CN1645137A - Assistant hot-pressed packing method for polymethylmethacrylate microflow controlled chip solvent - Google Patents
Assistant hot-pressed packing method for polymethylmethacrylate microflow controlled chip solvent Download PDFInfo
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- CN1645137A CN1645137A CN 200510023645 CN200510023645A CN1645137A CN 1645137 A CN1645137 A CN 1645137A CN 200510023645 CN200510023645 CN 200510023645 CN 200510023645 A CN200510023645 A CN 200510023645A CN 1645137 A CN1645137 A CN 1645137A
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Abstract
A packaging method includes selecting cyclopentaneous and ice-acetic with low solubility and high boiling point comparing to perspex as adhesive, preparing perspex microflow control chip substrate with microflow channel, drop-coating said adhesive on cover film of perspex and then closing it with substrate, placing them in oven at 75-85 deg.c, bring 1-2 N/cm2 pressure for 10-15 min, on it through two glass plates, cooling it to room temperature to obtain product of perspex microflow control chip.
Description
Technical field
The invention belongs to technical field of biological, be specifically related to the auxiliary hot-pressed packing method of a kind of polymethyl methacrylate micro flow control chip solvent.
Background technology
Since nineteen ninety Manz and Widmer[1] (since the μ-TAS), Nian Zhongyi develops into one of sciemtifec and technical sphere of forefront on the our times surplus short ten to propose micro-full analytical system first.As a frontier interdisciplinary, its target is to handle whole microminiaturized, the integrated and portability that detects by micro electronmechanical processing (MEMS) technology and biotechnology realization chemical analysis system from sample, is the important directions and the forward position of present analytical instrument development.Micro-fluidic chip is an architectural feature with the microchannel network then, it is the emphasis of current micro-total analysis system development, and efficient with it, fast, few, the low consumption of reagent dosage and integrated level advantages of higher caused domestic and international analysis and life science circle relevant expert's extensive concern, shown good prospects for application in fields such as environmental monitoring, clinical diagnosis, Pharmaceutical Analysis, legal medical expert and military affairs, various new micro-fluidic chip technologies of preparing emerge in an endless stream.
Micro-fluidic chip mainly uses glass and polymer chip [2], and the glass-chip process technology requires high, needs specialized apparatus, is difficult to adopt mould to be produced in enormous quantities, and the price comparison costliness has limited its application.So polymkeric substance is developed by chip, it makes the main technology such as injection moulding, die, casting and monomer injection molding in-situ polymerization that adopt, because cheap and easy production in enormous quantities, have good industrialization prospect, wherein polymethylmethacrylate is a polymkeric substance [3] commonly used in the facture of microchip.Usually polymethyl methacrylate micro flow control chip adopts common packaging by hot pressing, promptly under the condition that is higher than polymethylmethacrylate glass temperature (105 ℃), (5-10 newton/square centimeter) makes micro-fluidic chip substrate and epiphragma be bonded into chip by plus-pressure.Shortcoming is for when being higher than glass temperature, and the microchannel distortion is big, and stops up easily, becomes the bottleneck [4] that restriction polymethylmethacrylate chip puts into production and uses.In addition, split easily during the chip of pure packaging by hot pressing uses and scrap.
List of references
[1]Manz?A，Graber?N，Widmer?HM.Sens.Actuators?B?1990，1，244-248.
[2]Verpoorte?E.Electrophoesis?2002，23，677-712.
[3]Becker?H，Locascio，LE.Talanta?2002，56，267-287.
[4]Becker?H，Gartner?C.Electrophoesis?2000，21，12-26.
Summary of the invention
The objective of the invention is to propose a kind of auxiliary hot-pressed packing method of solvent of polymethyl methacrylate micro flow control chip, to reduce the temperature and pressure of Chip Packaging, thereby the distortion of microchannel in the Chip Packaging process in the reduction chip, improve the success ratio of Chip Packaging, for further industrialization lays the first stone.
The solvent hot-pressed packing method of the polymethyl methacrylate micro flow control chip that the present invention proposes, less and the organic solvent tool higher (as cyclopentanone and acetate etc.) is a bonding agent to polymethylmethacrylate solubleness in selection, the polymethyl methacrylate micro flow control chip substrate that contains microchannel that use is made by silicon formpiston in-situ polymerization, with above-mentioned organic solvent evenly drip be coated in the unidimensional polymethyl methacrylate epiphragma of substrate on, aim at the substrate that contains microchannel then and close, place 75-85 ℃ baking oven, on micro-fluidic chip to be packaged, apply pressure 10-15 minute of 1-2 newton/square centimeter by two glass plates and iron block, cool to room temperature promptly gets the polymethyl methacrylate micro flow control chip finished product again.
Packaging by hot pressing organic solvent such as cyclopentanone and acetate etc. that the present invention selects, lower and boiling point is higher (being higher than 100 ℃) to polymethylmethacrylate solubleness, the small dissolubility of polymethylmethacrylate is made the polymkeric substance swelling of very thin surface one deck by solvent, glass temperature is descended, thereby reduce the temperature and pressure of packaging by hot pressing, but because solvent is very little to the solubleness of polymethylmethacrylate, polymer glassization below the superficial layer is temperature-resistant, so the microchannel distortion is very little in the packaging by hot pressing process.It is little and can be from the channel outlet volatilization in hot pressing to body chip solubleness to remain in a small amount of solvent in the microchannel simultaneously, thereby avoids passage to stop up in packaging by hot pressing, makes Chip Packaging intensity and is packaged into power and significantly improve.Using the higher solvent mainly is in order to prevent the too fast volatilization of solvent in coating and encapsulation process, to influence packaging effect.This chip solvent auxiliary heat press seal packing technique is easy and simple to handle, and cost is low, can carry out large-scale production, and good prospects for application is arranged.
The method for making that the present invention relates to polymethyl methacrylate micro flow control chip is as follows:
Adopt the computer aided design software design chips, typical design as shown in Figure 1, constitute by single right-angled intersection microchannel and solution connection holes, adopt high resolving power (greater than 3000dpi) laser photocomposing system on transparent membrane, to be printed as the mask negative film, microchannel width on the mask is 40-100 μ m, solution connection holes diameter 1-2mm wherein separates microchannel 2 and sample intake passage 7 and solution hole 1,4,5 and 6 (Fig. 1) for transparent, and remainder is a black.The erect image of design drawing is seen Fig. 1.In silicon chip (p type through oxidation processes, thick 500 μ m, 4 inches of diameters, crystal orientation＜100 〉, surface silica dioxide oxidation bed thickness 100nm) applies one deck negative photoresist (as the SU-8 photoresist) by the spin-coating technology, cover mask (the chip capillary microfluxion that contains design) then, after ultraviolet exposure and baking processing, with supporting developer immersion treatment, the flush away photoresist layer of portion's exposed portion (kapillary and solution hole beyond zone) not in acetone and isopropyl alcohol respectively, the photoresist sclerosis that baking partly exposes capillary channel and solution connection holes in baking oven then is in rare HF-NH
4F solution etching off silicon chip surface is the SiO of portion's exposed portion not
2Layer, then in 50-70 ℃ with about 1 hour of the exposed silicon chip of 40%KOH aqueous solution (containing 5% isopropyl alcohol) etching, promptly make silicon chip formpiston 9, to have the silicon chip one side of kapillary tongue clamp one with one flat plate glass in the middle of hollow out be the aluminium sheet (about 2mm is thick) of the rectangle of chip size, the chip mould.
With methyl methacrylate monomer and small amount of thermal initiating agent azoisobutyronitrile (0.1-0.2% of methyl methacrylate monomer amount) and a little light initiating agent styrax (0.1-0.2% of methyl methacrylate monomer amount), in 50 ℃ of water-baths heating and shake and make its dissolving, in 80-90 ℃ of water-bath, heated 15-20 minute then, shook mixed solution once in per 5 minutes, and made molten this pre-polymerization of monomer become glycerine shape clear solution.Attention will prevent that sealing enters in pre-collecting process, avoid temperature too high simultaneously, otherwise can be sudden and violent poly-because of causing, and causes the waste of material.Pre-polymerization later stage polymerization speed is accelerated.Above-mentioned pre-gathering solutions is injected mould by the mould openings groove, and open slot caused bulk polymerization with 20W uviol lamp (356nm is apart from 4-5 centimetre) in 30-60 minute by mould glass irradiation pre-gathering solutions up.Simultaneously respective liquid potpourri injection molding is about polymerization between the sheet glass of 80-120 μ m in the slit, obtains the epiphragma of same material after the demoulding.After treating the polymeric solution sclerosis of pre-polymerization, with mould demoulding in ultrasonic 10 minutes in 30-50 ℃ of water-bath.The micro-fluidic chip substrate channel end boring (solution connection holes 1,4,5 and 6 is seen Fig. 1, aperture 2mm) of the demoulding is used to connect solution.The organic solvent that selection is less to polymethylmethacrylate solubleness and the tool boiling point is higher such as cyclopentanone and acetate etc. are bonding agent, with the polymethyl methacrylate micro flow control chip substrate 9 that contains microchannel that uses silicon formpiston in-situ polymerization to make, by solvent auxiliary heat press seal packing technique of the present invention and unidimensional polymethylmethacrylate epiphragma 10 bonding making micro-fluidic chips.Earlier above-mentioned organic solvent is evenly dripped and be coated on the polymethylmethacrylate epiphragma 10, aim at the substrate 9 that contains microchannel then and close, the microchannel one side is arranged between substrate 9 and epiphragma 10, inhale with filter paper and to remove the solvent that oozes out, then in 75-85 ℃ baking oven, apply pressure 10-15 minute of 1-2 newton/square centimeter by two glass plates (8 and 8 ') and irony weight 11 then, cool to room temperature promptly gets the polymethyl methacrylate micro flow control chip finished product.
The present invention encapsulates that the method for polymethyl methacrylate micro flow control chip is easy and simple to handle, favorable reproducibility, amount of samples are few, wherein lead the compartment analysis that the detector coupling successfully is used for three kinds of common organic anion oxalates, tartrate anion and acetates, analysis efficiency height with electricity with the polymethyl methacrylate micro flow control chip of cyclopentanone encapsulation.Concrete visible following test experiments result:
Use the polymethyl methacrylate micro flow control chip and the electricity of the present invention's encapsulation shown in Figure 1 to lead the detector coupling, the electrophoresis pattern of the electrophoretogram of 1mM oxalate, tartrate anion and the acetate of acquisition is seen Fig. 3.Test condition is: separation voltage is-1500V, sample introduction voltage is-1500V, sample injection time is 1s, buffer solution is 20mM 2-morpholino b acid (MES)-20mM histidine (pH6.1), electricity is led detection waveform, and (frequency is 200kHz for sine wave, the voltage peak-to-peak amplitude is 10V, and the non-contact conductance detecting electrode is to the end in separation capillary, i.e. right side.The anionic range of linearity to said determination is 0.01-5mM, detect lower limit in the 5-8 mu m range, the relative standard deviation of measuring the peak-to-peak signal of 1mM oxalate, tartrate anion and acetate for 10 times is respectively 3.1%, 2.9% and 4.1%, show that this polymethyl methacrylate micro flow control chip range of linearity is wide, reappearance is good and fast efficient, in 90 seconds, just can separate and detect simultaneously three kinds of negative ion fully, can be used for the mensuration of actual sample.
Description of drawings
Fig. 1 is the typical micro-fluidic chip design drawing that the present invention relates to.
The solvent auxiliary heat press seal assembling device synoptic diagram of Fig. 2 polymethyl methacrylate micro flow control chip.(a) exploded view of packaging by hot pressing device; (b) chip packaging device of cheek weight not; (c) chip packaging device of cheek weight.
Fig. 3 is three kinds of organic anions of polymethyl methacrylate micro flow control chip separation detection of the present invention's encapsulation: the electrophoresis pattern of 1mM oxalate (a), tartrate anion (b) and acetate (c).
Number in the figure: 1 is the sample solution hole, 2 for separating microchannel (separation capillary), 3 for containing the micro-fluidic chip of microchannel 2 and sample introduction kapillary 7 and solution hole 1,4,5 and 7,4,5 and 6 be the buffer solution hole, 7 is sample introduction microchannel (sample introduction kapillary), and 8 and 8 ' is glass plate, and 9 is the micro-fluidic chip substrate, 10 is the micro-fluidic chip epiphragma, and 11 is the irony weight.
Embodiment
Further describe the present invention below by embodiment and accompanying drawing:
1, the auxiliary packaging by hot pressing of the cyclopentanone of polymethyl methacrylate micro flow control chip
(A) microchannel and the solution connection holes of Adobe Illustrator 10.0 software design chips adopted in the design of micro-fluidic chip, adopt high resolving power (3600dpi) laser photocomposing system on the polyester transparent film, to be printed as the mask negative film, microchannel width on the mask is 50 μ m, solution connection holes is the circular hole of diameter 2mm, wherein microchannel (separation capillary 2 and sample introduction kapillary 7) and solution hole 1,4,5 and 6 (Fig. 1) are transparent, and remainder is a black.The erect image of micro-fluidic chip is seen Fig. 1.Separate microchannel 2 long 5.0cm, sample introduction microchannel 7 long 0.5cm, wherein kapillary 2 and 7 point of crossing are 0.5cm to the distance of three nearest solution connection holes.
(B) silicon chip (the p type of being produced on of silicon negative film and chip mould through oxidation processes, thick 500 μ m, 4 inches of diameters, crystal orientation＜100 〉, surface silica dioxide oxidation bed thickness 100nm) by spin-coating technology (rotating speed 3000rpm, 40 seconds) coating one deck negative photoresist (SU-8 photoresist), baking 40 minutes (preceding baking) in 65 ℃ of baking ovens, cover mask (the chip capillary microfluxion that contains design) then, (1.5-2mm) compresses with quartz glass plate, exposure 30min (365nm under ultraviolet ray, 45W), baking 25 minutes (baking of exposure back) in 65 ℃ of baking ovens, with the supporting developer immersion treatment of SU-8 after 90 seconds, rinsing 20 seconds is with the flush away photoresist layer of portion's exposed portion (zone beyond microchannel and the solution hole) not in acetone and isopropyl alcohol respectively, and baking 10 minutes (back baking) makes the photoresist sclerosis that capillary channel and solution connection holes partly expose on the silicon chip in 150 ℃ of baking ovens then, and silicon chip is dipped in 0.5M HF-0.5M NH
4F solution 3.5 minutes is with the SiO of silicon chip surface
2Layer etching off; then in 60 ℃ of about 1 hour of silicon chips (etching speed is 0.35 μ m/ minute) that expose with 40%KOH aqueous solution (containing 5% isopropyl alcohol) etching; form the outstanding capillary channel and the solution pore structure part of anode membrane; the silicon chip not photoresist on etched portions surface can come off in etching process automatically; silicon dioxide layer under the photoresist can not protected the silicon structure under the silicon dioxide layer by 40%KOH aqueous solution etching, promptly gets and makes the silicon chip formpiston.To have the silicon chip one side of kapillary tongue clamp one with one flat plate glass in the middle of hollow out be the aluminium sheet (about 2mm is thick) of the rectangle of chip size, the chip mould.
(C) injection molding and be aggregated in the methyl methacrylate monomer adds small amount of thermal initiating agent azoisobutyronitrile (methyl methacrylate monomer quality 0.15%) and a little light initiating agent styrax (methyl methacrylate monomer quality 0.15%), in 50 ℃ of water-baths heating and shake and make its dissolving, in 80-90 ℃ of water-bath, heated 15-20 minute then, shook mixed solution once in per 5 minutes, and made molten this pre-polymerization of monomer become glycerine shape clear solution.Attention will prevent that sealing enters in pre-collecting process, avoid temperature too high simultaneously, otherwise can be sudden and violent poly-because of causing, and causes the waste of material.Above-mentioned pre-gathering solutions is injected mould by the mould openings groove, and open slot caused bulk polymerization with 20W uviol lamp (365nm) in 30-60 minute by mould glass irradiation pre-gathering solutions up.Simultaneously respective liquid potpourri injection molding is about polymerization between the sheet glass of 100 μ m in the slit, obtains the epiphragma 10 of same material after the demoulding.
(D) after the auxiliary packaging by hot pressing of the demoulding of chip and cyclopentanone is treated the polymeric solution sclerosis of pre-polymerization, with mould demoulding in ultrasonic 10 minutes in 40 ℃ of water-baths.(solution connection holes 1,4,5 and 6 is seen Fig. 1 with the boring of micro-fluidic chip substrate 9 channel ends of the demoulding, aperture 2mm) is used to connect solution, the selection cyclopentanone (boiling point be 130.6 ℃) higher to the less boiling point of polymethylmethacrylate solubleness is bonding agent, with the polymethyl methacrylate micro flow control chip substrate 9 that contains microchannel that uses silicon formpiston in-situ polymerization to make, by solvent auxiliary heat press seal packing technique and unidimensional polymethylmethacrylate epiphragma 10 bonding making micro-fluidic chips.Specifically be cyclopentanone evenly to be dripped to be coated on the polymethylmethacrylate epiphragma 10 earlier, aim at the substrate 9 that contains microchannel then and close, the microchannel one side is arranged between substrate 9 and epiphragma 10, inhale with filter paper and to remove the solvent that oozes out, then in 80-85 ℃ baking oven, apply 1.5 (newton/square centimeter) pressure 10-15 minute by two glass plates (8 and 8 ') and irony weight 11 then, cool to room temperature promptly gets the polymethyl methacrylate micro flow control chip finished product.Experiment finds that cyclopentanone is the more satisfactory solvent of auxiliary heat press seal cartridge chip.
The auxiliary hot-pressed packing method of the solvent of this polymethyl methacrylate micro flow control chip is easy and simple to handle fast, can reduce the rejection rate of micro-fluidic chip preparation.The one side that epiphragma is arranged is a chip upper surface.The length of micro-fluidic chip is 6.5mm, and width is 2.0mm, and thickness is 2.0mm.
The chip of this method encapsulation successfully is used to detect three kinds of organic anion (see figure 3)s
2, the auxiliary packaging by hot pressing of the acetate of polymethyl methacrylate micro flow control chip
The making of the making of the design of electrophoresis chip, silicon formpiston and chip mould and polymethyl methacrylate micro flow control chip substrate 9 and epiphragma 10 is with embodiment 1.Micro-fluidic chip substrate 9 channel ends boring (solution connection holes 1 with the demoulding, 4,5 and 6 see Fig. 1, aperture 2mm) is used to connect solution, the selection acetate (boiling point be 117.9 ℃) higher to the less boiling point of polymethylmethacrylate solubleness is bonding agent, earlier above-mentioned organic solvent is evenly dripped and be coated on the polymethylmethacrylate epiphragma 10, aim at the substrate 9 that contains microchannel then and close, the microchannel one side is arranged between substrate 9 and epiphragma 10, inhale with filter paper and to remove the solvent that oozes out, then in 75-80 ℃ baking oven, apply 1.5 (newton/square centimeter) pressure 10-12 minute by two glass plates (8 and 8 ') and irony weight 11 then, cool to room temperature promptly gets the polymethyl methacrylate micro flow control chip finished product.Because acetate boiling point (117.9 ℃) is low than the cyclopentanone that uses among the embodiment (130.6 ℃ of boiling points), in packaging by hot pressing, used lower temperature.Using the deficiency of acetate is that volatilization gas is corrosive, but cheap.
The polymethyl methacrylate micro flow control chip that adopts acetate auxiliary heat press seal packing technique to prepare also successfully is used for the compartment analysis of embodiment 1 three kinds of common organic anion oxalates, tartrate anion and acetates, and the result is similar to embodiment 1.
Claims (1)
1, a kind of polymethyl methacrylate micro flow control chip solvent is assisted hot-pressed packing method, it is characterized in that selecting to polymethylmethacrylate solubleness less organic solvent cyclopentanone or acetate is bonding agent, the polymethyl methacrylate micro flow control chip substrate that contains microchannel that use is made by silicon formpiston in-situ polymerization, with above-mentioned organic solvent evenly drip be coated in the unidimensional polymethylmethacrylate epiphragma of substrate on, aim at substrate then and close, place 75-85 ℃ baking oven, on micro-fluidic chip to be packaged, apply pressure 10-15 minute of 1-2 newton/square centimeter by two glass plates and iron block, cool to room temperature gets the polymethyl methacrylate micro flow control chip finished product.
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| CN108144661B (en) * | 2017-12-27 | 2020-04-10 | 中国科学院长春光学精密机械与物理研究所 | Packaging method of micro-fluidic chip |
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