CN108502865B - Preparation method of novel porous carbon material with self-assembled carbon nano tubes - Google Patents
Preparation method of novel porous carbon material with self-assembled carbon nano tubes Download PDFInfo
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- CN108502865B CN108502865B CN201710102752.2A CN201710102752A CN108502865B CN 108502865 B CN108502865 B CN 108502865B CN 201710102752 A CN201710102752 A CN 201710102752A CN 108502865 B CN108502865 B CN 108502865B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 41
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 19
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 128
- 229910052742 iron Inorganic materials 0.000 claims abstract description 61
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 28
- RFFLAFLAYFXFSW-UHFFFAOYSA-N 1,2-dichlorobenzene Chemical compound ClC1=CC=CC=C1Cl RFFLAFLAYFXFSW-UHFFFAOYSA-N 0.000 claims abstract description 24
- 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
- 238000010438 heat treatment Methods 0.000 claims description 26
- 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
- 238000000034 method Methods 0.000 claims description 10
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 claims description 3
- 238000005336 cracking Methods 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
- 238000004321 preservation Methods 0.000 claims description 2
- 238000003795 desorption Methods 0.000 abstract description 8
- 210000002268 wool Anatomy 0.000 abstract description 8
- 238000001179 sorption measurement Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 3
- 230000004931 aggregating effect Effects 0.000 abstract 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 14
- 238000004140 cleaning Methods 0.000 description 12
- 239000012535 impurity Substances 0.000 description 8
- 238000001816 cooling Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 239000011148 porous material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002048 multi walled nanotube Substances 0.000 description 2
- 238000011160 research 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
- 229910021387 carbon allotrope Inorganic materials 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 239000007789 gas Substances 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
- 238000009396 hybridization Methods 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002074 nanoribbon 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
- 238000001338 self-assembly Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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
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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
- C01P2004/03—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
- C01P2004/50—Agglomerated particles
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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Abstract
The invention discloses a preparation method of a novel porous carbon material with self-assembled carbon nano tubes, which comprises the following steps of treating a pure iron sheet at a high temperature; growing the material by CVD with the treated iron sheet as a matrix and o-dichlorobenzene as a carbon source under the protection of inert atmosphere; preparing a novel wool ballThe prepared carbon material is formed by aggregating carbon nano tubes, and the specific surface area of the material is calculated through nitrogen adsorption and desorption and can reach 1500-2000 m2/g。
Description
Technical Field
The invention relates to a method for preparing a novel carbon material, in particular to a method for preparing a porous spherical carbon material with self-assembled carbon nano tubes.
Background
Carbon is one of the most closely related and important elements existing in nature and having diverse electron orbital characteristics (sp, sp)2、sp3Hybridization), and further sp2The anisotropy of the crystal and the anisotropy of the arrangement thereof are caused by the anisotropy of the crystal, so that carbon materials having carbon element as the only constituent element have various properties, and new carbon phases and new carbon materials are continuously found and artificially produced. Carbon element as a single element can form substances with completely different structures and properties, and allotropes of carbon include diamond, graphite, fullerene, carbon nanotubes, carbon fibers and the like. Researchers have conducted extensive research on carbon materials, and carbon materials of different forms and properties, such as carbon nanotubes, carbon fibers, carbon spiral tubes, carbon spheres, carbon triangular pyramids, carbon nanoribbons, graphene, and the like, have been prepared. Due to the diversity of forms and properties of carbon, many unexplored parts of carbon materials are still determined, and researchers are prompted to research the carbon materials more variously. At present, the main methods for preparing the carbon material comprise a chemical vapor deposition method and the like, and the chemical vapor deposition method is the most common technology for preparing the carbon material. The porous carbon material is a carbon material with different pore structures, and the pore size of the porous carbon material can be regulated according to the requirements of practical application, so that the pore size of the porous carbon material is between a nanometer-level micropore and a micron-level macropore. The porous carbon material has the advantages of good chemical stability, good conductivity, low price and the like of the carbon material; meanwhile, the porous structure has the characteristics of large specific surface area, controllable pore channel structure and the like. Porous carbon materials are widely used in the fields of gas separation, water purification, chromatographic analysis, photocatalysis, energy storage and the like.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a novel porous spherical carbon material, and the method successfully prepares the porous spherical carbon material formed by self-assembly of carbon nanotubes.
The technical purpose of the invention is realized by the following technical scheme:
a preparation method of a novel porous carbon material with self-assembled carbon nano tubes comprises the steps of placing an iron sheet in a tube furnace, heating the iron sheet from room temperature to 700-800 ℃ in an air atmosphere, and keeping the temperature for 10-30 min to activate iron atoms to serve as a matrix and a catalyst for growing a carbon material; and then, continuously heating to 800-950 ℃ under an inert atmosphere, keeping the temperature for 30-90 min, injecting carbon source o-dichlorobenzene into the tubular furnace, adsorbing carbon atoms obtained after cracking the carbon source to the surface of the iron sheet, and growing carbon nanotubes on the surface of the iron sheet under the catalytic action of the iron atoms to obtain the porous carbon material.
In the technical scheme, the iron sheet is pure iron sheet, is placed in acetone, is subjected to ultrasonic treatment for 10-20 min, is cleaned of impurities on the surface of the iron sheet, and is dried in air.
In the technical scheme, the iron sheet is placed in a tube furnace and is heated to 760-800 ℃ from room temperature in the air atmosphere for heat preservation for 20-30 min.
In the above technical scheme, the inert atmosphere is argon, helium or nitrogen.
In the above technical scheme, the inert atmosphere flow rate is 50-500 sccm.
In the technical scheme, the injection speed of the carbon source o-dichlorobenzene is 5-20 ml/h.
In the technical scheme, the temperature is increased to 850-900 ℃, and the temperature is kept for 60-90 min.
Compared with the prior art, the iron sheet in the technical scheme of the invention cleans impurities on the surface by ultrasound, and the iron sheet is annealed at high temperature to activate iron atoms to be used as a matrix and a catalyst for growing the carbon material, o-dichlorobenzene is used as a carbon source, the carbon atoms after the carbon source is cracked are adsorbed on the surface of the iron sheet, and the carbon material is grown under the catalytic action of the iron atoms. The invention adopts a chemical vapor deposition method to successfully prepare a novel carbon material, uses a high-temperature treated pure iron sheet as a matrix, and injects a liquid carbon source into a tubular furnace for chemical reactionAnd a new substance is produced to be deposited on the surface of the iron sheet, and the carbon material with the ball shape of the knitting wool is successfully prepared. The invention obtains a novel carbon material in a wool ball shape, which is formed by self-assembling carbon nano tubes, the structure is in the wool ball shape, the carbon ball has a porous structure, the diameter of the carbon ball is 20-50 mu m, the carbon ball has a large specific surface area, and the specific surface can reach 1500-2000 m through testing2In terms of/g (nitrogen desorption apparatus: Micromeritics ASAP 2020). The measurement was carried out using a Raman spectrometer RENISHAW inVia reflex, as can be seen from the Raman spectrum at 1360cm-1、1580cm-1、2700cm-1The peaks, namely the D peak, the G peak and the 2D peak, appear nearby respectively, and are characteristic peaks of the multi-wall carbon nanotube, which indicates that the material is composed of the multi-wall carbon nanotube.
Drawings
FIG. 1 is a scanning electron micrograph (1) of a carbon nanotube self-assembled wool spherical carbon material of the present invention.
FIG. 2 is a scanning electron micrograph (2) of the carbon nanotube self-assembled wool spherical carbon material of the present invention.
FIG. 3 is a scanning electron micrograph (3) of the carbon nanotube self-assembled wool spherical carbon material of the present invention.
FIG. 4 is a Raman spectrum of the carbon nanotube self-assembled wool spherical carbon material of the present invention.
Detailed Description
The following examples of the present invention are given as further illustrations of the invention. And not to limit the scope of the invention.
Example 1
Placing a pure iron sheet into acetone, ultrasonically cleaning for 15min, cleaning up the impurities on the surface of the iron sheet, and drying the iron sheet in an oven. Placing the iron sheet in a horizontal tube furnace in air atmosphere, heating from room temperature of 20-25 ℃ to 800 ℃ at a heating rate of 8 ℃/min, preserving heat for 10min, and carrying out high-temperature treatment on the iron sheet.
Heating the iron sheet after high-temperature treatment to 860 ℃ at a heating rate of 8 ℃/min under the protection of argon, adjusting the flow of argon to 50sccm, taking o-dichlorobenzene as a carbon source, and injectingSlowly injecting into a tube furnace at an injection speed of 5ml/h, and growing for 30 min. Stopping injection, and naturally cooling to room temperature of 20-25 ℃ under the protection of argon to obtain a sample. The prepared sample grows on the surface of an iron sheet, and the specific surface area of the sample is calculated to be 1660m through nitrogen adsorption and desorption2/g。
Example 2
Placing a pure iron sheet into acetone, ultrasonically cleaning for 15min, cleaning up the impurities on the surface of the iron sheet, and drying the iron sheet in an oven. Placing the iron sheet in a horizontal tube furnace in air atmosphere, heating from room temperature of 20-25 ℃ to 800 ℃ at a heating rate of 8 ℃/min, preserving heat for 10min, and carrying out high-temperature treatment on the iron sheet.
Heating the iron sheet after high-temperature treatment to 800 ℃ at the heating rate of 8 ℃/min under the protection of argon, adjusting the flow rate of argon to 50sccm, slowly injecting o-dichlorobenzene serving as a carbon source into a tubular furnace through an injector at the injection rate of 5ml/h, and growing for 30 min. Stopping injection, and naturally cooling to room temperature of 20-25 ℃ under the protection of argon to obtain a sample. The prepared sample grows on the surface of an iron sheet, and the specific surface area of the sample is up to 1920m calculated by nitrogen adsorption and desorption2/g。
Example 3
Placing a pure iron sheet into acetone, ultrasonically cleaning for 15min, cleaning up the impurities on the surface of the iron sheet, and drying the iron sheet in an oven. Placing the iron sheet in a horizontal tube furnace in air atmosphere, heating from room temperature of 20-25 ℃ to 800 ℃ at a heating rate of 8 ℃/min, preserving heat for 20min, and carrying out high-temperature treatment on the iron sheet.
Heating the iron sheet after high-temperature treatment to 860 ℃ at the heating rate of 8 ℃/min under the protection of argon, adjusting the flow rate of argon to 300sccm, slowly injecting o-dichlorobenzene serving as a carbon source into a tubular furnace through an injector at the injection rate of 10ml/h, and growing for 60 min. Stopping injection, and naturally cooling to room temperature of 20-25 ℃ under the protection of argon to obtain a sample. The prepared sample grows on the surface of the iron sheet, and the specific surface area of the sample is calculated to reach 1923m through nitrogen adsorption and desorption2/g。
Example 4
Placing a pure iron sheet into acetone, ultrasonically cleaning for 15min, cleaning up the impurities on the surface of the iron sheet, and drying the iron sheet in an oven. Placing the iron sheet in a horizontal tube furnace in air atmosphere, heating from room temperature of 20-25 ℃ to 700 ℃ at a heating rate of 5 ℃/min, and preserving heat for 20min, and carrying out high-temperature treatment on the iron sheet.
Heating the iron sheet after high-temperature treatment to 900 ℃ at the heating rate of 5 ℃/min under the protection of argon, adjusting the flow rate of argon to 300sccm, slowly injecting o-dichlorobenzene serving as a carbon source into a tubular furnace through an injector at the injection rate of 15ml/h, and growing for 60 min. Stopping injection, and naturally cooling to room temperature of 20-25 ℃ under the protection of argon to obtain a sample. The prepared sample grows on the surface of an iron sheet, and the specific surface area of the sample is calculated to be 1665m through nitrogen adsorption and desorption2/g。
Example 5
Placing a pure iron sheet into acetone, ultrasonically cleaning for 15min, cleaning up the impurities on the surface of the iron sheet, and drying the iron sheet in an oven. Placing the iron sheet in a horizontal tube furnace in air atmosphere, heating from room temperature of 20-25 ℃ to 750 ℃ at a heating rate of 10 ℃/min, preserving heat for 15min, and carrying out high-temperature treatment on the iron sheet.
Heating the iron sheet after high-temperature treatment to 860 ℃ at a heating rate of 10 ℃/min under the protection of argon, adjusting the flow rate of argon to be 500sccm, slowly injecting o-dichlorobenzene serving as a carbon source into a tubular furnace through an injector at an injection rate of 20ml/h, and growing for 30 min. Stopping injection, and naturally cooling to room temperature of 20-25 ℃ under the protection of argon to obtain a sample. The prepared sample grows on the surface of an iron sheet, and the specific surface area of the sample is calculated to reach 1831m through nitrogen adsorption and desorption2/g。
Example 6:
placing a pure iron sheet into acetone, ultrasonically cleaning for 15min, cleaning up the impurities on the surface of the iron sheet, and drying the iron sheet in an oven. Placing the iron sheet in a horizontal tube furnace in air atmosphere, heating from room temperature of 20-25 ℃ to 800 ℃ at a heating rate of 8 ℃/min, preserving heat for 25min, and carrying out high-temperature treatment on the iron sheet.
Treating at high temperatureHeating the iron sheet to 950 ℃ at a heating rate of 10 ℃/min under the protection of argon, adjusting the flow rate of argon to be 500sccm, slowly injecting o-dichlorobenzene serving as a carbon source into a tubular furnace through an injector at an injection rate of 10ml/h, and growing for 90 min. Stopping injection, and naturally cooling to room temperature of 20-25 ℃ under the protection of argon to obtain a sample. The prepared sample grows on the surface of the iron sheet, and the specific surface area of the sample is calculated to reach 1516m through nitrogen adsorption and desorption2/g。
The technical scheme recorded in the invention can be used for realizing the preparation of the novel carbon material by adjusting the process parameters, and the tested specific surface area shows 1500-2000 m2(ii) in terms of/g. The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (3)
1. A preparation method of a novel porous carbon material with self-assembled carbon nano tubes is characterized in that an iron sheet is placed in a tubular furnace and is heated from room temperature to 700-800 ℃ in air atmosphere for heat preservation for 10-30 min, so that iron atoms are activated and used as a matrix and a catalyst for growing a carbon material; and then, continuously heating to 800-950 ℃ under the inert atmosphere, keeping the temperature for 30-90 min, wherein the flow of the inert atmosphere is 50-500sccm, injecting carbon source o-dichlorobenzene into the tubular furnace, wherein the injection speed of the carbon source o-dichlorobenzene is 5-20 ml/h, adsorbing carbon atoms obtained after cracking the carbon source to the surface of the iron sheet, and growing carbon nanotubes on the surface of the iron sheet under the catalytic action of the iron atoms to obtain the porous carbon material.
2. The method for preparing a novel porous carbon material with self-assembled carbon nanotubes as claimed in claim 1, wherein the iron sheet is placed in a tube furnace and is heated from room temperature to 760-800 ℃ in an air atmosphere for 20-30 min.
3. The method for preparing a novel porous carbon material with self-assembled carbon nanotubes as claimed in claim 1, wherein the inert atmosphere is argon, helium or nitrogen.
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