CN106629672A - Carbon nanotube-graphene composite material and preparation method thereof - Google Patents
Carbon nanotube-graphene composite material and preparation method thereof Download PDFInfo
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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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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/02—Single-walled nanotubes
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- C01B2202/04—Nanotubes with a specific amount of walls
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/02—Single layer graphene
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- C01B2204/04—Specific amount of layers or specific thickness
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- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention relates to a carbon nanotube-graphene composite material and a preparation method thereof. The preparation method comprises the following steps: (1) preparing a graphene/template composite by using a chemical vapor deposition method; (2) dispersing the composite in deionized water, adding a mixed solution of ferric nitrate and ammonium molybdate, stirring, and dropwise adding ammonia water to obtain a mixed solution, wherein the molar ratio of the ferric nitrate to the ammonium molybdate is 1: (0.01-10), and the mass percentage concentration of the ammonia water is 25-30%; and (3) carrying out suction filtering and drying on the mixed solution, and calcining at the temperature of 300-700 DEG C to obtain a catalyst for preparing the carbon nanotube-graphene composite material. In the preparation method, two-time chemical vapor deposition processes are utilized, and structure features and nitrating situation of graphene and carbon nanotubes are controlled.
Description
Technical field
The present invention relates to material with carbon element preparing technical field, more particularly to a kind of carbon nanometer tube-graphene composite material and its
Preparation method.
Background technology
CNT (CNT) and Graphene (Graphene) found respectively at 1991 and 2004 by people, and
Just get most of the attention always from that day that they are found.CNT is a kind of One-dimensional Quantum material with special construction,
Its radial dimension can reach nanoscale, and axial dimension is micron order, and the two ends of pipe are typically all sealed, therefore it has very big strong
Degree, while huge draw ratio is expected to make it be fabricated to the fabulous carbon fiber of toughness.Graphene be one kind by carbon atom with sp2It is miscellaneous
Change the flat film of the hexangle type in honeycomb lattice of track composition, the two-dimentional material with carbon element of only one of which carbon atom thickness, zero dimension is rich
Strangle the carbon nanomaterial family that alkene, one-dimensional CNT, two-dimensional graphene have collectively constituted backbone, and can be between them
Conversion in form.
Graphene and CNT have similar property at the aspect such as electricity and mechanics, but due to structure difference, they
Also there are many differences.CNT and Graphene are respectively an excellent peacekeeping Two-dimensional Carbon materials, and they are embodied respectively
One-dimensional and two dimension anisotropy, such as electric conductivity, mechanical property and thermal conductivity, in order to combine both advantages, people
Graphene and CNT are provided commonly for into composite.Graphene and carbon nano tube compound material form tridimensional network,
By the cooperative effect between them so as to show the performance more excellent than any one homogenous material, such as preferably
The characteristics such as isotropism thermal conductivity, isotropic conductivity, three dimensions microporous network.Based on above property so that Graphene/
Carbon nano tube compound material has good at aspects such as ultracapacitor, solar cell, display, biological detection, fuel cells
Good application prospect.Carbon nanometer tube-graphene composite material is more and more applied by people so that graphene/carbon nanometer
The preparation and application of pipe composite obtains more widely paying close attention to.
Preparing the method for graphene/carbon nano-tube compound at present mainly has two kinds：One kind is mixing method, that is, by stone
Black alkene directly mixes with carbon nanotube-sample, for example；Another is direct growth method, by chemical vapor deposition processes simultaneously
Growth Graphene and CNT.In prepared by mixing method, the dispersion of CNT and Graphene is very crucial, to obtain mixing equal
Even CNT-graphene complex is relatively difficult.And in direct growth method, the ratio of CNT and Graphene is not allowed
It is easy to control, and the shape characteristic of Graphene and CNT cannot control respectively.
The content of the invention
For solve above-mentioned technical problem, it is an object of the invention to provide a kind of carbon nanometer tube-graphene composite material and its
Preparation method.By chemical vapor deposition processes twice, realization is carried out respectively to the structure and nitrating of CNT and Graphene
Control.
In order to achieve the above object, the invention provides a kind of for preparing urging for carbon nanometer tube-graphene composite material
Agent, it is prepared by following steps：
(1) by process for preparing graphenes by chemical vapour deposition/template compound；
(2) compound is disperseed to add the mixed solution of ferric nitrate and ammonium molybdate, stirring, drop in deionized water
Plus ammoniacal liquor obtains mixed solution, the ferric nitrate is 1 with the mol ratio of ammonium molybdate:(0.01-10), the quality percentage of the ammoniacal liquor
Specific concentration is 25%-30%；Preferably, the mol ratio of Fe and Mo is 1:(0.01-10)；
By the mixed solution suction filtration, drying, then calcine under 300 DEG C -700 DEG C (preferably 350 DEG C), obtain for making
The catalyst of standby carbon nanometer tube-graphene composite material.
In above-mentioned catalyst, it is preferable that step (1) template is powder, the template includes aluminum oxide, oxygen
Change the mixture of one or more in magnesium, zinc oxide, calcium oxide and silica.
In above-mentioned catalyst, it is preferable that during step (1) chemical vapor deposition：Introduce ammonia to be mixed
Nitrogen Graphene/template compound；Do not introduce ammonia and obtain not nitrogen-doped graphene/template compound.
In above-mentioned catalyst, it is preferable that contain Fe and Mo, the Fe and Mo matter in the catalyst in the catalyst
Amount percentage is 1 for the mol ratio of 0.1%-70%, Fe and Mo:(0.01-10).
The present invention also provides a kind of preparation method of carbon nanometer tube-graphene composite material, comprises the following steps：
(1) using above-mentioned catalyst, by chemical vapor deposition growth CNT；
(2) powder product is obtained after being cooled to room temperature under nitrogen or argon gas atmosphere；
(3) powder product is added in watery hydrochloric acid, stirring obtains mixed solution；
(4) by the mixed solution suction filtration, drying, carbon nanometer tube-graphene composite material is obtained.
In the preparation method of above-mentioned composite, it is preferable that the watery hydrochloric acid be 37.5% dense watery hydrochloric acid and water by
According to 1：(1-5) what mass ratio was mixed to get.
In the preparation method of above-mentioned composite, it is preferable that during step (1) chemical vapor deposition if
Introduce ammonia and obtain nitrogen doped carbon nanotube, the concentration of volume percent of the ammonia is 1%-10%；If not introducing ammonia to obtain
To not nitrogen doped carbon nanotube.
In the preparation method of above-mentioned composite, it is preferable that using the catalyst containing nitrogen-doped graphene and in chemistry
Introduce under conditions of ammonia in vapor deposition processes, obtain nitrogen-doped graphene-nitrogen doped carbon nanotube compound；Using containing nitrating
The catalyst of Graphene is not simultaneously introduced under conditions of ammonia in chemical vapor deposition processes, obtains the nitrating of nitrogen-doped graphene-not
Carbon mano-tube composite；Using introducing ammonia containing the not catalyst of nitrogen-doped graphene and in chemical vapor deposition processes
Under the conditions of, obtain not nitrogen-doped graphene-nitrogen doped carbon nanotube compound；Using containing the not catalyst of nitrogen-doped graphene and
Do not introduce under conditions of ammonia in chemical vapor deposition processes, obtain the not nitrogen doped carbon nanotube compound of nitrogen-doped graphene-not.
In the preparation method of above-mentioned composite, it is preferable that the composite of preparation includes multi-walled carbon nano-tubes-multilayer
Graphene complex, SWCN-multi-layer graphene compound, multi-walled carbon nano-tubes-few layer graphene compound and list
Wall carbon nano tube-few layer graphene compound.
The present invention can in batches prepare CNT-graphene complex, and Graphene and CNT be tightly combined, homogeneous；
The present invention, by the growth conditions for changing Graphene and CNT, controls Graphene using chemical vapor deposition processes twice
With the architectural feature and nitrating situation of CNT, and then multi-walled carbon nano-tubes-multi-layer graphene compound, single wall carbon is obtained
Nanotube-multi-layer graphene compound, multi-walled carbon nano-tubes-few layer graphene compound and SWCN-few layer graphite
Alkene compound；The nitrogen doped carbon nanotube of nitrogen-doped graphene-nitrogen doped carbon nanotube compound and nitrogen-doped graphene-not can also be obtained to answer
Compound.
Description of the drawings
Fig. 1 is the transmission electron micrograph of single-layer carbon nano-tube-single-layer graphene compound.
Fig. 2 is the transmission electron micrograph of multilayer carbon nanotube-single-layer graphene compound.
Fig. 3 is the transmission electron micrograph of nitrogen doped carbon nanotube-nitrogen-doped graphene compound.
Specific embodiment
In order to be more clearly understood to the technical characteristic of the present invention, purpose and beneficial effect, now to the skill of the present invention
Art scheme carry out it is described further below, but it is not intended that to the present invention can practical range restriction.
Embodiment 1
A kind of SWCN-single-layer graphene compound is present embodiments provided, it is through the following steps that prepare
's：
20g magnesium oxide powders are taken, in adding fluidized-bed reactor, with methane (1L/min) as carbon source, is reacted at 850 DEG C
20min, is obtained Graphene-magnesia compound, in being dispersed in deionized water, adds 3g ferric nitrates and 0.5g ammonium molybdates,
Stirring adds the ammoniacal liquor that 5mL mass percent concentrations are 25%, suction filtration, drying then to calcine 30min under conditions of 300 DEG C,
Obtain powder catalyst.
Argon gas (1L/min) is passed through in vertical reactor, the catalyst is added, methane (1L/ is passed through after being warmed up to 850 DEG C
Min), keep 30min, room temperature is cooled under an argon atmosphere, obtain powder product, be eventually adding mass fraction be 10% it is dilute
Hydrochloric acid, stirring and pickling prepares SWCN-single-layer graphene compound after suction filtration drying.
The transmission electron micrograph of the product that Fig. 1 is obtained for said process, it can be seen that there is tubulose in the visual field
The Graphene of CNT and sheet, the diameter about 1-4nm of CNT, the number of plies only has one layer, belongs to SWCN, and
The edge of Graphene also only has a solid black lines, thus it is single-layer graphene that may determine that.Therefore, what is prepared is single
Wall carbon nano tube-single-layer graphene compound.
Embodiment 2
A kind of multi-walled carbon nano-tubes-single-layer graphene compound is present embodiments provided, it is through the following steps that prepare
's：
20g magnesium oxide powders, plus fluidized bed are taken, with methane (1L/min) as carbon source, reaction 20min, prepared Graphene-
Magnesia compound, in being dispersed in deionized water, adds 20g ferric nitrates and 0.8g ammonium molybdates, stirring to add 10mL mass
The ammoniacal liquor of percent concentration 30%, 30min is calcined after suction filtration, drying under conditions of 350 DEG C, obtains powder catalyst.
Nitrogen (1L/min) is passed through in vertical reactor, the catalyst is added, 650 DEG C are warmed up to, H is passed through2(1L/
Min) 5min is reduced, ethene (1L/min) and ammonia (50mL/min) is passed through after being warmed up to 750 DEG C, 30min is kept, in nitrogen gas
Room temperature is cooled under atmosphere, black powder product is obtained, the watery hydrochloric acid that mass fraction is 15% is eventually adding, is prepared after pickling
Multi-walled carbon nano-tubes-single-layer graphene compound.
The transmission electron micrograph of the product that Fig. 2 is prepared for said process, it can be seen that larger many of wall thickness
Wall carbon nano tube, in the graphene sheet layer in Fig. 2 upper right corner, edge only has a solid black lines, it can be determined that be single-layer graphene.
Therefore, what is prepared is multi-walled carbon nano-tubes-single-layer graphene compound.
Embodiment 3
A kind of SWCN-multi-layer graphene compound is present embodiments provided, it is through the following steps that prepare
's：
20g alumina powders, plus fluidized bed are taken, with ethene (1L/min) as carbon source, 25min is reacted at 700 DEG C, made
Multi-layer graphene-alumina compound is obtained, in being dispersed in deionized water, 3g ferric nitrates and 0.8g ammonium molybdates, stirring is added
The ammoniacal liquor that 5mL mass percent concentrations are 26% is added, 30min is calcined under conditions of 350 DEG C after suction filtration, drying, obtain powder
Body catalyst.
Argon gas (1L/min) is passed through in vertical reactor, the catalyst is added, methane (1L/ is passed through after being warmed up to 850 DEG C
Min), keep 30min, be cooled to room temperature under an argon atmosphere, take out powder product, be eventually adding mass fraction be 15% it is dilute
Hydrochloric acid, stirring and pickling prepares SWCN-multi-layer graphene compound after suction filtration drying.
Embodiment 4
Present embodiments provide a kind of nitrating multi-walled carbon nano-tube-nitrogen-doped graphene compound, itself through the following steps that
Prepare：
20g magnesium oxide powders plus fluidized bed are taken, with ethene (1L/min) as carbon source, with ammonia (100mL/min) as nitrogen
Source, at 750 DEG C 20min is reacted, and nitrogen-doped graphene-magnesia compound is obtained.Then nitrogen-doped graphene-magnesia is combined
Thing disperses in deionized water, adds 20g ferric nitrates and 0.8g ammonium molybdates, and it is 28% that stirring adds 10mL mass percent concentrations
Ammoniacal liquor, suction filtration, drying after calcine 30min under conditions of 700 DEG C, obtain powder catalyst.
Nitrogen (1L/min) is passed through in vertical reactor, the catalyst is added, 650 DEG C are warmed up to, H is passed through2(1L/
Min) 5min is reduced, ethene (1L/min) and ammonia (100mL/min) is passed through after being warmed up to 750 DEG C, 30min is kept, in nitrogen
Room temperature is cooled under atmosphere, black powder product is obtained, the watery hydrochloric acid that mass fraction is 10% is eventually adding, is prepared into after pickling
To nitrating multi-walled carbon nano-tube-nitrogen-doped graphene compound.
Fig. 3 prepares the transmission electron micrograph of product for said process.The carbon in Bamboo-shaped that can be seen from figure is received
Mitron, this is the shape characteristic of typical nitrogen doped carbon nanotube.X-ray photoelectron spectroscopy test shows that sample nitrogen content is 3.5%
(atomic percent).Therefore, what is obtained is nitrating multi-walled carbon nano-tube-nitrogen-doped graphene compound.
Claims (10)
1. a kind of preparation method for preparing the catalyst of carbon nanometer tube-graphene composite material, it comprises the steps：
(1) by process for preparing graphenes by chemical vapour deposition/template compound；
(2) compound is disperseed to add the mixed solution of ferric nitrate and ammonium molybdate in deionized water, stirring is added dropwise ammonia
Water obtains mixed solution, and the ferric nitrate is 1 with the mol ratio of ammonium molybdate:(0.01-10), the mass percent of the ammoniacal liquor is dense
Spend for 25%-30%；
(3) by the mixed solution suction filtration, drying, then at 300 DEG C -700 DEG C calcine, obtain for prepare CNT -
The catalyst of graphene composite material.
2. preparation method as claimed in claim 1, wherein, in step (1), the template is powder, the template
Including the mixture of one or more in aluminum oxide, magnesia, zinc oxide, calcium oxide and silica.
3. preparation method as claimed in claim 1 or 2, wherein, in step (1), during chemical vapor deposition：Introduce
Ammonia obtains nitrogen-doped graphene/template compound；Do not introduce ammonia and obtain not nitrogen-doped graphene/template compound.
4. the preparation method any one of claim 1-3 is prepared nitrating or the not catalyst of nitrating.
5. catalyst as claimed in claim 4, wherein, Fe and Mo is contained in the catalyst, the Fe and Mo is in catalyst
In mass percent for 0.1%-70%, the Fe and Mo mol ratio be 1:(0.01-10).
6. a kind of preparation method of carbon nanometer tube-graphene composite material, it comprises the steps：
(1) using the catalyst described in claim 4 or 5, by chemical vapor deposition growth CNT；
(2) powder product is obtained after being cooled to room temperature under nitrogen or argon gas atmosphere；
(3) powder product is added in watery hydrochloric acid, stirring obtains mixed solution；Preferably, the watery hydrochloric acid is 37.5%
Dense watery hydrochloric acid and water according to 1：(1-5) what mass ratio was mixed to get, the mass percent of the watery hydrochloric acid is 10%-
15%；
(4) by the mixed solution suction filtration, drying, carbon nanometer tube-graphene composite material is obtained.
7. preparation method as claimed in claim 6, wherein, in step (1), ammonia is introduced during chemical vapor deposition
Nitrogen doped carbon nanotube is obtained, the concentration of volume percent of the ammonia is 1%-10%；Do not introduce ammonia and obtain not nitrating carbon and receive
Mitron.
8. preparation method as claimed in claims 6 or 7, wherein, using the catalyst containing nitrogen-doped graphene and in chemical gas
Introduce under conditions of ammonia in phase deposition process, obtain nitrogen-doped graphene-nitrogen doped carbon nanotube compound；Using containing nitrating stone
The catalyst of black alkene is not simultaneously introduced under conditions of ammonia in chemical vapor deposition processes, obtains the nitrating carbon of nitrogen-doped graphene-not
Nanotube complex；Using the bar that ammonia is introduced containing the not catalyst of nitrogen-doped graphene and in chemical vapor deposition processes
Under part, not nitrogen-doped graphene-nitrogen doped carbon nanotube compound is obtained；Using containing the not catalyst of nitrogen-doped graphene and in change
Learn and do not introduced under conditions of ammonia in vapor deposition processes, obtain the not nitrogen doped carbon nanotube compound of nitrogen-doped graphene-not.
9. the carbon nanometer tube-graphene composite material that the preparation method any one of claim 6-8 is prepared.
10. carbon nanometer tube-graphene composite material as claimed in claim 9, wherein, the CNT-Graphene composite wood
Material includes multi-walled carbon nano-tubes-multi-layer graphene compound, SWCN-multi-layer graphene compound, multi-wall carbon nano-tube
The combination of one or more in pipe-few layer graphene compound and SWCN-few layer graphene compound.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107101254A (en) * | 2017-05-25 | 2017-08-29 | 四川宏名新材料科技有限公司 | A kind of CNT graphene floor heating tiles |
| CN107252682A (en) * | 2017-06-10 | 2017-10-17 | 陈永 | A kind of preparation method and applications for being used for organic carbon vapor phase growth for the catalyst of carbide |
| CN110054174A (en) * | 2019-04-09 | 2019-07-26 | 中国人民解放军军事科学院军事医学研究院 | Nitrogen-doped carbon based composites and the preparation method and application thereof |
| CN111155331A (en) * | 2020-01-13 | 2020-05-15 | 苏州康丽达精密电子有限公司 | Preparation method of 3D graphene cross-linked conductive cloth composite material, electromagnetic shielding material and application |
| CN112023964A (en) * | 2019-06-04 | 2020-12-04 | 山西潞安矿业(集团)有限责任公司 | Hydrogenation catalyst, preparation method and application |
| CN113083231A (en) * | 2021-04-12 | 2021-07-09 | 贵州大学 | Preparation method and application of porous carbon adsorbent for deeply removing hydrogen sulfide |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107101254A (en) * | 2017-05-25 | 2017-08-29 | 四川宏名新材料科技有限公司 | A kind of CNT graphene floor heating tiles |
| CN107252682A (en) * | 2017-06-10 | 2017-10-17 | 陈永 | A kind of preparation method and applications for being used for organic carbon vapor phase growth for the catalyst of carbide |
| CN110054174A (en) * | 2019-04-09 | 2019-07-26 | 中国人民解放军军事科学院军事医学研究院 | Nitrogen-doped carbon based composites and the preparation method and application thereof |
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| CN112023964B (en) * | 2019-06-04 | 2022-11-01 | 山西潞安矿业(集团)有限责任公司 | Hydrogenation catalyst, preparation method and application |
| CN111155331A (en) * | 2020-01-13 | 2020-05-15 | 苏州康丽达精密电子有限公司 | Preparation method of 3D graphene cross-linked conductive cloth composite material, electromagnetic shielding material and application |
| CN113083231A (en) * | 2021-04-12 | 2021-07-09 | 贵州大学 | Preparation method and application of porous carbon adsorbent for deeply removing hydrogen sulfide |
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