CN107525832B - A kind of preparation method of the flexible fiber sensor electrode of silver nanowires modification - Google Patents
A kind of preparation method of the flexible fiber sensor electrode of silver nanowires modification Download PDFInfo
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Abstract
The present invention relates to sensor fields, disclose a kind of preparation method of the flexible fiber sensor electrode of silver nanowires 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-graphene is conductive material, and with silver nanowires modified electrode, obtain a kind of s-B-S/graphene/poly- 3 based on silver nanowires modification, 4- ethene dioxythiophene-polystyrolsulfon acid flexible fiber sensor electrode.Inventive sensor electrode can be applied to medical biological monitoring, the fields such as environment and the monitoring of hygiene.
Description
Technical field
The present invention relates to a kind of systems for the flexible fiber sensor electrode that sensor field more particularly to silver nanowires are modified
Preparation Method.
Background technique
Sensor is that mankind itself finds out the various sensory informations of nature, can be turned to unlike signal and perception information
Turn to can digitize, intelligentized important devices.During human civilization rapid development of information technology, sensor is played
Increasingly heavier effect is mankind's exploration outfield, while being 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.
Graphene is a new class of carbon two-dimensional nano light material, has unique monoatomic layer two dimensional crystal structure, greatly
Quantifier elimination the result shows that graphene has the highest intensity of known materials, excellent electric conductivity and lead by big specific surface area ratio
The excellent property such as hot, these excellent properties also determine it in such as composite material, and electronic device, solar energy etc. is many
Field has a wide range of applications.
Majority is combined to conductive material on platinum carbon electrode in the prior art, and composite material is relatively simple, electric conductivity
It is bad, existing defects, and do not have flexibility, it is impossible to be used in wearable device cannot preferably play the practical valence of sensor
Value.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of flexible fiber sensor electrodes of silver nanowires modification
Preparation method.The present invention is using Styrene-Butadiene-Styrene Block Copolymer as thin film flexible substrate, by poly- 3,4- ethylene
Dioxy thiophene-polystyrolsulfon acid and graphene carry out the compound conductive film for obtaining flexible and transparent, then silver nanowires is carried out
Modification opens up new diameter for its application in flexible sensor, has more excellent detection performance compared with traditional sensors.
The specific technical proposal of the invention is: a kind of preparation side of the flexible fiber sensor electrode of silver nanowires modification
Method includes the following steps:
(1) preparation of oiliness film forming solution: Styrene-Butadiene-Styrene Block Copolymer is taken to be added to chloroform
It in solution, is stood after stirring, is completely dissolved Styrene-Butadiene-Styrene Block Copolymer, obtain oiliness film forming solution,
For use.
S-B-S resin has the characteristic of plastics and rubber concurrently, can contact with water, weak acid, alkali etc.,
With excellent tensile strength, the advantages that big surface friction coefficient, low temperature performance well, excellent electrical properties, processing performance is good.
(2) ball-milling method prepares graphene: graphite powder being added in ball grinder and humid medium carries out ball milling, rotary-tray revolving speed
For 2800-3200rpm, Ball-milling Time 40-50h, can opening takes out graphene and undesired impurities in hydrochloric acid cleaning removing product is added,
It is being washed with deionized water, is being freeze-dried, obtains solid graphene.
Ball-milling method is a kind of mechanical stripping technology, environmentally protective, easy to operate, low cost.It avoids due to redox
Method uses reducing agents potential hazards caused by experiment operator and environment such as strong acid and hydrazine hydrate.
(3) poly- 3,4- ethene dioxythiophene-polystyrolsulfon acid-graphene conductive composite material preparation: solid is weighed
Graphene is added in polystyrolsulfon acid solution, ultrasonic disperse, 3,4-rthylene dioxythiophene monomer is then added, and stirring
Under the conditions of liquor ferri trichloridi is added dropwise, continue to be stirred to react 10-14h, be centrifugated resulting blackish green slurries, and respectively
It cleans repeatedly, collection solid colourless to cleaning solution repeatedly with dehydrated alcohol and distilled water, is dried in vacuo 10-14h at 70-80 DEG C,
Obtain poly- 3,4- ethene dioxythiophene-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, conductivity is high
The features such as high with transparency.For the insoluble infusibility for solving poly- 3,4-rthylene dioxythiophene, polystyrolsulfon acid is introduced into poly- 3,
4- ethene dioxythiophene, forms dispersibility and the good poly- 3,4- ethene dioxythiophene of processability-polystyrolsulfon acid suspends
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, its purpose is to make graphene functionalized,
By kayexalate load on graphene, and be poly- 3, the 4- ethylene dioxy of carrier situ polymerization using the graphene of functionalization
Thiophene makes it mutually combine closely.Poly- 3,4- ethene dioxythiophene-polystyrolsulfon acid-graphite is obtained by the method for polymerization
Alkene composite material is together with each other by the effect for then passing through chemical bond, substantially increases the migration rate of electronics, than inciting somebody to action
Poly- 3,4- ethene dioxythiophene-polystyrolsulfon acid solution and the simple physical mixed electric conductivity of graphene want it is superior very much.
By together with graphene and poly- 3,4- ethene dioxythiophene-polystyrolsulfon acid doping with obtain electric conductivity it is excellent plus
Material obtain the very superior flexible and transparent conductive of performance and using s-B-S as flexible plastic substrates
Film can be used as wearable biological sensor electrode, have very wide application prospect.
(4) preparation of waterborne conductive solution: poly- 3,4- ethene dioxythiophene-polystyrolsulfon acid-that step (3) is obtained
Graphene conductive composite material is added in water, ultrasonic disperse, obtains waterborne conductive solution, for use.
(5) preparation of conductive polymer fiber: the oiliness of the waterborne conductive solution of step (4) and step (1) is formed a film molten
Liquid is mixed, and with being ultrasonically treated, to obtain mixing oily (W/O) conducting solution of uniform water, takes conductive mixed liquor
It pours into special mold, after placing 20-30h, spontaneously dries, take out conductive fiber and dry.
(6) the conductive polymer fiber that step (5) obtains the preparation of flexible fiber sensor electrode: is cut to segment.
(7) preparation of silver nanowires: glycerine is added in 500mL three-necked flask, and 5-6gPVP is added, is warming up to 55-65
DEG C and mechanical stirring until PVP be completely dissolved；It is cooled to room temperature to system temperature, 1-2g silver nitrate is added, stirred to completely molten
Solution；Then the glycerin solution 8-12mL containing 56-60mg sodium chloride and 0.3-0.7mL water is added, persistently stirs under stiring
And heat, heating is closed after temperature reaches setting value, is down to room temperature；The water of same volume is added, goes to upper layer after standing overnight
Clear liquid again disperses the sediment of solution bottom with isopropanol, is then repeated several times solution in centrifugal treating, obtains
The silver nanowires being dispersed in aqueous isopropanol.
PVP is surfactant, and glycerine is solvent and reducing agent, and reproducibility is higher than ethylene glycol, silver nanoparticle obtained
Line yield is higher.It is carried out being centrifuged off impurity and unreacted PVP with isopropanol.
(8) preparation of the flexible fiber sensor electrode of silver nanowires modification: the height after being cut with oxygen plasma treatment
Then molecule conductive fiber surfaces invade conductive polymer fiber in the aqueous isopropanol containing silver nanowires, at room temperature
It is dry, obtain the flexible fiber sensor electrode of silver nanowires modification.
Since flexible fiber passes through corona treatment, silver nanowires is set to be adsorbed on fiber surface, because isopropanol is easy
Volatilization, silver nanowires is just adsorbed on fiber surface completely after volatilization in several hours.
Preferably, in step (1), Styrene-Butadiene-Styrene Block Copolymer in the oiliness film forming solution
Mass fraction is 5-20%.
Preferably, the humid medium is dimethylformamide, N-Methyl pyrrolidone, surfactant in step (2)
Aqueous solution, dry ice are one such.
Since dimethylformamide, N-Methyl pyrrolidone, aqueous surfactant solution etc. are organic solvent and medium, have
Certain toxicity, and extent of exfoliation is low, while ball-milling medium is decomposed as caused by high-energy, the ball milling solvent in mechanical milling process
Decomposition with medium not can avoid, and lead to fragmentation and defect, so that the defect and impurity introduced 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, in step (3), the matter of graphene and polystyrolsulfon acid, poly- 3,4-rthylene dioxythiophene, iron chloride
Amount is than being 1-2:1-2:1-3:1-3.
Preferably, the time of ultrasonic disperse is 25-35min, poly- 3,4- ethylene in waterborne conductive solution in step (4)
Dioxy thiophene-polystyrolsulfon acid-graphene mass fraction is 5-20%.
Preferably, the weight ratio of waterborne conductive solution and oiliness film forming solution is 0.1-1:1 in step (5)；At ultrasound
The reason time is 10-20min；The mold is a long body steel plate, and steel plate center is machined with the groove of a fiber shape, and groove is long
25-35cm, diameter 2.5-3.5mm, drying temperature are 65-75 DEG C, drying time 1.5-2.5h.
Preferably, the length of the conductive polymer fiber after cutting is 7-9mm in step (6).
Preferably, the volume of glycerine is 180-200mL, 200-220 DEG C of the temperature of heating, the body of water in step (7)
Product is 180-200mL, centrifugation rate 5000-7000rpm/min, centrifugation time 8-12min.
Preferably, the dry time is at least 5h at room temperature in step (8).
It is compared with the prior art, the beneficial effects of the present invention are:
1, the present invention has the characteristic of plastics and rubber, styrene-butadiene-concurrently with s-B-S resin
Styrene block copolymer can be contacted with water, weak acid, alkali etc., have excellent tensile strength, big surface friction coefficient, low temperature
The advantages that performance is good, excellent electrical properties, and processing performance is good.Make the conductive film of preparation that there is very flexibility and certain
Draftability.
2, 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- ethylene by carrier situ of the graphene of functionalization
Dioxy thiophene makes it mutually combine closely.Poly- 3,4- ethene dioxythiophene-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.
3, silver nanowires can be widely used in electrode material due to itself special one-dimentional structure and excellent conduction
Material, silver nanowires is as modification, additionally it is possible to which the defect for filling up graphene is that electric conductivity is more excellent.
Specific embodiment
The present invention will be further described with reference to the examples below.
Embodiment 1
(1) preparation of oiliness film forming solution
It takes the Styrene-Butadiene-Styrene Block Copolymer plastics of 1g to be added in the chloroform soln of 20mL, stirs
One day is stood after mixing, Styrene-Butadiene-Styrene Block Copolymer is completely dissolved in chloroform soln, makes
The oiliness film forming solution that mass fraction is 5%.
(2) ball-milling method prepares graphene
20g graphite powder and 400g dry ice are added in ball grinder, control rotary-tray revolving speed is 3000rpm, Ball-milling Time
For 48h, aterrimus graphene is obtained, can opening takes out graphene and impurity extra in hydrochloric acid cleaning removing product is added, spending
Ionized water cleans three times, and freeze-drying obtains solid graphene.
(3) poly- 3,4- ethene dioxythiophene-polystyrolsulfon acid-graphene conductive composite material preparation
The graphene of 20mg is taken to be added in the polystyrolsulfon acid solution of 20mL, then ultrasonic disperse 30min is added 3,
4- ethene dioxythiophene monomer 200uL, and 10mL, 14mmoL/L liquor ferri trichloridi are added dropwise in the case of stirring, after
It is continuous to be stirred to react 12h, prepared blackish green slurries are centrifugated, and cleaned repeatedly repeatedly with dehydrated alcohol and distilled water respectively
It is colourless to cleaning solution, it collects solid and is dried in vacuo 12h at 75 DEG C, obtain poly- 3,4-rthylene dioxythiophene-polystyrolsulfon acid-
Graphene conductive composite material.
(4) preparation of waterborne conductive solution
Poly- 3,4- ethene dioxythiophene-polystyrolsulfon acid-graphene conductive composite material of 1g is taken to be added to 20mL's
In aqueous solution, ultrasonic disperse 30min makes poly- 3,4-rthylene dioxythiophene-polystyrolsulfon acid-stone that mass fraction is 5%
Black alkene solution.
(5) preparation of conductive polymer fiber
It takes the oiliness film forming solution of 1mL aqueous solution and 10mL to be mixed, and is ultrasonically treated with ultrasonic processor
15min takes the conductive mixed liquor of 3mL to pour into fibrous type mold to obtain mixing oily (W/O) conducting solution of uniform water,
It after placing for 24 hours, spontaneously dries, taking-up conductive fiber, which is placed in 70 DEG C of constant temperature ovens, dries 2h.
(6) preparation of flexible sensor electrode
The conductive polymer fiber for taking step (5) to obtain, controlling its fibre length is 8mm.
(7) preparation of silver nanowires
The glycerine of 190mL is added in 500mL three-necked flask, 5.86gPVP is added, is warming up to 60 DEG C and mechanical stirring
Until PVP is dissolved completely in glycerine.It is cooled to room temperature to system temperature, 1.58g silver nitrate is added, stirred to completely molten
Solution.Then the glycerin solution 10mL containing 59mg sodium chloride and 0.5mL water is added, persistently stirred under low stirring rate and adds
Heat closes heating after temperature is raised to 210 DEG C, it is allowed to be slowly dropped to room temperature to 210 DEG C.It is added 190mL's with the ratio of 1:1
Water removes supernatant liquor after standing overnight, with isopropanol redisperse beaker bottom sediment, then by solution on centrifuge with
6000rpm/min high speed centrifugation 10min so repeats 3 times, has obtained being dispersed in the silver nanowires in aqueous isopropanol.
(8) preparation of the flexible fiber sensor electrode of silver nanowires modification
With oxygen plasma treatment fiber surface, then fiber is invaded in the aqueous isopropanol containing silver nanowires at least
5h, and be dried at room temperature for, obtain the flexible fiber sensor electrode of silver nanowires modification.
Embodiment 2
(1) preparation of oiliness film forming solution
It takes the Styrene-Butadiene-Styrene Block Copolymer plastics of 1g to be added in the chloroform soln of 20mL, stirs
One day is stood after mixing, Styrene-Butadiene-Styrene Block Copolymer is completely dissolved in chloroform soln, makes
The oiliness film forming solution that mass fraction is 5%.
(2) ball-milling method prepares graphene
20g graphite powder and 400g dry ice are added in ball grinder, control rotary-tray revolving speed is 3000rpm, Ball-milling Time
For 48h, aterrimus graphene is obtained, can opening takes out graphene and impurity extra in hydrochloric acid cleaning removing product is added, spending
Ionized water cleans three times, and freeze-drying obtains solid graphene.
(3) poly- 3,4- ethene dioxythiophene-polystyrolsulfon acid-graphene conductive composite material preparation
The graphene of 20mg is taken to be added in the polystyrolsulfon acid solution of 20mL, then ultrasonic disperse 30min is added 3,
4- ethene dioxythiophene monomer 200uL, and 10mL, 14mmoL/L liquor ferri trichloridi are added dropwise in the case of stirring, after
It is continuous to be stirred to react 12h, prepared blackish green slurries are centrifugated, and cleaned repeatedly repeatedly with dehydrated alcohol and distilled water respectively
It is colourless to cleaning solution, it collects solid and is dried in vacuo 12h at 75 DEG C, obtain poly- 3,4-rthylene dioxythiophene-polystyrolsulfon acid-
Graphene conductive composite material.
(4) preparation of waterborne conductive solution
Poly- 3,4- ethene dioxythiophene-polystyrolsulfon acid-graphene conductive composite material of 1g is taken to be added to 20mL's
In aqueous solution, ultrasonic disperse 30min makes poly- 3,4-rthylene dioxythiophene-polystyrolsulfon acid-stone that mass fraction is 5%
Black alkene solution.
(5) preparation of conductive polymer fiber
It takes the oiliness film forming solution of 5mL aqueous solution and 10mL to be mixed, and is ultrasonically treated with ultrasonic processor
15min takes the conductive mixed liquor of 3mL to pour into fibrous type mold to obtain mixing oily (W/O) conducting solution of uniform water,
It after placing for 24 hours, spontaneously dries, taking-up conductive fiber, which is placed in 70 DEG C of constant temperature ovens, dries 2h.
(6) preparation of flexible sensor electrode
The conductive polymer fiber for taking step (5) to obtain, controlling its fibre length is 8mm.
(7) preparation of silver nanowires
The glycerine of 190mL is added in 500mL three-necked flask, 5.86gPVP is added, is warming up to 60 DEG C and mechanical stirring
Until PVP is dissolved completely in glycerine.It is cooled to room temperature to system temperature, 1.58g silver nitrate is added, stirred to completely molten
Solution.Then the glycerin solution 10mL containing 59mg sodium chloride and 0.5mL water is added, persistently stirred under low stirring rate and adds
Heat closes heating after temperature is raised to 210 DEG C, it is allowed to be slowly dropped to room temperature to 210 DEG C.It is added 190mL's with the ratio of 1:1
Water removes supernatant liquor after standing overnight, with isopropanol redisperse beaker bottom sediment, then by solution on centrifuge with
6000rpm/min high speed centrifugation 10min so repeats 3 times, has obtained being dispersed in the silver nanowires in aqueous isopropanol.
(8) preparation of the flexible fiber sensor electrode of silver nanowires modification
With oxygen plasma treatment fiber surface, then fiber is invaded in the aqueous isopropanol containing silver nanowires at least
5h, and be dried at room temperature for, obtain the flexible fiber sensor electrode of silver nanowires modification.
Embodiment 3
(1) preparation of oiliness film forming solution
It takes the Styrene-Butadiene-Styrene Block Copolymer plastics of 1g to be added in the chloroform soln of 20mL, stirs
One day is stood after mixing, Styrene-Butadiene-Styrene Block Copolymer is completely dissolved in chloroform soln, makes
The oiliness film forming solution that mass fraction is 5%.
(2) ball-milling method prepares graphene
20g graphite powder and 400g dry ice are added in ball grinder, control rotary-tray revolving speed is 3000rpm, Ball-milling Time
For 48h, aterrimus graphene is obtained, can opening takes out graphene and impurity extra in hydrochloric acid cleaning removing product is added, spending
Ionized water cleans three times, and freeze-drying obtains solid graphene.
(3) poly- 3,4- ethene dioxythiophene-polystyrolsulfon acid-graphene conductive composite material preparation
The graphene of 20mg is taken to be added in the polystyrolsulfon acid solution of 20mL, then ultrasonic disperse 30min is added 3,
4- ethene dioxythiophene monomer 200uL, and 10mL, 14mmoL/L liquor ferri trichloridi are added dropwise in the case of stirring, after
It is continuous to be stirred to react 12h, prepared blackish green slurries are centrifugated, and cleaned repeatedly repeatedly with dehydrated alcohol and distilled water respectively
It is colourless to cleaning solution, it collects solid and is dried in vacuo 12h at 75 DEG C, obtain poly- 3,4-rthylene dioxythiophene-polystyrolsulfon acid-
Graphene conductive composite material.
(4) preparation of waterborne conductive solution
Poly- 3,4- ethene dioxythiophene-polystyrolsulfon acid-graphene conductive composite material of 1g is taken to be added to 20mL's
In aqueous solution, ultrasonic disperse 30min makes poly- 3,4-rthylene dioxythiophene-polystyrolsulfon acid-stone that mass fraction is 5%
Black alkene solution.
(5) preparation of conductive polymer fiber
It takes the oiliness film forming solution of 10mL aqueous solution and 10mL to be mixed, and is ultrasonically treated with ultrasonic processor
15min takes the conductive mixed liquor of 3mL to pour into fibrous type mold to obtain mixing oily (W/O) conducting solution of uniform water,
It after placing for 24 hours, spontaneously dries, taking-up conductive fiber, which is placed in 70 DEG C of constant temperature ovens, dries 2h.
(6) preparation of flexible sensor electrode
The conductive polymer fiber for taking step (5) to obtain, controlling its fibre length is 8mm.
(7) preparation of silver nanowires
The glycerine of 190mL is added in 500mL three-necked flask, 5.86gPVP is added, is warming up to 60 DEG C and mechanical stirring
Until PVP is dissolved completely in glycerine.It is cooled to room temperature to system temperature, 1.58g silver nitrate is added, stirred to completely molten
Solution.Then the glycerin solution 10mL containing 59mg sodium chloride and 0.5mL water is added, persistently stirred under low stirring rate and adds
Heat closes heating after temperature is raised to 210 DEG C, it is allowed to be slowly dropped to room temperature to 210 DEG C.It is added 190mL's with the ratio of 1:1
Water removes supernatant liquor after standing overnight, with isopropanol redisperse beaker bottom sediment, then by solution on centrifuge with
6000rpm/min high speed centrifugation 10min so repeats 3 times, has obtained being dispersed in the silver nanowires in aqueous isopropanol.
(8) preparation of the flexible fiber sensor electrode of silver nanowires modification
With oxygen plasma treatment fiber surface, then fiber is invaded in the aqueous isopropanol containing silver nanowires at least
5h, and be dried at room temperature for, obtain the flexible fiber sensor electrode of silver nanowires modification.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field；In the present invention
Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention
Technical spirit any simple modification, change and equivalent transformation to the above embodiments, still fall within the technology of the present invention side
The protection scope of case.
Claims (9)
1. a kind of preparation method of the flexible fiber sensor electrode of silver nanowires modification, it is characterised in that include the following steps:
(1) preparation of oiliness film forming solution: Styrene-Butadiene-Styrene Block Copolymer is taken to be added to chloroform soln
In, it is stood after stirring, is completely dissolved Styrene-Butadiene-Styrene Block Copolymer, obtain oiliness film forming solution, for use；
(2) ball-milling method prepares graphene: graphite powder being added in ball grinder and humid medium carries out ball milling, rotary-tray revolving speed is
2800-3200rpm, Ball-milling Time 40-50h, can opening take out graphene and undesired impurities in hydrochloric acid cleaning removing product are added, then
It is washed with deionized water, is freeze-dried, obtains solid graphene；
(3) poly- 3,4-rthylene dioxythiophene-polystyrolsulfon acid-graphene conductive composite material preparation: solid graphite is weighed
Alkene is added in polystyrolsulfon acid solution, ultrasonic disperse, 3,4-rthylene dioxythiophene monomer is then added, and in stirring condition
Under liquor ferri trichloridi is added dropwise, continue to be stirred to react 10-14h, be centrifugated resulting blackish green slurries, 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-rthylene dioxythiophene-polystyrolsulfon acid-graphene conductive composite material；
(4) preparation of waterborne conductive solution: poly- 3,4-rthylene dioxythiophene-polystyrolsulfon acid-graphite that step (3) is obtained
Alkene conducing composite material is added in water, ultrasonic disperse, obtains waterborne conductive solution, for use；
(5) preparation of conductive polymer fiber: by the waterborne conductive solution of step (4) and the oiliness film forming solution of step (1) into
Row mixing, and with being ultrasonically treated, to obtain mixing uniform water oil W/O conducting solution, conductive mixed liquor is taken to pour into spy
It in the mold of system, after placing 20-30h, spontaneously dries, takes out conductive fiber and dry；
(6) the conductive polymer fiber that step (5) obtains the preparation of flexible fiber sensor electrode: is cut to segment；
(7) preparation of silver nanowires: glycerine is added in 500mL three-necked flask, and 5-6gPVP is added, is warming up to 55-65 DEG C simultaneously
Mechanical stirring is until PVP is completely dissolved；It is cooled to room temperature to system temperature, 1-2g silver nitrate is 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, persistently stirs and heats, work as temperature
Heating is closed after reaching setting value, is down to room temperature；The water with glycerine same volume is added, removes supernatant liquor after standing overnight,
The sediment of solution bottom is dispersed again with isopropanol, solution is repeated several times in centrifugal treating then, is dispersed in
Silver nanowires in aqueous isopropanol；
(8) preparation of the flexible fiber sensor electrode of silver nanowires modification: the macromolecule after being cut with oxygen plasma treatment
Then conductive polymer fiber is invaded in the aqueous isopropanol containing silver nanowires, is dried at room temperature for by conductive fiber surfaces,
Obtain the flexible fiber sensor electrode of silver nanowires modification.
2. a kind of preparation method of the flexible fiber sensor electrode of silver nanowires modification as described in claim 1, feature
It is, in step (1), the mass fraction of Styrene-Butadiene-Styrene Block Copolymer is 5- in the oiliness film forming solution
20%.
3. a kind of preparation method of the flexible fiber sensor electrode of silver nanowires modification as described in claim 1, feature
It is, in step (2), the humid medium is dimethylformamide, N-Methyl pyrrolidone, aqueous surfactant solution, dry ice
It is one such.
4. a kind of preparation method of the flexible fiber sensor electrode of silver nanowires modification as described in claim 1, feature
It is, in step (3), the mass ratio of graphene and polystyrolsulfon acid, poly- 3,4-rthylene dioxythiophene, iron chloride is 1-2: 1-
2∶1-3∶1-3。
5. a kind of preparation method of the flexible fiber sensor electrode of silver nanowires modification as described in claim 1, feature
It is, in step (4), the time of ultrasonic disperse is 25-35min, poly- 3,4-rthylene dioxythiophene-polyphenyl in waterborne conductive solution
Vinyl sulfonic acid-graphene mass fraction is 5-20%.
6. a kind of preparation method of the flexible fiber sensor electrode of silver nanowires modification as described in claim 1, feature
It is, in step (5), the weight ratio of waterborne conductive solution and oiliness film forming solution is 0.1-1: 1；Sonication treatment time is 10-
20min；The mold 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 silver nanowires modification as described in claim 1, feature
It is, in step (6), 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 silver nanowires modification as described in claim 1, feature
It is, in step (7), 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 silver nanowires modification as described in claim 1, feature
It is, in step (8), the dry time is at least 5h at room temperature.
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| CN109281160B (en) * | 2018-08-30 | 2020-09-29 | 浙江理工大学 | Preparation method of silver nanowire modified temperature-sensitive variable resistance fiber with sterilization effect |
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