CN103440907A - Cellulose nanofibers and silver nanowires composite conductive film and preparation method of composite conductive film - Google Patents
Cellulose nanofibers and silver nanowires composite conductive film and preparation method of composite conductive film Download PDFInfo
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Abstract
The invention discloses a cellulose-based transparent conductive film which is provided with a dual-web structure of nanofibers and silver nanowires. Natural cellulose is utilized to prepare nanofiber dispersion liquid, and a liquid phase polyol method is utilized to prepare the silver nanowires. A vacuum pumping filtration technology is adopted so that the cellulose nanofibers and the silver nanowires are respectively deposited on the surface of a filter film. Therefore, a composite film of the cellulose nanofibers and the silver nanowires (CNFs/AgNWs) is prepared. The film is a flexible and transparent conductive film whose light transmittance rate ranges from 63.3 to 78.2% at 550nm, square resistance ranges from 0.38 to 3.47 kohm/sq, tensile strength is larger than or equal to 40MPa and elongation percentage is larger than or equal to 6%.
Description
Technical field
The present invention relates to cellulose technology field and flexible transparent conductive film field, relate in particular to the preparation method of cellulose base flexible transparent conductive film.
Background technology
General fibre and goods thereof are insulator, easily produce static, and applied production field and people's life is brought to inconvenience, even harm.In electronics industry, static discharge can cause spectral interference, affects the running of electronic equipment; In chemical industry, static discharge easily causes flammable and explosive substance, causes potential safety hazard; In addition, medical research shows, human body can cause the symptoms such as headache, insomnia and dysphoria for a long time in the static environment, even causes fash and arrhythmia cordis, larger to neurastheniac and mental patient's harm.Therefore, the research and development that have a cellulosics of conducting function have very important significance to modern society people's work and life.
That cellulose and goods thereof have is pliable and tough, light weight, cheapness, easily reclaim and can large-scale production etc. advantage, become in modern industry the membrane material that has much application prospect.All the time, cellulosics mostly is insulator, has limited its application in photoelectric device.Characteristics based on cellulose film forming, can make cellulose the flexible transparent conducting film material of cellulose base, and this material can cause driving, the energy and sensor field at demonstration, communication, electricity and have broad application prospects, and substitutes expensive ITO material.With traditional nesa coating, compare, the flexible and transparent conductive material of cellulose base, except having good light transmission and conductivity, also has the characteristics such as lightweight, bend-resistance, thermal coefficient of expansion be little.
Although having a extensive future of conductive cellulose film, also will consider the processing technology for preparing the cellulose base flexible transparent conducting film, is conducive to the flexible transparent conducting film post-production.At present the most frequently used cellulose conductive modified mode is to add conductive filler, is mainly in casting solution, to add to take inorganic nanoparticles and the conducting polymer of polypyrrole as leading of take that nanometer carbon black is representative.Wherein nanometer carbon black and carbon nano-tube have good electric conductivity, but nanometer carbon black and carbon nano-tube be because specific area is large, and the serious difficulties in dispersion of reuniting, greatly reduce its serviceability.Patent CN102102231 adopts ionic liquid that nanometer carbon black and even carbon nanotube are disperseed, and utilizes the interaction between cation and carbon in process of lapping intermediate ion liquid, the Van der Waals force between the reduction nano-sized carbon, thus the nano-sized carbon of agglomerated is dispersed.The fiber of making by this kind of method, the addition of carbon black is higher, can cause obtaining impact to the physical and mechanical properties of fiber and the processability of fiber, and the conductive carbon black particle must form cross-bond or approach as best one can strand in large molecule, once add electric field, electronics in carbon black particle will move and form electric current in cross-bond, and the conductivity of fiber also can be affected like this.Intrinsic conducting polymers such as the employing such as patent CN200510015491, CN102002858 aniline, pyrroles, thiophene or be scattered in casting solution blending or be coated on basic cellulose membrane surface, though technological operation is simple, but the uniformity coefficient of reaction and the firmness of conductive layer exist certain not enough, cellulosic quality of forming film also reduces, and has limited it and has promoted the use of.In addition, also have by the chemical impregnation method and realize the cellulose membrane conductive characteristic.The method is mainly flooded by reactant liquor, produce absorption on the cellulose membrane surface, then make metallic compound or deposition or be adsorbed in surface by chemical reaction, as patent CN97118822, CN8710462, but institute's plated metal compound have for noxious substance, some chemical properties are unstable, and after the plated metal compound, cellulose membrane surface quality variation, post-production difficulty and firmness, uniformity are general, fail to obtain extensive use.
In recent years along with Application of micron gradually deeply, the nano silver wire that conductance is high, lightweight is nontoxic gets more and more people's extensive concerning.Nano silver wire has excellent conduction, thermal conduction characteristic, nanocomposite optical effect and bactericidal action, and potential using value is huge.Utilize the compound flexible transparent conducting film material of making of cellulose and nano silver wire, the characteristics of cellulose environmental protection, cheapness both can have been brought into play, expand the function application of its flexible and transparent conductive in electronics industry, substitute and renewal hard transparent conducting membrane material, can improve again its electrostatic-proof function as cellulosics, improve the added value of cellulose products.
Summary of the invention
The present invention is based on cellulose and nano silver wire material, a kind of electric conductivity excellence, good cellulose and nano silver wire laminated film and the preparation method of physical and mechanical properties are provided.This cellulose and nano silver wire laminated film are a kind of good flexible transparent conducting film material.
The invention reside in cellulose nano-fibrous and nano silver wire are carried out to compound a kind of good flexible transparent conductive film material that makes, this material be by following method preparation:
Step 1, sieve native cellulose, in toluene solution, soaks and take off cured processing, then uses respectively sodium chlorite (NaClO
2) and potassium hydroxide (KOH) processing, remove lignin and hemicellulose.The products therefrom filtration washing, to neutral, is made into the cellulose suspension solution, cross beater and pulverize, ultrasonic or standing and defoaming process after as cellulosic casting solution.
Step 2, dilute the cellulose casting solution with deionized water, after stirring, suspension-turbid liquid is carried out to vacuum filtration, on the teflon membrane filter surface, obtains cellulose nano-fibrous rete.
Step 3; under argon shield atmosphere, magnetic agitation and condensing reflux condition; utilize oil bath to add the thermal control reaction temperature constant; add the ethylene glycol solution preheating in flask after, add silver nitrate/ethylene glycol solution and polyvinylpyrrolidone (PVP)/ethylene glycol solution (containing certain density controlling agent) simultaneously.Wherein liquor argenti nitratis ophthalmicus adds fast, and PVP solution slowly adds, the reaction certain hour.After the reactant liquor room temperature is cooling, carry out centrifugation in the centrifuge tube of packing into.Use the acetone of 3 ~ 5 times of mother liquor volumes as dispersion liquid, centrifugation 1 ~ 3 time.Finally, alcohol extract, dispersion for sediment, thus make the nano silver wire alcohol dispersion liquid after purification.
Step 4, be placed on the suction filtration cup by the dilution of nano silver wire alcohol dispersion liquid, carries out suction filtration.The surface that suction filtration obtains after adopting step 2 to complete is covered with cellulose nano-fibrous filter membrane.Form laminated film cellulose nano-fibrous and nano silver wire after suction filtration on the filter membrane surface.
Step 5 is dried filter membrane and laminated film under vacuum condition, peels off filter membrane, can obtain the laminated film of cellulose nanometer and nano silver wire.
Replace repetitive operation step 2 and step 4, then carry out the laminated film that step 5 can obtain the cellulose nano-fibrous and nano silver wire of multilayer repetitive structure.
Selecting native cellulose in described step 1 can be lignocellulosic, is also cotton cellulose.
Selecting cellulose degradation inhibitor and dispersant in described step 1 is watery hydrochloric acid, and sodium chlorite solution's concentration is 0.1 ~ 0.5M, and potassium hydroxide solution concentration is 0.3 ~ 0.5M, and being made into the cellulose solution quality classification is 0.1 ~ 1%.
In described step 3, reaction temperature is controlled at 160 ~ 180 ℃, and the ethylene glycol solution concentration of silver nitrate is 0.1 ~ 1.1M, and the ethylene glycol solution of PVP is 0.1 ~ 0.3M, 1 ~ 2 hour reaction time.
In described step 4, select PVP solution to serve as initator and bonding agent, with increase nano silver wire with cellulose nano-fibrous between in conjunction with firm degree.
Obtained cellulose nano-fibrous and the structure nano silver wire laminated film are: bottom fiber element nanofiber is crossed as latticed, upper strata is the nano silver wire rete, nano silver wire presents unordered juxtaposition shape, there is the part nano silver wire rete interface because the suction filtration effect is inserted in cellulose nano-fibrous grid, forms the gear shaping structure.
Described to make cellulose nano-fibrous and the light transmission rate scope of nano silver wire laminated film at the 550nm place be 66.3 ~ 78.2%, and the scope of square resistance is 0.38 ~ 3.47k Ω/sq, tensile strength >=40MPa, elongation >=6%.
The accompanying drawing explanation
Accompanying drawing 1 cellulose nano-fibrous with nano silver wire laminated film side structure schematic diagram.
Accompanying drawing 2 prepares the nano silver wire microscopic appearance.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment.
Specific embodiment 1
Preparation cellulose casting solution, lignocellulosic 5g is crossed to 60 mesh sieves, soak and within 6 hours, take off cured processing in toluene/ethanol (2:1) mixed solution, then process with sodium chlorite 0.5g, watery hydrochloric acid 1ml and potassium hydroxide 4.2g respectively, remove lignin and hemicellulose.Products therefrom is utilized, and the vacuum filtration cup is fully filtered, washing is until filtrate is neutral, obtains the purifying cellulose fiber.Get above-mentioned fiber and be made into cellulose and be suspended the aqueous solution (mass fraction 1%), cross beater and pulverize, ultrasonic or standing and defoaming process after as cellulosic casting solution.
Under magnetic agitation and condensing reflux condition, purifying argon gas later with continuing in there-necked flask to pass to, the temperature of utilizing oil bath to heat to control whole course of reaction maintains between 160 ~ 180 ℃.Adopt two-step method to prepare nano silver wire: the preparation of (1) crystal seed: add 2ml ethylene glycol, heating 10min, then add the lml silver nitrate with syringe: ethylene glycol solution (2 * 10 fast
-4m), reaction 15min; (2) crystal growing process: add the 5ml silver nitrate with syringe in 20s: ethylene glycol solution (0.1M), slowly drip the ethylene glycol solution (0.3M of 10mlPVP simultaneously, in the repetitive of PVP), be controlled at the 10min left and right and add, then continue reaction 2h.
After cooling Deng the reactant liquor room temperature, carry out centrifugation in the centrifuge tube of packing into.Use the acetone that mother liquor volume number is 5 times to be washed, centrifugation under the rotating speed of 3000rpm, centrifugation time 5min.Remove supernatant liquor, stay sediment, then add deionized water or the ethanol that the mother liquor volume fraction is 5 times in centrifuge tube, centrifugation under 3000rpm, remove supernatant liquor, stays sediment.After repetitive operation 3 times, with alcohol extract and dispersion sediment, make the nano silver wire alcohol dispersion liquid.
The cellulose casting solution is diluted to quality classification 0.1% with deionized water, after stirring 24h, suspension-turbid liquid is carried out to vacuum filtration, use teflon membrane filter (aperture 0.1 μ m) in the glass filter bowl, suction filtration 3 ~ 4h, obtain cellulose nano-fibrous rete on the filter membrane surface; The nano silver wire alcohol dispersion liquid is poured in the suction filtration cup, continue suction filtration with the filter membrane of deposit fiber element film, after suction filtration completes, filter membrane is placed in to 40 ℃ of vacuum drying chambers and dries 6h, teflon membrane filter is peeled off and obtained cellulose nano-fibrous and laminated film nano silver wire.
Obtained cellulose nano-fibrous and laminated film nano silver wire are 68% at 550nm place light transmission rate, and the scope of piece resistance is 1.25k Ω/sq, tensile strength 41.3MPa; Elongation 8.2%.
Specific embodiment 2
Preparation cellulose casting solution, weighing cotton fiber 5g, be placed in the 250ml beaker, adds distilled water 125ml, glacial acetic acid 0.5ml and sodium chlorite 0.6g, and magnetic agitation, after 4 hours, is placed in 75 ℃ of waters bath with thermostatic control or oil bath pan and heats 2h with the sealed membrane sealing.React the rear vacuum filtration of using, and be neutral with distilled water cyclic washing to filtered fluid, obtained the holocellulose fiber; The holocellulose fiber is packed in the 250ml beaker, add 100ml potassium hydroxide solution (mass fraction 4%), sealing is placed in 90 ℃ of waters bath with thermostatic control or oil bath pan heats 4h, carries out magnetic agitation simultaneously.Reacted rear and carried out suction filtration and use the distilled water cyclic washing with the vacuum filtration pump, until filtrate is neutral, to remove hemicellulose, obtained purifying cellulose.This cellulose is made into to the water suspension solution of quality classification 1%, then carries out milled processed, speed of grinding plate 2000rpm, abrasive disk space is 0mm, and grinding number of times is 20 times, and gained solution obtains the cellulose casting solution after ultrasonic deaeration processing or the deaeration processing of mourning in silence.
One-step method prepares nano silver wire solution: by additional controlling agent, in system, form fast the nano silver wire required crystal seed of growing, without independent seed crystal production process, only certain density silver nitrate ethylene glycol solution need be mixed with the PVP ethylene glycol solution that contains certain controlling agent and carry out seeded growth and get final product.Concrete test procedure is: under argon shield, magnetic agitation and condensing reflux condition, utilize oil bath to control in there-necked flask reaction temperature at 160 ± 5 ℃.Add 10ml ethylene glycol preheating 30min, then add fast the silver nitrate of 5ml (1M): ethylene glycol solution, then drip off 10ml (0.15M) PVP in the 10min left and right lentamente: ethylene glycol solution.Reaction timing 1h.
After question response liquid is cooled to room temperature, carry out centrifugation in the centrifuge tube of packing into.Centrifugation under the ethanol that use mother liquor volume is several 3 times, the rotating speed of 3000rpm, remove supernatant liquor, stays sediment.Repeat this operation 3 times, make the nano silver wire alcohol dispersion liquid after purification.
After cellulosic casting solution is stirred to 24h, suspension-turbid liquid is carried out to vacuum filtration, use teflon membrane filter (aperture 0.1 μ m) in the glass filter bowl, suction filtration 3 ~ 4h, obtain cellulose nano-fibrous rete on the filter membrane surface; The alcohol dispersion liquid of nano silver wire is continued to suction filtration on this filter membrane basis, after suction filtration completes, filter membrane is placed in to 40 ℃ of vacuum drying chambers and dries 6h, teflon membrane filter is peeled off and obtained the laminated film of cellulose fibre and nano silver wire.
Obtained cellulose nano-fibrous and laminated film nano silver wire are 71.3% at 550nm place light transmission rate, and the scope of piece resistance is 0.98k Ω/sq, tensile strength 40.6MPa; Elongation 8.5%.
Claims (8)
1. the preparation method of cellulose nano-fibrous and nano silver wire composite conductive thin film, it is characterized in that in the laminated film of described cellulose nano-fibrous and nano silver wire containing mass fraction at 50 ~ 60% nano silver wire, mass fraction 30 ~ 40% cellulose nano-fibrous.
2. the cellulose nano-fibrous and conductivity nano silver wire composite conductive thin film is 0.38 ~ 3.47k Ω/sq as claimed in claim 1, tensile strength >=40MPa, elongation >=6%.
3. a kind of preparation method of cellulose nano-fibrous and nano silver wire composite conductive thin film as claimed in claim 1 is characterized in that comprising following steps:
Step 1, cellulose is scattered in the aqueous solution, after de-cured, purification process, making beating is made into suspension-turbid liquid, carries out after the deaeration processing as casting solution;
Step 2, casting solution is placed in to the suction filtration cup, carries out vacuum filtration, treat to obtain cellulose nano-fibrous membrane after suction filtration, washing;
Step 3, utilize the liquid phase polyxol method to prepare nano silver wire suspension, wherein PVP is as initator and bonding agent;
Step 4, the suction filtration cup after nano silver wire suspension is placed in to step 2 and completes, vacuum filtration, nano silver wire is deposited on the cellulose membrane surface and forms the nano silver wire rete, and then obtains the cellulose nano-fibrous of filter membrane surface and nano silver wire composite film;
Step 5, the composite film of step 4 gained is dry under vacuum environment, peel off filter membrane, obtains cellulose nano-fibrous and laminated film nano silver wire.
4. a kind of preparation method of cellulose nano-fibrous and nano silver wire composite conductive thin film as claimed in claim 3, it is characterized in that: in step 1, the mass fraction of cellulose aqueous solution is 0.1 ~ 1%, in step 3, the concentration of nano silver wire suspension is at 0.1 ~ 1.1M, and in suspension, the ethylene glycol solution concentration range of initator and bonding agent PVP is at 0.1 ~ 0.3M.
5. a kind of preparation method of cellulose nano-fibrous and nano silver wire composite conductive thin film as claimed in claim 3, it is characterized in that adopting the suction filtration method to adhere to the nano silver wire film layer structure on cellulose nano-fibrous matrix, fibrage and silver nanoparticle interlayer adopt PVP as bonding agent.
6. a kind of preparation method of cellulose nano-fibrous and nano silver wire composite conductive thin film as claimed in claim 3, it is characterized in that: after step 1, step 3, step 2 and step 4 can repeat blocked operation, carry out again step 5, get final product to obtain the composite conductive thin film of cellulose nano-fibrous and nano silver wire of multilayer repetitive structure.
7. a kind of cellulose nano-fibrous and nano silver wire composite conductive thin film as claimed in claim 1, it is characterized in that cellulose nano-fibrous diameter is controlled in 50 ~ 400nm scope, the nano silver wire diameter is controlled in 80 ~ 300nm scope, and rete interface nano silver wire is filled in formation gear shaping structure in cellulose nano-fibrous grid-gap.
8. a kind of cellulose nano-fibrous and nano silver wire composite conductive thin film as claimed in claim 1, is characterized in that combining cheapness, environmental protection and the soft characteristic of cellulose membrane, increased its electrically conducting transparent function, has very strong industrial application prospect.
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| CN113072725A (en) * | 2021-03-31 | 2021-07-06 | 北京林业大学 | Nano-cellulose/MXene/silver nanowire sandwich-structure composite film and preparation method thereof |
| CN114822920A (en) * | 2022-04-15 | 2022-07-29 | 哈尔滨工业大学（深圳） | Composite material and preparation method and application thereof |
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