CN105948029A - Graphene roll/carbon nanotube composite aerogel material, preparation and application thereof - Google Patents
Graphene roll/carbon nanotube composite aerogel material, preparation and application thereof Download PDFInfo
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- CN105948029A CN105948029A CN201610301937.1A CN201610301937A CN105948029A CN 105948029 A CN105948029 A CN 105948029A CN 201610301937 A CN201610301937 A CN 201610301937A CN 105948029 A CN105948029 A CN 105948029A
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- C01P2004/00—Particle morphology
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a graphene roll/carbon nanotube composite aerogel material, preparation and application thereof. The composite material is a three-dimensional network skeleton structure composed of graphene and carbon nanotubes together. The preparation method consists of: mixing a graphene oxide dispersion solution and a carbon nanotube dispersion solution, and performing ultrasonic treatment to obtain a mixed solution, then conducting quenching in liquid nitrogen, freeze drying and carbonization, thus obtaining the composite aerogel material. The composite aerogel material can be applied as a flexible electrode or stress sensing material. According to the invention, by means of a simple liquid nitrogen quenching method, two-dimensional graphene and one-dimensional carbon nanotubes are compounded, the advantages of the two materials are brought into full play, and while graphene rolls are formed, the porous structure composite aerogel with good compression resilience can be obtained.
Description
Technical field
The invention belongs to composite aerogel and preparation thereof and application, be combined airsetting particularly to a kind of graphene roll/CNT
Glue material and preparation thereof and application.
Background technology
Graphene has the monolithic layer two-dimensional structure of uniqueness, and it is by sp2Carbon atom Hexagonal array forms.Meanwhile, Graphene has
Higher inside carrier mobility (200000cm2V-1s-1), good thermal conductivity (～5000W m-1K-1), high printing opacity
Rate (～97.7%) and theoretical specific surface area (2630m2g-1), and the mechanical strength of excellence.Therefore, Graphene extensively should
In electrochemical device.But, in actual applications, the π-π the strongest due to graphene film interlayer interacts, Graphene
Lamella is prone to again stack, and forms the structure of class graphite, and the performance making Graphene itself excellent cannot be fully used.Graphite
Alkene nanometer roll has one-dimensional tubular morphology, can pass through liquid nitrogen quenching, superactivity metal intercalation, from bottom to top high-temperature synthesis or
Graphene curling is obtained, owing to the pattern of its uniqueness can regulate the distance of interlayer by the methods such as person's nanoparticle template-mediated synthesis
Prevent the stacking between graphene sheet layer, thus effectively utilize the surface area of graphene sheet layer.
CNT has unique property such as higher carrier mobility, good electric conductivity, high-specific surface area, big L/D ratio
The fields such as energy, is widely used in sensing, energy storage device.Itself and Graphene are mixed aeroge, and carbon nanotube portion is attached
On graphene sheet layer, part is then involved in graphene roll, provides more effective transmission channel for electronics, improves
The electric conductivity of material.
Self assembly is by hydrogen bond, and π-π stacking interaction and electrostatic attraction effect obtain the hierarchical structure of physical crosslinking
A kind of effective method.The process of this self assembly is a kind of spontaneous process, and by reasonably design, self assembling process can be by
Multicomponent carries out simultaneously and does not affect the formation of product, and the structure of self assembly can give material some be different from bulk mass
Special performance, has widened its application.
Summary of the invention
The technical problem to be solved be to provide a kind of graphene roll/CNT aerogel composite and preparation thereof and
Application, preparation process of the present invention is simple, with low cost；By simple liquid nitrogen quenching method by two-dimensional graphene and one-dimensional carbon
Nanotube is combined so that both advantages are given full play to, and obtains having preferably pressure while forming graphene roll
Contract the composite aerogel of elastic loose structure.
A kind of graphene roll/CNT the aerogel composite of the present invention, it is characterised in that: described composite is: graphite
Alkene and CNT are built into the framing structure of three-dimensional network jointly, and wherein graphene roll is wrapped in CNT, simultaneously carbon nanometer
Pipe is again through between graphene sheet layer.
A kind of preparation method of the graphene roll/CNT aerogel composite of the present invention, including:
(1) graphene oxide is disperseed in deionized water, ultrasonic, obtain graphene oxide dispersion；CNT will be acidified
Dispersion is in deionized water, ultrasonic, obtains being acidified carbon nano tube dispersion liquid；
(2) by graphene oxide dispersion, acidifying carbon nano tube dispersion liquid mixing, ultrasonic, obtain mixed liquor, then at liquid nitrogen
Middle quenching, lyophilization, carbonization, obtain graphene roll/CNT aerogel composite.
In described step (1), graphene oxide is graphene oxide prepared by Hummers method；Graphene oxide dispersion dense
Degree is 4-10mg mL-1；The concentration of acidifying carbon nano tube dispersion liquid is 1-4mg mL-1。
In described step (1), acidifying CNT, is that 200mg multi-walled carbon nano-tubes joins 200mL concentrated sulphuric acid and dense nitre
The mixed liquor (volume ratio is 3:1) of acid prepares in 60-80 DEG C of reaction 1-3h.
In described step (2), graphene oxide dispersion, the volume ratio of acidifying carbon nano tube dispersion liquid are 1:1.
In described step (2), in mixed liquor, the mass ratio of graphene oxide and acidifying CNT is 8:1～2:1.
In described step (2), in liquid nitrogen, the cooling time of quenching is 10-20min.
In described step (2), lyophilization is: temperature is-30～-50 DEG C, and vacuum is 10-30Pa, and sublimation drying is
20-30h。
In described step (2), carbonization is: carbonization in noble gas, and carburizing temperature is 600-900 DEG C, and heating rate is 3-7 DEG C of min-1,
Carbonization constant temperature time is 1-3h.Preferably heating rate is 4-6 DEG C of min-1, carbonization constant temperature time is 1.5-2.5h.Described inertia
Gas is argon or nitrogen.
A kind of application of the graphene roll/CNT aerogel composite of the present invention, it is characterised in that: graphene roll/carbon nanometer
Pipe aerogel composite is as flexible electrode or the application of stress sensing material.
Graphene roll-CNT that the present invention uses the method for liquid nitrogen quenching to prepare compressive deformation excellent with rebound performance is combined gas
Gel rubber material.It is prepared raw material composition and includes: graphite oxide, multi-walled carbon nano-tubes etc..
Use the test of scanning electron microscope (SEM), load test, electrical conductivity to characterize graphene roll that the present invention obtained-
The structure and morphology of CNT aerogel composite, its result is as follows:
(1) SEM test result shows: graphene roll-CNT aerogel composite prepared in the present invention has porose
Hole structure, Graphene and CNT are built into the framing structure of three-dimensional network jointly, and graphene roll is wrapped in CNT, and
CNT is again through between graphene sheet layer simultaneously.This three-dimensional composite network not only defines hierarchical porous structure, improves
The specific surface area of material, and provide mass efficient passage for electric transmission, improve the electric conductivity of material.Quick at liquid nitrogen
Under the conditions of low temperature quenching, graphene sheet layer can curl into graphene roll, and masterpiece answered by these one-dimensional loose tubular structures
There is under with good deformation adaptability, be highly beneficial for improving material sensing sensitivity under weak deformation.See attached
Fig. 1.
(2) graphene roll prepared by the present invention-CNT pluralgel has good compression recovery performance, as in figure 2 it is shown,
After bearing the active force of own wt about 2000 times, still can be returned to original state, illustrate this material under relatively large deformation still
Initial three-dimensional conductive network structure can be kept, can be applicable to high performance flexible electrode and stress sensing material.
(3) electrical conductivity test result shows: the resistivity of pure graphene roll aeroge is 14.2 Ω cm, and adds carbon nanometer
The resistivity of the graphene roll of pipe-CNT composite aerogel is 8.6 Ω cm, and the electric conductivity of material is significantly improved.
Illustrate that the preparation-obtained material of the present invention has good electric conductivity and can be used as electrode material.
Self-assembling technique is used in graphene roll-CNT composite aerogel by the present invention, in the process forming three-dimensional network
In, CNT not only inhibits the stacking of graphene sheet layer, also provides more transmission channel for electronics, is greatly improved
The electric conductivity of material.Meanwhile, the three dimensional skeletal structure that graphene roll and CNT are mutually formed there through is composite aerogel material
Material provides good mechanical property, and has good compression recovery performance, is expected to become a kind of preferable high performance flexibility
Electrode and pressure-sensitive device material.
Graphene roll of the present invention-CNT aerogel composite utilizes strong π-π between Graphene and CNT mutual
Effect, a step can realize graphene oxide and CNT stable dispersion in aqueous by the method for simple solution blending,
Subsequently mixed solution is carried out liquid nitrogen fast low temperature quenching and then lyophilization, obtains graphene roll-carbon finally by high temperature cabonization and receive
Mitron aerogel composite.Graphene roll prepared by the present invention-CNT aerogel composite has good deformation and adapts to
Property, it is expected to become the flexible electrode of a kind of novel great prospect, strain gauge material.
Beneficial effect
(1) preparation process of the present invention is simple, environmental protection, it is easy to operation, is a kind of Green Chemistry preparation method；
(2) experimental design of the present invention is ingenious, two-dimensional graphene is carried out with one-dimensional CNT by simple liquid nitrogen quenching method
Compound so that both advantages are given full play to, and obtain that there is preferable compression and back while forming graphene roll
The composite aerogel of elastic loose structure.
(3) graphene roll prepared by the present invention-CNT composite aerogel, is expected to become the flexible electrical of a kind of novel great prospect
Pole, strain gauge material.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the graphene roll-carbon nanometer roll composite aerogel of embodiment 1 preparation；Wherein a, b, c, d represent respectively
Composite aerogel structure under different enlargement ratios.
Fig. 2 is that graphene roll-carbon nanometer roll composite aerogel (a) of embodiment 1 preparation is compressed (b) under applying stress and removes
The photo of resilience (c) after stress.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments be merely to illustrate the present invention and not
For limiting the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, those skilled in the art can
To make various changes or modifications the present invention, these equivalent form of values fall within the application appended claims limited range equally.
Embodiment 1
(1) graphite oxide is scattered in deionized water, ultrasonic obtains 4mg mL-1The graphene oxide dispersion of stable dispersion；
(2) acidifying CNT is scattered in deionized water, ultrasonic obtains 1mg mL-1Stable dispersion graphene oxide dispersion
Liquid；
(3) by 10mL 4mg mL-1Graphene oxide dispersion and 10mL 1mg mL-1Acidifying carbon nano tube dispersion liquid mixing,
Ultrasonic a period of time, form homogeneous dispersion liquid；
(4) mixed liquor of step (3) gained is placed in mould in liquid nitrogen freezing 20min；
(5) by composite lyophilization in freezer dryer of step (4) gained, lyophilization temperature is-30 DEG C, vacuum
Degree is 10Pa, and sublimation drying is 20h, forms graphene oxide volume-CNT composite aerogel；
(6) step (5) gained aeroge being carried out in nitrogen atmosphere high temperature cabonization, carburizing temperature is 700 DEG C, and heating rate is
5℃ min-1, the response time is 3h.
Embodiment 2
(1) graphite oxide is scattered in deionized water, ultrasonic obtains 8mg mL-1The graphene oxide dispersion of stable dispersion；
(2) acidifying CNT is scattered in deionized water, ultrasonic obtains 1mg mL-1Stable dispersion graphene oxide dispersion
Liquid；
(3) by 10mL 4mg mL-1Graphene oxide dispersion and 10mL 1mg mL-1Acidifying carbon nano tube dispersion liquid mixing,
Ultrasonic a period of time, form homogeneous dispersion liquid；
(4) mixed liquor of step (3) gained is placed in mould in liquid nitrogen freezing 20min；
(5) by composite lyophilization in freezer dryer of step (4) gained, lyophilization temperature is-30 DEG C, vacuum
Degree is 10Pa, and sublimation drying is 20h, forms graphene oxide volume-CNT composite aerogel；
(6) step (5) gained aeroge being carried out in nitrogen atmosphere high temperature cabonization, carburizing temperature is 700 DEG C, and heating rate is
5℃ min-1, the response time is 3h.
Embodiment 3
(1) graphite oxide is scattered in deionized water, ultrasonic obtains 4mg mL-1The graphene oxide dispersion of stable dispersion；
(2) acidifying CNT is scattered in deionized water, ultrasonic obtains 1mg mL-1Stable dispersion graphene oxide dispersion
Liquid；
(3) by 10mL 4mg mL-1Graphene oxide dispersion and 10mL 1mg mL-1Acidifying carbon nano tube dispersion liquid mixing,
Ultrasonic a period of time, form homogeneous dispersion liquid；
(4) mixed liquor of step (3) gained is placed in mould in liquid nitrogen freezing 20min；
(5) by composite lyophilization in freezer dryer of step (4) gained, lyophilization temperature is-30 DEG C, vacuum
Degree is 10Pa, and sublimation drying is 20h, forms graphene oxide volume-CNT composite aerogel；
(6) step (5) gained aeroge being carried out in nitrogen atmosphere high temperature cabonization, carburizing temperature is 800 DEG C, and heating rate is
5℃ min-1, the response time is 3h.
Claims (10)
1. graphene roll/CNT aerogel composite, it is characterised in that: described composite is: Graphene is received with carbon
Mitron is built into the framing structure of three-dimensional network jointly, and wherein graphene roll is wrapped in CNT, and CNT passes through again simultaneously
It is through between graphene sheet layer.
2. a preparation method for graphene roll as claimed in claim 1/CNT aerogel composite, including:
(1) graphene oxide is disperseed in deionized water, ultrasonic, obtain graphene oxide dispersion；CNT will be acidified
Dispersion is in deionized water, ultrasonic, obtains being acidified carbon nano tube dispersion liquid；
(2) by graphene oxide dispersion, acidifying carbon nano tube dispersion liquid mixing, ultrasonic, obtain mixed liquor, then at liquid nitrogen
Middle quenching, lyophilization, carbonization, obtain graphene roll/CNT aerogel composite.
The preparation method of a kind of graphene roll/CNT aerogel composite the most according to claim 2, it is characterised in that:
In described step (1), graphene oxide is graphene oxide prepared by Hummers method；Graphene oxide dispersion dense
Degree is 4-10mg mL-1；The concentration of acidifying carbon nano tube dispersion liquid is 1-4mg mL-1。
The preparation method of a kind of graphene roll/CNT aerogel composite the most according to claim 2, it is characterised in that:
In described step (2), graphene oxide dispersion, the volume ratio of acidifying carbon nano tube dispersion liquid are 1:1.
The preparation method of a kind of graphene roll/CNT aerogel composite the most according to claim 2, it is characterised in that:
In described step (2), in mixed liquor, the mass ratio of graphene oxide and acidifying CNT is 8:1～2:1.
The preparation method of a kind of graphene roll/CNT aerogel composite the most according to claim 2, it is characterised in that:
In described step (2), lyophilization is: temperature is-30～-50 DEG C, and vacuum is 10-30Pa, and sublimation drying is
20-30h。
The preparation method of a kind of graphene roll/CNT aerogel composite the most according to claim 2, it is characterised in that:
In described step (2), carbonization is: carbonization in noble gas, and carburizing temperature is 600-900 DEG C, and heating rate is 3-7 DEG C of min-1,
Carbonization constant temperature time is 1-3h.
The preparation method of a kind of graphene roll/CNT aerogel composite the most according to claim 7, it is characterised in that:
Described heating rate is 4-6 DEG C of min-1, carbonization time is 1.5-2.5h.
The preparation method of a kind of graphene roll/CNT aerogel composite the most according to claim 7, it is characterised in that:
Described noble gas is argon or nitrogen.
10. the application of graphene roll as claimed in claim 1/CNT aerogel composite, it is characterised in that: graphite
Alkene volume/CNT aerogel composite is as flexible electrode or the application of stress sensing material.
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| CN106531459A (en) * | 2016-10-27 | 2017-03-22 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七二研究所） | Preparation method of graphene/active carbon composite film |
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