CN106782747A - Silver nanoparticle fiber membrane and preparation method thereof and equipment and electronic device - Google Patents
Silver nanoparticle fiber membrane and preparation method thereof and equipment and electronic device Download PDFInfo
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- CN106782747A CN106782747A CN201710013591.XA CN201710013591A CN106782747A CN 106782747 A CN106782747 A CN 106782747A CN 201710013591 A CN201710013591 A CN 201710013591A CN 106782747 A CN106782747 A CN 106782747A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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Abstract
The present invention proposes silver nanoparticle fiber membrane and preparation method thereof and equipment and electronic device.The method of the preparation silver nanoparticle fiber membrane includes：By silver-colored precursor solution add injection-tube in, and using topping-up pump by the silver-colored precursor solution from be connected with liquid injection pipe syringe needle release, obtain fiber；The fiber is stretched using air-flow, obtains silver nanoparticle fiber；The silver nanoparticle fiber is collected on the collector, silver nanoparticle fiber membrane precursor is obtained；The silver nanoparticle fiber membrane precursor is post-processed, silver nanoparticle fiber membrane is obtained.Method proposed by the invention, is obtained in that the silver nanoparticle fiber membrane that transparency is good, performance is excellent, and the method without the complicated post-processing step of highly energy-consuming, and time-saving energy-saving is simple efficient, and low production cost, the potential with industrialized production.
Description
Technical field
The present invention relates to flexible electronics field, specifically, the present invention relates to silver nanoparticle fiber membrane and its preparation side
Method and equipment and electronic device.More particularly to preparing the method for silver nanoparticle fiber membrane, silver nanoparticle fiber membrane, system
The equipment and electronic device of standby silver nanoparticle fiber membrane.
Background technology
Recently as the widely available of flexible electronic product, associated specifications are increasingly improved, especially a new generation
Flexible electronic product proposes more harsh requirement to its light transmittance, electric conductivity, flexibility and environmental stability.And silver nanoparticle material
Especially nano silver wire is expected, with unique optics, electromagnetism, mechanics, catalytic performance, in various fields such as flexible and transparent electricity
The aspects such as pole, micro-nano circuit, opto-electronic device, flexible energy storage, flexible solar battery have particularly important effect, because
And silver nanoparticle fiber electrode will turn into the favourable replacer of present tin indium oxide conductive electrode.
The nano-silver thread of excellent performance simply how is prepared at low cost, as being widely used in touching in photoelectric field
Touch the key issue of the aspects such as panel, solar cell.
The content of the invention
It is contemplated that at least solving one of technical problem in correlation technique to a certain extent.
The present invention is to be based on the following discovery of inventor and complete：
Inventor has found in research process：Because silver is that electric good conductor, good conductivity, thus micro-nano silver wire are used as electricity
Pole material can be with reducing energy consumption (relative to oxide film electrode).The particle diameter of micro-nano silver wire is less than visible ray incidence wave simultaneously
When long, the plasma effect enhancing light transmission of metal micro-nano structure makes electrode have good photoelectric properties, is conducive to carrying
The efficiency of battery device high.However, high surface resistance and low surface adhesion force limit the large-area applications of nano-silver thread, it is existing
Stage can be using high annealing, high intensity pulses are laser sintered or the complicated aftertreatment technology such as surface encapsulation is solved
Above mentioned problem, but these techniques take, consume energy very much.The present inventor is by further investigation discovery, the side of gas spinning
Method make use of high pressure draught, can prepare fibre diameter in nano level silver fiber simple and efficient, safety and environmental protection.And it is logical
Cross using suitable collector, the silver nanoparticle fiber of uniform net distribution can be obtained, then by that after high temperature sintering, can obtain
The transparent reticulated film of silver nanoparticle fiber composition, can be used for the photoelectricity key area such as touch panel, solar cell, and the method
Simple and effective, yield are big, low consumption when and low power consuming, the potential with industrialized production.
In view of this, it is attached it is an object of the present invention to propose a kind of high grade of transparency, low sheet resistance, good substrate
Put forth effort, mechanical environment good stability, production environment be safer, time saving or preparation method of silver nanoparticle fiber membrane of energy-conservation.
In the first aspect of the present invention, the present invention proposes a kind of method for preparing silver nanoparticle fiber membrane.
Embodiments in accordance with the present invention, during silver-colored precursor solution added into injection-tube, and using topping-up pump by the forerunner
Liquid solution is released from the syringe needle being connected with liquid injection pipe, obtains fiber；The fiber is stretched using air-flow, obtains silver nanoparticle
Fiber；The silver nanoparticle fiber is collected on the collector, silver nanoparticle fiber membrane precursor is obtained；The silver nanoparticle fiber is thin
Film precursor is post-processed, and obtains silver nanoparticle fiber membrane.
Inventor is it was unexpectedly observed that the preparation method of the silver nanoparticle fiber membrane using the embodiment of the present invention, is obtained in that
The silver nanoparticle that transparency is good, low sheet resistance, good substrate adhesive force, mechanical environment good stability, performance are excellent is fine
Dimension film, and the method, without the complicated post-processing step of highly energy-consuming, time-saving energy-saving is simple efficient, and low production cost
Potential honest and clean, with industrialized production.
In addition, method according to the above embodiment of the present invention, can also have following additional technical characteristic：
Embodiments in accordance with the present invention, the silver-colored precursor solution contains inorganic salts, macromolecule and the solvent of silver.
Embodiments in accordance with the present invention, the inorganic salts of the silver are silver nitrate.
Embodiments in accordance with the present invention, the macromolecule is PVP.
Embodiments in accordance with the present invention, the solvent is acetonitrile.
Embodiments in accordance with the present invention, the gas for forming the air-flow is selected from compressed air, nitrogen, argon gas, helium
At least one.
Embodiments in accordance with the present invention, the pressure for forming the gas of the air-flow is 0.001MPa to 20MPa.
Embodiments in accordance with the present invention, the collector is nickel screen, sheet glass or glass fiber sheets.
Embodiments in accordance with the present invention, the post processing is selected from sintering processes, magnetron sputtering treatment, electroplating processes, ultraviolet
Treatment with irradiation or vapour deposition are processed.
In the second aspect of the present invention, the present invention proposes a kind of silver nanoparticle fiber membrane.
Embodiments in accordance with the present invention, the silver nanoparticle fiber membrane is prepared by the above method.
Inventor it was unexpectedly observed that using the silver nanoparticle fiber membrane of the embodiment of the present invention, with the high grade of transparency, low surface
The advantage of resistance, good substrate adhesive force and mechanical environment stability, these excellent performances make silver nanoparticle fiber thin
Film has application prospect in the key photoelectric field such as touch panel, solar cell.It will be appreciated to those of skill in the art that
Above for silver nanoparticle fiber membrane preparation method described by feature and advantage, be still applied to the silver nanoparticle fiber membrane,
Will not be repeated here.
In the third aspect of the present invention, the present invention proposes a kind of equipment for preparing silver nanoparticle fiber membrane.
Embodiments in accordance with the present invention, the equipment includes：Injection-tube, for accommodating silver-colored precursor solution；Syringe needle, it is described
Syringe needle is connected with the injection-tube, for projecting the silver-colored precursor solution；Topping-up pump, the post liquid pump and the injection-tube phase
Even, for the silver-colored precursor solution to be released；Feeder, for being stretched to obtain silver to the fiber using air-flow
Nanofiber；Collector, for collecting the silver nanoparticle fiber.
Inventor it was unexpectedly observed that the equipment of the preparation silver nanoparticle fiber membrane using the embodiment of the present invention, can quickly,
Foregoing silver nanoparticle fiber membrane is efficiently prepared, and without time consumption and energy consumption, complicated aftertreatment technology, is made
Environment is safer, and there is the silver nanoparticle fiber membrane for obtaining the high grade of transparency, low sheet resistance, good substrate to adhere to
Power, good mechanical environment stability.
In addition, equipment according to the above embodiment of the present invention, can also have following additional technical characteristic：
Embodiments in accordance with the present invention, the syringe needle is L-shaped.
Embodiments in accordance with the present invention, the collector is nickel screen, sheet glass or glass fiber sheets.
In the fourth aspect of the present invention, the present invention proposes a kind of electronic device.
Embodiments in accordance with the present invention, the electronic equipment contains above-mentioned silver nanoparticle fiber membrane.
Inventor is it was unexpectedly observed that transparency is high, sheet resistance is low, substrate is attached because above-mentioned silver nanoparticle fiber membrane has
Put forth effort, mechanical environment good stability the advantages of so that the electronic device can meet light transmittance requirement higher and with interior
Consumption low, compact conformation and the bent advantage of part.It will be appreciated to those of skill in the art that above for silver nanoparticle fiber
Feature and advantage described by the preparation method and silver nanoparticle fiber membrane of film, are still applied to the electronic device, herein no longer
Repeat.
Brief description of the drawings
Of the invention above-mentioned and/or additional aspect and advantage will become from description of the accompanying drawings below to embodiment is combined
Substantially and be readily appreciated that, wherein：
Fig. 1 is the schematic flow sheet of the preparation silver nanoparticle fiber membrane method of one embodiment of the invention；
Fig. 2 is the structural representation of the equipment of the preparation silver nanoparticle fiber membrane of one embodiment of the invention；
Fig. 3 is the photo of the silver nanoparticle fiber membrane of one embodiment of the invention；
Fig. 4 is the SEM photograph of the silver nanoparticle fiber membrane of one embodiment of the invention；
Fig. 5 is the SEM photograph after the silver nanoparticle fiber membrane doubling of one embodiment of the invention；
Fig. 6 is the photo of the transparency detection process of the silver nanoparticle fiber membrane of one embodiment of the invention；
Fig. 7 is the graph of a relation of the silver nanoparticle fiber membrane in the corresponding light transmittance of different sheet resistances of one embodiment of the invention；
Fig. 8 is the graph of a relation of the sheet resistance value with number of bends of the silver nanoparticle fiber membrane of one embodiment of the invention；
Fig. 9 is the graph of a relation of the sheet resistance value with stretch ratio of the silver nanoparticle fiber membrane of one embodiment of the invention；
Figure 10 is the graph of a relation of the sheet resistance value with bending radius of the silver nanoparticle fiber membrane of one embodiment of the invention；
Figure 11 is the demonstration photo of folding and the recovery of the silver nanoparticle fiber membrane of one embodiment of the invention；
Figure 12 is the elastic presentation process photo of the silver nanoparticle fiber membrane of one embodiment of the invention；
Figure 13 is the relation comparison diagram of the sheet resistance with light transmittance of the different materials of one embodiment of the invention.
Reference
100 injection-tubes
200 syringe needles
300 topping-up pumps
400 feeders
500 collectors
Specific embodiment
Embodiments of the invention are described below in detail.The embodiments described below is exemplary, is only used for explaining this hair
It is bright, and be not considered as limiting the invention.
In one aspect of the invention, the present invention proposes a kind of method for preparing silver nanoparticle fiber membrane.According to this hair
Bright embodiment, reference picture 1, the method is comprised the following steps：
S100：By silver-colored precursor solution add injection-tube in, and using topping-up pump by precursor solution from injection-tube phase
Syringe needle even is released, and obtains fiber.
In this step, the silver-colored precursor solution with spinnability is made first.Embodiments in accordance with the present invention, the silver
The specific composition of precursor solution is not particularly limited, and those skilled in the art can be selected according to actual conditions.It is specific and
Speech, the suitable silver precursor solution of configuration are, it is necessary to select suitable solvent to dissolve the inorganic salts of silver, suitable macromolecule adjustment silver
Precursor solution viscosity, stability are reduced in subsequent step to silver ion, and it is met its of spinning requirement
His additive.Therefore, some embodiments of the invention, silver-colored precursor solution contains inorganic salts, macromolecule and the solvent of silver.
Precursor solution containing mentioned component can effectively meet spinning requirement, beneficial to the Yin Na that excellent performance is obtained in subsequent step
Rice fiber membrane.
Embodiments in accordance with the present invention, the specific species of the silver-colored inorganic salts that can be used is not particularly limited, as long as through
The silver-colored presoma of ag material can be formed after overstretching and sintering, those skilled in the art can flexibly select as needed,
Silver nitrate is for example included but is not limited to, thus, the step such as stretched, sintering can effectively obtain silver nanoparticle fiber, and source
It is easy to get extensively.
Embodiments in accordance with the present invention, in order that silver-colored presoma (also referred to as silver-colored inorganic salts) is reduced in subsequent step
Into ag material, and make silver inorganic salts it is particle-stabilisedly dispersed in the solution, it usually needs to silver-colored precursor solution
Middle addition macromolecule.In an embodiment of the present invention, the high molecular specific species that can be used is not particularly limited, ability
Field technique personnel can flexibly select as needed.In some specific examples of the invention, the macromolecule that can be used includes
But it is not limited to PVP (polyvinylpyrrolidone).PVP both can be as the reducing agent of the inorganic salts of silver, again can be by its structure
In the highly polar lactam group that contains be coordinated with silver ion, the stabilising system of nano level metal colloidal sol is formed, so as to hinder
Only silver ion is reunited, and further improves the stability and spinnability of silver-colored precursor solution.
Embodiments in accordance with the present invention, the silver-colored precursor solution of gas spinning is suitable to, it is necessary to select suitable molten to obtain
The inorganic salts and additive (including macromolecule) of agent dissolving silver.In an embodiment of the present invention, the solvent that can be used it is specific
Species is not particularly limited, as long as the inorganic salts of silver and the solvent of additive can fully be dissolved.More of the invention
In specific example, the solvent that can be used includes but is not limited to acetonitrile.The present inventor is by long-term research discovery, second
Nitrile is the good solvent of silver-colored presoma and additive, various solutes can be made to be dissolved completely in silver-colored precursor solution, also with certain
Volatility, gas spinning and sintering during can effectively be removed.
Embodiments in accordance with the present invention, in the silver-colored precursor solution, the inorganic salts of silver, additive and solvent specifically contain
Amount is not particularly limited, as long as meeting spinning requirement and can obtain the silver nanoparticle fiber membrane for meeting use requirement, this area skill
Art personnel can neatly select.In some embodiments of the invention, based on every 1g solvents, contain in silver-colored precursor solution
The silver-colored inorganic salts and the additive of 0.01~0.5g of 0.1~1g.Under preferable case, based on every 1g solvents, silver-colored precursor solution
In the silver-colored inorganic salts containing 0.5g and 0.1g additive.In this way, the content of the inorganic salts of silver, additive and solvent is above-mentioned
In the range of, the silver-colored precursor solution of acquisition has suitable spinnability, is more easy to obtain fibre diameter in the presence of high pressure draught
In nanoscale and performance more preferably silver nanoparticle fiber.
Always according to embodiments of the invention, the concrete mode and charging sequence for preparing the silver-colored precursor solution are not limited especially
System, those skilled in the art can neatly be carried out.In some embodiments of the invention, by stirring, ultrasound or can add
Be well mixed for silver-colored presoma, reducing agent and stabilizer by the processing modes such as heat, will not be repeated here.
Embodiments in accordance with the present invention, are encased in the silver-colored precursor solution in injection-tube, the note that can be connected with injection-tube
Liquid pump is evenly released from the syringe needle being connected with injection-tube, forms fiber.Thus, can simply, quickly and easily obtain fiber.
In an embodiment of the present invention, the particular type of injection-tube and syringe needle is not particularly limited, as long as can be by solution from specific
The duct of bore is released, and those skilled in the art can be selected according to physical condition.Embodiments in accordance with the present invention,
The particular type of topping-up pump is not also particularly limited, as long as any fluid injection that the solution in injection-tube can be equably released
Pump, will not be repeated here.
Embodiments in accordance with the present invention, the speed for releasing silver-colored precursor solution also has no particular limits, as long as can be with
Air velocity, viscosity of precursor solution etc. match, and those skilled in the art can flexibly select as needed.In the present invention
Some embodiments in, the speed for releasing silver-colored precursor solution can be 0.05mL/h-0.5mL/h, thus, be conducive to acquired
The excellent silver nanoparticle fiber of energy.
S200：The fiber is stretched using air-flow, obtains silver nanoparticle fiber.
In this step, the air-flow of certain speed is coordinated on the direction that silver-colored precursor solution is pushed out, fiber quilt can be made
Rapidly it is drawn into silver nanoparticle fiber of the fibre diameter in Nano grade.Thus, it is possible to simple and effective ground obtains silver nanoparticle fiber,
Relative to methods such as existing electrostatic spinnings, the method has quick, safety, the advantage without high pressure, with realization of industrialization
Potentiality.
Embodiments in accordance with the present invention, the gas ground particular type of the formation air-flow that can be used is not particularly limited, only
Advantageously form uniform, continuous silver nanoparticle fiber, and the silver nanoparticle fiber that obtains will not be had a negative impact it is any
Gas, those skilled in the art can be selected according to the actual needs.In some specific examples of the invention, including
But it is not limited at least one in compressed air, nitrogen, argon gas, helium.Thus, gas source is abundant and with low cost.
Embodiments in accordance with the present invention, are evenly distributed and continuous silver nanoparticle fiber, people in the art to obtain diameter
Member can according to the actual requirements select suitable air velocity.In some embodiments of the invention, gas is represented with the pressure of air-flow
Flow velocity degree, then the pressure for forming the gas of air-flow can be 0.001MPa to 20MPa.In other words, when supplying air-flow to fiber, adjust
The pressure for saving air outlet valve is 0.001MPa to 20MPa.In this way, the pressure of air-flow is within the above range, before the speed and silver of air-flow
Speed, viscosity etc. that liquid solution releases is driven to be engaged, the fiber formed after being pushed out silver-colored precursor solution easily by it is uniform,
Silver nanoparticle fiber is continuously drawn into, is conducive to obtaining diameter is more evenly distributed, performance after subsequent treatment more preferably silver-colored
Nanofiber.
S300：Silver nanoparticle fiber is collected on the collector, silver nanoparticle fiber membrane precursor is obtained.
In this step, the silver nanoparticle fiber formed after being stretched by high pressure draught forms silver and receives collected by collector
The precursor of rice fiber membrane, can be used to post-process.Embodiments in accordance with the present invention, the material type of collector is not limited specifically
Determine, including but not limited to sheet glass, nickel screen and glass fiber sheets, as long as disclosure satisfy that post-processing step use requirement, this
Art personnel can be selected according to actual needs.Thus, using the collector of above-mentioned material, received in post-processing step
Collection substrate can keep shape invariance, so as to be further ensured that the planarization and the uniformity of the silver nanoparticle fiber membrane of acquisition.
Some embodiments of the invention, the collector can be nickel screen.Under preferable case, the nickel screen is with roundlet
The structure of shape hollow out, in this way, high pressure draught may pass through the nickel screen of hollow out, and silver nanoparticle fiber can be intercepted and uniform by nickel screen
Be arranged in the surface of nickel screen, and again by after follow-up sintering processes, unordered silver nanoparticle single can be transformed into transparent
Silver nanoparticle fiber membrane.
Embodiments in accordance with the present invention, the direction that nickel screen can be arranged to be projected from liquid injection pipe with fiber is perpendicular, nanometer
Fiber moves to nickel screen in the presence of air-flow, effectively can be attached on nickel screen, and acquisition silver can be collected by mobile nickel screen
The equally distributed silver nanoparticle fiber membrane of nanofiber.
S400：Silver nanoparticle fiber membrane precursor is post-processed, silver nanoparticle fiber membrane is obtained.
In this step, the collector that will collect has silver nanoparticle fiber membrane precursor is post-processed, in the mistake of post processing
Silver nanoparticle fiber membrane precursor can be made to be changed into the silver nanoparticle fiber membrane with conducting function in journey.Those skilled in the art
It is understood that the specific method of post processing is not particularly limited, as long as enabling to the fiber surface shape that spinning is obtained
Into Argent grain.For example include but is not limited to sintering processes, magnetron sputtering treatment, electroplating processes, ultraviolet irradiation process or
Vapour deposition treatment etc..
Some embodiments of the invention, sintering processes can will collect the collection for having silver nanoparticle fiber membrane precursor
Device, is transferred in Muffle furnace and is sintered, the silver in silver-colored presoma (inorganic salts of silver) in sintering process in silver nanoparticle fiber
Ion is fully changed into silver, you can obtain silver nanoparticle fiber membrane.
Embodiments in accordance with the present invention, the temperature and time of sintering processes is not particularly limited, before different silver
Body and additive are driven, those skilled in the art can be selected according to actual conditions, as long as silver nanoparticle fiber can be obtained effectively
Film.In some embodiments of the invention, for the precursor solution containing silver nitrate, the temperature of sintering processes can be with
It it is 200~300 degrees Celsius, soaking time is 1~3 hour.Thus, using above-mentioned sintering temperature and soaking time, can obtain
Obtain good transparency, low sheet resistance, good substrate adhesive force, the silver nanoparticle fiber membrane of mechanical environment good stability.According to
Some specific examples of the invention, preferred sintering processes condition so, it is possible to obtain power to be incubated 2 hours under 250 degrees Celsius
Learn performance and substrate adhesive force is more excellent and silver nanoparticle fiber membrane of highly transparent.
Some embodiments of the invention, magnetron sputtering treatment, electroplating processes, vapour deposition treatment can be according to ability
Domain routine operation is carried out, and in above-mentioned processing procedure, silver nanoparticle fiber membrane precursor surface forms Argent grain, is derived from target silver
Nano-fiber film.
Some embodiments of the invention, ultraviolet irradiation treatment can be collected using ultraviolet light silver nanoparticle fiber
The collector of film precursor, in irradiation process, silver ion is reduced into silver, obtains target silver nanoparticle fiber membrane.
In sum, embodiments in accordance with the present invention, the present invention proposes a kind of method for preparing silver nanoparticle fiber membrane,
The silver nanoparticle fiber membrane that transparency is good, performance is excellent is obtained in that using the method, and the method is without highly energy-consuming
Complicated post-processing step, time-saving energy-saving, it is simple efficiently, and low production cost, the potential with industrialized production.
In another aspect of the present invention, the present invention proposes a kind of silver nanoparticle fiber membrane.
Embodiments in accordance with the present invention, the silver nanoparticle fiber membrane is prepared by the above method.
Inventor find, silver nanoparticle fiber membrane according to embodiments of the present invention, with the high grade of transparency, low sheet resistance,
Good substrate adhesive force and the advantage of mechanical environment good stability, these excellent performances make silver nanoparticle fiber membrane exist
The key photoelectric field such as touch panel, solar cell has application prospect.It will be appreciated to those of skill in the art that above
For silver nanoparticle fiber membrane preparation method described by feature and advantage, be still applied to the silver nanoparticle fiber membrane, herein
Repeat no more.
In another aspect of the present invention, the present invention proposes a kind of equipment for preparing silver nanoparticle fiber membrane.Reference picture
2, equipment of the invention is described in detail.
Embodiments in accordance with the present invention, the equipment includes：Injection-tube 100, syringe needle 200, topping-up pump 300, feeder 400
With collector 500.Wherein, injection-tube 100 is used to accommodate silver-colored precursor solution；Syringe needle 200 and injection-tube 100 be connected to it is logical,
And for projecting the silver-colored precursor solution；What topping-up pump 300 and injection-tube 100 were connected to, and for by silver-colored precursor solution
Release；Feeder 400, for being stretched to obtain silver nanoparticle fiber to fiber using air-flow；Collector 500, for receiving
Collect the silver nanoparticle fiber.
Specifically, topping-up pump 300 can equably be released the silver-colored precursor solution in injection-tube 100, fiber is formed, while
Feeder 400 applies air-flow along the direction of fibre length, and high velocity air further stretches the fiber, and is rapidly formed
In nano level fiber, in drawing process, solvent can be removed fibre diameter by volatilizing；The silver nanoparticle of stretched formation
Fiber forms the precursor of silver nanoparticle fiber membrane collected by the collector 500 apart from syringe needle certain distance, by further burning
Knot treatment, you can obtain transparent silver nanoparticle fiber membrane.
Embodiments in accordance with the present invention, the particular type of injection-tube 100 is not particularly limited, as long as can by solution from
Container or design that the duct of specified caliber is released, those skilled in the art can be selected according to physical condition, example
It such as can be any of injection-tube for meeting use requirement.In embodiments of the invention, the particular type of topping-up pump 300
It is not particularly limited, as long as any topping-up pump that can equably release the solution in injection-tube, no longer goes to live in the household of one's in-laws on getting married herein
State.
Embodiments in accordance with the present invention, the concrete shape of syringe needle 200 is not also particularly limited, if it is any can silver before
The syringe needle that fiber is formed after liquid solution is released is driven, those skilled in the art can be selected according to physical condition.At this
In some embodiments of invention, the syringe needle 200 can be with L-shaped.In this way, to the right pushing direction of the topping-up pump 300 to injection-tube 100
Even if be set to the direction of supply backward of feeder 400 it is orthogonal, release fiber direction and gas circuit direction remain to
Be consistent, and gas outlet and the syringe needle 200 of feeder 400 the cleaning for being provided separately the equipment of also allowing for.Always according to this
Inventive embodiment, the specific internal diameter size of syringe needle 200 is not particularly limited, can be according to the silver nanoparticle fiber for going for
Specific size selected.In some embodiments of the invention, the internal diameter of the syringe needle 200 is 60 microns.
Embodiments in accordance with the present invention, the concrete shape of collector is not particularly limited, and those skilled in the art can be with root
Selected according to the shape of the silver nanoparticle fiber for expecting obtaining.In some embodiments of the invention, the collector 400 can be
Nickel screen, sheet glass or glass fiber sheets.Under preferable case, collector is nickel screen, and the nickel screen can be with small circular hollow out
Structure, the mesh size of nickel screen is 20~300 mesh.In this way, high pressure draught may pass through the nickel screen of above-mentioned hollow out, and silver nanoparticle is fine
Dimension can be intercepted by nickel screen and equably be arranged in the surface of nickel screen again, and again by after follow-up sintering processes, it is unordered
Silver nanoparticle single can be transformed into transparent silver nanoparticle fiber membrane.
In sum, using the equipment of the embodiment of the present invention, foregoing preparation silver nanoparticle fiber membrane can be implemented
Method, fast and efficiently prepare substantial amounts of silver nanoparticle fiber membrane, and without time consumption and energy consumption, complicated post processing
Technique.
In another aspect of the present invention, the present invention proposes a kind of electronic device.
Embodiments in accordance with the present invention, the electronic equipment contains above-mentioned silver nanoparticle fiber membrane.Those skilled in the art
It is understood that being not limited only to silver nanoparticle fiber membrane, the electronic device can also include other necessary parts, such as electricity
Pond, shell, chip, memory or input and output circuit etc., are no longer excessively repeated herein.
Some embodiments of the invention, the specific species of the electronic device is not particularly limited.For example, including but not
It is limited to touch-screen, flexible liquid crystal display, bimolecular sensors, optical information storage part, solar cell, electromagnetic shielding
Device etc..
In sum, embodiments in accordance with the present invention, the present invention proposes a kind of electronic device, because above-mentioned silver nanoparticle is fine
Dimension film has the advantages that transparency is high, sheet resistance is low, substrate adhesive force is good, mechanical environment good stability so that the electronics
Device can meet light transmittance requirement higher and have the advantages that low in-fighting, compact conformation and part is bent.This area skill
Art personnel are, it is understood that spy described by preparation method and silver nanoparticle fiber membrane above for silver nanoparticle fiber membrane
Seek peace advantage, be still applied to the electronic device, will not be repeated here.
Embodiments of the invention are described below in detail, unreceipted particular technique or condition in embodiment, according to this area
Technology or condition described by interior document are carried out according to product description.Agents useful for same or the unreceipted production firm of instrument
Person, is the conventional products that can be bought by city.
Embodiment 1：The preparation of silver nanoparticle fiber membrane and sign
Specific preparation method includes three key steps：Prepare silver-colored precursor solution, gas spinning and sintering processes.
First, 2g acetonitriles are taken, under conditions of the stirring of constant temperature magneton rotation condition, (marque is to add 0.2g PVP
K90), it is completely dissolved after after 30 minutes, adds 1g AgNO3, 5 hours when solution stands after stirring 4 hours, obtain silver-colored forerunner
Liquid solution.
Then, a certain amount of silver-colored precursor solution is sucked with disposable injection suction pipe, and loads onto the point that internal diameter is 60 microns
The syringe needle of glue, and by syringe needle with clip bend 90 degree after, then will injection suction pipe be mounted in syringe pump on.By the gas of feeder
Switch is opened, and regulate air velocity and syringe pump goes out liquid speed degree, then the nickel screen with small circular hollow out is placed on into syringe needle
Go out liquid direction, and collection nickel screen with liquid discharging pinhead apart from 50cm or so.Start gas spinning and prepare silver nanoparticle fiber, be used in combination
Nickel screen is collected, acquisition time about 10 minutes, the netted silver nanoparticle fiber membrane being evenly distributed.
Then, the nickel screen with mesh nano fiber membrane for preparing is placed in Muffle furnace and is sintered, programming rate
Be set in 5 degree mins, be warmed up to 250 degree, and after being incubated 2 hours, then it is natural lower the temperature with stove, that is, silver nanoparticle fibrous transparent net is obtained
Shape film.
The photo of the silver nanoparticle fiber membrane for preparing of the embodiment, as shown in Figure 3.From figure 3, it can be seen that the silver is received
The transparency of rice fiber membrane is very high, and the size of the silver nanoparticle fiber membrane of the method preparation can reach 10cm, explanation
The method is suitable to quickly and efficiently prepare transparent silver nanoparticle fiber membrane.
The SEM photograph of the silver nanoparticle fiber membrane that the embodiment is prepared is as shown in Figure 4.As can be seen from Figure 4, silver nanoparticle
The diameter of fiber is in below 200nm, and silver nanoparticle fiber membrane is microcosmic upper in unordered network structure, and is received through oversintering silver
Crosspoint between rice fiber is in the form of physical connection.
After the silver nanoparticle fiber membrane that the embodiment is prepared carries out doubling, then see under a scanning electron microscope
Examine, the SEM photograph of silver nanoparticle fiber membrane fold position can be obtained, as shown in Figure 5.Fig. 5 explanation silver nanoparticle fiber membranes have can
The performance of bending, even if bending will not also be broken.
Embodiment 2
In this embodiment, the sheet resistance and light transmittance of the silver nanoparticle fiber membrane that detection embodiment 1 is prepared.Sheet resistance is surveyed
Method for testing is as shown in Figure 6.
Silver nanoparticle tunica fibrosa is attached on common A4 paper or on pet substrate, is transferred it on four probe stations,
Machine is opened, four probes are gently ridden on sample, by measurement button, that is, obtain the sheet resistance value of sample.According to this method each
Sample is surveyed 5 times altogether, is averaged.
The testing result of the embodiment, as shown in Figure 7.As can be seen from Figure 7, silver nanoparticle fiber membrane has outstanding visible
Light transmission rate and low sheet resistance.
Embodiment 3
In this embodiment, the silver nanoparticle fiber membrane for being prepared to embodiment 1, carries out flexible test, while using
The platinum metal film of hot evaporation is used as control.Specifically, detection number of bends, stretch ratio and bending radius are to silver nanoparticle fiber
The influence that film is produced.
When influence of the number of bends to the sheet resistance of silver nanoparticle fiber membrane is carried out, silver nanoparticle fiber membrane is attached first
On flexible PET film, bending radius is constant for 2mm carries out crooked test.When different number of times are bent, its phase is detected
The square resistance answered.
When extension test is carried out, silver nanoparticle fiber membrane is attached on PDMS flexible extensible substrates first, then
The certain ratio of cross directional stretch, and be 5%, 10%, 15% in extensibility, its corresponding square resistance is recorded when 20% respectively,
And calculate corresponding sheet resistance increased percentage.
When bending radius test is carried out, processing mode and test number of bends are essentially the same.Difference is, bending radius
Respectively 1mm, 2mm, 5mm, 7mm, 9mm and 10mm, record its corresponding square resistance and sheet resistance increased percentage.
The number of bends test result of the silver nanoparticle fiber membrane of the embodiment, as shown in Figure 8.As can be seen from Figure 8, when curved
When bent number of times reaches 1000 times, the sheet resistance of silver nanoparticle fiber membrane (This work) does not increase substantially.And metal film (Metal
Films after bending 300 times, its sheet resistance increases 2500% to sheet resistance).
The stretch ratio test result of the silver nanoparticle fiber membrane of the embodiment, as shown in Figure 9.It can be seen in fig. 9 that silver is received
Rice fiber membrane (This work) though amount of tension reach 20%, its sheet resistance does not increase sign substantially, and metal film
(Metal films) is being stretched to 10% or so its sheet resistance growth rate more than 14000%.
The bending radius test result of the silver nanoparticle fiber membrane of the embodiment, as shown in Figure 10.As can be seen from Figure 10, silver
Between bending radius 0.5mm to the 10mm of nano-fiber film (This work), its sheet resistance does not have substantially change, and metal
The sheet resistance sharp increase after bending of film (Metal films), when bending radius gradually increases, its sheet resistance increases reduction
Trend.
Embodiment 4
In this embodiment, the silver nanoparticle fiber membrane for embodiment 1 being prepared, original is reverted to after arbitrarily folding again
Shape, silver nanoparticle fiber membrane remains unchanged with good electric conductivity.
The foldable the performance test results of the silver nanoparticle fiber membrane of the embodiment, as shown in figure 11.As can be seen from Figure 11,
Silver nanoparticle tunica fibrosa is attached on the miscellaneous paper smooth in a small pieces, paper is rubbed crush up afterwards, then opened and sprawl, silver nanoparticle
Tunica fibrosa still keeps complete and successful as wire connection LED and shinny.
Embodiment 5
In this embodiment, the substrate for collecting two-dimensional fiber film is prepared into the three-dimensional collector of the shapes such as circular cone, is entered
Row fiber collects the three-dimensional structure that can obtain presoma weave in composition.Carrying out post processing afterwards can obtain three-dimensional silver
Nanofiber.Demonstration is compressed to three-dimensional silver nanoparticle fiber, it is specific as shown in figure 12.
As can be seen from Figure 12, there is the silver nanoparticle fiber of the embodiment good pressure to recover function, produce under compression
Elastic deformation, and after pressure is withdrawn, silver nanoparticle fiber still reverts to original appearance.
Embodiment 6
In this embodiment, translucency and sheet resistance test are carried out to silver nanoparticle fiber membrane prepared by embodiment 1.Detection is adopted
Use the sheet resistance of multi-functional four-point probe, detection silver nanoparticle fiber membrane and other conventional conductive materials.Specifically, other are normal
Nano silver wire (AgNW), copper nano-wire (CuNW), Graphene (Graphene), tin indium oxide (ITO), copper are selected with conductive material
Nano wire mixes nanowires of gold (CuMW+AuNW), silver nanoparticle groove (Ag nanotrough), copper nanometer groove (Cu
Nanotrough), CNT (CNT) and conducting polymer (PEDOT：PSS).
The inspection result of the embodiment, as shown in figure 13.As can be seen from Figure 13, when with identical sheet resistance value, relatively
In other conventional conductive materials, silver nanoparticle fiber membrane (This work), with more preferable transparency.
Summarize
Integrated embodiment 1~6 can draw, the preparation method of silver nanoparticle fiber membrane proposed by the invention, be obtained in that
The silver nanoparticle fiber membrane of the high grade of transparency, low sheet resistance, good substrate adhesive force and mechanical environment stability, and the party
Method without highly energy-consuming complicated post-processing step, time-saving energy-saving, it is simple efficiently, and low production cost, with industrial metaplasia
The potential of product.
In the description of the invention, it is to be understood that term " " center ", " longitudinal direction ", " transverse direction ", " length ", " width ",
" thickness ", " on ", D score, "front", "rear", "left", "right", " vertical ", " level ", " top ", " bottom " " interior ", " outward ", " up time
The orientation or position relationship of the instruction such as pin ", " counterclockwise ", " axial direction ", " radial direction ", " circumference " be based on orientation shown in the drawings or
Position relationship, is for only for ease of the description present invention and simplifies description, must rather than the device or element for indicating or imply meaning
With specific orientation, with specific azimuth configuration and operation, therefore must be not considered as limiting the invention.
In the present invention, unless otherwise clearly defined and limited, term " installation ", " connected ", " connection ", " fixation " etc.
Term should be interpreted broadly, for example, it may be fixedly connected, or be detachably connected, or integrally；Can be that machinery connects
Connect, or electrically connect；Can be joined directly together, it is also possible to be indirectly connected to by intermediary, can be in two elements
The connection in portion or two interaction relationships of element.For the ordinary skill in the art, can be according to specific feelings
Condition understands above-mentioned term concrete meaning in the present invention.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means to combine specific features, structure, material or spy that the embodiment or example are described
Point is contained at least one embodiment of the invention or example.In this manual, to the schematic representation of above-mentioned term not
Identical embodiment or example must be directed to.And, the specific features of description, structure, material or feature can be with office
Combined in an appropriate manner in one or more embodiments or example.Additionally, in the case of not conflicting, the skill of this area
Art personnel can be tied the feature of the different embodiments or example described in this specification and different embodiments or example
Close and combine.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changes, replacing and modification.
Claims (10)
1. a kind of method for preparing silver nanoparticle fiber membrane, it is characterised in that including：
By silver-colored precursor solution add injection-tube in, and using topping-up pump by the silver-colored precursor solution from the injection-tube phase
Syringe needle even is released, and obtains fiber；
The fiber is stretched using air-flow, obtains silver nanoparticle fiber；
The silver nanoparticle fiber is collected on the collector, silver nanoparticle fiber membrane precursor is obtained；
The silver nanoparticle fiber membrane precursor is post-processed, silver nanoparticle fiber membrane is obtained.
2. method according to claim 1, it is characterised in that the silver-colored precursor solution contains inorganic salts, the high score of silver
Son and solvent；
The inorganic salts of the silver are silver nitrate；
The macromolecule is PVP；
The solvent is acetonitrile,
The gas for forming the air-flow is selected from least one in compressed air, nitrogen, argon gas, helium.
3. method according to claim 2, it is characterised in that formed the air-flow gas pressure for 0.001MPa extremely
20MPa。
4. method according to claim 1, it is characterised in that the collector is nickel screen, sheet glass or glass fiber sheets.
5. method according to claim 1, it is characterised in that the post processing be selected from sintering processes, magnetron sputtering treatment,
Electroplating processes, ultraviolet irradiation treatment or vapour deposition treatment.
6. a kind of silver nanoparticle fiber membrane, it is characterised in that prepared by the method any one of claim 1-5
's.
7. a kind of equipment for preparing silver nanoparticle fiber membrane, it is characterised in that including：
Injection-tube, for accommodating silver-colored precursor solution；
Syringe needle, the syringe needle is connected with the injection-tube, for projecting the silver-colored precursor solution；
Topping-up pump, the post liquid pump is connected with the injection-tube, for the silver-colored precursor solution to be released；
Feeder, for being stretched to obtain silver nanoparticle fiber to the fiber using air-flow；
Collector, for collecting the silver nanoparticle fiber.
8. equipment according to claim 7, it is characterised in that the syringe needle is L-shaped.
9. equipment according to claim 7, it is characterised in that the collector is nickel screen sheet glass or glass fiber sheets.
10. a kind of electronic device, it is characterised in that contain the silver nanoparticle fiber membrane described in claim 6.
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