CN104190482B - Take photosensitive dry film as the method that etching mask makes glass microfluidic devices - Google Patents
Take photosensitive dry film as the method that etching mask makes glass microfluidic devices Download PDFInfo
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- CN104190482B CN104190482B CN201410416124.8A CN201410416124A CN104190482B CN 104190482 B CN104190482 B CN 104190482B CN 201410416124 A CN201410416124 A CN 201410416124A CN 104190482 B CN104190482 B CN 104190482B
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Abstract
The invention belongs to microfluidic device and make field, provide a kind of method taking photosensitive dry film as etching mask and make glass microfluidic devices, the step of the method is as follows: (1) makes photo etched mask, (2) glass substrate is cleaned, (3) make photosensitive glass plate, (4) expose, and (5) develop, (6) microfluidic channel is etched, (7) bonding microfluidic device.The method of the invention can simplify manufacturing process, the raising make efficiency of glass microfluidic devices, and significantly reduce the cost of manufacture of glass microfluidic devices, the mass production for glass microfluidic devices provides a kind of new approach.
Description
Technical field
The invention belongs to microfluidic device and make field, particularly a kind of method taking photosensitive dry film as etching mask and make glass microfluidic devices.
Background technology
Be called as the micro-fluidic technologies of Lab-on-a-chip (LoC) since the nineties in 20th century comes out, the most effective fluid operated means under becoming micro-meter scale gradually.Because multiple monotechnics can be carried out flexible combination and large-scale integrated by micro-fluidic technologies on the microfluidic platform of several square centimeters even less, there is laboratory sample consumption few, the feature such as short consuming time, obtain in the field such as biological, chemical and study widely.But the complex manufacturing technology of current most of microfluidic device, manufacturing conditions is harsh, needs, with expensive experiment material and equipment, to this seriously inhibits the development and apply of micro-fluidic technologies in manufacturing process.
In prior art, the material for making microfluidic device mainly contains organic polymer dimethyl silicone polymer (PDMS), silicon and glass.It is high with PDMS to be that base material adopts the method for Soft lithograph fabrication techniques microfluidic device to have channel size control accuracy, the features such as complicated shape passage can be produced and be widely used, 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 receive certain restriction.Silicon has good chemical inertness and heat endurance, use the method for chemical etching can copy the complex passages of two dimension or three-dimensional accurately, but silicon on the high side, light tight, intensity is low, these shortcomings limit the use of silicon materials in microfluid system.
Compared to PDMS and silicon, glass material has good electric osmose characteristic, excellent optical characteristics and chemical inertness, and mechanical strength is high, high temperature resistant, surface easily modification, cheap, and these features make glass material be widely used in making microfluidic device.The method of current making glass microfluidic devices has capillary glass tube to splice (see A.Utada, E.Lorenceau, D.Link, P.Kaplan, H.Stone and D.Weitz, Science, 2005, 308, 537-541.), slide and cover glass splice (see 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 (see C.H.Lin, G.B.Lee, Y.H.Lin and G.L.Chang, Journal ofmicromechanics and microengineering, 2001, 11, 726-732.) etc.Wherein, it is fairly simple that capillary glass tube splicing method and slide and cover glass splice method, do not need special material and facility, can make in Routine Test Lab.But these two kinds of methods all need consummate skill hand-manipulated, accurately can not control the size of microfluidic channel, the make efficiency of device is extremely low, cannot carry out mass making.Etching can carry out flexible design to channel shape in conjunction with the method for photoetching making microfluidic device in a wet process, channel size precision is higher, low (see thanking to hypo to manual dependence, Fu Xin, Yang Huayong, journal of Zhejiang university: engineering version, 2007,41,560-563.), but the method has the following disadvantages: must at substrate surface depositing metal layers or spin coating photoresist as etching mask before (1) wet etching, the complicated process of preparation of this etching mask, length consuming time, adopting the method to make a glass microfluidic devices needs about 5 ~ 6h consuming time; (2) need the instrument and equipment adopting metal sputtering instrument, litho machine, spin coater etc. expensive in ultra-clean working environment, must use the material that the price such as liquid photoresist, sputtering precious metal is high, production cost is very high.According to the complex situations of microfluidic channel from hundreds of unit to tens thousand of unit not etc., fancy price seriously hinders the large-scale application of micro-fluidic technologies for the price of current 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 taking photosensitive dry film as etching mask and make glass microfluidic devices is provided, the method can simplify manufacturing process, the raising make efficiency of glass microfluidic devices, significantly reduce the cost of manufacture of glass microfluidic devices, the mass production for glass microfluidic devices provides a kind of new approach.
The method taking photosensitive dry film as etching mask and make glass microfluidic devices provided by the invention, step is as follows:
(1) photo etched mask is made
Use the microfluidic channel figure of mapping software design microfluidic device, with laser photocomposing machine, the microfluidic channel graphic printing designed is formed photo etched mask on transparent film;
(2) glass substrate is cleaned
Use washed with de-ionized water glass substrate again with after acetone, ethanol cleaning glass substrate respectively, to remove organic pollution and the solid particle of glass baseplate surface, then the glass substrate after cleaning is dried to its surface anhydrous;
(3) photosensitive glass plate is made
Photosensitive dry film is cut to the shape and size of step (2) described glass substrate, throw off the polyethylene film of photosensitive dry film and adopt wet film coating method to be attached on glass substrate by photosensitive dry film, photoresist oxidant layer in described photosensitive dry film contacts with glass substrate, then uses laminator at 90 ~ 95 DEG C of moulding one-tenth photosensitive glass plates of mistake;
(4) expose
Step (3) gained photosensitive glass plate is placed in uv-exposure case, described photosensitive glass plate is pasted with the placement that faces up of photosensitive dry film, then the photosensitive dry film photo etched mask that step (1) makes being covered photosensitive glass plate compresses, described photo etched mask print have carbon dust facing to photosensitive dry film, continue after make microfluidic channel Graphic transitions on photo etched mask on photosensitive dry film by uv-exposure, after end exposure, take off photo etched mask, photosensitive glass plate after exposure is taken out, lucifuge place at least 10min to make 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 developing liquid developing is used, developing time is 0.5 ~ 5min, continue after with the microfluidic channel figure on microscopic examination photosensitive dry film, if the blur margin remaining photosensitive dry film or microfluidic channel in the microfluidic channel in figure is clear, then repeat aforementioned development operation, until the photosensitive dry film that is inner and microfluidic channel edge of the microfluidic channel in figure is completely removed, after development, the dry water removed between photosensitive dry film and glass substrate;
Described developer solution is by Na
2cO
3formulated with deionized water, in developer solution, Na
2cO
3be 1:(50 ~ 100 with the mass ratio of deionized water);
(6) microfluidic channel is etched
It is etch microfluidic channel in the etching liquid of 20 ~ 40 DEG C that the glass substrate being pasted with photosensitive dry film after step (5) being developed is immersed in temperature, in etching process, disturbance is carried out to etching liquid, etch period is no more than the tolerance time of described photosensitive dry film in etching liquid, after etching terminates, the glass substrate being pasted with photosensitive dry film is taken out, be placed in the photosensitive dry film on deionized water washing removal glass substrate and etching liquid, namely obtain the glass substrate being etched with 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 adds the concentrated hydrochloric acid of 37.5wt% in the buffer oxide etching liquid after dilution, mixes and obtains etching liquid; Described NH
4the volume ratio of the F aqueous solution and the HF aqueous solution is (6 ~ 7): 1, the volume ratio of described deionized water and buffer oxide etching liquid is (1 ~ 7): 1, and 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 being covered step (6) gained is etched with on the glass substrate of microfluidic channel, uses ultraviolet light polymerization glue by described sheet glass and glass substrate bonding, namely forms microfluidic device; The entrance and exit corresponding section of described sheet glass and microfluidic channel is provided with through hole.
In step (1) in said method, the mapping software of design microfluidic channel figure can be AutoCAD, CorelDRAW or Protel99SE.
In the step (2) of said method, the complete glass substrate of cleaning is dried to its surface at 60 ~ 150 DEG C anhydrous.
In the step (3) of said method, use laminator to cross after being attached at by photosensitive dry film on glass plate and mould 2 ~ 4 times, cross after having moulded, preferably photosensitive glass plate is cooled to room temperature and carries out next step operation again.
The step (3) of said method 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 (4) of said method, the time of uv-exposure is relevant with the performance of uv-exposure case, and microfluidic channel figure during control uv-exposure on chien shih photo etched mask is transferred on photosensitive dry film completely.
In the step (5) of said method, the temperature controlling developer solution is 25 ~ 35 DEG C.
In the step (5) of said method, after development, carry out the dry water removed between photosensitive dry film and glass substrate at 60 ~ 100 DEG C.
In the step (6) of said method, the tolerance time of described photosensitive dry film in etching liquid refers to that photosensitive dry film starts to depart from the time of glass substrate disengaging in etching process, and etch period is preferably 1 ~ 30min.
In the step (6) of said method, by stirring or carrying out disturbance by the mode of bubbler bubbling to etching liquid.
In the step (6) of said method, after etching terminates, the glass substrate that will be pasted with photosensitive dry film takes out, and is placed in deionized water and removes photosensitive dry film on glass substrate and etching liquid in the mode of Ultrasonic Cleaning.
If the step of said method (6) gained glass substrate only includes a microfluidic channel, then the shape of the sheet glass above the microfluidic channel of step (7) described glass substrate and size at least should cover the microfluidic channel on described glass substrate completely; If the step of said method (6) gained glass substrate comprises multiple microfluidic channel, then described glass substrate first should be divided into the fritter only comprising a microfluidic channel by step (7), and the shape of step (7) described sheet glass and size at least should cover the microfluidic channel on the pieces of glass substrate after described segmentation 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 taking photosensitive dry film as etching mask and make glass microfluidic devices, because the method uses photosensitive dry film as the etching mask of glass microfluidic devices wet etching, adopt common laminator photosensitive dry film can be pasted when making microfluidic device and form etching mask on the glass substrate, avoid the troublesome operation of spin coating liquid photoresist in existing etching mask preparation process and depositing metal layers, therefore, the method of the invention simplifies the manufacturing process of glass microfluidic devices, reduce its manufacture difficulty simultaneously.
2, because the method for the invention is very low to the requirement of environment, making apparatus in the process making glass microfluidic devices, adopt conventional equipment can realize the making of glass microfluidic devices, without the need to using ultra-clean working environment, more without the need to 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 uses relative to liquid photoresist and sputtering precious metal price very cheap, therefore the method for the invention significantly reduces the cost of manufacture of glass microfluidic devices.
3, the method for the invention can attach disposable for photosensitive dry film on the glass substrate in large area when making glass microfluidic devices; then by wet etching, microfluidic channel figure mass is transferred to (see embodiment 6) on glass substrate; this kind of production method effectively can not only 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 etching the microfluidic channel obtained is high, the microfluidic channel inner wall smooth of the glass microfluidic devices made, remain 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 the photosensitive dry film material used in the described method of invention, in figure, the photoresist oxidant layer that polyethylene (PE) film of 1-photosensitive dry film inner surface, 2-photosensitive dry film are middle, polyester (PET) film of 3-photosensitive dry film outer surface.
Fig. 2 is the schematic flow sheet that the described method of invention makes 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 is b) the average etching rate curve of the microfluidic channel on glass substrate in the etching liquid of different temperatures, variable concentrations, and figure is c) the maximum etching depth block diagram of microfluidic channel on glass substrate in the etching liquid of different temperatures, variable concentrations.
Fig. 4 be etch different time in embodiment 2 glass substrate on the cross-sectional scans Electronic Speculum figure of microfluidic channel.
Fig. 5 is the relation curve that the width of microfluidic channel in embodiment 2 and the degree of depth change with etch period.
Fig. 6 is the common microfluidic channel figure using AutoCAD Software for Design, and a) being Y shape passage, b) is crisscrossing channels, c) be T-shaped passage, d) being 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 development in embodiment 3.
Fig. 8 is the optical microscope photograph having etched microfluidic channel on rear glass substrate in embodiment 3.
Fig. 9 is the photo of the glass microfluidic devices that embodiment 3 makes.
Figure 10 is the array T-shaped microfluidic channel figure using AutoCAD Software for Design in embodiment 6.
The photo of microfluidic channel when Figure 11 is embodiment 6 batch making glass microfluidic devices after development on photosensitive dry film;
Figure 12 has etched the photo of microfluidic channel on rear glass substrate when being embodiment 6 batch making glass microfluidic devices;
Figure 13 is the photo of the glass microfluidic devices of embodiment 6 batch making.
Detailed description of the invention
By the following examples and by reference to the accompanying drawings the method with photosensitive dry film being etching mask makes glass microfluidic devices of the present invention is described further.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 used in embodiment 1 ~ 5 is 1.1mm; The thickness of the soda-lime glass used 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, the schematic flow sheet making glass microfluidic devices is shown in Fig. 2, and step is as follows:
(1) photo etched mask is made
Use AutoCAD Software on Drawing linear microfluidic channel figure, the width place of microfluidic channel is 300 μm.After microfluidic channel graphic designs completes, use the laser photocomposing machine that resolution ratio is 25400dpi that microfluidic channel graphic printing is formed photo etched mask on transparent film, each photo etched mask is of a size of 20mm × 30mm.This step makes 12 photo etched masks altogether.
(2) glass substrate is cleaned
Be glass substrate (totally 12 pieces) to be of a size of the slide of 25mm × 76mm, with acetone, glass substrate is carried out to ultrasonic cleaning 10min, then carries out ultrasonic cleaning 10min with ethanol to glass substrate, continue after by deionized water, ultrasonic cleaning 10min is carried out to glass substrate, to remove organic pollution and the solid particle of glass baseplate surface, glass substrate after cleaning is put into vacuum drying chamber in 60 DEG C of dry 1h, and glass baseplate surface is anhydrous.
(3) photosensitive glass plate is made
Photosensitive dry film is cut into 30mm × 80mm size (totally 12), first drip deionized water in glass substrate one end, then polyethylene (PE) film (see Fig. 1) of photosensitive dry film inner surface is opened, be covered on one end of glass substrate, photoresist oxidant layer in described photosensitive dry film contacts with glass substrate, put into laminator again and mould 3 times 93 DEG C of mistakes, formed photosensitive glass plate, it is placed under room temperature (20 DEG C) at least 15min make photosensitive glass plate be cooled to room temperature carry out again next step operation.The operation of this step is all carried out under yellow fluorescent lamp.
(4) expose
Under yellow fluorescent lamp, the photosensitive glass plate obtained in step (3) is placed in uv-exposure case, described photosensitive glass plate is pasted with the placement that faces up of photosensitive dry film, then the photo etched mask obtained 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 the vacuum clip in uv-exposure case locked and open vavuum pump, exposure is started when being evacuated to photo etched mask pressed glass substrate, 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, place 15min with the light polymers complete reaction in the photosensitive dry film after making exposure in room temperature (20 DEG C) lucifuge.
(5) develop
Preparing developer liquid: by Na
2cO
3add deionized water for stirring and evenly form developer solution, Na
2cO
3be 1:70 with the mass ratio of deionized water.
Polyester (PET) film on removing step (4) gained photosensitive glass plate photosensitive dry film, then with developer solution, spray development is carried out to the photosensitive dry film after exposure, the temperature of developer solution is 30 DEG C, developing time is 2min, continue after to be transferred to microfluidic channel figure on photosensitive dry film with microscopic examination, find that the microfluidic channel pattern edge after development is clear, the appearance such as nothing left glue burr, the drying glue platform that glass substrate after development is placed on 65 DEG C is toasted 1.5h to remove the water between photosensitive dry film and glass substrate, thus 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 carries out being mixed to form buffer oxide etching liquid (Buffered oxide etchant according to volume ratio, be called for short BOE), get 4 parts of BOE, be 0:1 by deionized water according to the volume ratio of deionized water and BOE respectively, 1:1, 3:1, the ratio of 7:1 is diluted, the concentrated hydrochloric acid of 37.5wt% is added again in the BOE after dilution, BOE after described dilution and the volume ratio of concentrated hydrochloric acid are 10:2, mix the etching liquid obtaining 4 kinds of different B OE concentration, 1/1BOE is denoted as successively from low to high according to the extension rate of BOE, 1/2BOE, 1/4BOE, 1/8BOE.
Get 1/1BOE etching liquid 3 parts, respectively each for the glass substrate being pasted with photosensitive dry film after the development of step (5) gained 1 piece is hung vertically in etching liquid and etches microfluidic channel, the temperature using circulator bath to control etching liquid is respectively 20 DEG C, 30 DEG C, 40 DEG C, etching liquid should flood described glass substrate completely, uses bubbler to etching liquid bubbling to increase the disturbance of etching liquid in etching process.Observe the state of a photosensitive dry film and glass baseplate every 1min in etching process, when photosensitive dry film starts to depart from glass substrate, immediately glass substrate is taken out and be placed in the supersonic wave cleaning machine cleaning that deionized water is housed and remove photosensitive dry film on glass substrate and etching liquid, the glass substrate of microfluidic channel must be etched with.
Get 1/2BOE etching liquid 3 parts, respectively each for the glass substrate being pasted with photosensitive dry film after the development of step (5) gained 1 piece is hung vertically in etching liquid and etches microfluidic channel, the temperature using circulator bath to control etching liquid is respectively 20 DEG C, 30 DEG C, 40 DEG C, etching liquid should flood described glass substrate completely, uses bubbler to etching liquid bubbling to increase the disturbance of etching liquid in etching process.Observe the state of a photosensitive dry film and glass baseplate every 1min in etching process, when photosensitive dry film starts to depart from glass substrate, immediately glass substrate is taken out and be placed in the supersonic wave cleaning machine cleaning that deionized water is housed and remove photosensitive dry film on glass substrate and etching liquid, the glass substrate of microfluidic channel must be etched with.
Get 1/4BOE etching liquid 3 parts, respectively each for the glass substrate being pasted with photosensitive dry film after the development of step (5) gained 1 piece is hung vertically in etching liquid and etches microfluidic channel, the temperature using circulator bath to control etching liquid is respectively 20 DEG C, 30 DEG C, 40 DEG C, etching liquid should flood described glass substrate completely, uses bubbler to etching liquid bubbling to increase the disturbance of etching liquid in etching process.Observe the state of a photosensitive dry film and glass baseplate every 1min in etching process, when photosensitive dry film starts to depart from glass substrate, immediately glass substrate is taken out and be placed in the supersonic wave cleaning machine cleaning that deionized water is housed and remove photosensitive dry film on glass substrate and etching liquid, the glass substrate of microfluidic channel must be etched with.
Get 1/8BOE etching liquid 3 parts, respectively each for the glass substrate being pasted with photosensitive dry film after the development of step (5) gained 1 piece is hung vertically in etching liquid and etches microfluidic channel, the temperature using circulator bath to control etching liquid is respectively 20 DEG C, 30 DEG C, 40 DEG C, etching liquid should flood described glass substrate completely, uses bubbler to etching liquid bubbling to increase the disturbance of etching liquid in etching process.Observe the state of a photosensitive dry film and glass baseplate every 1min in etching process, when photosensitive dry film starts to depart from glass substrate, immediately glass substrate is taken out and be placed in the supersonic wave cleaning machine cleaning that deionized water is housed and remove photosensitive dry film on glass substrate and etching liquid, the glass substrate of microfluidic channel must be etched with.
Attach the photosensitive dry film on the glass substrate tolerance time curve in the etching liquid of different temperatures, variable concentrations as Fig. 3 a) shown in, from Fig. 3 a), when BOE concentration one timing in etching liquid, along with the increase of etching liquid temperature, the tolerance time of photosensitive dry film in etching liquid is in the trend shortened; When etching liquid temperature one timing, the tolerance time of photosensitive dry film in etching liquid shortens with the reduction of 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) shown in, from Fig. 3 b), when BOE concentration one timing in etching liquid, on glass substrate, the average etching rate of microfluidic channel increases along with the rising of etching liquid temperature; When etching liquid temperature one timing, on glass substrate microfluidic channel average etching rate along with the reduction of BOE concentration in etching solution be the trend of first increases and then decreases, the average etching rate in 1/2BOE is maximum; When the temperature of etching liquid be 40 DEG C, concentration be 1/2BOE time, etch rate is maximum, can reach 4.95 μm/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 DEG C, the etching liquid of 1/1BOE concentration and 30 DEG C, in the etching liquid of 1/2BOE concentration, the maximum microchannel etching depth of microfluidic channel is 102 μm, this degree of depth can meet the application requirement of most of fields micro-fluidic technologies, but because in the etching liquid of 1/1BOE concentration, HF concentration is higher, during operation, danger is higher, therefore, when preparing etching liquid, deionized water usually should be adopted to dilute BOE.
In actual fabrication process, can according to the temperature of different microfluidic devices to the concrete selective etching liquid of requirement of channel depth and width, the content of each composition and etch period in etching liquid.
(7) bonding microfluidic device
The slide being of a size of 25mm × 25mm being covered step (6) gained is etched with in the microfluidic channel of the glass substrate of microfluidic channel, marks at the entrance of microfluidic channel and exit with marking pen.The electric current arranging ultrasonic drilling machine is about 1.2A, and regulating frequency knob makes circuit resonance, punches in the position of mark, uses the mixed liquor of diamond dust and running water constantly to wash away punch position, to improve drilling quality and trepanning velocity in the process of punching.The slide punched is cleaned 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 the microfluidic channel on glass substrate, click and enter ultraviolet light polymerization glue in slide and the glass substrate edge that fits and examining under a microscope, solidified with ultra violet lamp 15s after ultraviolet light polymerization glue is full of bond area under capillary action, namely formed microfluidic device.
Embodiment 2
In the present embodiment, the schematic flow sheet making glass microfluidic devices is shown in Fig. 2, and step is as follows:
(1) photo etched mask is made
Use AutoCAD Software on Drawing linear microfluidic channel figure, the width place of microfluidic channel is 300 μm.After microfluidic channel graphic designs completes, use the laser photocomposing machine that resolution ratio is 25400dpi that microfluidic channel graphic printing is formed photo etched mask on transparent film, each photo etched mask is of a size of 20mm × 30mm.This step makes 6 photo etched masks altogether.
(2) glass substrate is cleaned
Be glass substrate (totally 6 pieces) to be of a size of the slide of 25mm × 76mm, with acetone, glass substrate is carried out to ultrasonic cleaning 10min, then carries out ultrasonic cleaning 10min with ethanol to glass substrate, continue after by deionized water, ultrasonic cleaning 10min is carried out to glass substrate, to remove organic pollution and the solid particle of glass baseplate surface, glass substrate after cleaning is put into vacuum drying chamber in 150 DEG C of dry 30min, and glass baseplate surface is anhydrous.
(3) photosensitive glass plate is made
Photosensitive dry film is cut into 30mm × 80mm size (totally 6), first drip deionized water in glass substrate one end, then polyethylene (PE) film (see Fig. 1) of photosensitive dry film inner surface is opened, be covered on one end of glass substrate, photoresist oxidant layer in described photosensitive dry film contacts with glass substrate, put into laminator again and mould 4 times 90 DEG C of mistakes, formed photosensitive glass plate, it is placed under room temperature (20 DEG C) at least 15min make photosensitive glass plate be cooled to room temperature carry out again next step operation.The operation of this step is all carried out under yellow fluorescent lamp.
(4) expose
Under yellow fluorescent lamp, the photosensitive glass plate obtained in step (3) is placed in uv-exposure case, described photosensitive glass plate is pasted with the placement that faces up of photosensitive dry film, then the photo etched mask obtained 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 the vacuum clip in uv-exposure case locked and open vavuum pump, exposure is started when being evacuated to photo etched mask pressed glass substrate, 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, place 15min with the light polymers complete reaction in the photosensitive dry film after making exposure in room temperature (20 DEG C) lucifuge.
(5) develop
Preparing developer liquid: by Na
2cO
3add deionized water for stirring and evenly form developer solution, Na
2cO
3be 1:70 with the mass ratio of deionized water.
Polyester (PET) film on removing step (4) gained photosensitive glass plate photosensitive dry film, then with developer solution, spray development is carried out to the photosensitive dry film after exposure, the temperature of developer solution is 30 DEG C, developing time is 2min, continue after to be transferred to microfluidic channel figure on photosensitive dry film with microscopic examination, find that the microfluidic channel pattern edge after development is clear, the appearance such as nothing left glue burr, the drying glue platform that glass substrate after development is placed on 100 DEG C is toasted 1h to remove the water between photosensitive dry film and glass substrate, thus 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 carries out being mixed to form buffer oxide etching liquid (BOE) according to volume ratio, dilute according to the ratio that the volume ratio of deionized water and BOE is 1:1 by deionized water respectively, the concentrated hydrochloric acid of 37.5wt% is added again in the BOE after dilution, BOE after described dilution and the volume ratio of concentrated hydrochloric acid are 10:2, mix and obtain etching liquid.
The glass substrate being pasted with photosensitive dry film after 6 pieces of step (5) gained developments is hung vertically in etching liquid and etches microfluidic channel, the temperature using circulator bath to control etching liquid is 30 DEG C, etching liquid should flood described glass substrate completely, bubbler is used to etching liquid bubbling to increase the disturbance of etching liquid in etching process, the etch period of 6 pieces of glass substrates is respectively 5min, 10min, 15min, 20min, 25min, 30min, after etching terminates, the glass substrate being pasted with photosensitive dry film is taken out and is placed in the supersonic wave cleaning machine cleaning that deionized water is housed and removes photosensitive dry film on glass substrate and etching liquid, the glass substrate of microfluidic channel must be etched with.
On the glass substrate of etching different time, the cross-sectional scans Electronic Speculum figure of microfluidic channel as shown in Figure 4, and as shown in Figure 4, along with the increase of etch period, the degree of depth of microfluidic channel increases, 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 and the width of microfluidic channel 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, suitable etch period can be selected according to the width of microfluidic channel and the degree of depth with the relation curve that etch period changes.
(7) bonding microfluidic device
The slide being of a size of 25mm × 25mm being covered step (6) gained is etched with in the microfluidic channel of the glass substrate of microfluidic channel, marks at the entrance of microfluidic channel and exit with marking pen.The electric current arranging ultrasonic drilling machine is about 1.2A, and regulating frequency knob makes circuit resonance, punches in the position of mark, uses the mixed liquor of diamond dust and running water constantly to wash away punch position, to improve drilling quality and trepanning velocity in the process of punching.The slide punched is cleaned 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 the microfluidic channel on glass substrate, click and enter ultraviolet light polymerization glue in slide and the glass substrate edge that fits and examining under a microscope, solidified with ultra violet lamp 15s after ultraviolet light polymerization glue is full of bond area under capillary action, namely formed microfluidic device.
Embodiment 3
In the present embodiment, the schematic flow sheet making glass microfluidic devices is shown in Fig. 2, and step is as follows:
(1) photo etched mask is made
Use AutoCAD Software on Drawing six kinds common microfluidic channel figure as shown in Figure 6, in Fig. 6, a) for Y shape passage, b) for crisscrossing channels, c) for T-shaped passage, d) for diesis shape passage, e) for snakelike hybrid channel, f) be concentration gradient passage.Its maximum width of design of micro fluidic channels is 400 μm, and minimum widith place is 200 μm.After microfluidic channel graphic designs completes, use the laser photocomposing machine that resolution ratio is 25400dpi that microfluidic channel graphic printing is formed photo etched mask on transparent film, each photo etched mask size is 20mm × 30mm.
(2) glass substrate is cleaned
To be of a size of the slide of 25mm × 76mm for glass substrate, with acetone, glass substrate is carried out to ultrasonic cleaning 10min, then carries out ultrasonic cleaning 10min with ethanol to glass substrate, continue after by deionized water, ultrasonic cleaning 10min is carried out to glass substrate, to remove organic pollution and the solid particle of glass baseplate surface, glass substrate after cleaning is put into vacuum drying chamber in 60 DEG C of dry 1h, and glass baseplate surface is anhydrous.
(3) photosensitive glass plate is made
Photosensitive dry film is cut into 30mm × 80mm size, first drip deionized water in glass substrate one end, then polyethylene (PE) film (see Fig. 1) of photosensitive dry film inner surface is opened, be covered on one end of glass substrate, photoresist oxidant layer in described photosensitive dry film contacts with glass substrate, put into laminator again and mould 3 times 93 DEG C of mistakes, formed photosensitive glass plate, it is placed under room temperature (20 DEG C) at least 15min make photosensitive glass plate be cooled to room temperature carry out again next step operation.The operation of this step is all carried out under yellow fluorescent lamp.
(4) expose
Under yellow fluorescent lamp, the photosensitive glass plate obtained in step (3) is placed in uv-exposure case, described photosensitive glass plate is pasted with the placement that faces up of photosensitive dry film, then the photo etched mask obtained 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 the vacuum clip in uv-exposure case locked and open vavuum pump, exposure is started when being evacuated to photo etched mask pressed glass substrate, 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, place 15min with the light polymers complete reaction in the photosensitive dry film after making exposure in room temperature (20 DEG C) lucifuge.
(5) develop
Preparing developer liquid: by Na
2cO
3add deionized water for stirring and evenly form developer solution, Na
2cO
3be 1:70 with the mass ratio of deionized water.
Polyester (PET) film on removing step (4) gained photosensitive glass plate photosensitive dry film, then carry out spray development with developer solution to the photosensitive dry film after exposure, the temperature of developer solution is 30 DEG C, developing time is 2min; Continue after to be transferred to microfluidic channel figure on photosensitive dry film with microscopic examination, the optical microscope photograph of the microfluidic channel figure on the photosensitive dry film of the rear photosensitive glass plate of 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, drying glue platform glass substrate being placed on 65 DEG C toasts 1.5h to remove the water between photosensitive dry film and glass substrate, thus 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 carries out being mixed to form buffer oxide etching liquid (being called for short BOE) according to volume ratio, dilute according to the ratio that the volume ratio of deionized water and BOE is 1:1 by deionized water respectively, the concentrated hydrochloric acid of 37.5wt% is added again in the BOE after dilution, BOE after described dilution and the volume ratio of concentrated hydrochloric acid are 10:2, mix and obtain etching liquid.
The glass substrate being pasted with photosensitive dry film after being developed by step (5) gained is hung vertically in etching liquid and etches microfluidic channel, the temperature using circulator bath to control etching liquid is 30 DEG C, etching liquid should flood described glass substrate completely, bubbler is used to etching liquid bubbling to increase the disturbance of etching liquid in etching process, etch period is 30min, after etching terminates, the glass substrate being pasted with photosensitive dry film is taken out and is placed in the supersonic wave cleaning machine cleaning that deionized water is housed and removes photosensitive dry film on glass substrate and etching liquid, the glass substrate of microfluidic channel must be etched with.Etch the optical microscope photograph of microfluidic channel on rear glass substrate as shown in Figure 8.
(7) bonding microfluidic device
The slide being of a size of 25mm × 25mm being covered step (6) gained is etched with in the microfluidic channel of the glass substrate of microfluidic channel, marks at the entrance of microfluidic channel and exit with marking pen.The electric current arranging ultrasonic drilling machine is about 1.2A, and regulating frequency knob makes circuit resonance, punches in the position of mark, uses the mixed liquor of diamond dust and running water constantly to wash away punch position, to improve drilling quality and trepanning velocity in the process of punching.The slide punched is cleaned 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 the microfluidic channel on glass substrate, click and enter ultraviolet light polymerization glue in slide and the glass substrate edge that fits and examining under a microscope, solidified with ultra violet lamp 15s after ultraviolet light polymerization glue is full of bond area under capillary action, namely formed microfluidic device.Finally paste at the tapping at perforate slide and connect polyethylene hose, after injecting methylene blue by polyethylene hose in microfluidic channel, the photo of glass microfluidic devices as shown in Figure 9, clearly can find out the shape of six kinds of microfluidic channel from Fig. 9.
In the present embodiment, the success rate using ultraviolet light polymerization glue to carry out bonding to microfluidic device is 100%, and the time needed for bonding microfluidic device is no more than 10min, and bonding efficiency is high.With ultraviolet light polymerization glue bonding glass microfluidic devices without the need to special installation and particular surroundings, the processing cost of glass microfluidic devices can be reduced.
Embodiment 4
In the present embodiment, the schematic flow sheet making glass microfluidic devices is shown in Fig. 2, and step is as follows:
(1) photo etched mask is made
Use AutoCAD Software on Drawing as Fig. 6 c) shown in T-shaped passage, its maximum width of design of micro fluidic channels is 400 μm, and minimum widith place is 200 μm.After microfluidic channel graphic designs completes, use the laser photocomposing machine that resolution ratio is 25400dpi that microfluidic channel graphic printing is formed photo etched mask on transparent film, photo etched mask is of a size of 20mm × 30mm.
(2) glass substrate is cleaned
To be of a size of the slide of 25mm × 76mm for glass substrate, with ethanol, glass substrate is carried out to ultrasonic cleaning 10min, then carries out ultrasonic cleaning 10min with acetone to glass substrate, continue after by deionized water, ultrasonic cleaning 10min is carried out to glass substrate, to remove organic pollution and the solid particle of glass baseplate surface, glass substrate after cleaning is put into vacuum drying chamber in 150 DEG C of dry 30min, and glass baseplate surface is anhydrous.
(3) photosensitive glass plate is made
Photosensitive dry film is cut into 30mm × 80mm size, first drip deionized water in glass substrate one end, then polyethylene (PE) film (see Fig. 1) of photosensitive dry film inner surface is opened, be covered on one end of glass substrate, photoresist oxidant layer in described photosensitive dry film contacts with glass substrate, put into laminator again and mould 2 times 95 DEG C of mistakes, formed photosensitive glass plate, it is placed under room temperature (20 DEG C) at least 15min make photosensitive glass plate be cooled to room temperature carry out again next step operation.The operation of this step is all carried out under yellow fluorescent lamp.
(4) expose
Under yellow fluorescent lamp, the photosensitive glass plate obtained in step (3) is placed in uv-exposure case, described photosensitive glass plate is pasted with the placement that faces up of photosensitive dry film, then the photo etched mask obtained 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 the vacuum clip in uv-exposure case locked and open vavuum pump, exposure is started when being evacuated to photo etched mask pressed glass substrate, 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, place 10min with the light polymers complete reaction in the photosensitive dry film after making exposure in room temperature (20 DEG C) lucifuge.
(5) develop
Preparing developer liquid: by Na
2cO
3add deionized water for stirring and evenly form developer solution, Na
2cO
3be 1:50 with the mass ratio of deionized water.
Polyester (PET) film on removing step (4) gained photosensitive glass plate photosensitive dry film, then carry out spray development with developer solution to the photosensitive dry film after exposure, the temperature of developer solution is 35 DEG C, developing time is 30s; Continue after to be transferred to microfluidic channel figure on photosensitive dry film with microscopic examination, 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, drying glue platform glass substrate being placed on 100 DEG C toasts 1h to remove the water between photosensitive dry film and glass substrate, thus 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 carries out being mixed to form buffer oxide etching liquid (BOE) according to volume ratio, dilute according to the ratio that the volume ratio of deionized water and BOE is 1:1 by deionized water respectively, the concentrated hydrochloric acid of 37.5wt% is added again in the BOE after dilution, BOE after described dilution and the volume ratio of concentrated hydrochloric acid are 10:1, mix and obtain etching liquid.
The glass substrate being pasted with photosensitive dry film after being developed by step (5) gained is hung vertically in etching liquid and etches microfluidic channel, the temperature using circulator bath to control etching liquid is 30 DEG C, etching liquid should flood described glass substrate completely, the disturbance stirring to increase etching liquid is carried out in etching process, etch period is 1min, after etching terminates, the glass substrate being pasted with photosensitive dry film is taken out and is placed in the supersonic wave cleaning machine cleaning that deionized water is housed and removes photosensitive dry film on glass substrate and etching liquid, the glass substrate of microfluidic channel must be etched with.
(7) bonding microfluidic device
The slide being of a size of 25mm × 25mm being covered step (6) gained is etched with in the microfluidic channel of the glass substrate of microfluidic channel, marks at the entrance of microfluidic channel and exit with marking pen.The electric current arranging ultrasonic drilling machine is about 1.2A, and regulating frequency knob makes circuit resonance, punches in the position of mark, uses the mixed liquor of diamond dust and running water constantly to wash away punch position, to improve drilling quality and trepanning velocity in the process of punching.The slide punched is cleaned 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 the microfluidic channel on glass substrate, click and enter ultraviolet light polymerization glue in slide and the glass substrate edge that fits and examining under a microscope, solidified with ultra violet lamp 15s after ultraviolet light polymerization glue is full of bond area under capillary action, namely formed microfluidic device.Finally paste at the tapping at perforate slide and connect polyethylene hose.
Embodiment 5
In the present embodiment, the schematic flow sheet making glass microfluidic devices is shown in Fig. 2, and step is as follows:
(1) photo etched mask is made
Use AutoCAD Software on Drawing as Fig. 6 a) shown in Y shape passage, its maximum width of design of micro fluidic channels is 400 μm, and minimum widith place is 200 μm.After microfluidic channel graphic designs completes, use the laser photocomposing machine that resolution ratio is 25400dpi that microfluidic channel graphic printing is formed photo etched mask on transparent film, photo etched mask is of a size of 20mm × 30mm.
(2) glass substrate is cleaned
To be of a size of the slide of 25mm × 76mm for glass substrate, with acetone, glass substrate is carried out to ultrasonic cleaning 10min, then carries out ultrasonic cleaning 10min with ethanol to glass substrate, continue after by deionized water, ultrasonic cleaning 10min is carried out to glass substrate, to remove organic pollution and the solid particle of glass baseplate surface, glass substrate after cleaning is put into vacuum drying chamber in 100 DEG C of dry 40min, and glass baseplate surface is anhydrous.
(3) photosensitive glass plate is made
Photosensitive dry film is cut into 30mm × 80mm size, first drip deionized water in glass substrate one end, then under yellow fluorescent lamp, open polyethylene (PE) film (see Fig. 1) of photosensitive dry film inner surface, be covered on one end of glass substrate, photoresist oxidant layer in described photosensitive dry film contacts with glass substrate, put into laminator again and mould 3 times 93 DEG C of mistakes, formed photosensitive glass plate, it is placed under room temperature (20 DEG C) at least 15min make photosensitive glass plate be cooled to room temperature carry out again next step operation.The operation of this step is all carried out under yellow fluorescent lamp.
(4) expose
Under yellow fluorescent lamp, the photosensitive glass plate obtained in step (3) is placed in uv-exposure case, described photosensitive glass plate is pasted with the placement that faces up of photosensitive dry film, then the photo etched mask obtained 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 the vacuum clip in uv-exposure case locked and open vavuum pump, exposure is started when being evacuated to photo etched mask pressed glass substrate, 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, place 15min with the light polymers complete reaction in the photosensitive dry film after making exposure in room temperature (20 DEG C) lucifuge.
(5) develop
The configuration of developer solution: by Na
2cO
3add deionized water for stirring and evenly form developer solution, Na
2cO
3be 1:100 with the mass ratio of deionized water.
Polyester (PET) film (as shown in Figure 1) on the photosensitive glass plate upper strata after the exposure obtained in step (4) is thrown off, uses Na
2cO
3developer solution carries out spray development to the photosensitive dry film after exposure, development temperature controls at 25 DEG C, and developing time is 5min, continue after to be transferred to microfluidic channel figure on photosensitive dry film with microscopic examination, find that the microfluidic channel pattern edge after development is clear, the appearance such as nothing left glue burr.After development, drying glue platform glass baseplate being positioned over 100 DEG C toasts 1h to remove the water of photosensitive dry film bottom, thus 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 carries out being mixed to form buffer oxide etching liquid (BOE) according to volume ratio, dilute according to the ratio that the volume ratio of deionized water and BOE is 1:1 by deionized water respectively, the concentrated hydrochloric acid of 37.5wt% is added again in the BOE after dilution, BOE after described dilution and the volume ratio of concentrated hydrochloric acid are 10:3, mix and obtain etching liquid.
The glass substrate being pasted with photosensitive dry film after being developed by step (5) gained is hung vertically in etching liquid and etches microfluidic channel, the temperature using circulator bath to control etching liquid is 30 DEG C, etching liquid should flood described glass substrate completely, bubbler is used to etching liquid bubbling to increase the disturbance of etching liquid in etching process, etch period is 20min, after etching terminates, the glass substrate being pasted with photosensitive dry film is taken out and is placed in the supersonic wave cleaning machine cleaning that deionized water is housed and removes photosensitive dry film on glass substrate and etching liquid, the glass substrate of microfluidic channel must be etched with.
(7) bonding microfluidic device
The slide being of a size of 25mm × 25mm being covered step (6) gained is etched with in the microfluidic channel of the glass substrate of microfluidic channel, marks at the entrance of microfluidic channel and exit with marking pen.The electric current arranging ultrasonic drilling machine is about 1.2A, and regulating frequency knob makes circuit resonance, punches in the position of mark, uses the mixed liquor of diamond dust and running water constantly to wash away punch position, to improve drilling quality and trepanning velocity in the process of punching.The slide punched is cleaned 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 the microfluidic channel on glass substrate, click and enter ultraviolet light polymerization glue in slide and the glass substrate edge that fits and examining under a microscope, solidified with ultra violet lamp 15s after ultraviolet light polymerization glue is full of bond area under capillary action, namely formed microfluidic device.Finally paste at the tapping at perforate slide and connect polyethylene hose.
Embodiment 6
In the present embodiment, for T-shaped microfluidic channel, the method for batch making glass microfluidic devices is described, step is as follows:
(1) photo etched mask is made
Use AutoCAD Software on Drawing array T-shaped microfluidic channel figure as shown in Figure 10, its maximum width of design of micro fluidic channels is 400 μm, and minimum widith place is 200 μm.After microfluidic channel graphic designs completes, use the laser photocomposing machine that resolution ratio is 25400dpi that microfluidic channel graphic printing is formed photo etched mask on transparent film, photo etched mask is of a size of 60mm × 180mm.
(2) glass substrate is cleaned
To be of a size of the soda-lime glass of 60mm × 180mm for glass substrate, with acetone, glass substrate is carried out to ultrasonic cleaning 10min, then carries out ultrasonic cleaning 10min with ethanol to glass substrate, continue after by deionized water, ultrasonic cleaning 10min is carried out to glass substrate, to remove organic pollution and the solid particle of glass baseplate surface, glass substrate after cleaning is put into vacuum drying chamber in 60 DEG C of dry 1h, and glass baseplate surface is anhydrous.
(3) photosensitive glass plate is made
Photosensitive dry film is cut into 70mm × 190mm size, first drip deionized water in glass substrate one end, then polyethylene (PE) film (see Fig. 1) of photosensitive dry film inner surface is opened, be covered on one end of glass substrate, photoresist oxidant layer in described photosensitive dry film contacts with glass substrate, put into laminator again and mould 3 times 93 DEG C of mistakes, formed photosensitive glass plate, it is placed under room temperature (20 DEG C) at least 15min make photosensitive glass plate be cooled to room temperature carry out again next step operation.The operation of this step is all carried out under yellow fluorescent lamp.
(4) expose
Under yellow fluorescent lamp, the photosensitive glass plate obtained in step (3) is placed in uv-exposure case, described photosensitive glass plate is pasted with the placement that faces up of photosensitive dry film, then the photo etched mask obtained 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 the vacuum clip in uv-exposure case locked and open vavuum pump, exposure is started when being evacuated to photo etched mask pressed glass substrate, 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, place 15min with the light polymers complete reaction in the photosensitive dry film after making exposure in room temperature (20 DEG C) lucifuge.
(5) develop
Preparing developer liquid: by Na
2cO
3add deionized water for stirring and evenly form developer solution, Na
2cO
3be 1:70 with the mass ratio of deionized water.
Polyester (PET) film on removing step (4) gained photosensitive glass plate photosensitive dry film, then carry out spray development with developer solution to the photosensitive dry film after exposure, the temperature of developer solution is 30 DEG C, developing time is 2min; Continue after to be transferred to microfluidic channel figure on photosensitive dry film with microscopic examination, find that the microfluidic channel pattern edge after development is clear, the appearance such as nothing left glue burr, the photosensitive glass plate after development is as shown in figure 11.After development, drying glue platform glass substrate being placed on 65 DEG C toasts 2h to remove the water between photosensitive dry film and glass substrate, thus 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 carries out being mixed to form buffer oxide etching liquid (BOE) according to volume ratio, dilute according to the ratio that the volume ratio of deionized water and BOE is 1:1 by deionized water respectively, the concentrated hydrochloric acid of 37.5wt% is added again in the BOE after dilution, BOE after described dilution and the volume ratio of concentrated hydrochloric acid are 10:2, mix and obtain etching liquid;
Glass substrate step (5) gained being pasted with photosensitive dry film is hung vertically in etching liquid and etches microfluidic channel, the temperature using circulator bath to control etching liquid is 30 DEG C, etching liquid should flood described glass substrate completely, bubbler is used to etching liquid bubbling to increase the disturbance of etching liquid in etching process, etch period is 20min, after etching terminates, the glass substrate being pasted with photosensitive dry film is taken out and is placed in the supersonic wave cleaning machine cleaning that deionized water is housed and removes photosensitive dry film on glass substrate and etching liquid, the glass substrate of array T-shaped microfluidic channel must be etched with, as shown in figure 12, 24 T-shaped passages have been transferred on glass substrate once.
(7) bonding microfluidic device
Glass substrate glass cutter step (6) gained being etched with array T-shaped microfluidic channel is slit into fritter (20mm × 20mm), every block has the T-shaped microfluidic channel that complete.The slide that will be of a size of 25mm × 25mm covers above the microfluidic channel of glass substrate after singulation, marks at the entrance of microfluidic channel and exit with marking pen.The electric current arranging ultrasonic drilling machine is about 1.2A, and regulating frequency knob makes circuit resonance, punches in the position of mark, uses the mixed liquor of diamond dust and running water constantly to wash away punch position, to improve drilling quality and trepanning velocity in the process of punching.The slide punched is cleaned 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 the microfluidic channel on glass substrate, click and enter ultraviolet light polymerization glue in slide and the glass substrate edge that fits and examining under a microscope, solidified with ultra violet lamp 15s after ultraviolet light polymerization glue is full of bond area under capillary action, namely formed microfluidic device.Finally paste at the tapping at perforate slide and connect polyethylene hose, after injecting methylene blue by polyethylene hose in microfluidic channel, the optical photograph of microfluidic device as shown in figure 13, clearly can find out the shape of microfluidic channel microfluidic device from Figure 13.
In this embodiment, make 24 glass microfluidic devices about 12h consuming time altogether, total cost is less than 8 yuan, namely the glass microfluidic devices about 30min consuming time of 1 20mm × 20mm is made, cost about 0.3 yuan, the described method of this explanation invention is that the mass production of glass microfluidic devices provides a kind of cheap, efficient new way.
Claims (10)
1. be the method that etching mask makes glass microfluidic devices with photosensitive dry film, it is characterized in that step is as follows:
(1) photo etched mask is made
Use the microfluidic channel figure of mapping software design microfluidic device, with laser photocomposing machine, the microfluidic channel graphic printing designed is formed photo etched mask on transparent film;
(2) glass substrate is cleaned
Use washed with de-ionized water glass substrate again with after acetone, ethanol cleaning glass substrate respectively, to remove organic pollution and the solid particle of glass baseplate surface, then the glass substrate after cleaning is dried to its surface anhydrous;
(3) photosensitive glass plate is made
Photosensitive dry film is cut to the shape and size of step (2) described glass substrate, throw off the polyethylene film of photosensitive dry film and adopt wet film coating method to be attached on glass substrate by photosensitive dry film, photoresist oxidant layer in described photosensitive dry film contacts with glass substrate, then uses laminator at 90 ~ 95 DEG C of moulding one-tenth photosensitive glass plates of mistake;
(4) expose
Step (3) gained photosensitive glass plate is placed in uv-exposure case, described photosensitive glass plate is pasted with the placement that faces up of photosensitive dry film, then the photosensitive dry film photo etched mask that step (1) makes being covered photosensitive glass plate compresses, described photo etched mask print have carbon dust facing to photosensitive dry film, continue after make microfluidic channel Graphic transitions on photo etched mask on photosensitive dry film by uv-exposure, after end exposure, take off photo etched mask, taken out by photosensitive glass plate after exposure, lucifuge places at least 10min;
(5) develop
Polyester film on photosensitive glass plate photosensitive dry film after the exposure of removing step (4) gained, then developing liquid developing is used, developing time is 0.5 ~ 5min, continue after with the microfluidic channel figure on microscopic examination photosensitive dry film, if the blur margin remaining photosensitive dry film or microfluidic channel in the microfluidic channel in figure is clear, then repeat aforementioned development operation, until the photosensitive dry film that is inner and microfluidic channel edge of the microfluidic channel in figure is completely removed, after development, the dry water removed between photosensitive dry film and glass substrate;
Described developer solution is by Na
2cO
3formulated with deionized water, in developer solution, Na
2cO
3be 1:(50 ~ 100 with the mass ratio of deionized water);
(6) microfluidic channel is etched
It is etch microfluidic channel in the etching liquid of 20 ~ 40 DEG C that the glass substrate being pasted with photosensitive dry film after step (5) being developed is immersed in temperature, in etching process, disturbance is carried out to etching liquid, etch period is no more than the tolerance time of described photosensitive dry film in etching liquid, after etching terminates, the glass substrate being pasted with photosensitive dry film is taken out, be placed in the photosensitive dry film on deionized water washing removal glass substrate and etching liquid, namely obtain the glass substrate being etched with 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 adds the concentrated hydrochloric acid of 37.5wt% in the buffer oxide etching liquid after dilution, mixes and obtains etching liquid; Described NH
4the volume ratio of the F aqueous solution and the HF aqueous solution is (6 ~ 7): 1, the volume ratio of described deionized water and buffer oxide etching liquid is (1 ~ 7): 1, and 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 being covered step (6) gained is etched with on the glass substrate of microfluidic channel, uses ultraviolet light polymerization glue by described sheet glass and glass substrate bonding, namely forms microfluidic device; The entrance and exit corresponding section of described sheet glass and microfluidic channel is provided with through hole.
2. be the method that etching mask makes glass microfluidic devices according to claim 1 with photosensitive dry film, it is characterized in that the temperature of developer solution in step (5) controls at 25 ~ 35 DEG C.
3. be the method that etching mask makes glass microfluidic devices with photosensitive dry film according to claim 1 or 2, it is characterized in that the etch period in step (6) is 1 ~ 30min.
4. be the method that etching mask makes glass microfluidic devices with photosensitive dry film according to claim 1 or 2, it is characterized in that step (3) is carried out under yellow fluorescent lamp, step (4) medium ultraviolet exposure before operate in yellow fluorescent lamp under carry out.
5. be that etching mask makes the method for glass microfluidic devices according to claim 3 with photosensitive dry film, it is characterized in that step (3) is carried out under yellow fluorescent lamp, before the exposure of step (4) medium ultraviolet operate in yellow fluorescent lamp under carry out.
6. be the method that etching mask makes glass microfluidic devices with photosensitive dry film according to claim 1 or 2, it is characterized in that in step (5) after development, carry out the dry water removed between photosensitive dry film and glass substrate at 60 ~ 100 DEG C.
7. be the method that etching mask makes glass microfluidic devices with photosensitive dry film according to claim 1 or 2, it is characterized in that in step (6) by stirring or carrying out disturbance by the mode of bubbler bubbling to etching liquid.
8. be the method that etching mask makes glass microfluidic devices with photosensitive dry film according to claim 1 or 2, after it is characterized in that in step (6), etching terminates, the glass substrate that will be pasted with photosensitive dry film takes out, and is placed in deionized water and removes photosensitive dry film on glass substrate and etching liquid in the mode of Ultrasonic Cleaning.
9. be the method that etching mask makes glass microfluidic devices with photosensitive dry film according to 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 DEG C anhydrous.
10. be the method that etching mask makes glass microfluidic devices with photosensitive dry film according to claim 1 or 2, use laminator to cross after it is characterized in that being attached at by photosensitive dry film in step (3) on glass substrate and mould 2 ~ 4 times.
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| CN105420103A (en) * | 2015-12-07 | 2016-03-23 | 内江师范学院 | Simple micro-fluidic chip and cell analysis method |
| 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 |
| CN111645426A (en) * | 2020-04-24 | 2020-09-11 | 应嘉企业有限公司 | Glass product with printed picture and printing method thereof |
| US11914304B2 (en) * | 2021-08-05 | 2024-02-27 | Toyota Motor Engineering & Manufacturing North America, Inc. | Controlling porosity of an interference lithography process by fine tuning exposure time |
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