CN1228631C - Preparation method of high polymer micro-fluidic chip - Google Patents
Preparation method of high polymer micro-fluidic chip Download PDFInfo
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- CN1228631C CN1228631C CN 02124100 CN02124100A CN1228631C CN 1228631 C CN1228631 C CN 1228631C CN 02124100 CN02124100 CN 02124100 CN 02124100 A CN02124100 A CN 02124100A CN 1228631 C CN1228631 C CN 1228631C
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Landscapes
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
Abstract
The invention relates to a method for manufacturing a high polymer microfluidic chip, in particular to a method for manufacturing a high polymer microfluidic chip by metal template printing, which is particularly suitable for the manufacturing of the microfluidic chip for separating micro-amount organic molecules such as DNA fragments with various sizes, amino acid, protein, organic pollutants and the like, metal ions, inorganic anions and the like. And coating photoresist on the metal plate, and carrying out exposure, development and etching to obtain the metal negative plate for preparing the high polymer microfluidic chip. Compared with the manufacturing method of the high polymer chip reported in the literature, the manufacturing method of the negative plate has the advantages of low price of the negative plate material, simple manufacturing method, good reproducibility, hard material, long service life and the like, can reduce the production cost, and is easy for batch production.
Description
Technical field
The present invention relates to a kind of manufacture method of high polymer micro-flow control chips, be particularly related to metal matrix and print the preparation method of high polymer micro-flow control chips, particularly be fit under the trace with the nucleic acid headed by the various sizes DNA part, amino acid, protein, organic molecules such as organic contaminant, metallic ion, the manufacture method of separatory micro-fluidic chip such as inorganic anion.
Background technology
Science and technology development requires analysis science with lower energy consumption, and easier method provides the information of test substance more quickly.The most representative research is the micro-total analysis system that utilizes the semiconductor microactuator process technology.Promptly on glass or piezoid, adopt optical etching technology to produce wide about 20-200 micron, the microchannel of about deeply 10-50 micron.Integrated chemical reaction on these passages, cellular incubation, " lab-on-a-chip " of experimental implementation processes such as separation detection, it is to be subjected to the concern in the world most as chip of future generation after the DNA chip.The report of micro-fluidic chip that is applied to compartment analysis at present is a lot, all is with glass-chip or quartz chip basically.It is strong that these materials have an optical transparence, advantage such as firm, but matter is crisp frangible, and the bonding of channel chip and cover plate need will be used severe corrosive acid in the passage corrosion process, the cost of manufacture height at the high temperature about 600 degree, poor reproducibility is difficult to carry out large-scale production.The exploitation of macromolecule chip has following sharp point: the pliability that macromolecule is good, ductility, good insulation performance, the chip that is fit to various flute profiles, manufacture craft is simple, material price is cheap, material modification is easy, is convenient to integrated other devices, is suitable for producing in batches and automation mechanized operation, can reduce cost, be specially adapted to the use of disposable chip.
At present the superpolymer chip of report be manufactured with following several method:
(1) DEEMO (Deep Etching, Electroplating, Molding) technology: earlier make a negative plate with the method for making of silicon or glass-chip or in spin coating on the silicon chip of photoresist, make the motherboard of a nickel by electrochemical plating, utilize this motherboard to make daughter board again, utilize this daughter board to make mould at last again, make many superpolymer chips with the method for injection moulding.(J.Elders, H.V.Jansen, M.Elwenspoek, W.Ehrfeld, DEEMO:a new technology for the fabrication ofmicrostructures, Proc.MEMS 95, Amsterdam 1995,238-244.McCormick R.M., Neison R.J, Goretty Alonso-Amigo M, Benvegnu D.J.Hooper H.H.Microchannel electrophoreticseparations of DNA in injection-molded plastic substrates.Anal.Chem.., 1997,69,2626-2630.US 20020056639A1) result shows the relative standard deviation of each time between separating less than 1%, the error at measurment between the different chips is 2-3%.
(2) method of tinsel die (hot wire impriting method) is made polymer chip.(Locascio, L.E, Perso, C.E.Cheng, S.L.J.Chromatogr., A, 1999,857,275-284.Martynova, L, Locascio L.E., Gaitan, M., Kramer, G.W., Christensen, R.G., MacCrehan, W.A., Fabrication of plastic microfluid channels by imprintingmethods, Anal.Chem.., 1997,69,4783-4789.) will be about 20 centimetres, diameter is that the two ends of the Ni-Cr alloy silk of 13-25 micron are fixed on the metal bow, makes it to tighten, and is placed on 1.6 millimeters PMMA sheets, add wave carrier piece up and down, with two aluminium blocks wave carrier piece is covered fully then, clamp aluminium block, put into stove, 105 degree heating 10 minutes, took out the cooling back.But the result shows that the deviation of this method is bigger, and the maximum deviation of theoretical value and actual value is 42%, and heat rose and makes notch that distortion take place when reason was bonding.
(3) make the superpolymer chip with the method for silicon negative film coining.(Martynova, L, Locascio L.E., Gaitan, M., Kramer, G.W., Christensen, R.G., MacCrehan, W.A., Fabrication of plastic microfluid channelsby imprinting methods, Anal.Chem., 1997,69,4783-4789.) the silicon negative film is placed between two smooth aluminium flakes, between silicon chip and last aluminium flake, put into the PMMA sheet, clamp equally then, be heated to 135 degree, 5 minutes.Cooling is taken out.The actual value of the chip surface width that the method makes and the relative error between the theoretical value are 13%, and degree of depth relative error is 2%.And the silicon slide is fragile.
(4) laser ablation legal system polymer chip is with high-intensity laser directive such as PMMA from the mask, tygon, and superpolymer such as polycarbonate, moment is ablated the ad-hoc location of superpolymer sheet, forms required shape.The groove that this method is made is vertical, rule, error is little, have electroosmotic flow and electroosmotic flow with adding field intensity become linear dependence.(Roberts M A, Rossier J S, Bercier P, Girault H.UV lasermachined polymaer substrates for the development ofmicrodiagnostic system, Anal.Chem., 1997,69,2035-2042.) the special instrument of the method needs, the cost of manufacture height.
(5) application of Japanese RIKEN patent--the spy opens among the 2000-039420 " resin chip " and has proposed disposable macromolecule chip production method, be on glass or silicon chip, to coat the film that negative photoresist SU-8 obtains 20 micron thickness, then mask is transferred on the photoresist and under UV-irradiation, exposed, in developer solution, develop then and obtain negative plate, again the pre-polymerization zoarium of silicon rubber PDMS is poured into that polymerization obtains microchip on the negative plate.It is very simple that the method is made a chip, but the photoresist on the negative plate comes off easily, is not suitable for producing in batches, and the method prepares chip and need consume a large amount of photoresists, can improve cost of manufacture.
The inventor of present patent application once attempted direct-on-line polymerization PMMA on the silicon negative film, but cooled off when taking off PMMA after polymerization, because unbalance stress is easy to the silicon negative film be broken into pieces troublesome poeration.
Summary of the invention
The objective of the invention is to propose a kind of simple low cost preparation method of high polymer micro-flow control chips,, on sheet metal, coat photoresist based on Micrometer-Nanometer Processing Technology, by exposure, develop, the step of etching obtains the negative plate of metal, is used for the preparation of high polymer micro-flow control chips.
The preparation method of the high polymer micro-flow control chips that the present invention proposes comprises the making of cover plate and substrate, and described method is:
(1) through hole on the cover plate is made (as shown in Figure 1):
(a) (metal column of the surface finish of Φ=1-3mm) as stainless steel column, is made the superpolymer cover plate that has liquid pool by online polymerization, injection moulding or hot padding method, and is stand-by to place appropriate size on the ad-hoc location on sheet metal or the glass plate.
Or
(b) the superpolymer cover plate for preparing is carried out mechanical punching or laser boring, stand-by.
(2) convex template in microchannel is the making (shown in Fig. 2-(a-e)) of the negative plate of metal:
On the sheet metal of clean light, coat photoresist, preliminary drying 1-30 minute, after the mask plate that will have a microchannel network pattern is placed on the photoresist, under UV-irradiation, expose, in developer solution, develop then, on sheet metal, form microchannel pattern; Corrode in corrosive liquid, behind the microchannel network of formation convex, remove the photoresist that covers on the network, water is rinsed well, obtains the negative plate of metal, dry for standby.
(3) method for making of high polymer micro-flow control chips substrate:
A. online polymerization (shown in Fig. 2-f):
In the performed polymer of polymer monomer, preliminary polymerization or the polycondensation of new distillation, add initiating agent, addition is the 0.01-0.5% of the performed polymer weight of polymer monomer, preliminary polymerization or polycondensation, simultaneously can add suitable additives as required, as plastifier or/and release agent etc., wherein the addition of plastifier is the 2wt%～10wt% of the performed polymer of new polymer monomer, preliminary polymerization or polycondensation of distilling, and the addition of release agent is the 1wt%～2wt% of the performed polymer of new polymer monomer, preliminary polymerization or polycondensation of distilling; Pre-polymerization is incorporated into certain viscosity (after 70～100Pa.s) in 75 ℃～90 ℃, be cooled to rapidly between 5 ℃～25 ℃, about vacuum outgas half an hour under 0.06～0.09Mpa pressure, be poured on the negative plate of metal of step (2), carried out cold polymerization 10～24 hours at 30 ℃～60 ℃ lower seals, slowly be warmed up to 90 ℃～130 ℃ then and carried out pyroprocessing 1～3 hour, slowly be cooled to 40 ℃ of bottom knockouts, obtain the high polymer micro-flow control chips substrate.
Or
B hot padding method:
Commercially available superpolymer plate level is placed on the negative plate of metal of step (2), clamp with thicker smooth smooth sheet metal respectively in the outside at negative plate of metal and superpolymer plate, as aluminium sheet or mirror face stainless steel plate etc., form a system, putting into pressing machine pressurizes, keep-up pressure more than 15Mpa, then system being put into heating furnace heats, the glass temperature of a little higher than superpolymer of control temperature, stop after 5～10 minutes, stop heating, open mould after being cooled to below 60 ℃ with furnace temperature and take out the moulding superpolymer, make the high polymer micro-flow control chips substrate.
Or
The C injection moulding:
The machine barrel of injection (mo(u)lding) machine will be put into behind the commercially available superpolymer drying and dehydrating, the rising barrel zone temperature is to the melt temperature of superpolymer, make superpolymer be molten condition, then with certain injection pressure and injection speed, the superpolymer vasopressing injection is born on the plate to the metal of closed step (2), the negative plate of metal this moment keeps proper temperature at 40 ℃～100 ℃, after keeping temperature and pressure a period of time (a few second), take out moulding superpolymer sheet after naturally cooling to room temperature, for bigger internal stress in the superpolymer sheet of eliminating injection mo(u)lding, in the air blast electrically heated drying cabinet, the superpolymer sheet is carried out heat treated, temperature is 60 ℃～85 ℃ after several hours, slowly cool to room temperature just makes the high polymer micro-flow control chips substrate.
(4) high polymer micro-flow control chips (shown in Fig. 2-g):
With the substrate of the cover plate of step (1) and step (3) bonding 5 minutes under softening point temperature, obtain high polymer micro-flow control chips.
The thickness of described high polymer micro-flow control chips substrate is 1-3mm.
Superpolymer by bulk polymerization all is fit to take online polymerization to make high polymer micro-flow control chips, typical case's superpolymer kind has polyacrylic acid low-carbon ester such as poly dimethyl methyl acrylate (PMMA), organic siliconresin such as dimethyl silicone polymer (PDMS), polystyrene (PS) resin, polythylene resin such as Polyvinylchloride (PVC) or isobutane tygon (TPS), phenolics, epoxy resin, unsaturated polyester resin, polyurethane, the polycaprolactam of base catalysis or any multipolymer between them, as the multipolymer (MAS) of methyl methacrylate and polystyrene, methyl methacrylate and styrol copolymer (SAN) etc.
Described initiating agent generally adopts per-compound, azo compound or their mutual composite initiators of forming that mixes, as benzoyl peroxide, dilauroyl peroxide, peroxide benzoate, di-isopropyl peroxydicarbonate, azoisobutyronitrile or ABVN etc.
The plastifier of described online polymerization has phthalate such as repefral, diethyl phthalate, dipropyl phthalate or dibutyl phthalate etc.; Also can adopt phenyl alkylsulf, polyol ester class or polyesters and phthalate and usefulness.
In order to improve stripping result, can add some release agents such as silicone oil, stearic acid, paraffin, glycerine or vaseline etc.
The described thermal plasticity high polymer resin that is fit to online polymerization forming all is fit to the hot padding method, polycarbonate resin such as diallyl diglycol carbonates (CR-39) or cellulosics also are fit to online polymerization, cellulosics such as cellulose acetate or cellulose nitrate in addition.
Described thermal plasticity high polymer resin and multipolymer thereof such as polymethylmethacrylate, polycarbonate or polystyrene etc. all are fit to injection moulding.
Sheet metal comprises titanium plate, corrosion resistant plate, mirror board or is coated with the sheet metal of films such as copper, nickel, zinc or chromium.
Photoresist can be the RZJ-390 of the auspicious red company in BP-213, the Suzhou of positive photoresist such as Beijing Inst. of Chemical Reagent production or JL-SR1000, Microchem.Corp (Newton, SU-8 MA) etc. of negative photoresist such as Beijing Jia Longtai development in science and technology company limited.
The time that dry by the fire preliminary drying before and after the exposure and back and temperature are according to the character of photoresist and different.Developer can make supporting with photoresist developer or use 0.1-0.5wt%NaOH or NaCO according to the character of photoresist
3Solution was at 15-50 ℃ of development 5-30 minute.Corrosive liquid acidic oxidation agent, as the acidic aqueous solution of ammonium persulfate, sodium peroxydisulfate, boron chloride, ferric trichloride, chlorine or their any mixture etc., in order to improve corrosive effect, increase the smooth finish of corrosion surface, can suitably add some doped quaternary ammonium salt corrosion inhibiter such as weight ratio and be 0.1～1.0% cetyl trimethyl ammonium bromide etc.
The superpolymer chip manufacture method of reporting in the present invention and the document is compared, and it is cheap to have a negative sheet material material, and method for making is simple, favorable reproducibility, and material is hard, and advantages such as long service life can reduce production costs, and are easy to produce in batches.
Description of drawings
Fig. 1. the front view (FV) of superpolymer cover plate;
Fig. 2. the making of the negative plate of metal and the manufacturing process of high polymer micro-flow control chips.
1. cover plate 2. sample cells 1 3. sample cells 2 4. damping fluids 1 5. damping fluids 2
Embodiment
Embodiment 1:
(1) making of cover plate: with diameter is 2mm, highly be positioned on the ad-hoc location of bright and clean glass for the stainless steel column of 2mm, with the potpourri of PMMA monomer and benzoyl peroxide (weight ratio is 1000: 5) through prepolymerization, the degassing after, it is on glass to transfer to this, get rid of clean air and sealing, after the high temperature polymerization (90 ℃) through 24 hours cold polymerizations (45 ℃) and two hours, take out lift-off stencil at 40 ℃.(2) the negative plate of metal is made: the titanium plate water is rinsed well, is placed in the lotion one day, removes surface and oil contaminant, and is clean with distilled water flushing, oven dry.Whirl coating on titanium plate (BP-213) and preliminary drying, the preliminary drying time is 5 minutes, temperature is 90 degree.The mask plate that will have the microchannel network is placed on the photoresist, and ultraviolet photoetching 1 minute uses the NaOH solution of 0.5wt% to develop 10 minutes in 15 ℃ then, removes the photoresist beyond the network of microchannel on the titanium plate, and the heat baking is 1 hour under 120 degree.With ferric trichloride acid etching solution room temperature etching titanium plate 30 minutes, ferric trichloride content was 35wt% in the corrosive liquid; Thereby form the negative plate of the titanium that has convex microchannel figure, the degree of depth of microchannel is 20 microns, and width is 90 microns.
(3) contain the making of microchannel POLYMER PMMA substrate: the size of the burr that the negative plate of the titanium of step (2) is produced is corresponding to the size of microchip split tunnel, PMMA monomer and benzoyl peroxide are mixing in 1000: 5 with weight ratio, after pre-polymerization is incorporated into viscosity and is 80Pa.s in 80 ℃, be cooled to 25 ℃ rapidly, about vacuum outgas half an hour under the 0.06Mpa pressure, be poured on the negative plate of titanium of step (2), carried out cold polymerization 24 hours at 45 ℃ of lower seals, slowly be warmed up to 90 ℃ then and carried out pyroprocessing 2 hours, slowly be cooled to 40 ℃ of bottom knockouts, obtain the high polymer micro-flow control chips substrate.
(4) cover plate and substrate are closed up, and, make its bonding 120 degree heating 10 minutes.Obtain long 5 centimetres of PMMA chip, wide 5 centimetres, thick 4 millimeters, split tunnel length is 3 centimetres, 90 microns of channel widths, and channel depth is 20 microns a PMMA chip.
Embodiment 2:
(1) the negative plate of metal is made: the corrosion resistant plate water is rinsed well, is placed in the lotion one day, removes surface and oil contaminant, and is clean with distilled water flushing, oven dry.Whirl coating on corrosion resistant plate (RZJ-390) and preliminary drying, the preliminary drying time is 1.5 minutes, temperature is 100 degree.The mask plate that will have the microchannel network pattern is placed on the photoresist, 20 seconds of ultraviolet photoetching, then sheet metal is put into the NaOH solution of 0.4wt%, 25 ℃ were developed 5 minutes, remove the photoresist beyond the network of microchannel on the corrosion resistant plate, heat is dried by the fire half an hour under 130 degree.50 ℃ of etching corrosion resistant plates 10 minutes, ferric trichloride content was 25wt% in the corrosive liquid, contains the doped quaternary ammonium salt corrosion inhibiter of 0.2wt% in the corrosive liquid with the ferric trichloride acid etching solution.Thereby form the negative plate of the stainless steel that has convex microchannel figure.The degree of depth of microchannel is about 20 microns, and width is 100 microns.
(2) contain the making of microchannel POLYMER PMMA substrate: the size of the burr that the negative plate of the stainless steel of step (1) is produced is corresponding to the size of microchip split tunnel, PMMA monomer and azoisobutyronitrile are mixing in 1000: 0.6 with weight ratio, after pre-polymerization is incorporated into viscosity and is 70Pa.s in 75 ℃, be cooled to 20 ℃ rapidly, about vacuum outgas half an hour under the 0.09Mpa pressure, be poured on the negative plate of stainless steel of step (1), carried out cold polymerization 15 hours at 45 ℃ of lower seals, slowly be warmed up to 90 ℃ then and carried out pyroprocessing 2 hours, slowly be cooled to 40 ℃ of bottom knockouts, obtain the high polymer micro-flow control chips substrate.
(3) making of cover plate: with diameter is 2mm, highly be positioned on the ad-hoc location of bright and clean corrosion resistant plate for the stainless steel column of 2mm, with PMMA monomer and azoisobutyronitrile weight ratio is that 1000: 0.6 ratios are mixed, potpourri is through after prepolymerization, outgasing, transfer on this corrosion resistant plate, get rid of clean air and sealing, after the high temperature polymerization (90 ℃) through 15 hours cold polymerizations (45 ℃) and two hours, take out lift-off stencil at 40 ℃.
(4) cover plate of step (3) and the substrate of step (1) are closed up, and, make its bonding 120 degree heating 10 minutes.Obtain 100 microns of PMMA chip channel width, channel depth is 20 microns a PMMA chip.
Embodiment 3:
(1) the negative plate of metal is made: the corrosion resistant plate water is rinsed well, is placed in the lotion one day, removes surface and oil contaminant, and is clean with distilled water flushing, oven dry.Take screen printing technology gluing JL-SR1000 and preliminary drying on corrosion resistant plate, the preliminary drying time is 30 minutes, and temperature is 80 degree.The mask plate that will have the microchannel network pattern is placed on the photoresist, in 20 seconds of ultraviolet photoetching, then sheet metal is put into the Na of 0.2wt%
2CO
3In the solution, 25 ℃ were developed 5 minutes, removed the photoresist beyond the network of microchannel on the corrosion resistant plate, and the heat baking is 15 minutes under 120 degree.50 ℃ of etching corrosion resistant plates 10 minutes, ferric trichloride content was 25wt% in the corrosive liquid, contains the doped quaternary ammonium salt corrosion inhibiter of 0.2wt% in the corrosive liquid with the ferric trichloride acid etching solution.Thereby form the negative plate of the stainless steel that has convex microchannel figure.The degree of depth of microchannel is about 20 microns, and width is 100 microns.
(2) contain the making of microchannel superpolymer polycarbonate substrate: the negative plate of metal with step (1) method is made, adopt the hot stamping compression moulding to make the micro-fluidic substrate of polycarbonate.Actual conditions is to live with the smooth smooth mirror face stainless steel plate holder of 5 millimeters thick respectively in the outside of negative plate of metal and polycarbonate plate, putting into pressing machine pressurizes, keep-up pressure more than 15Mpa, then system being put into heating furnace heats, after 150 degree stop 10 minutes, stop heating, open mould after being cooled to below 60 ℃ with furnace temperature and take out the moulding superpolymer, make polycarbonate micro-fluidic chip substrate.
(3) making of cover plate: buy thickness and be 2 millimeters POLYCARBONATE SHEET, boring is as the liquid bath of chip on ad-hoc location, and the aperture is 2 millimeters.
(4) substrate and cover plate thermal bonding: polycarbonate substrate and cover plate after using the deionized water ultrasonic cleaning close up substrate and cover plate, and thermal bonding is 10 minutes under 130 degree, obtains 100 microns of microchannel width, and channel depth is 20 microns a polycarbonate chip.
Embodiment 4:
(1) making of the negative plate of metal: use-case 2 methods are made the negative plate of metal.
(2) make PDMS microchannel substrate: on the negative plate ad-hoc location of metal, fix stainless steel column, post is high 2 millimeters, 2 millimeters of diameters, (Sylgard 184 with the monomer of PDMS and its hardening agent, Dow Cowing company) evenly is cast on the negative plate of metal after the mixing with 10: 1 (w/w), polymerization 4 hours under 65 degree, be cooled to room temperature after the demoulding get PDMS microchannel substrate, the relevant position has formed reservoir on the substrate.
(3) PDMS substrate and cover plate is bonding: after the PDMS substrate closes up with the PDMS cover plate of buying, utilize the viscosity of PDMS, need not heat directly bonding about 5 minutes after both sides clamp with glass sheet, obtain the PDMS micro-fluidic chip, channel width is 100 microns, and channel depth is 20 microns.
Embodiment 5:
With suspension polymerization to PMMA bead drying and dehydrating after put into the machine barrel of injection (mo(u)lding) machine, keep 200 ℃ of barrel zone temperatures, injection pressure 100Mpa, make the PMMA that is in molten condition in 10s, be expelled to (the negative plate of stainless steel adopts embodiment's 2) on the negative plate of closed stainless steel, the temperature of the negative plate of stainless steel this moment remains on 60 ℃, keep temperature and pressure after about 5 seconds, take out moulding superpolymer sheet after naturally cooling to room temperature, for bigger internal stress in the PMMA sheet of eliminating injection mo(u)lding, in the air blast electrically heated drying cabinet PMMA sheet being heated to 80 ℃ handled after 4 hours, slowly cool to room temperature just makes PMMA micro-fluidic chip substrate.Cover plate adopts embodiment's 2, with substrate with cover plate closes up and 105 ℃ of following thermal bondings 8 minutes, obtain the PMMA micro-fluidic chip.
Embodiment 6
(1) the negative plate of metal is made: use-case 2 methods are made the negative plate of stainless steel.
(2) contain the making of microchannel POLYMER PMMA substrate: the size of the burr that the negative plate of the stainless steel of step (1) is produced is corresponding to the size of microchip split tunnel, PMMA monomer and azoisobutyronitrile and stearic acid release agent are mixing in 1000: 0.6: 6 with weight ratio, after pre-polymerization is incorporated into viscosity and is 70Pa.s in 75 ℃, be cooled to 20 ℃ rapidly, about vacuum outgas half an hour under the 0.09Mpa pressure, be poured on the negative plate of stainless steel of step (1), carried out cold polymerization 15 hours at 45 ℃ of lower seals, slowly be warmed up to 90 ℃ then and carried out pyroprocessing 2 hours, slowly be cooled to 40 ℃ of bottom knockouts, obtain the high polymer micro-flow control chips substrate.
(3) making of cover plate: with diameter is 2mm, highly be positioned on the ad-hoc location of bright and clean corrosion resistant plate for the stainless steel column of 2mm, is 1000: 0.6: 6 with PMMA monomer, azoisobutyronitrile, stearic acid release agent and plasticizer phthalic acid dibutyl ester with weight ratio: 40 ratio is mixed, potpourri is through after prepolymerization, outgasing, transfer on this corrosion resistant plate, get rid of clean air and sealing, after the high temperature polymerization (90 ℃) through 15 hours cold polymerizations (45 ℃) and two hours, take out lift-off stencil at 40 ℃.
(4) cover plate and substrate are closed up, and, make its bonding 115 degree heating 10 minutes.Obtain the PMMA chip, channel width is 90 microns, and channel depth is 20 microns.
Claims (13)
1. the preparation method of a high polymer micro-flow control chips comprises the making of cover plate and substrate, it is characterized in that: described method is:
(1) through hole on the cover plate is made:
(a) metal column of placement surface polishing on the ad-hoc location on sheet metal or the glass plate, diameter is 1-3mm, makes the superpolymer cover plate that has liquid pool by online polymerization, injection moulding or hot padding method, and is stand-by;
Or
(b) the superpolymer cover plate for preparing is carried out mechanical punching or laser boring, stand-by;
(2) convex template in microchannel is the making of the negative plate of metal:
On sheet metal, coat photoresist, preliminary drying 1-30 minute, after the mask plate that will have a microchannel network pattern is placed on the photoresist, under UV-irradiation, expose, in developer solution, develop then, on sheet metal, form microchannel pattern; Corrode in corrosive liquid, behind the formation convex microchannel, remove the photoresist that covers on the microchannel, water is rinsed well, obtains the negative plate of metal, dry for standby;
(3) method for making of high polymer micro-flow control chips substrate:
A. online polymerization:
Polymer monomer to new distillation, in the performed polymer of preliminary polymerization or polycondensation, add initiating agent, addition is a polymer monomer, the 0.01-0.5% of the performed polymer weight of preliminary polymerization or polycondensation, vacuumizing is 0.04～0.1MPa, after pre-polymerization is incorporated into viscosity and is 70～100Pa.s in 75 ℃～90 ℃, be cooled to rapidly between 5 ℃～25 ℃, vacuum outgas under 0.06～0.09Mpa pressure, be poured on the negative plate of metal of step (2), carry out cold polymerization at 30 ℃～60 ℃ lower seals, slowly be warmed up to 90 ℃～130 ℃ then and carry out pyroprocessing, slowly cooling and demolding obtains the high polymer micro-flow control chips substrate;
Or
B hot padding method:
The superpolymer plate level is placed on the negative plate of metal of step (2), clamp with smooth smooth sheet metal respectively in the outside at negative plate of metal and superpolymer plate, form a system, pressurization keep-ups pressure more than 15Mpa, then system is heated, the control temperature is higher than the glass temperature of superpolymer, stops after 5～10 minutes, stops heating, open mould after the cooling and take out the moulding superpolymer, make the high polymer micro-flow control chips substrate;
Or
The C injection moulding:
The machine barrel of injection (mo(u)lding) machine will be put into behind the superpolymer drying and dehydrating, the rising barrel zone temperature is to the melt temperature of superpolymer, make superpolymer be molten condition, pressurizeing then is expelled to superpolymer on the negative plate of metal of closed step (2), and the negative plate of metal this moment maintains the temperature at 40 ℃～100 ℃, after several seconds, take out moulding superpolymer sheet after naturally cooling to room temperature, the superpolymer sheet is carried out heat treated, temperature is 60 ℃～85 ℃, slowly cool to room temperature just makes the high polymer micro-flow control chips substrate;
(4) high polymer micro-flow control chips:
With the cover plate of step (1) and substrate bonding under softening point temperature of step (3), obtain high polymer micro-flow control chips;
The thickness of described high polymer micro-flow control chips substrate is 1-3mm.
2. the method for claim 1, it is characterized in that: further contain plastifier or/and release agent in the described online polymerization, wherein the addition of plastifier is the 2wt%～10wt% of the performed polymer of new polymer monomer, preliminary polymerization or polycondensation of distilling, and the addition of release agent is the 1wt%～2wt% of the performed polymer of new polymer monomer, preliminary polymerization or polycondensation of distilling.
3. the method for claim 1, it is characterized in that: the time that cold polymerization is carried out in described sealing is 10～48 hours, and the pyroprocessing time is 1～3 hour.
4. the method for claim 1 is characterized in that:
The superpolymer of described online polymerization is the polycaprolactam of polyacrylic acid low-carbon ester, organic siliconresin, polystyrene resin, polythylene resin, phenolics, epoxy resin, unsaturated polyester resin, polyurethane, base catalysis or any multipolymer between them;
The polymeric resin of described hot padding method is the polycaprolactam of polyacrylic acid low-carbon ester, organic siliconresin, polystyrene resin, Corvic, phenolics, epoxy resin, unsaturated polyester resin, polyurethane, base catalysis or any multipolymer between them; Or polycarbonate resin, or cellulosics;
The polymeric resin of described injection moulding and multipolymer thereof are polymethylmethacrylate, polycarbonate or polystyrene.
5. the method for claim 1 is characterized in that: described initiating agent is that per-compound, azo compound or their are mixed the composite initiator of forming mutually.
6. method as claimed in claim 5 is characterized in that: described per-compound is benzoyl peroxide, dilauroyl peroxide, peroxide benzoate or di-isopropyl peroxydicarbonate; Azo compound is azoisobutyronitrile or ABVN.
7. method as claimed in claim 2 is characterized in that: described plastifier is phthalate, phenyl alkylsulf, polyol ester class or polyesters and phthalate and uses.
8. method as claimed in claim 7 is characterized in that: described phthalate is repefral, diethyl phthalate, dipropyl phthalate or dibutyl phthalate.
9. method as claimed in claim 2 is characterized in that: described release agent is silicone oil, stearic acid, paraffin, glycerine or vaseline.
10. method as claimed in claim 4 is characterized in that: described polycarbonate resin is the diallyl diglycol carbonates; Cellulosics are cellulose acetate or cellulose nitrate.
11. method as claimed in claim 10 is characterized in that: described sheet metal comprises titanium plate, corrosion resistant plate or is coated with the sheet metal of copper, nickel, zinc or chromium thin film.
12. the method for claim 1 is characterized in that: described photoresist is BP-213, RZJ-390, JL-SR1000 or SU-8.
13. the method for claim 1 is characterized in that: described corrosive liquid is the acidic aqueous solution of ammonium persulfate, sodium peroxydisulfate, boron chloride, ferric trichloride, chlorine or their any mixture.
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