CN107159072A - A kind of preparation method of the self-driven microreactor of regulatable drop - Google Patents
A kind of preparation method of the self-driven microreactor of regulatable drop Download PDFInfo
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- CN107159072A CN107159072A CN201710325224.3A CN201710325224A CN107159072A CN 107159072 A CN107159072 A CN 107159072A CN 201710325224 A CN201710325224 A CN 201710325224A CN 107159072 A CN107159072 A CN 107159072A
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- gradient
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- spin coating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
Abstract
The invention discloses a kind of preparation method of the regulatable self-driven microreactor of drop, comprise the following steps：（1）Prepare coating liquid；（2）Prepare mask plate；（3）Prepare with flexible multistage gradient body structure surface；（4）Prepare shutter；（5）Prepare the surface that chemical gradient is combined with flexible multilevel gradient-structure；（6）To at least 3 and pass through step（1）Extremely（5）The surface that obtained chemical gradient is combined with flexible multilevel gradient-structure, according to the order that surface pillar is close by dredging, is arranged in " Y " font by the surface of at least 3 said structures, is assembled into a microreactor from top to bottom；At least two reacting fluids can first come together in intersection reaction, flow to vertical runner again afterwards.The present invention is on the basis of flexible multilevel gradient-structure surface, and the chemical property for combining material surface changes the chemical gradient to be formed, and enhances the ability of material surface driving drop orientation transport.
Description
Technical field
The invention belongs to macromolecule material preparation area, more particularly to a kind of self-driven microreactor of regulatable drop
Preparation method.
Background technology
Microreactor is the miniaturization chemical reaction system that a kind of unit process interface width is micron dimension, is the nineties
The micro- Chemical Engineering Technology risen.It refers to react for main purpose, based on one or more microreactors, while being also possible to bag
Microring array, micro- heat exchange, differential are included from one of the key components such as servicing unit and microsensors and microactuators such as, micro-extraction
Micro- reaction system.Specifically, microreactor generally refer to by micro-processing technology and precision processing technology manufacture with micro-
Fluid passage or scattered yardstick in the consersion unit of structure, microreactor are in micron dimension, and the treating capacity of microreactor
Then the difference according to the purpose of its application is reached from the several microlitres of scales annual to tens thousand of cubic meters per minute.In recent years, it is based on
Requirement of some specific reactions to runner surface wettability, surface wettability is initially introduced into microreactor, utilizes profit
It is moist effectively to regulate and control movement of the fluid in runner.
Traditional micro- reaction system is mainly by the method for photoetching, etching and machining in silicon chip, glass, poly dimethyl
Made on the material such as siloxanes and polymethyl methacrylate, but these preparation methods have Preparation equipment costliness, prepare
Journey is complicated, the shortcomings of runner precision is inaccurate, and it is most of external aids are needed to provide power, greatly limit micro- anti-
Answer the process of industrialization of device.Wetability is combined in microreactor, the microreactor runner with wetting gradient, Ke Yishi is made
Now drop is self-driven, so that reducing needs the demand of external auxiliary.There is making apparatus costliness, system in current micro- reaction system
Standby process is complicated, and runner precision is inaccurate, can not regulate and control, it is necessary to the problems such as external auxiliary, and in the market will soak gradient with it is micro-
The research that reactor is combined is few, and the research of the self-driven microreactor of drop for that can regulate and control almost does not have.
The content of the invention
In order to solve the above problems, the present invention provides a kind of preparation method of the regulatable self-driven microreactor of drop,
In view of the shortcomings of the prior art, the self-driven of microfluid and its regulation and control are realized, fluid driving regulation and control cost, tool is greatly reduced
The features such as having portable, economic, quick, efficient, realizes extensive use.
Adopted the following technical scheme that for this：A kind of preparation method of the self-driven microreactor of regulatable drop, it is special
Levy and be to comprise the following steps：
Step（1）Prepare coating liquid：By the prepolymer of dimethyl silicone polymer and crosslinking agent using quality as 10:1 ratio mixing
Stir, be placed on afterwards in vacuum drying chamber and extract 20min with vavuum pump, remove the bubble in solution, poly- diformazan is made
The coating liquid of radical siloxane；
Step（2）Prepare mask plate：A length of a film 50mm, width 25mm, thickness 1mm silicon template are taken, three-dimensional drawing Software on Drawing is utilized
Go out gradient-structure layout viewing, the gradient-structure layout viewing be with a diameter of 10 μm, deep 40 μm cell orifice in template in ladder
Degree distribution, the gradient distribution mode along the long side of template to be defined, using unit pitch of holes in first 1mm distance as 10 μm,
Unit pitch of holes increases to 20 μm and so in second 1mm distance；Then using the gradient-structure layout viewing of drafting as
Reference, engraving processing is carried out to silicon template；The substrate of selection is substrate of glass, and carries out prerinse to it, i.e., by substrate of glass
10 ~ 20min of ultrasound in acetone, absolute alcohol, deionized water successively, supersonic frequency is 50 ~ 100Hz, is eluted with water afterwards simultaneously
Processing is dried；Then the silicon template handled well is fitted tightly on the glass basic surface after prerinse；By step（1）
Uniform fold is in silicon template surface by way of spin coating for the coating liquid of preparation, and the spin coating number of times of specific spin coating mode is 1 time, first
With 1500 turns per minute of speed spin coating 5s, then with 8000 turns per minute of speed spin coating 20s, finally with 1500 turns per minute
Speed spin coating 5s, afterwards has spin coating the silicon template of coating liquid using temperature as 75 DEG C of dry 20min, so that on silicon template surface
Form the film of coating liquid；
Step（3）Prepare with flexible multistage gradient body structure surface：Preparation thickness is 1mm, a width of 25mm VHB adhesive tapes, elder generation
By VHB Tape Pulls, and 50% dependent variable is maintained, then by step（2）Obtained mask plate spin coating has the one of coating liquid film
Face is brought into close contact with the VHB adhesive tapes after stretching, and 2 hours are handled in temperature is 80 DEG C of baking oven；Afterwards by substrate of glass with
Silicon template is taken off, and the coating liquid film for replicating silicon template gradient-structure is just brought into close contact with VHB adhesive tapes；Finally discharge to VHB
The pulling force of adhesive tape, the polydimethylsiloxanefilm film being close on VHB tape surfaces is just because convergent force is produced in its surface
The multilevel hierarchy that flexing is combined with gradient；
Step（4）Prepare shutter：Go out an antiparallelogram using three-dimensional drawing Software on Drawing, the trapezoidal upper long 25mm of short side, under
Long length of side 82.8mm, high 50mm, the long 115mm of two waists and be respectively 120 ° and 60 ° with upper following angle take a thickness 0.3mm, chi
Very little and above-mentioned antiparallelogram identical copper sheet, is allowed to angle in 90 ° along trapezoidal high fold by copper sheet, that is, is converted into the screening of a wedge shape
Baffle plate；
Step（5）Prepare the surface that chemical gradient is combined with flexible multilevel gradient-structure：By step（4）Obtained shutter
Triangle long edge position is covered in step（3）What is prepared has on flexible multistage gradient body structure surface, the wedge-like opening of shutter
Direction is the more dense direction of pillar on VHB adhesive tapes；Place it in Surface Treatment with Plasma machine to handle and taken out after 60min,
The surface that chemical gradient is combined with flexible multilevel gradient-structure is obtained after shutter is removed；
Step（6）To at least 3 and pass through step（1）Extremely（5）Obtained chemical gradient is combined with flexible multilevel gradient-structure
Surface, according to the order that surface pillar is close by dredging, the surface of at least 3 said structures is arranged in one " Y " from top to bottom
Font, is assembled into a microreactor；At least two reacting fluids can first come together in intersection reaction, and it is vertical to flow to again afterwards
Runner.
A kind of regulatable self-driven microreactor of drop prepared according to preparation method of the present invention is more in flexibility
On the basis of level gradient-structure surface, the chemical property for combining material surface changes the chemical gradient to be formed, and further enhances
The ability of material surface driving drop orientation transport.The physical arrangement and chemical constitution of material are changed simultaneously：In flexing
From left to right its graded is close by dredging to column structure, so as to cause the hydrophobicity of material from left to right by dying down by force；Through
The material crossed after plasma treatment is due to the effect of shutter, and from left to right its graded is by small to its extent of reaction being subject to
To big, material sheet can be changed into hydrophily after treatment as hydrophobicity, so as to cause the hydrophobicity of material from left to right by strong
Die down.Both combinations greatly improve directed driven ability of the material for drop, line up after " Y " font, two kinds of reactions
Fluid can first come together in intersection reaction, flow to vertical runner again afterwards.And due to being using flexible VHB adhesive tapes as substrate
The multilevel hierarchy of preparation, can also realize the change of multilevel hierarchy arranging density by the stretching to substrate, so as to realize pair
The control of drop directed driven speed, so as to regulate and control the speed that reaction is carried out.
The beneficial effects of the invention are as follows：
1）The physics gradient of material is set to be combined with chemical gradient, the ability of the material directed driven drop further improved.
2）With the arrangement density by changing gradient-structure to the stretching of flexible substrates, the hydrophobic of material surface is changed
Property degree, it is simple to operate so as to regulate and control to reacting fluid flow rate, without external accessory.
3）Drop can be sufficiently mixed and fast transportation by design, so as to improve microreactor efficiency.
4）Preparation method economy, simple operation.
Brief description of the drawings
Fig. 1 be preparing with flexible multistage gradient body structure surface in schematic diagram, figure marked as：1 is VHB adhesive tapes, and 2 are
Coating liquid film, 3 be silicon template, and 4 be substrate of glass, and 5 be the multilevel hierarchy that flexing is combined with gradient.
Fig. 2 is that multilevel hierarchy surface plasma handles schematic diagram, wherein 6 be shutter.
Embodiment
The present invention is further illustrated below in conjunction with the accompanying drawings.
Referring to the drawings.The present embodiment of embodiment 1 comprises the following steps：
Step（1）Prepare coating liquid：5g dimethyl silicone polymers（PDMS）The prepolymer of coating liquid is mixed with 0.5g crosslinking agents and stirred
Mix uniform, be placed on afterwards in vacuum drying chamber and extract 20min with vavuum pump, remove the bubble in solution, poly dimethyl is made
The coating liquid of siloxanes；
Step（2）Prepare mask plate：A length of a film 50mm, wide 25mm, thickness 1mm silicon template 3 are taken, three-dimensional drawing Software on Drawing is utilized
Go out gradient-structure layout viewing, the gradient-structure layout viewing be with a diameter of 10 μm, deep 40 μm cell orifice in template in ladder
Degree distribution, the gradient distribution mode along the long side of template to be defined, using unit pitch of holes in first 1mm distance as 10 μm,
Unit pitch of holes increases to 20 μm and so in second 1mm distance；Then using the gradient-structure layout viewing of drafting as
Reference, engraving processing is carried out to silicon template；The substrate of selection is substrate of glass, and carries out prerinse to it, i.e., by substrate of glass
10 ~ 20min of ultrasound in acetone, absolute alcohol, deionized water successively, supersonic frequency is 50 ~ 100Hz, is eluted with water afterwards simultaneously
Processing is dried；Then the silicon template handled well is fitted tightly on the glass basic surface after prerinse；By step（1）
Uniform fold is in silicon template surface by way of spin coating for the coating liquid of preparation, and the spin coating number of times of specific spin coating mode is 1 time, first
With 1500 turns per minute of speed spin coating 5s, then with 8000 turns per minute of speed spin coating 20s, finally with 1500 turns per minute
Speed spin coating 5s, afterwards has spin coating the silicon template of coating liquid using temperature as 75 DEG C of dry 20min, so that on the surface of silicon template 3
Upper formation coating liquid film 2；
Step（3）Prepare with flexible multistage gradient body structure surface：Preparation thickness is 1mm, a width of 25mm VHB adhesive tapes 1, elder generation
By VHB Tape Pulls, and 50% dependent variable is maintained, then by step（2）Obtained mask plate spin coating has coating liquid film 2
Simultaneously it is brought into close contact with the VHB adhesive tapes after stretching, 2 hours is handled in temperature is 80 DEG C of baking oven；Afterwards by substrate of glass
Taken off with silicon template, the coating liquid film for replicating silicon template gradient-structure is just brought into close contact with VHB adhesive tapes；Finally release pair
The pulling force of VHB adhesive tapes, the polydimethylsiloxanefilm film being close on VHB tape surfaces is just because convergent force is produced in its surface
The multilevel hierarchy 5 that raw flexing is combined with gradient；
Step（4）Prepare shutter 6：Go out an antiparallelogram using three-dimensional drawing Software on Drawing, the trapezoidal upper long 25mm of short side, under
Long length of side 82.8mm, high 50mm, the long 115mm of two waists and be respectively 120 ° and 60 ° with upper following angle take a thickness 0.3mm, chi
Very little and above-mentioned antiparallelogram identical copper sheet, is allowed to angle in 90 ° along trapezoidal high fold by copper sheet, that is, is converted into the screening of a wedge shape
Baffle plate；
Step（5）Prepare the surface that chemical gradient is combined with flexible multilevel gradient-structure：By step（4）Obtained shutter
Triangle long edge position is covered in step（3）What is prepared has on flexible multistage gradient body structure surface, the wedge-like opening of shutter
Direction is the more dense direction of pillar on VHB adhesive tapes；Place it in Surface Treatment with Plasma machine to handle and taken out after 60min,
The surface that chemical gradient is combined with flexible multilevel gradient-structure is obtained after shutter is removed.
Step（6）Pass through step by 3（1）Extremely（5）Obtained chemical gradient is combined with flexible multilevel gradient-structure
Surface, according to the order that surface pillar is close by dredging, " Y " font is arranged in by the surface of 3 said structures from top to bottom,
It is assembled into a microreactor；Described " Y " font arrangement, is the microreactor of two kinds of liquid reactant mixtures, can be optionally
It is further added by required runner.Reaction liquid flows first to " Y " font middle and collects mixing, and the end of " Y " font is then flowed to again
End.
The present embodiment of embodiment 2 and the difference of embodiment 1 are：Suitably substrate is stretched, material can be caused
Material surface pillar arrangement becomes more sparse, so that the hydrophobicity of material surface is slightly changed, and then to the flowing speed of fluid
Degree produces influence.
There is buckling structure on a kind of regulatable self-driven microreactor of drop prepared by this method, material surface,
Also there is the column structure of distribution gradient, and material surface has a chemical gradient on buckling structure, wetability by hydrophobicity by
Fade to hydrophily.Liquid contact angle on material surface different length direction is different, so as to be dropped in the anti-of " Y " font upper end
Answer fluid to be occurred displacement by the driving of surface tension, the reaction of " Y " font intersection is come together in, most after vertical runner
Upper outflow.
Claims (1)
1. a kind of preparation method of the self-driven microreactor of regulatable drop, it is characterised in that comprise the following steps：
Step（1）Prepare coating liquid：By the prepolymer of dimethyl silicone polymer and crosslinking agent using quality as 10:1 ratio mixing
Stir, be placed on afterwards in vacuum drying chamber and extract 20min with vavuum pump, remove the bubble in solution, poly- diformazan is made
The coating liquid of radical siloxane；
Step（2）Prepare mask plate：A length of a film 50mm, width 25mm, thickness 1mm silicon template are taken, three-dimensional drawing Software on Drawing is utilized
Go out gradient-structure layout viewing, the gradient-structure layout viewing be with a diameter of 10 μm, deep 40 μm cell orifice in template in ladder
Degree distribution, the gradient distribution mode along the long side of template to be defined, using unit pitch of holes in first 1mm distance as 10 μm,
Unit pitch of holes increases to 20 μm and so in second 1mm distance；Then using the gradient-structure layout viewing of drafting as
Reference, engraving processing is carried out to silicon template；The substrate of selection is substrate of glass, and carries out prerinse to it, i.e., by substrate of glass
10 ~ 20min of ultrasound in acetone, absolute alcohol, deionized water successively, supersonic frequency is 50 ~ 100Hz, is eluted with water afterwards simultaneously
Processing is dried；Then the silicon template handled well is fitted tightly on the glass basic surface after prerinse；By step（1）
Uniform fold is in silicon template surface by way of spin coating for the coating liquid of preparation, and the spin coating number of times of specific spin coating mode is 1 time, first
With 1500 turns per minute of speed spin coating 5s, then with 8000 turns per minute of speed spin coating 20s, finally with 1500 turns per minute
Speed spin coating 5s, afterwards has spin coating the silicon template of coating liquid using temperature as 75 DEG C of dry 20min, so that on silicon template surface
Form the film of coating liquid；
Step（3）Prepare with flexible multistage gradient body structure surface：Preparation thickness is 1mm, a width of 25mm VHB adhesive tapes, elder generation
By VHB Tape Pulls, and 50% dependent variable is maintained, then by step（2）Obtained mask plate spin coating has the one of coating liquid film
Face is brought into close contact with the VHB adhesive tapes after stretching, and 2 hours are handled in temperature is 80 DEG C of baking oven；Afterwards by substrate of glass with
Silicon template is taken off, and the coating liquid film for replicating silicon template gradient-structure is just brought into close contact with VHB adhesive tapes；Finally discharge to VHB
The pulling force of adhesive tape, the polydimethylsiloxanefilm film being close on VHB tape surfaces is just because convergent force is produced in its surface
The multilevel hierarchy that flexing is combined with gradient；
Step（4）Prepare shutter：Go out an antiparallelogram using three-dimensional drawing Software on Drawing, the trapezoidal upper long 25mm of short side, under
Long length of side 82.8mm, high 50mm, the long 115mm of two waists and be respectively 120 ° and 60 ° with upper following angle take a thickness 0.3mm, chi
Very little and above-mentioned antiparallelogram identical copper sheet, is allowed to angle in 90 ° along trapezoidal high fold by copper sheet, that is, is converted into the screening of a wedge shape
Baffle plate；
Step（5）Prepare the surface that chemical gradient is combined with flexible multilevel gradient-structure：By step（4）Obtained shutter
Triangle long edge position is covered in step（3）What is prepared has on flexible multistage gradient body structure surface, the wedge-like opening of shutter
Direction is the more dense direction of pillar on VHB adhesive tapes；Place it in Surface Treatment with Plasma machine to handle and taken out after 60min,
The surface that chemical gradient is combined with flexible multilevel gradient-structure is obtained after shutter is removed；
Step（6）To at least 3 and pass through step（1）Extremely（5）Obtained chemical gradient is combined with flexible multilevel gradient-structure
Surface, according to the order that surface pillar is close by dredging, the surface of at least 3 said structures is arranged in one " Y " from top to bottom
Font, is assembled into a microreactor；At least two reacting fluids can first come together in intersection reaction, and it is vertical to flow to again afterwards
Runner.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114700004A (en) * | 2022-05-20 | 2022-07-05 | 东莞理工学院 | Soap film type microchemical reactor |
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| CN1654311A (en) * | 2005-03-09 | 2005-08-17 | 吉林大学 | Method for constructing non-close packing colloid balls ordered arrangement using soft-graving technology |
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| CN107159072B (en) | 2019-03-19 |
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