Microscopy contact measurement method, this method resolution ratio with higher, but average probe draw ratio (length/straight
The ratio of diameter) it is smaller, resolution limitations are in the radius of curvature of needle point, it is difficult to meet the measurement demand of high aspect ratio structure.
The probe of atomic force microscope is its most crucial one of component, is played a decisive role to imaging performance.1-dimention nano
Material, such as nano wire, nanotube, nanobelt, nanometer rods, due to its excellent electricity, mechanics, the performances such as optics, always by
Research extensively.Monodimension nanometer material compares for two-dimensional nano-film and zero-dimension nano particle, has the advantages that many: first
Monodimension nanometer material can be made under more easy growth conditions of chemical method, and material to substrate and shape are almost
Without any requirement, the nano thin-film that is obtained as Atomic layer deposition method, growth conditions is extremely just carved needed for particle, and equipment is very high
It is expensive；Secondly because monodimension nanometer material size is nanoscale on two dimensions, thus its mechanical elasticity, yield limit and
First property, even if the mechanical deformations such as very big bending occur, is also not easy structure breaking and strain, is able to bear all far beyond bulk
Biggish active force and strain, and nano thin-film just easily generates rhegma under very little strain, nano particle is almost without machine
Tool elasticity.The biggish monodimension nanometer material of draw ratio and atomic force microscope are combined, it is aobvious that atomic force can be greatly improved
The imaging performance of micro mirror.At present just like conductive adhesive method, pore development method, method etc. is manually assembled and prepares carbon nanotube probes
Method.Wherein conductive adhesive method uses optical microscopy, and when bonding carbon nanotube, readily selected thicker carbon is received
Mitron beam, rather than most thin carbon nanotube influence the resolution ratio of imaging.The key problem for restricting the application at present is to prepare effect
Rate is lower, at high cost, is also easy to produce image artifacts.
Summary of the invention
For above-mentioned defect existing in the prior art and deficiency, it is an object of the present invention to provide a kind of bases
In the big L/D ratio probe preparation method of monodimension nanometer material, meet high aspect ratio structure measurement it is reliable and stable, precision is high etc.
It is required that.
The present invention adopts the following technical scheme that realize:
A kind of big L/D ratio probe preparation method based on monodimension nanometer material, the probe include that atomic force microscope is common
Silicon probe and the nanostructure at tip, the probe the preparation method comprises the following steps:
Atomic Force Microscopy Silicon probe is mounted on first and is set equipped with the atomic force microscope that can make tapping-mode liquid tank
On standby gauge head；Then injected into liquid pool on a small quantity by two kinds of solution mixing systems at solution i.e. growth-promoting media, hand-guided inserting needle
To pick up growth-promoting media；Last liquid to be grown, which picks up, to be completed, and in prefabricated silicon needle point tip synthesizing one-dimensional nano material, is prepared and is greatly enhanced
The needle point of diameter ratio.
A further improvement of the present invention lies in that this method specifically includes the following steps:
1) cleaning of substrate
Using new explanation from mica sheet as substrate, use culture dish as the liquid pool for containing liquid, successively use acetone, ethyl alcohol
Mica sheet is cleaned with deionized water；
2) configuration of growth-promoting media
Match the first solution first: six trichloride hydrate aluminium being dissolved in ethanol solution, are then slowly infused with pipettor
Enter silicon tetrachloride solution, the solution prepared is placed in constant temperature magnetic heating stirrer and is uniformly mixed；It is reconfigured second of solution:
Iron(III) chloride hexahydrate is dissolved in ethanol solution, two kinds of solution are mixed, are placed in constant temperature magnetic heating stirrer
Stirring, after stand 12-24h at room temperature；
3) pickup of growth-promoting media
Needle point sensitivity is demarcated first；After the completion of calibration, using the glue insoluble in growth-promoting media by base material
It is fixed on liquid pool bottom surface, is fully cured to glue, prefabricated silicon probe is mounted on atomic force microscope gauge head；Adjustment
The position of laser, due to most sensitive to power at needle point, adjustment laser is beaten at needle point, adjusts needle by the detection of feedback system
The contact of point and growth liquid level, and then micro-cantilever amplitude is controlled, to be picked up to growth-promoting media；
4) synthesis at needle point tip
It is chemically reacted on needle point using chemical vapour deposition technique to prepare the probe at different type tip.
A further improvement of the present invention lies in that using acetone, ethyl alcohol and deionized water carry out clearly mica sheet in step 1)
The time washed is followed successively by 5-10min.
A further improvement of the present invention lies in that in step 2), six trichloride hydrate aluminium in the first solution in growth-promoting media
Quality is 2.4-4.8g, and the capacity of ethyl alcohol is 15-30mL, silicon tetrachloride solution 1.2-2.4mL.
A further improvement of the present invention lies in that in step 2), Iron(III) chloride hexahydrate in second of solution in growth-promoting media
Quality is 2-4g, and the capacity of ethyl alcohol is 5-10mL.
A further improvement of the present invention lies in that in step 3), using doing the method for force curve to rigid silicon sample to sensitive
Degree is demarcated.
A further improvement of the present invention lies in that in step 3), using the peak force tapping-mode of atomic force microscope to life
Long liquid is picked up.
A further improvement of the present invention lies in that the nano material of probe tip synthesis includes nano wire, nanometer in step 4)
Stick, nanotube and nanofiber.
The present invention has following beneficial technical effect:
Implement according to the step of preparation method of the present invention, synthesizes big major diameter in needle point using after prefabricated needle point pickup growth-promoting media
Than tip, this method is simple and easy, the equipment for not needing complex and expensive, save the cost.The present invention overcomes currently used atoms
The problem of common silicon probe of power is also easy to produce image artifacts to suitable to fine structure with high depth-width ratio imaging, the probe draw ratio that this method obtains
It is larger, it is more than or equal to 10:1, better resolution ratio available to the measurement of structure.
Detailed description of the invention
Illustrate the embodiment of the present invention or technical solution in the prior art in order to clearer, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described.
Fig. 1 is to pick up growth-promoting media operation chart using prefabricated needle point in the specific embodiment of the invention.
Fig. 2 is to pick up power in growth-promoting media operating process in the specific embodiment of the invention to change with time schematic diagram.
Fig. 3 is the dual heating zones vacuum tube furnace that preparation tip uses in the specific embodiment of the invention.
Fig. 4 is the scanning electron microscope diagram piece for the probe being prepared in the specific embodiment of the invention.
Fig. 5 is the scanning electron microscope diagram piece of high-aspect-ratio sample in the specific embodiment of the invention.
Fig. 6 be in the specific embodiment of the invention probe that is prepared to the topography measurement picture of high-aspect-ratio sample.
Specific embodiment
The present invention is further explained below in conjunction with the drawings and specific embodiments.
A kind of preparation method of probe for the measurement of high length-diameter ratio fine structure provided by the invention, which includes original
The common silicon probe of sub- force microscope and the nanostructure at tip, the probe the preparation method comprises the following steps: first by atomic force microscope
Silicon probe is mounted on equipped with the atomic force microscopy mirror device (Bruker Dimension Icon) that can make tapping-mode liquid tank
On gauge head, a small amount of growth-promoting media is then injected into liquid pool, hand-guided inserting needle picks up growth-promoting media, and last liquid to be grown picked up
At preparing the needle point of big L/D ratio in prefabricated silicon needle point tip nano materials.
Specific step is as follows:
1) cleaning of substrate
Using new explanation from mica sheet as substrate, use culture dish as the liquid pool for containing liquid, successively use acetone, ethyl alcohol
Mica sheet is cleaned with deionized water.The time that wherein mica sheet is cleaned with acetone, ethyl alcohol and deionized water according to
Secondary is 5-10min.
2) configuration of growth-promoting media
Match the first solution first: six trichloride hydrate aluminium being dissolved in ethanol solution, are then slowly infused with pipettor
Enter silicon tetrachloride solution, the solution prepared is placed in constant temperature magnetic heating stirrer and is uniformly mixed；It is reconfigured second of solution:
Iron(III) chloride hexahydrate is dissolved in ethanol solution.Two kinds of solution are mixed, are placed in constant temperature magnetic heating stirrer
Stirring, after stand 12-24h at room temperature.The matter of six trichloride hydrate aluminium in the first solution that wherein configuration growth-promoting media uses
Amount is 2.4-4.8g, and the capacity of ethyl alcohol is 15-30mL, silicon tetrachloride solution 1.2-2.4mL, configures growth-promoting media uses first
The quality of Iron(III) chloride hexahydrate is 2-4g in kind solution, and the capacity of ethyl alcohol is 5-10mL.
3) pickup of growth-promoting media
It is demarcated firstly the need of to needle point sensitivity, and uses and the method for force curve is done to sensitive to rigid silicon sample
Degree is demarcated.After the completion of calibration, base material is fixed on liquid pool bottom surface using the glue insoluble in growth-promoting media, to glue
Water is fully cured, and prefabricated silicon probe is mounted on atomic force microscope gauge head.The position for adjusting laser, due at needle point pairs
Power is most sensitive, and adjustment laser is beaten at needle point.The contact of needle point with growth liquid level is adjusted by the detection of feedback system, in turn
Micro-cantilever amplitude is controlled, to be picked up to growth-promoting media.
4) synthesis at needle point tip
It is chemically reacted on needle point using chemical vapour deposition technique to prepare the probe at different type tip, wherein visiting
The nano material of needle tip synthesis includes nano wire, nanometer rods, nanotube and nanofiber.
Embodiment 1
(1) cleaning of substrate
Using new explanation from mica sheet as substrate, use culture dish as the liquid pool for containing liquid, to guarantee the pure of liquid
Degree is avoided introducing impurity, can be polluted to needle point, therefore, to assure that the cleannes of sample surfaces.Mica sheet is immersed in first
In acetone, be put into ethyl alcohol and impregnated with tweezers clamping mica sheet after 10min, after 10min with tweezers clamping mica sheet use go from
Sub- water is rinsed 5min, is dried up immediately with nitrogen, and the mica sheet substrate cleaned is put into closed container and is protected
It deposits, prevents vapor excessive in absorption air.
(2) configuration of growth-promoting media
Match the first solution first: six trichloride hydrate aluminium of 2.4g being dissolved in 15mL ethanol solution, liquid relief is then used
Device is slowly injected into 1.2mL silicon tetrachloride solution, and the solution prepared is placed in constant temperature magnetic heating stirrer and is uniformly mixed；Match again
It sets second of solution: 2.0g Iron(III) chloride hexahydrate is dissolved in 5mL ethanol solution.Two kinds of solution are mixed, are placed on
Stirred in constant temperature magnetic heating stirrer, after stand 12-24 hours at room temperature.Above two solution allocation does not have sequencing
Relationship.
(3) pickup of growth-promoting media
It is demarcated firstly the need of to needle point sensitivity, by doing force curve method to sensitive to rigid silicon sample in experiment
Degree is demarcated.The curve of cantilever beam deformation quantity Yu piezoelectric ceramics relative sample apparent height is obtained by sensitivity.It tested
The peak force tapping-mode of Cheng Caiyong atomic force microscope, that is, the vibration of driving micro-cantilever makes needle point and growth liquid level interruption when scanning
Contact, amplitude reduces when needle point is by substrate effect power, and feedback system is by detecting variation adjustment needle point and growing liquid level
Contact, and then micro-cantilever amplitude is controlled, to be picked up to growth-promoting media.The pick-up operation schematic diagram of growth-promoting media as shown in Figure 1,
Wherein, 1 is substrate, and 2 be liquid pool, and 3 detect for position sensitive, and 4 be laser, and 5 be cantilever beam, and 6 be growth liquid level, and 7 be needle point.
Pick process is divided into five states, respectively corresponds A~E point in Fig. 2, and A point is probe close to growth liquid level and not in contact with state；
B-C sections, power suffered by needle point is gradually increased, and needle point is in contact with liquid level at C point；Due to the reprimand of needle point and growth-promoting media sample room
Power effect, after needle point is detached from liquid surface, growth-promoting media can generate adhesive force with needle point and be attached on tip；As needle point is constantly remote
From the power that needle point is subject to is gradually reduced as shown in E point in Fig. 2.
(4) synthesis at needle point tip
After the completion of growth-promoting media picks up, in prefabricated needle point tip synthesizing carbon nanotubes, detailed process as shown in Figure 3 double plus
It is realized in the vacuum tube furnace of hot-zone, wherein 8 be tube furnace, and 9 be quartz ampoule, and 10 be quartz boat.Prefabricated needle point is placed in quartz boat
On, using methane as carbon source, it is passed through the methane of 1000sccm flow, 950 DEG C of temperature, time 10min；It is passed through 130sccm stream again
Measure hydrogen, time 10min；Finally in-furnace temperature is cooled to room temperature in hydrogen atmosphere.The needle point being prepared such as Fig. 4 institute
Show.
The biggish groove-like structure of high-aspect-ratio is had chosen as sample, scanning electron microscope diagram piece such as Fig. 5 of the structure
It is shown.Fig. 6 is consistent to the imaging results of high aspect ratio structure sample with practical pattern using the probe being prepared.This knot
Fruit proves that the probe that the present invention makes can get the feature image of suitable to fine structure with high depth-width ratio high quality.
Embodiment 2
The cleaning of substrate and the pickup step of growth-promoting media are the same as embodiment 1；The present embodiment and 1 difference are step (2)
Six trichloride hydrate aluminium are 4.8g in the first solution of middle configuration, and ethyl alcohol capacity is 30mL, and silicon tetrachloride capacity is 2.4mL；
Iron(III) chloride hexahydrate is 4g in second of solution, and ethyl alcohol capacity is in 10mL step (4) after the completion of growth-promoting media pickup, prefabricated
Needle point tip synthetic silica nano wire, using silane gas as silicon source, flow control 10sccm, while being passed through 100sccm
High-pure helium is as carrier gas, and reaction time 2h, sample is rapidly cooled to room temperature under high-purity helium-atmosphere after reaction.
Claims (8)
1. a kind of big L/D ratio probe preparation method based on monodimension nanometer material, which is characterized in that the probe includes atomic force
The common silicon probe of microscope and the nanostructure at tip, the probe the preparation method comprises the following steps:
Atomic Force Microscopy Silicon probe is mounted on equipped with the atomic force microscopy mirror device that can make tapping-mode liquid tank first
On gauge head；Then injected into liquid pool on a small quantity by two kinds of solution mixing systems at solution i.e. growth-promoting media, hand-guided inserting needle picks up
Take growth-promoting media；Last liquid to be grown, which picks up, to be completed, and in prefabricated silicon needle point tip synthesizing one-dimensional nano material, prepares big L/D ratio
Needle point.
2. a kind of big L/D ratio probe preparation method based on monodimension nanometer material according to claim 1, feature exist
In, this method specifically includes the following steps:
1) cleaning of substrate
Using new explanation from mica sheet as substrate, use culture dish as the liquid pool for containing liquid, successively use acetone, ethyl alcohol and go
Ionized water cleans mica sheet；
2) configuration of growth-promoting media
Match the first solution first: six trichloride hydrate aluminium being dissolved in ethanol solution, are then slowly injected into four with pipettor
Silicon chloride solution, the solution prepared are placed in constant temperature magnetic heating stirrer and are uniformly mixed；It is reconfigured second of solution: by six
Iron chloride hexahydrate is dissolved in ethanol solution, and two kinds of solution are mixed, is placed in constant temperature magnetic heating stirrer and stirs,
Stand 12-24h at room temperature afterwards；
3) pickup of growth-promoting media
Needle point sensitivity is demarcated first；After the completion of calibration, base material is fixed using the glue insoluble in growth-promoting media
It in liquid pool bottom surface, is fully cured to glue, prefabricated silicon probe is mounted on atomic force microscope gauge head；Adjust laser
Position, due to most sensitive to power at needle point, adjustment laser is beaten at needle point, by the detection of feedback system adjust needle point and
The contact of liquid level is grown, and then controls micro-cantilever amplitude, to be picked up to growth-promoting media；
4) synthesis at needle point tip
It is chemically reacted on needle point using chemical vapour deposition technique to prepare the probe at different type tip.
3. a kind of big L/D ratio probe preparation method based on monodimension nanometer material according to claim 2, feature exist
In in step 1), using acetone, the time that ethyl alcohol and deionized water clean mica sheet is followed successively by 5-10min.
4. a kind of big L/D ratio probe preparation method based on monodimension nanometer material according to claim 2, feature exist
In in step 2), the quality of six trichloride hydrate aluminium is 2.4-4.8g in the first solution in growth-promoting media, and the capacity of ethyl alcohol is
15-30mL, silicon tetrachloride solution 1.2-2.4mL.
5. a kind of big L/D ratio probe preparation method based on monodimension nanometer material according to claim 2, feature exist
In in step 2), the quality of Iron(III) chloride hexahydrate is 2-4g in second of solution in growth-promoting media, and the capacity of ethyl alcohol is 5-
10mL。
6. a kind of big L/D ratio probe preparation method based on monodimension nanometer material according to claim 2, feature exist
In being demarcated using the method for doing force curve to rigid silicon sample to sensitivity in step 3).
7. a kind of big L/D ratio probe preparation method based on monodimension nanometer material according to claim 2, feature exist
In being picked up using the peak force tapping-mode of atomic force microscope to growth-promoting media in step 3).
8. a kind of big L/D ratio probe preparation method based on monodimension nanometer material according to claim 2, feature exist
In in step 4), the nano material of probe tip synthesis includes nano wire, nanometer rods, nanotube and nanofiber.
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| CN110488208A (en) * | 2019-08-26 | 2019-11-22 | 上海大学 | A kind of shape detecting probe collateral elaboration microfluidic platform and production method based on magnetic force sensing |
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| CN110658360A (en) * | 2019-09-16 | 2020-01-07 | 浙江大学 | Method and device for preparing superfine atomic force microscope metal probe |
| CN111693737A (en) * | 2020-06-18 | 2020-09-22 | 中国科学院力学研究所 | Method for manufacturing nanofiber probe tip for sample surface topography measurement |
| WO2022227229A1 (en) * | 2021-04-28 | 2022-11-03 | 西安交通大学 | Method for preparing nanoprobe |
| GB2611841A (en) * | 2021-04-28 | 2023-04-19 | Univ Xi An Jiaotong | Method for preparing nanoprobe |
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