CN110371922A - A kind of system and method for control micro-nano composite material in-situ locally growth - Google Patents
A kind of system and method for control micro-nano composite material in-situ locally growth Download PDFInfo
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- CN110371922A CN110371922A CN201910590829.4A CN201910590829A CN110371922A CN 110371922 A CN110371922 A CN 110371922A CN 201910590829 A CN201910590829 A CN 201910590829A CN 110371922 A CN110371922 A CN 110371922A
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- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/005—Bulk micromachining
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00555—Achieving a desired geometry, i.e. controlling etch rates, anisotropy or selectivity
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Abstract
The invention discloses a kind of system and method for control micro-nano composite material in-situ locally growth, and the system of stating includes: visual feedback Observation Blocks, is made of microscope and electro-conductive glass；Microelectrode mobile module comprising mobile device, the mobile device are equipped with microelectrode tube；Micro-injection pump oozes the reaction solution for injecting gas into the microelectrode tube from the microelectrode；Ohmic contact feedback module comprising sequentially connected amplifier, AD converter and computer, the amplifier in are inserted into the microelectrode tube and connect with the reaction solution in the microelectrode.The present invention carries out real time management with visual feedback observation, is changed using resistance and judges whether microelectrode contacts with substrate material surface, realizes the small area fixed point growth of micro-nano composite material and precision is good, controllability is good.
Description
Technical field
The invention belongs to micro-nano composite materials to grow field, and in particular to a kind of control micro-nano composite material in-situ locally is raw
Long system and method.
Background technique
With the maturing, diversification and industrialization of micron technology and nanotechnology, micro-nano complex technique and micro-nano are compound
Material comes into being.The characteristics of micro-nano composite material not only has special structure, further comprises micro materials and nano material
Many properties, make its biology, in terms of show special application value；And due to which overcome
Single base material intensity itself is not high, especially the poor disadvantage of mechanical property, receives more and more attention in recent years, phase
Pass technology emerges one after another.
Application No. is a kind of micro-nano structure In is described in 201710504905 Chinese patent2O3/SnO2Composite material
Growth in situ mode: it is using indium oxide or tin oxide microparticle as matrix, and in above-mentioned microparticle in the way of hot evaporation
Upper growth in situ includes the nanocrystalline of another material (tin oxide or indium oxide), meanwhile, pass through control growing environment and growth
Time make it is above-mentioned it is nanocrystalline form one-dimensional or quasi-one-dimensional structure and be interconnected, and then it is netted to constitute indium oxide/tin oxide
Structural composite material.But wherein thermal evaporation deposition is a kind of technology for being mainly used for deposition film, and raw material are added in the vacuum chamber
Thermal evaporation is adhered directly to be placed on the substrate on the upside of raw material at gaseous state, and the obvious deficiency of this method is, due to thermal evaporation
Gaseous source material mainly adhered in substrate with a direction, the roughness of substrate also will affect the quality of deposition film,
And for production be micro/nano level material, hot evaporation more seems with high costs, reaction environment and the uncontrollable disadvantage of precision.
Application No. is the micro-nano composite fibre materials that a kind of loaded optic catalyst is proposed in 201810998005 Chinese patent
Material: it is using 50-100 μm of diameter of micrometer fibers as core material, then with electrostatic spinning technique in the conductive height of micrometer fibers surface aggregates
Molecularly Imprinted Polymer makes surface cover the nanofiber of 5-10 μm of a layer thickness of loaded optic catalyst.This compound fibre of micro-nano
Dimension material flexibility is good, has opened up a kind of new approaches of composite photo-catalyst；But the electrostatic spinning that this complex fiber material uses
Technology is concentrated mainly on micrometer fibers surface and discharges the polymer to form package, can not completely attach to and pinpoint generation reaction generation
Required composite material.
Although micro-nano composite material growth at present there are many kinds of method, technology also relative maturity, however existing technology is all
Only the growth of larger area and can only carry out spreadability reaction growth, while without good Real-time Feedback make precision and
Controllability is also bad.
Summary of the invention
Based on this, the present invention provides a kind of system of control micro-nano composite material in-situ locally growth, the present invention is used
Visual feedback observation carries out real time management, and reaction solution is accurately moved to substrate surface areas, then uses contact resistance conduct
Accurate feedback is changed using resistance and judges whether microelectrode contacts with substrate material surface, and solving the prior art can only
The growth of large area spreadability, while precision and the bad problem of controllability.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of system of control micro-nano composite material in-situ locally growth, the system comprises:
Visual feedback Observation Blocks, are made of microscope and electro-conductive glass, and the electro-conductive glass is fixed on described microscopical
On objective table, for placing base material, and the electro-conductive glass is grounded；It is understood that microscope here can select
From simple microscope, can also selected from be inverted, just setting, high resolution industrial microscope etc., be mainly used for base material
It is observed in real time, preferred metallographic microscope in the present invention.
Microelectrode mobile module comprising mobile device, the mobile device are equipped with microelectrode tube, the microelectrode tube
On be connected with microelectrode, be mounted with reaction solution in the microelectrode, the mobile device be used to control the drive of the microelectrode into
It is mobile；It, can also be with it is understood that microelectrode here can be mounted on one end of the microelectrode tube by sealed tube
It is directly prepared into microelectrode tube and microelectrode is integrally formed.Here mobile device is mainly used for mobile microelectrode tube to mobile
Micro- glass electrode, including rotation translation and two kinds of D translation mobile dimensions.
Micro-injection pump is connected to the microelectrode tube, for injecting gas into the microelectrode tube thus by institute
Reaction solution is stated to ooze from the microelectrode；Further, through-hole is offered on the side wall of microelectrode tube, it is micro- for being connected to
Measuring syringe pump oozes the reaction solution in microelectrode tip so that micro-injection pump of checking card injects gas into microelectrode tube.
Ohmic contact feedback module comprising sequentially connected amplifier, AD converter and display device, the amplifier
One of input terminal be inserted into the microelectrode tube and connect with the reaction solution in the microelectrode, another input terminal company
Power supply is connect, the output end of the amplifier is connect with the input terminal of the AD converter, the output end of the AD converter and institute
State the input terminal connection of display device.Here display device is mainly used for showing that signal uses, and can be used commonly used in the art
Computer.When the microelectrode and base material contact, base material, electro-conductive glass, microelectrode reaction solution feedback electricity
Road conducting, signal source inputs in AD converter after amplifier amplifies, and after being converted into analog signal, shows in input and display device
Show.
This system obtains basis material target morphology pose with visual feedback Observation Blocks, then according to target morphology position
Appearance carries out the mobile microelectrode of real time management, and is further fed back using Ohmic contact, accurately judges reactant according to resistance
The accurate control micro-nano composite material of contact growth district, improve the precision and controllability of the growth of micro-nano composite material.
Further, the microscope is metallographic microscope, and CMOS camera is housed on the metallographic microscope.Here CMOS
Therefore the conventional means for being installed as those skilled in the art and all knowing of camera are no longer described in detail.The CMOS camera is main
It is for clearly extracting the needle point coordinate of growth coordinate and microelectrode needed for base material, to be realized by mobile device
The translational rotation movement of microelectrode makes needle point reach specified region.
Further, the microelectrode is glass electrode, and the tip internal diameter of the glass electrode is less than 1 μm.
It is another object of the present invention to provide a kind of methods of control micro-nano composite material in-situ locally growth, use
Above system preparation comprising following steps:
S1, in oxygen barrier environment, base material is placed on electro-conductive glass；
S2, microelectrode is moved to the base material near zone using micro- sem observation, then mould is fed back by Ohmic contact
Block signal is controlled using microelectrode mobile module the microelectrode being moved to the substrate material surface specific position；
S3, reaction solution is oozed using the micro-injection pump control microelectrode, carries out in-situ locally growth；
S4, after the reaction was completed observes the base after unreacted ion remaval in the base material after step S3 reaction
The growth district of bottom material.
In-situ locally growth method refers under conditions of not disturbed specimen dynamic process and not mobile example position, in material
The process that the specific position of material realizes reaction condition and reacts.Exactly using base material as object in the present invention, pass through tune
Whole microelectrode angles and positions are by reaction solution micro-injection therein to the surface of base material and particular position inside to send out
Raw reaction forms micro-nano composite material.In the process with vision positioning feedback i.e. by machine vision images processing system at
Reason, obtains target morphology pose and feeds back to user, then real time management is carried out according to target morphology pose, with contact resistance
As feedback, using resistance variation judge microelectrode whether with hydrogel surface precise contact so that micro-nano composite material
Realize accurate and controllable preparation.
Preferably, the base material be hydrogel model, the hydrogel model the preparation method comprises the following steps: by 1 ~ 3mol/
LFe3O4Solution and 1 ~ 3mol/LFeCl3After solution is sufficiently mixed, dispersed system is obtained, it is preferred that Fe3O4Solution and
FeCl3The volume ratio of solution is 2:3；The hydrogel material that will be provided with different porosities is immersed in the dispersed system,
Soaking time does not limit specifically, on the basis of hydrogel material immersion sufficiently, preferred leaching in an embodiment of the present invention
The bubble time is 1 ~ 6h, when hydrogel material is immersed in above-mentioned dispersed system, since the pore structure of hydrogel is special
Property, iron ion enters inside hydrogel grid under the action of osmotic pressure and equally distributed trend is presented on the whole；
The reaction solution is NaOH solution, and concentration can need to be adjusted according to preparation, preferably 1mol/ in the present invention
The NaOH solution of L.
Preferably, the hydrogel material include Sodium Alginate Hydrogel Films, acrylamide gel, PEGDA hydrogel,
At least one of PEG hydrogel, it is to be understood that the hydrogel material of this field routine is used equally in the application, on
Stating to the citing of hydrogel material includes but is not limited to mentioned kind.And the hydrogel of different porosities can be by adjusting preparation
The material rate of hydrogel carries out, as PEGDA hydrogel can be by adjusting the percentage of PEGDA molecular weight and photoinitiator levels
Than etc. conditions realize, this belongs to the conventional means that those skilled in the art know, therefore, no longer do here it is detailed repeat,
It can specifically be adjusted according to actual needs.
Preferably, in step S3, while oozing reaction solution using the micro-injection pump control microelectrode, additional magnetic
?.Here mainly using permanent magnet externally-applied magnetic field so as to shorten the time of reaction.
Preferably, in step S4, the specific steps of extra unreacted ion are removed are as follows: will be after step S3 reaction
Base material steeps in deionized water.
Compared with prior art, the invention has the following advantages:
1, this system can realize the fixed point growth in situ of micro-nano composite material, and microelectrode is moved to water using Visual Feedback Control
Gel near zone recycles high-precision contact resistance feedback control that microelectrode is moved to hydrogel surface specific position,
Overcome the larger response area of traditional micro-nano composite material, precision is low, poor controllability defect, proposes that new fixed point is in situ
The method of growth of micro-nano composite material, sufficiently high-precision reaction simultaneously can be according to requiring personalized growth；
2, the cost of this system is low, and the period grown using this system micro-nano composite material in-situ locally is short, and components are succinct, former
Manage it is simple and reliable, be conducive to realize, have excellent performance.
Detailed description of the invention
Fig. 1 is the system structure signal of control micro-nano composite material in-situ locally growth in a preferred embodiment of the present invention
Figure；
Fig. 2 is the structural schematic diagram of microelectrode tube and microelectrode in Fig. 1；
Fig. 3 is phenogram of the micro-nano composite material under 40 times of mirrors in the embodiment of the present invention after the reaction was completed.
In figure: 11- metallographic microscope；
21- glass microelectrode, 22- microelectrode tube, 23- mobile device；
30- micro-injection pump, 41- amplifier, 42-AD converter, 43- computer, 44- conducting wire.
Specific embodiment
To facilitate the understanding of the present invention, below in conjunction with specific embodiments to invention is more fully described.But
It is that the invention can be realized in many different forms, however it is not limited to embodiments described herein.On the contrary, providing
The purpose of these embodiments is to make to make the present disclosure more fully understandable.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.
A kind of system of control micro-nano composite material in-situ locally growth, including visual feedback Observation Blocks, microelectrode move
Dynamic model block, micro-injection pump and Ohmic contact feedback module composition.
Fig. 1 is please referred to, visual feedback Observation Blocks are mainly made of metallographic microscope 11, in the load of metallographic microscope 11
Electro-conductive glass is fixed on object platform, and electro-conductive glass is grounded, while being equipped with CMOS on metallographic microscope 11 in this embodiment
Camera.
Microelectrode mobile module, including glass microelectrode 21, microelectrode tube 22 and mobile device 23, the mobile device 23
For controlling the movement of the glass microelectrode 21, the mobile device 23 in the present embodiment is rotated by northern light PRS100 Series Manual
Platform and northern light MTS200 series motorized precision translation stage composition are, it can be achieved that can be manually rotated translation and the higher Electronic control three-dimensional of precision is flat
It moves.In the present embodiment, it is mounted with the NaOH solution of 1mol/L in glass microelectrode 21, while micro- glass electrode 21 is passed through into pipe
Set is connected to one end of microelectrode tube 22, and in the present embodiment, glass microelectrode 21 draws instrument using laser and is prepared, tip
Internal diameter is less than 1 μm.Through-hole is offered on the side wall of microelectrode tube 22, for being connected to micro-injection pump 30.
More specifically, Ohmic contact feedback module comprising sequentially connected amplifier 41, AD converter 42 and computer
43, as shown in fig. 1, a wherein input terminal and the NaOH reaction solution in the glass microelectrode 21 for the amplifier 41 connects
It connects, another input terminal connects power supply.Specifically, as shown in Fig. 2, in the present embodiment, 21 tip of glass microelectrode it is opposite
End is fixed on one end of microelectrode tube 22, and is connected to microelectrode tube 22, and amplification is inserted in the other end of microelectrode tube 22
The conducting wire 44 of device 41, so that amplifier 41 is connect with the NaOH reaction solution in glass microelectrode 21, furthermore amplifier 41 is defeated
Outlet is connected with the input terminal of AD converter 42, and the output end of AD converter 42 is connect with the input terminal of computer 43.This implementation
Example in amplifier 41, AD converter 42 and computer 43 be it is commercially available, those skilled in the art have normal according to it
Knowledge can be attached, and therefore, be no longer described in detail.
When specific works, base material is fixed on electro-conductive glass, is extracted by CMOS camera raw needed for base material
The needle point coordinate of long coordinate and microelectrode 21 passes through in the present embodiment then by the mobile microelectrode 21 of mobile device 23
The tip needle point of the rotation of mobile microelectrode 21 manually, the then translation of Electronic control microelectrode 21, control microelectrode 21 reaches
Specified region；
When microelectrode 21 and base material contact, between electro-conductive glass, base material, microelectrode reaction solution and amplifier 41
Circuit conducting, shows resistance on computer 43, then by continuing to adjust mobile device 23, according to the resistance on computer 43
The further precise contact of variation control microelectrode 21；
After confirming microelectrode 21 and base material precise contact, micro-injection pump 30 is opened, by the reaction drop in microelectrode 21
The in-situ locally growth of micro-nano composite material is realized on base material.
The present embodiment also discloses the method for control micro-nano composite material in-situ locally growth, is based on above-mentioned control micro-nano
What the system of composite material in-situ locally growth carried out, the specific steps are as follows:
By 1.0mol/LFe3O4Solution 10mL and 1.0mol/LFeCl3It is uniformly dispersed, obtains evenly dispersed after solution 15mL mixing
System；
By PEGDA and PEG hydrogel material, (wherein PEGDA:PEG mass ratio 1:2, photoinitiator 819 is according to mass fraction 1%
It is added, ultra-violet curing is at hydrogel) it is immersed in 6h in the uniform dispersion, due to the pore structure properties of hydrogel,
Fe2+And Fe3+It will enter inside hydrogel grid under the action of osmotic pressure and equally distributed trend is presented on the whole, obtain
Hydrogel model；
The NaOH solution of 1mol/L will be loaded in glass microelectrode 21 of the tip internal diameter less than 1 μm, while by glass microelectrode 21
The conducting wire 44 of interior NaOH solution connection amplifier 41, and the hydrogel material after abundant impregnate is placed on electro-conductive glass；
Growth position needed for extracting hydrogel model by CMOS camera on metallographic microscope 11 and 21 tip of glass microelectrode
Glass microelectrode 21 is moved to hydrogel model near zone by control mobile device 23 by needle point coordinate, and control glass is micro-
Electrode 21 makes its tip carry out extremely slow contact with growth site needed for hydrogel model, and feed circuit is connected when contacting, root
It is shown according to the resistance on computer 43, it has been determined that contact；
Further by, as feedback, judging glass microelectrode 21 and hydrogel using resistance variation with contact resistance
Then model surface specific position precise contact opens micro-injection pump 30 and injects gas into microelectrode tube 22, keeps glass micro-
NaOH solution in electrode 21 drips the specific position in hydrogel model from tip, while using permanent magnet externally-applied magnetic field to shorten
Reaction time, under the action of NaOH solution, the Fe of hydrogel specific position2+And Fe3+It is common to generate Fe3O4Magnetic-particle.
After the reaction was completed, reacted hydrogel model is steeped and removes extra iron ion in deionized water；
It is observed finally by growth district of the metallographic microscope 11 to above-mentioned realization hydrogel.
The growth of final micro-nano composite material is as shown in Figure 3, it can be seen that it is raw to realize small area in composite material
It is long, illustrate the small area growth that method of the invention accurate can realize micro-nano composite material, and become according to the resistance value of resistance value
Change accurate control, operating process controllability is good.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (8)
1. a kind of system and method for control micro-nano composite material in-situ locally growth, which is characterized in that the system comprises:
Visual feedback Observation Blocks, are made of microscope and electro-conductive glass, and the electro-conductive glass is fixed on described microscopical
On objective table, for placing base material, and the electro-conductive glass is grounded；
Microelectrode mobile module comprising mobile device, the mobile device are equipped with microelectrode tube, connect in the microelectrode tube
It is connected to microelectrode, is mounted with reaction solution in the microelectrode, the mobile device is used to control the drive of the microelectrode into movement；
Micro-injection pump is connected to the microelectrode tube, for injecting gas into the microelectrode tube thus will be described anti-
Liquid is answered to ooze from the microelectrode；
Ohmic contact feedback module comprising sequentially connected amplifier, AD converter and display device, the amplifier its
In an input terminal be inserted into the microelectrode tube and connect with the reaction solution in the microelectrode, another input terminal connects electric
Source, the output end of the amplifier are connect with the input terminal of the AD converter, and the output end of the AD converter is shown with described
The input terminal of showing device connects.
2. the system of control micro-nano composite material in-situ locally growth as described in claim 1, which is characterized in that described micro-
Mirror is metallographic microscope, and CMOS camera is housed on the metallographic microscope.
3. the system of control micro-nano composite material in-situ locally growth as described in claim 1, which is characterized in that micro- electricity
Extremely glass electrode, the tip internal diameter of the glass electrode is less than 1 μm.
4. a kind of method of control micro-nano composite material in-situ locally growth, which is characterized in that any using such as claim 1 ~ 3
System preparation described in comprising following steps:
S1, in oxygen barrier environment, base material is placed on electro-conductive glass；
S2, microelectrode is moved to the base material near zone using micro- sem observation, then mould is fed back by Ohmic contact
The microelectrode is moved to the substrate material surface specific position using the control of microelectrode mobile module and accurately determined by block signal
Position；
S3, reaction solution is oozed using the micro-injection pump control microelectrode, carries out in-situ locally growth；
S4, after the reaction was completed observes the base after unreacted ion remaval in the base material after step S3 reaction
The growth district of bottom material.
5. the method for control micro-nano composite material in-situ locally growth as claimed in claim 4, which is characterized in that the substrate
Material be hydrogel model, the hydrogel model the preparation method comprises the following steps: by 1 ~ 3mol/LFe3O4Solution and 1 ~ 3mol/LFeCl3
After solution is sufficiently mixed, dispersed system is obtained；The hydrogel material that will be provided with different porosities is immersed in described uniform point
In granular media system；
The reaction solution is NaOH solution.
6. the method for control micro-nano composite material in-situ locally growth as claimed in claim 5, which is characterized in that the water-setting
Glue material includes at least one of Sodium Alginate Hydrogel Films, acrylamide gel, PEGDA hydrogel, PEG hydrogel.
7. the method for control micro-nano composite material in-situ locally growth as claimed in claim 4, which is characterized in that step S3
In, while oozing reaction solution using the micro-injection pump control microelectrode, externally-applied magnetic field.
8. the method for control micro-nano composite material in-situ locally growth as claimed in claim 4, which is characterized in that step S4
In, remove the specific steps of extra unreacted ion are as follows: steep the base material after step S3 reaction into deionized water
In.
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