CN108502865A - A kind of preparation method of the novel porous carbon material of carbon nanotube self assembly - Google Patents
A kind of preparation method of the novel porous carbon material of carbon nanotube self assembly Download PDFInfo
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- CN108502865A CN108502865A CN201710102752.2A CN201710102752A CN108502865A CN 108502865 A CN108502865 A CN 108502865A CN 201710102752 A CN201710102752 A CN 201710102752A CN 108502865 A CN108502865 A CN 108502865A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 39
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 22
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 22
- 238000001338 self-assembly Methods 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 124
- 229910052742 iron Inorganic materials 0.000 claims abstract description 65
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 239000011159 matrix material Substances 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 40
- 239000007789 gas Substances 0.000 claims description 23
- 229910052786 argon Inorganic materials 0.000 claims description 20
- 238000002347 injection Methods 0.000 claims description 14
- 239000007924 injection Substances 0.000 claims description 14
- 238000010792 warming Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- 238000004321 preservation Methods 0.000 claims description 4
- 150000001721 carbon Chemical group 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000005336 cracking Methods 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 238000009940 knitting Methods 0.000 abstract description 8
- 238000002336 sorption--desorption measurement Methods 0.000 abstract description 8
- 210000002268 wool Anatomy 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- 238000000034 method Methods 0.000 description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 14
- 230000008569 process Effects 0.000 description 13
- 239000000243 solution Substances 0.000 description 8
- 238000004506 ultrasonic cleaning Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002048 multi walled nanotube Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000011514 reflex Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
- C01P2006/12—Surface area
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- Carbon And Carbon Compounds (AREA)
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Abstract
The present invention discloses a kind of preparation method of the novel porous carbon material of carbon nanotube self assembly, after pure iron piece is handled at high temperature;Using treated iron plate as matrix, using o-dichlorohenzene as carbon source under inert atmosphere protection, pass through CVD growth material;A kind of novel knitting wool spherical carbon material is prepared, the carbon material of preparation is reunited by carbon nanotube, and calculating this material by nitrogen adsorption desorption has very high specific surface area, can reach 1500~2000m2/g。
Description
Technical field
The present invention relates to a kind of methods prepared by new carbon, relate in particular to a kind of the more of carbon nanotube self assembly
The preparation method of hole spherical carbon material.
Background technology
Carbon be present in nature with the mankind are most closely related, one of most important element, it has various
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.Carbon can form structure and the entirely different object of performance as single-element
The allotrope of matter, carbon includes diamond, graphite, fullerene, carbon nanotube, carbon fiber etc..Researcher is to carbon materials
Material has carried out extensive research, is prepared for carbon nanotube, carbon fiber, carbon helix tube, carbon ball, carbon pyrometric cone, carbon nanobelts, graphene
Etc. different forms and property carbon material.Since carbon has form and property qualitative diversity, have perhaps to determine carbon material still
Mostly untapped part has promoted scientific research personnel to carry out more diversified research to carbon material.The main side of carbon material is prepared at present
It is to prepare the most commonly used technology of carbon material that method, which has chemical vapor infiltration etc., chemical vapor infiltration,.Porous carbon materials are one
Carbon material of the kind with Different Pore Structures, aperture can be regulated and controled according to the requirement of practical application, be made at its pore size
Between the nanometer level microporous macropore to micron order.Porous carbon materials in addition to the chemical stability with carbon material it is good, conductive
The advantages that property is good, cheap;Meanwhile the features such as porous structure makes it have large specific surface area again, pore passage structure is controllable.It is porous
Carbon material is used widely in fields such as gas separation, the purification of water, chromatography, photocatalysis and energy stores.
Invention content
Present invention aims to overcome that deficiency in the prior art, provides the preparation side of novel porous spherical carbon material
Method, this method are successfully prepared a kind of porous spherical carbon material being self-assembly of by carbon nanotube.
The technical purpose of the present invention is achieved by following technical proposals:
A kind of preparation method of the novel porous carbon material of carbon nanotube self assembly, iron plate is placed in tube furnace and in sky
10~30min of heat preservation is carried out from room temperature to 700-800 degrees Celsius in gas atmosphere, so that iron atom activates, as growth carbon
The matrix and catalyst of material;It is changed to again under inert atmosphere and continues to heat up from 800-950 degrees Celsius and keep the temperature 30~90min,
Carbon source o-dichlorohenzene is injected into tube furnace, the carbon atom after carbon source cracking is adsorbed onto the surface of iron plate, in urging for iron atom
Carbon nanotube is grown on iron plate surface under change effect, obtains porous carbon materials.
In the above-mentioned technical solutions, iron plate selects pure iron piece, is placed in acetone, 10-20min of ultrasound clean out iron plate
It is dried in air after the impurity on surface.
In the above-mentioned technical solutions, iron plate is placed in tube furnace and in air atmosphere from room temperature to 760-800
Degree Celsius carry out 20~30min of heat preservation.
In the above-mentioned technical solutions, inert atmosphere is argon gas, helium or nitrogen.
In the above-mentioned technical solutions, inert atmosphere flow is 50-500sccm.
In the above-mentioned technical solutions, the injection speed of carbon source o-dichlorohenzene is 5~20ml/h.
In the above-mentioned technical solutions, 850-900 degrees Celsius are warming up to, 60-90min are kept the temperature.
Compared with prior art, iron plate cleans up the impurity on surface, by height by ultrasound in technical solution of the present invention
The lower annealing of temperature, makes iron atom activate, and as the matrix and catalyst of growth carbon material, o-dichlorohenzene is as carbon source, carbon source cracking
Carbon atom afterwards is adsorbed onto the surface of iron plate, and carbon material is grown under the catalytic action of iron atom.The present invention is using chemical gas
Phase sedimentation successfully prepares a kind of novel carbon material, and using the pure iron piece after high-temperature process as matrix, liquid carbon source is noted
It penetrates as chemically reacted in tube furnace, a kind of new electrodeposition substance of production has successfully prepared knitting wool ball on the surface of iron plate
The carbon material of shape.Present invention obtains a kind of new carbons spherical in knitting wool, and this material is by carbon nanotube self assembly
It forms, structure is spherical in knitting wool, and there is porous structure, a diameter of 20-50 μm of carbon ball to have prodigious specific surface area, pass through survey
Examination specific surface can reach 1500~2000m2/ g (nitrogen adsorption desorption instruments:Micromeritics ASAP2020).Use drawing
Graceful spectrometer RENISHAW inVia reflex are tested, from Raman spectrum as can be seen that in 1360cm-1、1580cm-1、2700cm-1Nearby occur peak respectively, is the peaks D, the peaks G and the peaks 2D respectively, is the characteristic peak of multi-walled carbon nanotube, illustrates this
Kind material is made of multi-walled carbon nanotube.
Description of the drawings
Fig. 1 is the electron scanning micrograph (1) of the carbon nanotube self assembly knitting wool spherical carbon material of the present invention.
Fig. 2 is the electron scanning micrograph (2) of the carbon nanotube self assembly knitting wool spherical carbon material of the present invention.
Fig. 3 is the electron scanning micrograph (3) of the carbon nanotube self assembly knitting wool spherical carbon material of the present invention.
Fig. 4 is the Raman spectrogram of the carbon nanotube self assembly knitting wool spherical carbon material of the present invention.
Specific implementation mode
The embodiment of the present invention is given below, is the further explanation to the present invention.Rather than it limits the scope of the invention.
Embodiment 1
By one piece of pure iron piece as in acetone, ultrasonic cleaning 15min cleans out the magazine on iron plate surface, by iron plate
It dries in an oven.Iron plate is positioned over horizontal pipe furnace in air atmosphere, with the heating rate of 8 DEG C/min from room temperature 20-
25 degrees Celsius are warming up at 800 DEG C and keep the temperature 10min, and high-temperature process is carried out to iron plate.
Under protection of argon gas by the iron plate after high-temperature process, 860 DEG C are warming up to the heating rate of 8 DEG C/min, adjust argon
The flow of gas is that 50sccm is slowly injected into tube furnace, injection speed is using o-dichlorohenzene as carbon source by syringe
5ml/h grows 30min.Stop injection, 20-25 degrees Celsius of cooled to room temperature obtains sample under protection of argon gas.It prepares
Sample grown on the surface of iron plate, its specific surface area is calculated by nitrogen adsorption desorption and reaches 1660m2/g。
Embodiment 2
By one piece of pure iron piece as in acetone, ultrasonic cleaning 15min cleans out the magazine on iron plate surface, by iron plate
It dries in an oven.Iron plate is positioned over horizontal pipe furnace in air atmosphere, with the heating rate of 8 DEG C/min from room temperature 20-
25 degrees Celsius are warming up at 800 DEG C and keep the temperature 10min, and high-temperature process is carried out to iron plate.
Under protection of argon gas by the iron plate after high-temperature process, 800 DEG C are warming up to the heating rate of 8 DEG C/min, adjust argon
The flow of gas is that 50sccm is slowly injected into tube furnace, injection speed is using o-dichlorohenzene as carbon source by syringe
5ml/h grows 30min.Stop injection, 20-25 degrees Celsius of cooled to room temperature obtains sample under protection of argon gas.It prepares
Sample grown on the surface of iron plate, its specific surface area is calculated by nitrogen adsorption desorption and reaches 1920m2/g。
Embodiment 3
By one piece of pure iron piece as in acetone, ultrasonic cleaning 15min cleans out the magazine on iron plate surface, by iron plate
It dries in an oven.Iron plate is positioned over horizontal pipe furnace in air atmosphere, with the heating rate of 8 DEG C/min from room temperature 20-
25 degrees Celsius are warming up at 800 DEG C and keep the temperature 20min, and high-temperature process is carried out to iron plate.
Under protection of argon gas by the iron plate after high-temperature process, 860 DEG C are warming up to the heating rate of 8 DEG C/min, adjust argon
The flow of gas is that 300sccm is slowly injected into tube furnace, injection speed is using o-dichlorohenzene as carbon source by syringe
10ml/h grows 60min.Stop injection, 20-25 degrees Celsius of cooled to room temperature obtains sample under protection of argon gas.It prepares
Sample grown on the surface of iron plate, its specific surface area is calculated by nitrogen adsorption desorption and reaches 1923m2/g。
Embodiment 4
By one piece of pure iron piece as in acetone, ultrasonic cleaning 15min cleans out the magazine on iron plate surface, by iron plate
It dries in an oven.Iron plate is positioned over horizontal pipe furnace in air atmosphere, with the heating rate of 5 DEG C/min from room temperature 20-
25 degrees Celsius are warming up at 700 DEG C and keep the temperature 20min, and high-temperature process is carried out to iron plate.
Under protection of argon gas by the iron plate after high-temperature process, 900 DEG C are warming up to the heating rate of 5 DEG C/min, adjust argon
The flow of gas is that 300sccm is slowly injected into tube furnace, injection speed is using o-dichlorohenzene as carbon source by syringe
15ml/h grows 60min.Stop injection, 20-25 degrees Celsius of cooled to room temperature obtains sample under protection of argon gas.It prepares
Sample grown on the surface of iron plate, its specific surface area is calculated by nitrogen adsorption desorption and reaches 1665m2/g。
Embodiment 5
By one piece of pure iron piece as in acetone, ultrasonic cleaning 15min cleans out the magazine on iron plate surface, by iron plate
It dries in an oven.Iron plate is positioned over horizontal pipe furnace in air atmosphere, with the heating rate of 10 DEG C/min from room temperature
20-25 degrees Celsius are warming up at 750 DEG C and keep the temperature 15min, and high-temperature process is carried out to iron plate.
Under protection of argon gas by the iron plate after high-temperature process, 860 DEG C are warming up to the heating rate of 10 DEG C/min, adjust argon
The flow of gas is that 500sccm is slowly injected into tube furnace, injection speed is using o-dichlorohenzene as carbon source by syringe
20ml/h grows 30min.Stop injection, 20-25 degrees Celsius of cooled to room temperature obtains sample under protection of argon gas.It prepares
Sample grown on the surface of iron plate, its specific surface area is calculated by nitrogen adsorption desorption and reaches 1831m2/g。
Embodiment 6:
By one piece of pure iron piece as in acetone, ultrasonic cleaning 15min cleans out the magazine on iron plate surface, by iron plate
It dries in an oven.Iron plate is positioned over horizontal pipe furnace in air atmosphere, with the heating rate of 8 DEG C/min from room temperature 20-
25 degrees Celsius are warming up at 800 DEG C and keep the temperature 25min, and high-temperature process is carried out to iron plate.
Under protection of argon gas by the iron plate after high-temperature process, 950 DEG C are warming up to the heating rate of 10 DEG C/min, adjust argon
The flow of gas is that 500sccm is slowly injected into tube furnace, injection speed is using o-dichlorohenzene as carbon source by syringe
10ml/h grows 90min.Stop injection, 20-25 degrees Celsius of cooled to room temperature obtains sample under protection of argon gas.It prepares
Sample grown on the surface of iron plate, its specific surface area is calculated by nitrogen adsorption desorption and reaches 1516m2/g。
The adjustment that technological parameter is carried out according to the technical solution that the content of present invention is recorded, can be achieved the system of new carbon
Standby, specific surface area shows 1500~2000m after tested2/g.Illustrative description is done to the present invention above, it should explanation
It is that, in the case where not departing from core of the invention, any simple deformation, modification or other skilled in the art can
The equivalent replacement of creative work is not spent to each fall within protection scope of the present invention.
Claims (6)
1. a kind of preparation method of the novel porous carbon material of carbon nanotube self assembly, which is characterized in that iron plate is placed in tubular type
10~30min of heat preservation is carried out from room temperature to 700-800 degrees Celsius in stove and in air atmosphere, so that iron atom activates,
Matrix and catalyst as growth carbon material;It is changed to again under inert atmosphere and continues heating from 800-950 degrees Celsius and keep the temperature
Carbon source o-dichlorohenzene is injected into tube furnace by 30~90min, and the carbon atom after carbon source cracking is adsorbed onto the surface of iron plate,
Carbon nanotube is grown on iron plate surface under the catalytic action of iron atom, obtains porous carbon materials.
2. a kind of preparation method of the novel porous carbon material of carbon nanotube self assembly according to claim 1, feature
Be, iron plate is placed in tube furnace and in air atmosphere from room temperature to 760-800 degrees Celsius carry out heat preservation 20~
30min。
3. a kind of preparation method of the novel porous carbon material of carbon nanotube self assembly according to claim 1, feature
It is, inert atmosphere is argon gas, helium or nitrogen.
4. a kind of preparation method of the novel porous carbon material of carbon nanotube self assembly according to claim 1, feature
It is, inert atmosphere flow is 50-500sccm.
5. a kind of preparation method of the novel porous carbon material of carbon nanotube self assembly according to claim 1, feature
It is, the injection speed of carbon source o-dichlorohenzene is 5~20ml/h.
6. a kind of preparation method of the novel porous carbon material of carbon nanotube self assembly according to claim 1, feature
It is, is warming up to 850-900 degrees Celsius, keeps the temperature 60-90min.
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CN114597428A (en) * | 2022-03-10 | 2022-06-07 | 湖南金博氢能科技有限公司 | Flexible carbon paper, preparation method thereof, gas diffusion layer and fuel cell |
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CN106082163A (en) * | 2016-06-07 | 2016-11-09 | 中山大学 | A kind of preparation method of large area nitrogen doped carbon nanotube paper |
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CN103420355A (en) * | 2012-05-22 | 2013-12-04 | 海洋王照明科技股份有限公司 | Method for preparing carbon nanometer walls from solid carbon source |
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CN114597428A (en) * | 2022-03-10 | 2022-06-07 | 湖南金博氢能科技有限公司 | Flexible carbon paper, preparation method thereof, gas diffusion layer and fuel cell |
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