CN109754951A - A kind of cellulose-graphene composite transparent conductive film and preparation method thereof - Google Patents
A kind of cellulose-graphene composite transparent conductive film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of cellulose-graphene compound transparent electricity conductive films and preparation method thereof.The present invention first prepares cellulose alkalinuria solution, add graphene, the sodium hydroxide that alkalinuria solution is formed in subzero environment-urea hydrate can be easily inserted into the interlayer region of graphene, and be attached in host layer, to destroy original hydrogen bond network, form new hydrogen bond network, realize the removing layer by layer of graphene, graphene-the cellulose solution that is uniformly dispersed is obtained, crosslinking agent is then added and forms cellulose-Graphene gel, conductive film is being obtained by hot pressing formation process.Scattered graphene and cellulose form stable cross-linked structure under the action of crosslinking agent in conductive film of the invention, the electric conductivity of graphene can be given full play to, the also additional conductive film that assigns is simultaneously with excellent anti-microbial property, hot water resistance and antistatic property, the multi-functional conductive film of high transparency is constructed, application prospect is wide.
Description
Technical field
The invention belongs to transparent conducting Composite material fields, and in particular to a kind of cellulose-graphene composite transparent is conductive
Film and preparation method thereof.
Background technique
With electronic product update quickening, lightweight, high transparency conductive film material increasingly made extensively
With.These transparent conductive films are widely used on the display, thin property solar battery, photoelectric material of electronic product, and
Possess long-range application prospect.Currently, the transparent conductive film base material in photoelectric material, mainly uses some transparencies
Height, the good organic polymer material of thermal stability.However these artificial high-molecular organic material degradations are difficult, to ecological environment meeting
It damages.In order to realize resources sustainable development, using new material substitution fossil feedstock demand oneself through extremely urgent.
Graphene is most thin, most tough material in the world so far, and there is superhigh-current-density, superhigh current carrying to move
Many superiority such as shifting rate, chemical inertness, high thermal conductivity, excellent light transmittance, super-hydrophobicity, the mechanical strength of superelevation
Can, so that it is widely used in the fields such as sensor, lithium ion battery, solar battery, fuel cell, photoelectricity.Especially its is good
The properties such as good translucency, high conductivity, preferable mechanical strength, receive the extensive concern in transparent conductive film field in recent years
With research.Compared with tin indium oxide (ITO) film, graphene transparent conductive film have translucency and stability it is good, it is flexible more preferably
The features such as.
Cellulose is not only from a wealth of sources, at low cost, light, renewable and biological as cheap natural macromolecular material
Degradation, while also possessing biggish specific surface area and superpower adsorption capacity, the cellulose membrane of preparation is increasingly closed extensively
Note, huge natural reserves can satisfy demand of the electronic product to conductive film completely.
In the prior art, the Related product of graphene composite nano fiber element is relatively more, such as patent CN103937032A
In describe a kind of composite coloured film of Cellulose nanocrystal/graphene and its fast preparation method, pass through the fiber that will be prepared
The nanocrystalline solution that is prepared into of element is mixed with graphene, and ultrasonic disperse, vacuum filtration obtains colour film.There are also patents
A kind of method that graphene oxide co-catalysis sour water solution prepares nano micro crystal cellulose is described in CN104910394A, it is above-mentioned special
Graphene is described in benefit can carry out the compound the relevant technologies to form joint product with nano-cellulose, but problem exists
In there are graphene particles in nano-cellulose in it ensure that joint product while certain graphene additive amount
Dispersion is uneven, and granular size is inhomogenous, is easy to happen the problem of interlayer is reunited, so different piece diameter graphene substances
Bring stress concentration point can be easy to be broken, and influence the performance for preparing product.
Summary of the invention
In order to solve the problems in background technique, the present invention provides a kind of cellulose-graphene of high-strength and high-ductility is saturating
Bright conductive film and preparation method thereof.
Technical scheme is as follows, specifically includes the following steps:
(1) graphene-cellulose solution preparation: 0.01~0.05g graphene is added in 100mL cellulose solution,
After stirring 10~60min, -10~-20 DEG C of progress low temperature removings obtain graphene-cellulose solution；
(2) graphene-cellulose gel preparation: crosslinking agent being added in the graphene-cellulose solution of step (1),
30~60 DEG C of 0.5~1h of stirring are warming up to, pour to form graphene-cellulose gel under 20~60 DEG C of water bath condition, are used
Deionized water is washed to pH=7；
(3) graphene-cellulose gel of step (2) is passed through into hot-forming rear acquisition graphene-cellulose membrane.Pass through
Hot-forming process, cellulose-Graphene gel form thin film, keep improving power while transparent type and electric conductivity
Learn intensity and toughness.
The cellulose solution is the cellulose alkalinuria solution obtained by cellulose and alkalinuria solution mixed preparing, wherein fine
The proportion of dimension element and alkalinuria solution are as follows: 2~5:95~98.
The cellulose alkalinuria solution is prepared using following methods: cellulose being added in alkalinuria solution, -10
0.5~2h is freezed under the conditions of~-20 DEG C, is persistently stirred 30-60min and is thawed, centrifugation obtains fine under 4000~6000rpm revolving speed
Tie up plain solution.
The alkalinuria solution is obtained by sodium hydroxide, urea and water mixed preparing, wherein the matter of sodium hydroxide, urea and water
Amount is than being 7:12:81.
The low temperature splitting time of the step (1) is 10~60min.
Crosslinking agent in the step (2) is N,N methylene bis acrylamide, epoxychloropropane, peroxidating diisopropyl
One of benzene, glutaraldehyde, dosage of crosslinking agent 1.5-2wt%.Be added crosslinking agent make graphene in conjunction with cellulose more
Securely, while the elasticity and mechanical strength of gel being improved.Washing is increased to remove the NaOH inside gel in deionized water
Add its transparency.
In the step (2), cellulose-graphene solution is poured with a thickness of 3mm-8mm；Bath temperature is at 20-30 DEG C
Gel is more readily formed under environment.
Hot-forming process conditions in the step (3) are as follows: hot pressing time 0.5-5h, temperature are 30-100 DEG C, pressure
Power is 20-100pa.Cellulose-the graphene composite film prepared using hot-forming principle is more tough, finer and close, improves its power
Learn performance.
Alkalinuria removes graphene while dissolving cellulose.Cellulose solution makes as dispersing agent and stabilizer
Graphene keeps dispersity.The cellulose solution of preparation is the stripping for next step to graphene there is no alkalinuria is dialysed
From.
The alkalinuria solution of cellulose plays key effect to the dispersion of graphene: 1) alkalinuria destroys graphene layer
Hydrogen bond and Van der Waals force realize the removing layer by layer of graphene；2) graphene being stripped is due to layer and interlayer cellulose
In the presence of so that it no longer reunites again, while cellulose surface is rich in polarity oxygen-containing group, hydrogen bond can occur with graphene and make
With with the noncovalent interactions such as electrostatic force, graphene is removed layer by layer, improves the dispersibility of graphene, even if standing two weeks
It is generated without precipitating.
The beneficial effects of the present invention are:
1, the hydrogen for the compound and the direct action breaks down cellulose of cellulose that the present invention is formed using NaOH and urea molecule
Key, by being self-assembly of urea-NaOH- cellulose between small solvent molecule and cellulose macromolecule under low temperature induction effect
Inclusion compound, so the addition of alkalinuria promotes the dissolution of cellulose.Meanwhile sodium hydroxide/the urea formed in subzero environment
Hydrate can be easily inserted into the interlayer region of graphene, and be attached in host layer, to destroy original hydrogen bond net
Network forms new hydrogen bond network, realizes the removing layer by layer of graphene；The presence of cellulose in the solution to be stripped
Graphene no longer reunite again, while cellulose surface be rich in polarity oxygen-containing group, can with graphene occur hydrogen bond action
With the noncovalent interactions such as electrostatic force, graphene is removed layer by layer, improves the dispersibility of graphene.The alkalinuria of cellulose is molten
Liquid is used to dispersed graphite alkene, this is a quantum jump of the invention.
2, in conductive film prepared by the present invention, scattered graphene and cellulose are formed surely under the action of crosslinking agent
Fixed cross-linked structure can give full play to the electric conductivity of graphene, improve the mobility of electronics, while also additional imparting conductive thin
Film constructs the multi-functional conductive film of high transparency with excellent anti-microbial property, hot water resistance and antistatic property, more function
Energy transparent conductive film can be widely applied on the display, flexible solar battery, photoelectric material of electronic product.
3, in all techniques of the invention, it is not directed to any high temperature link, securely and reliably；The present invention is shelled using low temperature
From facilitating the dispersion that alkalinuria generates the more advantageous graphene of new hydrogen bond between graphene layer.
4, the present invention does not take the subsequent techniques such as alkalinuria dialysis after dissolving cellulose solution, while this alkalinuria is also next
It plays a key effect in step separation graphene, significantly reduces experimental cost；Zero surfactant-dispersed graphene, it is environmentally friendly
Also reduce cost simultaneously, the later period sensor impurity of preparation is less, does not need exacting terms and can achieve the goal reducing
While cost secondary pollution will not be caused to environment；The addition of crosslinking agent keeps the combination of graphene and cellulose stronger
To enhance the mechanical property of composite membrane.
5, the present invention directly extracts the conductive film of cellulose and the compound preparation of graphene from the natural plants such as cotton, fiber crops, no
Flexibility, the transparency and conducting function are only assigned, also greatly and is reduced costs, is had and utilize large-scale application；It is selected simultaneously
Conductive graphene and the conductive film of biodegradable cellulose preparation will not cause secondary pollution and be conducive to environment
It recycles.
Specific embodiment
The present invention will be further described with reference to the examples below.
Embodiment 1
1) cellulose-graphene solution preparation:
It takes 3g cotton to be added in 97g alkalinuria solution, freezes 1h under the conditions of -15 DEG C；Persistently stirring 30min thaws, centrifugation
(4500rpm, 10min) obtains cellulose solution.30min is stirred under the conditions of -15 DEG C after adding 0.01g graphene.
2) cellulose gel-Graphene gel preparation:
By 1.6g N, N- methylene-bisacrylamide is added in 100ml cellulose-graphene solution, is warming up to 30-60 DEG C
1h is stirred, gel is formed under 30 DEG C of water bath condition, is replaced in deionized water to pH=7.
3) cellulose-graphene film preparation:
Film is made at method by hot-forming in cellulose-Graphene gel.Hot press pressure is 50pa, time
1h, temperature 60 C obtain transparent cellulose-graphene film.
Embodiment 2
1) cellulose-graphene solution preparation:
It takes 3g cotton to be added in 97g alkalinuria solution, freezes 1h under the conditions of -15 DEG C；Persistently stirring 30min thaws, centrifugation
(4500rpm, 10min) obtains cellulose solution.30min is stirred under the conditions of -15 DEG C after adding 0.01g graphene.
2) cellulose gel-Graphene gel preparation:
2g glutaraldehyde is added in 100ml cellulose-graphene solution, 40 DEG C of stirring 1h are warming up to, in 40 DEG C of water-bath
Under the conditions of form gel, replaced in deionized water to pH=7.
3) cellulose-graphene film preparation:
Film is made at method by hot-forming in cellulose-Graphene gel.Hot press pressure is 80pa, time
1.5h, temperature 60 C obtain transparent cellulose-graphene film.
Embodiment 3
1) cellulose-graphene solution preparation:
It takes 3g cotton to be added in 97g alkalinuria solution, freezes 1.5h under the conditions of -12 DEG C；Persistently stirring 30min thaws, from
The heart (5000rpm, 10min) obtains cellulose solution.30min is stirred under the conditions of -12 DEG C after adding 0.01g graphene.
2) cellulose gel-Graphene gel preparation:
2g epoxychloropropane is added in 100ml cellulose-graphene solution, 60 DEG C of stirring 1h are warming up to, at 30 DEG C
Gel is formed under water bath condition, is replaced in deionized water to pH=7.
3) cellulose-graphene film preparation:
Film is made at method by hot-forming in cellulose-Graphene gel.Hot press pressure is 50pa, time
2h, temperature 60 C obtain transparent cellulose-graphene film.
Embodiment 4
1) cellulose-graphene solution preparation:
It takes 3g cotton to be added in 97g alkalinuria solution, freezes 2h under the conditions of -12 DEG C；Persistently stirring 30min thaws, centrifugation
(5000rpm, 10min) obtains cellulose solution.30min is stirred under the conditions of -20 DEG C after adding 0.01g graphene.
2) cellulose gel-Graphene gel preparation:
2g cumyl peroxide is added in 100ml cellulose-graphene solution, 60 DEG C of stirring 1h are warming up to, 30
DEG C water bath condition under form gel, replaced in deionized water to pH=7.
3) cellulose-graphene film preparation:
Film is made at method by hot-forming in cellulose-Graphene gel.Hot press pressure is 50pa, time
2h, temperature 60 C obtain transparent cellulose-graphene film.
Experimental result
It is of the invention that the experimental results are shown inthe following table:
| Embodiment | Crosslinking agent | Strongly (mpa) | Light transmittance (%) | Resistivity (Ω m) |
| 1 | N,N methylene bis acrylamide | 3.56 | 90 | 305.44 |
| 2 | Glutaraldehyde | 4.41 | 80 | 405.15 |
| 3 | Epoxychloropropane | 5.68 | 83 | 389.74 |
| 4 | Cumyl peroxide | 6.46 | 62 | 588.64 |
By above table, it can be seen that, cellulose-graphene film that the method for the present invention is prepared has excellent saturating
Optical property, mechanical property outstanding and good electric conductivity.Transparency cellulose-graphene prepared by the embodiment of the present invention 1
The light transmittance of film is close to glass (light transmittance=90% of simple glass), the light transmittance with superelevation, and can be in proof strength
While with certain flexibility, can be applied to the display of electronic product, on thin property solar battery and photoelectric material.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field；In the present invention
Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention
Technical spirit any simple modification, change and equivalent transformation to the above embodiments, still fall within the technology of the present invention side
The protection scope of case.
Claims (7)
1. a kind of cellulose-graphene composite transparent conductive film preparation method, which comprises the following steps:
(1) graphene-cellulose solution preparation: 0.01~0.05g graphene is added in 100mL cellulose solution, stirring
After 10~60min, -10~-20 DEG C of progress low temperature removings obtain graphene-cellulose solution；
(2) graphene-cellulose gel preparation: crosslinking agent being added in the graphene-cellulose solution of step (1), heating
To 30~60 DEG C of 0.5~1h of stirring, pour to form graphene-cellulose gel under 20~60 DEG C of water bath condition, spend from
Sub- water washing is to pH=7；
(3) graphene-cellulose gel of step (2) is passed through into hot-forming rear acquisition graphene-cellulose membrane.
2. a kind of preparation method of cellulose-graphene composite transparent conductive film according to claim 1, feature exist
In the cellulose solution is the cellulose alkalinuria solution obtained by cellulose and alkalinuria solution mixed preparing, wherein cellulose
With the proportion of alkalinuria solution are as follows: 2~5:95~98.
3. a kind of preparation method of cellulose-graphene composite transparent conductive film according to claim 1, feature exist
In the alkalinuria solution is obtained by sodium hydroxide, urea and water mixed preparing, wherein the mass ratio of sodium hydroxide, urea and water
For 7:12:81.
4. a kind of preparation method of cellulose-graphene composite transparent conductive film according to claim 1, feature exist
In the low temperature splitting time of the step (1) is 10~60min.
5. a kind of preparation method of cellulose-graphene composite transparent conductive film according to claim 1, feature exist
In crosslinking agent is N, N- methylene-bisacrylamide, epoxychloropropane, cumyl peroxide, glutaraldehyde in the step (2)
One of, dosage of crosslinking agent 1.5-2wt%；Cellulose-graphene solution pours with a thickness of 3mm-8mm.
6. a kind of preparation method of cellulose-graphene composite transparent conductive film according to claim 1, feature exist
In hot-forming process conditions in the step (3) are as follows: hot pressing time 0.5-5h, temperature are 30-100 DEG C, and pressure is
20-100pa。
7. a kind of preparation method of cellulose-graphene composite transparent conductive film according to claim 1, feature exist
In the cellulose-graphene composite transparent conductive film being prepared using any preparation method of claim 1-6.
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| CN112143041A (en) * | 2020-09-04 | 2020-12-29 | 五邑大学 | Elementary sequence structured cellulose-based nano-fluid ionic conductor material, and preparation method and application thereof |
| CN113096885A (en) * | 2021-04-07 | 2021-07-09 | 宁波龙圣新材料科技有限公司 | Preparation method of low-resistance high-transparency conductive film |
| CN114854062A (en) * | 2022-06-10 | 2022-08-05 | 南京理工大学 | Preparation method of regenerated cellulose/graphene nanosheet membrane |
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