CN107525832A - A kind of preparation method of the flexible fiber sensor electrode of nano silver wire modification - Google Patents
A kind of preparation method of the flexible fiber sensor electrode of nano silver wire modification Download PDFInfo
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- CN107525832A CN107525832A CN201710755720.2A CN201710755720A CN107525832A CN 107525832 A CN107525832 A CN 107525832A CN 201710755720 A CN201710755720 A CN 201710755720A CN 107525832 A CN107525832 A CN 107525832A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 51
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000013305 flexible fiber Substances 0.000 title claims abstract description 29
- 230000004048 modification Effects 0.000 title claims abstract description 28
- 238000012986 modification Methods 0.000 title claims abstract description 28
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 58
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000000835 fiber Substances 0.000 claims abstract description 35
- 239000002253 acid Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 34
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 22
- 239000002131 composite material Substances 0.000 claims description 19
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 16
- 235000011187 glycerol Nutrition 0.000 claims description 16
- 238000000498 ball milling Methods 0.000 claims description 15
- 229920001940 conductive polymer Polymers 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- 235000011089 carbon dioxide Nutrition 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 5
- 239000000178 monomer Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 239000013049 sediment Substances 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical class [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 229910000831 Steel Inorganic materials 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000010959 steel Substances 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims 1
- -1 graphite Alkene Chemical class 0.000 claims 1
- 229920002521 macromolecule Polymers 0.000 claims 1
- 229920006389 polyphenyl polymer Polymers 0.000 claims 1
- 238000000527 sonication Methods 0.000 claims 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims 1
- 229920002554 vinyl polymer Polymers 0.000 claims 1
- 239000000758 substrate Substances 0.000 abstract description 3
- 239000004020 conductor Substances 0.000 abstract description 2
- 229920000468 styrene butadiene styrene block copolymer Polymers 0.000 abstract 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 abstract 2
- 238000012544 monitoring process Methods 0.000 abstract 2
- FACXGONDLDSNOE-UHFFFAOYSA-N buta-1,3-diene;styrene Chemical compound C=CC=C.C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 FACXGONDLDSNOE-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 47
- 239000010408 film Substances 0.000 description 19
- 239000007788 liquid Substances 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 229920003023 plastic Polymers 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 241000790917 Dioxys <bee> Species 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000703 high-speed centrifugation Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000007306 functionalization reaction Methods 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229930192474 thiophene Natural products 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- DSVGQVZAZSZEEX-UHFFFAOYSA-N [C].[Pt] Chemical compound [C].[Pt] DSVGQVZAZSZEEX-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- DMGKBWHEBNPKJB-UHFFFAOYSA-N benzene;buta-1,3-diene;styrene Chemical compound C=CC=C.C1=CC=CC=C1.C=CC1=CC=CC=C1 DMGKBWHEBNPKJB-UHFFFAOYSA-N 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000003851 corona treatment Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229920002457 flexible plastic Polymers 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 229940059939 kayexalate Drugs 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000008447 perception Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 229920001467 poly(styrenesulfonates) Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The present invention relates to sensor field, discloses a kind of preparation method of the flexible fiber sensor electrode of nano silver wire modification, compliant conductive fiber is prepared by solution mixing method, wherein with styrene butadiene styrene block copolymer(Styrene butadiene styrene block copolymer)For flexible substrates, with poly- 3,4 ethene dioxythiophene polystyrolsulfon acid graphenes are conductive material, and with nano silver wire modified electrode, obtain a kind of flexible fiber sensor electrode of styrene butadiene styrene/graphene/poly- 3,4 ethene dioxythiophene polystyrolsulfon acid based on nano silver wire modification.Inventive sensor electrode can be applied to medical biological monitoring, the field such as environment and the monitoring of hygiene.
Description
Technical field
The present invention relates to sensor field, more particularly to a kind of system of the flexible fiber sensor electrode of nano silver wire modification
Preparation Method.
Background technology
Sensor is that mankind itself finds out to the various sensory informations of nature, and unlike signal and perception information can be turned
Turn to can digitize, intelligentized important devices.During human civilization rapid development of information technology, sensor serves
Increasingly heavier effect, it is that the mankind explore outfield, while is also that the mankind understand real world, observes the important of peripheral information
One of means.Sensor be it is a kind of the non-electrical signal such as electricity, light, temperature and chemical action can be converted into electrical signal can
The component of regulation and control.
Graphene is a kind of new carbon two-dimensional nano light material, has unique monoatomic layer two dimensional crystal structure, greatly
Quantifier elimination result shows that graphene has known materials highest intensity, big specific surface area ratio, excellent electric conductivity and leads
The excellent property such as hot, these excellent properties also determine that it is many in such as composite, electronic device, solar energy etc.
Field has a wide range of applications.
Majority is that conductive material is combined on platinum carbon electrode in the prior art, and composite is relatively simple, electric conductivity
It is bad, existing defects, and without flexibility, it is impossible to be used in wearable device, i.e., it can not preferably play the practical valency of sensor
Value.
The content of the invention
In order to solve the above-mentioned technical problem, the invention provides a kind of flexible fiber sensor electrode of nano silver wire modification
Preparation method.The present invention is using SBS as thin film flexible substrate, by poly- 3,4- ethene
Dioxy thiophene-polystyrolsulfon acid and graphene carry out it is compound obtain the conductive film of flexible and transparent, then nano silver wire is carried out
Modification, new footpath is opened up in the application of flexible sensor for it, there is more excellent detection performance compared with traditional sensors.
The present invention concrete technical scheme be:A kind of preparation side of the flexible fiber sensor electrode of nano silver wire modification
Method, comprise the following steps:
(1)The preparation of oiliness film forming solution:SBS is taken to be added to chloroform soln
In, stood after stirring, be completely dissolved SBS, obtain oiliness film forming solution, it is stand-by.
S-B-S resin has the characteristic of plastics and rubber concurrently, can be contacted with water, weak acid, alkali etc.,
With excellent tensile strength, big surface friction coefficient, low temperature performance well, excellent electrical properties, the advantages that processing characteristics is good.
(2)Ball-milling method prepares graphene:Graphite powder is added in ball grinder and humid medium carries out ball milling, rotary-tray rotating speed
For 2800-3200rpm, Ball-milling Time 40-50h, can opening takes out graphene and adds undesired impurities in hydrochloric acid cleaning removing product,
It is net being washed with deionized water, freeze-drying, obtain solid graphene.
Ball-milling method is a kind of mechanical stripping technology, green, simple to operate, low cost.Avoid due to redox
Method uses reducing agent potential hazards to caused by experiment operator and environment such as strong acid and hydrazine hydrate.
(3)The preparation of poly- 3,4- ethene dioxythiophenes-polystyrolsulfon acid-graphene conductive composite material:Weigh solid
Graphene is added in polystyrolsulfon acid solution, ultrasonic disperse, then adds 3,4-rthylene dioxythiophene monomer, and stirring
Under the conditions of be added dropwise liquor ferri trichloridi, continue stirring reaction 10-14h, centrifuge the blackish green slurries of gained, and respectively
Clean repeatedly, collection solid colourless to cleaning solution repeatedly with absolute ethyl alcohol and distilled water, 10-14h be dried in vacuo at 70-80 DEG C,
Obtain poly- 3,4- ethene dioxythiophenes-polystyrolsulfon acid-graphene conductive composite material.
Derivative of the poly- 3,4-rthylene dioxythiophene as polythiophene, with molecular structure is simple, energy gap is small, electrical conductivity is high
With transparency it is high the features such as.To solve the insoluble infusibility of poly- 3,4-rthylene dioxythiophene, polystyrolsulfon acid is introduced into poly- 3,
4- ethene dioxythiophenes, form the poly- 3,4- ethene dioxythiophenes-polystyrolsulfon acid of dispersiveness and processability well and suspend
Liquid, poly- 3,4-rthylene dioxythiophene-polystyrolsulfon acid aqueous solution have good film forming and environmental stability.
Graphene is added in polystyrolsulfon acid solution, ultrasonic disperse, will be poly- its purpose is to make graphene functionalized
In SSS load and graphene, and it polymerize poly- 3,4- ethylene dioxies thiophene by carrier situ of the graphene of functionalization
Fen, it is set mutually to combine closely.Poly- 3,4- ethene dioxythiophenes-polystyrolsulfon acid-graphene is obtained by the method for polymerization
Composite is together with each other by the effect for then passing through chemical bond, substantially increases the migration rate of electronics, than that will gather
3,4- ethene dioxythiophenes-polystyrolsulfon acid solution and the simple physical mixed electric conductivity of graphene want it is superior a lot.
By together with graphene and poly- 3,4- ethene dioxythiophenes-polystyrolsulfon acid doping with obtain electric conductivity it is excellent plus
Material, and using s-B-S as flexible plastic substrates, obtain the very superior flexible and transparent conductive of performance
Film, wearable biological sensor electrode can be used as, there is very wide application prospect.
(4)The preparation of waterborne conductive solution:By step(3)Obtained poly- 3,4- ethene dioxythiophenes-polystyrolsulfon acid-
Graphene conductive composite material is added in water, ultrasonic disperse, obtains waterborne conductive solution, stand-by.
(5)The preparation of conductive polymer fiber:By step(4)Waterborne conductive solution and step(1)Oiliness film forming it is molten
Liquid is mixed, and with being ultrasonically treated, so as to obtain mixing homogeneous water oil(W/O)Conducting solution, take conductive mixed liquor
Pour into special mould, after placing 20-30h, spontaneously dry, take out conductive fiber and dry.
(6)The preparation of flexible fiber sensor electrode:By step(5)Obtained conductive polymer fiber is cut to segment.
(7)The preparation of nano silver wire:Glycerine is added in 500mL three-necked flasks, 5-6gPVP is added, is warming up to 55-65
DEG C and mechanical agitation until PVP be completely dissolved;After system temperature is down to room temperature, 1-2g silver nitrates are added, are stirred to completely molten
Solution;Then the glycerin solution 8-12mL containing 56-60mg sodium chloride and 0.3-0.7mL water is added, is persistently stirred under agitation
And heat, heating is closed after temperature reaches setting value, is down to room temperature;The water of same volume is added, upper strata is gone to after standing overnight
Clear liquid, the sediment of solution bottom is disperseed again with isopropanol, then solution is repeated several times, obtained in centrifugal treating
The nano silver wire being dispersed in aqueous isopropanol.
PVP is surfactant, and glycerine is solvent and reducing agent, and reproducibility is higher than ethylene glycol, obtained silver nanoparticle
Line yield is higher.Carried out being centrifuged off impurity and unreacted PVP with isopropanol.
(8)The preparation of the flexible fiber sensor electrode of nano silver wire modification:The height after cutting is handled with oxygen plasma
Molecule conductive fiber surfaces, then conductive polymer fiber is invaded in the aqueous isopropanol containing nano silver wire, at room temperature
Dry, obtain the flexible fiber sensor electrode of nano silver wire modification.
Because flexible fiber passes through corona treatment, nano silver wire is set to adsorb in fiber surface, because isopropanol is easy
Volatilization, nano silver wire just adsorbs in fiber surface completely after the volatilization of several hours.
Preferably, step(1)In, SBS in the oiliness film forming solution
Mass fraction is 5-20%.
Preferably, step(2)In, the humid medium is dimethylformamide, 1-METHYLPYRROLIDONE, surfactant
The aqueous solution, dry ice one kind therein.
Because dimethylformamide, 1-METHYLPYRROLIDONE, aqueous surfactant solution etc. are organic solvent and medium, have
Certain toxicity, and extent of exfoliation is low, while ball-milling medium is due to decomposition, the ball milling solvent in mechanical milling process caused by high-energy
Decomposition with medium can not avoid, and cause fragmentation and defect, and the defects of so as to introduce and impurity is also uncontrollable.Dry ice is on the one hand
Charge stripping efficiency can be improved, on the other hand can reduce graphene size, while it is controllable to introduce impurity.
Preferably, step(3)In, graphene and polystyrolsulfon acid, poly- 3,4-rthylene dioxythiophene, the matter of iron chloride
It is 1-2 to measure ratio:1-2:1-3:1-3.
Preferably, step(4)In, time of ultrasonic disperse is 25-35min, poly- 3,4- ethene in waterborne conductive solution
The mass fraction of dioxy thiophene-polystyrolsulfon acid-graphene is 5-20%.
Preferably, step(5)In, the weight ratio of waterborne conductive solution and oiliness film forming solution is 0.1-1:1;At ultrasound
The reason time is 10-20min;The mould is a long body steel plate, and steel plate center is machined with the groove of a fiber shape, groove length
25-35cm, diameter 2.5-3.5mm, drying temperature are 65-75 DEG C, drying time 1.5-2.5h.
Preferably, step(6)In, the length of the conductive polymer fiber after cutting is 7-9mm.
Preferably, step(7)In, the volume of glycerine is 180-200mL, 200-220 DEG C of the temperature of heating, the body of water
Product is 180-200mL, centrifugation rate 5000-7000rpm/min, centrifugation time 8-12min.
Preferably, step(8)In, the time dried at room temperature is at least 5h.
It is compared with the prior art, the beneficial effects of the invention are as follows:
1st, the present invention has the characteristic of plastics and rubber, styrene-butadiene-benzene second concurrently with s-B-S resin
Alkene block copolymer can contact with water, weak acid, alkali etc., have excellent tensile strength, big surface friction coefficient, cryogenic property
It is good, excellent electrical properties, the advantages that processing characteristics is good.Make the conductive film of preparation there is very flexibility and certain stretching
Property.
2nd, graphene is added in polystyrolsulfon acid solution, ultrasonic disperse, its purpose is to make graphite olefinic functionality
Change, kayexalate is loaded on graphene, and polymerize poly- 3,4- ethene by carrier situ of the graphene of functionalization
Dioxy thiophene, it is set mutually to combine closely.Poly- 3,4- ethene dioxythiophenes-polystyrolsulfon acid-is obtained by the method for polymerization
Graphene composite material is together with each other by the effect for then passing through chemical bond, considerably increases the migration rate of electronics,
Improve the electric conductivity of film.
3rd, nano silver wire can be widely used in electrode material due to itself special one-dimentional structure and excellent conduction
Material, nano silver wire is as modification, additionally it is possible to the defects of filling up graphene, is that electric conductivity is more excellent.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
(1)The preparation of oiliness film forming solution
1g SBS plastics are taken to be added in 20mL chloroform soln, after stirring
One day is stood, SBS is completely dissolved in chloroform soln, prepares mass
Fraction is 5% oiliness film forming solution.
(2)Ball-milling method prepares graphene
20g graphite powders and 400g dry ice are added in ball grinder, it is 3000rpm to control rotary-tray rotating speed, and Ball-milling Time is
48h, obtains aterrimus graphene, and can opening, which takes out graphene and adds hydrochloric acid cleaning, removes impurity unnecessary in product, spend from
Sub- water cleaning three times, freeze-drying, obtains solid graphene.
(3)The preparation of poly- 3,4- ethene dioxythiophenes-polystyrolsulfon acid-graphene conductive composite material
Take 20mg graphene to be added in 20mL polystyrolsulfon acid solution, ultrasonic disperse 30min, then add 3,4- second
Alkene dioxythiophene monomers 200uL, and 10mL, 14mmoL/L liquor ferri trichloridi are added dropwise in the case of stirring, continue to stir
Reaction 12h is mixed, centrifuges prepared blackish green slurries, and is cleaned repeatedly repeatedly with absolute ethyl alcohol and distilled water to washing respectively
It is colourless to wash liquid, collects solid and is dried in vacuo 12h at 75 DEG C, obtain poly- 3,4-rthylene dioxythiophene-polystyrolsulfon acid-graphite
Alkene conducing composite material.
(4)The preparation of waterborne conductive solution
1g poly- 3,4- ethene dioxythiophenes-polystyrolsulfon acid-graphene conductive composite material is taken to be added to the water-soluble of 20mL
In liquid, ultrasonic disperse 30min, poly- 3,4-rthylene dioxythiophene-polystyrolsulfon acid-graphene that mass fraction is 5% is made
Solution.
(5)The preparation of conductive polymer fiber
Take 1mL aqueous solutions and 10mL oiliness film forming solution to be mixed, and be ultrasonically treated with ultrasonic processor
15min, so as to obtain mixing homogeneous water oil(W/O)Conducting solution, 3mL conductive mixed liquor is taken to pour into fibrous type mould,
After placing 24h, spontaneously dry, taking-up conductive fiber, which is placed in 70 DEG C of constant temperature ovens, dries 2h.
(6)The preparation of flexible sensor electrode
Take step(5)Obtained conductive polymer fiber, it is 8mm to control its fibre length.
(7)The preparation of nano silver wire
190mL glycerine is added in 500mL three-necked flasks, adds 5.86gPVP, be warming up to 60 DEG C and mechanical agitation until
PVP is dissolved completely in glycerine.After system temperature is down to room temperature, 1.58g silver nitrates are added, stirring is to being completely dissolved.So
The glycerin solution 10mL containing 59mg sodium chloride and 0.5mL water is added afterwards, is persistently stirred and heated under low stir speed (S.S.)
210 DEG C, heating is closed after temperature is raised to 210 DEG C, allows it to be slowly dropped to room temperature.With 1:1 ratio adds 190mL water, quiet
Remove supernatant liquor after putting overnight, with isopropanol redisperse beaker bottom sediment, then by solution on centrifuge with
6000rpm/min high speed centrifugation 10min, so repeat 3 times, obtained being dispersed in the nano silver wire in aqueous isopropanol.
(8)The preparation of the flexible fiber sensor electrode of nano silver wire modification
Fiber surface is handled with oxygen plasma, fiber is then invaded at least 5h in the aqueous isopropanol containing nano silver wire,
And be dried at room temperature for, obtain the flexible fiber sensor electrode of nano silver wire modification.
Embodiment 2
(1)The preparation of oiliness film forming solution
1g SBS plastics are taken to be added in 20mL chloroform soln, after stirring
One day is stood, SBS is completely dissolved in chloroform soln, prepares mass
Fraction is 5% oiliness film forming solution.
(2)Ball-milling method prepares graphene
20g graphite powders and 400g dry ice are added in ball grinder, it is 3000rpm to control rotary-tray rotating speed, and Ball-milling Time is
48h, obtains aterrimus graphene, and can opening, which takes out graphene and adds hydrochloric acid cleaning, removes impurity unnecessary in product, spend from
Sub- water cleaning three times, freeze-drying, obtains solid graphene.
(3)The preparation of poly- 3,4- ethene dioxythiophenes-polystyrolsulfon acid-graphene conductive composite material
Take 20mg graphene to be added in 20mL polystyrolsulfon acid solution, ultrasonic disperse 30min, then add 3,4- second
Alkene dioxythiophene monomers 200uL, and 10mL, 14mmoL/L liquor ferri trichloridi are added dropwise in the case of stirring, continue to stir
Reaction 12h is mixed, centrifuges prepared blackish green slurries, and is cleaned repeatedly repeatedly with absolute ethyl alcohol and distilled water to washing respectively
It is colourless to wash liquid, collects solid and is dried in vacuo 12h at 75 DEG C, obtain poly- 3,4-rthylene dioxythiophene-polystyrolsulfon acid-graphite
Alkene conducing composite material.
(4)The preparation of waterborne conductive solution
1g poly- 3,4- ethene dioxythiophenes-polystyrolsulfon acid-graphene conductive composite material is taken to be added to the water-soluble of 20mL
In liquid, ultrasonic disperse 30min, poly- 3,4-rthylene dioxythiophene-polystyrolsulfon acid-graphene that mass fraction is 5% is made
Solution.
(5)The preparation of conductive polymer fiber
Take 5mL aqueous solutions and 10mL oiliness film forming solution to be mixed, and be ultrasonically treated with ultrasonic processor
15min, so as to obtain mixing homogeneous water oil(W/O)Conducting solution, 3mL conductive mixed liquor is taken to pour into fibrous type mould,
After placing 24h, spontaneously dry, taking-up conductive fiber, which is placed in 70 DEG C of constant temperature ovens, dries 2h.
(6)The preparation of flexible sensor electrode
Take step(5)Obtained conductive polymer fiber, it is 8mm to control its fibre length.
(7)The preparation of nano silver wire
190mL glycerine is added in 500mL three-necked flasks, adds 5.86gPVP, be warming up to 60 DEG C and mechanical agitation until
PVP is dissolved completely in glycerine.After system temperature is down to room temperature, 1.58g silver nitrates are added, stirring is to being completely dissolved.So
The glycerin solution 10mL containing 59mg sodium chloride and 0.5mL water is added afterwards, is persistently stirred and heated under low stir speed (S.S.)
210 DEG C, heating is closed after temperature is raised to 210 DEG C, allows it to be slowly dropped to room temperature.With 1:1 ratio adds 190mL water, quiet
Remove supernatant liquor after putting overnight, with isopropanol redisperse beaker bottom sediment, then by solution on centrifuge with
6000rpm/min high speed centrifugation 10min, so repeat 3 times, obtained being dispersed in the nano silver wire in aqueous isopropanol.
(8)The preparation of the flexible fiber sensor electrode of nano silver wire modification
Fiber surface is handled with oxygen plasma, fiber is then invaded at least 5h in the aqueous isopropanol containing nano silver wire,
And be dried at room temperature for, obtain the flexible fiber sensor electrode of nano silver wire modification.
Embodiment 3
(1)The preparation of oiliness film forming solution
1g SBS plastics are taken to be added in 20mL chloroform soln, after stirring
One day is stood, SBS is completely dissolved in chloroform soln, prepares mass
Fraction is 5% oiliness film forming solution.
(2)Ball-milling method prepares graphene
20g graphite powders and 400g dry ice are added in ball grinder, it is 3000rpm to control rotary-tray rotating speed, and Ball-milling Time is
48h, obtains aterrimus graphene, and can opening, which takes out graphene and adds hydrochloric acid cleaning, removes impurity unnecessary in product, spend from
Sub- water cleaning three times, freeze-drying, obtains solid graphene.
(3)The preparation of poly- 3,4- ethene dioxythiophenes-polystyrolsulfon acid-graphene conductive composite material
Take 20mg graphene to be added in 20mL polystyrolsulfon acid solution, ultrasonic disperse 30min, then add 3,4- second
Alkene dioxythiophene monomers 200uL, and 10mL, 14mmoL/L liquor ferri trichloridi are added dropwise in the case of stirring, continue to stir
Reaction 12h is mixed, centrifuges prepared blackish green slurries, and is cleaned repeatedly repeatedly with absolute ethyl alcohol and distilled water to washing respectively
It is colourless to wash liquid, collects solid and is dried in vacuo 12h at 75 DEG C, obtain poly- 3,4-rthylene dioxythiophene-polystyrolsulfon acid-graphite
Alkene conducing composite material.
(4)The preparation of waterborne conductive solution
1g poly- 3,4- ethene dioxythiophenes-polystyrolsulfon acid-graphene conductive composite material is taken to be added to the water-soluble of 20mL
In liquid, ultrasonic disperse 30min, poly- 3,4-rthylene dioxythiophene-polystyrolsulfon acid-graphene that mass fraction is 5% is made
Solution.
(5)The preparation of conductive polymer fiber
Take 10mL aqueous solutions and 10mL oiliness film forming solution to be mixed, and be ultrasonically treated with ultrasonic processor
15min, so as to obtain mixing homogeneous water oil(W/O)Conducting solution, 3mL conductive mixed liquor is taken to pour into fibrous type mould,
After placing 24h, spontaneously dry, taking-up conductive fiber, which is placed in 70 DEG C of constant temperature ovens, dries 2h.
(6)The preparation of flexible sensor electrode
Take step(5)Obtained conductive polymer fiber, it is 8mm to control its fibre length.
(7)The preparation of nano silver wire
190mL glycerine is added in 500mL three-necked flasks, adds 5.86gPVP, be warming up to 60 DEG C and mechanical agitation until
PVP is dissolved completely in glycerine.After system temperature is down to room temperature, 1.58g silver nitrates are added, stirring is to being completely dissolved.So
The glycerin solution 10mL containing 59mg sodium chloride and 0.5mL water is added afterwards, is persistently stirred and heated under low stir speed (S.S.)
210 DEG C, heating is closed after temperature is raised to 210 DEG C, allows it to be slowly dropped to room temperature.With 1:1 ratio adds 190mL water, quiet
Remove supernatant liquor after putting overnight, with isopropanol redisperse beaker bottom sediment, then by solution on centrifuge with
6000rpm/min high speed centrifugation 10min, so repeat 3 times, obtained being dispersed in the nano silver wire in aqueous isopropanol.
(8)The preparation of the flexible fiber sensor electrode of nano silver wire modification
Fiber surface is handled with oxygen plasma, fiber is then invaded at least 5h in the aqueous isopropanol containing nano silver wire,
And be dried at room temperature for, obtain the flexible fiber sensor electrode of nano silver wire modification.
Raw materials used in the present invention, equipment, it is the conventional raw material, equipment of this area unless otherwise noted;It is used in the present invention
Method, it is the conventional method of this area unless otherwise noted.
It is described above, only it is presently preferred embodiments of the present invention, not the present invention is imposed any restrictions, it is every according to the present invention
Any simple modification, change and the equivalent transformation that technical spirit is made to above example, still fall within the technology of the present invention side
The protection domain of case.
Claims (9)
1. a kind of preparation method of the flexible fiber sensor electrode of nano silver wire modification, it is characterised in that comprise the following steps:
(1)The preparation of oiliness film forming solution:SBS is taken to be added to chloroform soln
In, stood after stirring, be completely dissolved SBS, obtain oiliness film forming solution, it is stand-by;
(2)Ball-milling method prepares graphene:Graphite powder is added in ball grinder and humid medium carries out ball milling, rotary-tray rotating speed is
2800-3200rpm, Ball-milling Time 40-50h, can opening take out graphene and add undesired impurities in hydrochloric acid cleaning removing product,
It is washed with deionized water only, freeze-drying, obtains solid graphene;
(3)The preparation of poly- 3,4- ethene dioxythiophenes-polystyrolsulfon acid-graphene conductive composite material:Weigh solid graphite
Alkene is added in polystyrolsulfon acid solution, ultrasonic disperse, then adds 3,4-rthylene dioxythiophene monomer, and in stirring condition
Under be added dropwise liquor ferri trichloridi, continue stirring reaction 10-14h, centrifuge the blackish green slurries of gained, and use nothing respectively
Water-ethanol and distilled water clean repeatedly, collection solid colourless to cleaning solution repeatedly, are dried in vacuo 10-14h at 70-80 DEG C, obtain
Poly- 3,4- ethene dioxythiophenes-polystyrolsulfon acid-graphene conductive composite material;
(4)The preparation of waterborne conductive solution:By step(3)Obtained poly- 3,4- ethene dioxythiophenes-polystyrolsulfon acid-graphite
Alkene conducing composite material is added in water, ultrasonic disperse, obtains waterborne conductive solution, stand-by;
(5)The preparation of conductive polymer fiber:By step(4)Waterborne conductive solution and step(1)Oiliness film forming solution enter
Row mixing, and with being ultrasonically treated, so as to obtain mixing homogeneous water oil(W/O)Conducting solution, conductive mixed liquor is taken to pour into
In special mould, after placing 20-30h, spontaneously dry, take out conductive fiber and dry;
(6)The preparation of flexible fiber sensor electrode:By step(5)Obtained conductive polymer fiber is cut to segment;
(7)The preparation of nano silver wire:Glycerine is added in 500mL three-necked flasks, 5-6gPVP is added, is warming up to 55-65 DEG C simultaneously
Mechanical agitation is until PVP is completely dissolved;After system temperature is down to room temperature, 1-2g silver nitrates are added, stirring is to being completely dissolved;So
The glycerin solution 8-12mL containing 56-60mg sodium chloride and 0.3-0.7mL water is added afterwards, is persistently stirred and is added under agitation
Heat, heating is closed after temperature reaches setting value, is down to room temperature;The water of same volume is added, supernatant liquor is removed after standing overnight,
The sediment of solution bottom is disperseed again with isopropanol, then solution is repeated several times, is dispersed in centrifugal treating
Nano silver wire in aqueous isopropanol;
(8)The preparation of the flexible fiber sensor electrode of nano silver wire modification:The macromolecule after cutting is handled with oxygen plasma
Conductive fiber surfaces, then conductive polymer fiber is invaded in the aqueous isopropanol containing nano silver wire, is dried at room temperature for,
Obtain the flexible fiber sensor electrode of nano silver wire modification.
2. a kind of preparation method of the flexible fiber sensor electrode of nano silver wire modification as claimed in claim 1, its feature
It is, step(1)In, the mass fraction of SBS is 5- in the oiliness film forming solution
20%。
3. a kind of preparation method of the flexible fiber sensor electrode of nano silver wire modification as claimed in claim 1, its feature
It is, step(2)In, the humid medium is dimethylformamide, 1-METHYLPYRROLIDONE, aqueous surfactant solution, dry ice
One kind therein.
4. a kind of preparation method of the flexible fiber sensor electrode of nano silver wire modification as claimed in claim 1, its feature
It is, step(3)In, graphene is 1-2 with polystyrolsulfon acid, poly- 3,4-rthylene dioxythiophene, the mass ratio of iron chloride:1-
2:1-3:1-3。
5. a kind of preparation method of the flexible fiber sensor electrode of nano silver wire modification as claimed in claim 1, its feature
It is, step(4)In, time of ultrasonic disperse is 25-35min, poly- 3,4-rthylene dioxythiophene-polyphenyl in waterborne conductive solution
The mass fraction of vinyl sulfonic acid-graphene is 5-20%.
6. a kind of preparation method of the flexible fiber sensor electrode of nano silver wire modification as claimed in claim 1, its feature
It is, step(5)In, the weight ratio of waterborne conductive solution and oiliness film forming solution is 0.1-1:1;Sonication treatment time is 10-
20min;The mould is a long body steel plate, and steel plate center is machined with the groove of a fiber shape, the long 25-35cm of groove, diameter
2.5-3.5mm, drying temperature are 65-75 DEG C, drying time 1.5-2.5h.
7. a kind of preparation method of the flexible fiber sensor electrode of nano silver wire modification as claimed in claim 1, its feature
It is, step(6)In, the length of the conductive polymer fiber after cutting is 7-9mm.
8. a kind of preparation method of the flexible fiber sensor electrode of nano silver wire modification as claimed in claim 1, its feature
It is, step(7)In, the volume of glycerine is 180-200mL, and 200-220 DEG C of the temperature of heating, the volume of water is 180-
200mL, centrifugation rate 5000-7000rpm/min, centrifugation time 8-12min.
9. a kind of preparation method of the flexible fiber sensor electrode of nano silver wire modification as claimed in claim 1, its feature
It is, step(8)In, the time dried at room temperature is at least 5h.
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