CN108654711A - A kind of method of solid liquid interface stick-slip under reduction electric field - Google Patents

A kind of method of solid liquid interface stick-slip under reduction electric field Download PDF

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Publication number
CN108654711A
CN108654711A CN201810581254.5A CN201810581254A CN108654711A CN 108654711 A CN108654711 A CN 108654711A CN 201810581254 A CN201810581254 A CN 201810581254A CN 108654711 A CN108654711 A CN 108654711A
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liquid interface
microlayer model
solid liquid
stick
voltage
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CN108654711B (en
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张亚锋
王永宁
吴晓兰
余家欣
姚永瑰
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Sichuan Minhui Technology Co.,Ltd.
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Southwest University of Science and Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B01L3/50273—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 means or forces applied to move the fluids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/06—Auxiliary integrated devices, integrated components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/12—Specific details about materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/16—Surface properties and coatings
    • B01L2300/161—Control and use of surface tension forces, e.g. hydrophobic, hydrophilic
    • B01L2300/165—Specific details about hydrophobic, oleophobic surfaces
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2400/00—Moving or stopping fluids
    • B01L2400/04—Moving fluids with specific forces or mechanical means
    • B01L2400/0403—Moving fluids with specific forces or mechanical means specific forces
    • B01L2400/0415—Moving fluids with specific forces or mechanical means specific forces electrical forces, e.g. electrokinetic
    • B01L2400/0427—Electrowetting

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
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  • Clinical Laboratory Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

The invention discloses a kind of methods of solid liquid interface stick-slip behavior under reduction electric field, this method can significantly improve microlayer model the surface of solids motor behavior, the microlayer model under electric field is set to be run in the surface of solids more smooth, this method is the loading speed by changing DC voltage, microlayer model three-phase line of contact is set to be mutated under the effect of high direct current loading speed, to overcome solid liquid interface to damp, achieve the purpose that effectively to reduce solid liquid interface stick-slip behavior；It can observe that microlayer model is in the stick-slip behavior of solid liquid interface under different voltages loading speed in real time with the increased relational graph of electrowetting constant by comparing microlayer model three-phase line of contact length under different DC voltage loading speeds.The present invention can make microlayer model improve 2 times or more in the operation fluency of the surface of solids；Present invention is primarily based on direct current programmable power supply, contact angle measurement and image processing software, experimental method is easy, visual result, accurately, reliably.

Description

A kind of method of solid liquid interface stick-slip under reduction electric field
Technical field
The invention belongs to microfluidic control system technical fields, and in particular to solid liquid interface is stick-slip under a kind of reduction electric field The method of behavior.
Background technology
Microfluidic control system is integrated in microchip using microchannel network as structure feature, the function in entire laboratory On, it has broad application prospects in fields such as biological monitoring, environmental protection, space flight and aviation.The core of microfluidic control system Technology is the accurate driving and control to microlayer model.And electrowetting on dielectric is excellent with its low energy consumption, simple, the reliability height of preparation etc. Point has become one of the microlayer model actuation techniques to enjoy great popularity.Electrowetting on dielectric refers to conductive surface and microlayer model with insulating layer Isolation changes the wetting characteristics of solid liquid interface by electric field, realizes the driving to microlayer model.Currently, electrowetting on dielectric is The movement to microlayer model, separation and mixing may be implemented, but still there are many problems demands to solve.Microlayer model under electric field is in solid The movement on surface is influenced by factors such as solid liquid interface adhesion strength, surface roughnesses, often shows stick-slip, i.e. microlayer model It will appear motion stage stopping during the motion.Stick-slip makes microlayer model continuously can not smoothly be transported in the surface of solids It is dynamic, adverse effect will produce to accurately controlling for microlayer model.The stick-slip phenomenon of three-phase line of contact to be based on electrowetting on dielectric The fluency of Related product, reliability can not ensure, largely effect on application and development of the electrowetting on dielectric technology on product.
Reducing electrowetting on dielectric solid liquid interface stick-slip at present has following methods：1) preparing has sufficiently low surface The surface of energy；2) it gives additional " vibration energy " and overcomes the stick-slip effect of solid liquid interface；3) it is reduced by high-frequency alternating current solid Liquid interface stick-slip.With regard to method 1) for, the surface energy of solid endless can not reduce, when surface energy reaches certain threshold After value, because being influenced by material attribute itself, surface energy can not further decrease；Method 2) although solid liquid interface can be reduced Stick-slip, but this method needs to be additionally provided vibration source, equipment occupation space is larger, high energy consumption, and microvibration can be difficult Accurately to apply, so can not be applied in actual condition；Method 3) although can be shown by applying high-frequency alternating current Writing reduces electrowetting on dielectric solid liquid interface stick-slip, but needs Special alternating-current power supply.Moreover, with micro-fluidic System is towards micromation, miniaturization, intelligent development, and the offer of power source is mainly based on direct current, therefore AC power Use system will be made increasingly complex.Based on this, invention it is a kind of based on reduced under direct current electrowetting on dielectric solid liquid interface it is viscous- The method of sliding phenomenon seems particularly important.
Invention content
It is excellent it is an object of the invention to solve at least the above and/or defect, and provide at least to will be described later Point.
In order to realize these purposes and other advantages according to the present invention, solid-liquid circle under a kind of reduction electric field is provided The method of face stick-slip, includes the following steps：
Step 1: using conductive material as substrate, it is no more than 2 μm of insulating layer in conductive material surface coating thickness, to exhausted Edge layer surface carries out hydrophobic treatment or coating hydrophobic coating, forms the laboratory sample with sandwich structure；
Step 2: laboratory sample is adhered to fine copper copper coin surface with silver paste, fine copper copper coin is placed in contact angle measurement The microlayer model of arbitrary volume is added dropwise to sample surfaces in platform, and fine copper copper coin is connect with programmable DC positive pole；It will be straight Diameter is inserted into much smaller than the thin copper wire electrode of microlayer model volume inside microlayer model, and by thin copper wire and programmable DC power cathode phase Even；Programmable DC supply voltage range and voltage-drop loading rate are set；Start contact angle measurement, dynamic contact angle is selected to survey Function is measured, the video to change by drop pattern increases with voltage is recorded by contact angle measurement；
Step 3: repeating step 2, new microlayer model is added dropwise to the super-hydrophobic laboratory sample surface of silicon substrate, changes DC power supply Voltage-drop loading rate, obtain different voltages loading speed under drop pattern with voltage change video；
Step 4: microlayer model volume is with voltage change video under the different voltages loading speed that contact angle measurement is recorded It exports frame by frame；Then drop apparent contact angle and contact line length are respectively obtained using contact angle measurement and image processing software The relational graph changed with electrowetting constant；
Step 5: by microlayer model apparent contact angle under the different DC voltage loading speeds of comparison and contact line length with electricity The variation diagram of constant is soaked, quantifies the variation tendency of solid liquid interface stick-slip under different voltages loading speed, to be dropped The optimum voltage loading speed parameter of low solid liquid interface stick-slip.
Preferably, the process of the step 1 is：The SiO of 100~500nm is plated in substrate silicon chip surface2Insulating layer, with Afterwards with the 800 mesh sand paper polishing sample back side, until measuring its resistance value R with digital multimeter<Sample is then placed in super by 20 Ω It in sound wave cleaning machine, is cleaned repeatedly with alcohol and deionized water, until sample surfaces water droplet can not adhere to, finally by laboratory sample It is placed in thermal insulation cabinet；The silicon chip sample cleaned up is placed in desk-top sol evenning machine, uses spin-coating method spin coating Teflon AF1600 breasts Liquid obtains having the super-hydrophobic laboratory sample of the silicon substrate of sandwich structure.
Preferably, the parameter of the spin-coating method is：Low speed 500r/min, time 20s；High speed 3000r/min, time 30s；The silicon chip of spin coating is placed in vacuum drying chamber, using 200 DEG C of baking 3h, natural cooling obtains the super-hydrophobic experiment of silicon substrate Sample.
Preferably, a diameter of 50~200um of the thin copper wire electrode.
Preferably, the programmable DC supply voltage range is set as 0V-120V, and voltage-drop loading rate is 1~ 50V/s。
The basic principle for the method that the present invention uses for：Microlayer model is in works such as its own gravity, interface adhesion, interfacial tensions Reach equipoise in the surface of solids under firmly.Under electric field action, positive and negative charge gathers at solid-liquid-gas three-phase line of contact Collection, these positive and negative charges are similar to activator so that droplet surface can change, after accumulation reaches certain threshold value, just The electric field force that negative electrical charge generates so that drop breaks through solid-liquid interfacial tension and blocked force, microlayer model three-phase line of contact slide, Microlayer model enters unbalance dynamic state.Solid-liquid interfacial tension, electric field force, blocked force form one not in microlayer model sliding process Stable mechanical balance system, from static state is dynamically converted to, will reach rebalancing within the extremely short time, and drop stops again Movement.With the increase of voltage, such phenomenon periodically occurs, thus three contact lines movements of microlayer model show as it is stick-slip existing As.When improving DC voltage loading speed, charge accumulation rate of the positive and negative charge at three-phase line of contact increases, and makes three to connect The unstability for touching line maintains wider range of range, to make to span the stick-slip process under the low loading speed in many places, reaches Reduce the stick-slip purpose of solid liquid interface.
The present invention includes at least following advantageous effect：
(1) present invention proposes that a kind of method reducing solid liquid interface stick-slip under electric field, this method are straight by increasing The loading speed of galvanic electricity pressure makes microlayer model three-phase line of contact remain at unstable state, to overcome solid liquid interface it is viscous- Sliding phenomenon, by microlayer model three-phase line of contact length under the different DC voltage loading speeds of comparison with the increased pass of electrowetting constant System's figure, can observe that microlayer model is in the stick-slip of solid liquid interface under different voltages loading speed in real time.
(2) method through the invention is finally with silicon substrate super hydrophobic surface drop apparent contact angle and contact line length Ordinate, and map by abscissa of electrowetting constant.From Fig. 3 and Fig. 4, it is apparent that when DC voltage loading speed increases Added-time, silicon substrate super hydrophobic surface solid liquid interface stick-slip significantly reduce, and the method can effectively reduce solid liquid interface Stick-slip provides better control accuracy for the product based on electrowetting on dielectric such as chip lab, electrowetting lens, Avoid the hysteresis effect of such product.
Part is illustrated to embody by further advantage, target and the feature of the present invention by following, and part will also be by this The research and practice of invention and be understood by the person skilled in the art.
Description of the drawings：
Fig. 1 is the experimental principle figure of present example one.
Fig. 2 is the experiment schematic diagram of present example one.
Fig. 3 obtains silicon substrate super hydrophobic surface drop apparent contact angle with electrowetting number variation relation by present example one Figure.
Fig. 4 obtains silicon substrate super hydrophobic surface drop contact line length with electrowetting number variation relation by present example one Figure.
Specific implementation mode：
Present invention will be described in further detail below with reference to the accompanying drawings, to enable those skilled in the art with reference to specification text Word can be implemented according to this.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more The presence or addition of a other elements or combinations thereof.
Embodiment 1：
The method of solid liquid interface stick-slip, includes the following steps under a kind of reduction electric field：
Step 1: the surfaces diameter 150mm are coated with 300nm SiO2Silicon chip be divided into 15mm*15mm samples, then use The sample back side after the polishing segmentation of 800 mesh sand paper, until measuring its resistance value R with digital multimeter<20 Ω will then test sample Product are placed in supersonic wave cleaning machine, are cleaned repeatedly with alcohol and deionized water, until sample surfaces water droplet can not adhere to, finally will Laboratory sample is placed in thermal insulation cabinet；The silicon chip sample cleaned up is placed in desk-top sol evenning machine, using spin-coating method in sample front Spin coating Teflon AF1600 lotions；Spin coating parameters are as follows：Low speed 500r/min, time 20s；High speed 3000r/min, time 30s；The silicon chip of spin coating is placed in vacuum drying chamber, using 200 DEG C of baking 3h, natural cooling is obtained with sandwich structure The super-hydrophobic laboratory sample of silicon substrate；
Step 2: the back side of laboratory sample is adhered to fine copper copper coin surface with silver paste, make laboratory sample and fine copper copper coin It forms access and there is good electric conductivity；Fine copper copper coin is placed in contact angle measurement platform, and by fine copper copper coin with can compile Journey DC power anode connects, and the microlayer model of volume 10uL is added dropwise to the super-hydrophobic laboratory sample surface of silicon substrate；By diameter 100um's Thin copper wire electrode is inserted into inside microlayer model, and thin copper wire is connected with programmable DC power cathode；Programmable DC electricity is set Source voltage range is 0V-120V, voltage-drop loading rate 1V/s；Start contact angle measurement, select dynamic contact angular measurement function, The video to change by drop pattern increases with voltage is recorded by contact angle measurement；
Step 3: repeating step 2, new microlayer model is added dropwise to the super-hydrophobic laboratory sample surface of silicon substrate, changes DC power supply Voltage-drop loading rate obtains under different voltages loading speed drop pattern with voltage change video such as 30V/s, 50V/s；
Step 4: microlayer model volume is with voltage change video under the different voltages loading speed that contact angle measurement is recorded It exports frame by frame；Then drop apparent contact angle and contact line length are respectively obtained using contact angle measurement and image processing software The relational graph changed with electrowetting constant；Electrowetting constant η is calculated using following formula：
Wherein, ε in formula0For permittivity of vacuum, εdFor dielectric layer constant, d is that (i.e. silicon substrate is super for medium thickness Hydrophobic medium thickness), γLVFor Surface Tension of Liquid Drops used, U is voltage；Wherein, ε in the embodiment0=8.85 × 10-12, εd=2.5, d=2 × 10^ (- 6) m, γLV=0.072N/m；The voltage of selection and obtained electrowetting constant η are as shown in table 1：d It is measured using nano-hardness tester；
Step 5: by microlayer model apparent contact angle under the different DC voltage loading speeds of comparison and contact line length with electricity The variation diagram (as shown in table 2 and table 3) of constant is soaked, the change of solid liquid interface stick-slip under different voltages loading speed is quantified Change trend, to obtain the optimum voltage loading speed parameter for reducing solid liquid interface stick-slip；With silicon substrate super hydrophobic surface liquid It is ordinate to drip apparent contact angle and contact line length, and is mapped by abscissa of electrowetting constant；As shown in Figure 3 and Figure 4, may be used With, it is evident that when DC voltage loading speed increases, significantly drop occurs for silicon substrate super hydrophobic surface solid liquid interface stick-slip It is low.The method can effectively reduce solid liquid interface stick-slip, be powered on based on medium for chip lab, electrowetting lens etc. The product of wetting provides better control accuracy, avoids the hysteresis effect of such product.
Table 1
Table 2
Table 3
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited In specific details and legend shown and described herein.

Claims (5)

1. a kind of method reducing solid liquid interface stick-slip under electric field, which is characterized in that include the following steps：
Step 1: using conductive material as substrate, it is no more than 2 μm of insulating layer in conductive material surface coating thickness, to insulating layer Surface carries out hydrophobic treatment or coating hydrophobic coating, forms the laboratory sample with sandwich structure；
Step 2: laboratory sample is adhered to fine copper copper coin surface with silver paste, fine copper copper coin is placed in contact angle measurement platform, And connect fine copper copper coin with programmable DC positive pole, the microlayer model of arbitrary volume is added dropwise to sample surfaces；Diameter is remote Thin copper wire electrode less than microlayer model volume is inserted into inside microlayer model, and thin copper wire is connected with programmable DC power cathode； Programmable DC supply voltage range and voltage-drop loading rate are set；Start contact angle measurement, selects dynamic contact angular measurement Function records the video to change by drop pattern increases with voltage by contact angle measurement；
Step 3: repeating step 2, new microlayer model is added dropwise to the super-hydrophobic laboratory sample surface of silicon substrate, changes direct current power source voltage Loading speed, obtain different voltages loading speed under drop pattern with voltage change video；
Step 4: frame by frame with voltage change video by microlayer model volume under the different voltages loading speed of contact angle measurement recording Export；Then drop apparent contact angle and contact line length are respectively obtained with electricity using contact angle measurement and image processing software Soak the relational graph of constant variation；
Step 5: by microlayer model apparent contact angle under the different DC voltage loading speeds of comparison and contact line length with electrowetting The variation diagram of constant quantifies the variation tendency of solid liquid interface stick-slip under different voltages loading speed, is reduced admittedly to obtain The optimum voltage loading speed parameter of liquid interface stick-slip.
2. the method for reducing solid liquid interface stick-slip under electric field as described in claim 1, which is characterized in that the step One process is：The SiO of 100~500nm is plated in substrate silicon chip surface2Insulating layer, then with the 800 mesh sand paper polishing sample back of the body Face, until measuring its resistance value R with digital multimeter<Sample, is then placed in supersonic wave cleaning machine by 20 Ω, with alcohol and goes Ionized water cleans repeatedly, until sample surfaces water droplet can not adhere to, finally laboratory sample is placed in thermal insulation cabinet；It will clean up Silicon chip sample be placed in desk-top sol evenning machine, using spin-coating method spin coating Teflon AF1600 lotions, obtain that there is sandwich structure The super-hydrophobic laboratory sample of silicon substrate.
3. the method for reducing solid liquid interface stick-slip under electric field as claimed in claim 2, which is characterized in that the spin coating The parameter of method is：Low speed 500r/min, time 20s；High speed 3000r/min, time 30s；The silicon chip of spin coating is placed in vacuum to do In dry case, using 200 DEG C of baking 3h, natural cooling obtains the super-hydrophobic laboratory sample of silicon substrate.
4. the method for reducing solid liquid interface stick-slip under electric field as described in claim 1, which is characterized in that the thin copper A diameter of 50~200um of silk electrode.
5. the method for reducing solid liquid interface stick-slip under electric field as described in claim 1, which is characterized in that described to compile Journey direct current power source voltage range is set as 0V-120V, and voltage-drop loading rate is 1~50V/s.
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