CN103440907B - A kind of cellulose nano-fibrous with nano silver wire composite conductive thin film and preparation method thereof - Google Patents
A kind of cellulose nano-fibrous with nano silver wire composite conductive thin film and preparation method thereof Download PDFInfo
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- CN103440907B CN103440907B CN201310399562.3A CN201310399562A CN103440907B CN 103440907 B CN103440907 B CN 103440907B CN 201310399562 A CN201310399562 A CN 201310399562A CN 103440907 B CN103440907 B CN 103440907B
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Abstract
The invention discloses a kind of cellulose base transparent conductive film, there is in described conductive film nanofiber and nano silver wire dual-network structure.The present invention utilizes native cellulose to prepare nanofiber dispersion liquid, liquid phase polyxol method prepares nano silver wire, then adopt vacuum filtration technology at filter membrane surface deposit fiber element nanofiber and nano silver wire respectively, thus obtained cellulose nano-fibrous with nano silver wire (CNFs/AgNWs) laminated film.This film is flexible transparent conductive film, is 63.3 ~ 78.2% at 550nm place light transmission rate, square resistance scope 0.38 ~ 3.47k Ω/sq, tensile strength >=40MPa, elongation >=6%.
Description
Technical field
The present invention relates to cellulose technology field and flexible transparent conductive film field, particularly relate to the preparation method of cellulose base flexible transparent conductive film.
Background technology
General fibre and goods thereof are insulator, easily produce electrostatic, bring inconvenience, even endanger the life of applied production field and people.In the 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 is in electrostatic environment symptoms such as can causing headache, insomnia and dysphoria for a long time, even causes fash and arrhythmia cordis, larger to the harm of neurastheniac and mental patient.Therefore, the research and development with the cellulosics of conducting function have very important significance to the work of modern society people and life.
Cellulose and goods thereof have pliable and tough, light weight, cheapness, easily to reclaim and can the advantage such as large-scale production, become in modern industry the membrane material having much application prospect.All the time, cellulosics mostly is insulator, limits its application in the opto-electronic device.Based on the feature of cellulose film forming, cellulose can be made the flexible transparent conducting film material of cellulose base, this material can have broad application prospects in display, communication, electroluminescent driving, the energy and sensor field, the ITO material of fictitious hosts costliness.Compared with traditional nesa coating, the flexible and transparent conductive material of cellulose base, except having excellent light transmission and conductivity, also has the features such as lightweight, bend-resistance, thermal coefficient of expansion be little.
Although having a extensive future of conductive cellulose film, also to consider the processing technology preparing cellulose base flexible transparent conducting film, be conducive to flexible transparent conducting film post-production.Cellulose conductive modified mode the most frequently used at present adds conductive filler, and mainly adding in casting solution with nanometer carbon black is the inorganic nanoparticles of representative and the conducting polymer based on polypyrrole.Wherein nanometer carbon black and carbon nano-tube have excellent electric conductivity, but nanometer carbon black and carbon nano-tube due to specific area large, serious difficulties in dispersion of reuniting, greatly reduces its serviceability.Patent CN102102231 adopts ionic liquid nanometer carbon black and even carbon nanotube to be disperseed, and utilizes the interaction between process of lapping intermediate ion liquid cationic and carbon, reduce the Van der Waals force between nano-sized carbon, thus the nano-sized carbon of agglomerated is dispersed.With the fiber that this kind of method is made, 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 conductive carbon black particle must form cross-bond in large molecule or as best one can close to strand, once add electric field, electronics in carbon black particle will move and form electric current in cross-bond, and the conductivity of such fiber also can be affected.Patent CN200510015491, CN102002858 etc. adopt the intrinsic conducting polymer such as aniline, pyrroles, thiophene or to be scattered in casting solution blending or to 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 reduced, and limits it and promotes the use of.In addition, also have and realize cellulose membrane conductive characteristic by chemical dip method.The method is flooded mainly through reactant liquor, absorption is produced on cellulose membrane surface, then make metallic compound or deposition by chemical reaction or be adsorbed in surface, as patent CN97118822, CN8710462, but institute's depositing metallic compounds have for noxious substance, some chemical properties are unstable, and after depositing metallic compounds, cellulose membrane poor surface quality, post-production is difficult and firmness, uniformity are general, fails to obtain extensive use.
Going deep into gradually in recent years along with Application of micron, 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.Cellulose and nano silver wire compound is utilized to make flexible transparent conducting film material, both cellulose environmental protection, cheap feature can have been played, expand the function application of its flexible and transparent conductive in electronics industry, substitute and upgrade hard transparent conducting membrane material, its electrostatic-proof function as cellulosics can be improved again, 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 is excellent, physical and mechanical properties is good cellulose and nano silver wire laminated film and preparation method are provided.This cellulose and nano silver wire laminated film are a kind of excellent flexible transparent conducting film material.
The invention reside in and carry out compound with nano silver wire obtain a kind of excellent flexible transparent conductive film material by cellulose nano-fibrous, this material be prepared by following method:
Step one, sieves native cellulose, soaks and carries out de-cured process, then use sodium chlorite (NaClO respectively in toluene solution
2) and potassium hydroxide (KOH) process, remove lignin and hemicellulose.Products therefrom filtration washing, to neutral, is made into cellulose suspension solution, crosses beater and pulverizes, as cellulosic casting solution after ultrasonic or standing and defoaming process.
Step 2, dilutes cellulose casting solution deionized water, carries out vacuum filtration after stirring to suspension-turbid liquid, obtains cellulose nano-fibrous rete on teflon membrane filter surface.
Step 3; under argon atmosphere, magnetic agitation and condensing reflux condition; utilize oil bath computer heating control reaction temperature constant; add 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, reaction certain hour.After the cooling of reactant liquor room temperature, load in centrifuge tube and carry out centrifugation.Use the acetone of mother liquor volume 3 ~ 5 times as dispersion liquid, centrifugation 1 ~ 3 time.Finally, sediment alcohol extract, dispersion, thus the nano silver wire alcohol dispersion liquid after obtained purification.
Step 4, is placed on 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.Laminated film that is cellulose nano-fibrous and nano silver wire is formed at filter membrane surface after suction filtration.
Step 5, dries under vacuum by filter membrane and laminated film, peels off filter membrane, can obtain the laminated film of cellulose nanometer and nano silver wire.
Alternately repetitive operation step 2 and step 4, then the laminated film carrying out that step 5 can obtain the cellulose nano-fibrous of multilayer repetitive structure and nano silver wire.
Selecting native cellulose can be lignocellulosic in described step one, be also cotton cellulose.
Select cellulose degradation inhibitor and dispersant to be watery hydrochloric acid in described step one, sodium chlorite solution's concentration is 0.1 ~ 0.5M, and potassium hydroxide solution concentration is 0.3 ~ 0.5M, and being made into cellulose solution quality classification is 0.1 ~ 1%.
In described step 3, reaction temperature controls at 160 ~ 180 DEG C, and the ethylene glycol solution concentration of silver nitrate is the ethylene glycol solution of 0.1 ~ 1.1M, PVP is 0.1 ~ 0.3M, 1 ~ 2 hour reaction time.
Select PVP solution to serve as initator and bonding agent in described step 4, with increase nano silver wire and cellulose nano-fibrous between in conjunction with firmness.
Obtained cellulose nano-fibrously with the structure of nano silver wire laminated film be: bottom fiber element nanofiber is crossed as latticed, upper strata is nano silver wire rete, nano silver wire presents unordered juxtaposition shape, rete interface has part nano silver wire to insert in cellulose nano-fibrous grid due to suction filtration effect, forms gear shaping structure.
Described obtained cellulose nano-fibrous be 66.3 ~ 78.2% with nano silver wire laminated film in the light transmission rate scope at 550nm place, the scope of square resistance is 0.38 ~ 3.47k Ω/sq, tensile strength >=40MPa, elongation >=6%.
Accompanying drawing explanation
Accompanying drawing 1 is cellulose nano-fibrous with nano silver wire laminated film side structure schematic diagram.
Nano silver wire microscopic appearance prepared by accompanying drawing 2.
Embodiment
The present invention is set forth further below in conjunction with specific embodiment.
Specific embodiment 1
Preparation cellulose casting solution, lignocellulosic 5g is crossed 60 mesh sieves, soak in toluene/ethanol (2:1) mixed solution and within 6 hours, carry out de-cured process, then respectively with sodium chlorite 0.5g, watery hydrochloric acid 1ml and potassium hydroxide 4.2g process, remove lignin and hemicellulose.Products therefrom carries out utilizing vacuum filtration cup fully to carry out filtering, washing until filtrate is in neutral, obtains cleaning cellulose cellulose fiber.Get above-mentioned fiber to be made into cellulose and to be suspended the aqueous solution (mass fraction 1%), cross beater and pulverize, as cellulosic casting solution after ultrasonic or standing and defoaming process.
In magnetic agitation and under condensing reflux condition, with continue in there-necked flask to pass to cleaned after argon gas, utilize oil bath to heat the temperature controlling whole course of reaction and maintain between 160 ~ 180 DEG C.Adopt two-step method to prepare nano silver wire: (1) JZPD capsule: add 2ml ethylene glycol, heating 10min, then adds lml silver nitrate with syringe: ethylene glycol solution (2 × 10 fast
-4m), 15min is reacted; (2) crystal growing process: add 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), control to add at about 10min, then continue reaction 2h.
After the cooling of reactant liquor room temperature, load in centrifuge tube and carry out centrifugation.Use mother liquor volume number is that the acetone of 5 times washs, centrifugation under the rotating speed of 3000rpm, centrifugation time 5min.Remove supernatant liquor, leave sediment, then in centrifuge tube, add deionized water or the ethanol that mother liquor volume fraction is 5 times, centrifugation at 3,000 rpm, removes supernatant liquor, leaves sediment.After repetitive operation 3 times, with alcohol extract and dispersion sediment, obtained nano silver wire alcohol dispersion liquid.
Cellulose casting solution deionized water is diluted to quality classification 0.1%, after stirring 24h, vacuum filtration is carried out to suspension-turbid liquid, in glass filter bowl, use teflon membrane filter (0.1 μm, aperture), suction filtration 3 ~ 4h, obtains cellulose nano-fibrous rete at filter membrane surface; Nano silver wire alcohol dispersion liquid is poured in suction filtration cup, suction filtration is continued with the filter membrane of deposit fiber element film, after suction filtration completes, filter membrane is placed in 40 DEG C of vacuum drying chambers and dries 6h, peel off teflon membrane filter and obtain laminated film that is cellulose nano-fibrous and nano silver wire.
The obtained cellulose nano-fibrous laminated film with nano silver wire is 68% at 550nm place light transmission rate, and the scope of block resistance is 1.25k Ω/sq, tensile strength 41.3MPa; Elongation 8.2%.
Specific embodiment 2
Preparation cellulose casting solution, weighs cotton fiber 5g, is placed in 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 DEG C of waters bath with thermostatic control or oil bath pan with sealed membrane sealing and heats 2h.React rear vacuum filtration, and be neutral with distilled water cyclic washing to filtered fluid, obtain holocellulose fiber; Loaded in 250ml beaker by holocellulose fiber, add 100ml potassium hydroxide solution (mass fraction 4%), sealing is placed in 90 DEG C of waters bath with thermostatic control or oil bath pan heats 4h, carries out magnetic agitation simultaneously.React rear vacuum filtration pump carry out suction filtration and use distilled water cyclic washing, until filtrate is in neutral, to remove hemicellulose, obtain purifying cellulose.This cellulose is made into 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 cellulose casting solution after ultrasonic deaeration process or deaeration process of mourning in silence.
One-step method prepares nano silver wire solution: namely in system, form the crystal seed needed for silver nanowire growth fast by additional controlling agent, without the need to independent seed crystal production process, only certain density silver nitrate ethylene glycol solution need be mixed with the PVP ethylene glycol solution containing certain controlling agent and carry out seeded growth.Concrete test procedure is: under argon shield, magnetic agitation and condensing reflux condition, utilizes oil bath to control in there-necked flask reaction temperature at 160 ± 5 DEG C.Add 10ml ethylene glycol preheating 30min, then add the silver nitrate of 5ml (1M) fast: ethylene glycol solution, then drip off 10ml (0.15M) PVP at about 10min lentamente: ethylene glycol solution.Reaction timing 1h.
After question response liquid is cooled to room temperature, loads in centrifuge tube and carry out centrifugation.Centrifugation under the ethanol of use mother liquor volume number 3 times, the rotating speed of 3000rpm, removes supernatant liquor, leaves sediment.Repeat this operation 3 times, the nano silver wire alcohol dispersion liquid after obtained purification.
After cellulosic casting solution is stirred 24h, carry out vacuum filtration to suspension-turbid liquid, in glass filter bowl, use teflon membrane filter (0.1 μm, aperture), suction filtration 3 ~ 4h, obtains cellulose nano-fibrous rete at filter membrane surface; The alcohol dispersion liquid of nano silver wire is continued suction filtration on this filter membrane basis, after suction filtration completes, filter membrane is placed in 40 DEG C 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.
The obtained cellulose nano-fibrous laminated film with nano silver wire is 71.3% at 550nm place light transmission rate, and the scope of block resistance is 0.98k Ω/sq, tensile strength 40.6MPa; Elongation 8.5%.
Claims (4)
1. a cellulose nano-fibrous preparation method with nano silver wire composite conductive thin film, is characterized in that comprising following steps:
Step one, be scattered in the aqueous solution by cellulose, after de-cured, purification process, making beating is made into suspension-turbid liquid, carries out after deaeration process as casting solution;
Step 2, casting solution is placed in suction filtration cup, carries out vacuum filtration, after treating suction filtration, washing, obtain cellulose nano-fibrous membrane;
Step 3, utilize liquid phase polyxol method to prepare nano silver wire suspension, wherein PVP is as initator and bonding agent;
Step 4, nano silver wire suspension is placed in step 2 complete after suction filtration cup, vacuum filtration, nano silver wire is deposited on cellulose nano-fibrous membrane surface and forms 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 conditions, peel off filter membrane, obtain composite conductive thin film that is cellulose nano-fibrous and nano silver wire;
In step 2, the cellulose nano-fibrous diameter of gained is controlled within the scope of 50 ~ 400nm;
Nano silver wire diameter in step 3 is controlled within the scope of 80 ~ 300nm;
In step 5 gained cellulose nano-fibrous with the composite conductive thin film of nano silver wire in containing mass fraction 50 ~ 60% nano silver wire, mass fraction 30 ~ 40% cellulose nano-fibrous; Cellulose nano-fibrous is 0.38 ~ 3.47k Ω/sq with the conductivity of nano silver wire composite conductive thin film, tensile strength >=40MPa, elongation >=6%; Cellulose nano-fibrous being filled in cellulose nano-fibrous grid-gap with the composite conductive thin film rete interface nano silver wire of nano silver wire forms gear shaping structure.
2. a kind of cellulose nano-fibrous preparation method with nano silver wire composite conductive thin film as claimed in claim 1, it is characterized in that: in step one, 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.
3. a kind of cellulose nano-fibrous preparation method with nano silver wire composite conductive thin film as claimed in claim 1, it is characterized in that adopting the suction filtration method in step 4 to adhere to nano silver wire film layer structure on the surface at cellulose nano-fibrous membrane, between cellulose nano-fibrous layer and nano silver wire rete, adopt PVP as bonding agent.
4. a kind of cellulose nano-fibrous preparation method with nano silver wire composite conductive thin film as claimed in claim 1, it is characterized in that: after step one, step 3, step 2 and step 4 can repeat blocked operation, carry out step 5 again, the composite conductive thin film of cellulose nano-fibrous and nano silver wire of multilayer repetitive structure.
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| CN112971725B (en) * | 2021-02-10 | 2023-12-26 | 武汉理工大学 | Preparation of electromagnetic radiation resistant nanocellulose/silver nanowire flexible sensor |
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