CN104627977B - Graphene oxide reinforced composite carbon nanopaper and production method thereof - Google Patents
Graphene oxide reinforced composite carbon nanopaper and production method thereof Download PDFInfo
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- CN104627977B CN104627977B CN201310548650.5A CN201310548650A CN104627977B CN 104627977 B CN104627977 B CN 104627977B CN 201310548650 A CN201310548650 A CN 201310548650A CN 104627977 B CN104627977 B CN 104627977B
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Abstract
The invention discloses a graphene oxide reinforced composite carbon nanopaper and a production method thereof. The above carbon paper includes: a carbon nanotube substrate including a skeleton network mainly formed by carbon nanotubes; and at least an enhanced network for connecting the carbon nanotubes in the skeleton network, wherein the enhanced network is mainly formed by graphene oxide dispersed in the skeleton network. The production method comprises the following steps: uniformly mixing a carbon nanotube dispersion with a graphite oxide graphene dispersion filtering to form a film, and peeling the formed film from a substrate filter film in order to obtain a target product. The composite carbon nanopaper has greatly improved mechanical properties, has no apparent loss of the excellent electrical conductivity or thermal conductivity, fully solves the problem of poor mechanical strength of present carbon tube nanopaper, and has the characteristics of electrical conduction, thermal conduction, light weight, flexibility and high efficiency. The production method has the advantages of simplicity, easy operation, good controllability, low cost and wide application prospect.
Description
Technical field
The present invention relates to a kind of paper-like material based on formation such as CNTs, increased by graphene oxide particularly to one kind
Composite nanometer carbon paper of strong carbon nanotube paper and preparation method thereof, belongs to nano-carbon material preparing technical field.
Background technology
CNT has excellent mechanics, heat conduction and electric conductivity, has been widely used in recent years and electronics device
Part and field of compound material.And CNT overcome its have to rely on the array of substrate can self supporting structure, for example public
The number of opening is the method preparing carbon nanotube paper by dispersion liquid sucking filtration described in application for a patent for invention of CN 102351165 A,
Have been realized in the preparation of large area freestanding carbon nanotube paper.At present, carbon nanotube paper has been widely used in sensing
The fields such as device, artificial-muscle, ultracapacitor, lithium ion battery, polymer matrix composites.However, in carbon nanotube paper, carbon
It is mutually to be tangled connection by van der Waals interaction between nanotube, pipe intermolecular forces are weak, and between CNT and CNT
Contact resistance and thermal contact resistance are big, cause the excellent mechanical property of CNT itself, conductive and heat conductivility in CNT
Do not embody well in paper.The tensile break strength of single CNT is 110GPa, and carbon nanotube paper
Mechanical strength only has less than 10MPa, and this makes the extensive application of carbon nanotube paper receive serious restriction.For overcoming carbon nanometer
The deficiency of pipe paper mechanical strength difference, researchers develop and modify using to functionalization, improve between CNT
Active force, realize the method for the self-crosslinking between the CNT mechanical strength to improve carbon nanotube paper, but general adopts
Functional modification is required for being acted on and being realized using the strong acid of severe corrosive or highly basic, and this causes certain journey to the structure of CNT
The destruction of degree, causes the mechanical strength improvement of the carbon nanotube paper of final preparation limited, simultaneously its conductive and heat conductivility
Significantly lose.
Content of the invention
Present invention is primarily targeted at for the deficiency such as existing carbon nanotube paper mechanical strength difference, provide a kind of by aoxidizing
Graphene strengthens the composite nanometer carbon paper of carbon nanotube paper, and it passes through the functional group of surface of graphene oxide, and CNT is mutual
Connect, constitute in carbon nanotube paper and strengthen network, thus the mechanical property of carbon nanotube paper is significantly increased.
For achieving the above object, present invention employs following technical scheme：
A kind of enhanced composite nanometer carbon paper of graphene oxide, including：
CNT matrix, including the back bone network mainly being formed by CNT, and,
At least in order to by interconnective for the CNT in described back bone network enhancing network, described enhancing network is main
It is made up of the graphene oxide being dispersed in described back bone network；
And, it is 0.01 ~ 1 that described composite nanometer carbon paper comprises mass ratio：1 graphene oxide and CNT.
As more one of preferred embodiment, the enhanced composite nanometer carbon paper of described graphene oxide comprises 0.1-
50wt% graphene oxide.
Further, the thickness of described composite nanometer carbon paper is 1 μm of -1mm.
Further, described composite nanometer carbon paper has the organizational structure of stacking stacking form, and wherein graphite oxide
Alkene is mainly connected through π-π effect with CNT, or, also it is regarded as oxygen-containing functional group energy and the carbon of surface of graphene oxide
Some groups of nanotube surface occur chemical action to realize bonding, by CNT with CNT by graphene oxide even
Connect, form a network structure, so that carbon nanotube paper obtains excellent mechanical property.
Further, described graphene oxide can be selected for monolayer, few layer graphene oxide or a combination thereof, and not limited to this
Further, described CNT can be selected for single wall, double-walled, multi-walled carbon nano-tubes or its combination in any.
Another object of the present invention also resides in the preparation method providing a kind of enhanced composite nanometer carbon paper of graphene oxide,
Including：
After carbon nano tube dispersion liquid is uniformly mixed with graphene oxide dispersion, refilter film forming, thereafter by formation
Film is peeled off with substrate filter membrane, obtains described composite nanometer carbon paper, and described composite nanometer carbon paper includes：
CNT matrix, including the back bone network mainly being formed by CNT, and,
At least in order to by interconnective for the CNT in described back bone network enhancing network, described enhancing network is main
It is made up of the graphene oxide being dispersed in described back bone network；
And, it is 0.01 ~ 1 that described composite nanometer carbon paper comprises mass ratio：1 graphene oxide and CNT.
In this preparation method, be sufficiently mixed the scheme of absorption based on aforementioned dispersion liquid, ensure that graphene oxide with
CNT dispersed, CNT can be linked to be network by wherein relatively small number of graphene oxide sheet, thus playing
Bonding action, realizes the raising of mechanical property, overcomes the poor weak point of single carbon nanotube paper mechanical property.
As more one of preferred embodiment, described carbon nano tube dispersion liquid or described graphene oxide dispersion
Concentration is 0.05mg/ml～5mg/ml.
Further, the solvent employed in described graphene oxide dispersion or carbon nano tube dispersion liquid can be selected for water,
Any one in ethanol, isopropanol, DMF, N-Methyl pyrrolidone, ethyl acetate and chloroform or two kinds
Above combination, and not limited to this.
In the present invention, because surface of graphene oxide contains the oxygen-containing official such as substantial amounts of hydroxyl, carbonyl, carboxyl, epoxy-functional
Can roll into a ball, be easily dispersed in aforementioned solvents, and after the mixing of the dispersion liquid of CNT and graphene oxide, and graphene oxide
Presence can also assist the dispersion of CNT further.
Further, also contain dispersant in described graphene oxide dispersion or carbon nano tube dispersion liquid, described dispersion
Agent can be selected for the polymer such as polyvinyl alcohol, Polyvinylpyrrolidone, cellulose, sodium lauryl sulphate, DBSA
Any one in sodium, cetyl trimethylammonium bromide, tween 80 and TritonX -100 or two or more combinations, and not
It is limited to this.By these dispersants, graphene oxide can be promoted further dispersed with CNT.
Further, the process for dispersing in order to form described graphene oxide dispersion or carbon nano tube dispersion liquid includes grinding
Mill dispersion, ball milling dispersion, any one or two or more combinations of ultrasound wave dispersant high speed shear process for dispersing.
As more one of preferred embodiment, this preparation method also includes：By described graphene oxide dispersion with
Described carbon nano tube dispersion liquid mix and blend 1-60min, rotating speed 30rpm-300rpm, are subsequently pressed through using vacuum filter or nothing
The mode filtering coating of filter.
Further, described filter membrane can be selected for cellulose filter membrane, teflon membrane filter, nylon leaching film, polyolefin filters
Or ordinary filter paper.
As one of more typical application scheme, this preparation method may comprise steps of：
（1）Carbon nanotube dust is mixed in solvent, is dispersed through the uniform dispersion that CNT is made in agent effect；
（2）Graphene oxide powder is mixed in solvent, the uniform dispersion of graphene oxide is made in dispersion；
（3）By graphene oxide and carbon nano tube dispersion liquid mixing, agitated or ultrasonic disperse, to uniform, makes graphite oxide
Alkene sufficiently adsorbs CNT, obtains graphene oxide-carbon nano tube dispersion liquid；
（4）Pumping and filtering device carries out sucking filtration process to dispersion liquid；
（5）The composite nanometer carbon paper that graphene oxide is strengthened CNT is separated with the filter membrane in pumping and filtering device, and dries
Dry forming, obtains target product.
Postscript, the graphene oxide of the present invention can easily be obtained by ultrasonic disperse graphite oxide, and can be molten
Stable dispersion in agent, preparation is easy, low cost, and then using the technology path with CNT mixing sucking filtration, can receive in carbon
Graphene oxide is introduced in mitron paper（Its mass fraction is preferably 0.1%-50%）, CNT can be connected into network, send out
Wave collaborative reinforced effects.
Again and, the present invention can adjust prepared conveniently by the concentration controlling graphene oxide and CNT
The content of the graphene oxide in nano combined carbon paper, then in also controllable composite mechanical property and conductive capability flat
Weighing apparatus（Graphene oxide is unfavorable for the raising of material conductivity too much, and content is unfavorable for that mechanics strengthens very little）.
Summarize it, compared with prior art, advantages of the present invention at least that：
（1）The present invention adopts graphene oxide as raw material, and graphene oxide powder easily disperses to form stable oxidation
Interaction between graphene solution, and the functional group of graphene oxide and the functional group of CNT, makes CNT
Connect into network, so that the mechanical strength of the composite nanometer carbon paper of formation is had and be substantially greatly improved, fully solve existing
The problem of carbon nanotube paper mechanical strength difference, is also taking into account materials conductive, heat conduction, the efficient feature of light flexible, the present invention
Have wide application prospects in fields such as new forms of energy, advanced chemical industry, electronic device, film preparations.
（2）, it is easy to operate, controllability is good and with low cost for the preparation process is simple of composite nanometer carbon paper of the present invention.
Brief description
Fig. 1 is the preparation technology flow chart of the enhanced composite nanometer carbon paper of graphene oxide of the present invention；
Fig. 2 a is the mechanical strength collection of illustrative plates of obtained composite nanometer carbon paper in embodiment of the present invention 1-7；
Fig. 2 b is the stretch moduluses collection of illustrative plates of obtained composite nanometer carbon paper in embodiment of the present invention 1-7；
Fig. 3 a-3f is the electromicroscopic photograph of obtained composite nanometer carbon paper section in embodiment of the present invention 1-7；
Fig. 4 is the electric conductivity collection of illustrative plates of obtained composite nanometer carbon paper in embodiment of the present invention 1-7.
Specific embodiment
In view of many defects of the prior art, inventor through long-term theory research and a large amount of practice it is proposed that this
The enhanced composite nanometer carbon paper of graphene oxide of invention, also referred to as " self-supporting graphene oxide/CNT is combined and receives for it
Rice carbon paper ", this composite nanometer carbon paper is made up of graphene oxide and CNT, with CNT as back bone network, based on oxygen
CNT is connected with each other, in carbon nanotube paper by the π-π effect between graphite alkene and CNT as binding agent
Middle composition strengthens network, and final acquisition has the composite being laminated stacking organizational structure, and its mechanical property is than existing nanometer
Carbon paper is greatly improved.
This composite nanometer carbon paper has following characteristic：
The group of I, the functional group of surface of graphene oxide and carbon nano tube surface is connected with each other, so forming cross-linked network
Structure；
II, thickness and can control thickness in a few micrometers to several millimeters as needed；
III, area are more than 10 cm2, and can be controlled as needed；
CNT in IV, material, graphene oxide content controlled, it is preferred that graphene oxide account for compound
Nano-sized carbon paper weight percentage ratio 0～50%；
V, material have suitable flexibility；
VI, can self-supporting it is not necessary to rely on other substrates；
VII, can be completed using ordinary filtration.
Foregoing carbon nanotubes can be using chemical vapour deposition technique, catalysis pyrolysis, arc discharge, template or laser evaporization method
Deng in any one method make, and described CNT is SWCN, multi-walled carbon nano-tubes or Nano carbon fibers
Any one or more in dimension.
Additionally, described CNT can be the modified carbon nanometer having the groups such as carboxyl, amino, hydroxyl, fluorine or amide
Pipe is it is also possible to no modify.
Aforementioned oxidation Graphene can be prepared by any one method in chemical oxidization method, chemical vapor deposition, combustion method etc.
Form, it need not carry out any functionalization further.
Further, refering to Fig. 1, as one of wherein more typical embodiment, this self-supporting graphene oxide/carbon
Nanotube composite nanometer carbon paper can be prepared via a method which：
A. CNT dispersion：Carbon nanotube dust is mixed in solvent, is dispersed through making relatively more uniform dispersion
Liquid, can contain dispersant in aforementioned solvents, concentration in dispersion liquid for this dispersant can be according to solvent property, predetermined carbon nanometer
Depending on property of pipe degree of scatter and carbon nanotube dust etc., especially preferably 0.1-4wt%；
B. graphene oxide dispersion：Graphene oxide powder is mixed in solvent, is dispersed through making uniform dispersion liquid.
C. dispersion liquid mixing：Graphene oxide is proportionally mixed with the dispersion liquid of CNT, agitated or ultrasonic
It is dispersed to uniformly.Make graphene oxide sufficiently adsorb CNT, obtain graphene oxide-carbon nano tube dispersion liquid；
D. pumping and filtering device carries out sucking filtration process to the dispersion liquid of mixing；
E. composite nanometer carbon paper graphene oxide being strengthened CNT is separated with the filter membrane in pumping and filtering device, and dries
Molding, obtains target product.
Aforementioned solvents can be selected for water, ethanol, isopropanol, N, dinethylformamide（DMF）, N-Methyl pyrrolidone
（NMP）, ethyl acetate, any one in chloroform equal solvent, and not limited to this, and scattered method can be selected for and is not limited to height
Fast shearing, grinding, ball milling, the process for dispersing such as ultrasonic any one.
According to dispersant, then dispersant can be selected for but is not limited to polyvinyl alcohol（PVA）, Polyvinylpyrrolidone（PVP）、
The polymer such as cellulose, sodium lauryl sulphate（SDS）, dodecylbenzene sodium sulfonate（SDBS）, cetyl trimethyl bromination
Ammonium（CTAB）, tween 80, the surfactant such as TritonX -100 any one or more.
Below in conjunction with accompanying drawing and some preferred embodiments, technical scheme is elaborated.
Embodiment 1 weighs 475 mg CNT through hydrochloric acid after purification, is scattered in 1L deionized water, dispersant is
Polyvinylpyrrolidone, stirs several minutes with high-shear impeller, forms pulpous state distribution to CNT in dispersion liquid.Weigh
The graphene oxide of 25mg, is scattered in 1L deionized water, stirs several minutes with high-shear impeller, is dividing to graphene oxide
Form pulpous state distribution in dispersion liquid.The dispersion liquid of the dispersion liquid of CNT and graphene oxide is mixed, is stirred with blender
Mix several minutes and both mix homogeneously are formed stable dispersion liquid.Cellulosic filter paper is layered on the buchner funnel bottom of a diameter of 25cm
Portion, uses vacuum pump sucking filtration, makes the mixed dispersion liquid of CNT and graphene oxide uniform deposition on filter paper, will when half-dried
The composite nanometer carbon paper of graphene oxide/CNT is separated with filter paper, obtains the compound of 5% graphene oxide/CNT and receives
Rice carbon paper, its thickness is about 100 μm, obtains target product after oven drying.Its performance is as shown in figs. 2 a and 2b.Its structure
As shown in Figure 3 a.
Embodiment 2 weighs 450mg CNT through hydrochloric acid after purification, weighs the graphene oxide of 50mg, same to embodiment
1 method is prepared for the composite nanometer carbon paper that graphene oxide content is 10%.Its section structure is as shown in Figure 3 b.
Embodiment 3 weighs 425 mg CNT through hydrochloric acid after purification, weighs the graphene oxide of 75mg, with enforcement
The method of example 1 is prepared for the composite nanometer carbon paper that graphene oxide content is 15%.Its structure is as shown in Figure 3 c.
Embodiment 4 weighs 400 mg CNT through hydrochloric acid after purification, weighs the graphene oxide of 100mg, with real
The method applying example 1 is prepared for the composite nanometer carbon paper that graphene oxide content is 20%.Its structure is as shown in Figure 3 d.
Embodiment 5 weighs 350 mg CNT through hydrochloric acid after purification, weighs the graphene oxide of 150mg, with real
The method applying example 1 is prepared for the composite nanometer carbon paper that graphene oxide content is 30%.Its structure is as shown in Figure 3 e.
Embodiment 6 weighs 300 mg CNT through hydrochloric acid after purification, weighs the graphene oxide of 200mg, with real
The method applying example 1 is prepared for the composite nanometer carbon paper that graphene oxide content is 40%.
Embodiment 7 weighs 250 mg CNT through hydrochloric acid after purification, weighs the graphene oxide of 250mg, with real
The method applying example 1 is prepared for the composite nanometer carbon paper that graphene oxide content is 50%.Its structure is as illustrated in figure 3f.
The composite nanometer carbon paper of the present invention substantially improves than existing nanometer carbon paper, not only mechanical property, and nanometer
The original excellent conduction of carbon paper and heat conductivility also significantly do not lose, and fully solve existing carbon nanotube paper mechanics strong
Degree difference the problems such as, also taken into account materials conductive, heat conduction, the efficient feature of light flexible, meanwhile, its preparation process is simple it is easy to
Operation, controllability is good and with low cost.The present invention has extensively in fields such as new forms of energy, advanced chemical industry, electronic device, film preparations
General application prospect.
Described above, and the embodiment shown in drawing, can not parse is limited determines the design philosophy of the present invention.At this
Hold identical skill in bright technical field the technical thought of the present invention can be changed with various form improvement, so
Improvement and change be interpreted as belonging in protection scope of the present invention.
Claims (9)
1. a kind of enhanced composite nanometer carbon paper of graphene oxide is it is characterised in that it includes：
CNT matrix, including the back bone network mainly being formed by CNT, and,
At least in order to by interconnective for the CNT in described back bone network enhancing network, described enhancing network mainly by point
The graphene oxide being dispersed in described back bone network is constituted；
And, described composite nanometer carbon paper comprises mass ratio and is more than or equal to 0.01：1 and be less than 1：1 graphene oxide and carbon
Nanotube, described composite nanometer carbon paper has the organizational structure of stacking stacking form, and wherein graphene oxide and carbon nanometer
Pipe mainly acts on through π-π and connecting.
2. the enhanced composite nanometer carbon paper of graphene oxide according to claim 1 is it is characterised in that it comprises 0.1-
50wt% graphene oxide.
3. the enhanced composite nanometer carbon paper of graphene oxide according to claim 1 is it is characterised in that described composite Nano
The thickness of carbon paper is 1 μm of -1mm.
4. a kind of preparation method of the enhanced composite nanometer carbon paper of graphene oxide is it is characterised in that include：
Carbon nano tube dispersion liquid is stirred 1-60min with graphene oxide dispersion, rotating speed is 30rpm-300rpm, uniformly mixes
Afterwards, refilter film forming, thereafter the film being formed and substrate filter membrane are peeled off, obtain described composite nanometer carbon paper, described composite Nano
Carbon paper includes：
CNT matrix, including the back bone network mainly being formed by CNT, and,
At least in order to by interconnective for the CNT in described back bone network enhancing network, described enhancing network mainly by point
The graphene oxide being dispersed in described back bone network is constituted；
And, described composite nanometer carbon paper comprises mass ratio and is more than or equal to 0.01：1 and be less than 1：1 graphene oxide and carbon
Nanotube.
5. according to claim 4 the preparation method of the enhanced composite nanometer carbon paper of graphene oxide it is characterised in that described
The concentration of carbon nano tube dispersion liquid or described graphene oxide dispersion is 0.05mg/ml～5mg/ml.
6. according to claim 4 the preparation method of the enhanced composite nanometer carbon paper of graphene oxide it is characterised in that described
Solvent employed in graphene oxide dispersion or carbon nano tube dispersion liquid includes water, ethanol, isopropanol, N, N- dimethyl methyl
Any one in amide, N-Methyl pyrrolidone, ethyl acetate and chloroform or two or more combinations.
7. according to claim 4 the preparation method of the enhanced composite nanometer carbon paper of graphene oxide it is characterised in that described
Also dispersant is contained, described dispersant includes polyvinyl alcohol, polyethylene in graphene oxide dispersion or carbon nano tube dispersion liquid
Ketopyrrolidine, cellulose, sodium lauryl sulphate, dodecylbenzene sodium sulfonate, cetyl trimethylammonium bromide, tween 80
With any one in TritonX -100 or two or more combinations.
8. according to claim 4 the enhanced composite nanometer carbon paper of graphene oxide preparation method it is characterised in that its wrap
Include：After described graphene oxide dispersion is mixed homogeneously with described carbon nano tube dispersion liquid, using vacuum filter or no press
The mode filtering coating filtering.
9. according to claim 4 the preparation method of the enhanced composite nanometer carbon paper of graphene oxide it is characterised in that described
Filter membrane includes cellulose filter membrane, teflon membrane filter, nylon leaching film, polyolefin filters or ordinary filter paper.
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| CN105218841B (en) * | 2014-07-02 | 2019-03-01 | 中国科学院金属研究所 | It is a kind of by graphite to the simple preparation method of composite graphite alkene paper |
| TWI642621B (en) * | 2015-05-29 | 2018-12-01 | National Taiwan University Of Science And Technology | Composite carbon material and method of preparing the same |
| CN105502353B (en) * | 2015-12-14 | 2018-08-17 | 湖南科技大学 | A kind of coated single-layer graphene oxide/carbon mano-tube composite and preparation method thereof |
| CN106146932A (en) * | 2016-09-27 | 2016-11-23 | 钟光 | A kind of carbon nano ring protects rubber composite and preparation method thereof |
| CN106684397B (en) * | 2017-01-23 | 2019-11-01 | 中南大学 | A kind of modified carbon/carbon composite preparation method of graphene oxide |
| CN108521683B (en) * | 2018-05-15 | 2021-06-11 | 广西大学 | Nano-cellulose graphene oxide electric heating material and preparation method thereof |
| CN108658615B (en) * | 2018-06-14 | 2020-04-28 | 华南理工大学 | High-thermal-conductivity graphene-based composite film and preparation method thereof |
| CN109052371A (en) * | 2018-07-17 | 2018-12-21 | 重庆大学 | A kind of graphene oxide dispersing Nano carbon tubes solution and preparation method thereof |
| CN109273135A (en) * | 2018-10-16 | 2019-01-25 | 浙江云墨绿能科技有限公司 | A kind of graphene/carbon nano-tube conductive film and preparation method thereof |
| CN109651891A (en) * | 2018-12-29 | 2019-04-19 | 宁波石墨烯创新中心有限公司 | A kind of graphene water-based composition, preparation method and graphene water-soluble conducting ink |
| CN110317582A (en) * | 2019-07-03 | 2019-10-11 | 桂林理工大学 | A kind of imide derivative functionalization graphene/carbon nanotube composite heat-conducting film and preparation method thereof |
| CN110473670B (en) * | 2019-07-09 | 2021-03-09 | 广东工业大学 | Method for manufacturing nano conductive film |
| CN111640526B (en) * | 2020-06-08 | 2021-09-14 | 淮北市吉耐新材料科技有限公司 | Composite carbon nanotube conductive slurry and preparation process thereof |
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| US9455094B2 (en) * | 2011-11-18 | 2016-09-27 | William Marsh Rice University | Graphene-carbon nanotube hybrid materials and use as electrodes |
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