CN112194115A - Preparation method of hollow carbon nanospheres and hollow carbon nanospheres - Google Patents
Preparation method of hollow carbon nanospheres and hollow carbon nanospheres Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 60
- 239000002077 nanosphere Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910021392 nanocarbon Inorganic materials 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 18
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 18
- 239000007789 gas Substances 0.000 claims abstract description 18
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 18
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 18
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000012670 alkaline solution Substances 0.000 claims abstract description 3
- 238000007654 immersion Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 14
- 239000003513 alkali Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000011805 ball Substances 0.000 description 18
- 238000006243 chemical reaction Methods 0.000 description 18
- 238000000151 deposition Methods 0.000 description 10
- 230000008021 deposition Effects 0.000 description 10
- 239000011807 nanoball Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 238000005336 cracking Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
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- 239000004094 surface-active agent Substances 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KVBYPTUGEKVEIJ-UHFFFAOYSA-N benzene-1,3-diol;formaldehyde Chemical compound O=C.OC1=CC=CC(O)=C1 KVBYPTUGEKVEIJ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229960001948 caffeine Drugs 0.000 description 1
- 239000007833 carbon precursor Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- RYYVLZVUVIJVGH-UHFFFAOYSA-N trimethylxanthine Natural products CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
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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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention discloses a preparation method of hollow carbon nanospheres and hollow carbon nanospheres, which comprises the following steps: s1, mixing SiO2Placing the ball in a tube furnace, vacuumizing, and then heating to 750-800 ℃ in Ar atmosphere; s2, according to 1: 3, introducing argon and methane according to the gas flow ratio, carrying out the radio frequency discharge under the furnace pressure of 140-; s3, turning off the radio frequency power supply and methane, and cooling to room temperature in Ar atmosphere to obtain SiO as the inner core2The carbon nanospheres of (1); s4, removing SiO in the nano carbon spheres by using alkaline solution immersion2Filtering and drying to obtain hollow carbon nanospheres; by using the method, the wall thickness of the hollow carbon nanospheres can be controlled in the preparation process, so that the hollow carbon nanospheres with different wall thicknesses can be prepared according to actual requirements, and the centering can be realizedThe method is effective in preparation and utilization of hollow carbon nanospheres.
Description
Technical Field
The invention relates to the field of nano carbon sphere preparation, in particular to a preparation method of hollow nano carbon spheres and hollow nano carbon spheres prepared by the preparation method.
Background
Carbon materials having a particular morphology and structure, and their properties and applications are also receiving increasing attention. As a nano material with high specific surface area and low density, the hollow nano carbon sphere not only has the characteristics of good permeability, higher chemical and thermal stability, adsorption property, nontoxicity, biocompatibility and the like, but also has a regular spherical structure, so that the hollow nano carbon sphere has huge potential application value in many fields of electrochemical energy, gas storage, adsorption separation, catalysis and the like. Currently, researchers have developed various methods for preparing hollow nanocarbon spheres, and the template method is most widely used, but the non-template method is less frequently used.
The template method is the most widely used method for preparing hollow nano carbon spheres, and mainly adopts rigid structures such as SiO2, Si, Ag, Au and the like or flexible structures such as microemulsion particles, surfactants, supermolecule micelles, high polymer vesicles and even bubbles and the like to prepare a spherical template, a carbon precursor is coated on the surface of the spherical template, and finally the template is removed to prepare the hollow carbon nanospheres. However, in the preparation process of the template, a large amount of toxic organic solvents and catalysts such as phenolic resin, reverse microemulsion, reverse micelle, resorcinol formaldehyde, polystyrene and the like are used, and a large amount of surfactants are often added in order to relieve the agglomeration phenomenon of the template. The processes not only introduce a large amount of toxic substances to cause harm to human bodies and the environment, but also have complicated steps and poor repeatability, and are not suitable for large-scale production and application. In addition, with the continuous development of society, the application range of the hollow carbon nanospheres is wider and wider, the requirements of applications in different fields on the hollow carbon nanospheres are higher and higher, and the hollow carbon nanospheres need to have higher requirements on the inner diameter, the outer diameter, the uniformity of the particle size, the sphericity and the like, and how to prepare the hollow carbon nanospheres with uniform particle size, good sphericity and controllable size (wall thickness) is still a difficult problem in the industry at present.
Disclosure of Invention
Based on the above technical problems in the prior art, the inventors have conducted extensive studies and experiments to provide a method for preparing hollow nanocarbon spheres from SiO2The ball is used as a template, a chemical vapor deposition method is adopted, deposition reaction is carried out at high temperature, and the outer diameter size of the hollow nano carbon ball can be effectively controlled by controlling the radio frequency power, the carbon source concentration and the reaction time during the deposition reaction, so that the hollow nano carbon ball can be effectively controlled, and the preparation method thereofThe wall thickness of the formed hollow carbon nanospheres is effectively controlled, and the hollow carbon nanospheres with different wall thicknesses can be prepared according to the practical application scene of the hollow carbon nanospheres.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of hollow carbon nanospheres comprises the following steps:
s1, mixing SiO2Placing the ball in a tube furnace, vacuumizing, and then heating to 750-800 ℃ in Ar atmosphere;
s2, according to 1: 3, introducing argon and methane in a gas flow ratio, keeping the furnace pressure of 140-;
s3, turning off the radio frequency power supply and methane, and cooling to room temperature in Ar atmosphere to obtain SiO as the inner core2The carbon nanospheres of (1);
s4, removing SiO in the nano carbon spheres by using alkaline solution immersion2Filtering and drying to obtain the hollow carbon nanospheres.
In some embodiments, in step S1, the temperature is raised to 750-800 ℃ at a rate of 5-10 ℃/min.
In some embodiments, in step S2, the flow rate of argon gas is 5 to 50Sccm and the flow rate of methane is 15 to 150 Sccm.
In some embodiments, in step S4, the alkali solution is a sodium hydroxide solution.
In some embodiments, in step S4, the inner core is SiO2The nano carbon spheres are put into sodium hydroxide solution, heated to 80 ℃ and stirred for more than 24 hours.
In some embodiments, the drying temperature is 60-80 ℃.
In some embodiments, the wall thickness of the hollow nanocarbon sphere is 20 nm to 100 nm.
Another object of the present invention is to provide a hollow nanocarbon sphere, which is prepared by the preparation method according to any one of the above embodiments.
Compared with the prior art, the invention has the following beneficial effects:
the invention uses chemical vapor deposition method to prepare SiO2The ball is used as a template, the surface of the template is coated with a carbon layer through deposition reaction to prepare a nano carbon ball, and then the SiO in the nano carbon ball is removed through alkali solution2To prepare the hollow nano carbon spheres. In the method provided by the invention, argon is used as carrier gas, methane is used as a carbon source, and the ratio of argon to methane is 1: 3, the gas flow ratio is brought into the vapor deposition furnace, the methane concentration in the tubular furnace is controlled by controlling the argon flow and the furnace pressure, the methane is subjected to cracking reaction at high temperature to generate carbon, and the radio frequency current is increased in the furnace to effectively avoid SiO2The balls are agglomerated and the carbon generated after cracking can be uniformly deposited on the SiO2On a ball, avoid SiO2The carbon on the spheres agglomerates.
The invention can prepare the carbon nanospheres with uniform particle size and controllable outer diameter size without using catalysts or other toxic substances harmful to human bodies, is green and environment-friendly, and has simple preparation process and easy operation.
Besides, the invention has the following advantages:
the method of the invention can effectively avoid SiO2The balls are agglomerated and can treat more SiO in one time2The ball is deposited to prepare the hollow nanometer carbon ball, thereby greatly improving the production efficiency.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is SiO2SEM images before and after the coating of the carbon layer is deposited on the template; wherein, the figure A is before coating, and the figure B is after coating.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed as broadly as the present invention is capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
SiO used in the following examples2The preparation method of the ball comprises the following steps:
adding 400ml of ethanol, 100ml of deionized water, 10ml of tetraethyl silicate and 40ml of ammonia water into a 1000ml beaker in sequence, stirring at the speed of 600r/min for 6 hours for reaction, and then carrying out centrifugal separation to obtain SiO 400nm with the particle size of 350-2A ball. SiO to be produced2SEM analysis was performed, and the analysis results are shown in FIG. 2, Panel A.
The NaOH solutions used in the following examples were prepared by the following method:
8g of NaOH was dissolved in 100ml of water, and the solution was stirred with heating to form a NaOH solution.
The tube furnace used is PECVD.
Example 1
As shown in fig. 1, a method for preparing a hollow carbon nanoball includes the steps of:
s1, mixing SiO2Placing the ball in a crucible, then placing the crucible in a tube furnace, and heating to 800 ℃ at a heating rate of 10 ℃/min in Ar atmosphere;
s2, turning on a radio frequency power supply, carrying methane by Ar gas, introducing the methane into a tubular furnace for deposition reaction, wherein the flow of the Ar gas is 12Sccm, the flow of the methane gas is 36Sccm, the furnace pressure is kept at 210Pa, the radio frequency power is 350W, and the deposition reaction is carried out for 2 h;
s3, after the reaction is finished, closing the radio frequency power supply and the methane, cooling to room temperature in Ar atmosphere, and taking out the product;
s4, putting the product obtained in the step S3 into an excessive NaOH solution, heating to 80 ℃ and stirring for 24 hours to remove SiO in the product2A ball;
s5, filtering after the treatment of the step S4 is finished, and drying at the temperature of 60-80 ℃ to obtain the hollow carbon nanospheres.
SEM analysis of the nanocarbon sphere obtained in step S2 showed that the nanocarbon sphere was coated with SiO by the method of the present example as shown in B of FIG. 22The nano carbon spheres prepared on the surfaces of the spheres have uniform outer diameters.
The method of this example detects the hollow carbon nanoball by the conventional method in this field, and the wall thickness of the hollow carbon nanoball prepared by this example is 50-60 nm.
Example 2
A method for preparing a hollow carbon nanoball, comprising the steps of:
s1, mixing SiO2Placing the ball in a crucible, then placing the crucible in a tube furnace, and heating to 800 ℃ at a heating rate of 5 ℃/min in Ar atmosphere;
s2, turning on a radio frequency power supply, carrying methane by Ar gas, introducing the methane into the tubular furnace for deposition reaction, wherein the flow of the Ar gas is 10Sccm, the flow of the methane gas is 30Sccm, the furnace pressure is kept at 140Pa, the radio frequency power is 350W, and the deposition reaction is carried out for 2 h;
s3, after the reaction is finished, closing the radio frequency power supply and the methane, cooling to room temperature in Ar atmosphere, and taking out the product;
s4, putting the product obtained in the step S3 into an excessive NaOH solution, heating to 80 ℃ and stirring for 24 hours to remove SiO in the product2A ball;
s5, filtering after the treatment of the step S4 is finished, and drying at the temperature of 60-80 ℃ to obtain the hollow carbon nanospheres.
The hollow carbon nanoball obtained was examined using a conventional method in the art, and the wall thickness of the hollow carbon nanoball obtained in this example was examined to be 20-30 nm.
As can be seen from embodiments 1 and 2, the method provided by the present invention can effectively control the outer diameter of the hollow carbon nanospheres by controlling the furnace pressure, the rf power and the methane gas flow during the deposition reaction, so as to effectively control the wall thickness of the hollow carbon nanospheres (i.e. effectively control the thickness of the carbon coating layer generated by the deposition reaction), and further prepare hollow carbon nanospheres with different outer diameters according to actual requirements, wherein the hollow carbon nanospheres have uniform size and uniform wall thickness.
Note that SiO used in the present application2And NaOH solution, not limited to self-made, but also commercially available; in addition, theIn the method, strict requirements are imposed on reaction temperature, gas flow, reaction furnace pressure, radio frequency power, reaction time and the like, if the reaction temperature is too high, hydrogen formed after methane cracking is dangerous due to too high temperature, and if the reaction temperature is too low, the methane cracking is not facilitated to generate carbon simple substances; if the carbon source gas flow is too large, it is not favorable for SiO2The surface carbon coating layer is formed, because the carbon gas flow is too large, more carbon simple substances are generated, the problem of uneven deposition can occur, the carbon gas flow is too small, the generated carbon simple substances are few, and SiO cannot be uniformly coated2Dissolving SiO on the surface of the template by NaOH solution2After the template is formed, the nano hollow carbon spheres collapse due to the fact that the wall thickness is too thin; if the furnace pressure is too high, the SiO causes2Has a certain porosity and is deposited on SiO2The carbon simple substance on the surface is embedded into SiO due to the over-high furnace pressure2In the gap, the generation of hollow structure is not facilitated, the furnace pressure is too low, and the formed carbon simple substance cannot be stably deposited on SiO2And forming hollow nanometer carbon spheres.
In summary, the method provided by the present invention requires specific furnace pressure, reaction temperature, carbon source and radio frequency power to effectively control the formation of the wall thickness of the hollow carbon nanospheres.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (8)
1. A preparation method of hollow carbon nanospheres is characterized by comprising the following steps:
s1, mixing SiO2Placing the ball in a tube furnace, vacuumizing, and then heating to 750-800 ℃ in Ar atmosphere;
s2, according to 1: 3, introducing argon and methane according to the gas flow ratio, carrying out the radio frequency discharge under the furnace pressure of 140-;
s3, turning off the radio frequency power supply and methane, and cooling to room temperature in Ar atmosphere to obtain SiO as the inner core2The carbon nanospheres of (1);
s4, removing SiO in the nano carbon spheres by using alkaline solution immersion2Filtering and drying to obtain the hollow carbon nanospheres.
2. The method as claimed in claim 1, wherein the temperature is raised to 750-800 ℃ at a rate of 5-10 ℃/min in the step S1.
3. The method for preparing hollow nanocarbon spheres of claim 1, wherein in the step S2, the flow rate of the argon gas is 5 to 50Sccm, and the flow rate of the methane is 15 to 150 Sccm.
4. The method for preparing hollow nanocarbon spheres of claim 1, wherein in the step S4, the alkali solution is a sodium hydroxide solution.
5. The method for preparing hollow nanocarbon spheres of claim 4, wherein in the step S4, the inner core is SiO2The nano carbon spheres are put into sodium hydroxide solution, heated to 80 ℃ and stirred for more than 24 hours.
6. The method for preparing hollow nanocarbon spheres of claim 1, wherein the drying temperature is 60 to 80 ℃.
7. The method for preparing hollow nanocarbon spheres of any one of claims 1 to 6, wherein the wall thickness of the hollow nanocarbon spheres is 20 to 100 nm.
8. A hollow nanocarbon sphere, characterized by being produced by the production method according to any one of claims 1 to 7.
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| CN113415798A (en) * | 2021-05-12 | 2021-09-21 | 江西农业大学 | Preparation method of phosphorus-doped microporous, mesoporous and macroporous coexisting grade pore structure nano carbon spheres |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113415798A (en) * | 2021-05-12 | 2021-09-21 | 江西农业大学 | Preparation method of phosphorus-doped microporous, mesoporous and macroporous coexisting grade pore structure nano carbon spheres |
| CN113415798B (en) * | 2021-05-12 | 2023-02-24 | 江西农业大学 | Preparation method of phosphorus-doped microporous, mesoporous and macroporous coexisting grade pore structure carbon nanospheres |
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