CN110423374A - In the method that microfluidic channel plate surface prepares wettability gradient - Google Patents
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- CN110423374A CN110423374A CN201910687661.9A CN201910687661A CN110423374A CN 110423374 A CN110423374 A CN 110423374A CN 201910687661 A CN201910687661 A CN 201910687661A CN 110423374 A CN110423374 A CN 110423374A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
- B01L3/502707—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by the manufacture of the container or its components
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01L2300/161—Control and use of surface tension forces, e.g. hydrophobic, hydrophilic
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- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
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- C08J2325/04—Homopolymers or copolymers of styrene
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2333/10—Homopolymers or copolymers of methacrylic acid esters
- C08J2333/12—Homopolymers or copolymers of methyl methacrylate
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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
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Abstract
The invention discloses a kind of methods for preparing wettability gradient in microfluidic channel plate surface, comprising the following steps: microfluidic channel plate material surface preparation, acquisition prepare the microfluidic channel plate material of surface active；By the alkene microfluidic channel plate material after activating pretreatment directly with the polyethylene glycol oxide reaction solution system containing different molecular weight, different location, which graft reacting, obtains the microfluidic channel plate material of different wetting；Microfluidic channel plate material after grafting is sufficiently cleaned, through being dried in vacuo after removal residual reactants to obtain the final product.The modified surface that this method carries out grafting acquisition can obtain different degrees of wetability, and it has excellent stability, surface can greatly reduce the interaction with substances such as albumen, and all kinds of medical materials or field of medical appliances using microfluidic channel plate as raw material can be widely used.This method is easy to operate, controllable strong, can industrialization.
Description
Technical field
The present invention relates to material surface modifying methods, and in particular to a kind of in microfluidic channel plate surface preparation wetability ladder
The method of degree.
Background technique
Immediately detection (point-of-care testing, POCT) is the clinical inspection that can be carried out at one's side in patient
It surveys, i.e., a kind of analyzing detecting method analyzed immediately in sampling location.This method not only eliminates sample in laboratory
The processing routine of various complexity when detection, and very can fast and accurately obtain a kind of new methods of testing result.
And microflow control technique is easy to operate, low manufacture cost, high sensitivity, high throughput and the features such as device miniaturization meet the skill of POCT
Art theory and growth requirement.In these years, microflow control technique has gradually become the hot research object and core in real-time test field
Heart technology.
Microfluidic chip technology set Micromechanics, microelectronics, microorganism and nanotechnology, are an emerging intersections
Property new disciplines.It is related to many basic subjects, such as physics, biology and chemistry.Purpose is by microfluid in microcontroller
Operation and control realize analytical equipment miniaturization, it is integrated and automation.It is able to achieve the analytic function of chemical laboratory,
It such as sampling, pre-processes, reaction, separation and one step of detection are completed.Final to realize chip, this is known as " array experiment
Room ".
Biomaterial is contacted with each other by surface and human body, therefore the outermost property of material determines organism to implant
Reaction and material it is also critically important to the bioenvironmental reaction of surrounding.Currently, the polymer of many unmodified mistakes is implanted into
After organism, local injected organism tissue often repels it as foreign matter, to can cause some adverse reactions.And pass through modification
Later polymer can be received by injected organism tissue, to reduce adverse reaction, strengthen between material and injected organism tissue
Adaptability.And the hydrophilic and hydrophobic of material surface is also a key factor for influencing protein absorption and cell adherence.Largely
Experimental studies results discovery hydrophilic surface have better wetability and biocompatibility.
The phenomenon that wetting refers to liquid and solid contact, declines solid surface energy, wetting action mainly pass through measurement
Contact angle come carry out characterization material wetability.The chemical component of material surface and it is microcosmic on construction be influence surface wettability
The main reason for, transition material wettability of the surface can be carried out via the micro forming of surface modification and surface.So for
Studying intensively for material surface wetability has great meaning in material engineering.
The micro/nano structure of microchannel inner surface also influence whether microfluid wherein flow when heat transfer, mass transport process.
Various functional groups (amino, sulfydryl, carboxyl etc.) are introduced by people usually using the silane coupling agent for having different activities end group
In microfluidic channel after pre-processing, to change material surface wetability.
Polyethylene glycol oxide, also known as polyethylene oxide (PEO) are a kind of white particulate powder.With crystallinity and thermoplastic
Property, it is a kind of water-soluble polymer, has the characteristics that non-toxic, thickening, lubrication and water-retaining property.Due to its good hydrophily
Can, after pretreatment or method for oxidation, it is grafted the polyethylene glycol oxide of different molecular weight on the surface of the material, protein can be reduced
Absorption with blood platelet on surface substantially increases the biocompatibility of material.
Microfluidic chip technology in the great potential in the fields such as biology, chemistry, medicine, have been developed as a biology,
The brand-new research field of the subject crossings such as chemistry, medicine, fluid, electronics, material, machinery.Therefore, to the surface of micro-fluidic chip
Modification, regulation wetability have important research significance.The surface modification of material is a kind of easy-to-use method, can be according to material
Material itself selects adaptable selection.The properties such as its mechanics for neither influencing itself, physics and chemistry, and material surface property can be made to obtain
To improvement, surface post-processing is carried out again especially suitable for material to be made after biology device.
Summary of the invention
Goal of the invention: the technologies such as uncontrollable are reacted for above-mentioned introducing harmful substance of the existing technology and grafting
Problem, this application provides one kind to graft different molecular weight polyethylene glycol oxide in microfluidic channel plate surface to prepare wetability ladder
The method of degree.
Technical solution: a kind of method preparing wettability gradient in microfluidic channel plate surface of the present invention, including
Following steps:
(1) microfluidic channel plate material surface preparation prepares the microfluidic channel plate material of surface active；
(2) aqueous solution of microfluidic channel plate material and different molecular weight polyethylene glycol oxide after activating pretreatment is carried out
Grafting reaction, obtains the microfluidic channel plate material of different wetting gradient；
(3) it by the microfluidic channel plate material cleaning removal residual reactants after grafting, is dried in vacuo to obtain the final product.
In step (1), the method selection dopamine for carrying out activating pretreatment to microfluidic channel plate material surface is pre-processed
Method, activation microfluidic channel plate material surface obtain hydrophily adsorption activity position, and the processing time is treatment temperature 25 for 24 hours
℃.Wherein, dopamine concentration 0.5-40mM, preferably 2mg/mL.
In step (1), the method for carrying out activating pretreatment to microfluidic channel plate material surface can also select ozone oxygen
Change processing, processing time are 10-60 minutes, ozone concentration 2-80mgL-1。
Preferably, the ozone Oxidation Treatment reaction time is 15-30 minutes, ozone concentration 10-20mgL-1。
In step (2), the different molecular weight polyethylene glycol oxide includes 1000,2000,10000,100000,300000 points
The polyethylene glycol oxide of son amount.
The aqueous solution of microfluidic channel plate material and different molecular weight polyethylene glycol oxide after the activating pretreatment carries out
The grafting of different parts is reacted, i.e. can graft different molecular weight polyethylene glycol oxide in different portions on one block of microfluidic channel plate
Position, is allowed to generate the gradient of different wetting.
In step (2), the concentration of aqueous solution of the polyethylene glycol oxide is 0.8-8.5%, preferably 2-4%, most preferably
4%；Grafting reaction carries out in air, and the time is 6-48 hours, and preferably 20~30 DEG C reactions 12~for 24 hours.
The microfluidic channel plate material is dimethyl siloxane, polystyrene, polymethyl methacrylate, polyester etc..
In step (3), after the cleaning refers to and makes to be washed with deionized 3-8 times at normal temperature, then in deionized water
It is cleaned by ultrasonic 5-10min.
The modification microfluidic channel plate surface that present invention processing obtains is stablized, and is connect using the water that dopamine pre-processes its surface
Feeler controlled range realizes the coarse adjustment of surfaces of microfluidic channels wetability at 20-85 °；Its surface is pre-processed using ozone oxidation
Water contact angle controlled range at 60-85 °, realize surfaces of microfluidic channels wetability fine tuning.
The utility model has the advantages that technical solution process provided by the invention is simple controllable strong, can industrialization, pre-process microfluidic channel
Hydrophilic characteristics are presented to obtain adsorption activity position in plate material surface.The surface object of high molecular polymer can thus be improved
Physical chemistry characteristic, and then change the adsorbed state of hydrophilic polymer presoma, to simplify subsequent technique and improve grafting effect
Rate can be combined with surface texture easily.The adsorption structure of hydrophilic polymer presoma changes and adsorbance increases, to rear
Continuous graft polymerization reaction generates important influence.Therefore, before dipping absorption, suitable surface treatment and improvement adsorption bar
Part, so that grafting coating procedure has many advantages, such as that reactant composition is easy regulation, the harmful substance in reduction and elimination reaction.Example
The addition of additive is such as reduced, and reaction condition controllability is strong in engineering, industrialized production easy to accomplish.Polyethylene glycol oxide
With not with the protein-interacting in serum, improve test correctness the advantages of.After pretreatment, different molecular weight polyoxy
The grafting for changing ethylene, allows material to form different wettability gradient structures.
Detailed description of the invention
Fig. 1 is the contact angle after the polyethylene glycol oxide modification of typical different molecular weight；
Fig. 2 is the wetability of typical microfluidic channel plate surface after surface modification.
Specific embodiment
The present invention is described in detail below in conjunction with embodiment.
Technical solution of the present invention can specifically use following steps:
(1) microfluidic channel plate material surface clean uses deionized water respectively, and ethyl alcohol cleaning is stand-by after vacuum drying；It is micro-
Fluid channel plate material, is pre-processed by dopamine, and to obtain sufficient surface-active, the processing for after provides basis；
(2) polyoxyethylene for 2000,10000,100000,300000 molecular weight that concentration is 4% is prepared in ultrapure water
Aqueous solution.Polyethylene glycol oxide needs evenly dispersed and dissolution wherein.Microfluidic channel plate material is added in reaction solution, In
It is reacted under constant temperature.Wherein, 25 DEG C of reaction temperature, reaction time are 24 hours.
(3) the microfluidic channel plate material after reacting washs 3 times in deionized water, is cleaned by ultrasonic in deionized water
5min is saved after vacuum drying and is used.In last cleaning process, wash temperature is 25 DEG C in deionized water.
Wherein, dopamine pretreatment may is that by dopamine (2mg/mL) be dissolved in Tris-HCL buffer solution (pH=8.5,
In 50mM).Microfluidic channel plate immerses in Tris-HCL buffer solution 24 hours in the quiescent state.Examination is thoroughly rinsed with deionized water
Sample three times, obtains the microfluidic channel plate of dopamine coating.It saves and uses after vacuum drying 5 hours.
Embodiment 1: the sufficiently cleaning in 5 minutes of dimethyl siloxane microfluidic channel plate plate ultrasound is dried in vacuo 5 hours
Afterwards, it takes out stand-by；20mL Tris-HCl buffer solution is taken, wherein by the dopamine dissolution of 2mg/mL, by the miniflow after drying
After body channel plate immerses 24 hours, taking-up deionized water is rinsed three times, stand-by after vacuum drying；With 1% 300000 molecules
The polyoxyethylene aqueous solution of amount immerses the pretreated microfluidic channel plate after drying 24 hours, and deionization is used in taking-up
Water rinses three times, dry.After tested, water contact angle is directly down to 13 ° from 85 °, and modified effect is obvious.
Embodiment 2: by the sufficiently cleaning of polystyrene microfluidic channel ultrasound 5 minutes, after vacuum drying 5 hours, take out to
With；20mL Tris-HCl buffer solution is taken, wherein by the dopamine dissolution of 2mg/mL, by the microfluidic channel plate after drying
After immersing 24 hours, taking-up deionized water is rinsed three times, stand-by after vacuum drying；With 4% 1000,2000,10000,
100000, the pretreated microfluidic channel plate after drying is immersed 24 by the polyoxyethylene aqueous solution of 300000 molecular weight
Hour, taking-up deionized water rinses three times, dry.
Embodiment 3
It is compared to embodiment 2, step 1 is revised as using 15mgL by the present embodiment-1Ozone pre-process 15 minutes,
Concrete operations are as follows: clean polystyrene microfluidic channel material is placed in a reservoir, is 15mgL by concentration-1Ozone gas
Body slowly flows across, and surface contact activation is kept for the reaction time 15 minutes.
By the microfluidic channel material of embodiment 2 and embodiment 3, a sample test 6 is not all in water contact angle instrument
Position, 3 samples are one group, and statistics obtains water contact angle.As a result as shown in Figure 1, the water on the surface that dopamine pretreatment obtains
Contact angle controlled range uses the surface water of ozone treatment to contact controlled range as 60-85 ° at 20-85 °.It can be seen that this Shen
Please method may be implemented to prepare wettability gradient in microfluidic channel plate surface, and the control of two kinds of different accuracies may be implemented
System.Specifically, can control using the pretreating scheme of ozone oxidation in 5 ° or so the high-precisions as a gradient.And
And water contact angle is 60-85 ° of common wetability claimed range in industrial application.It, can using the pretreating scheme of dopamine
To control in 12 ° or so as one gradient.The two combines, and can realize diversified side in terms of microfluidic channel wetability
Case.
Embodiment 4: by the sufficiently cleaning of polystyrene microfluidic channel ultrasound 5 minutes, after vacuum drying 5 hours, take out to
With；20mL Tris-HCl buffer solution is taken, wherein by the dopamine dissolution of 2mg/mL, by the microfluidic channel plate after drying
After immersing 24 hours, taking-up deionized water is rinsed three times, stand-by after vacuum drying；With 4% 300000,100000 and
The polyoxyethylene aqueous solution of its 300000 molecular weight is dripped and is led in microfluid by the polyoxyethylene aqueous solution of 10000 molecular weight
The time control area of guidance tape, for the drop of 100000 molecular weight in the sample application zone of microfluidic channel plate, the drop of 10000 molecular weight is logical in microfluid
In the microballoon area of guidance tape, after reaction 24 hours, taking-up deionized water is rinsed three times, dry.This method can be in microfluid
Different zones form different wetabilitys on channel plate, and typically the wetability of microfluidic channel plate surface after surface modification is such as
Shown in Fig. 2.
Embodiment 5: the sufficiently cleaning in 5 minutes of polymethyl methacrylate microfluidic channel plate ultrasound is dried in vacuo 5 hours
Afterwards, it takes out stand-by；20mL Tris-HCl buffer solution is taken, wherein by the dopamine dissolution of 2mg/mL, by the miniflow after drying
After body channel plate immerses 24 hours, taking-up deionized water is rinsed three times, stand-by after vacuum drying；With 8.2% 300000,
The polyoxyethylene aqueous solution of 10000 and 2000 molecular weight drips the polyoxyethylene aqueous solution of its 300000 molecular weight micro-
The time control area and waste fluid channel area of fluid channel plate, the drops of 10000 molecular weight is in the microballoon area of microfluidic channel plate, and 2000 points
The drop of son amount is in the microballoon area of microfluidic channel plate, and after reaction 24 hours, taking-up deionized water is rinsed three times, dry.This
Kind method different zones can form different wetabilitys on microfluidic channel plate.
Embodiment 6
It is compared to embodiment 4, step 1 is revised as using 25mgL by the present embodiment-1Ozone pre-process 30 minutes.
Remaining operation is the same as embodiment 4.
Embodiment 7
It is compared to embodiment 5, step 1 is revised as using 10mgL by the present embodiment-1Ozone pre-process 45 minutes.
Remaining operation is the same as embodiment 5.
Embodiment 8
It is compared to embodiment 5, step 1 is revised as using 5mgL by the present embodiment-1Ozone pre-process 45 minutes.
Remaining operation is the same as embodiment 5.
Embodiment 9
It is compared to embodiment 5, step 1 is revised as using 80mgL by the present embodiment-1Ozone pre-process 25 minutes.
Remaining operation is the same as embodiment 5.
Claims (10)
1. a kind of method for preparing wettability gradient in microfluidic channel plate surface, which comprises the following steps:
(1) microfluidic channel plate material surface preparation prepares the microfluidic channel plate material of surface active；
(2) by after activating pretreatment microfluidic channel plate material and the aqueous solution of different molecular weight polyethylene glycol oxide graft
Reaction, obtains the microfluidic channel plate material of different wetting gradient；
(3) it by the microfluidic channel plate material cleaning removal residual reactants after grafting, is dried in vacuo to obtain the final product.
2. the method according to claim 1 for preparing wettability gradient in microfluidic channel plate surface, which is characterized in that step
Suddenly in (1), the method selection dopamine preprocess method of activating pretreatment is carried out to microfluidic channel plate material surface, is activated micro-
Fluid channel plate material surface obtains hydrophily adsorption activity position.
3. the method according to claim 2 for preparing wettability gradient in microfluidic channel plate surface, which is characterized in that institute
State dopamine concentration 0.5-40mM.
4. the method according to claim 1 for preparing wettability gradient in microfluidic channel plate surface, which is characterized in that step
Suddenly in (1), to the method selection ozone Oxidation Treatment of microfluidic channel plate material surface progress activating pretreatment, the processing time is
10-60 minutes, ozone concentration 2-80mgL-1。
5. the method according to claim 1 for preparing wettability gradient in microfluidic channel plate surface, which is characterized in that step
Suddenly in (2), the different molecular weight polyethylene glycol oxide includes the polyoxy of 1000,2000,10000,100000,300000 molecular weight
Change ethylene.
6. the method according to claim 1 for preparing wettability gradient in microfluidic channel plate surface, which is characterized in that step
Suddenly in (2), the concentration of aqueous solution of the polyethylene glycol oxide is 0.8-8.5%.
7. the method according to claim 1 for preparing wettability gradient in microfluidic channel plate surface, which is characterized in that step
Suddenly (2) grafting reaction carry out in air, 20~30 DEG C reaction 6-48 hours.
8. the method according to claim 1 for preparing wettability gradient in microfluidic channel plate surface, which is characterized in that institute
Stating microfluidic channel plate material is dimethyl siloxane, polystyrene, polymethyl methacrylate or polyester.
9. the method according to claim 1 for preparing wettability gradient in microfluidic channel plate surface, which is characterized in that step
Suddenly in (3), after the cleaning refers to and makes to be washed with deionized 3-8 times at normal temperature, then it is cleaned by ultrasonic 5- in deionized water
10min。
10. the method according to claim 1 for preparing wettability gradient in microfluidic channel plate surface, which is characterized in that
The modified surface of the acquisition is stablized, and the water contact angle controlled range for pre-processing its surface using dopamine is realized at 20-85 °
The coarse adjustment of surfaces of microfluidic channels wetability；The water contact angle controlled range on its surface is pre-processed in 60- using ozone oxidation
85 °, realize the fine tuning of surfaces of microfluidic channels wetability.
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Cited By (1)
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| CN116003863A (en) * | 2023-01-05 | 2023-04-25 | 大连理工大学 | Oxygen plasma modification-based spatial wettability gradient surface modification device and surface modification method |
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| CN116003863A (en) * | 2023-01-05 | 2023-04-25 | 大连理工大学 | Oxygen plasma modification-based spatial wettability gradient surface modification device and surface modification method |
| CN116003863B (en) * | 2023-01-05 | 2024-02-02 | 大连理工大学 | Oxygen plasma modification-based spatial wettability gradient surface modification device and surface modification method |
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