CN108611695A - A kind of preparation method of the flexible photoreceptor conductive fiber of azo-based benzene/graphene oxide/nano silver wire - Google Patents

A kind of preparation method of the flexible photoreceptor conductive fiber of azo-based benzene/graphene oxide/nano silver wire Download PDF

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CN108611695A
CN108611695A CN201810236387.9A CN201810236387A CN108611695A CN 108611695 A CN108611695 A CN 108611695A CN 201810236387 A CN201810236387 A CN 201810236387A CN 108611695 A CN108611695 A CN 108611695A
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graphene oxide
solution
nano silver
silver wire
preparation
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万军民
丁文凤
胡智文
王秉
彭志勤
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Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/02Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/09Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/18Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances

Abstract

Disclosed by the invention is a kind of preparation method of the flexible photoreceptor conductive fiber of azo-based benzene/graphene oxide/nano silver wire, and preparation process includes:Graphene oxide is modified with azobenzene first, obtain photosensitive material, photosensitive material is blended with nano silver wire again, obtain the internal component of coaxial spinning, then using sodium carboxymethylcellulose as the cladding material of coaxial spinning, the flexible photoreceptor conductive fiber of azobenzene/graphene oxide/nano silver wire is finally obtained using coaxial wet spinning technology, filamentary conductive prepared by the present invention can be good, mechanical property is excellent, also there is photosensitive property simultaneously, in photoelectric device, flexible wearable equipment, sensor, there is huge application value in the fields such as photosensitive material.

Description

A kind of flexible photoreceptor conductive fiber of azo-based benzene/graphene oxide/nano silver wire Preparation method
Technical field
The present invention relates to a kind of preparation methods of flexible photoreceptor conductive fiber, more specifically say, are related to a kind of based on even The preparation method of the flexible photoreceptor conductive fiber of pyridine/graphene oxide/nano silver wire.
Background technology
Sensor is the important devices that mankind itself finds out the various sensory informations of nature, can to unlike signal and Perception information, which is converted into, to be digitized, intelligent, and during human civilization rapid development of information technology, sensor plays Increasingly heavier effect is increasingly becoming the mankind and understands one of the important means of real world, observation peripheral information, and sensor is It is a kind of to act on (response) with certain particular matters in environment, measured information is experienced, and these information are pressed one Set pattern rule is changed into the output of the signals such as electricity, light and realizes a kind of device detected.Flexible wearable sensor is directed generally to feel It should be suffered from motional induction, personal health monitoring, intelligent robot and man-machine mutual friendship etc. with monitoring human body various activities It is widely applied.
21 century is the new stage developed from photoelectronics to photonic propulsion, in order to meet future society to high-speed transfer, place The requirement of reason and operation large capacity information is carried out the technologies such as acquisition, the storage of data using photon and has become current photoelectron device The development trend of part, associated Information Photonics material become one of key technology therein.Azobenzene polymer is due to it Excellent Photo alignment, nonlinear optical properties and the distinctive easy preparation of polymer, workability energy, in optics device Part field, has a wide range of applications, and-N=N- the groups in azobenzene are to ultraviolet-sensitive, in ultraviolet light and blue light illumination Lower configuration meeting cis-trans isomerism, it is trans- to have very big difference, usually, the cis-structure of azobenzene molecule with cis- absorption spectrum Thermal stability it is excessively poor be a kind of metastable structure, so usually at room temperature azobenzene molecule be all to be stablized with transconfiguration Existing, when azobenzene molecule is exposed under the light or heating condition of certain wavelength, cis-trans isomerization occurs for molecular structure, leads The great variety of molecular shape and dipole moment is caused, azobenzene photo-isomerisable chemoattractant molecule is in different wavelengths of light irradiation or fuel factor Under conditions of can its two kinds of conformation (cisoid conformation and anti conformation) reversibly mutually conversion, the phase of this cis and trans Mutually conversion is not due to what any chemical bond rupture was formed, but caused by electronics and nuclear structure are reset, The key core of azobenzene molecule and its derivative as photoresponse functional composite material can equally be such that graphene has excellent Optical Response.
Inorganic nano material refers to the material that size is in 1-100nm, relative to other nano materials, inorganic nano material With preparing simple, the advantages such as of low cost, uniform particle diameter, photocatalysis, solar cell, biology, medicine, weaving, printing and dyeing, There are extensive research and application in the fields such as wearable electronic.In the inorganic nano material of numerous types, nano silver accounts for According to important position, the nano silver wire of one-dimentional structure has high-specific surface area, heat conduction, conduction, light transmission, ductility, machinery strong The performances such as degree and flexibility, have in fields such as flexible conductive film, solar cell, touch screen, display screen, sensors and potentially answer With value.
Mostly in the prior art is that azobenzene is applied to membrane technology as one of coating, forms biosensor, But being almost absent for fiber is made, therefore, develops a kind of preparation of flexible photoreceptor conductive fiber simple for process, easily operated Method is particularly significant, and the present invention uses coaxial wet spinning, using azobenzene/graphene oxide/nano silver wire as the core of fiber, carboxylic Sodium carboxymethylcellulose pyce is the shell of fiber, and novelty is had more compared with traditional photosensitive material.
Invention content
In order to solve above-mentioned prior art problem, the present invention provides with environmentally protective, method is simple, electric conductivity and thoroughly The preparation of the flexible photoreceptor conductive fiber of kind azo-based benzene/graphene oxide/nano silver wire of the excellent equal technical characterstics of photosensitiveness Method.
To achieve the goals above, the present invention is achieved by the following technical solutions:
A kind of preparation method of the flexible photoreceptor conductive fiber of azo-based benzene/graphene oxide/nano silver wire, including such as Lower preparation process:
Step 1):The preparation of graphene oxide water solution:By graphene oxide powder ultrasonic disperse in water, it is prepared 1mg/mL graphene oxide water solutions;
Step 2):AzoC4OBr is added in the mixed solution of trimethylamine ethanol solution and acetonitrile solution, is warming up to 60- 80 DEG C, reaction 8-12h postcoolings to room temperature remove ethyl alcohol using rotary distillation method and acetonitrile obtain crude product, crude product is used Ethyl alcohol recrystallization twice, is placed under room temperature in vacuo dry 8-12h, and it is water-soluble to be distributed to acquisition cationic azo benzene in deionized water Liquid;
Step 3):1-4g polyvinylpyrrolidones are added in the ethylene glycol of 30-70mL, ultrasonic disperse 20-40min with It makes it completely dissolved, is transferred in three-necked flask, the ethylene glycol of 30-70mL is added, be vigorously stirred under the conditions of being placed in 150-170 DEG C anti- Answer 1h, then the 10-50mL ethylene glycol for being dissolved in 0.2-0.8g silver nitrates be slowly added dropwise, the reaction was continued 1h after being added dropwise to complete, it is cooling simultaneously Centrifuge washing is carried out with deionized water and ethyl alcohol respectively, is placed in water dispersion, obtains nano silver wire solution;
Step 4):The cationic azo benzene aquatic solution that 0.6nM steps 2) obtain is taken to be slowly dropped into the acquisition of 80mL steps 1) In graphene oxide water solution, it is placed in continuous ultrasound 1-2h at room temperature, is filtered, filtering, and it is extra that removing is washed with deionized Cationic azobenzene, obtain azobenzene/graphene oxide, the dispersion of pyridine/graphene oxide obtained into azobenzene/oxidation stone Black alkene solution;
Step 5):The nano silver wire solution that step 3) obtains is added to azobenzene/graphene oxide of step 4) acquisition In solution, stirring 20-30min, ultrasound 1-2h obtain internal layer spinning solution;
Step 6):The sodium carboxymethylcellulose of a concentration of 10mg/mL is dissolved in the water, 1-2h is stirred, outer layer is obtained and spins Silk liquid;
Step 7):The spinning solution that step 5) and step 6) obtain is transferred in the internal layer and outer layer of syringe respectively, profit Spinning is carried out with device for spinning, the spinning solution is placed in and dries at room temperature through 30-60min coagulating baths, obtains azobenzene/oxidation Graphene/nano silver wire fiber.
As an improvement graphene oxide is prepared using modified Hummers methods in step 1), using crystalline flake graphite as raw material It is pre-oxidized, graphite powder drying at room temperature will be pre-oxidized, carried out oxidation reaction and obtain graphene oxide, graphene oxide is carried out cold It is lyophilized dry, grinds to obtain graphene oxide powder.
As an improvement 60 DEG C of reaction temperature in step 2), reaction time 10h, vacuum drying time 10h.
As an improvement the 25mL ethylene glycol times that dropwise addition is dissolved in 0.5g silver nitrates in step 3) are 10-15min, institute State deionized water centrifuge washing 3 times, the ethyl alcohol centrifuge washing 2 times.
As an improvement step 4) middle-jiao yang, function of the spleen and stomach ion azobenzene by the carboxylic group of electrostatic interaction and graphene oxide into Row combines.
Graphene oxide is stirred while as an improvement azobenzene is added dropwise in step 4), the suction filtration filter Film is miillpore filter, and the miillpore filter aperture is 200um.
As an improvement internal layer spinning speed described in step 7) is 100um/min, outer layer spinning speed is 150um/ Min, the coagulating bath are made of ethyl alcohol, water and calcium chloride, and the ethyl alcohol and water volume ratio are 5:1, the quality of the calcium chloride Score is 5%.
It is compared with the prior art beneficial effects of the present invention:
1) present invention is combined using azobenzene as photosensitive material by electrostatic self-assembled and graphene oxide, when change light Wavelength when azobenzene structure change, formed photosensitive material;
2) nano silver wire (AgNWs) is because it is with excellent electric conductivity, thermal conductivity and good biocompatibility, antibacterial The features such as property, catalytic, it is widely used in the fields such as transparent electrode, medicinal antibiosis, Industrial Catalysis, the present invention is with nano silver wire As intermediate conductive layer, increase the electric conductivity of fiber;
3) sodium carboxymethylcellulose is the flexibility and mechanical performance that fibrous outer increases fiber, while being played to photosensitive material Protective effect, sodium carboxymethylcellulose good biocompatibility, can be used for pharmaceutical carrier, using sodium carboxymethylcellulose as protective layer It can also be by this fiber applications in biological fields such as human nerves.
Specific implementation mode
Below by way of specific embodiment, the present invention is further illustrated, but embodiments of the present invention not by The limitation of following embodiment.
Embodiment 1
A kind of preparation method of the flexible photoreceptor conductive fiber of azo-based benzene/graphene oxide/nano silver wire, including such as Lower preparation process:
Step 1):The preparation of graphene oxide water solution:By graphene oxide powder ultrasonic disperse in water, it is prepared 1mg/mL graphene oxide water solutions, graphene oxide powder are specifically prepared by graphene oxide using modified Hummers methods, with Crystalline flake graphite is that raw material is pre-oxidized, and will pre-oxidize graphite powder drying at room temperature, carries out oxidation reaction and obtains graphene oxide, by oxygen Graphite alkene is freeze-dried, and graphene oxide powder is ground to obtain;
Step 2):AzoC4OBr is added in the mixed solution of trimethylamine ethanol solution and acetonitrile solution, is warming up to 60 DEG C, reaction 8h postcoolings to room temperature remove ethyl alcohol using rotary distillation method and acetonitrile solvent obtain crude product, by crude product second Alcohol recrystallizes twice, is placed under room temperature in vacuo dry 8h, is distributed to acquisition cationic azo benzene aquatic solution in deionized water;
Step 3):1g polyvinylpyrrolidones are added in the ethylene glycol of 30mL, ultrasonic disperse 20min is so that it is complete Dissolving, is transferred in three-necked flask, the ethylene glycol of 30mL is added, and reaction 1h is vigorously stirred under the conditions of being placed in 150 DEG C, then be slowly added dropwise Be dissolved in the 10mL ethylene glycol of 0.2g silver nitrates, the reaction was continued 1h after being added dropwise to complete, it is cooling and use respectively deionized water and ethyl alcohol into Row centrifuge washing is placed in water dispersion, obtains nano silver wire solution, the deionized water centrifuge washing 3 times, the ethyl alcohol centrifugation Washing 2 times;
Step 4):The cationic azo benzene aquatic solution that 0.6nM steps 2) obtain is taken to be slowly dropped into the acquisition of 80mL steps 1) In graphene oxide water solution, it is placed in continuous ultrasound 1h at room temperature, is filtered, filtering, and it is extra that removing is washed with deionized Cationic azobenzene obtains azobenzene/graphene oxide, and pyridine/graphene oxide dispersion is obtained azobenzene/graphite oxide Alkene solution, the cationic azo benzene are combined by the carboxylic group of electrostatic interaction and graphene oxide, and azobenzene is added dropwise While graphene oxide is stirred, suction filtration filter membrane be miillpore filter, the miillpore filter aperture be 200um;
Step 5):The nano silver wire solution that step 3) obtains is added to azobenzene/graphene oxide of step 4) acquisition In solution, stirring 20min, ultrasound 1h obtain internal layer spinning solution;
Step 6):The sodium carboxymethylcellulose of a concentration of 10mg/mL is dissolved in the water, 1h is stirred, obtains outer layer spinning Liquid;
Step 7):The spinning solution that step 5) and step 6) obtain is transferred in the internal layer and outer layer of syringe respectively, profit Spinning is carried out with device for spinning, the internal layer spinning speed is 100um/min, and the outer layer spinning speed is 150um/min, is spun Silk liquid through 30min coagulating baths, be placed in and dry at room temperature, obtain azobenzene/graphene oxide/nano silver wire fiber, coagulating bath by Ethyl alcohol, water and calcium chloride composition, ethyl alcohol and water volume ratio are 5:1, the mass fraction of calcium chloride is 5%.
Embodiment 2
A kind of preparation method of the flexible photoreceptor conductive fiber of azo-based benzene/graphene oxide/nano silver wire, including such as Lower preparation process:
Step 1):The preparation of graphene oxide water solution:By graphene oxide powder ultrasonic disperse in water, it is prepared 1mg/mL graphene oxide water solutions, graphene oxide powder are specifically prepared by graphene oxide using modified Hummers methods, with Crystalline flake graphite is that raw material is pre-oxidized, and will pre-oxidize graphite powder drying at room temperature, carries out oxidation reaction and obtains graphene oxide, by oxygen Graphite alkene is freeze-dried, and graphene oxide powder is ground to obtain;
Step 2):AzoC4OBr is added in the mixed solution of trimethylamine ethanol solution and acetonitrile solution, is warming up to 70 DEG C, reaction 10h postcoolings to room temperature remove ethyl alcohol using rotary distillation method and acetonitrile solvent obtain crude product, crude product is used Ethyl alcohol recrystallization twice, is placed under room temperature in vacuo dry 10h, is distributed to acquisition cationic azo benzene aquatic solution in deionized water;
Step 3):2.5g polyvinylpyrrolidones are added in the ethylene glycol of 50mL, ultrasonic disperse 30min is so that its is complete Fully dissolved is transferred in three-necked flask, and the ethylene glycol of 50mL is added, and reaction 1h, then slowly drop are vigorously stirred under the conditions of being placed in 160 DEG C Solubilization is in the 30mL ethylene glycol of 0.5g silver nitrates, and the reaction was continued 1h after being added dropwise to complete is cooling simultaneously to use deionized water and ethyl alcohol respectively Carry out centrifuge washing, be placed in water dispersion, acquisition nano silver wire solution, the deionized water centrifuge washing 3 times, the ethyl alcohol from The heart washs 2 times;
Step 4):The cationic azo benzene aquatic solution that 0.6nM steps 2) obtain is taken to be slowly dropped into the acquisition of 80mL steps 1) In graphene oxide water solution, it is placed in continuous ultrasound 1.5h at room temperature, is filtered, filtering, and it is extra that removing is washed with deionized Cationic azobenzene, obtain azobenzene/graphene oxide, the dispersion of pyridine/graphene oxide obtained into azobenzene/oxidation stone Black alkene solution, the cationic azo benzene are combined by the carboxylic group of electrostatic interaction and graphene oxide, filter filter membrane For miillpore filter, the miillpore filter aperture is 200um;
Step 5):The nano silver wire solution that step 3) obtains is added to azobenzene/graphene oxide of step 4) acquisition In solution, stirring 25min, ultrasound 1.5h obtain internal layer spinning solution;
Step 6):The sodium carboxymethylcellulose of a concentration of 10mg/mL is dissolved in the water, 1.5h is stirred, outer layer is obtained and spins Silk liquid;
Step 7):The spinning solution that step 5) and step 6) obtain is transferred in the internal layer and outer layer of syringe respectively, profit Spinning is carried out with device for spinning, the internal layer spinning speed is 100um/min, and the outer layer spinning speed is 150um/min, is spun Silk liquid through 45min coagulating baths, be placed in and dry at room temperature, obtain azobenzene/graphene oxide/nano silver wire fiber, coagulating bath by Ethyl alcohol, water and calcium chloride composition, ethyl alcohol and water volume ratio are 5:1, the mass fraction of calcium chloride is 5%.
Embodiment 3
A kind of preparation method of the flexible photoreceptor conductive fiber of azo-based benzene/graphene oxide/nano silver wire, including such as Lower preparation process:
Step 1):The preparation of graphene oxide water solution:By graphene oxide powder ultrasonic disperse in water, it is prepared 1mg/mL graphene oxide water solutions, graphene oxide powder are specifically prepared by graphene oxide using modified Hummers methods, with Crystalline flake graphite is that raw material is pre-oxidized, and will pre-oxidize graphite powder drying at room temperature, carries out oxidation reaction and obtains graphene oxide, by oxygen Graphite alkene is freeze-dried, and graphene oxide powder is ground to obtain;
Step 2):AzoC4OBr is added in the mixed solution of trimethylamine ethanol solution and acetonitrile solution, is warming up to 80 DEG C, reaction 12h postcoolings to room temperature remove ethyl alcohol using rotary distillation method and acetonitrile solvent obtain crude product, crude product is used Ethyl alcohol recrystallization twice, is placed under room temperature in vacuo dry 12h, is distributed to acquisition cationic azo benzene aquatic solution in deionized water;
Step 3):4g polyvinylpyrrolidones are added in the ethylene glycol of 70mL, ultrasonic disperse 40min is so that it is complete Dissolving, is transferred in three-necked flask, the ethylene glycol of 70mL is added, and reaction 1h is vigorously stirred under the conditions of being placed in 170 DEG C, then be slowly added dropwise Be dissolved in the 50mL ethylene glycol of 0.8g silver nitrates, the reaction was continued 1h after being added dropwise to complete, it is cooling and use respectively deionized water and ethyl alcohol into Row centrifuge washing is placed in water dispersion, obtains nano silver wire solution, the deionized water centrifuge washing 3 times, the ethyl alcohol centrifugation Washing 2 times;
Step 4):The cationic azo benzene aquatic solution that 0.6nM steps 2) obtain is taken to be slowly dropped into the acquisition of 80mL steps 1) In graphene oxide water solution, it is placed in continuous ultrasound 2h at room temperature, is filtered, filtering, and it is extra that removing is washed with deionized Cationic azobenzene obtains azobenzene/graphene oxide, and pyridine/graphene oxide dispersion is obtained azobenzene/graphite oxide Alkene solution, the cationic azo benzene are combined by the carboxylic group of electrostatic interaction and graphene oxide, are filtered filter membrane and are Miillpore filter, the miillpore filter aperture are 200um;
Step 5):The nano silver wire solution that step 3) obtains is added to azobenzene/graphene oxide of step 4) acquisition In solution, stirring 30min, ultrasound 2h obtain internal layer spinning solution;
Step 6):The sodium carboxymethylcellulose of a concentration of 10mg/mL is dissolved in the water, 2h is stirred, obtains outer layer spinning Liquid;
Step 7):The spinning solution that step 5) and step 6) obtain is transferred in the internal layer and outer layer of syringe respectively, profit Spinning is carried out with device for spinning, the internal layer spinning speed is 100um/min, and the outer layer spinning speed is 150um/min, is spun Silk liquid through 60min coagulating baths, be placed in and dry at room temperature, obtain azobenzene/graphene oxide/nano silver wire fiber, coagulating bath by Ethyl alcohol, water and calcium chloride composition, ethyl alcohol and water volume ratio are 5:1, the mass fraction of calcium chloride is 5%.
Finally it should be noted that present invention is not limited to the above embodiments, there can also be many variations.This field it is general All deformations that logical technical staff directly can export or associate from present disclosure are considered as the present invention's Protection domain.

Claims (7)

1. a kind of preparation method of the flexible photoreceptor conductive fiber of azo-based benzene/graphene oxide/nano silver wire, feature exist In including following preparation process:
Step 1):The preparation of graphene oxide water solution:By graphene oxide powder ultrasonic disperse in water, 1mg/ is prepared ML graphene oxide water solutions;
Step 2):AzoC4OBr is added in the mixed solution of trimethylamine ethanol solution and acetonitrile solution, is warming up to 60-80 DEG C, reaction 8-12h postcoolings to room temperature remove ethyl alcohol using rotary distillation method and acetonitrile obtain crude product, by crude product second Alcohol recrystallizes twice, is placed under room temperature in vacuo dry 8-12h, is distributed to acquisition cationic azo benzene aquatic solution in deionized water;
Step 3):1-4g polyvinylpyrrolidones are added in the ethylene glycol of 30-70mL, ultrasonic disperse 20-40min so that its It is completely dissolved, is transferred in three-necked flask, the ethylene glycol of 30-70mL is added, reaction is vigorously stirred under the conditions of being placed in 150-170 DEG C 1h, then the 10-50mL ethylene glycol for being dissolved in 0.2-0.8g silver nitrates is slowly added dropwise, the reaction was continued after being added dropwise to complete 1h, it is cooling simultaneously point Centrifuge washing is not carried out with deionized water and ethyl alcohol, is placed in water dispersion, obtains nano silver wire solution;
Step 4):The cationic azo benzene aquatic solution that 0.6nM steps 2) obtain is taken to be slowly dropped into the oxidation of 80mL steps 1) acquisition In graphene aqueous solution, it is placed in continuous ultrasound 1-2h at room temperature, is filtered, filtering, and be washed with deionized and remove extra sun Ionic azobenzene obtains azobenzene/graphene oxide, and pyridine/graphene oxide dispersion is obtained azobenzene/graphene oxide Solution;
Step 5):The nano silver wire solution that step 3) obtains is added to azobenzene/graphene oxide solution of step 4) acquisition In, stirring 20-30min, ultrasound 1-2h obtain internal layer spinning solution;
Step 6):Sodium carboxymethylcellulose is dissolved in the water, the sodium carboxymethylcellulose for preparing a concentration of 10mg/mL is molten Liquid stirs 1-2h, obtains outer layer spinning solution;
Step 7):The spinning solution that step 5) and step 6) obtain is transferred in the internal layer and outer layer of syringe respectively, utilizes spinning Silk device carries out spinning, and the spinning solution is placed in and dries at room temperature through 30-60min coagulating baths, obtains azobenzene/graphite oxide Alkene/nano silver wire fiber.
2. a kind of flexible photoreceptor conductive fiber of azo-based benzene/graphene oxide/nano silver wire according to claim 1 Preparation method, which is characterized in that graphene oxide powder is prepared using modified Hummers methods in step 1), with crystalline flake graphite It is pre-oxidized for raw material, graphite powder drying at room temperature will be pre-oxidized, carried out oxidation reaction and obtain graphene oxide, by graphene oxide It is freeze-dried, grinds to obtain graphene oxide powder.
3. a kind of flexible photoreceptor conductive fiber of azo-based benzene/graphene oxide/nano silver wire according to claim 1 Preparation method, which is characterized in that 60 DEG C of reaction temperature in step 2), reaction time 10h, vacuum drying time 10h.
4. a kind of flexible photoreceptor conductive fiber of azo-based benzene/graphene oxide/nano silver wire according to claim 1 Preparation method, which is characterized in that be added dropwise that be dissolved in the 25mL ethylene glycol times of 0.5g silver nitrates be 10-15min, institute in step 3) State deionized water centrifuge washing 3 times, the ethyl alcohol centrifuge washing 2 times.
5. a kind of flexible photoreceptor conductive fiber of azo-based benzene/graphene oxide/nano silver wire according to claim 1 Preparation method, which is characterized in that the carboxylic group that step 4) middle-jiao yang, function of the spleen and stomach ion azobenzene passes through electrostatic interaction and graphene oxide It is combined.
6. a kind of flexible photoreceptor conductive fiber of azo-based benzene/graphene oxide/nano silver wire according to claim 1 Preparation method, which is characterized in that graphene oxide is stirred while azobenzene is added dropwise in step 4), suctions filtration is filtered Film is miillpore filter, and the miillpore filter aperture is 200um.
7. a kind of flexible photoreceptor conductive fiber of azo-based benzene/graphene oxide/nano silver wire according to claim 1 Preparation method, which is characterized in that internal layer spinning speed described in step 7) is 100um/min, and outer layer spinning speed is 150um/min, the coagulating bath are made of ethyl alcohol, water and calcium chloride, and the ethyl alcohol and water volume ratio are 5:1, the calcium chloride Mass fraction be 5%.
CN201810236387.9A 2018-03-21 2018-03-21 A kind of preparation method of the flexible photoreceptor conductive fiber of azo-based benzene/graphene oxide/nano silver wire Pending CN108611695A (en)

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Application publication date: 20181002