CN108461177B - A kind of preparation method of the composite and flexible conductive film of carbon nanotube loaded graphene-copper nano particles - Google Patents
A kind of preparation method of the composite and flexible conductive film of carbon nanotube loaded graphene-copper nano particles Download PDFInfo
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- CN108461177B CN108461177B CN201810250732.4A CN201810250732A CN108461177B CN 108461177 B CN108461177 B CN 108461177B CN 201810250732 A CN201810250732 A CN 201810250732A CN 108461177 B CN108461177 B CN 108461177B
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C01B32/00—Carbon; Compounds thereof
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
- H01B1/026—Alloys based on copper
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
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- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/02—Single-walled nanotubes
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- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/30—Purity
Abstract
The invention discloses a kind of preparation methods of the composite and flexible conductive film of carbon nanotube loaded graphene-copper nano particles, belong to conductive film preparation and technical field of composite preparation.This method is on the basis of carbon nanotube conductive thin film well prepared in advance, using spray pyrolysis by copper salt solution, graphene oxide suspension atomization, after heat resolve on carbon nanotube conductive thin film carrier forming core, growing up generates graphene-cuprous oxide, it finally restores, obtains copper-graphite alkene-carbon nano tube flexible conductive film band.Testing result show the particle size of copper in 200nm hereinafter, and graphene-copper be uniformly distributed and be embedded on carrier；Copper-graphite alkene-carbon nano tube flexible conductive film band conductivity improves an order of magnitude, and the flexible conductive film is simple to operation with the preparation method of carbon nanotube loaded graphene-copper, does not need large scale equipment, and process flow is shorter.
Description
Technical field
The present invention relates to a kind of preparation sides of the composite and flexible conductive film of carbon nanotube loaded graphene-copper nano particles
Method belongs to conductive film preparation and technical field of composite preparation.
Background technique
With the development of economy, the demand of people increasingly diversification, the position that flexible conducting material occupies on the market
More and more important and development is rapidly.Flexible conducting material has both excellent mechanical tensility and high conduction performance, that is,
Say its stretched under biggish elongation strain (100%) and repeatedly it is up to a hundred time after electric conductivities variation and little, thus passed in flexibility
Sensor, flexible thin-film solar cell, flexible super capacitor etc. have potential applying value.
Although but carbon nanotube conductive thin film has met ductility and tensile property, in terms of conduction
Still there is the space promoted, for now, it is more preferably conductive how with relatively simple easy-operating method to prepare performance
Film is a research hotspot.
It is well known that the conductivity of copper is very high, because it contains a large amount of free electron, thus copper is added to carbon nanometer
Pipe film enhances its electric conductivity, can better meet the needs of conductive film, and graphene has good flexibility, and still
Possess very high electric conductivity, has high specific surface area, associativity can be improved.Therefore, graphene and copper are added to when simultaneously
In carbon nano-tube film, the conductivity and its flexibility of carbon nanotube can be improved, to reach common enhancing conductive film electricity
The effect of conductance.But how the two is uniformly incorporated to carbon nanotube, make its evenly dispersed, uniform deposition makes material
It is still a problem that performance, which reaches optimal performance,.
Someone deposits copper in different electroplate liquids once using carbon nano-tube film as template, the results showed that, copper can be embedded into
In carbon nano-tube film, and show that the carbon nano-tube film of this method preparation deposits the conductance of carbon/carbon-copper composite material through survey calculation
Rate reaches 1.7*105S*m-1.But such operation needs to pre-process carbon nano-tube film, that is, purifies, is sensitized, and holds very much
Carbon nano-tube film easy to damage brings certain difficulty to the operability of experiment, is difficult to control, thus to the material of preparation
Certain influence can be will cause.
Summary of the invention
The purpose of the present invention is to provide a kind of composite and flexible conductive films of carbon nanotube loaded graphene-copper nano particles
Preparation method, specifically includes the following steps:
(1) chemical vapor deposition for carbon nanotubes conductive film is used, arbitrary dimension is cut into.
(2) graphene oxide is dissolved in deionized water in the ratio of 0.1-0.2g/3000mL, ultrasonic disperse 0.2-2h,
Obtain graphene oxide suspension.
(3) mantoquita is dissolved in deionized water and obtains copper salt solution, the concentration of copper salt solution is 0.0017-0.01mol/L
Magnetic agitation is stirred for uniform (1-3min) at room temperature.
(4) graphene oxide suspension and copper salt solution are respectively poured into after mixing evenly in an atomizer, by carbon nanometer
Pipe film is fixed on tube furnace low temperature zone position after being fixed with fixture, temperature is 150-250 DEG C, the high-temperature region temperature to tube furnace
When degree rises to 400-900 DEG C, while two atomizers are opened into spray patterns, is atomized the precursor liquid droplet of generation by high-temperature region
After chemistry thermal decomposition, synthesis cuprous oxide-graphene, spreads, moves, being loaded to forming core on the carrier of low-temperature space, growing up, thus
Obtain the carrier of carbon nanotube loaded graphene-cuprous oxide nano particle.
(5) complex carrier that step (4) obtains is placed in vacuum tube furnace, leads to reducing atmosphere, reduction temperature is set
It is 250-300 DEG C, the time is that 3-8h is restored to obtain the composite and flexible conduction of carbon nanotube loaded graphene-copper nano particles
Film.
Preferably, step (1) the of the present invention carbon nanotube conductive thin film can be bent repeatedly with a thickness of 1-20 microns, electricity
Conductance is 3-8*104S/m。
Preferably, of the present invention that there are a large amount of oxygen-containing groups, there is good Solvent Solubility, graphene oxide purity
It is 99% or more, the number of plies is less than three layers.
Preferably, mantoquita described in step (3) of the present invention is copper acetate, copper stearate, copper sulphate, copper nitrate, ethylenediamine
One or more of tetraacethyl sodium copper, EDTA copper sodium are mixed to get according to arbitrary proportion.
Preferably, reducibility gas described in step (5) of the present invention be hydrogen, decompose ammonia, carbon monoxide, hydrogen with it is lazy
One of the mixed gas of property gas.
Preferably, during using chemical vapor deposition for carbon nanotubes conductive film, the carbon nanotube of selection is
One or more of single wall, double-walled or multi-walled carbon nanotube are mixed to get according to any proportion, the major diameter of carbon nanotube
Than for any draw ratio, being also possible to the carbon nanotube by being surface-treated or modifying, the purity of carbon nanotube be 95% with
On.
The beneficial effects of the present invention are:
(1) the carbon nanotube loaded graphene of the method for the invention preparation-copper conductive film band method is simple to operation,
Large scale equipment is not needed, it is cheap.
(2) graphene being prepared, copper grain diameter size are substantially at nanoscale fine grained, without other field trashes,
And graphene-copper is uniformly distributed and is embedded on carrier；Copper-graphite alkene-carbon nano tube flexible conductive film band conductivity mentions
High an order of magnitude.
Detailed description of the invention
Fig. 1 is the SEM figure of the composite conductive thin film prepared in embodiment 1；
Fig. 2 is the SEM figure of the composite conductive thin film prepared in embodiment 1.
Specific embodiment
Invention is further described in detail in the following with reference to the drawings and specific embodiments, but protection scope of the present invention is simultaneously
It is not limited to the content.
Embodiment 1
The preparation method of the carbon nanotube loaded graphene-copper nano particles of flexible conductive film described in the present embodiment, specifically
The following steps are included:
(1) carbon nanotube conductive thin film prepared by preparatory chemical vapour deposition technique is cut into the small cube of 20*20mm, is led to
It crosses cubic probe measuring resistance to measure its sheet resistance, be fixed later with fixture.
(2) it weighs using the graphene oxide 0.1g for improving the preparation of Hummers method, is dissolved in the deionized water of 3000ml
In, ultrasonic disperse 0.2h obtains graphene oxide suspension.
(3) configuration concentration is the copper acetate solution of 0.0017mol/L, and work is sufficiently stirred in magnetic stirring apparatus.
(4) atomizer is respectively poured into after stirring suspension and copper salt solution that step (2) (3) obtains
In；The carbon nano-tube film cut is fixed on to the low temperature zone position (temperature is 150 DEG C) of tube furnace with fixture, to tube furnace
When high-temperature region temperature is warming up to 400 DEG C, while two atomizers are opened into spray patterns, the precursor liquid droplet for being atomized generation passes through
Chemistry thermal decomposition in high-temperature region after being synthetically generated graphene-cuprous oxide, spreads, moves, being supported on to shape on the carrier of low-temperature space
Core is grown up, so that it is particle studded in carbon nano-tube film carrier, microscopic appearance such as Fig. 1 and 2 institute to obtain graphene-cuprous oxide
Show, copper particle is in nanometer scale as seen from the figure, and evenly dispersed and be embedded in conductive film, and the carbon on conductive film is received
Mitron and graphene are high-visible.
(5) vacuum tube is placed in carbon nano-tube film carrier by graphene-cuprous oxide that step (4) obtains is particle studded
Lead to hydrogen atmosphere in formula furnace to be restored to obtain the conductive film that graphene-copper is supported on carbon nanotube；Reducing atmosphere is argon hydrogen
Body, temperature are 250 DEG C, time 3h.
The conductive film that graphene-copper nano particles that this experiment is prepared are embedded in carbon nano-tube film passes through utilization
Cubic probe surveys its sheet resistance, and conversion obtains its conductivity；It is computed, graphene-copper nano particles of preparation are embedded in carbon nanometer
The conductivity of the conductive film of pipe film is 1.21*105 S*m-1, the conductivity of flexible conductive film of this method preparation is substantially better than
Not plus the carbon nanotube conductive film of graphene and copper.
Embodiment 2
(1) carbon nanotube conductive thin film is cut into the small cube of 20*20mm with stainless steel scissors, is surveyed by cubic probe
Resistance measures its sheet resistance, and the fixture made of copper sheet fixes later.
(2) 0.2g graphene oxide is dissolved in 3000ml deionized water, ultrasonic disperse 2h obtains the oxidation stone of brown color
Black alkene suspension.
(3) compound concentration is the copper acetate solution of 0.01mol/L, magnetic agitation 30min.
(4) suspension and copper salt solution that step (2) (3) obtains respectively are poured into an atomizer after mixing evenly respectively
In；Carbon nano-tube film is fixed on to the low temperature zone position (temperature is 250 DEG C) of tube furnace with copper fixture, to tube furnace high temperature
When area's temperature rises to 900 DEG C, two atomizers are opened into spray patterns, the drop for being atomized generation is thermally decomposed by high-temperature region chemistry
And spread, move, being supported on to forming core on the carrier of low-temperature space and grow up after generation graphene-cuprous oxide after combining, thus
Obtain the composite material that graphene-cuprous oxide nano particle is embedded in carbon nano-tube film carrier.
(5) graphene-cuprous oxide nano particle that step (4) obtains is embedded in answering for carbon nano-tube film carrier again
Condensation material is put in vacuum tube furnace, and logical CO gas is restored, and reduction temperature is 300 DEG C, and the time is 5h；Obtain stone
Black alkene-copper nano particles are embedded in the flexible conductive film of carbon nano-tube film carrier.
(6) flexibility that graphene-copper nano particles that this example is prepared are embedded in carbon nano-tube film carrier is led
Electrolemma is by surveying its sheet resistance using cubic probe, then obtaining its conductivity by conversion is 1.32*105 S*m-1。
Embodiment 3
(1) carbon nanotube conductive thin film is cut into the small cube of 20*20mm with stainless steel scissors, is surveyed by cubic probe
Sheet resistance, the fixture made of copper sheet fixes later.
(2) 0.1g graphene oxide is dissolved in 3000ml deionized water, ultrasonic disperse 1h obtains the oxidation stone of brown color
Black alkene suspension.
(3) compound concentration is the copper acetate solution of 0.003mol/L, magnetic agitation 10min.
(4) suspension and copper salt solution that step (2) (3) obtains respectively are poured into an atomizer after mixing evenly respectively
In；Carbon nano-tube film is fixed on to the low temperature zone position (temperature is 210 DEG C) of tube furnace with copper fixture, to tube furnace high temperature
When area's temperature rises to 480 DEG C, two atomizers are opened into spray patterns, the drop for being atomized generation is thermally decomposed by high-temperature region chemistry
And spread, move, being supported on to forming core on the carrier of low-temperature space and grow up after generation graphene-cuprous oxide after combining, thus
Obtain the composite material that graphene-cuprous oxide nano particle is embedded in carbon nano-tube film carrier.
(5) graphene-cuprous oxide nano particle that step (4) obtains is embedded in answering for carbon nano-tube film carrier again
Condensation material is put in vacuum tube furnace, and reduction of fractions to a common denominator solution ammonia gas is restored, and reduction temperature is 270 DEG C, and the time is 5h.Obtain stone
Black alkene-copper nano particles are embedded in the flexible conductive film of carbon nano-tube film carrier.
Graphene-copper nano particles that this example is prepared are embedded in the flexible conductive film of carbon nano-tube film carrier
By surveying its sheet resistance using cubic probe, then obtaining its conductivity by conversion is 1.18*105 S*m-1。
Embodiment 4
(1) carbon nanotube conductive thin film is cut into the small cube of 20*20mm with stainless steel scissors, is surveyed by cubic probe
Sheet resistance, the fixture made of copper sheet fixes later.
(2) 0.1g graphene oxide is dissolved in 3000ml deionized water, ultrasonic disperse 120min obtains the oxygen of brown color
Graphite alkene suspension.
(3) compound concentration is the copper acetate solution of 0.003mol/L, magnetic agitation 3min.
(4) suspension and copper salt solution that step (2) (3) obtains respectively are poured into an atomizer after mixing evenly respectively
In；Carbon nano-tube film is fixed on to the low temperature zone position (temperature is 180 DEG C) of tube furnace with copper fixture, to tube furnace high temperature
When area's temperature rises to 500 DEG C, two atomizers are opened into spray patterns, the drop for being atomized generation is thermally decomposed by high-temperature region chemistry
And spread, move, being supported on to forming core on the carrier of low-temperature space and grow up after generation graphene-cuprous oxide after combining, thus
Obtain the composite material that graphene-cuprous oxide nano particle is embedded in carbon nano-tube film carrier.
(5) graphene-cuprous oxide nano particle that step (4) obtains is embedded in answering for carbon nano-tube film carrier again
Condensation material is put in vacuum tube furnace, and logical argon hydrogen mixture is restored, and reduction temperature is 280 DEG C, and the time is 5h；Obtain stone
Black alkene-copper nano particles are embedded in the flexible conductive film of carbon nano-tube film carrier.
Graphene-copper nano particles that this example is prepared are embedded in the flexible conductive film of carbon nano-tube film carrier
By surveying its sheet resistance using cubic probe, then obtaining its conductivity by conversion is 1.2*105S*m-1；Therefore, the experimental method
The conductivity of the flexible conductive film of preparation is not substantially better than not plus graphene and copper.
Comparative experiments
Carbon nanotube conductive thin film is cut into the small cube of 20*20mm with stainless steel scissors, by utilizing cubic probe
It is that 602.30 Ω cm(survey is averaged again three times that method, which measures its sheet resistance)；It is 5.0908*10 that its conductivity is obtained after conversion4S*m-1。
Claims (5)
1. a kind of preparation method of the composite and flexible conductive film of carbon nanotube loaded graphene-copper nano particles, it is characterised in that:
Specifically includes the following steps:
(1) chemical vapor deposition for carbon nanotubes conductive film is used, required arbitrary dimension is cut into；
(2) graphene oxide is dissolved in deionized water in the ratio of 0.1-0.2g/3000mL, ultrasonic disperse 0.2-2h is obtained
Graphene oxide suspension；
(3) mantoquita is dissolved in deionized water and obtains copper salt solution, the concentration of copper salt solution is 0.0017-0.01mol/L, room temperature
Lower magnetic agitation is stirred for uniformly；
(4) graphene oxide suspension and copper salt solution are respectively poured into an atomizer after mixing evenly respectively, by carbon nanometer
Pipe film is fixed on tube furnace low temperature zone position after being fixed with fixture, temperature is 150-250 DEG C, the high-temperature region temperature to tube furnace
When degree rises to 400-900 DEG C, while two atomizers are opened into spray patterns, is atomized the precursor liquid droplet of generation by high-temperature region
After chemistry thermal decomposition, synthesis cuprous oxide-graphene, spreads, moves, being loaded to forming core on the carrier of low-temperature space, growing up, thus
Obtain the carrier of carbon nanotube loaded graphene-cuprous oxide nano particle；
(5) complex carrier that step (4) obtains is placed in vacuum tube furnace, leads to reducing atmosphere, setting reduction temperature is
250-300 DEG C, the time is that 3-8h is restored to obtain the composite and flexible conduction of carbon nanotube loaded graphene-copper nano particles
Film.
2. the preparation side of the composite and flexible conductive film of carbon nanotube loaded graphene-copper nano particles according to claim 1
Method, it is characterised in that: step (1) carbon nanotube conductive thin film can be bent repeatedly with a thickness of 1-20 microns, conductivity 3-
8*104S/m。
3. the preparation side of the composite and flexible conductive film of carbon nanotube loaded graphene-copper nano particles according to claim 1
Method, it is characterised in that: the graphene oxide purity is 99% or more, and the number of plies is less than three layers.
4. the preparation side of the composite and flexible conductive film of carbon nanotube loaded graphene-copper nano particles according to claim 1
Method, it is characterised in that: mantoquita described in step (3) is copper acetate, copper stearate, copper sulphate, copper nitrate, sodium ethylene diamine tetracetate
One or more of copper is mixed to get according to arbitrary proportion.
5. the preparation side of the composite and flexible conductive film of carbon nanotube loaded graphene-copper nano particles according to claim 1
Method, it is characterised in that: reducing atmosphere described in step (5) is hydrogen, decomposes ammonia, carbon monoxide, hydrogen and inert gas
One of mixed gas.
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| CN110686589B (en) * | 2019-10-18 | 2021-03-26 | 南京理工大学 | High-sensitivity large-strain flexible strain sensor and preparation method thereof |
| CN115124030B (en) * | 2022-08-02 | 2023-12-22 | 武汉市碳翁科技有限公司 | Method for preparing flexible self-supporting carbon nano tube film on large scale |
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| JP2015143165A (en) * | 2014-01-31 | 2015-08-06 | 株式会社日本触媒 | Metal-containing carbon nanotube and carbon nanotube film |
| CN105081312A (en) * | 2015-08-17 | 2015-11-25 | 天津大学 | Method for preparing grapheme/copper composite material by loading solid carbon source on copper powder surface in impregnation manner |
| CN106622236A (en) * | 2017-01-03 | 2017-05-10 | 昆明理工大学 | Preparation method of nanometer cuprous oxide particle-loaded type carbon nanotube-graphene material for photocatalysis |
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| JP2015143165A (en) * | 2014-01-31 | 2015-08-06 | 株式会社日本触媒 | Metal-containing carbon nanotube and carbon nanotube film |
| CN105081312A (en) * | 2015-08-17 | 2015-11-25 | 天津大学 | Method for preparing grapheme/copper composite material by loading solid carbon source on copper powder surface in impregnation manner |
| CN106622236A (en) * | 2017-01-03 | 2017-05-10 | 昆明理工大学 | Preparation method of nanometer cuprous oxide particle-loaded type carbon nanotube-graphene material for photocatalysis |
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