CN107252707B - A kind of microfluidic system and its preparation process - Google Patents
A kind of microfluidic system and its preparation process Download PDFInfo
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- CN107252707B CN107252707B CN201710405953.XA CN201710405953A CN107252707B CN 107252707 B CN107252707 B CN 107252707B CN 201710405953 A CN201710405953 A CN 201710405953A CN 107252707 B CN107252707 B CN 107252707B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
- B01L3/502707—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by the manufacture of the container or its components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B7/00—Microstructural systems; Auxiliary parts of microstructural devices or systems
- B81B7/0032—Packages or encapsulation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C3/00—Assembling of devices or systems from individually processed components
Abstract
The invention discloses a kind of microfluidic system and its preparation processes, the microfluidic system is mainly made of micro-fluidic chip and flexible battery chip, the flexible battery chip includes matrix and the tooth form area on matrix, the surface in tooth form area is provided with interdigital collector, the root of the interdigital collector and the stupefied line in top of tooth form area triangle are perpendicular, the finger portion of the interdigital collector is located at two central planes of triangle and parallel with the stupefied line in the top of triangle, is also covered with positive/negative active material in the finger portion of the interdigital collector.The present invention mainly combines 3D printing and micro-nano processing technology, quick Fabrication goes out the three-dimensional batteries system that energy density is high, small in size, integrated level is high, can bend repeatedly, the three-dimensional batteries system and micro-fluidic chip constitute an entirety, can power directly to micro-fluidic chip.
Description
Technical field
The invention belongs to microfluidic art more particularly to a kind of microfluidic systems and its preparation process.
Background technique
It is micro-fluidic to refer to the skill manipulated into the wide channel system of several hundred microns to fluid or gas at more than ten microns
Art.Using microflow control technique as core, the core applied to the fields such as biology, chemistry, biomedicine processed by MEMS technology
Piece type micro-total analysis system is referred to as micro-fluidic chip.Microfluidic chip technology main advantage has: required sample volume is small, detects
It is high-efficient, use cost is low and be easy to other technologies integration of equipments, be real with good compatibility, following developing direction
Existing portable inspectiont.
But micro mation system higher for integrated level, how to look for a micromation energy supply that can be matched
Device is the problem of currently encountering.Although having had on the market much about minicell, the product of flexible battery, he
Manufacturing process it is much all to be improved, need more innovative technologies to change it.Such as the Thinergy in the U.S.
The minicell for the MEC225 model that company produces, open electric circuit 4.1V, planar dimension are 12.7mm × 12.7mm, with a thickness of
0.17mm, the rated capacity 0.13mAh of battery.This product has been most reliable, most representative in minicell field
One of product.But its towards field be more electronic product, such as mobile phone, computer, manufacturing process majority also uses
The manufacturing process of film lithium cell is not met by the demand of more products customizable.Product at present on the market is made a general survey of, also
Do not have it is a both there is certain flexibility, and be the three-dimensional micro battery of high capacity.For micro-fluidic chip system, development side
To also to wearable, integrated level is high, portable etc. to be developed.It is this to have and bend repeatedly, it can be with mass production
Minicell be precisely at present required for micro-fluidic field.Since three-dimensional batteries have higher appearance relative to two-dimentional battery
Amount also can have more certain advantage relative to general hull cell in performance.
Summary of the invention
The main object of the present invention is to combine 3D printing and micro-nano processing technology, and quick Fabrication goes out energy density
It is high, small in size, can recurvation folding three-dimensional batteries system, and by the three-dimensional batteries system and micro-fluidic chip composition one it is whole
Body forms microfluidic system, and the microfluidic system integrated level is high, does not need additional circuit, can bend repeatedly.
In order to achieve the above object, present invention employs following preparation processes:
PDMS (dimethyl silicone polymer) glue is poured into production micro-fluidic chip matrix, flexible battery in mold by step 1
Chip basal body and upper cover, so that flexible battery chip basal body after molding and upper cover have tooth form area；Step 2, micro-fluidic
Microfluidic system is made in chip basal body, obtains micro-fluidic chip；Step 3 coats in the tooth form area of flexible battery chip basal body
Photoresist, Lithographic template in pressure recycle ultraviolet photolithographic machine photocuring, then sputter under the blocking of fixed exposure mask in tooth form area
Metal, grows positive/negative collector, the positive/negative collector is distributed in interdigital, wherein positive/negative collector
Root and the stupefied line in top of tooth form area triangle are perpendicular, the finger portion of positive/negative collector be located at two central planes of triangle and with
The stupefied line in the top of triangle is parallel, cleans photoresist, then positive/negative slurry is printed upon respectively on positive/negative collector, is obtained
To flexible battery chip；Step 4, using upper cover by micro-fluidic chip together with flexible battery chip package, the upper cover with
The tooth form area of flexible battery chip mutually coincide, and internal voids constitute the memory space of electrolyte.
As the improved technical solution of the present invention: in step 1, the micro-fluidic chip matrix uses gas permeability PMDS mono-
Body formed, the flexible battery chip basal body is integrally formed using air impermeability PMDS.
As the improved technical solution of the present invention: in step 1, the tooth form area of flexible battery chip basal body after molding has
There are the irrigation canals and ditches of interdigital, the root of the irrigation canals and ditches and the stupefied line in top of tooth form area triangle are perpendicular, the finger portion of the irrigation canals and ditches
Positioned at two central planes of triangle and parallel with the stupefied line in the top of triangle, the positive/negative collector is grown in the intersection
In the irrigation canals and ditches of finger-type.
As the improved technical solution of the present invention: in step 1, the peak height of tooth form area triangle is 50~3000 μm,
The bottom edge side length of triangle is 100~5000 μm.
As the improved technical solution of the present invention: in step 1, the bottom edge of tooth form area triangle is located at described matrix
Split on.
As the improved technical solution of the present invention: in step 1, micro-fluidic chip matrix and flexible battery core after molding
The engaging portion of sheet matrix is provided with concave-convex fit structure.
Preferably, the male-female engagement mode is tooth form, rivet type, T-type, circle.
As the improved technical solution of the present invention, in step 3, sputtered first under the blocking of permanent mask in tooth form area
Metallic nickel or chromium it is one or more, then respectively by custom mask, the splash-proofing sputtering metal aluminium on plus plate current-collecting body, negative pole currect collecting
Splash-proofing sputtering metal copper on body, metallic nickel, crome metal, metallic aluminium and metallic copper with a thickness of 1~100 μm.
Further, it makes super-hydrophobic channel: by specific laser pattern, laser burning being carried out to molding collector two sides
Knot after sintered, is respectively formed to form 50~500 μm wide of super-hydrophobic channel in interdigitation collector two sides, water droplet is on it
Hydrophobic angular region is 140 °~160 °.
As the improved technical solution of the present invention, in step 3, the positive/negative slurry the preparation method comprises the following steps: 1) will just/
Ball milling 4~for 24 hours in ball mill is added in negative electrode active material, conductive agent, and rotational speed of ball-mill is 100~1000rpm；It 2) will be after ball milling
Mixture is transferred in the glove box full of inert gas, and dispersing agent is added and grinds altogether, and grinding the time altogether is 5~60min, then will be total to
In mixture investment NMP after grinding, B/C slurry is obtained；3) in the glove box full of inert gas, binder is put into Isosorbide-5-Nitrae-
Dioxane dissolution, forms solution A；4) solution A and B/C slurry are mixed, is put into planet batch mixer and is blended, planet
The revolving speed of batch mixer is 1000~8000rpm, and the time is 2~20min, obtains positive/negative slurry.
Wherein, 1g positive/negative active material needs 0.05~0.1g of adapted conductive agent, 0.008~0.02g of dispersing agent, bonding
0.1~0.5g of agent, NMP1~3mL, 0.5~1mL of 1,4- dioxane.
As the improved technical solution of the present invention, in step 3, fid is printed while printing positive/negative slurry
Positive/negative slurry, i.e., is put into the center cavity of printer, backing material is put into the edge chamber of center cavity two sides, is beaten simultaneously by material
Print, removes backing material after printing.
Further, several layers of positive/negative slurries and backing material are first printed jointly, then only print on this basis several layers of
Positive/negative slurry.
Preferably, the configuration method of the backing material are as follows: 5~10 parts by weight parental type triblock copolymers are dissolved in 20
In the deionized water of parts by weight, it is put into magnetic agitation 6 in temperature control magnetic stirrer~for 24 hours, controlled at 2~6 DEG C to get arriving
Backing material.
Preferably, during printing positive/negative slurry, agitating device is in stirring, and mixing speed is 50~
200rpm, the temperature of slurry are 30~50 DEG C, and squeeze pressure is 200~1000psi, and sweep speed is 100~1000 μm/s.
As the improved technical solution of the present invention, in step 3, one of substance in the positive/negative active material
It is printed upon on positive or negative pole collector in U-typed, another substance is printed upon on cathode or plus plate current-collecting body in T-shape.
As the improved technical solution of the present invention: the subsequent operation of step 3 be it is printed after chip be put into -100~-
1~12h is dried in vacuo in 40 DEG C of vacuum oven.
As the improved technical solution of the present invention: the subsequent operation of step 4 is that injection is utilized under the protection of inert gas
Syringe needle pours into electrolyte in the electrolyte memory space of flexible battery chip, then blocks injection orifice using PMMA.Preferably,
The electrolyte is mixed using ethylene carbonate, dimethyl carbonate, methyl ethyl carbonate enester according to 1~3:1~3:1~3.
Had the following structure using microfluidic system made from above-mentioned technique: microfluidic system mainly by micro-fluidic chip and
Flexible battery chip is constituted, wherein flexible battery chip includes matrix and the tooth form area on matrix, on the surface in tooth form area
It is provided with interdigital collector, the root of the interdigital collector and the stupefied line in top of tooth form area triangle are perpendicular,
The finger portion of the interdigital collector is located at two central planes of triangle and parallel with the stupefied line in the top of triangle, in the intersection
Positive/negative active material is also covered in the finger portion of finger-type collector.
Further, it further includes upper cover, and the upper cover also has tooth form area, the tooth form area of the upper cover and the flexibility
The tooth form area of battery chip mutually coincide, to form the memory space of electrolyte.
Further, two central planes of the triangle have the irrigation canals and ditches that concave, the interdigital collector and described
Positive/negative active material is located in the irrigation canals and ditches.
Further, the peak height of the triangle is 50~3000 μm, and the bottom edge side length of the triangle is 100~5000
μm。
Further, the bottom edge of the triangle is located on the split of described matrix.
Further, the collector is divided into plus plate current-collecting body and negative current collector, the bottom of plus plate current-collecting body be nickel or
Person's chromium, surface layer are aluminium, and the bottom of negative current collector is nickel, and surface layer is copper.
Further, collector two sides are provided with super-hydrophobic channel, hydrophobic angle of the water droplet in the super-hydrophobic channel is
140~160 °.
Further, one of substance in the positive/negative active material is covered on positive or negative pole collection in U-typed
On fluid, another substance is covered on cathode or plus plate current-collecting body in T-shape.
Further, the micro-fluidic chip and the flexible battery chip male-female engagement, constitute an entirety.
Preferably, the male-female engagement mode is at least one of tooth form, rivet type, T-type or circle.
Beneficial effect
Compared with prior art, the present invention combines 3D printing and micro-nano processing technology, and it is close that quick Fabrication goes out energy
Three-dimensional batteries system that is high, small in size, can bending repeatedly is spent, it is then that three-dimensional batteries system and micro-fluidic chip composition one is whole
Body forms microfluidic system, and the integrated level of the microfluidic system is high, does not need additional circuit, can bend repeatedly, use is very square
Just.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of microfluidic system of the present invention；
Fig. 2 is the electrical block diagram of microfluidic system of the present invention；
Fig. 3 is the structural schematic diagram of the mold of present invention production flexible battery chip basal body；
Fig. 4 is the structural schematic diagram of present invention flexible battery chip basal body after molding；
Fig. 5 is the schematic diagram that three spray heads print positive/negative slurry and its backing material simultaneously；
Fig. 6 is to print the schematic diagram of cell size in tooth form area；
Fig. 7 is the fit structure schematic diagram of micro-fluidic chip of the present invention and flexible battery chip.
Specific embodiment
The present invention is legibly understood in order to be more clear those skilled in the art, now in conjunction with specific embodiment and attached
Figure, the present invention is described in detail.
The preparation process of microfluidic system mainly includes four steps in the present invention: step 1 prepares micro-fluidic chip base
Body 206, flexible battery chip basal body 102 and upper cover (without display in figure)；Step 2 is made on micro-fluidic chip matrix 206
Make microflow path system (201,202,203,204,205), obtains micro-fluidic chip；Step 3, in flexible battery chip basal body 102
Upper production 3-d microbatteries system, obtains flexible battery chip；Step 4, using upper cover by micro-fluidic chip and flexible battery core
Piece is packaged into an entirety, obtains microfluidic system.The structure of micro-fluidic chip and flexible battery chip is as illustrated in fig. 1 and 2.
Embodiment 1
Production micro-fluidic chip: it carries out 184 colloid of DOW CORNING and curing agent that PDMS is made by mixing according to 10:1, then put
In the mold for entering to prepare micro-fluidic chip matrix 206, die cast obtains micro-fluidic chip matrix 206.Then pass through MEMS
Technology makes microflow path system (201,202,203,204,205) on micro-fluidic chip matrix 206, obtains micro-fluidic chip.
Production flexible battery chip basal body 102: the colloid of SE1700 is mixed with curing agent according to 10:1, is containing tooth
Die cast in the mold 301 (as shown in Figure 3) in shape area, obtains flexible battery chip basal body 102 (as shown in Figure 4).It obtains
Flexible battery chip basal body 102 has the tooth form area 101 being made of continuous triangle shape 105.The peak height of triangle 105 is preferably 50
~3000 μm, the bottom edge side length of the triangle 105 is preferably 100~5000 μm.Plane where 105 bottom edge of triangle is preferred
For the split of flexible battery chip basal body 102.Using such design, flexible battery chip can be made by bending force
When, the surface of triangle 105 is not influenced by bending stress, while keeping the overall structure of flexible battery chip stronger.
Production interdigital collector (106,107): photoetching is coated in the tooth form area 101 of flexible battery chip basal body 102
Glue irradiates 10~20s then in Lithographic template pressure on ultraviolet photolithographic machine, waits photoetching adhesive curing.It then will be after solidification
Flexible battery chip basal body 102 is put into magnetron sputter, regulation power size, at the blocking of permanent mask lower in tooth form area
101 splash-proofing sputtering metal nickel, with a thickness of 10~50 μm.Lead to respectively by the flexible battery chip basal body 102 after sputtering nickel or chromium again
Custom mask is crossed, the splash-proofing sputtering metal aluminium on plus plate current-collecting body 106, splash-proofing sputtering metal copper on negative current collector 107, thickness is 10~
50μm.Finally the flexible battery chip basal body 102 for having sputtered aluminium and copper is put into acetone soln, washes away photoresist, then use wine
Seminal plasma is washed, with being dried with nitrogen, to grow the collector of finger-inserting type in the tooth form area 101 of flexible battery chip basal body 102
(106,107).
Make super-hydrophobic channel: it is laser sintered to the progress of molding collector two sides by specific laser pattern, it is sintered
Afterwards, it is respectively formed to form 200 μm wide of super-hydrophobic channel in interdigitation collector two sides, hydrophobic angular region is water droplet on it
140 °~160 °.
It prepares positive/negative slurry (108,109): (1) pressing the materials such as active material such as LFP, LTO with ethanol solution respectively
Mixing is carried out according to 0.1g/ml and is transferred to ball milling 12h in ball mill, and revolving speed is set in 400rpm, obtains the thinner active material of granularity
Material；(2) by the mixture of (1) treated active material LFP, LTO etc. and ethyl alcohol, conductive agent Super-P, binder PVDF,
Dispersing agent pvp is respectively put into culture dish, is sealed culture dish top with dust-free paper, is put into 150 DEG C of vacuum drying ovens, toasts 12h, takes
It is put into drying basin and is stored after out；(3) in the glove box full of argon gas, 8g binder PVDF is taken to be dissolved in 20ml Isosorbide-5-Nitrae-
In dioxane solution, it is to be mixed completely after obtain solution A；(4) 1g Super-P, 14g LFP, 0.18g pvp is taken to carry out
Mixing, under the shining of 50 DEG C of drying lamp, carries out grinding 30min in Yan Portland, it is molten that the powder after grinding is put into 20ml NMP
It in liquid, is stirred evenly with glass bar, obtains B slurry；(4) 1g Super-P, 14g LTO, 0.18g pvp is taken to be mixed,
Under the shining of 50 DEG C of drying lamp, 20~30min of grinding is carried out in Yan Portland, the powder after grinding is put into 20ml nmp solution
In, it is stirred evenly with glass bar, obtains C slurry；(5) it takes 10ml solution A to be mixed in planet batch mixer with B slurry, turns
Speed is set in 4000rpm, time 10min, and anode sizing agent 108 is made；(6) 10ml solution A and C slurry are taken, in planet mixing
It is mixed in machine, revolving speed is set in 4000rpm, time 10min, and negative electrode slurry 109 is made.Solution A and B/C is respectively configured
It allows it to mix after slurry again, the dissolubility of positive/negative active material can be significantly improved, it is made to be more conducive to print.In addition, this hair
It is bright to be more suitable for electronic printable different from common water system positive/negative slurry (108,109) using oleaginous system.
It prepares backing material 406: taking 5~10g Planck F127 to be dissolved in 20g deionized water, be put into temperature control magnetic agitation
Magnetic agitation 12h in machine, the temperature of stirring are set as 4 DEG C, and backing material 406 is made.
It prints positive/negative active material (103,104): positive/negative slurry (108,109) is packed into three nozzle printing machines
In 401 intermediate cavity 403, backing material 406 is packed into the edge chamber (402,404) of three nozzle printing machines 401, is beaten simultaneously
Print, squeeze pressure 405 are 600psi, and sweep speed is 500 μm/s, and temperature is controlled at 40 DEG C, thus by positive/negative slurry
(108,109) print on positive/negative collector (106,107), as shown in Figure 5.Since high-rise pressure is smaller, Ke Yixuan
Select the positive/negative slurry (108,109) for only printing battery.Such as 16 layers of positive/negative slurry (108,109) are printed altogether, it can be with
Positive/negative slurry (108,109) and backing material 406 are printed simultaneously at 1-10 layers, only prints positive/negative at 11-16 layers
Slurry (108,109).It is of course also possible to which 1-16 layers all only print positive/negative slurry (108,109).It is described in order to save material
Positive/negative material is only with the finger portion for being printed upon interdigital collector (106,107).In order to increase in flexible battery chip just/
The quality of negative electrode active material (103,104), one of substance in the positive/negative slurry (108,109) are covered in U-typed
Cover on positive or negative pole collector (106,107), another substance in T-shape be covered on cathode or plus plate current-collecting body (106,
107) on.Such as anode sizing agent 108 all prints on plus plate current-collecting body 106 in T-shape, corresponding negative electrode slurry 109 is in U-typed
It prints on negative current collector 107, as shown in Figure 6.It can also be alternately arranged and print in U-typed and T-shape with anode sizing agent 108
On plus plate current-collecting body 106, negative electrode slurry 109 is alternately arranged and prints on negative current collector 107 in T-shape and U-typed.Triangle
At least one U-typed of 105 central plane and T-shape pairing.Since positive/negative active material (103,104) is located at triangle 105
Central plane, therefore when flexible battery chip bends, the top stress of the triangle 105 in tooth form area 101 deforms larger, waist
Face is barely affected, therefore positive/negative active material (103,104) will not be shelled with the bending of flexible battery chip
It falls, electrode structure is stablized, and the chemical property of battery is unaffected.In addition, positive/negative active material (103,104) is located at three
Angular 105 central plane, with respect to the horizontal plane on interdigital positive/negative active material (103,104), the present invention has bigger
Surface, more positive/negative active materials (103,104) can be accommodated, so that the total capacitance of flexible battery chip is more
It is high.It is stronger in order to combine positive/negative active material (103,104) of the invention with flexible battery chip basal body 102, one
It is body formed when preparing flexible battery chip basal body 102, it can be constructed in two central planes of the triangle 105 in tooth form area 101 interdigital
Type irrigation canals and ditches (as shown in fig. 4 in enlargement), are then splashed to interdigital irrigation canals and ditches for metallic nickel or chromium, metallic aluminium and metallic copper
In, then positive/negative slurry (108,109) is also printed in interdigital irrigation canals and ditches.
The post-processing of flexible battery chip: printed flexible battery chip basal body 102 is put into deionized water, punching
Wash off backing material 406.Then flexible battery chip basal body 102 is put into -80 DEG C of vacuum oven and is dried in vacuo 4h.
The gold thread for being 100 μm with diameter is good with conducting resinl dispensing respectively and in the connection of the both ends of positive/negative collector (106,107), will
Gold thread is led in micro-fluidic chip.PDMS colloid is mixed with curing agent according to 10:1, interdigital is extruded in by syringe
The root of collector (106,107) and exposed metallic region, the needle diameter of syringe are 100~300 μm, are then placed in
10min is toasted to 80 DEG C of baking ovens.
Preparation upper cover: PDMS glue is mixed with curing agent according to 10:1, is then placed in the mold of preparation upper cover,
Die cast obtains upper cover.The mold of the preparation upper cover also has tooth form area, so that the upper cover of preparation has and flexibility
The tooth form area that battery chip matrix 102 matches.
Encapsulation: upper cover and micro-fluidic chip, flexible battery chip are put into plasma washing machine, oxygen flow is
100sccm, power 200w, surface active 1min are obtained by upper cover and micro-fluidic chip, flexible battery chip bonding after activation
The microfluidic system arrived.The microfluidic system made is put into vacuum oven room temperature to stand for 24 hours.In order to make micro-fluidic chip
It is combined with flexible battery chip stronger, is making micro-fluidic chip matrix 206 and when flexible battery chip basal body 102, it can be with
Concave-convex fit structure, such as tooth form, rivet type, T-type or circle are produced with being integrally formed in its engaging portion, as shown in Figure 7.
Chip: being finally transferred in glove box by the post-processing of microfluidic system, with 100 μm of syringes in argon atmosphere
Syringe needle pours into electrolyte, electrolyte select ethylene carbonate (EC), dimethyl carbonate (DMC), methyl ethyl carbonate enester (EMC) according to
1:1:1 is mixed, and blocks injection orifice with 100-250 μm of PMMA microtrabeculae after injection is good, encapsulation finishes.
Embodiment 2
Embodiment 2 is substantially the same manner as Example 1, the difference is that the configuration of positive/negative slurry (108,109) is different,
Itself the specific process is as follows: (1) by active material such as LFP, the materials such as LTO are mixed with ethanol solution according to 0.1g/ml respectively
It is transferred to ball milling 8h in ball mill, revolving speed is set in 500rpm；(2) by the mixture of active material LFP, LTO and ethyl alcohol, multi wall
Carbon nanotube, binder HPC (hydroxypropyl cellulose, molecular weight 1,000,000), dispersing agent pvp is respectively put into culture dish, with nothing
Dirt paper seals culture dish top, is put into 150 DEG C of vacuum drying ovens, toasts 12h, is put into drying basin and is stored after taking-up；(3)
In the glove box full of argon gas, takes 4g binder HPC to be dissolved in 20ml Isosorbide-5-Nitrae-dioxane solution, be put into 0.5g every time, use glass
Glass stick uniform stirring is wound in reagent bottle cover port with sealing tape, is put into 80 DEG C of water-baths and is carried out 5~10min of heating, preparation
Obtained as clear as crystal solution is as solution A；(4) 1g multi-walled carbon nanotube is taken, 14g LFP, 0.18g pvp are mixed,
Under the shining of 50 DEG C of drying lamp, 20~30min of grinding is carried out in Yan Portland, the powder after grinding is put into 20ml nmp solution
In, it is stirred evenly with glass bar, obtains B slurry；(5) 1g multi-walled carbon nanotube is taken, 14g LTO, 0.18g pvp are mixed,
Under the shining of 50 DEG C of drying lamp, 20~30min of grinding is carried out in Yan Portland, the powder after grinding is put into 20ml nmp solution
In, it is stirred evenly with glass bar, obtains C slurry；(6) it takes 10ml solution A to be mixed in planet batch mixer with B slurry, turns
Speed is set in 4000rpm, time 10min, and anode sizing agent 108 is made；(7) 10ml solution A and C slurry are taken, in planet mixing
It is mixed in machine, revolving speed is set in 4000rpm, time 10min, and negative electrode slurry 109 is made.
Had the following structure using microfluidic system made from above-mentioned technique: microfluidic system mainly by micro-fluidic chip and
Flexible battery chip is constituted, wherein flexible battery chip includes matrix 102 and the tooth form area 101 on matrix 102, in tooth
The surface in shape area 101 is provided with interdigital collector (106,107), the root of the interdigital collector (106,107)
Perpendicular with the stupefied line in top of 101 triangle 105 of tooth form area, the finger portion of the interdigital collector (106,107) is located at three
Angular 105 two central planes and parallel with the stupefied line in the top of triangle 105, in the finger of the interdigital collector (106,107)
Positive/negative active material (103,104) are also covered in portion.Two central planes of the triangle have the irrigation canals and ditches to concave, described
Interdigital collector (106,107) and the positive/negative active material (103,104) are located in the irrigation canals and ditches.The triangle
The peak height of shape 105 is 50~1000 μm, and the bottom edge side length of the triangle 105 is 100~5000 μm.The triangle 105
Bottom edge is located on the split of described matrix 102.The collector (106,107) is divided into plus plate current-collecting body 106 and negative pole currect collecting
Body 107, the bottom of plus plate current-collecting body 106 are nickel or chromium, and surface layer is aluminium, and the bottom of negative current collector 107 is nickel or chromium, table
Layer is copper.One of substance in the positive/negative active material (103,104) is covered on positive or negative pole collection in U-typed
On fluid (106,107), another substance is covered on cathode or plus plate current-collecting body (106,107) in T-shape.It is described micro-fluidic
Chip and the flexible battery chip male-female engagement, constitute an entirety.It further includes upper cover, and the upper cover also has tooth form
The tooth form area 101 of area, the tooth form area of the upper cover and the flexible battery chip mutually coincide, to form the storage of electrolyte
Space.
Obviously, above-described embodiment is just for the sake of clearly demonstrating example, rather than the limitation to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.As long as being made on the basis of the embodiment of the present invention
The change scheme of common-sense, among protection scope of the present invention.
Claims (29)
1. a kind of microfluidic system is mainly made of micro-fluidic chip and flexible battery chip, it is characterised in that: the flexible electrical
Chamber chip includes matrix and the tooth form area on matrix, and the surface in tooth form area is provided with interdigital collector, the friendship
The root of interdigitation collector and the stupefied line in top of tooth form area triangle are perpendicular, and the finger portion of the interdigital collector is located at
Two central planes of triangle and parallel with the stupefied line in the top of triangle, are also covered in the finger portion of the interdigital collector
Positive/negative active material.
2. microfluidic system according to claim 1, it is characterised in that: further include upper cover, the upper cover also has tooth form
The tooth form area of area, the tooth form area of the upper cover and the flexible battery chip mutually coincide, so that the storage for forming electrolyte is empty
Between.
3. microfluidic system according to claim 1, it is characterised in that: two central planes of the triangle, which have, to concave
Irrigation canals and ditches, the interdigital collector and the positive/negative active material are located in the irrigation canals and ditches.
4. microfluidic system according to claim 1, it is characterised in that: the peak height of the triangle is 50~3000 μm,
The bottom edge side length of the triangle is 100~5000 μm.
5. microfluidic system according to claim 1, it is characterised in that: the bottom edge of the triangle is located at described matrix
On split.
6. microfluidic system according to claim 1, it is characterised in that: the collector is divided into plus plate current-collecting body and cathode
Collector, the bottom of plus plate current-collecting body are nickel or chromium, and surface layer is aluminium, and the bottom of negative current collector is nickel or chromium, and surface layer is
Copper.
7. microfluidic system according to claim 1, it is characterised in that: collector two sides are provided with super-hydrophobic channel,
Hydrophobic angle of the water droplet in the super-hydrophobic channel is 140~160 °.
8. microfluidic system according to claim 1, it is characterised in that: wherein one in the positive/negative active material
Kind substance is covered on positive or negative pole collector in U-typed, and another substance is covered on cathode or plus plate current-collecting body in T-shape
On.
9. microfluidic system according to claim 1, it is characterised in that: the micro-fluidic chip and the flexible battery core
Piece male-female engagement constitutes an entirety.
10. microfluidic system according to claim 9, it is characterised in that: the male-female engagement mode is tooth form, rivet
At least one of type, T-type or circle.
11. a kind of preparation process of microfluidic system, which comprises the steps of:
PDMS glue is poured into and makes micro-fluidic chip matrix, flexible battery chip basal body and upper cover in mold by step 1, so that
Flexible battery chip basal body and upper cover after molding have tooth form area；
Step 2 makes microfluidic system on micro-fluidic chip matrix, obtains micro-fluidic chip；
Step 3 coats photoresist in the tooth form area of flexible battery chip basal body, and Lithographic template in pressure recycles ultraviolet photolithographic machine
Then photocuring grows positive/negative collector, the positive/negative in tooth form area splash-proofing sputtering metal under the blocking of fixed exposure mask
Collector is distributed in interdigital, and wherein the root of positive/negative collector and the stupefied line in top of tooth form area triangle are perpendicular,
The finger portion of positive/negative collector is located at two central planes of triangle and, cleaning photoresist parallel with the stupefied line in the top of triangle, then
Positive/negative slurry is printed upon respectively on positive/negative collector, flexible battery chip is obtained；
Step 4, using upper cover by micro-fluidic chip together with flexible battery chip package, the upper cover and flexible battery core
The tooth form area of piece mutually coincide, and internal voids constitute the memory space of electrolyte.
12. the preparation process of microfluidic system according to claim 11, it is characterised in that: in step 1, the miniflow
Chip basal body is controlled to be integrally formed using gas permeability PMDS, the flexible battery chip basal body using air impermeability PMDS it is integrated at
Type.
13. the preparation process of microfluidic system according to claim 11, it is characterised in that: flexible battery core after molding
The tooth form area of sheet matrix has the irrigation canals and ditches of interdigital, and the root of the irrigation canals and ditches is mutually hung down with the stupefied line in top of tooth form area triangle
Directly, the finger portion of the irrigation canals and ditches be located at triangle two central planes and, the positive/negative afflux parallel with the stupefied line in the top of triangle
Body is grown in the irrigation canals and ditches of the interdigital.
14. the preparation process of microfluidic system according to claim 11, it is characterised in that: the peak height of the triangle is
50~3000 μm, the bottom edge side length of the triangle is 100~5000 μm.
15. the preparation process of microfluidic system according to claim 11, it is characterised in that: the bottom edge position of the triangle
In on the split of described matrix.
16. the preparation process of microfluidic system according to claim 11, it is characterised in that: micro-fluidic chip after molding
The engaging portion of matrix and flexible battery chip basal body is provided with concave-convex fit structure.
17. the preparation process of microfluidic system according to claim 16, it is characterised in that: the male-female engagement mode is
Tooth form, rivet type, T-type, circle.
18. the preparation process of microfluidic system according to claim 11, it is characterised in that: in step 3, first solid
Determine in tooth form area splash-proofing sputtering metal nickel or chromium under the blocking of mask, then is sputtered on plus plate current-collecting body by custom mask respectively
Metallic aluminium, splash-proofing sputtering metal copper on negative current collector, metallic nickel, crome metal, metallic aluminium and metallic copper with a thickness of 1~100 μm.
19. the preparation process of microfluidic system according to claim 11, it is characterised in that: pass through specific laser figure
Case, carries out molding collector two sides laser sintered, after sintered, 50 are respectively formed in interdigital collector two sides~
500 μm wide of super-hydrophobic channel, hydrophobic angular region is 140 °~160 ° to water droplet on it.
20. the preparation process of microfluidic system according to claim 11, it is characterised in that: the positive/negative slurry
The preparation method comprises the following steps: 1) positive/negative active material, conductive agent are added ball milling 4~for 24 hours in ball mill, rotational speed of ball-mill is 100~
1000rpm；2) mixture after ball milling is transferred in the glove box full of inert gas, dispersing agent is added and grinds altogether, when grinding altogether
Between be 5~60min, after then grinding altogether mixture investment NMP in, obtain B/C slurry；3) in the gloves for being full of inert gas
In case, binder is put into Isosorbide-5-Nitrae-dioxane and is dissolved, solution A is formed；4) solution A and B/C slurry are mixed, is put into
It is blended in planet batch mixer, the revolving speed of planet batch mixer is 1000~8000rpm, and the time is 2~20min, obtains positive/negative slurry
Material.
21. the preparation process of microfluidic system according to claim 20, it is characterised in that: 1g positive/negative active material
Need 0.05~0.1g of adapted conductive agent, 0.008~0.02g of dispersing agent, 0.1~0.5g of binder, NMP1~3mL, 1,4- dioxy
Six 0.5~1mL of ring.
22. the preparation process of microfluidic system according to claim 20, it is characterised in that: in printing positive/negative slurry
While print backing material, i.e., positive/negative slurry is put into the center cavity of printer, backing material is put into center cavity two sides
Edge chamber, print simultaneously, backing material removed after printing.
23. the preparation process of microfluidic system according to claim 20, it is characterised in that: first print jointly it is several layers of just/
Negative electrode slurry and backing material, then several layers of positive/negative slurries are only printed on this basis.
24. the preparation process of microfluidic system according to claim 23, it is characterised in that: the configuration of the backing material
Method are as follows: 5~10 parts by weight parental type triblock copolymers are dissolved in the deionized water of 20 parts by weight, temperature control magnetic force is put into and stirs
Magnetic agitation 6 in machine~for 24 hours is mixed, controlled at 2~6 DEG C to get arriving backing material.
25. the preparation process of microfluidic system according to claim 20, it is characterised in that: in printing positive/negative slurry
During, agitating device is in stirring, and mixing speed is 50~200rpm, and the temperature of slurry is 30~50 DEG C, squeezes
Pressure is 200~1000psi, and sweep speed is 100~1000 μm/s.
26. the preparation process of microfluidic system according to claim 11, it is characterised in that: the positive/negative active matter
One of substance in matter is printed upon on positive or negative pole collector in U-typed, and another substance is printed upon cathode in T-shape
Or on plus plate current-collecting body.
27. the preparation process of microfluidic system according to claim 11, it is characterised in that: the subsequent operation of step 3 is
Chip after printed, which is put into -100~-40 DEG C of vacuum oven, is dried in vacuo 1~12h.
28. the preparation process of microfluidic system according to claim 11, it is characterised in that: the subsequent operation of step 4 is
Electrolyte is poured into the electrolyte memory space of flexible battery chip using injection needle under the protection of inert gas, then
Injection orifice is blocked using PMMA.
29. the preparation process of microfluidic system according to claim 27, it is characterised in that: the electrolyte uses carbonic acid
Vinyl acetate, dimethyl carbonate, methyl ethyl carbonate enester are mixed according to 1~3:1~3:1~3.
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| CN109786777B (en) * | 2019-01-30 | 2020-10-16 | 中国科学院理化技术研究所 | Liquid metal battery device based on micro-fluidic chip and preparation method thereof |
| CN112452251B (en) * | 2020-10-27 | 2021-12-14 | 山东大学 | Crescent-shaped and deformed ceramic microparticle, preparation method, application and preparation device thereof |
| CN112641957B (en) * | 2020-12-31 | 2023-03-14 | 山西铁居环保科技有限公司 | Method for encapsulating gold nanoparticles by self-assembly of segmented copolymer PCL-b-PEO based on micro-fluidic chip |
| CN113956527A (en) * | 2021-12-07 | 2022-01-21 | 深圳大学 | Surface-metallized liquid crystal polymer and preparation method thereof |
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