CN100494978C - Method for making micro-fluidic chip with Z-shape spectrophotometric detection cell - Google Patents
Method for making micro-fluidic chip with Z-shape spectrophotometric detection cell Download PDFInfo
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- CN100494978C CN100494978C CNB2006100122324A CN200610012232A CN100494978C CN 100494978 C CN100494978 C CN 100494978C CN B2006100122324 A CNB2006100122324 A CN B2006100122324A CN 200610012232 A CN200610012232 A CN 200610012232A CN 100494978 C CN100494978 C CN 100494978C
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Abstract
The related preparation method for micro flow control chip with Z-shape luminosity detector comprises: 1) drawing figure for top and lower layers by a graphic software for output; 2) light etching to prepare two male moulds for alkylation; 3) adding a U-shape washer between former moulds to form a U-shape liquid slot; 4) pouring dimethyl silicone polymer and initiator processed in vacuum, heating for curing; 5) unfolding moulds to obtain the PDMS film; 6) preparing top and lower covers; 7) sticking cover to the PDMS film, irradiating with light source, and obtaining the final product. This invention is simple and low cost, and fit to wide application.
Description
Technical field
The present invention relates to a kind of method for making of chip, particularly about a kind of method for making of the micro-fluidic chip with Z type photometric detection flow cell.
Background technology
Microfluidic system is a kind of analytical technology that last century, the nineties began to develop, it utilizes micro fabrication to make functional units formation micro-systems such as microchannel, microreactor and little detecting device on chip, the operating process that be used for finishing traditional chemical and biology etc. analyses, detects has characteristics such as portable, high flux, flexible function, low sample and low reagent consumption.
Absorbance detection is a kind of important detection mode, in liquid phase systems, capillary electrophoresis system, have a wide range of applications, but the research of directly carrying out at present absorbance detection on micro-fluidic chip seldom, main cause is: (1) micro-fluidic chip channel diameter is very little, effectively light path generally has only tens of microns, much smaller than the requirement of absorbance detection; (2) generally more than 2mm, the background absorption of introducing is relatively very big for the outer wall thickness of micro-fluidic chip passage, and can increase light path and disperse area; (3) optical window that uses maximum photoetching processes to make at present is the planoconcave mirror, is on-plane surface, and its surface is comparatively coarse, easily causes light path refraction and scattering.Above reason causes present micro-fluidic chip capillary channel to be not suitable for directly carrying out photometric detection as absorption cell.
Z type absorbance detection pond is a kind of structure that increases light path under small flow cell volume, improve detection sensitivity that grows up in little liquid phase systems, at present a lot of commercial apparatuss all adopt this flow detection pool structure, some instruments can be accomplished the 5mm light path under the flow cell volume that rise tens of receiving, this technology is applied to the integrated photometric detection of micro-fluidic chip, can solves micro-fluidic chip can't carry out photometric detection at present because light path is short problem better.Yet Z type photometric detection flow cell is integrated into the certain degree of difficulty that is manufactured with on the micro-fluidic chip: (1) makes the passage of broken line type on micro-fluidic chip, detect in the direction parallel with chip, be not easy to realize, because the microchannel sidewall that present low cost method is made mostly is arc, and light path need introduce parts such as light transmitting fiber, and it is also bad to be difficult for processing and measuring repeatability; (2) use the regular absorption cell of fabrication techniques shape such as the deep erosion of ion, its cost is too high; And the method that passage is etched on the cover plate up and down is not suitable for making Z type flow cell, because the optical window on the two sides made from common lithographic method is difficult for making the plane; (3) adopt the method for external detection cell to carry out the micro-fluidic chip photometric detection, can cause signal broadening because of increasing dead volume, simultaneously also can be because of system complex cause cost too high, solution that neither be desirable.
Summary of the invention
At the problems referred to above, it is low to the purpose of this invention is to provide a kind of cost, and optical window is bright and clean, the method for making of the micro-fluidic chip in band Z type photometric detection pond easy to process.
For achieving the above object, the present invention takes following technical scheme: a kind of method for making of the micro-fluidic chip with Z type photometric detection pond, it may further comprise the steps: 1) utilize mapping software to draw the figure and the output of upper and lower two-layer passage in the chip, described upper strata figure comprises upper strata passage, liquid storage tank groove, liquid storage tank through hole and Z type pond through hole, lower floor's figure comprise lower floor's passage, liquid storage tank through hole and Z type pond through hole; 2) adopt conventional photoetching method to make two formpistons, the one side of two described formpistons is carved with the figure of projection respectively, adopts conventional method that male mold surfaces is carried out alkylation then and handles; 3) protruding figure of two described formpistons is aimed at, and in the middle of two described anode membranes, be encased inside a U-shaped packing ring, vertically add press fit with described two formpistons of clamp then, form a U-shaped liquid bath; 4) with described U-shaped liquid bath opening upwards, in described U-shaped liquid bath, pour into dimethyl silicone polymer monomer and the initiating agent handled through vacuum outgas, and described U-shaped liquid bath placed vacuum drying oven, under 0.005～0.02MPa vacuum tightness, 50～55 ℃ of heating 3～5h are to full solidification; 5) take out the U-shaped liquid bath then, take the both sides formpiston apart and obtain two-sided concave channel groove and the recessed liquid storage tank through-hole groove of being carved with, end face is carved with the PDMS thin slice of liquid storage tank groove, on described PDMS thin slice, get through Z type pond through hole with punch device and be communicated with the levels passage, get through the described liquid storage tank through hole on the PDMS thin slice; 6) with the conventional method PDMS film that to produce two thickness be 20～200um, wherein a slice does not contain the PDMS film of structure as lower cover slip, another sheet PDMS film is as upper cover plate, with described PDMS thin slice on liquid storage tank groove and the corresponding through hole of offering of liquid storage tank through hole; 7) the PDMS thin slice of step 6) being made is placed between described upper cover plate and the lower cover slip as intermediate, adopt conventional method that upper and lower cover plate and intermediate are fit together, and shine with light source, promptly get the micro-fluidic chip that contains Z type photometric detection pond.
In step 7), after described upper and lower cover plate and intermediate fit together, utilize ultraviolet source, irradiation time is 2～8h.
In implementation step 7) preceding, earlier respectively described upper and lower cover plate and intermediate are carried out ultraviolet source irradiation below the 2h, more described upper and lower cover plate and intermediate are fit together, continue to shine 2～6h.
Before implementation step 7, respectively described upper and lower cover plate and intermediate are carried out fitting behind the plasma radiation again earlier.
In implementation step 4) preceding, earlier dimethyl silicone polymer monomer and initiating agent are placed open-top receptacle, under 0.005～0.02MPa vacuum tightness, 50～55 ℃ were heated 30～60 minutes in vacuum drying oven.
The thickness of described U-shaped packing ring is 100～2000um.
The thickness of described upper and lower cover plate is respectively 20～200um.
The bracing frame of one thin slice as fixed chip is set at least, and punch on described thin slice in corresponding at least described Z type photometric detection pond on one of described upper and lower cover plate.
The present invention is owing to take above technical scheme, and it has the following advantages: 1, because the absorbance detection pond of adopting the inventive method to make on micro-fluidic chip has Z type photometric detection pool structure, so the detection cell volume is little, and light path can be accomplished longer; The size of detection cell is not influenced by the shape and size of passage, can design and produce as required; While is because the method for employing applying translucent sheet is made optical window, so optical window is bright and clean, smooth, thin thickness and parallel to each other; The Z type photometric detection pond that above characteristic is made the present invention has good performance, is suitable for the micro-fluidic chip absorbance detection.2, the micro-fluidic chip that adopts the inventive method to make, the absorbance detection pond of containing the vertical chip plane, can make the detection light path pass through Z type photometric detection pond perpendicular to micro-fluidic chip, therefore light source and detecting device can hang down and be provided with as for the chip plane, make things convenient for the design and fabrication of absorbance detection instrument.3, the present invention is owing to used the method for low temperature polymerization at a slow speed, vacuumizing and exhausting in (polymerization) process in processing, so two-sided PDMS thin slice that has passage that processes, thickness is the thinnest can to reach 100um, has overcome the difficult problem of discharging of bubble that conventional method produces in the PDMS polymerization process in so thin liquid pool.4, the inventive method can be as required, design three-dimensional micro-fluidic chip passage, need not any high-level instrument and equipment can make at any time, and process is simple and easy to do, and cost is low, and speed is fast, particularly adopt the inventive method, both can produce the bilayer or the layer stereo passage of different shape easily and flexibly, can on same PDMS thin slice, produce many double-deck stereo passages again, satisfy high-throughout detection requirement.The inventive method can be widely used in the processing and fabricating of various micro-fluidic chips.
Description of drawings
Fig. 1 is the schematic cross-section of common chip in the chip thickness direction
Fig. 2 is the schematic cross-section of the present invention in the chip thickness direction
Fig. 3 is a upper strata of the present invention glass anode membrane structural representation
Fig. 4 is a lower floor of the present invention glass anode membrane structural representation
Fig. 5 is that the present invention makes schematic flow sheet
Fig. 6 is an integral core chip architecture synoptic diagram of the present invention
Embodiment
Below in conjunction with accompanying drawing the inventive method is elaborated.
As shown in Figure 1, the passage 2 of common chip 1 sees it is level on chip 1 thickness direction; As shown in Figure 2, passage 2 of the present invention sees it is the Z type at chip 1 thickness direction, the method for making in band Z type photometric detection of the present invention pond unlike the prior art, it may further comprise the steps:
1, makes the photoetching film
As shown in Figure 3, Figure 4, distinguish upper and lower two-layer passage figure in the design chips 1 according to need, the upper strata figure comprises a cross passage 3, three liquid storage tank grooves 4, a liquid storage tank through hole 5 and a Z type pond through hole 6, lower floor's figure comprises a straight channel 7, a liquid storage tank through hole 5 and a Z type pond through hole 6, the figure of two-layer up and down passage 3,7 overlaps at through hole 6 places, two Z type ponds, and two liquid storage tank through holes 5 also overlap.Utilize mapping software (as CorelDraw etc.) to draw out upper and lower two layer patterns respectively, and output (as printing) with laser photocomposing machine to two films as photoetching with version;
2, photoetching molding
Utilize above-mentioned hectograph, adopt conventional photoetching method to make two sheet glass or quartz or silicon materials formpiston 8,9 respectively, one side in each sheet formpiston 8,9 is carved with the passage 3,7 of projection respectively, and the projection of liquid storage tank groove 4, liquid storage tank through hole 5 and Z type pond through hole 6, and adopt routine techniques that alkylation is carried out on formpiston 8,9 surfaces and handle, as smearing male mold surfaces with isooctane;
3, assembling casting pool
As shown in Figure 5,8,9 lobed of two formpistons are relative, the figure of projection is aimed at according to pre-designed channel position, guarantees that the Z type pond through hole 6 of upper and lower two- layer passage 3,7 and liquid storage tank through hole 5 positions overlap, so that the casting back forms corresponding double-deck passage.In the middle of two glass sheet anode membranes 8,9, be encased inside a U-shaped packing ring 10, then with vertically adding press fit behind two formpistons 8,9 of anchor clamps 11 clampings.Because 10 on U-shaped packing ring has sealed 8,9 three limits of two formpistons, the 4th limit vacated, so after clamping two formpistons 8,9, form a U-shaped liquid bath in the U-shaped packing ring 10 that is encased inside in the middle of it, the thickness of U-shaped packing ring 10 is identical with the required optical path length in Z type photometric detection pond; The material of U-shaped packing ring 10 is that plastics, nylon, rubber or metal etc. all can.
4, casting
U-shaped liquid bath opening is upwards placed, carefully poured into dimethyl silicone polymer (PDMS) monomer and the initiating agent (normal starter) handled through vacuum outgas in the U-shaped liquid bath, careful operation tries not to bring into bubble.This U-shaped liquid bath is placed vacuum drying oven, and under 0.005～0.02MPa vacuum tightness, 50～55 ℃ of heating 3～5h are to full solidification, and heating-up temperature high curing rate more is fast more, but curing rate is unfavorable for the discharge of minute bubbles when too fast.
Said method also can place an open-top receptacle with dimethyl silicone polymer monomer and initiating agent earlier, in vacuum drying oven under 0.005～0.02MPa vacuum tightness, 50～55 ℃ were heated 30～60 minutes, carry out above-mentioned casting curing operation again, can guarantee the gas discharge better, be unlikely to excessive influence perfusion as long as guarantee the viscosity of mixing material.
5, form removal (dismounting casting pool)
Take out the U-shaped liquid bath, take both sides formpiston 8,9 apart and obtain two-sidedly being carved with concave channel groove and recessed liquid storage tank through-hole groove, and end face is carved with the PDMS thin slice 12 of three liquid storage tank grooves 4.On PDMS thin slice 12, get through Z type pond through hole 6 with excimer laser or other punch devices at last and form Z type photometric detection of the present invention pond, and connection levels passage 3,7, form a Z type passage 2 of the present invention (as Fig. 2, shown in Figure 6) that is communicated with, get through the liquid storage tank through hole 5 on the PDMS thin slice 12.
6, make cover plate up and down
With the conventional method PDMS film that to produce two thickness be 100～200um, wherein a slice do not contain structure the PDMS film as lower cover slip 13, another sheet PDMS film is as upper cover plate 14.On the upper cover plate 14 with PDMS thin slice 12 on liquid storage tank groove 4 corresponding positions three through holes 15 are set, so that with each through hole 15 and each liquid storage tank groove 4 common passage 2 import liquid storage tank of forming, simultaneously with PDMS thin slice 12 on liquid storage tank through hole 5 corresponding positions a through hole 16 is set so that with through hole 16 and the liquid storage tank through hole 5 common passages 2 outlet liquid storage tanks of forming.Above-mentioned upper cover plate 14 and lower cover slip 13 can also be made of glass or quartzy thin slice, and piezoid intensity can do thinlyyer greatly, and its thickness is 20～200um, and does not have uv absorption, better effects if.
7, assembling
The two-sided PDMS thin slice 12 that is carved with the concave channel groove that step 5 is made is placed between upper cover plate 14 and the lower cover slip 13 as intermediate, each structure of upper cover plate 14 is aimed at intermediate (being PDMS thin slice 12) corresponding structure, adopt conventional method that upper cover plate 14, lower cover slip 13 and intermediate are fit together, UV-irradiation 2～the 8h that utilizes common 10～40W ultraviolet lamp tube to produce then, finish applying, promptly get the stereo channel micro-fluidic chip that contains Z type photometric detection flow cell.
Above-mentioned steps 7 also can be used in ultraviolet light pre-irradiation upper cover plate 14, lower cover slip 13 and the intermediate 2h earlier, and then it is fit together, and continues irradiation 2～6h.The mode that above-mentioned steps 7 also can be taked to fit with the plasma radiation surface is earlier again finished, and it can obtain better effect.Above-mentioned general ultraviolet fluorescent tube also can change xenon lamp into or other can produce the light source of ultraviolet light.
From above steps as can be seen, the optical length and the volume in the Z type photometric detection pond in the chip 1 of the present invention all can be controlled as required.Utilize the thickness of U-shaped pad 10, control the thickness of intermediate (PDMS thin slice 12), just can control the optical length in Z type photometric detection pond, this optical length is generally at 100～2000um; The volume in Z type photometric detection pond can be by optical length and diameter control, and the diameter in Z type photometric detection pond is generally at 30～300um.
Convenient for using, can cut and the glass of chip 1 size coupling or the thin slice of organic glass or plastic or other material, the position of the Z type pond through hole 6 of the through hole 15,16 of corresponding upper cover plate 14 and intermediate punching on thin slice, and this thin slice is attached to upper cover plate 14 tops, as the bracing frame of fixed chip 1.Can also on a thin slice, punch the position of corresponding Z type pond through hole 6, and thin slice is fixed on lower cover slip 13 bottoms.More can on upper and lower cover plate 14,13, above-mentioned thin slice be set respectively.
The present invention can have a plurality of Z type passages 2 on a chip 1, promptly design and make the upper and lower double-deck passage of a plurality of composition Z types on a chip 1 simultaneously, is used for high throughput analysis and uses.Adopt the present invention can also make the layer stereo passage in addition, this layer stereo passage can be made up of multilayer PDMS thin slice, is communicated with by a plurality of Z type pond through holes and liquid storage tank.The figure of the double-deck passage of the present invention simultaneously can be that cross is linear, linear, shaped form various channel shapes such as (upper strata passages as shown in Figure 5).These variations belong to that those skilled in the art are easy to according to the present invention expect, these conversion should not got rid of outside protection scope of the present invention.Two formpistons 8,9 of the present invention in addition also can adopt other method to make, and the change of two formpistons, 8,9 method for makings should be regarded the replacement that is equal to of the present invention as, should not get rid of outside protection scope of the present invention.
When the present invention detects, light source and detecting device are separately positioned on the two ends in the Z type photometric detection pond of chip 1, the light that light source is sent passes through Z type photometric detection pond (as shown in Figure 2), when flow of liquid is crossed detection cell, just can carry out absorbance detection by detecting device.
Claims (10)
1, a kind of method for making of the micro-fluidic chip with Z type photometric detection pond, it may further comprise the steps:
1) utilize mapping software to draw the figure and the output of upper and lower two-layer passage in the chip, described upper strata figure comprises upper strata passage, liquid storage tank groove, and liquid storage tank through hole and Z type pond through hole, lower floor's figure comprise lower floor's passage, liquid storage tank through hole and Z type pond through hole;
2) adopt conventional photoetching method to make two formpistons, the one side of two described formpistons is carved with the figure of projection respectively, adopts conventional method that male mold surfaces is carried out alkylation then and handles;
3) protruding figure of two described formpistons is aimed at, and in the middle of two described anode membranes, be encased inside a U-shaped packing ring, vertically add press fit with described two formpistons of clamp then, form a U-shaped liquid bath;
4) with described U-shaped liquid bath opening upwards, in described U-shaped liquid bath, pour into dimethyl silicone polymer monomer and the initiating agent handled through vacuum outgas, and described U-shaped liquid bath placed vacuum drying oven, under 0.005～0.02MPa vacuum tightness, 50～55 ℃ of heating 3～5h are to full solidification;
5) take out the U-shaped liquid bath then, take the both sides formpiston apart and obtain two-sided concave channel groove and the recessed liquid storage tank through-hole groove of being carved with, end face is carved with the dimethyl silicone polymer thin slice of liquid storage tank groove, on described dimethyl silicone polymer thin slice, get through Z type pond through hole with punch device and be communicated with the levels passage, get through the described liquid storage tank through hole on the dimethyl silicone polymer thin slice;
6) with the conventional method dimethyl silicone polymer film that to produce two thickness be 20～200um, wherein a slice does not contain the dimethyl silicone polymer film of structure as lower cover slip, another sheet dimethyl silicone polymer film is as upper cover plate, corresponding on the described upper cover plate three through holes are set with the liquid storage tank groove on the described dimethyl silicone polymer thin slice, and with the corresponding through hole of offering of the liquid storage tank through hole on the described dimethyl silicone polymer thin slice;
7) the dimethyl silicone polymer thin slice of step 6) being made is placed between described upper cover plate and the lower cover slip as intermediate, employing fits together upper and lower cover plate and intermediate, and shine with ultraviolet source, promptly get the micro-fluidic chip that contains Z type photometric detection pond.
2, the method for making of a kind of micro-fluidic chip with Z type photometric detection pond as claimed in claim 1 is characterized in that: in step 7), after described upper and lower cover plate and intermediate fit together, utilize ultraviolet source, irradiation time is 2～8h.
3, the method for making of a kind of micro-fluidic chip with Z type photometric detection pond as claimed in claim 1, it is characterized in that: in implementation step 7) preceding, earlier respectively described upper and lower cover plate and intermediate are carried out ultraviolet source irradiation below the 2h, again described upper and lower cover plate and intermediate are fit together, continue irradiation 2～6h.
4, the method for making of a kind of micro-fluidic chip with Z type photometric detection pond as claimed in claim 1 is characterized in that: before implementation step 7, respectively described upper and lower cover plate and intermediate are carried out fitting behind the plasma radiation again earlier.
5, as the method for making of claim 1 or 2 or 3 or 4 described a kind of micro-fluidic chips with Z type photometric detection pond, it is characterized in that: in implementation step 4) preceding, earlier dimethyl silicone polymer monomer and initiating agent are placed open-top receptacle, under 0.005～0.02MPa vacuum tightness, 50～55 ℃ were heated 30～60 minutes in vacuum drying oven.
6, as the method for making of claim 1 or 2 or 3 or 4 described a kind of micro-fluidic chips with Z type photometric detection pond, it is characterized in that: the thickness of described U-shaped packing ring is 100～2000um.
7, the method for making of a kind of micro-fluidic chip with Z type photometric detection pond as claimed in claim 5, it is characterized in that: the thickness of described U-shaped packing ring is 100～2000um.
8, as the method for making of claim 1 or 2 or 3 or 4 or 7 described a kind of micro-fluidic chips with Z type photometric detection pond, it is characterized in that: the bracing frame of a thin slice as fixed chip is set at least, and punch on described thin slice in corresponding at least described Z type photometric detection pond on one of described upper and lower cover plate.
9, the method for making of a kind of micro-fluidic chip with Z type photometric detection pond as claimed in claim 5, it is characterized in that: the bracing frame of a thin slice as fixed chip is set at least, and punch on described thin slice in corresponding at least described Z type photometric detection pond on one of described upper and lower cover plate.
10, the method for making of a kind of micro-fluidic chip with Z type photometric detection pond as claimed in claim 6, it is characterized in that: the bracing frame of a thin slice as fixed chip is set at least, and punch on described thin slice in corresponding at least described Z type photometric detection pond on one of described upper and lower cover plate.
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| CN101424660B (en) * | 2007-10-31 | 2012-01-04 | 南京大学 | Design and production of portable highly effective capillary pipe electrophoresis chip sampling by chink |
| CN102319593B (en) * | 2011-08-16 | 2013-11-20 | 北京博晖创新光电技术股份有限公司 | Cytosis polymer microfluidic chip and preparation method thereof |
| CN103293050A (en) * | 2013-05-27 | 2013-09-11 | 苏州扬清芯片科技有限公司 | Serum filter chip and preparation chip thereof |
| CN107159329A (en) * | 2017-05-22 | 2017-09-15 | 天津微纳芯科技有限公司 | A kind of chip and its method for packing for sample detection |
| CN109289952B (en) * | 2018-11-08 | 2024-03-08 | 沈阳化工大学 | Preparation method of microfluidic chip with high-viscosity micron-sized channel |
| CN113522379B (en) * | 2020-04-20 | 2023-04-07 | 中国科学院化学研究所 | Micro-wall array and preparation method and application thereof, micro-channel and preparation method thereof, micro-channel reactor and application thereof |
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| 基于复合型微流控芯片的紫外检测电泳分析系统的优化及应用. 曹晓丹，方群，方肇伦.高等学校化学学报，第25卷. 2004 |
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