CN103183310A - Low temperature bonding method of microfluidic chip - Google Patents
Low temperature bonding method of microfluidic chip Download PDFInfo
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- CN103183310A CN103183310A CN2011104449834A CN201110444983A CN103183310A CN 103183310 A CN103183310 A CN 103183310A CN 2011104449834 A CN2011104449834 A CN 2011104449834A CN 201110444983 A CN201110444983 A CN 201110444983A CN 103183310 A CN103183310 A CN 103183310A
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Abstract
The invention belongs to the field of micro-fine processing, relates to a microfluidic chip technology, and particular relates to a low temperature bonding method of microfluidic chips used in ordinary laboratories. The bonding of the present invention is completed at low temperature, the entire operation procedure is completed in a non-ultraclean environment, and the method is simple and practical, helps to reduce production costs, is high in yield, and is suitable for preparation of microfluidic chips in ordinary laboratories. According to the invention, an external assistance adhesive (such as a UV curable adhesive) is used for sealing, and the microfluidic chip is effectively protected, so that the microfluidic chip is not damaged in a bonding process.
Description
Technical field
The invention belongs to little retrofit field, relate to the micro-fluidic chip technology, particularly a kind of method of low-temperature bonding of the micro-fluidic chip that is applied to common lab.
Background technology
(Micro Total Analysis Systems, μ-TAS) be is the interdisciplinary frontier that base growth is got up with analytical chemistry to micro-total analysis system.It is based on micro electronmechanical (MEMS), and by process 10～100 microns passage and network at silicon, glass, quartz, polymer surface, microminiaturization, the portability of realization analytical equipment are used for this kind purpose chip and are commonly referred to as micro-fluidic chip.Glass and quartz material are ideal chip manufacturing materials with its good ultraviolet light transmission, surface stability, electric osmose performance.Yet as a step of the most critical of chip manufacturing, the fine or not degree of the bonding of chip has influenced the quality of chip greatly.
The bonding of hyaline-quartz material generally adopts thermal bonding, anode linkage, bonding process is generally finished in clean room, the flatness of para-linkage material, factors such as thermal coefficient of expansion are had relatively high expectations, and it is transparent inadequately that potteryization phenomenon surface at high temperature easily takes place quartzy material, influence bonding effect, it is not high to be bonded to power, and experimental cost is higher.Anode linkage is had relatively high expectations to glass material, is unsuitable for extensive popularization.
Based on above problem, the technology of low-temperature bonding glass, quartzy material chip is widely studied in recent years.Existing low-temperature bonding technology mainly adopts HF acid and sodium metasilicate as adhesive, yet adopt sodium metasilicate bonding malleable raceway groove pattern, utilize HF acid bonding to need strict operating key resultant pressure and HF acid concentration, and HF acid corrosion glass ability is stronger, destructible fine structure raceway groove.
Summary of the invention
The object of the present invention is to provide a kind of low-temperature bonding method that is applied to the micro-fluidic chip of common lab, to solve the bonding problem of chip under the low temperature.
The low-temperature bonding method that is applied to the micro-fluidic chip of common lab of the present invention may further comprise the steps:
(1) makes a call to a hole that is not connected with described raceway groove at the hand-hole that has raceway groove and the reactant liquor that is connected with raceway groove (structure that the Experimental Area is designed) and the non-channel region for the preparation of the edge of the substrate of micro-fluidic chip that portals; Clean this substrate and for the preparation of the cover plate (can use deionized water to clean) of micro-fluidic chip, dry cover plate and substrate;
(2) be that 1%～3% sodium silicate solution splashes into the cover plate that obtains after step (1) drying and the non-channel region between the substrate with mass percent concentration, be squeezed to cover plate and substrate fits tightly;
(3) cover plate that fits tightly that step (2) is obtained and substrate are put into vacuum drying chamber to vacuumize and be heated to temperature are 110 ℃～120 ℃, and preliminary bonding (time of general insulation is 12～24 hours) is finished in insulation;
(4) be under 65 ℃～80 ℃ in temperature, paraffin is melted, cover plate and the substrate of step (3) being finished preliminary bonding are dipped in the atoleine, described hand-hole or the place of portalling at substrate apply negative pressure, utilize negative pressure with atoleine by described hand-hole or portal and be drawn in the raceway groove, with cover plate and substrate clamping, fixing, cool to room temperature is finished the protection to raceway groove;
(5) cover plate and the substrate (can use deionized water to carry out soaking and washing repeatedly) that obtain of soaking and washing step (4) repeatedly removed the sodium metasilicate dissolving of the solubility between cover plate and the substrate, vacuumizes drying under the room temperature;
(6) cover plate that obtains in step (5) and substrate around edge front cover circle ultraviolet cured adhesive, the place, described hole that is not connected with described raceway groove at substrate applies negative pressure, and ultraviolet cured adhesive is drawn into non-channel region by the slit between cover plate and the substrate;
(7) carry out UV-irradiation around the cover plate that earlier step (6) is obtained and the substrate, the channel region to substrate carries out UV-irradiation again, aged at room temperature (generally wearing out about a week);
(8) cover plate that obtains after step (7) aged at room temperature and substrate being heated to temperature is 65 ℃～80 ℃, by on-chip described hand-hole or portal the atoleine sucking-off in the raceway groove; Cool to room temperature, by on-chip described hand-hole or portal, with the paraffin of benzinum erase residual in raceway groove, use the alcohol wash benzinum, the last immersion cover plate of flushing repeatedly and substrate are to remove the inner remaining sodium metasilicate (can use deionized water to wash immersion) of dechannelling, vacuum drying under the room temperature;
(9) under the room temperature, with the concentrated sulfuric acid (mass concentration is 98%): the volume ratio of hydrogen peroxide is that 1: 1～7: 3 mixed liquor is by on-chip described hand-hole or in the raceway groove of the substrate of the cover plate that obtains after (inject or apply negative pressure) step (8) drying of portalling and be full of and substrate, heating cover plate and substrate to temperature are 100～120 ℃, insulation (time of general insulation is 1～2 minute) is to remove the middle remaining ultraviolet cured adhesive of dechannelling; By on-chip described hand-hole or portal, clean raceway groove (can use deionized water to clean repeatedly) repeatedly, finish bonding after the vacuum drying, obtain micro-fluidic chip.
The aperture in the described hole that is not connected with described raceway groove is 2～4mm.
Described substrate and cover plate do not have specific requirement, and the raw material for preparation in this area is adopted during micro-fluidic chip can be glass or quartz etc.
The present invention has following effect:
Bonding of the present invention is finished at low temperatures, and the whole operation process is finished under non-super-clean environment, and is simple and practical, reduced cost of manufacture, and the yield rate height is highly suitable for the preparation of the micro-fluidic chip of common lab.(1) the bonding micro-fluidic chip does not have specific requirement, glass, quartz medium all can, greatly enlarged the scope of application of the technology of bonding.(2) adopt foreign aid's glue class (as ultraviolet cured adhesive) sealing-in, effectively protected micro-fluidic chip, micro-fluidic chip is not destroyed in bonding.(3) need not high temperature heating in the bonding process, the highlyest under the general condition be heated to 120 ℃, reduced the requirement of para-linkage equipment.(4) micro-fluidic chip is as stoppage phenomenon in the experimental implementation process, can not dredge with conventional method, can be warming up to 300 ℃ of heating and open sealing-in in about five hours, using volume ratio is that 7: 3 the concentrated sulfuric acid and the mixed liquor of hydrogen peroxide boil, micro-fluidic chip is cleaned, clean back repeat key closing operation step, reusable micro-fluidic chip has prolonged service life of micro-fluidic chip greatly.
Description of drawings
Fig. 1. the bonding effect figure of the embodiment of the invention 1.
The specific embodiment
Embodiment 1
(1) making a call to an aperture that is not connected with described raceway groove at the hand-hole that has raceway groove and the reactant liquor that is connected with raceway groove (structure that the Experimental Area is designed) and the non-channel region for the preparation of the edge of the glass substrate of micro-fluidic chip that portals is the hole of 2mm, have on the described glass substrate at this moment the hole that is connected with described raceway groove and with described raceway groove non-intercommunicating pore; Use deionized water to clean this glass substrate and for the preparation of the cover glass of micro-fluidic chip, with hair dryer cover glass and glass substrate are dried up;
(2) be that 3% sodium silicate solution splashes into the cover glass that obtains after step (1) dries up and the non-channel region between the glass substrate with mass percent concentration, be squeezed to cover glass and glass substrate fits tightly;
(3) cover glass that fits tightly that step (2) is obtained and glass substrate are put into vacuum drying chamber to vacuumize and be heated to temperature are 110 ℃, are incubated 12 hours and finish preliminary bonding;
(4) be under 65 ℃ in temperature, paraffin is melted, cover glass and the glass substrate of step (3) being finished preliminary bonding are dipped in the atoleine, described hand-hole or the place of portalling at glass substrate apply negative pressure, utilize negative pressure with atoleine by described hand-hole or portal and be drawn in the raceway groove, cover glass and glass substrate are clamped, fix, and cool to room temperature is finished the protection to raceway groove;
(5) use deionized water to carry out repeatedly cover glass and the glass substrate that soaking and washing step (4) obtains, the sodium metasilicate dissolving of the solubility between cover glass and the glass substrate is removed, vacuumize drying under the room temperature;
(6) cover glass that obtains in step (5) and glass substrate around edge front cover circle ultraviolet cured adhesive, the place, described hole that is not connected with described raceway groove at glass substrate applies negative pressure, and ultraviolet cured adhesive is drawn into non-channel region by the slit between cover glass and the glass substrate;
(7) cover glass that earlier step (6) is obtained and glass substrate carries out UV-irradiation all around, again UV-irradiation is carried out on the surface (reverse side of glass substrate is described channel region) of glass substrate, make the ultraviolet light polymerization adhesive curing, aged at room temperature is about one week;
(8) cover glass that obtains after step (7) aged at room temperature and glass substrate being heated to temperature is 65 ℃, by the described hand-hole on the glass substrate or portal the atoleine sucking-off in the raceway groove; Cool to room temperature, by the described hand-hole on the glass substrate or portal, with the paraffin of benzinum erase residual in raceway groove, use the alcohol wash benzinum, use deionized water to wash repeatedly at last to soak cover glass and glass substrate with the sodium metasilicate except the inner remnants that dechannel, vacuum drying under the room temperature;
(9) under the room temperature, be 98% the concentrated sulfuric acid with mass concentration: the volume ratio of hydrogen peroxide is that 1: 1 mixed liquor is by the described hand-hole on the glass substrate or portal and be full of in the raceway groove of the cover glass that obtains after step (8) drying and the glass substrate in the glass substrate, heating glass cover plate and glass substrate to temperature is 100 ℃, be incubated 1 minute, with the ultraviolet cured adhesive except remnants in dechannelling; By the described hand-hole on the glass substrate or portal, use deionized water to clean raceway groove repeatedly, finish bonding after the vacuum drying, obtain micro-fluidic chip.Bonding effect as shown in Figure 1.
Embodiment 2
(1) making a call to an aperture that is not connected with described raceway groove at the hand-hole that has raceway groove and the reactant liquor that is connected with raceway groove (structure that the Experimental Area is designed) and the non-channel region for the preparation of the edge of the glass substrate of micro-fluidic chip that portals is the hole of 4mm, have on the described glass substrate at this moment the hole that is connected with described raceway groove and with described raceway groove non-intercommunicating pore; Use deionized water to clean this glass substrate and for the preparation of the cover glass of micro-fluidic chip, with hair dryer cover glass and glass substrate are dried up;
(2) be that 1% sodium silicate solution splashes into the cover glass that obtains after step (1) dries up and the non-channel region between the glass substrate with mass percent concentration, be squeezed to cover glass and glass substrate fits tightly;
(3) cover glass that fits tightly that step (2) is obtained and glass substrate are put into vacuum drying chamber to vacuumize and be heated to temperature are 120 ℃, are incubated 24 hours and finish preliminary bonding;
(4) be under 80 ℃ in temperature, paraffin is melted, cover glass and the glass substrate of step (3) being finished preliminary bonding are dipped in the atoleine, described hand-hole or the place of portalling at glass substrate apply negative pressure, utilize negative pressure with atoleine by described hand-hole or portal and be drawn in the raceway groove, cover glass and glass substrate are clamped, fix, and cool to room temperature is finished the protection to raceway groove;
(5) use deionized water to carry out repeatedly cover glass and the glass substrate that soaking and washing step (4) obtains, the sodium metasilicate dissolving of the solubility between cover glass and the glass substrate is removed, vacuumize drying under the room temperature;
(6) cover glass that obtains in step (5) and glass substrate around edge front cover circle ultraviolet cured adhesive, the place, described hole that is not connected with described raceway groove at glass substrate applies negative pressure, and ultraviolet cured adhesive is drawn into non-channel region by the slit between cover glass and the glass substrate;
(7) cover glass that earlier step (6) is obtained and glass substrate carries out UV-irradiation all around, again UV-irradiation is carried out on the surface (reverse side of glass substrate is described channel region) of glass substrate, make the ultraviolet light polymerization adhesive curing, aged at room temperature is about one week;
(8) cover glass that obtains after step (7) aged at room temperature and glass substrate being heated to temperature is 80 ℃, by the described hand-hole on the glass substrate or portal the atoleine sucking-off in the raceway groove; Cool to room temperature, by the described hand-hole on the glass substrate or portal, with the paraffin of benzinum erase residual in raceway groove, use the alcohol wash benzinum, use deionized water to wash repeatedly at last to soak cover glass and glass substrate with the sodium metasilicate except the inner remnants that dechannel, vacuum drying under the room temperature;
(9) under the room temperature, be 98% the concentrated sulfuric acid with mass concentration: the volume ratio of hydrogen peroxide is that 7: 3 mixed liquor is by the described hand-hole on the glass substrate or portal and be full of in the raceway groove of the cover glass that obtains after step (8) drying and the glass substrate in the glass substrate, heating glass cover plate and glass substrate to temperature is 120 ℃, be incubated 2 minutes, with the ultraviolet cured adhesive except remnants in dechannelling; By the described hand-hole on the glass substrate or portal, use deionized water to clean raceway groove repeatedly, finish bonding after the vacuum drying, obtain micro-fluidic chip.
Embodiment 3
(1) making a call to an aperture that is not connected with described raceway groove at the hand-hole that has raceway groove and the reactant liquor that is connected with raceway groove (structure that the Experimental Area is designed) and the non-channel region for the preparation of the edge of the quartz substrate of micro-fluidic chip that portals is the hole of 3mm, have on the described quartz substrate at this moment the hole that is connected with described raceway groove and with described raceway groove non-intercommunicating pore; Use deionized water to clean this quartz substrate and for the preparation of the quartzy cover plate of micro-fluidic chip, with hair dryer quartzy cover plate and quartz substrate are dried up;
(2) be that 2% sodium silicate solution splashes into the quartzy cover plate that obtains after step (1) dries up and the non-channel region between the quartz substrate with mass percent concentration, be squeezed to quartzy cover plate and quartz substrate and fit tightly;
(3) the quartzy cover plate that fits tightly that step (2) is obtained and quartz substrate are put into vacuum drying chamber to vacuumize and be heated to temperature are 110 ℃, are incubated 18 hours and finish preliminary bonding;
(4) be under 75 ℃ in temperature, paraffin is melted, quartzy cover plate and the quartz substrate of step (3) being finished preliminary bonding are dipped in the atoleine, described hand-hole or the place of portalling at quartz substrate apply negative pressure, utilize negative pressure with atoleine by described hand-hole or portal and be drawn in the raceway groove, quartzy cover plate and quartz substrate are clamped, fix, and cool to room temperature is finished the protection to raceway groove;
(5) use deionized water to carry out repeatedly quartzy cover plate and the quartz substrate that soaking and washing step (4) obtains, the sodium metasilicate dissolving of the solubility between quartzy cover plate and the quartz substrate is removed, vacuumize drying under the room temperature;
(6) the quartzy cover plate that obtains in step (5) and quartz substrate around edge front cover circle ultraviolet cured adhesive, the place, described hole that is not connected with described raceway groove at quartz substrate applies negative pressure, and ultraviolet cured adhesive is drawn into non-channel region by the slit between quartzy cover plate and the quartz substrate;
(7) the quartzy cover plate that earlier step (6) is obtained and quartz substrate carries out UV-irradiation all around, again UV-irradiation is carried out on the surface (reverse side of quartz substrate is described channel region) of quartz substrate, make the ultraviolet light polymerization adhesive curing, aged at room temperature is about one week;
(8) the quartzy cover plate that obtains after step (7) aged at room temperature and quartz substrate being heated to temperature is 75 ℃, by the described hand-hole on the quartz substrate or portal the atoleine sucking-off in the raceway groove; Cool to room temperature, by the described hand-hole on the quartz substrate or portal, with the paraffin of benzinum erase residual in raceway groove, use the alcohol wash benzinum, use deionized water to wash repeatedly at last to soak quartzy cover plate and quartz substrate with the sodium metasilicate except the inner remnants that dechannel, vacuum drying under the room temperature;
(9) under the room temperature, be 98% the concentrated sulfuric acid with mass concentration: the volume ratio of hydrogen peroxide is that 7: 5 mixed liquor is by the described hand-hole on the quartz substrate or portal and be full of in the raceway groove of the quartzy cover plate that obtains after step (8) drying and the quartz substrate in the quartz substrate, heating quartzy cover plate and quartz substrate to temperature is 110 ℃, be incubated 1.5 minutes, with the ultraviolet cured adhesive except remnants in dechannelling; By the described hand-hole on the quartz substrate or portal, use deionized water to clean raceway groove repeatedly, finish bonding after the vacuum drying, obtain micro-fluidic chip.
Claims (4)
1. the low-temperature bonding method of a micro-fluidic chip is characterized in that, described low-temperature bonding method may further comprise the steps:
(1) makes a call to a hole that is not connected with described raceway groove at the hand-hole that has raceway groove and the reactant liquor that is connected with raceway groove and the non-channel region for the preparation of the edge of the substrate of micro-fluidic chip that portals; Clean this substrate and for the preparation of the cover plate of micro-fluidic chip, dry cover plate and substrate;
(2) be that 1%～3% sodium silicate solution splashes into the cover plate that obtains after step (1) drying and the non-channel region between the substrate with mass percent concentration, be squeezed to cover plate and substrate fits tightly;
(3) cover plate that fits tightly that step (2) is obtained and substrate are put into vacuum drying chamber to vacuumize and be heated to temperature are 110 ℃～120 ℃, and preliminary bonding is finished in insulation;
(4) be under 65 ℃～80 ℃ in temperature, paraffin is melted, cover plate and the substrate of step (3) being finished preliminary bonding are dipped in the atoleine, described hand-hole or the place of portalling at substrate apply negative pressure, utilize negative pressure with atoleine by described hand-hole or portal and be drawn in the raceway groove, with cover plate and substrate clamping, fixing, cool to room temperature is finished the protection to raceway groove;
(5) cover plate and the substrate that obtain of soaking and washing step (4) repeatedly removed the sodium metasilicate dissolving of the solubility between cover plate and the substrate, vacuumizes drying under the room temperature;
(6) cover plate that obtains in step (5) and substrate around edge front cover circle ultraviolet cured adhesive, the place, described hole that is not connected with described raceway groove at substrate applies negative pressure, and ultraviolet cured adhesive is drawn into non-channel region by the slit between cover plate and the substrate;
(7) cover plate that earlier step (6) is obtained and substrate carry out UV-irradiation all around, the channel region to substrate carries out UV-irradiation, aged at room temperature again;
(8) cover plate that obtains after step (7) aged at room temperature and substrate being heated to temperature is 65 ℃～80 ℃, by on-chip described hand-hole or portal the atoleine sucking-off in the raceway groove; Cool to room temperature by on-chip described hand-hole or portal, with the paraffin of benzinum erase residual in raceway groove, use the alcohol wash benzinum, and last flushing is repeatedly soaked cover plate and substrate with the sodium metasilicate except the inside remnants that dechannel, vacuum drying under the room temperature;
(9) under the room temperature, with the concentrated sulfuric acid: the volume ratio of hydrogen peroxide is that 1: 1～7: 3 mixed liquor is by on-chip described hand-hole or portal and be full of in the raceway groove of the cover plate that obtains after step (8) drying and the substrate in the substrate, heating cover plate and substrate to temperature are 100～120 ℃, insulation is with the ultraviolet cured adhesive except remnants in dechannelling; By on-chip described hand-hole or portal, clean raceway groove repeatedly, finish bonding after the vacuum drying, obtain micro-fluidic chip.
2. the low-temperature bonding method of micro-fluidic chip according to claim 1, it is characterized in that: the aperture in the described hole that is not connected with described raceway groove is 2～4mm.
3. the low-temperature bonding method of micro-fluidic chip according to claim 1, it is characterized in that: the time of the described insulation of step (3) is 12～24 hours.
4. the low-temperature bonding method of micro-fluidic chip according to claim 1, it is characterized in that: the time of the described insulation of step (9) is 1～2 minute.
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| CN106626219A (en) * | 2017-03-03 | 2017-05-10 | 广东工业大学 | Bonding system for polymer micro-fluidic chips |
| CN109025983A (en) * | 2018-07-27 | 2018-12-18 | 中国石油大学(北京) | A kind of simulation compact oil reservoir micromodel production method |
| CN109126914A (en) * | 2018-09-29 | 2019-01-04 | 江苏芯力特电子科技有限公司 | A kind of bonding method of micro-fluidic chip |
| CN109991346A (en) * | 2019-04-18 | 2019-07-09 | 南京大学 | A kind of micro-fluidic Ultraviolet Oxidation device for organic nitrogen analysis |
| CN111589477A (en) * | 2020-05-28 | 2020-08-28 | 韶关学院 | Micro-channel device processing technology |
| CN111943133A (en) * | 2020-08-25 | 2020-11-17 | 东北电力大学 | Micro-channel chip-PDMS-nano structure chip bonding method |
| CN114988723A (en) * | 2022-06-01 | 2022-09-02 | 北方夜视技术股份有限公司 | Optical light-transmitting element bonding method based on water glass |
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| CN114988723A (en) * | 2022-06-01 | 2022-09-02 | 北方夜视技术股份有限公司 | Optical light-transmitting element bonding method based on water glass |
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