Trickle flow control valve of double-liquid capillary in the micro-fluidic chip and preparation method thereofTechnical field
The present invention relates to be used for realize on the micro-fluidic chip two kinds of liquid capillary microfluidic control valve of sample introduction simultaneously, particularly a kind of being applicable to realized two kinds of control gears with micro liquid synchro-feed of different close dielectric properties in the biological detection.
Background technology
Micro-fluidic chip is the hot fields of current micro-total analysis system (Miniaturized Total Analysis Systems) development.Micro-fluidic chip will be used to accomplish sample preparation, transport, quantitatively, the microstructure of processes such as mixing and detection is integrated on the chip, constitutes the main platform that microflow control technique is realized.On chip, the married operation of liquid needs two kinds of liquid to get into micro-mixer simultaneously, and this function is accomplished by Y type sample introduction microchannel.Usually in the Y type sample introduction microchannel two kinds of liquid intersection's capillary flow of two sample introduction branches by realizing that by little valve of hydrophobic region or expansive valve the mode through the liquid triggering realizes the unlatching of the little valve of intersection then, thereby sample introduction when realizing two kinds of liquid.Local deposits C in the microchannel4F8, or making OTS hydrophobic region can form drain valve; The capillary expansive valve mainly is the function of ending that realizes capillary flow through the sudden change of the degree of depth in the microchannel or Width size.The making of drain valve need be carried out topical surface treatment, can increase process complexity and difficulty of processing, and processing compatibility is poor; Expansive valve mainly is to rely on ending that the expansion of size realizes flowing, and high lyophile is prone to lose efficacy.Therefore, common Y type sample introduction microchannel exists processing technology complicated, and processing compatibility is poor, is difficult to realize high lyophile sample introduction and the shortcoming that has liquid residue simultaneously.
Summary of the invention
The objective of the invention is to realize two kinds of micro liquids with different close dielectric properties technical barriers of sample introduction simultaneously, propose trickle flow control valve of double-liquid capillary in a kind of micro-fluidic chip and preparation method thereof for solving being difficult to of existing in the present microflow control technique.
The trickle flow control valve of double-liquid capillary in the micro-fluidic chip of the present invention; Be that dimethyl silicone polymer (PDMS) substrate that the surface is provided with groove posts the Y type capillary channel that on glass sheet surface, constitutes, the groove on the said PDMS substrate surface comprises the first tributary groove, the second tributary groove, output groove and air flue groove; The cross-sectional width of the said first tributary groove, the second tributary groove and output groove equates; The cross-sectional width of said air flue groove is less than the cross-sectional width of the first tributary groove, the second tributary groove and output groove; The deep equality of said second tributary groove and output groove, the degree of depth of the first tributary groove is less than the degree of depth of the second tributary groove; The degree of depth of the second tributary groove and output groove is less than the degree of depth of air flue groove; The end of the said first tributary groove and the second tributary groove converges in the input end of output groove; Before the end of air flue groove converges in the end of the second tributary groove; The entrance point of said air flue groove apart from the length of output groove input end greater than the first tributary groove entrance point and the second tributary groove entrance point apart from the length of exporting the groove input end; Described capillary microfluidic control valve provides the rotation center of centrifugal force to be positioned at entrance point one side of two the tributary fluid passages and the gas passage of the trickle flow control valve of double-liquid capillary; Rotation center provides centrifugal force to make to be plugged in the first tributary fluid passage and the terminal gas of the second tributary fluid passage to discharge to the motion of rotation center direction and by the import of gas passage; Liquid in the second tributary fluid passage and the liquid in the first tributary fluid passage converge at the expansive valve place; And then two flow of liquid are flowed out simultaneously along the output liquid passage; Capillary microfluidic control valve has the rotation center that centrifugal force is provided; Rotation center is positioned at entrance point one side of the first tributary fluid passage that the first tributary groove of the trickle flow control valve of double-liquid capillary constitutes, the second tributary fluid passage that the second tributary groove constitutes and the second tributary fluid passage and the gas passage of air flue groove formation; The import discharge of the gas passage that the terminal gas of the second tributary fluid passage that rotation center provides centrifugal force to make to be plugged in the first tributary fluid passage that the first tributary groove constitutes and the second tributary groove to constitute constitutes to the motion of rotation center direction and by the second tributary fluid passage and air flue groove; Liquid in the first tributary fluid passage that the liquid in the second tributary fluid passage that the second tributary groove constitutes and the first tributary groove constitute converges at the expansive valve place, and then two flow of liquid are flowed out along the output liquid passage simultaneously.
The method for making of the trickle flow control valve of double-liquid capillary in the micro-fluidic chip, the concrete steps of this method are:
Step 1, on the surface of the silicon single crystal flake after the oxidation spin coating photoresist; Make the photoresist figure of the said first tributary groove, the second tributary groove, output groove and air flue groove by lithography; With wet etching silicon dioxide behind the said photoresist figure post bake; Then the photoresist of the first tributary groove, the second tributary groove, output groove and air flue groove remainder is removed, obtained the silicon dioxide mask figure of the first tributary groove, the second tributary groove, output groove and air flue recess channels;
Step 2, on the silicon dioxide mask figure thatstep 1 obtains the thick aluminium film ofvapor deposition 1 μ m; Spin coating photoresist on said aluminium film then; Make the photoresist figure of the described second tributary groove, output groove and air flue groove by lithography, wet etching aluminium behind the post bake obtains the aluminium mask graph; Then the photoresist of the remainder of the said second tributary groove, output groove and air flue groove is removed, obtained the aluminium mask graph of the second tributary groove, output groove and air flue groove;
Step 3, on the silicon wafer of the aluminium mask graph thatstep 2 obtains the spin coating photoresist, make the photoresist figure of air flue groove by lithography, remove photoresist behind the post bake, obtain the glue mask graph;
The silicon wafer of the glue mask graph that step 4, the aluminium mask graph thatstep 2 is obtained and step 3 obtain carries out the inductively coupled plasma dry etching, obtains silica-based former mould; The process of said inductively coupled plasma dry etching is:
Steps A, etching 10 μ m at first remove the mask that removes photoresist then, obtain to contain the silicon wafer of aluminium and silicon dioxide mask figure;
Step B, on the basis of steps A, continue etching 170 μ m, remove the aluminium mask then, continue etching 30 μ m, obtain silica-based former mould;
Step 5, adopt little die casting process, liquid dimethyl silicone polymer is cast on the silica-based former mould, carry out the demoulding after vacuum outgas, heating, the cooling then; Obtain the dimethyl silicone polymer male mold;
Step 6, on the described dimethyl silicone polymer male mold of step 5 the pouring liquid dimethyl silicone polymer, carry out the demoulding after vacuum outgas, heating, the cooling then; Obtain the dimethyl silicone polymer substrate;
Punching respectively in the end of step 7, the on-chip first tributary groove of dimethyl silicone polymer, the second tributary groove and air flue groove that step 6 is obtained, is respectively the entrance point in first tributary, the entrance point of the second tributary groove and the entrance point of air flue groove;
Dimethyl silicone polymer substrate after step 8, the punching that step 7 is obtained is fitted with glass sheet, obtains the interior trickle flow control valve of double-liquid capillary of micro-fluidic chip.
The principle of work of the trickle flow control valve of double-liquid capillary of the present invention is:
The second tributary fluid passage that first tributary fluid passage that the first less tributary groove of the degree of depth is constituted and the second bigger tributary groove of the degree of depth are constituted forms two expansive valves respectively with the intersection of the output output liquid passage that groove constituted, and the intersection of the gas passage that the second tributary fluid passage and air flue groove are constituted also has expansive valve to form.After a kind of liquid was added by the import of the first tributary fluid passage, when liquid arrived the expansive valve place with output liquid passage intersection under capillary action, capillary flow was ended.Inflow point by the second tributary fluid passage adds another kind of liquid then; This liquid also flows to its this channel end under capillary action; Owing to be compressed at the first tributary fluid passage and the terminal gas of the second tributary fluid passage by shutoff; Make air pressure and capillary equilibrium, and make the liquid of the second tributary fluid passage end in the intersection of gas passage and this second tributary fluid passage.Centrifugal force is provided then; Rotation center is positioned at above-mentioned two the tributary fluid passages of the trickle flow control valve of this double-liquid capillary and entrance point one side of gas passage; Under centrifugal action; Be plugged in the terminal gas of the first tributary fluid passage and the second tributary fluid passage because of discharging by the import of gas passage to the motion of rotation center direction; Liquid in the second tributary fluid passage arrives the intersection of two tributary fluid passages, converges at the expansive valve place with liquid in the first tributary fluid passage, and then two flow of liquid are flowed out along the output liquid passage simultaneously.The trickle flow control valve of this double-liquid capillary is simple in structure; Can realize of the blocking-up of the capillary flow of two kinds of liquid (wherein a kind of can be high lyophile) simultaneously in intersection; And then sample introduction when realizing under centrifugal force two kinds of liquid, and Y type microchannel intersection no liquid is remaining; In addition, select cheap materials such as polymkeric substance for use, manufacture craft is greatly simplified, cost reduces.
Beneficial effect of the present invention: the trickle flow control valve of double-liquid capillary in the micro-fluidic chip of the present invention, can realize of the blocking-up of high lyophile in Y type microchannel intersection; Gas is prone to discharge smoothly in centrifugal force field, has improved the reliability that high lyophile capillary flow is ended in intersection, thereby has effectively guaranteed the simultaneity of two kinds of liquid sample introductions; And the remnants of liquid have been avoided in Y type microchannel intersection; Its structured material is cheap, and technology is simple, can effectively shorten the fabrication cycle and reduction cost of manufacture of device.
Description of drawings
Fig. 1 is the schematic perspective view of the trickle flow control valve of double-liquid capillary in the micro-fluidic chip of the present invention;
Fig. 2 is the schematic perspective view of the substrate of PDMS shown in Fig. 1;
Fig. 3 is the A-A diagrammatic cross-section of the substrate of PDMS shown in Fig. 2.
Among the figure: 1, PDMS substrate, 1-1, the first tributary groove, 1-1-1, the first tributary groove entrance point; 1-2, the second tributary groove, 1-2-1, the second tributary groove entrance point, 1-3, output groove; 1-4, air flue groove, 1-4-1, air flue groove entrance point, 2, glass sheet.
Embodiment
Embodiment one, combination Fig. 1 to Fig. 3 explain this embodiment; The trickle flow control valve of double-liquid capillary in the micro-fluidic chip; Be that thePDMS substrate 1 that the surface is provided with groove posts the Y type capillary channel that onglass sheet 2 surfaces, constitutes, saidPDMS substrate 1 lip-deep groove comprises the first tributary groove 1-1, the second tributary groove 1-2, output groove 1-3 and air flue groove 1-4; The cross-sectional width of the said first tributary groove 1-1, the second tributary groove 1-2 and output groove 1-3 equates; The cross-sectional width of said air flue groove 1-4 is less than the cross-sectional width of the first tributary groove 1-1, the second tributary groove 1-2 and output groove 1-3; The deep equality of said second tributary groove 1-2 and output groove 1-3, the degree of depth of the first tributary groove 1-1 is less than the degree of depth of the second tributary groove 1-2; The degree of depth of the second tributary groove 1-2 and output groove 1-3 is less than the degree of depth of air flue groove 1-4; The end of the said first tributary groove 1-1 and the second tributary groove 1-2 converges in the input end of output groove 1-3; Before the end of air flue groove 1-4 converges in the end of the second tributary groove 1-2, the entrance point 1-4-1 of said air flue groove 1-4 apart from the length of output groove 1-3 input end greater than the first tributary groove 1-1 entrance point 1-1-1 and the second tributary groove 1-2 entrance point 1-2-1 apart from the length of exporting groove 1-3 input end.
Before the end of the said air flue groove of this embodiment 1-4 converges in the end of the second tributary groove 1-2, be meant before the described end: the end of the first tributary groove 1-1 and the second tributary groove 1-2 converges in the input end position arbitrarily before of output groove 1-3.
The degree of depth of the described first tributary groove 1-1 of this embodiment, output groove 1-3 and the second tributary groove 1-2 is respectively 30 μ m, 200 μ m and 200 μ m, and its width is 600 μ m; The degree of depth of said air flue groove 1-4 is that 240 μ m, width are 100 μ m.
Embodiment two, this embodiment are the method for making of the trickle flow control valve of double-liquid capillary in the embodiment one described micro-fluidic chip, and the concrete steps of this method are:
Step 1, on the surface of the Si single-chip after the oxidation spin coating photoresist; Make the photoresist figure of the said first tributary groove 1-1, the second tributary groove 1-2, output groove 1-3 and air flue groove 1-4 by lithography, then with wet etching SiO behind the said photoresist figure post bake2, then the photoresist of the first tributary groove 1-1, the second tributary groove 1-2, output groove 1-3 and air flue groove 1-4 remainder is removed, obtain the SiO of the first tributary groove 1-1, the second tributary groove 1-2, output groove 1-3 and air flue groove 1-4 passage2Mask graph;
Step 2, the SiO that obtains instep 12The thick aluminium film ofvapor deposition 1 μ m on the mask graph; Spin coating photoresist on said aluminium film then; Make the photoresist figure of the described second tributary groove 1-2, output groove 1-3 and air flue groove 1-4 by lithography, wet etching aluminium behind the post bake obtains the aluminium mask graph; Then the photoresist of the remainder of the said second tributary groove 1-2, output groove 1-3 and air flue groove 1-4 is removed, obtained the aluminium mask graph of the second tributary groove 1-2, output groove 1-3 and air flue groove 1-4;
Step 3, on the Si wafer of the aluminium mask graph thatstep 2 obtains the spin coating photoresist, make the photoresist figure of air flue groove 1-4 by lithography, remove photoresist behind the post bake, obtain the glue mask graph;
The Si wafer of the glue mask graph that step 4, the aluminium mask graph thatstep 2 is obtained and step 3 obtain carries out the ICP dry etching, obtains Si base former mould; The process of said ICP dry etching is:
Steps A, etching 10 μ m at first remove the mask that removes photoresist then, obtain to contain the Si wafer of aluminium mask graph;
Step B, on the basis of steps A, continue etching 170 μ m, remove the aluminium mask then, continue etching 30 μ m, obtain Si base former mould;
Step 5, adopt little die casting method, liquid PDMS is cast on the Si base former mould, carry out the demoulding after vacuum outgas, heating, the cooling then; Obtain the PDMS male mold;
Step 6, on the described PDMS male mold of step 5 pouring liquid PDMS, carry out the demoulding after vacuum outgas, heating, the cooling then; ObtainPDMS substrate 1;
Punching respectively in the end of the first tributary groove 1-1, the second tributary groove 1-2 and air flue groove 1-4 on step 7, thePDMS substrate 1 that step 6 is obtained, is respectively the entrance point 1-1-1 of the first tributary 1-1, the entrance point 1-2-1 of the second tributary groove 1-2 and the entrance point 1-4-1 of air flue groove 1-4;
PDMS substrate 1 after step 8, the punching that step 7 is obtained is fitted withglass sheet 2, obtains the trickle flow control valve of double-liquid capillary in the micro-fluidic chip.
The thickness of the described Si single-chip ofstep 1 can be 380 μ m, 600 μ m or 800 μ m in this embodiment.
Step 5 and step 6 are described in this embodiment carries out vacuum outgas, heating, cooling and the demoulding; Obtain the PDMS male mold; Described heating-up temperature is 120 ℃, and the time of being heating and curing is 15 minutes.
The complementary structure of the Si base former mould that the structure of the PDMS male mold that step 5 obtains in this embodiment and step 4 obtain; Described liquid PDMS and hardening agent form by 10: 1 mixed.
The structure of thePDMS substrate 1 that step 6 obtains in this embodiment is identical with the structure of the Si base former mould that step 4 obtains.
The material of the described glass sheet of this embodiment (2) is the Pyrex sheet, the size of said Pyrex sheet and SiO2Single-chip measure-alike; Thickness is 1mm.