CN109205604A - Carbon nanotube-graphene composite material method is prepared by vapor deposited catalytic - Google Patents
Carbon nanotube-graphene composite material method is prepared by vapor deposited catalytic Download PDFInfo
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- CN109205604A CN109205604A CN201710552096.6A CN201710552096A CN109205604A CN 109205604 A CN109205604 A CN 109205604A CN 201710552096 A CN201710552096 A CN 201710552096A CN 109205604 A CN109205604 A CN 109205604A
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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Abstract
The present invention, which is disclosed, prepares carbon nanotube-graphene composite material method by vapor deposited catalytic, graphene and ferrocene are sealed in stainless steel cauldron, by heating up and cooling down, so that catalyst ferrocene is uniformly adhered to the surface of graphene, it is placed in tube furnace again, passes through CVD growth carbon nanotube；Prepare carbon nanotube-graphene composite material.It can be seen that the evengranular attachment of ferrocene on the surface of graphene by scanning electron microscope and transmission electron microscope, particle size is in 15~30nm or so.The composite material of preparation, carbon nanotube are equably grown between graphene layer.Since the method for this supported catalyst is by the way that graphene to be placed in the steam of ferrocene, come into full contact with graphene with catalyst, so as to so that catalyst is uniformly adhered on inside and outside graphene surface, to carry out basis to prepare excellent composite material.
Description
Technical field
The present invention relates to a kind of new methods for preparing carbon composite, relate in particular to a kind of by vapor deposition load
Catalyst, the method for preparing carbon nano tube/graphene composite material.
Background technique
Carbon be present in nature with the mankind are most closely related, one of most important element, it has multiplicity
Electron orbit characteristic (sp, sp2、sp3Hydridization), sp in addition2Anisotropy and cause crystal anisotropy and its arrangement it is each
Anisotropy, therefore there is miscellaneous property with the carbon material that carbon is unique constitution element, and new carbon phase and new
Type carbon material is also constantly found and is manually made.The carbon material of graphene and carbon nanotube as nano-scale has super large
Specific surface area, excellent mechanical performance, the conduction of superelevation and heating conduction.It just attracts tremendous attention from being found they.Preparation
Graphene/carbon nanotube composite material can produce synergistic effect, enhance its various performance, to make this compound
Material has great application prospect in many fields.Therefore, preparation carbon nano tube/graphene composite material becomes grinding for people
Study carefully emphasis, the disclosure or authorization of many similar patents also occurs.State Intellectual Property Office of the People's Republic of China's Publication No.
The patents of invention such as CN104852021A, CN103832996A, CN106241782A, CN103725263A, which disclose, prepares graphite
Alkene/carbon nano tube compound material method.But patent of invention described above is essentially all by existing graphene and carbon nanometer
Pipe ultrasonic disperse or mechanical lapping mixing in the liquid phase, prepares composite material.On the one hand this method not can guarantee graphene
Uniform with carbon nanotube mixes, and two kinds of materials are mixed simply by physical action, are not combined well, from
It and not can guarantee the performance of composite material.Therefore, existing patent of invention Graphene/carbon nanotube composite material obtained
Requirement is unable to satisfy in terms of uniformly compound and good combination.
Summary of the invention
It is an object of the invention to overcome deficiency in the prior art, provides and carbon nanometer is prepared by vapor deposited catalytic
Pipe-graphene composite material method, by the method for novel supported catalyst, to prepare carbon nano tube/graphene
Composite material.
Technical purpose of the invention is achieved by following technical proposals:
By vapor deposited catalytic prepare carbon nanotube-graphene composite material method, as steps described below into
Row:
Step 1, catalyst ferrocene and graphene are separately placed in reaction kettle, are passed through inertia after sealing into reaction kettle
Protective gas, to exclude air in reaction kettle；It is warming up to 200-260 degrees Celsius and keeps the temperature, cooled to room temperature 20-25 is taken the photograph
Family name's degree obtains the graphene of attached catalyst ferrocene；
In step 1, inert protective gas be nitrogen, helium or argon gas, into reaction kettle circulation be passed through 3-5 times it is lazy
Property protective gas, to drain air in kettle.
In step 1,200-are warming up to from 20-25 degrees Celsius of room temperature with 5-10 degrees Celsius per minute of heating rate
260 degrees Celsius, preferably 250-260 degrees Celsius keep the temperature at least 1 hour, preferably 3-5 hours.
In step 1, the quality of ferrocene is 10~20 times, preferably 10-15 times of graphene quality.
Step 2, the graphene of attached catalyst ferrocene prepared by step 1 is placed in tube furnace, it will by CVD method
Phase carbon source solution is injected into tube furnace, and the carbon atom after carbon source cracking is on the surface of graphene under the action of catalyst, in stone
Black alkene surface grows carbon nanotube, forms carbon nanotube-graphene composite material in situ, i.e., the attachment prepared step 1
The graphene of catalyst ferrocene is placed in tube furnace, from 5-10 degrees Celsius per minute of room temperature of speed in inert protective gas
Degree is warming up to 800-900 degrees Celsius and keeps the temperature, and adjusting inert protective gas flow is 500-600sccm, is passed through hydrogen flowing quantity
For 50-150sccm, carbon source solution is injected into tube furnace by syringe and is reacted, protects gas in inertia after reaction
20-25 degrees Celsius of room temperature are cooled to the furnace under body protection, obtain Graphene/carbon nanotube composite material.
In step 2, phase carbon source solution is made of ethyl alcohol, dimethylbenzene and ethylenediamine, ethyl alcohol, dimethylbenzene and ethylenediamine
Mass ratio is 5:5:2.
In step 2, adjusting inert protective gas flow is 550-600sccm, and being passed through hydrogen flowing quantity is 50-
100sccm。
In step 2, injection speed is 10-30ml/h, at the uniform velocity 5-30min of injection, i.e., under 800-900 degrees Celsius
5~30min of heat preservation growth.
In step 2, inert protective gas is nitrogen, helium or argon gas.
In the technical solution of the present invention, graphene and ferrocene are sealed in stainless steel cauldron, the fusing point of ferrocene is
172~174 DEG C, boiling point is 249 DEG C, and will not all decompose within 400 DEG C.At high temperature, ferrocene is formed in a kettle
High steam comes into full contact with graphene；After temperature reduces, ferrocene cooling is recrystallized, and is uniformly adhered to graphene
Surface obtains the graphene of uniform load catalyst ferrocene；Graphene with catalyst is placed in tube furnace, is passed through
CVD growth carbon nanotube；Prepare carbon nano tube/graphene composite material.
Compared with prior art, the present invention using graphene surface in-situ growing carbon nano tube successfully prepare graphene/
Carbon nano tube compound material.By the cooling in ferrocene steam by graphene, so that ferrocene is deposited to graphene surface, formed
The graphene of uniform load catalyst, then by CVD method, the injection of liquid carbon source is in situ raw on the surface of graphene such as in tube furnace
Long carbon nanotube, prepares Graphene/carbon nanotube composite material.Present invention obtains Graphene/carbon nanotube composite material,
This material be by carbon nanotube homoepitaxial on the surface of graphene, be combined together carbon nanotube well with graphene,
The very big specific surface area of composite material, excellent conduction and heating conduction simultaneously.
Detailed description of the invention
Fig. 1 is the electron scanning micrograph (1) of the graphene surface uniform load catalyst prepared in the present invention.
Fig. 2 is the electron scanning micrograph (2) of the graphene surface uniform load catalyst prepared in the present invention.
Fig. 3 is the transmission electron microscope photo (1) of the graphene surface uniform load catalyst prepared in the present invention.
Fig. 4 is the transmission electron microscope photo (2) of the graphene surface uniform load catalyst prepared in the present invention.
Fig. 5 is the electron scanning micrograph (1) of the Graphene/carbon nanotube composite material prepared in the present invention.
Fig. 6 is the electron scanning micrograph (2) of the Graphene/carbon nanotube composite material prepared in the present invention.
Specific embodiment
The embodiment of the present invention is given below, is to further explanation of the invention.It is not intended to limit the scope of the invention.
Embodiment 1
(1) ferrocene for weighing 200mg is placed in stainless steel cauldron, and the graphene for weighing 10mg is placed in small silica crucible
In, it is placed into stainless steel cauldron, closes reaction kettle and seal and tighten, argon gas is slowly then passed through by intake valve, recycle
It is passed through three times, drains air in kettle, finally tighten intake valve and air outlet valve.It will be placed in heating mantle in reaction kettle, with per minute
10 degrees Celsius of speed is warming up to 260 DEG C of temperature, keeps the temperature 3h.After being naturally cooling to 20-25 degrees Celsius of room temperature, reaction kettle is opened,
Obtain the graphene of attached catalyst ferrocene.
(2) ethyl alcohol, dimethylbenzene and ethylenediamine are configured to mixed solution as carbon source solution using mass ratio 5:5:2.
(3) graphene with catalyst is placed in porcelain boat, is placed in quartz ampoule middle position, is warming up under argon gas protection
860 DEG C, heating rate is 10 DEG C/min, after rising to 860 DEG C, is passed through hydrogen 100sccm, and adjusting argon flow is 500sccm, is led to
It crosses syringe and injects carbon source into tube furnace, injection speed 15ml/h injects 15min, after reaction under protection of argon gas
It cools to room temperature with the furnace, obtains Graphene/carbon nanotube composite material.
Embodiment 2
(1) ferrocene for weighing 150mg is placed in stainless steel cauldron, and the graphene for weighing 10mg is placed in small silica crucible
In, it is placed into stainless steel cauldron, closes reaction kettle and seal and tighten, argon gas is slowly then passed through by intake valve, recycle
It is passed through three times, drains air in kettle, finally tighten intake valve and air outlet valve.It will be placed in heating mantle in reaction kettle, with per minute
10 degrees Celsius of speed is warming up to 250 DEG C of temperature, keeps the temperature 5h.After being naturally cooling to 20-25 degrees Celsius of room temperature, reaction kettle is opened,
Obtain the graphene of attached catalyst.
(2) ethyl alcohol, dimethylbenzene and ethylenediamine are configured to mixed solution as carbon source solution using mass ratio 5:5:2.
(3) graphene with catalyst is placed in porcelain boat, is placed in quartz ampoule middle position, is warming up under argon gas protection
850 DEG C, heating rate is 10 DEG C/min, after rising to 850 DEG C, is passed through hydrogen 100sccm, and adjusting argon flow is 600sccm, is led to
It crosses syringe and injects carbon source into tube furnace, injection speed 15ml/h injects 15min, after reaction under protection of argon gas
It cools to room temperature with the furnace, obtains Graphene/carbon nanotube composite material.
Embodiment 3
(1) ferrocene for weighing 100mg is placed in stainless steel cauldron, and the graphene for weighing 10mg is placed in small silica crucible
In, it is placed into stainless steel cauldron, closes reaction kettle and seal and tighten, argon gas is slowly then passed through by intake valve, recycle
It is passed through three times, drains air in kettle, finally tighten intake valve and air outlet valve.It will be placed in heating mantle in reaction kettle, with per minute 5
Degree Celsius speed be warming up to 200 DEG C of temperature, keep the temperature 6h.After being naturally cooling to 20-25 degrees Celsius of room temperature, reaction kettle is opened, is obtained
To the graphene of attached catalyst.
(2) ethyl alcohol, dimethylbenzene and ethylenediamine are configured to mixed solution as carbon source solution using mass ratio 5:5:2.
(3) graphene with catalyst is placed in porcelain boat, is placed in quartz ampoule middle position, is warming up under argon gas protection
860 DEG C, heating rate is 10 DEG C/min, after rising to 860 DEG C, is passed through hydrogen 150sccm, and adjusting argon flow is 500sccm, is led to
Cross syringe and inject carbon source into tube furnace, injection speed 30ml/h injects 5min, after reaction under protection of argon gas with
Furnace is cooled to room temperature.Obtain Graphene/carbon nanotube composite material.
Embodiment 4
(1) ferrocene for weighing 150mg is placed in stainless steel cauldron, and the graphene for weighing 10mg is placed in small silica crucible
In, it is also placed into stainless steel cauldron, closes reaction kettle and seal and tighten, argon gas is slowly then passed through by intake valve, is followed
Ring is passed through three times, is drained air in kettle, is finally tightened intake valve and air outlet valve.It will be placed in heating mantle in reaction kettle, with every point
The speed that 10 degrees Celsius of clock is warming up to 220 DEG C of temperature, keeps the temperature 2h.After being naturally cooling to 20-25 degrees Celsius of room temperature, reaction is opened
Kettle obtains the graphene of attached catalyst.
(2) ethyl alcohol, dimethylbenzene and ethylenediamine are configured to mixed solution as carbon source solution using mass ratio 5:5:2.
(3) graphene with catalyst is placed in porcelain boat, is placed in quartz ampoule middle position, is warming up under argon gas protection
860 DEG C, heating rate is 10 DEG C/min, after rising to 860 DEG C, is passed through hydrogen 150sccm, and adjusting argon flow is 550sccm, is led to
It crosses syringe and injects carbon source into tube furnace, injection speed 20ml/h injects 15min, after reaction under protection of argon gas
Cool to room temperature with the furnace.Obtain Graphene/carbon nanotube composite material.
Embodiment 5
(1) ferrocene for weighing 200mg is placed in stainless steel cauldron, and the graphene for weighing 10mg is placed in small silica crucible
In, it is also placed into stainless steel cauldron, closes reaction kettle and seal and tighten, argon gas is slowly then passed through by intake valve, is followed
Ring is passed through three times, is drained air in kettle, is finally tightened intake valve and air outlet valve.It will be placed in heating mantle in reaction kettle, with every point
The speed that 5 degrees Celsius of clock is warming up to 250 DEG C of temperature, keeps the temperature 2h.After being naturally cooling to 20-25 degrees Celsius of room temperature, reaction is opened
Kettle obtains the graphene of attached catalyst.
(2) ethyl alcohol, dimethylbenzene and ethylenediamine are configured to mixed solution as carbon source solution using mass ratio 5:5:2.
(3) graphene with catalyst is placed in porcelain boat, is placed in quartz ampoule middle position, is warming up under argon gas protection
860 DEG C, heating rate is 10 DEG C/min, after rising to 860 DEG C, is passed through hydrogen 100sccm, and adjusting argon flow is 500sccm, is led to
It crosses syringe and injects carbon source into tube furnace, injection speed 15ml/h injects 30min, after reaction under protection of argon gas
Cool to room temperature with the furnace.Obtain Graphene/carbon nanotube composite material.
Embodiment 6
(1) ferrocene for weighing 180mg is placed in stainless steel cauldron, and the graphene for weighing 10mg is placed in small silica crucible
In, it is also placed into stainless steel cauldron, closes reaction kettle and seal and tighten, argon gas is slowly then passed through by intake valve, is followed
Ring is passed through three times, is drained air in kettle, is finally tightened intake valve and air outlet valve.It will be placed in heating mantle in reaction kettle, with every point
The speed that 10 degrees Celsius of clock is warming up to 240 DEG C of temperature, keeps the temperature 5h.After being naturally cooling to 20-25 degrees Celsius of room temperature, reaction is opened
Kettle obtains the graphene of attached catalyst.
(2) ethyl alcohol, dimethylbenzene and ethylenediamine are configured to mixed solution as carbon source solution using mass ratio 5:5:2.
(3) graphene with catalyst is placed in porcelain boat, is placed in quartz ampoule middle position, is warming up under argon gas protection
860 DEG C, heating rate is 10 DEG C/min, after rising to 860 DEG C, is passed through hydrogen 50sccm, and adjusting argon flow is 550sccm, is led to
It crosses syringe and injects carbon source into tube furnace, injection speed 10ml/h injects 10min, after reaction under protection of argon gas
Cool to room temperature with the furnace.Obtain Graphene/carbon nanotube composite material.
Content carries out parameter adjustment according to the present invention, and the preparation of composite material can be achieved.The present invention is shown above
Example property description, it should explanation, in the case where not departing from core of the invention, it is any it is simple deformation, modification or
Other skilled in the art can not spend the equivalent replacement of creative work to each fall within protection scope of the present invention.
Claims (9)
1. preparing carbon nanotube-graphene composite material method by vapor deposited catalytic, which is characterized in that under
State step progress:
Step 1, catalyst ferrocene and graphene are separately placed in reaction kettle, are passed through inertia protection after sealing into reaction kettle
Gas, to exclude air in reaction kettle；It is warming up to 200-260 degrees Celsius and keeps the temperature, cooled to room temperature 20-25 is Celsius
Degree, obtains the graphene of attached catalyst ferrocene；
Step 2, the graphene of attached catalyst ferrocene prepared by step 1 is placed in tube furnace, by CVD method by liquid phase
Carbon source solution is injected into tube furnace, and the carbon atom after carbon source cracking is on the surface of graphene under the action of catalyst, in graphene
Surface grows carbon nanotube, forms carbon nanotube-graphene composite material in situ.
2. according to claim 1 prepare carbon nanotube-graphene composite material side by vapor deposited catalytic
Method, which is characterized in that in step 2, the graphene of attached catalyst ferrocene prepared by step 1 is placed in tube furnace,
Speed in inert protective gas from 5-10 degrees Celsius per minute of room temperature is warming up to 800-900 degrees Celsius and keeps the temperature, and adjusts lazy
Property shield gas flow rate be 500-600sccm, be passed through hydrogen flowing quantity be 50-150sccm, infused by syringe into tube furnace
RaC source solution is reacted, and cools to 20-25 degrees Celsius of room temperature with the furnace under inert protective gas protection after reaction,
Obtain Graphene/carbon nanotube composite material.
3. according to claim 1 prepare carbon nanotube-graphene composite material side by vapor deposited catalytic
Method, which is characterized in that in step 1, inert protective gas is nitrogen, helium or argon gas, and circulation is passed through 3-into reaction kettle
5 inert protective gas, to drain air in kettle.
4. according to claim 1 prepare carbon nanotube-graphene composite material side by vapor deposited catalytic
Method, which is characterized in that in step 1, be warming up to 5-10 degrees Celsius per minute of heating rate from 20-25 degrees Celsius of room temperature
200-260 degrees Celsius, preferably 250-260 degrees Celsius keep the temperature at least 1 hour, preferably 3-5 hours.
5. according to claim 1 prepare carbon nanotube-graphene composite material side by vapor deposited catalytic
Method, which is characterized in that in step 1, the quality of ferrocene is 10~20 times, preferably 10-15 times of graphene quality.
6. according to claim 2 prepare carbon nanotube-graphene composite material side by vapor deposited catalytic
Method, which is characterized in that in step 2, phase carbon source solution is made of ethyl alcohol, dimethylbenzene and ethylenediamine, ethyl alcohol, dimethylbenzene and second
The mass ratio of diamines is 5:5:2.
7. according to claim 2 prepare carbon nanotube-graphene composite material side by vapor deposited catalytic
Method, which is characterized in that in step 2, adjusting inert protective gas flow is 550-600sccm, and being passed through hydrogen flowing quantity is 50-
100sccm。
8. according to claim 2 prepare carbon nanotube-graphene composite material side by vapor deposited catalytic
Method, which is characterized in that in step 2, injection speed is 10-30ml/h, at the uniform velocity 5-30min of injection, i.e., takes the photograph 800-900
5~30min of heat preservation growth under family name's degree.
9. according to claim 2 prepare carbon nanotube-graphene composite material side by vapor deposited catalytic
Method, which is characterized in that in step 2, inert protective gas is nitrogen, helium or argon gas.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110176582A (en) * | 2019-05-10 | 2019-08-27 | 天津大学 | Preparation method of dendritic graphene/carbon nanotube composite structure |
| CN111715259A (en) * | 2020-06-22 | 2020-09-29 | 西南交通大学 | Preparation method of reduced graphene oxide loaded iron-based nanoparticle composite electrocatalytic material |
| CN114068927A (en) * | 2020-08-04 | 2022-02-18 | 北京大学 | Graphene carbon nanotube composite material and preparation method thereof |
| CN115724424A (en) * | 2021-08-25 | 2023-03-03 | 天津大学 | Graphene-oriented carbon nanotube array-based oriented heat conduction and heat dissipation integrated all-carbon material |
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Application publication date: 20190115 |