CN107252707A - A kind of microfluidic system and its preparation technology - Google Patents
A kind of microfluidic system and its preparation technology Download PDFInfo
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- CN107252707A CN107252707A CN201710405953.XA CN201710405953A CN107252707A CN 107252707 A CN107252707 A CN 107252707A CN 201710405953 A CN201710405953 A CN 201710405953A CN 107252707 A CN107252707 A CN 107252707A
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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
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Abstract
The invention discloses a kind of microfluidic system and its preparation technology, the microfluidic system is mainly made up 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, and positive/negative active material is also covered with the finger portion of the interdigital collector.3D printing and micro-nano process technology are mainly combined by the present invention, quick Fabrication goes out the three-dimensional batteries system that energy density height, small volume, integrated level are high, can bend repeatedly, the three-dimensional batteries system constitutes an entirety with micro-fluidic chip, can be powered directly to micro-fluidic chip.
Description
Technical field
The invention belongs to microfluidic art, more particularly to a kind of microfluidic system and its preparation technology.
Background technology
The micro-fluidic skill for referring to manipulate fluid or gas in more than ten microns to hundreds of microns wide channel systems
Art.The core for being applied to the fields such as biology, chemistry, biomedicine processed using microflow control technique as core, 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, detection
Efficiency high, use cost it is low and be easy to other technologies integration of equipments, be real with good compatibility, following developing direction
Existing portable inspectiont.
But for the higher micro mation system of integrated level, how to look for a miniaturization energy supply that can be matched
Device is the problem of currently encountering.Although having had many on minicell, the product of flexible battery on the market, he
Manufacturing process it is many all to be improved, it is necessary to which more innovative technologies are changed to it.The Thinergy in such as U.S.
The minicell for the MEC225 models that company produces, open electric circuit is 4.1V, and planar dimension is 12.7mm × 12.7mm, and thickness is
0.17mm, the rated capacity 0.13mAh of battery.This product has been most reliable, most representational in minicell field
One of product.But its towards field be more electronic product, such as mobile phone, computer, its 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
There is no a both with certain flexibility, and be the three-dimensional micro battery of high power capacity.For micro-fluidic chip system, its development side
To also to wearable, integrated level is high, it is portable in terms of developed.It is this to have and bend repeatedly, can be with mass production
Minicell be precisely current micro-fluidic field required for.Due to three-dimensional batteries relative to two-dimentional battery with higher appearance
Amount, also certain advantage can be had more in performance relative to general hull cell.
The content of the invention
The main object of the present invention is to be combined 3D printing and micro-nano process technology, and quick Fabrication goes out energy density
Height, small volume, 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, it is not necessary to additional circuit, can bend repeatedly.
In order to achieve the above object, present invention employs following preparation technology:
Step one, PDMS (dimethyl silicone polymer) glue is poured into and micro-fluidic chip matrix, flexible battery is made in mould
Chip basal body and upper lid so that flexible battery chip basal body and upper lid after shaping have tooth form area;Step 2, micro-fluidic
Microfluidic system is made in chip basal body, micro-fluidic chip is obtained;Step 3, is coated in the tooth form area of flexible battery chip basal body
Lithographic template in photoresist, pressure, recycles ultraviolet photolithographic machine photocuring, then in the sputtering of tooth form area under the blocking of fixed mask
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 top of triangle is parallel, cleans photoresist, then positive/negative slurry is printed upon on positive/negative collector respectively, obtained
To flexible battery chip;Step 4, using it is upper lid by micro-fluidic chip together with flexible battery chip package, it is described it is upper lid with
The tooth form area of flexible battery chip mutually coincide, and its internal voids constitutes the memory space of electrolyte.
It is used as improved technical scheme of the invention:In step one, 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.
It is used as improved technical scheme of the invention:In step one, the tooth form area tool of the flexible battery chip basal body after shaping
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.
It is used as improved technical scheme of the invention:In step one, the peak height of tooth form area triangle is 50~3000 μm,
The base length of side of triangle is 100~5000 μm.
It is used as improved technical scheme of the invention:In step one, the base of tooth form area triangle is located at described matrix
Split on.
It is used as improved technical scheme of the invention:In step one, micro-fluidic chip matrix and flexible battery core after shaping
The joint portion of sheet matrix is provided with concave-convex fit structure.
Preferably, the male-female engagement mode is tooth form, rivet type, T-shaped, circle.
As improved technical scheme of the invention, in step 3, sputtered first under the blocking of permanent mask in tooth form area
The one or more of metallic nickel or chromium, 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, the thickness of metallic aluminium and metallic copper are 1~100 μm.
Further, super-hydrophobic passage is made:By specific laser pattern, laser burning is carried out to shaping collector both sides
Knot, it is sintered after, in interdigitation collector both sides formation super-hydrophobic passage 50~500 μm wide respectively, water droplet is thereon
Hydrophobic angular region is 140 °~160 °.
As improved technical scheme of the invention, in step 3, the preparation method of the positive/negative slurry is:1) will just/
Negative active core-shell material, conductive agent add 4~24h of ball milling in ball mill, and rotational speed of ball-mill is 100~1000rpm;2) by after ball milling
Mixture is transferred in the glove box full of inert gas, is added dispersant and is ground altogether, and the time is ground altogether for 5~60min, then will altogether
In mixture input NMP after grinding, B/C slurries are obtained;3) in the glove box full of inert gas, by binding agent be put into Isosorbide-5-Nitrae-
Dioxane dissolves, and forms solution A;4) solution A and B/C slurries are mixed, is put into planet batch mixer and is blended, planet
The rotating speed of batch mixer is 1000~8000rpm, and the time is 2~20min, obtains positive/negative slurry.
Wherein, 1g positive/negatives active material needs 0.05~0.1g of adapted conductive agent, 0.008~0.02g of dispersant, bonding
0.1~0.5g of agent, NMP1~3mL, 0.5~1mL of 1,4- dioxane.
As improved technical scheme of the invention, in step 3, fid is printed while positive/negative slurry is printed
Positive/negative slurry, i.e., be put into the center cavity of printer, backing material be put into the edge chamber of center cavity both sides, beaten simultaneously by material
Print, printing removes backing material after finishing.
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 collocation method of the backing material is:5~10 parts by weight parental type triblock copolymers are dissolved in 20
In the deionized water of parts by weight, 6~24h of magnetic agitation in temperature control magnetic stirrer is put into, it is 2~6 DEG C to control temperature, that is, is obtained
Backing material.
Preferably, print positive/negative slurry during, agitating device be in stirring, mixing speed be 50~
200rpm, the temperature of slurry is 30~50 DEG C, and squeeze pressure is 200~1000psi, and sweep speed is 100~1000 μm/s.
As improved technical scheme of the invention, in step 3, the one of which material in the positive/negative active material
It is printed upon in " U " type on negative or positive electrode collector, another material is printed upon on negative pole or plus plate current-collecting body in T-shape.
It is used as improved technical scheme of the invention:The subsequent operation of step 3 is put into -100 for the chip after printed~-
1~12h of vacuum drying in 40 DEG C of vacuum drying chamber.
It is used as improved technical scheme of the 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 using ethylene carbonate, dimethyl carbonate, methyl ethyl carbonate alkene ester according to 1~3:1~3:1~3 is mixed.
There is following structure using microfluidic system made from above-mentioned technique:Microfluidic system it is main by micro-fluidic chip and
Flexible battery chip is constituted, wherein, flexible battery chip includes matrix and the tooth form area on matrix, the surface in tooth form area
Interdigital collector is provided with, 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, intersects described
Positive/negative active material is also covered with the finger portion of finger-type collector.
Further, it also includes upper lid, and the upper lid also has tooth form area, tooth form area and the flexibility of the upper lid
The tooth form area of battery chip mutually coincide, so as 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 base length of side of the triangle is 100~5000
μm。
Further, the base 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 for nickel or
Person's chromium, top layer is aluminium, and the bottom of negative current collector is nickel, and top layer is copper.
Further, super-hydrophobic passage is provided with collector both sides, water droplet is in the hydrophobic angle of the super-hydrophobic passage
140~160 °.
Further, the one of which material in the positive/negative active material is covered in negative or positive electrode collection in " U " type
On fluid, another material is covered on negative pole 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 be tooth form, it is rivet type, T-shaped or at least one of circular.
Beneficial effect
Compared with prior art, 3D printing and micro-nano process technology are combined by the present invention, and it is close that quick Fabrication goes out energy
Degree height, small volume, the three-dimensional batteries system that can be bent repeatedly, 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, it is not necessary to additional circuit, can bend repeatedly, use is very square
Just.
Brief description of the drawings
Fig. 1 is the structural representation of microfluidic system of the present invention;
Fig. 2 is the electrical block diagram of microfluidic system of the present invention;
Fig. 3 makes the structural representation of the mould of flexible battery chip basal body for the present invention;
Fig. 4 is the structural representation of the flexible battery chip basal body after present invention shaping;
Fig. 5 is the schematic diagram that three shower nozzles 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.
Embodiment
In order that those skilled in the art becomes apparent from legibly understanding the present invention, in conjunction with embodiment and attached
Figure, the present invention is described in detail.
The preparation technology of microfluidic system mainly includes four steps in the present invention:Step one, micro-fluidic chip base is prepared
Body 206, flexible battery chip basal body 102 and upper lid (without display in figure);Step 2, makes on micro-fluidic chip matrix 206
Make microflow path system (201,202,203,204,205), obtain micro-fluidic chip;Step 3, in flexible battery chip basal body 102
Upper making 3-d microbatteries system, obtains flexible battery chip;Step 4, is covered micro-fluidic chip and flexible battery core using upper
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
Make micro-fluidic chip:By the colloid of DOW CORNING 184 and curing agent according to 10:1 carries out that PDMS, Ran Houfang is made by mixing
Among the mould for entering to prepare micro-fluidic chip matrix 206, die cast obtains micro-fluidic chip matrix 206.Then MEMS is passed through
Technology makes microflow path system (201,202,203,204,205) on micro-fluidic chip matrix 206, obtains micro-fluidic chip.
Make flexible battery chip basal body 102:By SE1700 colloid and curing agent according to 10:1 is mixed, containing tooth
Die cast in the mould (as shown in Figure 3) in shape area, obtains flexible battery chip basal body 102 (as shown in Figure 4).Obtained flexibility
Battery chip matrix 102 has the tooth form area 101 being made up of continuous triangle shape 105.The peak height of triangle 105 is preferably 50~
3000 μm, the base length of side of the triangle 105 is preferably 100~5000 μm.Plane where the base of triangle 105 is preferably
The split of flexible battery chip basal body 102.Using such design, flexible battery chip can be made when by bending force,
The surface of triangle 105 is not influenceed by bending stress, while making the overall structure of flexible battery chip more firm.
Make interdigital collector (106,107):Photoetching is coated in the tooth form area 101 of flexible battery chip basal body 102
Glue, then with Lithographic template pressure, irradiates 10~20s on ultraviolet photolithographic machine, waits photoetching adhesive curing.Then by after solidification
Flexible battery chip basal body 102 is put into magnetron sputter, adjusts watt level, in lower of the blocking of permanent mask in tooth form area
101 splash-proofing sputtering metal nickel, thickness is 10~50 μm.The flexible battery chip basal body 102 after by sputtering nickel or chromium is led to respectively 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, photoresist is washed away, then use wine
Seminal plasma is washed, and is dried up with nitrogen, so as 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 passage:It is laser sintered to the progress of shaping collector both sides by specific laser pattern, it is sintered
Afterwards, super-hydrophobic passage 200 μm wide is formed respectively in interdigitation collector both sides, hydrophobic angular region is water droplet thereon
140 °~160 °.
Prepare positive/negative slurry (108,109):(1) materials such as active material such as LFP, LTO are pressed with ethanol solution respectively
Mixing is carried out according to 0.1g/ml and is transferred to ball milling 12h in ball mill, and speed setting obtains the thinner active material of granularity in 400rpm
Material;(2) active material LFP, LTO etc. after (1) is handled and the mixture of ethanol, conductive agent Super-P, binding agent PVDF,
Dispersant 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 deposited after go out;(3) in the glove box full of argon gas, take 8g binding agents PVDF be dissolved in 20ml Isosorbide-5-Nitraes-
Among dioxane solution, it is to be mixed completely after obtain solution A;(4) 1gSuper-P, 14gLFP, 0.18gpvp is taken to be mixed
Close, under the shining of 50 DEG C of drying lamp, be ground 30min in Yan Portland, the powder after grinding is put into 20mlNMP solution
In, stirred with glass bar, obtain B slurries;(4) 1gSuper-P, 14gLTO, 0.18gpvp is taken to be mixed, at 50 DEG C
Under the shining of drying lamp, 20~30min is ground in Yan Portland, the powder after grinding is put into 20mlNMP solution, uses glass
Rod stirs, and obtains C slurries;(5) 10mlA solution is taken to be mixed with B slurries in planet batch mixer, speed setting exists
4000rpm, the time is 10min, and anode sizing agent 108 is made;(6) 10mlA solution and C slurries are taken, is carried out in planet batch mixer
Mix, speed setting is in 4000rpm, and the time is 10min, cathode size 109 is made.It is respectively configured after solution A and B/C slurries again
Allow it to mix, the dissolubility of positive/negative active material can be significantly improved, it is more conducive to printing.In addition, what the present invention was used
It is oleaginous system, different from common water system positive/negative slurry (108,109), it is more suitable for electronic printable.
Prepare backing material 406:Take 5~10g Plancks F127 to be dissolved in 20g deionized waters, be put into temperature control magnetic agitation
Magnetic agitation 12h in machine, the temperature of stirring is set as 4 DEG C, and backing material 406 is made.
Print positive/negative active material (103,104):Positive/negative slurry (108,109) is loaded into three nozzle printing machines
In intermediate cavity 403, in the edge chamber (402,404) that backing material 406 is loaded to three nozzle printing machines, print simultaneously, extruding pressure
Power 405 is 600psi, and sweep speed is 500 μm/s, and temperature control is at 40 DEG C, so that positive/negative slurry (108,109) be printed
Onto positive/negative collector (106,107), as shown in Figure 5.Because high-rise pressure is smaller, only printing battery can be selected
Positive/negative slurry (108,109).16 layers of positive/negative slurry (108,109) are for example printed altogether, can be same at 1-10 layers
When printing positive/negative slurry (108,109) and backing material 406, only printed at 11-16 layers positive/negative slurry (108,
109).It is of course also possible to which 1-16 layers all only print positive/negative slurry (108,109).In order to save material, the positive/negative material
Material is only with the finger portion for being printed upon interdigital collector (106,107).In order to increase positive/negative active matter in flexible battery chip
One of which material in the quality of matter (103,104), the positive/negative slurry (108,109) in " U " type be covered in positive pole or
On negative current collector (106,107), another material is covered on negative pole or plus plate current-collecting body (106,107) in T-shape.For example
Anode sizing agent 108 is all printed on plus plate current-collecting body 106 in T-shape, and corresponding cathode size 109 prints to negative pole in " U " type
On collector 107, as shown in Figure 6.Can also anode sizing agent 108 be alternately arranged in " U " type and T-shape and print to plus plate current-collecting body
On 106, cathode size 109 is alternately arranged in T-shape and " U " type and printed on negative current collector 107.The central plane of triangle 105
At least one " U " type and T-shape pairing.Because positive/negative active material (103,104) is located at the central plane of triangle 105, therefore
When flexible battery chip bends, the top stress of the triangle 105 in tooth form area 101, deform it is larger, central plane hardly by
Influence, therefore positive/negative active material (103,104) will not be peeled off, electrode structure with the bending of flexible battery chip
Stable, the chemical property of battery is unaffected.In addition, positive/negative active material (103,104) is located at the waist of triangle 105
Face, with respect to the horizontal plane on interdigital positive/negative active material (103,104), the present invention have bigger surface, can
More positive/negative active materials (103,104) are accommodated, so that the total capacitance of flexible battery chip is higher.In order that this
The positive/negative active material (103,104) of invention is combined more firm with flexible battery chip basal body 102, is being integrally formed preparation
During flexible battery chip basal body 102, you can construct interdigital irrigation canals and ditches (as schemed in two central planes of the triangle 105 in tooth form area 101
Shown in enlarged drawing in 4), then metallic nickel or chromium, metallic aluminium and metallic copper are splashed in interdigital irrigation canals and ditches, then will
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, rushed
Wash backing material 406 off.Then flexible battery chip basal body 102 is put into -80 DEG C of vacuum drying chamber and is dried in vacuo 4h.
Connected respectively with the two ends of positive/negative collector (106,107) with a diameter of 100 μm of gold threads, it is good with conducting resinl dispensing, will
Gold thread is led in micro-fluidic chip.By PDMS colloids and curing agent according to 10:1 mixing is squeezed in interdigital by syringe
The root of collector (106,107) and exposed metallic region, the needle diameter of syringe is 100~300 μm, is then placed in
To 80 DEG C of baking oven baking 10min.
Covered in preparation:By PDMS glue and curing agent according to 10:1 is mixed, and is then placed among the mould covered on preparing,
Die cast, obtains lid.The mould covered in the preparation also has tooth form area, so that the upper lid prepared has and flexibility
The tooth form area that battery chip matrix 102 matches.
Encapsulation:Upper lid and micro-fluidic chip, flexible battery chip are put into plasma washing machine, oxygen flow is
100sccm, power is 200w, surface active 1min, by upper lid and micro-fluidic chip, flexible battery chip bonding after activation, is obtained
The microfluidic system arrived.The microfluidic system made is put into vacuum drying chamber normal temperature and stands 24h.In order that micro-fluidic chip
Combined with flexible battery chip more firm, making micro-fluidic chip matrix 206 and during flexible battery chip basal body 102, can be with
Produce concave-convex fit structure in its joint portion with being integrally formed, such as tooth form, rivet type, T-shaped or circle, as shown in Figure 7.
The post processing of microfluidic system:Finally chip is transferred in glove box, with 100 μm of syringes in argon atmosphere
Syringe needle pours into electrolyte, electrolyte from ethylene carbonate (EC), dimethyl carbonate (DMC), methyl ethyl carbonate alkene ester (EMC) according to
1:1:1 is mixed, and blocks injection orifice with 100-250 μm of PMMA microtrabeculaes after injection is good, encapsulation is finished.
Embodiment 2
Embodiment 2 is substantially the same manner as Example 1, and difference is that the configuration of positive/negative slurry (108,109) is different,
Its concrete technology is as follows:(1) by active material such as LFP, the material such as LTO is mixed with ethanol solution according to 0.1g/ml respectively
Ball milling 8h in ball mill is transferred to, speed setting is in 500rpm;(2) by active material LFP, LTO and the mixture of ethanol, many walls
CNT, binding agent HPC (hydroxypropyl cellulose, molecular weight 1,000,000), dispersant 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 deposited after taking-up;(3)
In the glove box full of argon gas, take 4g binding agents HPC to be dissolved in 20ml Isosorbide-5-Nitraes-dioxane solution, 0.5g is put into every time, glass is used
Glass rod 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, prepares
Obtained as clear as crystal solution is as solution A;(4) 1g multi-walled carbon nanotubes are taken, 14gLFP, 0.18gpvp is mixed, 50
DEG C drying lamp shining under, be ground 20~30min in Yan Portland, the powder after grinding is put into 20mlNMP solution, use
Glass bar stirs, and obtains B slurries;(5) 1g multi-walled carbon nanotubes are taken, 14gLTO, 0.18gpvp is mixed, at 50 DEG C
Under the shining of drying lamp, 20~30min is ground in Yan Portland, the powder after grinding is put into 20mlNMP solution, uses glass
Rod stirs, and obtains C slurries;(6) 10mlA solution is taken to be mixed with B slurries in planet batch mixer, speed setting exists
4000rpm, the time is 10min, and anode sizing agent 108 is made;(7) 10mlA solution and C slurries are taken, is carried out in planet batch mixer
Mix, speed setting is in 4000rpm, and the time is 10min, cathode size 109 is made.
There is following structure using microfluidic system made from above-mentioned technique:Microfluidic system it is main 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)
The stupefied line in top with the triangle 105 of tooth form area 101 is perpendicular, and 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) is also covered with portion.Two central planes of the triangle have the irrigation canals and ditches concaved, 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 base length of side of the triangle 105 is 100~5000 μm.The triangle 105
Base 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 is nickel or chromium, and top layer is aluminium, and the bottom of negative current collector 107 is nickel or chromium, table
Layer is copper.One of which material in the positive/negative active material (103,104) is covered in negative or positive electrode collection in " U " type
On fluid (106,107), another material is covered on negative pole 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 also includes upper lid, and the upper lid also has tooth form
Area, the tooth form area of the upper lid and the tooth form area 101 of the flexible battery chip mutually coincide, so as to form the storage of electrolyte
Space.
Obviously, above-described embodiment is used for the purpose 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 change or
Change.There is no necessity and possibility to exhaust all the enbodiments.As long as 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 (7)
1. a kind of microfluidic system, is mainly made up 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 interdigital collector, the friendship are provided with the surface in tooth form area
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 with the finger portion of the interdigital collector
Positive/negative active material.
2. microfluidic system according to claim 1, it is characterised in that:Also include upper lid, the upper lid also has tooth form
Area, the tooth form area of the upper lid and the tooth form area of the flexible battery chip mutually coincide, so that the storage for forming electrolyte is empty
Between, it is preferable that two central planes of the triangle have the irrigation canals and ditches concaved, the interdigital collector and the positive/negative
Active material is located in the irrigation canals and ditches, it is preferable that the peak height of the triangle is 50~3000 μm, the base side of the triangle
A length of 100~5000 μm, it is preferable that the base of the triangle is located on the split of described matrix, it is preferable that the afflux
Body is divided into plus plate current-collecting body and negative current collector, and the bottom of plus plate current-collecting body is nickel or chromium, and top layer is aluminium, negative current collector
Bottom is nickel or chromium, and top layer is copper, further, super-hydrophobic passage is provided with collector both sides, water droplet is described super thin
The hydrophobic angle of aquaporin is 140~160 °, it is preferable that the one of which material in the positive/negative active material covers in " U " type
Cover on negative or positive electrode collector, another material is covered on negative pole or plus plate current-collecting body in T-shape, it is preferable that described
Micro-fluidic chip and the flexible battery chip male-female engagement, constitute an entirety, further, the male-female engagement mode is
It is tooth form, rivet type, T-shaped or at least one of circular.
3. a kind of preparation technology of microfluidic system, it is characterised in that comprise the following steps:
Step one, PDMS glue is poured into and micro-fluidic chip matrix, flexible battery chip basal body and upper lid is made in mould so that
Flexible battery chip basal body and upper lid after shaping have tooth form area;
Step 2, makes microfluidic system on micro-fluidic chip matrix, obtains micro-fluidic chip;
Step 3, Lithographic template in photoresist, pressure is coated in the tooth form area of flexible battery chip basal body, recycles ultraviolet photolithographic machine
Photocuring, then grows positive/negative collector, the positive/negative under the blocking of fixed mask in tooth form area splash-proofing sputtering metal
Collector is distributed in interdigital, and the wherein root of positive/negative collector and the stupefied line in top of tooth form area triangle is perpendicular,
The finger portion of positive/negative collector is located at two central planes of triangle and parallel with the stupefied line in the top of triangle, cleans photoresist, then
Positive/negative slurry is printed upon on positive/negative collector respectively, flexible battery chip is obtained;
Step 4, is covered by micro-fluidic chip together with flexible battery chip package using upper, the upper lid and flexible battery core
The tooth form area of piece mutually coincide, and its internal voids constitutes the memory space of electrolyte.
4. the preparation technology of micro-fluidic chip according to claim 3, it is characterised in that:It is described micro-fluidic in step one
Chip basal body is integrally formed using gas permeability PMDS, and the flexible battery chip basal body is integrally formed using air impermeability PMDS,
Preferably, the tooth form area of the flexible battery chip basal body after shaping has the irrigation canals and ditches of interdigital, the root of the irrigation canals and ditches and tooth
The stupefied line in top of shape area triangle is perpendicular, and the finger portions of the irrigation canals and ditches is located at two central planes of triangle and stupefied with the top of triangle
Line is parallel, and the positive/negative collector is grown in the irrigation canals and ditches of the interdigital, it is preferable that the peak height of the triangle
For 50~3000 μm, the base length of side of the triangle is 100~5000 μm, it is preferable that the base of the triangle is located at institute
State on the split of matrix, it is preferable that the joint portion of micro-fluidic chip matrix and flexible battery chip basal body after shaping is set
There is concave-convex fit structure, further, the male-female engagement mode is tooth form, rivet type, T-shaped, circle.
5. the preparation technology of micro-fluidic chip according to claim 3, it is characterised in that:In step 3, first in fixation
In tooth form area splash-proofing sputtering metal nickel or chromium under the blocking of mask, then respectively by custom mask, gold is sputtered on plus plate current-collecting body
Belong to aluminium, splash-proofing sputtering metal copper on negative current collector, metallic nickel, crome metal, the thickness of metallic aluminium and metallic copper are 1~100 μm, enter one
Step ground, by specific laser pattern, the collector both sides of shaping are carried out it is laser sintered, it is sintered after, in interdigital collection
Fluid both sides form super-hydrophobic passage 50~500 μm wide respectively, and water droplet is 140 °~160 ° in hydrophobic angular region thereon, preferably
Ground, the preparation method of the positive/negative slurry is:1)By positive/negative active material, conductive agent add ball mill in ball milling 4~
24h, rotational speed of ball-mill is 100~1000rpm;2)Mixture after ball milling is transferred in the glove box full of inert gas, plus
Enter dispersant to grind altogether, the time is ground altogether for 5~60min, in the mixture input NMP after then grinding altogether, obtain B/C slurries;3)
In the glove box full of inert gas, binding agent is put into Isosorbide-5-Nitrae-dioxane and dissolved, solution A is formed;4)By solution A and B/
C slurries are mixed, and are put into planet batch mixer and are blended, and the rotating speed of planet batch mixer is 1000~8000rpm, and the time is 2
~20min, obtains positive/negative slurry, it is preferable that 1g positive/negative active materials need 0.05~0.1g of adapted conductive agent, dispersant
0.008~0.02g, 0.1~0.5g of binding agent, NMP1~3mL, Isosorbide-5-Nitrae -0.5~1mL of dioxane, it is preferable that printing just/
Backing material is printed while cathode size, i.e., positive/negative slurry is put into the center cavity of printer, during backing material is put into
The edge chamber of chambers of the heart both sides, is printed simultaneously, and printing removes backing material after finishing, it is preferable that first print several layers of positive/negatives jointly
Slurry and backing material, then several layers of positive/negative slurries are only printed on this basis, it is preferable that the configuration side of the backing material
Method is:5~10 parts by weight parental type triblock copolymers are dissolved in the deionized water of 20 parts by weight, temperature control magnetic agitation is put into
6~24h of magnetic agitation in machine, it is 2~6 DEG C to control temperature, that is, obtains backing material, it is preferable 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, extruding pressure
Power is 200~1000psi, and sweep speed is 100~1000 μm/s, it is preferable that wherein one in the positive/negative active material
Plant material to be printed upon on negative or positive electrode collector in " U " type, another material is printed upon negative pole or plus plate current-collecting body in T-shape
On.
6. the preparation technology of micro-fluidic chip according to claim 3, it is characterised in that:The subsequent operation of step 3 is to beat
Chip after printed is put into 1~12h of vacuum drying in -100~-40 DEG C of vacuum drying chamber.
7. the preparation technology of micro-fluidic chip according to claim 3, it is characterised in that:The subsequent operation of step 4 be
Electrolyte is poured into the electrolyte memory space of flexible battery chip using injection needle under the protection of inert gas, Ran Houli
Injection orifice is blocked with PMMA, it is preferable that the electrolyte is using ethylene carbonate, dimethyl carbonate, methyl ethyl carbonate alkene ester according to 1
~3:1~3:1~3 is mixed.
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CN112452251A (en) * | 2020-10-27 | 2021-03-09 | 山东大学 | Crescent-shaped and deformed ceramic microparticle, preparation method, application and preparation device thereof |
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