CN105689026B - A kind of method for separating and preparing of microlayer model and microarray - Google Patents
A kind of method for separating and preparing of microlayer model and microarray Download PDFInfo
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- CN105689026B CN105689026B CN201410681689.9A CN201410681689A CN105689026B CN 105689026 B CN105689026 B CN 105689026B CN 201410681689 A CN201410681689 A CN 201410681689A CN 105689026 B CN105689026 B CN 105689026B
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Abstract
The invention discloses the method that the single drop of a kind of separation for belonging to material interface imbibition technique field prepares microlayer model and microarray.This method be by drop in the hydrophilic/hydrophobic substrate of patterning, by controlling the contact force between drop and substrate, and the Relative sliding speed between drop and substrate, the volume of drop can accurately be controlled isolated microlayer model and microarray.Microlayer model separation of the present invention and microarray preparation method, substantial amounts of fine droplet can be prepared using a drop sample solution, microlayer model small volume with separation, low is required to sample solution, required sample is few, and separative efficiency is high, equipment is simple, it is easy to operate, prepare that cost is low, the series of advantages such as application is wider.Drop separation of the present invention and microarray preparation method are with a wide range of applications in patterned surface, bioanalysis and detection, chemical reaction, Field of Drug Discovery.
Description
Technical field
The invention belongs to material interface imbibition technique field, more particularly to separate single drop and prepare microlayer model and microarray
Method.
Background technology
Microlayer model is prepared in bioanalysis and detection, chemical reaction, medicament research and development, patterned surface field with extensive
Application prospect.Current microlayer model preparation method mainly includes physics confinement (bibliography：R.J.Jackman,D.C.Duffy,
E.Ostuni,N.D.Willmore,G.M.Whitesides,Anal.Chem.1998,70,2280-2287；E.Ostuni,
C.S.Chen, D.E.Ingber, G.M.Whitesides, Langmuir 2001,17,2828-2834.), T-shaped duct it is micro-fluidic
Prepare (Patents number：CN104084247A, CN104107734A, CN104130932A), printing prepare (Patents number：
CN104004652A, CN103974547A) etc..But, there is many defects, including required sample size in currently used method
Greatly, required equipment is costly or complicated, and the microlayer model of preparation, which is among oil phase is surrounded, to be difficult to separate, and the microlayer model body prepared
Product is big.For sample it is very expensive or amount and its it is few in the case of, using current techniques be difficult to realize a large amount of microlayer models separation and
The simple preparation of microarray.
The content of the invention
To solve above-mentioned the problems of the prior art, the present invention provides one kind and realizes that drop is cut using surface differential
The method for preparing microlayer model and microarray.
Cutting liquid dripping proposed by the present invention is for the technical scheme of microlayer model and microarray：By drop patterning parent
On aqueous/hydrophobic substrate, by controlling the contact force between drop and substrate, and the Relative sliding between drop and substrate
Speed, can accurately be controlled isolated microlayer model and microarray by the volume of drop.
Microlayer model separation method of the present invention is：
1) hydrophilic region and water repellent region of patterning, are constructed in substrate surface；
2) drop, is dragged in substrate surface with 0-650 μ N pressure and 1-20mm/s speed.
Described water repellent region contact angle is more than 100 °, preferably 140-180 °；Described hydrophilic region contact angle is small
In 60 °, preferably 0-20 °.
Described drop is the liquid between polarity 28-80mN/m, and the volume of the drop is more than the resolution ratio of pattern.
One or more of the drop in water, ethylene glycol, propane diols, glycerine, dimethyl sulfoxide (DMSO), or be selected from
Inorganic salt solution, nano-particle solution, cell solution, protein solution, DNA solution, blood plasma.
By hydrophilic material, either hydrophilic base is constituted or obtained through Hydrophilic modification described hydrophilic region；
Described water repellent region is made up of hydrophobic material or hydrophobic substrate, or is obtained through hydrophobically modified.
Described hydrophilic base is selected from hydrophilic metal, hydrophilic metal oxide, glass, silicon chip, hydrophilic polymer
One or more in thing film, hydrophily timber, paper, hydrophilic fiber fabric.
Described hydrophobic substrate in hydrophobic metals, hydrophobic metal oxide, hydrophobic polymer film one
Plant or several.
Described hydrophilic material is selected from hydrophilic nanoparticles, hydrophily micro particles, hydrophilic polymer, hydrophily
One or more in molecule.
Described hydrophobic material be selected from dimethyl silicone polymer, polystyrene, polytetrafluoroethylene (PTFE), poly(perfluoropropene), dredge
Aqueous nanoparticle, silane, silicon fluoride, chlorosilane, fluorosilicone, chlorine siloxanes, polyvinyl chloride, in one or more.
Described Hydrophilic modification method be uv-exposure, ion beam etching, corona treatment, at Piranha washing lotion
One or more in reason, spin-coating method, spraying process, electrospinning, printing, electrochemical corrosion.
Described hydrophobically modified method be gas phase modification method, liquid phase modification method, spin-coating method, spraying process, electrospinning, printing,
One or more in electrochemical corrosion.
After solvent volatilization in the above-mentioned microlayer model prepared, remaining solute formation microarray.
Above-mentioned microlayer model separation method bioanalysis and detection, chemical reaction, medicament research and development, sample separation field should
With.
Microlayer model separation of the present invention and microarray preparation method, can be prepared a large amount of using a drop sample solution
Fine droplet, the microlayer model small volume with separation requires low, required sample is few, separative efficiency is high, equipment to sample solution
Simply, it is easy to operate, prepare that cost is low, the series of advantages such as application is wider.Drop separation of the present invention and micro- battle array
Row preparation method is before patterned surface, bioanalysis and detection, chemical reaction, Field of Drug Discovery have a wide range of applications
Scape.
Brief description of the drawings
Drop separation prepares the home-built equipment schematic diagram used in microlayer model array in Fig. 1 present invention；
The schematic diagram of microlayer model array prepared by Fig. 2 drop separations of the present invention；
Reference：1-X-Y mobile controllers, 2- a ten thousandth balances, 3- has the hydrophobicity of hydrophily area of the pattern
Substrate, 4- is used for the original slip drop that drop cutting prepares microlayer model, microlayer model prepared by the cutting of 5- drops.
Embodiment
Embodiment 1
Ethylene glycol microlayer model array is prepared using a drop ethylene glycol solution.Silicon chip is subjected to cleaning treatment, specific steps are such as
Under：It is ultrasonic three times to silicon chip respectively with acetone and ethanol solution, rinsed well with deionized water.Then silicon chip is immersed into volume integral
In toluene solution of the number for 1% octadecyl trichlorosilane alkane, soak 10 minutes, dried up after taking-up with nitrogen.Whole process is all
Carried out in clean room, prevent dust in air etc. from polluting silicon chip.Now the contact angle of silicon chip is 106 °.Then hydrophily is carried out
The preparation in region.Silicon chip is placed under photomask board, is then placed under the ultraviolet light that wavelength is 365nm, is exposed 10 minutes.
In exposure process, the octadecyl trichlorosilane alkane molecule in transmission region is decomposed, and the region is changed into hydrophilic region simultaneously.
A drop ethylene glycol solution is fixed with suction pipe, ethylene glycol drop is being contained hydrophily with the speed of 650 μ N pressure and 10mm/s
The hydrophobicity silicon chip surface in region is slided.Because hydrophilic region is different to the adhesiveness of ethylene glycol solution with water repellent region,
Therefore the microlayer model array of ethylene glycol can be obtained in hydrophilic region.
Embodiment 2
Dyestuff pattern is prepared with a drop dye solution.The filter paper that laboratory is commonly used carries out hydrophobization modification.Proved recipe in fact
Method is：By filter paper be placed in cleaning vacuum desiccator in, a piece of slide is placed wherein, to slide on drip the perfluor last of the ten Heavenly stems
Base trimethoxy silane.Then vacuum desiccator is vacuumized 10 minutes with oil pump.Then by drier in 60 degrees Celsius of baking ovens
It is middle to place 2 hours.After taking-up, the static contact angle of filter paper is 140 °.The hydrophilic region preparation method of hydrophobicity filter paper is as follows：
5 milliliters of water and 5 milliliters of ethylene glycol are well mixed, the PAA (molecular weight 3000) that mass fraction is 1% is added thereto.Stirring
After uniform, the ink of inkjet printing is used as.Printed with ink-jet printer on hydrophobicity filter paper, the region of ink in printing
It is changed into hydrophilic region, the region for not printing ink remains as water repellent region.One drop dye solution is fixed with dropper,
Rolled with 0 pressure and 20mm/s speed in hydrophobe patterning its surface.Because hydrophilic region glues to dye solution
Attached property is high, and water repellent region is low to the adhesiveness of dye solution, and the difference of adhesiveness causes dye solution to be cut into microlayer model.
The hydrophilic region of its surface is prepared into pattern, then can obtain the microlayer model pattern of dye solution.After solvent is evaporated completely,
Dyestuff pattern is just obtained on filter paper.
Embodiment 3
The preparation of sodium chloride crystal.It is prepared by hydrophilic base：Slide ethanol and acetone is ultrasonic three times, then with steaming
Distilled water is rinsed well, then is dried up with nitrogen.Whole process is carried out in clean room, it is ensured that glass sheet surface is not by air
Impurity pollution.Then surface is prepared to the pattern of hydrophobicity Teflon with micro-machined method.Pattern thickness is at 50 nanometers to 10
Between micron.Now, the surface coated by Teflon is water repellent region, is not hydrophilic by the surface coated region of Teflon
Property region.One drop saturated nacl aqueous solution is fixed with dropper, 200 μ N pressure and 1mm/s speed are in close and distant water patterns
The Teflon of change/hydrophilic glass surface is slided.Teflon surface is small to saturated nacl aqueous solution adhesion, and hydrophilic glass piece is to full
It is big with sodium chloride solution adhesion.Saturated nacl aqueous solution is cut in the big hydrophilic glass panel region of adhesion, as micro- liquid
Drop.With the evaporation of the microlayer model reclaimed water under cutting, sodium chloride gradually forms nucleus and starts to grow up to crystal.It is prepared by this kind of method
Sodium chloride crystal efficiency high, the time is short, easy to operate.
Embodiment 4
The controllable ration separation of microballoon.It is prepared by hydrophobe patterned substrate：Silicon chip is subjected to cleaning treatment, concrete operations are such as
Under：It is ultrasonic three times to silicon chip respectively with acetone and ethanol solution, then cleaned with distilled water, and dried up with nitrogen.Then in silicon
One layer of photoresist positive photoresist of spin coating on piece, photoresist positive photoresist thickness is between 200 nanometers to 3 microns.Under photomask board protection, use
Ultraviolet light carries out selection uv-exposure to photoresist.The region being mapped to by ultraviolet lighting can be washed with developed dose, not by
Still there is photoresist in the region that ultraviolet lighting is mapped to.After being handled completely with developer, silicon chip is carried out with the method for vapour deposition
Hydrophobically modified, concrete operation method is with example 2.After the completion of modification, the silicon chip that part is covered into photoresist is small with acetone ultrasound 1
When, remove remaining photoresist.Now, the region of photoresist is newly removed due to not being modified during hydrophobically modified,
Therefore it is hydrophilic region.The wafer sections exposed during hydrophobically modified are changed into water repellent region.Then dropper control is used
The polystyrene microsphere solution (mass fraction 5%) of a diameter of 5 microns of the drop of system one is existed with the speed of 500 μ N pressure and 15mm/s
The silicon chip surface of hydrophobe patterning is slided.Because hydrophilic and hydrophobic region is different to the adhesion of microspheres solution, therefore microballoon is molten
Liquid drop is cut, as microlayer model.After solvent is evaporated in microlayer model, then the separation to microballoon can be achieved.Pass through capping
Speed and pressure that the size and microspheres solution drop of hydrophilic region are slided in silicon chip surface, it is possible to achieve micro- to isolating
The quantity of ball is controlled, so as to realize the separation of the controlled quantity of microballoon.
Embodiment 5
Unicellular separation.The preparation of hydrophobe patterned substrate：By butyl methacrylate, dimethacrylate time second
Ester, 1- decyl alcohol, cyclohexanol, 2,2- dimethoxy -2- phenyl acetophenones in mass ratio 10:16：24:49:1 ratio mixing is equal
It is even.Then mixture is placed in distance between 1mm two parallel glass pieces, to add photomask board, it is then ultraviolet in 365nm
Irradiated 10 minutes under light, carry out selective light initiation polymerization.Remove sheet glass after polymerization, the polymer film of formation is hydrophobe
Property patterned film.The region of printing opacity can trigger photopolymerization on photomask board, contact angle after the polymer polymerizing below the region
For 155 °.Other lighttight regions can not trigger photopolymerization on photomask board, the polymer film contact angle below the region
For 20 °.A drop cell liquid is fixed with dropper, the substrate surface patterned with the speed of 300 μ N pressure and 5mm/s in hydrophobe
Slide.Because hydrophilic region is different to the adhesiveness of cell liquid with water repellent region, therefore cell liquid drop can be cut
Into the microlayer model containing cell.By controlling the concentration of cell liquid and the size of hydrophilic region, it is possible to achieve single celled point
From.
Claims (8)
1. a kind of microlayer model separation method, it is characterised in that its concrete operation step is：
1) hydrophilic region and water repellent region of patterning are constructed in substrate surface；
2) drop is dragged in substrate surface with 0-650 μ N pressure and 1-20mm/s speed.
2. microlayer model separation method according to claim 1, it is characterised in that described water repellent region contact angle is more than
100°；Described hydrophilic region contact angle is less than 60 °.
3. microlayer model separation method according to claim 1, it is characterised in that described drop is polarity 28-80mN/m
Between liquid, the volume of the drop is more than the resolution ratio of pattern.
4. microlayer model separation method according to claim 1, it is characterised in that the drop is selected from water, ethylene glycol, the third two
One or more in alcohol, glycerine, dimethyl sulfoxide (DMSO), or selected from inorganic salt solution, nano-particle solution, cell solution,
Protein solution, DNA solution, blood plasma.
5. microlayer model separation method according to claim 1, it is characterised in that described hydrophilic region is by hydrophily material
Either hydrophilic base is constituted or obtained through Hydrophilic modification material；Described water repellent region is by hydrophobic material or hydrophobic
Property substrate constitute, or obtained through hydrophobically modified.
6. microlayer model separation method according to claim 5, it is characterised in that described hydrophilic base is selected from hydrophily
In metal, hydrophilic metal oxide, glass, silicon chip, hydrophilic polymer film, hydrophily timber, paper, hydrophilic fiber fabric
One or more；
One kind in hydrophobic metals, hydrophobic metal oxide, hydrophobic polymer film of described hydrophobic substrate or
It is several；
Described hydrophilic material is selected from hydrophilic nanoparticles, hydrophily micro particles, hydrophilic polymer, hydrophilic molecule
In one or more；
Described hydrophobic material is selected from dimethyl silicone polymer, polystyrene, polytetrafluoroethylene (PTFE), poly(perfluoropropene), hydrophobicity
One or more in nano-particle, silane, silicon fluoride, chlorosilane, fluorosilicone, chlorine siloxanes, polyvinyl chloride；
Described Hydrophilic modification method is uv-exposure, ion beam etching, corona treatment, the processing of Piranha washing lotion, rotation
One or more in coating, spraying process, electrospinning, printing, electrochemical corrosion；
Described hydrophobically modified method is gas phase modification method, liquid phase modification method, spin-coating method, spraying process, electrospinning, printing, electrification
Learn the one or more in corrosion.
7. after the solvent volatilization in the microlayer model prepared according to any described microlayer model separation methods of claim 1-6,
Remaining solute formation microarray.
8. microlayer model separation method according to claim 1 is in bioanalysis and detection, chemical reaction, medicament research and development, sample
The application of product separation field.
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