CN104190482A - Method for manufacturing glass microfluid device by using photosensitive dry film as anti-corrosion mask - Google Patents
Method for manufacturing glass microfluid device by using photosensitive dry film as anti-corrosion mask Download PDFInfo
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- CN104190482A CN104190482A CN201410416124.8A CN201410416124A CN104190482A CN 104190482 A CN104190482 A CN 104190482A CN 201410416124 A CN201410416124 A CN 201410416124A CN 104190482 A CN104190482 A CN 104190482A
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Abstract
The invention belongs to the field of microfluid device manufacturing and provides a method for manufacturing a glass microfluid device by using a photosensitive dry film as an anti-corrosion mask. The method comprises the following steps: (1) manufacturing a photolithographic mask; (2) cleaning a glass substrate; (3) manufacturing a photosensitive glass plate; (4) performing exposure; (5) performing development; (6) etching a microfluid channel; and (7) performing bonding to obtain the microfluid device. According to the method, the manufacturing process of the glass microfluid device is simplified, the manufacturing efficiency is enhanced, the manufacturing cost of the glass microfluid device is lowered greatly and a new approach is provided for the large-batch production of the glass microfluid device.
Description
Technical field
The invention belongs to microfluidic device and make field, particularly a kind ofly take the method that photosensitive dry film makes glass microfluidic devices as etching mask.
Background technology
Be called as the micro-fluidic technologies of Lab-on-a-chip (LoC) since coming out the nineties in 20th century, become gradually the most effective fluid operated means under micro-meter scale.Because micro-fluidic technologies can be carried out flexible combination and large-scale integrated by multiple monotechnics on several square centimeters of even less microfluidic platforms, there is laboratory sample consumption few, the feature such as short consuming time, has obtained research widely in the field such as biological, chemical.But, the complex manufacturing technology of most microfluidic device, manufacturing conditions is harsh, needs with expensive experiment material and equipment in manufacturing process, and this has seriously hindered development and the application of micro-fluidic technologies.
In prior art, for making the material of microfluidic device, mainly contain organic polymer dimethyl silicone polymer (PDMS), silicon and glass.It is high that the PDMS method that soft lithographic technique is made microfluidic device as base material adopts of take has channel size control accuracy, can produce the features such as complicated shape passage and be used in a large number, but the complex manufacturing process of PDMS microfluidic device, need expensive instrument and equipment, in addition PDMS is under high pressure yielding, poor chemical stability, surface modification difficulty, causes the application of PDMS microfluidic device to be subject to certain restriction.Silicon has good chemical inertness and heat endurance, use the method for chemical etching can copy accurately two dimension or three-dimensional complex passages, but silicon on the high side, light tight, intensity is low, these drawbacks limit the uses of silicon materials in microfluid system.
Than PDMS and silicon, glass material has good electric osmose characteristic, good optical characteristics and chemical inertness, and mechanical strength is high, high temperature resistant, easily modification of surface, cheap, these features make glass material be widely used in making microfluidic device.The method of making at present glass microfluidic devices has capillary glass tube splicing (to see A.Utada, E.Lorenceau, D.Link, P.Kaplan, H.Stone and D.Weitz, Science, 2005, 308, 537-541.), slide and cover glass splicing (are shown in N.N.Deng, Z.J.Meng, R.Xie, X.J.Ju, C.L.Mou, W.Wang and L.Y.Chu, Lab on a Chip, 2011, 11, 3963-3969.), the wet etching of glass (is shown in C.H.Lin, G.B.Lee, Y.H.Lin and G.L.Chang, Journal of micromechanics and microengineering, 2001, 11, 726-732.) etc.Wherein, capillary glass tube splicing method and slide and cover glass splicing method are fairly simple, do not need special material and facility, in Routine Test Lab, can make.Yet these two kinds of methods all need consummate skill hand-manipulated, can not accurately control the size of microfluidic channel, and the make efficiency of device is extremely low, cannot carry out mass making.With wet etching, in conjunction with the method for photoetching making microfluidic device, can carry out flexible design to channel shape, channel size precision is higher, to manual dependence is low, (sees and thank to hypo, Fu Xin, Yang Huayong, journal of Zhejiang university: engineering version, 2007,41,560-563.), but the method has the following disadvantages: must be at substrate surface depositing metal layers or spin coating photoresist as etching mask before (1) wet etching, and the complicated process of preparation of this etching mask, length consuming time, adopting the method to make a glass microfluidic devices needs approximately 5～6h consuming time; (2) need in ultra-clean working environment, adopt the instrument and equipment that metal sputtering instrument, litho machine, spin coater etc. are expensive, must use the high materials of price such as liquid photoresist, sputter precious metal, production cost is very high.At present according to the complex situations of microfluidic channel from hundreds of units to tens thousand of units not etc., fancy price has seriously hindered the large-scale application of micro-fluidic technologies to the price of domestic commercially available glass microfluidic devices.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of method of photosensitive dry film as etching mask making glass microfluidic devices of take is provided, the method can be simplified manufacturing process, the raising make efficiency of glass microfluidic devices, significantly reduce the cost of manufacture of glass microfluidic devices, for the mass production of glass microfluidic devices provides a kind of new approach.
Provided by the inventionly take photosensitive dry film and be that etching mask makes the method for glass microfluidic devices, step is as follows:
(1) make photo etched mask
The microfluidic channel figure that uses mapping software design microfluidic device forms photo etched mask with laser photocomposing machine by the microfluidic channel graphic printing designing on transparent film;
(2) clean glass substrate
With using again washed with de-ionized water glass substrate after acetone, ethanol cleaning glass substrate, to remove organic pollution and the solid particle of glass baseplate surface, then the glass substrate after cleaning is dried to its surface anhydrous respectively;
(3) make photosensitive glass plate
Photosensitive dry film is cut to the shape and size of the described glass substrate of step (2), throw off the polyethylene film of photosensitive dry film and adopt wet film coating method that photosensitive dry film is attached on glass substrate, photoresist layer in described photosensitive dry film contacts with glass substrate, then uses laminator at 90～95 ℃ of moulding one-tenth photosensitive glass plates of mistake;
(4) exposure
Step (3) gained photosensitive glass plate is placed in to uv-exposure case, described photosensitive glass plate is pasted with the placement that faces up of photosensitive dry film, then the photo etched mask of step (1) being made covers on the photosensitive dry film of photosensitive glass plate and compresses, described photo etched mask print have carbon dust facing to photosensitive dry film, continue after by uv-exposure, the microfluidic channel figure on photo etched mask is transferred on photosensitive dry film, after end exposure, take off photo etched mask, photosensitive glass plate after exposure is taken out, lucifuge places 10min at least so that the light polymers complete reaction in the photosensitive dry film after exposure,
(5) develop
Polyester film on photosensitive glass plate photosensitive dry film after the exposure of removing step (4) gained, then use developing liquid developing, developing time is 0.5～5min, continue after with the microfluidic channel figure on microscopic examination photosensitive dry film, if it is clear to remain the blur margin of photosensitive dry film or microfluidic channel in the microfluidic channel in figure, repeat aforementioned development operation, until the photosensitive dry film at the microfluidic channel inside in figure and microfluidic channel edge is completely removed, after development, the dry water of removing between photosensitive dry film and glass substrate;
Described developer solution is by Na
2cO
3formulated with deionized water, in developer solution, Na
2cO
3with the mass ratio of deionized water be 1:(50～100);
(6) etching microfluidic channel
It is etching microfluidic channel in the etching liquid of 20～40 ℃ that the glass substrate that is pasted with photosensitive dry film after step (5) is developed is immersed in temperature, in etching process, etching liquid is carried out to disturbance, etch period is no more than the tolerance time of described photosensitive dry film in etching liquid, after etching finishes, the glass substrate that is pasted with photosensitive dry film is taken out, be placed in deionized water washing and remove photosensitive dry film and the etching liquid on glass substrate, obtain being etched with the glass substrate of microfluidic channel;
The compound method of described etching liquid is as follows: by the NH of 40wt%
4the HF aqueous solution of the F aqueous solution and 40wt% forms buffer oxide etching liquid, then uses deionized water dilution buffer oxide etch liquid, then to the concentrated hydrochloric acid that adds 37.5wt% in the buffer oxide etching liquid after dilution, mixes and obtain etching liquid; Described NH
4the volume ratio of the F aqueous solution and the HF aqueous solution is (6～7): 1, and the volume ratio of described deionized water and buffer oxide etching liquid is (1～7): 1, the buffer oxide etching liquid after described dilution and the volume ratio of concentrated hydrochloric acid are 10:(1～3);
(7) bonding microfluidic device
Sheet glass is covered to step (6) gained and be etched with on the glass substrate of microfluidic channel, use ultraviolet light polymerization glue by described sheet glass and glass substrate bonding, form microfluidic device; The entrance and exit corresponding section of described sheet glass and microfluidic channel is provided with through hole.
In step in said method (1), the mapping software of design microfluidic channel figure can be AutoCAD, CorelDRAW or Protel99SE.
In the step of said method (2), the complete glass substrate of cleaning is dried to its surface at 60～150 ℃ anhydrous.
In the step of said method (3), after photosensitive dry film is attached on glass plate, use laminator to cross and mould 2～4 times, after crossing and having moulded, preferably photosensitive glass plate is cooled to room temperature and carries out again next step operation.
The step of said method (3) is preferably carried out under yellow fluorescent lamp, and the operation before the exposure of step (4) medium ultraviolet is preferably carried out under yellow fluorescent lamp.
In the step of said method (4), the time of uv-exposure is relevant with the performance of uv-exposure case, and the microfluidic channel figure while controlling uv-exposure on chien shih photo etched mask is transferred on photosensitive dry film completely.
In the step of said method (5), the temperature of controlling developer solution is 25～35 ℃.
In the step of said method (5), after development, at 60～100 ℃, be dried the water of removing between photosensitive dry film and glass substrate.
In the step of said method (6), the tolerance time of described photosensitive dry film in etching liquid refers to that photosensitive dry film starts to depart from the time that glass substrate departs from etching process, and etch period is preferably 1～30min.
In the step of said method (6), by stirring or by the mode of bubbler bubbling, etching liquid being carried out to disturbance.
In the step of said method (6), after etching finishes, the glass substrate that is pasted with photosensitive dry film is taken out, be placed in deionized water and remove photosensitive dry film and the etching liquid on glass substrate in the mode of Ultrasonic Cleaning.
If only include a microfluidic channel on the step of said method (6) gained glass substrate, the shape of the sheet glass of the microfluidic channel of the described glass substrate of step (7) top and size at least should cover the microfluidic channel on described glass substrate completely; If comprise a plurality of microfluidic channel on the step of said method (6) gained glass substrate, step (7) should first be divided into by described glass substrate the fritter that only comprises a microfluidic channel, the microfluidic channel on the pieces of glass substrate after cutting apart described in the shape of the described sheet glass of step (7) and size at least should cover completely.
In said method, the thickness of described glass substrate is at least 1mm.
Compared with prior art, the present invention has following beneficial effect:
1, the invention provides a kind of method of photosensitive dry film as etching mask making glass microfluidic devices of take, because the method is used photosensitive dry film as the etching mask of glass microfluidic devices wet etching, while making microfluidic device, adopt common laminator photosensitive dry film can be pasted and on glass substrate, form etching mask, spin coating liquid photoresist in existing etching mask preparation process and the troublesome operation of depositing metal layers have been avoided, therefore, the method of the invention has been simplified the manufacturing process of glass microfluidic devices, reduced its manufacture difficulty simultaneously.
2, because the method for the invention is very low to the requirement of environment, making apparatus in the process of making glass microfluidic devices, adopt conventional equipment can realize the making of glass microfluidic devices, without using ultra-clean working environment, more without using the instrument and equipment that metal sputtering instrument, litho machine, spin coater etc. are expensive, and the photosensitive dry film that the method for the invention is used is very cheap with respect to liquid photoresist and sputter precious metal price, so the method for the invention has greatly reduced the cost of manufacture of glass microfluidic devices.
3, the method for the invention can be attached on glass substrate in large area by photosensitive dry film is disposable when making glass microfluidic devices; then by wet etching by microfluidic channel figure mass be transferred on glass substrate and (see embodiment 6); this kind of production method can not only effectively reduce the Production Time of single glass microfluidic devices; enhance productivity, and be conducive to mass, the large-scale production of glass microfluidic devices.
4, the method for the invention can design flexibly to the channel shape of microfluidic device, the dimensional accuracy of the microfluidic channel that etching obtains is high, the microfluidic channel inner wall smooth of the glass microfluidic devices of making, residual without deposit seed, and the method for the invention is low to manual dependence, be easy to realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the structural representation of inventing the photosensitive dry film material using in described method, in figure, photoresist layer in the middle of the polyethylene of 1-photosensitive dry film inner surface (PE) film, 2-photosensitive dry film, the polyester of 3-photosensitive dry film outer surface (PET) film.
Fig. 2 is the schematic flow sheet that the described method of invention is made glass microfluidic devices, in figure, and the entrance of 4-photosensitive dry film, 5-photo etched mask, 6-microfluidic channel or outlet, 7-ultraviolet light polymerization glue.
Fig. 3 is the corrosion resistance test result to wet etching etching mask (photosensitive dry film) in embodiment 1, wherein, figure is a) the tolerance time curve of photosensitive dry film in the etching liquid of different temperatures, variable concentrations, figure b) be microfluidic channel on the glass substrate average etching rate curve in the etching liquid of different temperatures, variable concentrations, scheme c) be the maximum etching depth block diagram of microfluidic channel in the etching liquid of different temperatures, variable concentrations on glass substrate.
Fig. 4 is the cross-sectional scans Electronic Speculum figure of microfluidic channel on the glass substrate of etching different time in embodiment 2.
Fig. 5 is the width of microfluidic channel in embodiment 2 and the relation curve that the degree of depth changes with etch period.
Fig. 6 is the common microfluidic channel figure that uses AutoCAD Software for Design, a) is Y shape passage, is b) cross passage, is c) T shape passage, is d) diesis shape passage, e) is snakelike hybrid channel, f) is concentration gradient passage.
Fig. 7 is the optical microscope photograph of the microfluidic channel figure on the photosensitive dry film of photosensitive glass plate after developing in embodiment 3.
Fig. 8 be in embodiment 3 etching complete after the optical microscope photograph of microfluidic channel on glass substrate.
Fig. 9 is the photo of the glass microfluidic devices of embodiment 3 making.
Figure 10 is the array T shape microfluidic channel figure that uses AutoCAD Software for Design in embodiment 6.
The photo of the microfluidic channel after developing when Figure 11 is embodiment 6 batch making glass microfluidic devices on photosensitive dry film;
When Figure 12 is embodiment 6 batch making glass microfluidic devices etching complete after the photo of microfluidic channel on glass substrate;
Figure 13 is the photo of the glass microfluidic devices of embodiment 6 batch makings.
The specific embodiment
By the following examples and by reference to the accompanying drawings to take photosensitive dry film be that the method that etching mask is made glass microfluidic devices is described further to of the present invention.In following each embodiment, described transparent film is purchased from Dongguan City Yu Guan Electronic Science and Technology Co., Ltd.; The model of described photosensitive dry film is Etertec HT-115T, purchased from Changxing chemistry limited company; The thickness of the slide using in embodiment 1～5 is 1.1mm; The thickness of the soda-lime glass using in embodiment 6 is 2.1mm; The model of described laminator is KH-320C, purchased from Foochow Ke Hai Electronics Co., Ltd.; The model of described uv-exposure case is KVB30, buys from Taiwan gold electronics limited company.
Embodiment 1
In the present embodiment, make the schematic flow sheet of glass microfluidic devices and see Fig. 2, step is as follows:
(1) make photo etched mask
Use AutoCAD Software on Drawing linear microfluidic channel figure, the width place of microfluidic channel is 300 μ m.After microfluidic channel graphic designs completes, use the laser photocomposing machine that resolution ratio is 25400dpi that microfluidic channel graphic printing is formed to photo etched mask on transparent film, each photo etched mask is of a size of 20mm * 30mm.This step is made 12 photo etched masks altogether.
(2) clean glass substrate
The slide that is of a size of 25mm * 76mm of take is glass substrate (totally 12), with acetone, glass substrate is carried out ultrasonic cleaning 10min, then with ethanol, glass substrate carried out to ultrasonic cleaning 10min, continue after by deionized water, glass substrate is carried out to ultrasonic cleaning 10min, with organic pollution and the solid particle except glass baseplate surface, glass substrate after cleaning is put into vacuum drying chamber in 60 ℃ of dry 1h, and glass baseplate surface is anhydrous.
(3) make photosensitive glass plate
Photosensitive dry film is cut into 30mm * 80mm size (totally 12), first in glass substrate one end, drip deionized water, then open polyethylene (PE) film (seeing Fig. 1) of photosensitive dry film inner surface, be covered on one end of glass substrate, photoresist layer in described photosensitive dry film contacts with glass substrate, putting into laminator moulds 3 times 93 ℃ of mistakes again, form photosensitive glass plate, it is placed under room temperature (20 ℃) at least to 15min and make photosensitive glass plate be cooled to room temperature to carry out again next step operation.The operation of this step is all carried out under yellow fluorescent lamp.
(4) exposure
Under yellow fluorescent lamp, the photosensitive glass plate obtaining in step (3) is placed in to uv-exposure case, described photosensitive glass plate is pasted with the placement that faces up of photosensitive dry film, then the photo etched mask obtaining in step (1) is covered on the photosensitive dry film of photosensitive glass plate, photo etched mask print have carbon dust facing to photosensitive dry film, continue after vavuum pump is locked and opened to the vacuum clip in uv-exposure case, while being evacuated to photo etched mask pressed glass substrate, start exposure, time for exposure is 20s, microfluidic channel figure on photo etched mask is transferred on photosensitive dry film completely, close vavuum pump.After end exposure, take off photo etched mask, the photosensitive glass plate after exposure is taken out, in room temperature (20 ℃) lucifuge, place 15min so that the light polymers complete reaction in the photosensitive dry film after exposure.
(5) develop
Preparing developer liquid: by Na
2cO
3add deionized water for stirring evenly to form developer solution, Na
2cO
3with the mass ratio of deionized water be 1:70.
Polyester (PET) film on removing step (4) gained photosensitive glass plate photosensitive dry film, then with developer solution, the photosensitive dry film after exposing is sprayed to development, the temperature of developer solution is 30 ℃, developing time is 2min, continue after with microscopic examination, be transferred to the microfluidic channel figure on photosensitive dry film, find that the microfluidic channel pattern edge after developing is clear, the appearance such as nothing left glue burr, glass substrate after developing is placed on the drying glue platform of 65 ℃ and toasts 1.5h to remove the water between photosensitive dry film and glass substrate, thereby increase the adhesion property of photosensitive dry film etching mask and glass substrate.
(6) wet etching microfluidic channel
Preparation etching liquid: by the NH of 40wt%
4the HF aqueous solution of the F aqueous solution and 40wt% is that 7:1 is mixed to form buffer oxide etching liquid (Buffered oxide etchant according to volume ratio, be called for short BOE), get 4 parts of BOE, by deionized water, according to the volume ratio of deionized water and BOE, be 0:1 respectively, 1:1, 3:1, the ratio of 7:1 is diluted, in the BOE after dilution, add the concentrated hydrochloric acid of 37.5wt% again, BOE after described dilution and the volume ratio of concentrated hydrochloric acid are 10:2, mix the etching liquid that obtains 4 kinds of different B OE concentration, according to the extension rate of BOE, be denoted as successively from low to high 1/1BOE, 1/2BOE, 1/4BOE, 1/8BOE.
Get 3 parts of 1/1BOE etching liquids, each 1 of the glass substrate that is pasted with photosensitive dry film after respectively step (5) gained being developed is hung vertically in etching microfluidic channel in etching liquid, the temperature of using respectively circulator bath to control etching liquid is 20 ℃, 30 ℃, 40 ℃, etching liquid should flood described glass substrate completely, uses bubbler disturbance with increase etching liquid to etching liquid bubbling in etching process.In etching process, every 1min, observe the state of photosensitive dry film and glass baseplate, when photosensitive dry film starts to depart from glass substrate, immediately glass substrate is taken out to the photosensitive dry film and the etching liquid that are placed on the supersonic wave cleaning machine cleaning removal glass substrate that deionized water is housed, must be etched with the glass substrate of microfluidic channel.
Get 3 parts of 1/2BOE etching liquids, each 1 of the glass substrate that is pasted with photosensitive dry film after respectively step (5) gained being developed is hung vertically in etching microfluidic channel in etching liquid, the temperature of using respectively circulator bath to control etching liquid is 20 ℃, 30 ℃, 40 ℃, etching liquid should flood described glass substrate completely, uses bubbler disturbance with increase etching liquid to etching liquid bubbling in etching process.In etching process, every 1min, observe the state of photosensitive dry film and glass baseplate, when photosensitive dry film starts to depart from glass substrate, immediately glass substrate is taken out to the photosensitive dry film and the etching liquid that are placed on the supersonic wave cleaning machine cleaning removal glass substrate that deionized water is housed, must be etched with the glass substrate of microfluidic channel.
Get 3 parts of 1/4BOE etching liquids, each 1 of the glass substrate that is pasted with photosensitive dry film after respectively step (5) gained being developed is hung vertically in etching microfluidic channel in etching liquid, the temperature of using respectively circulator bath to control etching liquid is 20 ℃, 30 ℃, 40 ℃, etching liquid should flood described glass substrate completely, uses bubbler disturbance with increase etching liquid to etching liquid bubbling in etching process.In etching process, every 1min, observe the state of photosensitive dry film and glass baseplate, when photosensitive dry film starts to depart from glass substrate, immediately glass substrate is taken out to the photosensitive dry film and the etching liquid that are placed on the supersonic wave cleaning machine cleaning removal glass substrate that deionized water is housed, must be etched with the glass substrate of microfluidic channel.
Get 3 parts of 1/8BOE etching liquids, each 1 of the glass substrate that is pasted with photosensitive dry film after respectively step (5) gained being developed is hung vertically in etching microfluidic channel in etching liquid, the temperature of using respectively circulator bath to control etching liquid is 20 ℃, 30 ℃, 40 ℃, etching liquid should flood described glass substrate completely, uses bubbler disturbance with increase etching liquid to etching liquid bubbling in etching process.In etching process, every 1min, observe the state of photosensitive dry film and glass baseplate, when photosensitive dry film starts to depart from glass substrate, immediately glass substrate is taken out to the photosensitive dry film and the etching liquid that are placed on the supersonic wave cleaning machine cleaning removal glass substrate that deionized water is housed, must be etched with the glass substrate of microfluidic channel.
Be attached to photosensitive dry film on the glass substrate tolerance time curve in the etching liquid of different temperatures, variable concentrations as Fig. 3 a) as shown in, from Fig. 3 a), in etching liquid, BOE concentration one regularly, along with the increase of etching liquid temperature, the tolerance time of photosensitive dry film in etching liquid is the trend of shortening; When etching liquid temperature one regularly, the tolerance time of photosensitive dry film in etching liquid reduces and shortens with BOE concentration in etching liquid, and tends towards stability after 1/4BOE.
The average etching rate curve of microfluidic channel on glass substrate in the etching liquid of different temperatures, variable concentrations is as Fig. 3 b) as shown in, from Fig. 3 b), in etching liquid, regularly, on glass substrate, the average etching rate of microfluidic channel increases along with the rising of etching liquid temperature BOE concentration one; When one timing of etching liquid temperature, on glass substrate, the average etching rate of microfluidic channel is along with the trend that reduces to be first increases and then decreases of BOE concentration in etching solution, and the average etching rate in 1/2BOE is maximum; When the temperature of etching liquid is 40 ℃, concentration while being 1/2BOE, etch rate is maximum, can reach 4.95 μ m/min.
On glass substrate, the maximum etching depth block diagram of microfluidic channel in the etching liquid of different temperatures, variable concentrations is shown in figure c), from figure c), at 20 ℃, the etching liquid of 1/1BOE concentration and 30 ℃, in the etching liquid of 1/2BOE concentration, the maximum microchannel etching depth of microfluidic channel is 102 μ m, this degree of depth can meet the application requirements of most of fields micro-fluidic technologies, but because HF concentration in the etching liquid of 1/1BOE concentration is higher, during operation, danger is higher, therefore when preparing etching liquid, conventionally should adopt deionized water to dilute BOE.
In actual fabrication process, can be according to different microfluidic devices the temperature to the concrete selective etching liquid of the requirement of channel depth and width, the content of each composition and etch period in etching liquid.
(7) bonding microfluidic device
The slide that is of a size of 25mm * 25mm is covered in the microfluidic channel of glass substrate that step (6) gained is etched with microfluidic channel, with marking pen, in entrance and the exit of microfluidic channel, carry out mark.The electric current that ultrasonic drilling machine is set is 1.2A left and right, and regulating frequency knob makes circuit resonance, on the position of mark, punches, and uses the mixed liquor of diamond dust and running water constantly to wash away punch position in the process of punching, to improve drilling quality and punching speed.The slide that punching is completed cleans with deionized water and acetone successively, then electricity consumption dries up, again the hole on slide is aimed at the entrance and exit place of microfluidic channel on glass substrate, at slide and glass substrate laminating edge, click and enter ultraviolet light polymerization glue and examining under a microscope, after ultraviolet light polymerization glue is full of bonding region under capillarity, with ultra violet lamp 15s, solidified, formed microfluidic device.
Embodiment 2
In the present embodiment, make the schematic flow sheet of glass microfluidic devices and see Fig. 2, step is as follows:
(1) make photo etched mask
Use AutoCAD Software on Drawing linear microfluidic channel figure, the width place of microfluidic channel is 300 μ m.After microfluidic channel graphic designs completes, use the laser photocomposing machine that resolution ratio is 25400dpi that microfluidic channel graphic printing is formed to photo etched mask on transparent film, each photo etched mask is of a size of 20mm * 30mm.This step is made 6 photo etched masks altogether.
(2) clean glass substrate
The slide that is of a size of 25mm * 76mm of take is glass substrate (totally 6), with acetone, glass substrate is carried out ultrasonic cleaning 10min, then with ethanol, glass substrate carried out to ultrasonic cleaning 10min, continue after by deionized water, glass substrate is carried out to ultrasonic cleaning 10min, with organic pollution and the solid particle except glass baseplate surface, glass substrate after cleaning is put into vacuum drying chamber in 150 ℃ of dry 30min, and glass baseplate surface is anhydrous.
(3) make photosensitive glass plate
Photosensitive dry film is cut into 30mm * 80mm size (totally 6), first in glass substrate one end, drip deionized water, then open polyethylene (PE) film (seeing Fig. 1) of photosensitive dry film inner surface, be covered on one end of glass substrate, photoresist layer in described photosensitive dry film contacts with glass substrate, putting into laminator moulds 4 times 90 ℃ of mistakes again, form photosensitive glass plate, it is placed under room temperature (20 ℃) at least to 15min and make photosensitive glass plate be cooled to room temperature to carry out again next step operation.The operation of this step is all carried out under yellow fluorescent lamp.
(4) exposure
Under yellow fluorescent lamp, the photosensitive glass plate obtaining in step (3) is placed in to uv-exposure case, described photosensitive glass plate is pasted with the placement that faces up of photosensitive dry film, then the photo etched mask obtaining in step (1) is covered on the photosensitive dry film of photosensitive glass plate, photo etched mask print have carbon dust facing to photosensitive dry film, continue after vavuum pump is locked and opened to the vacuum clip in uv-exposure case, while being evacuated to photo etched mask pressed glass substrate, start exposure, time for exposure is 20s, microfluidic channel figure on photo etched mask is transferred on photosensitive dry film completely, close vavuum pump.After end exposure, take off photo etched mask, the photosensitive glass plate after exposure is taken out, in room temperature (20 ℃) lucifuge, place 15min so that the light polymers complete reaction in the photosensitive dry film after exposure.
(5) develop
Preparing developer liquid: by Na
2cO
3add deionized water for stirring evenly to form developer solution, Na
2cO
3with the mass ratio of deionized water be 1:70.
Polyester (PET) film on removing step (4) gained photosensitive glass plate photosensitive dry film, then with developer solution, the photosensitive dry film after exposing is sprayed to development, the temperature of developer solution is 30 ℃, developing time is 2min, continue after with microscopic examination, be transferred to the microfluidic channel figure on photosensitive dry film, find that the microfluidic channel pattern edge after developing is clear, the appearance such as nothing left glue burr, glass substrate after developing is placed on the drying glue platform of 100 ℃ and toasts 1h to remove the water between photosensitive dry film and glass substrate, thereby increase the adhesion property of photosensitive dry film etching mask and glass substrate.
(6) wet etching microfluidic channel
Preparation etching liquid: by the NH of 40wt%
4the HF aqueous solution of the F aqueous solution and 40wt% is that 7:1 is mixed to form buffer oxide etching liquid (BOE) according to volume ratio, by the ratio that deionized water is 1:1 according to the volume ratio of deionized water and BOE, dilute respectively, in the BOE after dilution, add the concentrated hydrochloric acid of 37.5wt% again, BOE after described dilution and the volume ratio of concentrated hydrochloric acid are 10:2, mix and obtain etching liquid.
The glass substrate that is pasted with photosensitive dry film after 6 steps (5) gained is developed is hung vertically in etching microfluidic channel in etching liquid, the temperature of using circulator bath to control etching liquid is 30 ℃, etching liquid should flood described glass substrate completely, in etching process, use bubbler disturbance with increase etching liquid to etching liquid bubbling, the etch period of 6 glass substrates is respectively 5min, 10min, 15min, 20min, 25min, 30min, after etching finishes, the glass substrate that is pasted with photosensitive dry film is taken out to photosensitive dry film and the etching liquid being placed on the supersonic wave cleaning machine cleaning removal glass substrate that deionized water is housed, must be etched with the glass substrate of microfluidic channel.
On the glass substrate of etching different time, as shown in Figure 4, as shown in Figure 4, along with the increase of etch period, the degree of depth of microfluidic channel increases the cross-sectional scans Electronic Speculum figure of microfluidic channel, and microfluidic channel inner wall smooth, produces without deposit seed.
As shown in Figure 5, as shown in Figure 5, due to glass substrate material isotropism, the degree of depth of microfluidic channel and width all increase with the increase of etch period the relation curve that on glass substrate, the width of microfluidic channel and the degree of depth change with etch period.In actual production, can with the relation curve of etch period variation, select suitable etch period according to the width of microfluidic channel and the degree of depth.
(7) bonding microfluidic device
The slide that is of a size of 25mm * 25mm is covered in the microfluidic channel of glass substrate that step (6) gained is etched with microfluidic channel, with marking pen, in entrance and the exit of microfluidic channel, carry out mark.The electric current that ultrasonic drilling machine is set is 1.2A left and right, and regulating frequency knob makes circuit resonance, on the position of mark, punches, and uses the mixed liquor of diamond dust and running water constantly to wash away punch position in the process of punching, to improve drilling quality and punching speed.The slide that punching is completed cleans with deionized water and acetone successively, then electricity consumption dries up, again the hole on slide is aimed at the entrance and exit place of microfluidic channel on glass substrate, at slide and glass substrate laminating edge, click and enter ultraviolet light polymerization glue and examining under a microscope, after ultraviolet light polymerization glue is full of bonding region under capillarity, with ultra violet lamp 15s, solidified, formed microfluidic device.
Embodiment 3
In the present embodiment, make the schematic flow sheet of glass microfluidic devices and see Fig. 2, step is as follows:
(1) make photo etched mask
Use six kinds of AutoCAD Software on Drawings common microfluidic channel figure as shown in Figure 6, in Fig. 6, a) be Y shape passage, b) be cross passage, c) be T shape passage, d) be diesis shape passage, e) be snakelike hybrid channel, f) be concentration gradient passage.Its maximum width of microfluidic channel design is 400 μ m, and minimum widith place is 200 μ m.After microfluidic channel graphic designs completes, use the laser photocomposing machine that resolution ratio is 25400dpi that microfluidic channel graphic printing is formed to photo etched mask on transparent film, each photo etched mask size is 20mm * 30mm.
(2) clean glass substrate
The slide that is of a size of 25mm * 76mm of take is glass substrate, with acetone, glass substrate is carried out ultrasonic cleaning 10min, then with ethanol, glass substrate carried out to ultrasonic cleaning 10min, continue after by deionized water, glass substrate is carried out to ultrasonic cleaning 10min, with organic pollution and the solid particle except glass baseplate surface, glass substrate after cleaning is put into vacuum drying chamber in 60 ℃ of dry 1h, and glass baseplate surface is anhydrous.
(3) make photosensitive glass plate
Photosensitive dry film is cut into 30mm * 80mm size, first in glass substrate one end, drip deionized water, then open polyethylene (PE) film (seeing Fig. 1) of photosensitive dry film inner surface, be covered on one end of glass substrate, photoresist layer in described photosensitive dry film contacts with glass substrate, putting into laminator moulds 3 times 93 ℃ of mistakes again, form photosensitive glass plate, it is placed under room temperature (20 ℃) at least to 15min and make photosensitive glass plate be cooled to room temperature to carry out again next step operation.The operation of this step is all carried out under yellow fluorescent lamp.
(4) exposure
Under yellow fluorescent lamp, the photosensitive glass plate obtaining in step (3) is placed in to uv-exposure case, described photosensitive glass plate is pasted with the placement that faces up of photosensitive dry film, then the photo etched mask obtaining in step (1) is covered on the photosensitive dry film of photosensitive glass plate, photo etched mask print have carbon dust facing to photosensitive dry film, continue after vavuum pump is locked and opened to the vacuum clip in uv-exposure case, while being evacuated to photo etched mask pressed glass substrate, start exposure, time for exposure is 20s, microfluidic channel figure on photo etched mask is transferred on photosensitive dry film completely, close vavuum pump.After end exposure, take off photo etched mask, the photosensitive glass plate after exposure is taken out, in room temperature (20 ℃) lucifuge, place 15min so that the light polymers complete reaction in the photosensitive dry film after exposure.
(5) develop
Preparing developer liquid: by Na
2cO
3add deionized water for stirring evenly to form developer solution, Na
2cO
3with the mass ratio of deionized water be 1:70.
Polyester (PET) film on removing step (4) gained photosensitive glass plate photosensitive dry film, then with developer solution, the photosensitive dry film after to exposure sprays development, and the temperature of developer solution is that 30 ℃, developing time are 2min; Continue after with microscopic examination, be transferred to the microfluidic channel figure on photosensitive dry film, the optical microscope photograph of the microfluidic channel figure after developing on the photosensitive dry film of photosensitive glass plate as shown in Figure 7, the appearance such as shown in Figure 7, the microfluidic channel pattern edge after development is clear, nothing left glue burr.After development, glass substrate is placed on the drying glue platform of 65 ℃ and toasts 1.5h to remove the water between photosensitive dry film and glass substrate, thereby increase the adhesion property of photosensitive dry film etching mask and glass substrate.
(6) wet etching microfluidic channel
Preparation etching liquid: by the NH of 40wt%
4the HF aqueous solution of the F aqueous solution and 40wt% is that 7:1 is mixed to form buffer oxide etching liquid (being called for short BOE) according to volume ratio, by the ratio that deionized water is 1:1 according to the volume ratio of deionized water and BOE, dilute respectively, in the BOE after dilution, add the concentrated hydrochloric acid of 37.5wt% again, BOE after described dilution and the volume ratio of concentrated hydrochloric acid are 10:2, mix and obtain etching liquid.
The glass substrate that is pasted with photosensitive dry film after step (5) gained is developed is hung vertically in etching microfluidic channel in etching liquid, the temperature of using circulator bath to control etching liquid is 30 ℃, etching liquid should flood described glass substrate completely, in etching process, use bubbler disturbance with increase etching liquid to etching liquid bubbling, etch period is 30min, after etching finishes, the glass substrate that is pasted with photosensitive dry film is taken out to photosensitive dry film and the etching liquid being placed on the supersonic wave cleaning machine cleaning removal glass substrate that deionized water is housed, must be etched with the glass substrate of microfluidic channel.After etching completes, on glass substrate, the optical microscope photograph of microfluidic channel is as shown in Figure 8.
(7) bonding microfluidic device
The slide that is of a size of 25mm * 25mm is covered in the microfluidic channel of glass substrate that step (6) gained is etched with microfluidic channel, with marking pen, in entrance and the exit of microfluidic channel, carry out mark.The electric current that ultrasonic drilling machine is set is 1.2A left and right, and regulating frequency knob makes circuit resonance, on the position of mark, punches, and uses the mixed liquor of diamond dust and running water constantly to wash away punch position in the process of punching, to improve drilling quality and punching speed.The slide that punching is completed cleans with deionized water and acetone successively, then electricity consumption dries up, again the hole on slide is aimed at the entrance and exit place of microfluidic channel on glass substrate, at slide and glass substrate laminating edge, click and enter ultraviolet light polymerization glue and examining under a microscope, after ultraviolet light polymerization glue is full of bonding region under capillarity, with ultra violet lamp 15s, solidified, formed microfluidic device.Finally at the tapping at perforate slide, paste and connect polyethylene hose, by polyethylene hose, in microfluidic channel, inject after methylene blue, the photo of glass microfluidic devices as shown in Figure 9, can clearly be found out the shape of six kinds of microfluidic channel from Fig. 9.
In the present embodiment, the success rate of using ultraviolet light polymerization glue to carry out bonding to microfluidic device is 100%, and the required time of microfluidic device of bonding is no more than 10min, and bonding efficiency is high.With ultraviolet light polymerization glue bonding glass microfluidic devices, without special installation and particular surroundings, can reduce the processing cost of glass microfluidic devices.
Embodiment 4
In the present embodiment, make the schematic flow sheet of glass microfluidic devices and see Fig. 2, step is as follows:
(1) make photo etched mask
Use AutoCAD Software on Drawing as Fig. 6 c) as shown in T shape passage, its maximum width of microfluidic channel design is 400 μ m, minimum widith place is 200 μ m.After microfluidic channel graphic designs completes, use the laser photocomposing machine that resolution ratio is 25400dpi that microfluidic channel graphic printing is formed to photo etched mask on transparent film, photo etched mask is of a size of 20mm * 30mm.
(2) clean glass substrate
The slide that is of a size of 25mm * 76mm of take is glass substrate, with ethanol, glass substrate is carried out ultrasonic cleaning 10min, then with acetone, glass substrate carried out to ultrasonic cleaning 10min, continue after by deionized water, glass substrate is carried out to ultrasonic cleaning 10min, with organic pollution and the solid particle except glass baseplate surface, glass substrate after cleaning is put into vacuum drying chamber in 150 ℃ of dry 30min, and glass baseplate surface is anhydrous.
(3) make photosensitive glass plate
Photosensitive dry film is cut into 30mm * 80mm size, first in glass substrate one end, drip deionized water, then open polyethylene (PE) film (seeing Fig. 1) of photosensitive dry film inner surface, be covered on one end of glass substrate, photoresist layer in described photosensitive dry film contacts with glass substrate, putting into laminator moulds 2 times 95 ℃ of mistakes again, form photosensitive glass plate, it is placed under room temperature (20 ℃) at least to 15min and make photosensitive glass plate be cooled to room temperature to carry out again next step operation.The operation of this step is all carried out under yellow fluorescent lamp.
(4) exposure
Under yellow fluorescent lamp, the photosensitive glass plate obtaining in step (3) is placed in to uv-exposure case, described photosensitive glass plate is pasted with the placement that faces up of photosensitive dry film, then the photo etched mask obtaining in step (1) is covered on the photosensitive dry film of photosensitive glass plate, photo etched mask print have carbon dust facing to photosensitive dry film, continue after vavuum pump is locked and opened to the vacuum clip in uv-exposure case, while being evacuated to photo etched mask pressed glass substrate, start exposure, time for exposure is 20s, microfluidic channel figure on photo etched mask is transferred on photosensitive dry film completely, close vavuum pump.After end exposure, take off photo etched mask, the photosensitive glass plate after exposure is taken out, in room temperature (20 ℃) lucifuge, place 10min so that the light polymers complete reaction in the photosensitive dry film after exposure.
(5) develop
Preparing developer liquid: by Na
2cO
3add deionized water for stirring evenly to form developer solution, Na
2cO
3with the mass ratio of deionized water be 1:50.
Polyester (PET) film on removing step (4) gained photosensitive glass plate photosensitive dry film, then with developer solution, the photosensitive dry film after to exposure sprays development, and the temperature of developer solution is that 35 ℃, developing time are 30s; Continue after with microscopic examination, be transferred to the microfluidic channel figure on photosensitive dry film, the optical microscope photograph of the photosensitive glass plate after development as shown in Figure 7, as shown in Figure 7, the appearance such as the microfluidic channel pattern edge after development is clear, nothing left glue burr.After development, glass substrate is placed on the drying glue platform of 100 ℃ and toasts 1h to remove the water between photosensitive dry film and glass substrate, thereby increase the adhesion property of photosensitive dry film etching mask and glass substrate.
(6) wet etching microfluidic channel
Preparation etching liquid: by the NH of 40wt%
4the HF aqueous solution of the F aqueous solution and 40wt% is that 6:1 is mixed to form buffer oxide etching liquid (BOE) according to volume ratio, by the ratio that deionized water is 1:1 according to the volume ratio of deionized water and BOE, dilute respectively, in the BOE after dilution, add the concentrated hydrochloric acid of 37.5wt% again, BOE after described dilution and the volume ratio of concentrated hydrochloric acid are 10:1, mix and obtain etching liquid.
The glass substrate that is pasted with photosensitive dry film after step (5) gained is developed is hung vertically in etching microfluidic channel in etching liquid, the temperature of using circulator bath to control etching liquid is 30 ℃, etching liquid should flood described glass substrate completely, in etching process, stir to increase the disturbance of etching liquid, etch period is 1min, after etching finishes, the glass substrate that is pasted with photosensitive dry film is taken out to photosensitive dry film and the etching liquid being placed on the supersonic wave cleaning machine cleaning removal glass substrate that deionized water is housed, must be etched with the glass substrate of microfluidic channel.
(7) bonding microfluidic device
The slide that is of a size of 25mm * 25mm is covered in the microfluidic channel of glass substrate that step (6) gained is etched with microfluidic channel, with marking pen, in entrance and the exit of microfluidic channel, carry out mark.The electric current that ultrasonic drilling machine is set is 1.2A left and right, and regulating frequency knob makes circuit resonance, on the position of mark, punches, and uses the mixed liquor of diamond dust and running water constantly to wash away punch position in the process of punching, to improve drilling quality and punching speed.The slide that punching is completed cleans with deionized water and acetone successively, then electricity consumption dries up, again the hole on slide is aimed at the entrance and exit place of microfluidic channel on glass substrate, at slide and glass substrate laminating edge, click and enter ultraviolet light polymerization glue and examining under a microscope, after ultraviolet light polymerization glue is full of bonding region under capillarity, with ultra violet lamp 15s, solidified, formed microfluidic device.Finally at the tapping at perforate slide, paste and connect polyethylene hose.
Embodiment 5
In the present embodiment, make the schematic flow sheet of glass microfluidic devices and see Fig. 2, step is as follows:
(1) make photo etched mask
Use AutoCAD Software on Drawing as the Y shape passage of Fig. 6 as shown in a), its maximum width of microfluidic channel design is 400 μ m, and minimum widith place is 200 μ m.After microfluidic channel graphic designs completes, use the laser photocomposing machine that resolution ratio is 25400dpi that microfluidic channel graphic printing is formed to photo etched mask on transparent film, photo etched mask is of a size of 20mm * 30mm.
(2) clean glass substrate
The slide that is of a size of 25mm * 76mm of take is glass substrate, with acetone, glass substrate is carried out ultrasonic cleaning 10min, then with ethanol, glass substrate carried out to ultrasonic cleaning 10min, continue after by deionized water, glass substrate is carried out to ultrasonic cleaning 10min, with organic pollution and the solid particle except glass baseplate surface, glass substrate after cleaning is put into vacuum drying chamber in 100 ℃ of dry 40min, and glass baseplate surface is anhydrous.
(3) make photosensitive glass plate
Photosensitive dry film is cut into 30mm * 80mm size, first in glass substrate one end, drip deionized water, then under yellow fluorescent lamp, open polyethylene (PE) film (seeing Fig. 1) of photosensitive dry film inner surface, be covered on one end of glass substrate, photoresist layer in described photosensitive dry film contacts with glass substrate, putting into laminator moulds 3 times 93 ℃ of mistakes again, form photosensitive glass plate, it is placed under room temperature (20 ℃) at least to 15min and make photosensitive glass plate be cooled to room temperature to carry out again next step operation.The operation of this step is all carried out under yellow fluorescent lamp.
(4) exposure
Under yellow fluorescent lamp, the photosensitive glass plate obtaining in step (3) is placed in to uv-exposure case, described photosensitive glass plate is pasted with the placement that faces up of photosensitive dry film, then the photo etched mask obtaining in step (1) is covered on the photosensitive dry film of photosensitive glass plate, photo etched mask print have carbon dust facing to photosensitive dry film, continue after vavuum pump is locked and opened to the vacuum clip in uv-exposure case, while being evacuated to photo etched mask pressed glass substrate, start exposure, time for exposure is 20s, microfluidic channel figure on photo etched mask is transferred on photosensitive dry film completely, close vavuum pump.After end exposure, take off photoetching press mold, the photosensitive glass plate after exposure is taken out, in room temperature (20 ℃) lucifuge, place 15min so that the light polymers complete reaction in the photosensitive dry film after exposure.
(5) develop
The configuration of developer solution: by Na
2cO
3add deionized water for stirring evenly to form developer solution, Na
2cO
3with the mass ratio of deionized water be 1:100.
Polyester (PET) film (as shown in Figure 1) on the photosensitive glass plate upper strata after the exposure obtaining in step (4) is thrown off, used Na
2cO
3developer solution sprays development to the photosensitive dry film after exposing, development temperature is controlled at 25 ℃, and developing time is 5min, continue after with microscopic examination, be transferred to the microfluidic channel figure on photosensitive dry film, find that the microfluidic channel pattern edge after developing is clear, the appearance such as nothing left glue burr.After development, glass baseplate is positioned on the drying glue platform of 100 ℃ and toasts 1h to remove the water of photosensitive dry film bottom, thereby increase the adhesion property of photosensitive dry film etching mask and glass baseplate.
(6) microfluidic channel wet etching
Preparation etching liquid: by the NH of 40wt%
4the HF aqueous solution of the F aqueous solution and 40wt% is that 6:1 is mixed to form buffer oxide etching liquid (BOE) according to volume ratio, by the ratio that deionized water is 1:1 according to the volume ratio of deionized water and BOE, dilute respectively, in the BOE after dilution, add the concentrated hydrochloric acid of 37.5wt% again, BOE after described dilution and the volume ratio of concentrated hydrochloric acid are 10:3, mix and obtain etching liquid.
The glass substrate that is pasted with photosensitive dry film after step (5) gained is developed is hung vertically in etching microfluidic channel in etching liquid, the temperature of using circulator bath to control etching liquid is 30 ℃, etching liquid should flood described glass substrate completely, in etching process, use bubbler disturbance with increase etching liquid to etching liquid bubbling, etch period is 20min, after etching finishes, the glass substrate that is pasted with photosensitive dry film is taken out to photosensitive dry film and the etching liquid being placed on the supersonic wave cleaning machine cleaning removal glass substrate that deionized water is housed, must be etched with the glass substrate of microfluidic channel.
(7) bonding microfluidic device
The slide that is of a size of 25mm * 25mm is covered in the microfluidic channel of glass substrate that step (6) gained is etched with microfluidic channel, with marking pen, in entrance and the exit of microfluidic channel, carry out mark.The electric current that ultrasonic drilling machine is set is 1.2A left and right, and regulating frequency knob makes circuit resonance, on the position of mark, punches, and uses the mixed liquor of diamond dust and running water constantly to wash away punch position in the process of punching, to improve drilling quality and punching speed.The slide that punching is completed cleans with deionized water and acetone successively, then electricity consumption dries up, again the hole on slide is aimed at the entrance and exit place of microfluidic channel on glass substrate, at slide and glass substrate laminating edge, click and enter ultraviolet light polymerization glue and examining under a microscope, after ultraviolet light polymerization glue is full of bonding region under capillarity, with ultra violet lamp 15s, solidified, formed microfluidic device.Finally at the tapping at perforate slide, paste and connect polyethylene hose.
Embodiment 6
In the present embodiment, the T shape microfluidic channel of take is example, and the method for batch making glass microfluidic devices is described, step is as follows:
(1) make photo etched mask
Use AutoCAD Software on Drawing array T shape microfluidic channel figure as shown in figure 10, its maximum width of microfluidic channel design is 400 μ m, and minimum widith place is 200 μ m.After microfluidic channel graphic designs completes, use the laser photocomposing machine that resolution ratio is 25400dpi that microfluidic channel graphic printing is formed to photo etched mask on transparent film, photo etched mask is of a size of 60mm * 180mm.
(2) clean glass substrate
The soda-lime glass that is of a size of 60mm * 180mm of take is glass substrate, with acetone, glass substrate is carried out ultrasonic cleaning 10min, then with ethanol, glass substrate carried out to ultrasonic cleaning 10min, continue after by deionized water, glass substrate is carried out to ultrasonic cleaning 10min, with organic pollution and the solid particle except glass baseplate surface, glass substrate after cleaning is put into vacuum drying chamber in 60 ℃ of dry 1h, and glass baseplate surface is anhydrous.
(3) make photosensitive glass plate
Photosensitive dry film is cut into 70mm * 190mm size, first in glass substrate one end, drip deionized water, then open polyethylene (PE) film (seeing Fig. 1) of photosensitive dry film inner surface, be covered on one end of glass substrate, photoresist layer in described photosensitive dry film contacts with glass substrate, putting into laminator moulds 3 times 93 ℃ of mistakes again, form photosensitive glass plate, it is placed under room temperature (20 ℃) at least to 15min and make photosensitive glass plate be cooled to room temperature to carry out again next step operation.The operation of this step is all carried out under yellow fluorescent lamp.
(4) exposure
Under yellow fluorescent lamp, the photosensitive glass plate obtaining in step (3) is placed in to uv-exposure case, described photosensitive glass plate is pasted with the placement that faces up of photosensitive dry film, then the photo etched mask obtaining in step (1) is covered on the photosensitive dry film of photosensitive glass plate, photo etched mask print have carbon dust facing to photosensitive dry film, continue after vavuum pump is locked and opened to the vacuum clip in uv-exposure case, while being evacuated to photo etched mask pressed glass substrate, start exposure, time for exposure is 20s, microfluidic channel figure on photo etched mask is transferred on photosensitive dry film completely, close vavuum pump.After end exposure, take off photo etched mask, the photosensitive glass plate after exposure is taken out, in room temperature (20 ℃) lucifuge, place 15min so that the light polymers complete reaction in the photosensitive dry film after exposure.
(5) develop
Preparing developer liquid: by Na
2cO
3add deionized water for stirring evenly to form developer solution, Na
2cO
3with the mass ratio of deionized water be 1:70.
Polyester (PET) film on removing step (4) gained photosensitive glass plate photosensitive dry film, then with developer solution, the photosensitive dry film after to exposure sprays development, and the temperature of developer solution is that 30 ℃, developing time are 2min; Continue after with microscopic examination, be transferred to the microfluidic channel figure on photosensitive dry film, the microfluidic channel pattern edge after find developing is clear, the appearance such as nothing left glue burr, the photosensitive glass plate after development is as shown in figure 11.After development, glass substrate is placed on the drying glue platform of 65 ℃ and toasts 2h to remove the water between photosensitive dry film and glass substrate, thereby increase the adhesion property of photosensitive dry film etching mask and glass substrate.
(6) wet etching microfluidic channel
Preparation etching liquid: by the NH of 40wt%
4the HF aqueous solution of the F aqueous solution and 40wt% is that 7:1 is mixed to form buffer oxide etching liquid (BOE) according to volume ratio, by the ratio that deionized water is 1:1 according to the volume ratio of deionized water and BOE, dilute respectively, in the BOE after dilution, add the concentrated hydrochloric acid of 37.5wt% again, BOE after described dilution and the volume ratio of concentrated hydrochloric acid are 10:2, mix and obtain etching liquid;
The glass substrate that step (5) gained is pasted with to photosensitive dry film is hung vertically in etching microfluidic channel in etching liquid, the temperature of using circulator bath to control etching liquid is 30 ℃, etching liquid should flood described glass substrate completely, in etching process, use bubbler disturbance with increase etching liquid to etching liquid bubbling, etch period is 20min, after etching finishes, the glass substrate that is pasted with photosensitive dry film is taken out to photosensitive dry film and the etching liquid being placed on the supersonic wave cleaning machine cleaning removal glass substrate that deionized water is housed, must be etched with the glass substrate of array T shape microfluidic channel, as shown in figure 12, 24 T shape passages have been transferred on glass substrate once.
(7) bonding microfluidic device
The glass substrate that step (6) gained is etched with to array T shape microfluidic channel is slit into fritter (20mm * 20mm) with glass cutter, has a complete T shape microfluidic channel on every.The slide that is of a size of 25mm * 25mm is covered to the microfluidic channel top of the glass substrate after cutting apart, with marking pen, in entrance and the exit of microfluidic channel, carry out mark.The electric current that ultrasonic drilling machine is set is 1.2A left and right, and regulating frequency knob makes circuit resonance, on the position of mark, punches, and uses the mixed liquor of diamond dust and running water constantly to wash away punch position in the process of punching, to improve drilling quality and punching speed.The slide that punching is completed cleans with deionized water and acetone successively, then electricity consumption dries up, again the hole on slide is aimed at the entrance and exit place of microfluidic channel on glass substrate, at slide and glass substrate laminating edge, click and enter ultraviolet light polymerization glue and examining under a microscope, after ultraviolet light polymerization glue is full of bonding region under capillarity, with ultra violet lamp 15s, solidified, formed microfluidic device.Finally at the tapping at perforate slide, paste and connect polyethylene hose, by polyethylene hose, in microfluidic channel, inject after methylene blue, the optical photograph of microfluidic device as shown in figure 13, can clearly be found out the shape of microfluidic channel microfluidic device from Figure 13.
In this embodiment, make 24 glass microfluidic devices about 12h consuming time altogether, always spend less than 8 yuan, make the glass microfluidic devices about 30min consuming time of 1 20mm * 20mm, approximately 0.3 yuan of cost, the mass production that the described method of this explanation invention is glass microfluidic devices provides a kind of cheapness, efficient new way.
Claims (10)
1. the method that the photosensitive dry film of take is made glass microfluidic devices as etching mask, is characterized in that step is as follows:
(1) make photo etched mask
The microfluidic channel figure that uses mapping software design microfluidic device forms photo etched mask with laser photocomposing machine by the microfluidic channel graphic printing designing on transparent film;
(2) clean glass substrate
With using again washed with de-ionized water glass substrate after acetone, ethanol cleaning glass substrate, to remove organic pollution and the solid particle of glass baseplate surface, then the glass substrate after cleaning is dried to its surface anhydrous respectively;
(3) make photosensitive glass plate
Photosensitive dry film is cut to the shape and size of the described glass substrate of step (2), throw off the polyethylene film of photosensitive dry film and adopt wet film coating method that photosensitive dry film is attached on glass substrate, photoresist layer in described photosensitive dry film contacts with glass substrate, then uses laminator at 90～95 ℃ of moulding one-tenth photosensitive glass plates of mistake;
(4) exposure
Step (3) gained photosensitive glass plate is placed in to uv-exposure case, described photosensitive glass plate is pasted with the placement that faces up of photosensitive dry film, then the photo etched mask of step (1) being made covers on the photosensitive dry film of photosensitive glass plate and compresses, described photo etched mask print have carbon dust facing to photosensitive dry film, continue after by uv-exposure, the microfluidic channel figure on photo etched mask is transferred on photosensitive dry film, after end exposure, take off photo etched mask, photosensitive glass plate after exposure is taken out, and lucifuge is placed at least 10min;
(5) develop
Polyester film on photosensitive glass plate photosensitive dry film after the exposure of removing step (4) gained, then use developing liquid developing, developing time is 0.5～5min, continue after with the microfluidic channel figure on microscopic examination photosensitive dry film, if it is clear to remain the blur margin of photosensitive dry film or microfluidic channel in the microfluidic channel in figure, repeat aforementioned development operation, until the photosensitive dry film at the microfluidic channel inside in figure and microfluidic channel edge is completely removed, after development, the dry water of removing between photosensitive dry film and glass substrate;
Described developer solution is by Na
2cO
3formulated with deionized water, in developer solution, Na
2cO
3with the mass ratio of deionized water be 1:(50～100);
(6) etching microfluidic channel
It is etching microfluidic channel in the etching liquid of 20～40 ℃ that the glass substrate that is pasted with photosensitive dry film after step (5) is developed is immersed in temperature, in etching process, etching liquid is carried out to disturbance, etch period is no more than the tolerance time of described photosensitive dry film in etching liquid, after etching finishes, the glass substrate that is pasted with photosensitive dry film is taken out, be placed in deionized water washing and remove photosensitive dry film and the etching liquid on glass substrate, obtain being etched with the glass substrate of microfluidic channel;
The compound method of described etching liquid is as follows: by the NH of 40wt%
4the HF aqueous solution of the F aqueous solution and 40wt% forms buffer oxide etching liquid, then uses deionized water dilution buffer oxide etch liquid, then to the concentrated hydrochloric acid that adds 37.5wt% in the buffer oxide etching liquid after dilution, mixes and obtain etching liquid; Described NH
4the volume ratio of the F aqueous solution and the HF aqueous solution is (6～7): 1, and the volume ratio of described deionized water and buffer oxide etching liquid is (1～7): 1, the buffer oxide etching liquid after described dilution and the volume ratio of concentrated hydrochloric acid are 10:(1～3);
(7) bonding microfluidic device
Sheet glass is covered to step (6) gained and be etched with on the glass substrate of microfluidic channel, use ultraviolet light polymerization glue by described sheet glass and glass substrate bonding, form microfluidic device; The entrance and exit corresponding section of described sheet glass and microfluidic channel is provided with through hole.
2. the method that the photosensitive dry film of take is according to claim 1 made glass microfluidic devices as etching mask, is characterized in that the temperature of developer solution in step (5) is controlled at 25～35 ℃.
3. according to take the method for photosensitive dry film as etching mask making glass microfluidic devices described in claim 1 or 2, it is characterized in that the etch period in step (6) is 1～30min.
4. according to take the method that photosensitive dry film makes glass microfluidic devices as etching mask described in claim 1 or 2, it is characterized in that step (3) carries out under yellow fluorescent lamp, operating under yellow fluorescent lamp before the exposure of step (4) medium ultraviolet carried out.
5. the photosensitive dry film of take is according to claim 3 that etching mask makes the method for glass microfluidic devices, it is characterized in that step (3) carries out under yellow fluorescent lamp, and operating under yellow fluorescent lamp before the exposure of step (4) medium ultraviolet carried out.
6. according to take the method for photosensitive dry film as etching mask making glass microfluidic devices described in claim 1 or 2, after it is characterized in that the middle development of step (5), at 60～100 ℃, be dried the water of removing between photosensitive dry film and glass substrate.
7. according to take the method for photosensitive dry film as etching mask making glass microfluidic devices described in claim 1 or 2, it is characterized in that in step (6) by stirring or by the mode of bubbler bubbling, etching liquid being carried out to disturbance.
8. according to take the method for photosensitive dry film as etching mask making glass microfluidic devices described in claim 1 or 2, after it is characterized in that the middle etching of step (6) finishes, the glass substrate that is pasted with photosensitive dry film is taken out, be placed in deionized water and remove photosensitive dry film and the etching liquid on glass substrate in the mode of Ultrasonic Cleaning.
9. according to take the method for photosensitive dry film as etching mask making glass microfluidic devices described in claim 1 or 2, it is characterized in that, in step (2), the complete glass substrate of cleaning is dried to its surface at 60～150 ℃ anhydrous.
10. according to take the method that photosensitive dry film makes glass microfluidic devices as etching mask described in claim 1 or 2, use laminator to cross after it is characterized in that photosensitive dry film being attached on glass plate in step (3) and mould 2～4 times.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN109407472A (en) * | 2018-12-20 | 2019-03-01 | 张家港康得新光电材料有限公司 | Preparation method, making apparatus and the product of light microchannel plate |
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