CN109759154A - Microfluidic chip based on polypyrrole electrochemical transistor and preparation method thereof - Google Patents
Microfluidic chip based on polypyrrole electrochemical transistor and preparation method thereof Download PDFInfo
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- CN109759154A CN109759154A CN201910181299.8A CN201910181299A CN109759154A CN 109759154 A CN109759154 A CN 109759154A CN 201910181299 A CN201910181299 A CN 201910181299A CN 109759154 A CN109759154 A CN 109759154A
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- source electrode
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- 229920000128 polypyrrole Polymers 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 53
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 53
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims abstract description 53
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 53
- 239000000758 substrate Substances 0.000 claims abstract description 35
- 239000004020 conductor Substances 0.000 claims abstract description 23
- 230000008021 deposition Effects 0.000 claims abstract description 7
- 238000001311 chemical methods and process Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 51
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 36
- 239000000243 solution Substances 0.000 claims description 35
- 239000004065 semiconductor Substances 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 19
- 239000003792 electrolyte Substances 0.000 claims description 18
- 239000000178 monomer Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 238000001259 photo etching Methods 0.000 claims description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 239000012528 membrane Substances 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 239000004094 surface-active agent Substances 0.000 claims description 10
- 238000000151 deposition Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000011161 development Methods 0.000 claims description 8
- 239000010931 gold Substances 0.000 claims description 8
- 238000004528 spin coating Methods 0.000 claims description 8
- 239000012530 fluid Substances 0.000 claims description 7
- 229920002120 photoresistant polymer Polymers 0.000 claims description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 238000002174 soft lithography Methods 0.000 claims description 5
- 238000005292 vacuum distillation Methods 0.000 claims description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 4
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 239000011651 chromium Substances 0.000 claims description 4
- 230000005518 electrochemistry Effects 0.000 claims description 4
- 238000004070 electrodeposition Methods 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000008236 heating water Substances 0.000 claims description 4
- 229910044991 metal oxide Inorganic materials 0.000 claims description 4
- 150000004706 metal oxides Chemical class 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910000510 noble metal Inorganic materials 0.000 claims description 4
- 238000012536 packaging technology Methods 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims description 4
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 238000005538 encapsulation Methods 0.000 claims description 3
- NEXSMEBSBIABKL-UHFFFAOYSA-N hexamethyldisilane Chemical compound C[Si](C)(C)[Si](C)(C)C NEXSMEBSBIABKL-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 238000002444 silanisation Methods 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 238000007711 solidification Methods 0.000 claims description 3
- 230000008023 solidification Effects 0.000 claims description 3
- BMVIGGFETHGRGF-UHFFFAOYSA-N 1-butyl-3-methyl-1,2-dihydroimidazol-1-ium;benzoate Chemical compound [O-]C(=O)C1=CC=CC=C1.CCCC[NH+]1CN(C)C=C1 BMVIGGFETHGRGF-UHFFFAOYSA-N 0.000 claims description 2
- PBIDWHVVZCGMAR-UHFFFAOYSA-N 1-methyl-3-prop-2-enyl-2h-imidazole Chemical compound CN1CN(CC=C)C=C1 PBIDWHVVZCGMAR-UHFFFAOYSA-N 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 2
- 239000004793 Polystyrene Substances 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- SIXOAUAWLZKQKX-UHFFFAOYSA-N carbonic acid;prop-1-ene Chemical compound CC=C.OC(O)=O SIXOAUAWLZKQKX-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000003431 cross linking reagent Substances 0.000 claims description 2
- 238000002848 electrochemical method Methods 0.000 claims description 2
- YAGKRVSRTSUGEY-UHFFFAOYSA-N ferricyanide Chemical compound [Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] YAGKRVSRTSUGEY-UHFFFAOYSA-N 0.000 claims description 2
- 230000013011 mating Effects 0.000 claims description 2
- 239000007769 metal material Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 238000003672 processing method Methods 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
- -1 tetrabutyl phosphine tetrafluoroborate Chemical compound 0.000 claims description 2
- BJQWBACJIAKDTJ-UHFFFAOYSA-N tetrabutylphosphanium Chemical compound CCCC[P+](CCCC)(CCCC)CCCC BJQWBACJIAKDTJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000003466 welding Methods 0.000 claims description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 6
- 239000010408 film Substances 0.000 description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000000520 microinjection Methods 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 230000007812 deficiency Effects 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000007641 inkjet printing Methods 0.000 description 2
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- 238000012123 point-of-care testing Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
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- 239000002070 nanowire Substances 0.000 description 1
- 239000002547 new drug Substances 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 150000003233 pyrroles Chemical class 0.000 description 1
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- 238000011895 specific detection Methods 0.000 description 1
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- Thin Film Transistor (AREA)
Abstract
The invention belongs to the technical fields of micro-fluidic chip, and in particular to a kind of micro-fluidic chip and its in-situ preparation method of integrated polypyrrole electrochemical transistor；Technical problem to be solved are as follows: a kind of micro-fluidic chip and preparation method thereof based on polypyrrole electrochemical transistor is provided；Solve the technical solution of technical problem use are as follows: including substrate, the layer deposition of the substrate has conductor layer, and the conductor layer is provided with electrical cable and substrate pad；The upper layer of the conductor layer is also deposited with insulating layer, is provided with electrode window through ray on the insulating layer；Microelectrode is also deposited on the insulating layer, one end of the microelectrode is exposed on the insulating layer, and the other end of microelectrode passes through electrode window through ray and connect with conductor layer；The microelectrode includes source electrode, grid, drain electrode；The substrate, conductor layer, insulating layer, electrode window through ray, microelectrode collectively form substrate, and the substrate is bonded together with PDMS cover plate by mechanical or physico-chemical process；It is prepared by the micro-fluidic chip that the present invention is applied to electrochemical transistor.
Description
Technical field
The invention belongs to the technical fields of micro-fluidic chip, and in particular to a kind of integrated polypyrrole electrochemical transistor it is micro-
Fluidic chip and its in-situ preparation method.
Technical background
Organic electrochemistry transistor micro-fluidic chip is a kind of care diagnostic POCT core equipment having a high potential.Researcher
The specific detection of a variety of large biological molecules such as DNA has been realized by electrochemical transistor micro-fluidic chip.Also, DNA
It detects up to 10pM.Researcher constructs the electrochemical transistor sensor-based system for being integrated in organ chip interior, thin to realize
The multi-parameter of born of the same parents' pattern, differentiation and integrality is monitored on-line.This chip makes up animal model deficiency, provides new drug development body
The new platform of external model.
Most common method is that ink-jet is beaten in the formation preparation of organic semiconductive channel layer in electrochemical transistor at present
Print method and spin-coating method.Ink-jet printing is widely used in current organic electronic device processing, and the diameter of ink droplet can be controlled
For system in 20um or so, but because the size of its single ink droplet limits, precision is limited, and coffee ring effect often results in its film forming not
?.After introducing aerosol inkjet printing, precision is improved, but it is more demanding to the physico-chemical attributes of solution, and equipment is high
It is expensive.
Spin-coating method simple process and low cost.But the area of spin-coating film is bigger.When for micro-fluidic chip, need
Further spin-coating film is patterned, it could be with fluid channel bonding packaging.But organic semiconductor channel layer is for solution ring
The variation in border is more sensitive.In MEMS patterning process, repeatedly and chemical reagent, it will make reduced performance, even send out
Raw structural failure.In addition, MEMS patterning depends on expensive device, it will reduce spin coating proceeding cost advantage.Based on micro-fluidic
The device of technical research is prepared in situ in chip, while having both high-performance, inexpensive feature, will push the quick of correlation POCT equipment
Development.
Summary of the invention
The present invention is in order to overcome the deficiencies in the prior art, technical problem to be solved are as follows: provides one kind and is based on
The micro-fluidic chip and preparation method thereof of polypyrrole electrochemical transistor；In order to solve the above-mentioned technical problem, the present invention uses
Technical solution are as follows: a kind of micro-fluidic chip based on polypyrrole electrochemical transistor, including substrate, the layer deposition of the substrate
There is conductor layer, the conductor layer is provided with electrical cable and substrate pad；The upper layer of the conductor layer is also deposited with insulating layer,
Electrode window through ray is provided on the insulating layer；
Microelectrode is also deposited on the insulating layer, one end of the microelectrode is exposed on the insulating layer, the other end of microelectrode
It is connect across electrode window through ray with conductor layer；
The microelectrode includes source electrode, grid, drain electrode；
The substrate, conductor layer, insulating layer, electrode window through ray, microelectrode collectively form substrate, and the substrate passes through with PDMS cover plate
Mechanical or physico-chemical process is bonded together；
The PDMS cover plate includes inlet, fluid transport channel, miniature circular pond, liquid outlet, and the inlet is located at PDMS lid
Piece side, the liquid outlet are located at the entrance opposite side of PDMS cover plate, and the inlet, liquid outlet pass through fluid transport channel
It is connected with miniature circular pond；
The microelectrode is arranged in the center in miniature circular pond；
Source electrode, drain electrode and the grid of the microelectrode, mutual setting triangular in shape, wherein source electrode, drain electrode are horizontal positioned, grid
It is extremely vertical to place；Organic semiconductor film is deposited between the source electrode and drain electrode.
The source electrode and drain electrode is specially the microelectrode pair of two opposite noble metal microelectrode compositions, the microelectrode pair
Spacing determined by the pattern of organic semiconductor film with structure；
The grid is source electrode and 2-10 times of the spacing that drains at a distance from organic semiconductor film；
The source electrode, grid, drain electrode are specifically made by metal or conductive metal oxide；
Source electrode, grid in the microelectrode, drain electrode are respectively served as the source electrode, grid, drain electrode of electrochemical transistor.
The organic semiconductor film specifically, using electrochemical method preparation doping one or more surfactants
Polypyrrole.
Microelectrode, the method that soft lithography prepares PDMS cover plate, electrochemical deposition system are prepared more particularly to a kind of MEMS
Standby organic semiconductor thin-film, includes the following steps:
S1: it includes: source electrode, drain and gate that microelectrode is prepared in substrate using MEMS laminated process；
S2: designing and producing PCB adapter board, the fixation for chip；
S3: the S1 chip processed is transferred on PCB, by the method for gold ball bonding by source electrode, the pad pad of drain and gate
It is connect with the small pad on pcb board；
S4: PDMS cover plate is prepared using soft lithography；
S5: the chip that S3 is obtained is bonded with PDMS cover plate, realizes encapsulation；
S6: (vacuum distillation) processing is purified to pyrrole monomer；
S7: one or more surfactants and pyrrole monomer are added in a solvent, is sufficiently stirred and is uniformly mixed so as to obtain electrolyte；
S8: by electrolyte pumping into PDMS cover plate, using the method for electrochemistry by bath deposition between source electrode and drain electrode,
Organic semiconductor film is formed, prefabricated source electrode and drain electrode is made to contact with each other；
S9: dielectric solution is pumped in PDMS cover plate, it is made sufficiently with organic semiconductor film, gate contact, to carry out electrification
Learn the test of transistor performance.
5, a kind of micro-flow control chip preparation method based on polypyrrole electrochemical transistor according to claim 4,
It is characterized by: the detailed process of the step S1 are as follows:
S101: substrate is soaked in chromic acid 24 hours, and is cleaned and is dried for standby with deionized water；First layer is deposited in substrate
Metal layer simultaneously passes through photoetching and lift-off technique, forms the electrical cable and pad pad for drawing each electrode；
S102: depositing insulating layer simultaneously etches, and forms window corresponding with source electrode, drain electrode, grid and pad pad locations；
S103: deposition second layer metal layer simultaneously passes through photoetching and lift-off technique, formation source electrode, drain and gate；
S104: source electrode, drain and gate are connect with conductor layer by the metal in electrode window through ray, and are connected with pad pad；
The pad is rectangular or square, and minimum edge is long to be greater than 1mm；The length and width of microelectrode are at least 2 μm；
The substrate can be glass, silica etc.；
The preferred metal material of microelectrode is noble metals or the metal oxides such as gold, platinum, palladium.
The detailed process of the step S2 are as follows:
S201: with Altium Designer software design PCB drawing and PCB manufacturer is submitted to；
S202: several conducting wires are respectively fixed on big pad by welding gun；
Multiple big pads, and the multiple small pads being connected by printed circuit with big pad are provided on the pcb board.
The detailed process of the step S4 are as follows:
S401: slide is soaked in chromic acid 24 hours, and is cleaned and is dried with deionized water；
S402: by slide hexamethyldisilane (HDMS) silanization；
Photoresist: being uniformly spun on slide by S403 using photoresist spinner, is then heated some time, is finally made it restore to room
Temperature；
S404: it is exposed development using ultraviolet photolithographic machine, mating developer solution obtains photoetching anode membrane；
S405: the anode membrane after development is clean；
S406: trimethylchloro-silicane alkanisation reagent (TMCS) steam treatment anode membrane is used, and with being dried with nitrogen；
S407: it pours and spin coating PDMS；
S408: it removes the bubble in PDMS and makes its solidification；
S409: cured PDMS is separated and is punched, PDMS cover plate is obtained.
The detailed process of the step S5 are as follows:
S501: PDMS miniature circular pond center is aligned with the organic semiconductor film between source electrode, drain electrode, while by conductor layer end
Pad pad expose；
S502: the PDMS cover plate of alignment is bonded with substrate by packaging technology, is packaged；
The packaging technology can be pressure sintering, light and heat catalyzed adhesive Method for bonding, organic solvent Method for bonding, bond naturally
Method, oxygen plasma oxidation sealing-in method, ultraviolet irradiation method, crosslinking agent adjust method or mechanical processing method.
The detailed process of the step S6 are as follows:
S601: the various components of distilling apparatus are cleaned, assemble distilling apparatus after waiting device is dry；
S602: it takes a certain amount of pyrrole monomer liquid to be poured into rotary flask, opens condensed water, vacuumize, in waiting device
Vacuum reaches requirement；
S603: carrying out heating water bath, bath temperature be set as 60 ~ 100 DEG C, after distillation terminates, stops heating, cooling
To room temperature, vacuum rubber pipe is pulled out, closes vacuum pump；
S604: the liquid inside rotary flask is changed into the pyrrole monomer solution after distilling for the first time, repeats above-mentioned vacuum distillation
The step of, the pyrrole monomer solution after being purified again is then in an argon atmosphere by the chromium solution after secondary purification, low
Temperature saves.
The detailed process of the step S7 are as follows:
S701: appropriate solvent is added in volumetric flask；
S702: quantitative surfactant is taken to be added in volumetric flask；
Quantitative pyrrole monomer is added dropwise in S703: Xiang Shangshu solution, later constant volume；It is stirred continuously to being completely dissolved, required for obtaining
Electrolyte；
The solvent can be the organic solutions such as aqueous solution, ethyl alcohol, acetonitrile or propene carbonate；The surfactant can be with
For lauryl sodium sulfate (SDS), neopelex (SDBS), polyvinylpyrrolidone (PVP) and polystyrene
Sodium sulfonate (PSS) etc.；The surfactant concentration ranges are 10mmol ~ 0.5mol/L；The pyrrole monomer concentration range is
10mmol~0.5mol/L。
The detailed process of the step S8 are as follows:
S801: will be between the source electrode and drain electrode in electrolyte pumping to PDMS cover plate；
S802: applying electric signal using electrochemical workstation on source-drain electrode, makes electrolyte that polymerization reaction occur, and forms organic half
Electrically conductive film connects source electrode and drain electrode；
S803: deionized water is pumped in PDMS cover plate, and remaining electrolyte is rinsed well, is then done in drying box
It is dry；
The electrical signal types can specifically use square wave, triangular wave and sine wave:
When using square wave AC signal, voltage range is 1.6V ~ 6V, and frequency is 50Hz ~ 2MHz；
When using triangular wave AC signal, voltage range is 1.6V ~ 10V, and frequency is 200Hz ~ 5MHz；
When using sine wave AC signal, voltage range is 1.6V ~ 8V, and frequency is 50Hz ~ 3MHz.
The detailed process of the step S9 are as follows:
S901: the lead of source electrode, drain and gate is connected with semiconductor analysis instrument or digital sourcemeter respectively；
S902: dielectric solution is pumped on organic semiconductor film and grid, sufficiently covers organic semiconductor film and grid；
S903: the test of device performance is carried out；
S904: deionized water is pumped in PDMS cover plate, remaining dielectric solution is rinsed well, then in drying box
It is dry；
Above-mentioned dielectric solution can be NaCl, KCl plasma water solution or 1- butyl -3- methylimidazole benzoate, 1-
Allyl -3- methylimidazole villaumite, four ferricyanide of tetrabutyl phosphine, tetrabutyl phosphine tetrafluoroborate plasma liquid.
What the present invention had compared with the existing technology has the beneficial effect that the present invention provides a kind of electrochemistry crystal of polypyrrole
Pipe micro-fluidic chip and its integrated manufacturing method in situ, can prepare electrochemical transistor, specifically quick, efficient, integratedly
It is related to that the organic semiconductor channels layers such as nano wire, the film of polypyrrole are prepared in situ using the method for AC electrochemical, forms gold
Belong to the hetero-junctions of semiconductor contact to make highly integrated electrochemical transistor array chip and preparation method thereof, the present invention mentions
The method overcome the deficiencies in the prior art that electrochemical transistor is prepared in situ based on polypyrrole out, solve its be difficult to it is integrated
Production, and the requirement to equipment and solution is lower, and more cheap.
Detailed description of the invention
The present invention will be further described in detail with reference to the accompanying drawing:
Fig. 1 is MEMS laminated process schematic diagram in present example；
Fig. 2 is PDMS cover plate preparation technology flow chart；
Fig. 3 is chip overall structure figure；
Fig. 4 is PDMS cover plate structural schematic diagram；
Fig. 5 is electrochemical deposition schematic diagram；
Fig. 6 is electrochemical transistor performance test schematic diagram；
Fig. 7 is the measurement output curve diagram of the embodiment of the present invention 1；
In figure: 1 being substrate, 2 be conductor layer, 3 be insulating layer, 4 be electrode window through ray, 5 be microelectrode, 6 be source electrode, 7 be grid, 8
It is PDMS cover plate for drain electrode, 9,10 be inlet, 11 be fluid transport channel, 12 be miniature circular pond, 13 is liquid outlet, 44 to have
Machine semiconductor film, 15 be pad pad, 20 be substrate；
31 be syringe, 32 be micro-injection pump, 33 be electrochemical workstation, 34 be microscope, 35 be semiconductor analysis instrument or
Digital sourcemeter.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below with reference in the embodiment of the present invention
Attached drawing, technical solution in the embodiment of the present invention is purged, is fully described by, it is clear that the embodiment is the present invention
A part of the embodiment, instead of all the embodiments；Based on the embodiments of the present invention, those of ordinary skill in the art do not have
It makes and obtains every other embodiment under the premise of creative work, shall fall within the protection scope of the present invention.
Micro-fluidic chip of the present invention has the advantage of array.It specifically can be by forming the miniature of array
Justify pond 12, the microelectrode 5 of array and its pad pad 15 to increase parallel detection flux.
Embodiment 1:
One, the preparation of substrate:
1, as shown in Fig. 1 (a), quartz glass is selected to be cleaned respectively with acetone, ethyl alcohol, deionized water as substrate, and dried
It does spare.First layer layer gold is deposited in substrate and by photoetching and lift-off technique, formed for draw source electrode, drain electrode and
The electrical cable and pad of grid.More specifically, using mask plate to carry out photoetching firstly, spin coating and dry on the glass sheet
Development；Then, adhesion layer of the titanium (Ti) as sheet glass and metal with a thickness of 30nm is sputtered, then is sputtered with a thickness of 200nm's
Golden (Au)；Finally, wafer is placed on 2min in the ultrasonic tank equipped with acetone, lift-off is completed, realizes the graphical of conductor layer.
2, it as shown in Fig. 1 (b), depositing insulating layer and etches, forms the window being connected with source electrode, drain and gate end
With the window for leaking out conductor layer end pad.Specifically, use PECVD growth thickness in substrate exhausted for the silica of 200nm
Edge layer, and being exposed using reticle, and with the mixed solution etching insulating layer of hydrofluoric acid and ammonium fluoride, formed with it is each micro-
The window of window and leakage conductor layer end pad that electrode end position is overlapped.
3, shown in such as Fig. 1 (c), deposit second layer metal layer and being processed by photoetching and lift-off technique to be formed source electrode,
Drain and gate microelectrode, Au layers with a thickness of 500nm.
Two, PDMS cover plate is prepared on the chip of processing preparation using soft lithography and is packaged, cover plate is prepared:
1, slide is cleaned with acetone, ethyl alcohol, deionized water respectively, removes the dirt of surface of glass slide, is subsequently placed at 80
10~20min in~100 DEG C of drying box.
2, slide hexamethyldisilane (HDMS) silylating reagent is steamed into 2min.
3, in 23 degree of darkrooms Celsius, SU8-2025 negative photoresist is toppled on slide, drips glue 6s, is used to prepare photoetching sun
Mould；Then it after above-mentioned slide being stood 10~30min, is transferred on photoresist spinner, with 2500r/min whirl coating 30s, so that photoresist
It is evenly distributed on surface of glass slide；After standing 20~40min, chip and 80 DEG C of dry 60min in drying box are taken out, 120 DEG C dry
Dry 10min.Finally above-mentioned slide is placed into 30min in draught cupboard, makes it restore to room temperature.
4, by the lithography mask version for being printed with liquid input/output port, fluid transport channel and miniature circular pond prepared according to
It is secondary to be exposed with ultraviolet photolithographic machine；After exposure, slide is immersed in configured developer solution the 5min that develops, finally uses isopropyl
Alcohol rinses the slide after 30s development, obtains photoetching anode membrane.
5, then the anode membrane after development is heated into 20min in drying box at 110 DEG C, with being dried with nitrogen after heating.
6, anode membrane trimethylchloro-silicane alkanisation reagent (TMCS) is steamed into 3min, be dried with nitrogen.
7, the formpiston chip of silanization is placed in a reservoir, configured PDMS is poured on anode membrane slide, PDMS
The thickness of layer is about 4mm.
8, said vesse is transferred in vacuum oven, vacuumizes 2~3min, remove remaining bubble in PDMS, so
80 DEG C of dry 2h in drying box afterwards solidify PDMS.
9, the PDMS cover plate after solidification is removed from formpiston, the size of needs is cut into scalpel, it is ensured that its ruler
It is very little to be less than substrate, the pad of microelectrode is exposed, the inlet of PDMS cover plate is finally got on PDMS with punch and goes out
Liquid mouth.
10, PDMS miniature circular pond center is aligned with the organic semiconductor layer between source-drain electrode, then sets them together
In plasma cleaner, oxygen plasma cleans 60s, is bonded the two, completes encapsulation.
Three, (vacuum distillation) processing is purified to pyrrole monomer:
1, the various components of distilling apparatus are cleaned, assemble distilling apparatus after waiting device is dry.
2, it takes a certain amount of pyrrole monomer liquid to be poured into rotary flask, opens condensed water, vacuumize, in waiting device
Vacuum reaches requirement.
3, heating water bath is carried out, bath temperature is set as 70 DEG C, after distillation terminates, stops heating, is cooled to
Room temperature pulls out vacuum rubber pipe, closes vacuum pump.
4, the liquid inside rotary flask is changed into the pyrrole monomer solution after distilling for the first time, repeats the step of above-mentioned 1-3
Suddenly, the chromium solution after obtaining secondary purification, then by the cryo-conservation in an argon atmosphere of the chromium solution after secondary purification.
Four, the configuration of electrolyte:
1, the volumetric flask of 5ml is added after the PSS of weighing 0.35g.
2, the pyrrole monomer of 34.16ul is added dropwise again to volumetric flask.
3,30 DEG C of heating water baths stir 1 hour after adding deionized water to be settled to 5ml, until pyrroles is completely dissolved with PSS.
Five, electrochemical deposition:
1, the configured electrolyte of 1mL is drawn with syringe 31.
2, syringe 31 is fixed on micro-injection pump 32, sets 32 parameter of micro-injection pump, it will by rubber tube
Syringe 31 is connected with the inlet of PDMS cover plate.
3, micro-injection pump 32 is opened, electrolyte is made to enter liquid transport channel by inlet, miniature circular pond is reached, makes
Electrolyte covers source electrode and drain electrode.
4, apply electric signal between source and drain microelectrode pair with electrochemical workstation 33 and prepare organic semiconductor film.Work as use
When square wave AC signal, voltage 2V, frequency 200Hz；When using triangular wave AC signal, voltage 3V, frequency is
5KHz；When using sine wave AC signal, voltage 2.5V, frequency 1KHz.
5, organic semiconductor upgrowth situation is observed by 34 observing system of microscope to stop after reaching expected upgrowth situation
Only apply electric signal.
6,3mL deionized water is drawn with another syringe 31.
7, repeat the above steps 2-3, removes the remaining electrolyte in PDMS cover plate, chip is finally put into vacuum drying
60 DEG C of dry 2h in case.
Six, the test of electrochemical transistor device performance:
1, it is respectively 4200SCS with semiconductor analysis instrument 35(instrument model by the lead of source electrode, drain and gate) or digital source
Table (mter model 2636B) is connected.
2, survey engineering is established, measurement parameter is set.
3,3mL 0.1M NaCl dielectric solution is drawn with syringe 31.
4, syringe 31 is fixed on micro-injection pump 32, sets syringe pump parameter, by rubber tube by syringe
31 are connected with the inlet of PDMS cover plate.
5, syringe pump is opened, NaCl solution is made to enter liquid transport channel by inlet, miniature circular pond is reached, covers it
Lid organic semiconductor film and grid.
6, survey engineering is opened, the test of device performance is carried out.
7,3mL deionized water is drawn with another syringe 31.
8, repeat the above steps 4-5, removes the remaining dielectric solution in PDMS cover plate, chip is finally put into vacuum
60 DEG C of dry 2h in drying box.
Seven, experimental result
Electrochemical transistor performance measurement method: using 0.1M NaCl solution as electrolyte, by 2636B digital sourcemeter into
Row measurement.When measuring curve of output, source and drain scanning voltage is 600mV ~ -600mV, stepping 80mV, grid gradient voltage is set as -
600mV ~ 600mV, stepping 100mV.When measuring transfer curve, source-drain voltage is fixed on -600mV, and gated sweep voltage is -
600mV ~ 600mV, stepping 50mV.Measurement result is as shown below.
Analysis measurement result can obtain:
Claims (10)
1. a kind of micro-fluidic chip based on polypyrrole electrochemical transistor, it is characterised in that: including substrate (1), the substrate
(1) layer deposition has conductor layer (2), and the conductor layer (2) is provided with electrical cable and substrate pad；The conductor layer (2)
Upper layer be also deposited with insulating layer (3), be provided with electrode window through ray (4) on the insulating layer (3)；
It is also deposited with microelectrode (5) on the insulating layer (3), one end of the microelectrode (5) is exposed on insulating layer (3), micro-
The other end of electrode (5) passes through electrode window through ray (4) and connect with conductor layer (2)；
The microelectrode (5) includes source electrode (6), grid (7), drain electrode (8)；
The substrate (1), conductor layer (2), insulating layer (3), electrode window through ray (4), microelectrode (5) collectively form substrate (20), institute
It states substrate (20) and is bonded together with PDMS cover plate (9) by mechanical or physico-chemical process；
The PDMS cover plate (9) includes inlet (10), fluid transport channel (11), miniature circular pond (12), liquid outlet (13), institute
It states inlet (10) and is located at PDMS cover plate (9) side, the liquid outlet (13) is located at the entrance opposite side of PDMS cover plate (9), institute
Inlet (10), liquid outlet (13) is stated to be connected by fluid transport channel (11) with miniature circular pond (12)；
The microelectrode (5) is arranged in the center of miniature circular pond (12)；
The source electrode (6) of the microelectrode, drain (8) and grid (7), mutual setting triangular in shape, wherein source electrode (6), leakage
Pole (8) is horizontal positioned, and grid (7) is placed vertically；Organic semiconductor film (44) are deposited between the source electrode (6) and drain electrode (8).
2. a kind of micro-fluidic chip based on polypyrrole electrochemical transistor according to claim 1, it is characterised in that:
The source electrode (6) and drain electrode (8) are specially the microelectrode pair of two opposite noble metal microelectrode compositions, the microelectrode
Pair spacing determined by the pattern of organic semiconductor film (44) with structure；
The grid (7) is source electrode (6) and 2-10 times of (8) spacing that drains at a distance from organic semiconductor film (44)；
The source electrode (6), grid (7), drain electrode (8) are specifically made by metal or conductive metal oxide；
Source electrode (6), grid (7), drain electrode (8) in the microelectrode are respectively served as the source electrode, grid, leakage of electrochemical transistor
Pole；
The organic semiconductor film (44) specifically, using electrochemical method preparation doping one or more surfactants
Polypyrrole.
3. a kind of micro-flow control chip preparation method based on polypyrrole electrochemical transistor, it is characterised in that: more particularly to one kind
MEMS is prepared microelectrode (5), the method that soft lithography prepares PDMS cover plate (9), and electrochemical deposition prepares organic semiconductor film
Film (44), includes the following steps:
S1: it includes: source electrode (6), drain electrode (8) and grid (7) that microelectrode (5) is prepared on substrate (1) using MEMS laminated process；
S2: designing and producing PCB adapter board, the fixation for chip；
S3: the S1 chip processed is transferred on PCB, by the method for gold ball bonding by source electrode (6), drain electrode (8) and grid (7)
Pad pad (15) connect with the small pad on pcb board；
S4: soft lithography preparation PDMS cover plate (9) is utilized；
S5: the chip that S3 is obtained is bonded with PDMS cover plate (9), realizes encapsulation；
S6: (vacuum distillation) processing is purified to pyrrole monomer；
S7: one or more surfactants and pyrrole monomer are added in a solvent, is sufficiently stirred and is uniformly mixed so as to obtain electrolyte；
S8: it by electrolyte pumping into PDMS cover plate (9), by bath deposition to source electrode (6) and is leaked using the method for electrochemistry
It between pole (8), is formed organic semiconductor film (44), prefabricated source electrode (6) and drain electrode (8) is made to contact with each other；
S9: dielectric solution is pumped in PDMS cover plate (9), connects it sufficiently with organic semiconductor film (44), grid (7)
Touching carries out the test of electrochemical transistor performance.
4. a kind of micro-flow control chip preparation method based on polypyrrole electrochemical transistor according to claim 3, special
Sign is: the detailed process of the step S1 are as follows:
S101: substrate (1) is soaked in chromic acid 24 hours, and is cleaned and is dried for standby with deionized water；It is deposited on substrate (1)
First layer metal layer simultaneously passes through photoetching and lift-off technique, forms the electrical cable and pad for drawing each electrode
Pad (15)；
S102: depositing insulating layer (3) simultaneously etches, and is formed and source electrode (6), drain electrode (8), grid (7) and pad pad (15) position
Corresponding window；
S103: deposition second layer metal layer simultaneously passes through photoetching and lift-off technique, formation source electrode (6), drain electrode (8) and grid
(7)；
S104: source electrode (6), drain electrode (8) and grid (7) are connect by the metal in electrode window through ray (4) with conductor layer (2), and with
Pad pad (15) is connected；
The pad is rectangular or square, and minimum edge is long to be greater than 1mm；The length and width of microelectrode (5) are at least 2 μm；
The substrate (1) can be glass, silica etc.；
The preferred metal material of the microelectrode (5) is noble metals or the metal oxides such as gold, platinum, palladium.
5. a kind of micro-flow control chip preparation method based on polypyrrole electrochemical transistor according to claim 4, special
Sign is: the detailed process of the step S2 are as follows:
S201: with Altium Designer software design PCB drawing and PCB manufacturer is submitted to；
S202: several conducting wires are respectively fixed on big pad by welding gun；
Multiple big pads, and the multiple small pads being connected by printed circuit with big pad are provided on the pcb board；
The detailed process of the step S4 are as follows:
S401: slide is soaked in chromic acid 24 hours, and is cleaned and is dried with deionized water；
S402: by slide hexamethyldisilane (HDMS) silanization；
Photoresist: being uniformly spun on slide by S403 using photoresist spinner, is then heated some time, is finally made it restore to room
Temperature；
S404: it is exposed development using ultraviolet photolithographic machine, mating developer solution obtains photoetching anode membrane；
S405: the anode membrane after development is clean；
S406: trimethylchloro-silicane alkanisation reagent (TMCS) steam treatment anode membrane is used, and with being dried with nitrogen；
S407: it pours and spin coating PDMS；
S408: it removes the bubble in PDMS and makes its solidification；
S409: separating cured PDMS and punch, obtains PDMS cover plate (9).
6. a kind of micro-flow control chip preparation method based on polypyrrole electrochemical transistor according to claim 5, special
Sign is: the detailed process of the step S5 are as follows:
S501: PDMS miniature circular pond (12) center is aligned with the organic semiconductor film (44) between source electrode (6), drain electrode (8), together
When the Pad pad (15) of conductor layer (2) end is exposed；
S502: the PDMS cover plate (9) of alignment is bonded with substrate (20) by packaging technology, is packaged；
The packaging technology can be pressure sintering, light and heat catalyzed adhesive Method for bonding, organic solvent Method for bonding, bond naturally
Method, oxygen plasma oxidation sealing-in method, ultraviolet irradiation method, crosslinking agent adjust method or mechanical processing method.
7. a kind of micro-flow control chip preparation method based on polypyrrole electrochemical transistor according to claim 6, special
Sign is: the detailed process of the step S6 are as follows:
S601: the various components of distilling apparatus are cleaned, assemble distilling apparatus after waiting device is dry；
S602: it takes a certain amount of pyrrole monomer liquid to be poured into rotary flask, opens condensed water, vacuumize, in waiting device
Vacuum reaches requirement；
S603: carrying out heating water bath, bath temperature be set as 60 ~ 100 DEG C, after distillation terminates, stops heating, cooling
To room temperature, vacuum rubber pipe is pulled out, closes vacuum pump；
S604: the liquid inside rotary flask is changed into the pyrrole monomer solution after distilling for the first time, repeats above-mentioned vacuum distillation
The step of, the pyrrole monomer solution after being purified again is then in an argon atmosphere by the chromium solution after secondary purification, low
Temperature saves.
8. a kind of micro-flow control chip preparation method based on polypyrrole electrochemical transistor according to claim 7, special
Sign is: the detailed process of the step S7 are as follows:
S701: appropriate solvent is added in volumetric flask；
S702: quantitative surfactant is taken to be added in volumetric flask；
Quantitative pyrrole monomer is added dropwise in S703: Xiang Shangshu solution, later constant volume；It is stirred continuously to being completely dissolved, required for obtaining
Electrolyte；
The solvent can be the organic solutions such as aqueous solution, ethyl alcohol, acetonitrile or propene carbonate；The surfactant can be with
For lauryl sodium sulfate (SDS), neopelex (SDBS), polyvinylpyrrolidone (PVP) and polystyrene
Sodium sulfonate (PSS) etc.；The surfactant concentration ranges are 10mmol ~ 0.5mol/L；The pyrrole monomer concentration range is
10mmol~0.5mol/L。
9. a kind of micro-flow control chip preparation method based on polypyrrole electrochemical transistor according to claim 8, special
Sign is: the detailed process of the step S8 are as follows:
S801: by the source electrode (6) in electrolyte pumping to PDMS cover plate (9) and between drain electrode (8)；
S802: applying electric signal using electrochemical workstation on source-drain electrode, makes electrolyte that polymerization reaction occur, and forms organic half
Electrically conductive film (44) connects source electrode (6) and drain electrode (8)；
S803: deionized water is pumped in PDMS cover plate (9), remaining electrolyte is rinsed well, then in drying box
It is dry；
The electrical signal types can specifically use square wave, triangular wave and sine wave:
When using square wave AC signal, voltage range is 1.6V ~ 6V, and frequency is 50Hz ~ 2MHz；
When using triangular wave AC signal, voltage range is 1.6V ~ 10V, and frequency is 200Hz ~ 5MHz；
When using sine wave AC signal, voltage range is 1.6V ~ 8V, and frequency is 50Hz ~ 3MHz.
10. a kind of micro-flow control chip preparation method based on polypyrrole electrochemical transistor according to claim 9, special
Sign is: the detailed process of the step S9 are as follows:
S901: the lead of source electrode (6), drain electrode (8) and grid (7) is connected with semiconductor analysis instrument or digital sourcemeter respectively；
S902: dielectric solution is pumped on organic semiconductor film (44) and grid (7), sufficiently covering organic semiconductor film
(44) and grid (7)；
S903: the test of device performance is carried out；
S904: deionized water is pumped in PDMS cover plate (9), remaining dielectric solution is rinsed well, then in drying
It is dry in case；
Above-mentioned dielectric solution can be NaCl, KCl plasma water solution or 1- butyl -3- methylimidazole benzoate, 1-
Allyl -3- methylimidazole villaumite, four ferricyanide of tetrabutyl phosphine, tetrabutyl phosphine tetrafluoroborate plasma liquid.
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