CN1266307C - Preparing onion shape fulven by chemical vapour phase deposition - Google Patents
Preparing onion shape fulven by chemical vapour phase deposition Download PDFInfo
- Publication number
- CN1266307C CN1266307C CN 200410012502 CN200410012502A CN1266307C CN 1266307 C CN1266307 C CN 1266307C CN 200410012502 CN200410012502 CN 200410012502 CN 200410012502 A CN200410012502 A CN 200410012502A CN 1266307 C CN1266307 C CN 1266307C
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- China
- Prior art keywords
- onion
- fullerene
- fulven
- ferrocene
- silica tube
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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
Abstract
The present invention relates to a method for preparing onion-shaped fulven by chemical vapour phase deposition, which belongs to the technical field of synthesizing and processing engineering of a new material. The present invention uses inert gas Ar with low price as carrier gas and adopts a traditional CVD technique to disclose a multi-state onion-shaped fulven group in mass preparation by the catalysis of nanometer particles and a preparation technology thereof. The onion-shaped fulven group provides a concentric spherical shell formed by covering C60 as a core with multiple layers, the nanometer particles are coated in an onion-shaped fulven cavity, and the onion-shaped fulven group is formed by the catalysis of the nanometer particle and is mainly used as a functional material. Therefore, the process for converting the theoretical research for the onion-shaped fulven to the application research is impelled.
Description
Technical field
The method (chemical Vapor deposition process be called for short CVD method) that chemical Vapor deposition process of the present invention prepares onion-like fullerene belongs to the synthetic and processing engineering technology category of novel material, relates generally to numerous areas such as Materials science such as nano material, carbon material, information material, functional materials and physics, chemistry, medical science.
Background technology
C continues
60, carbon nanotube discovery since, its special physics, chemical property just become the focus of scientific circles research.Onion-like fullerene more and more is subjected to extensive concern as a kind of novel carbon nano-functional material.But existing methods such as ion beam irradiation just can obtain onion-like fullerene by trace, and this is unfavorable for it is carried out the research of physics, chemical property.And chemical Vapor deposition process can magnanimity be prepared carbon nanotube and onion-like fullerene under lower temperature.Given this characteristics of method this respect, the investigator attempts to adopt the CVD method to prepare onion-like fullerene, in the hope of effective magnanimity ground preparation nano-onions shape soccerballene.Onion-like fullerene is that a kind of several layers by different sizes are with C
60The bigger carbon atom cluster of forming for the concentric graphite pebbles shell of core, form by lamellar compound (intercalationcompounds), onion-like fullerene film, metal/onion-like fullerene nano thin-film that monokaryon onion-like fullerene, multinuclear onion-like fullerene, interior genus nanoparticle onion-like fullerene covered with gold leaf, atoms metal are between the onion-like fullerene shell, coating the form layers spacing is the concentric spherical shell of 0.34nm, inner shell has 60 carbon atoms, and each shell carbonatoms is 60n later on
2(n is the shell number).
Summary of the invention
The method purpose that chemical Vapor deposition process of the present invention prepares onion-like fullerene is that it is simple to disclose a kind of technology, and cost is low, condition easily control prepare the technical scheme of onion-like fullerene with chemical Vapor deposition process.
Chemical Vapor deposition process of the present invention prepares the method for onion-like fullerene, it is characterized in that, be a kind of catalyzer that need not to prepare, directly adopt acetylene pyrolysis organo-metallic primitive reaction thing ferrocene to prepare the method for the onion-like fullerene that comes in every shape, the processing step of concrete preparation process is:
I. the silica tube in the preheating oven is at first got 1-2.5g purity then and is 99.9% ferrocene and places a porcelain boat, is placed on air intake one end of silica tube;
II. closed quartz tube feeds argon gas with the air in the emptying silica tube;
III. after treating that temperature in the silica tube is raised to 1173-1473K (900-1200 ℃), open the valve of acetylene, make argon gas and acetylene with 8-10: 1 ratio mixes, and Continuous Flow is through reaction chamber;
IV. heat the ferrocene in the porcelain boat, ferrocene is subjected to heat sublimation decompose to generate nano level small iron particulate catalyzer and is blown in the stove by argon gas stream to react, acetylene forms carbon source after the catalyst surface cracking, carbon source spreads by catalyzer, progressively generates onion-like fullerene;
Its advantage of method that chemical Vapor deposition process of the present invention prepares onion-like fullerene is: utilize cheap Ar to do carrier gas, by effective control reaction temperature, time, processing parameters such as airshed have been realized the magnanimity preparation of onion-like fullerene on the basis that reduces cost.Also have advantages such as simply quick, that generation onion-like fullerene shape is regular, and hollow is less when CVD prepares onion-like fullerene, this application for onion-like fullerene provides may.
The CVD method for making of onion-like fullerene of the present invention, its purposes is the higher onion-like fullerene of purity that can utilize this method to prepare magnanimity, and onion-like fullerene has engagement characteristics, electroconductibility, quantum mechanical effects (quantum well, little can the band etc.) etc. key property, become and to satisfy the electronic component that property requires, filter element, the material of Device elements such as senser element, superconducting material, biomaterial, medical material, the new pattern laser material, nonlinear optical material, information storage material, photoelectric material, catalystic material, waste water, new function materials such as waste-gas cleaning material, range of application is very wide, and application prospect is very tempting.
Description of drawings
The low power shape appearance figure of Fig. 1 onion-like fullerene
The shape appearance figure of the onion-like fullerene that belongs to covered with gold leaf in Fig. 2
Embodiment
Embodiment 1
Silica tube in the preheating oven is got 1g purity and is 99.9% ferrocene and places a porcelain boat, is placed on air intake one end of silica tube, and closed quartz tube feeds argon gas with the air in the emptying silica tube.After treating that temperature in the silica tube is raised to 900 ℃, open the valve of acetylene, argon gas and acetylene are mixed with 10: 1 ratio, Continuous Flow is through reaction chamber.Ferrocene in the heating porcelain boat, ferrocene is subjected to heat sublimation decompose to generate nano level small iron particle (catalyzer) and is blown in the stove by argon gas stream to react, acetylene forms carbon source in the catalyst surface cracking, and carbon source spreads by catalyzer, progressively generates onion-like fullerene.After ferrocene is exhausted, stop logical acetylene, treat that silica tube cool off in argon gas stream after, open the interior sedimentary onion-like fullerene black product that is rich in of silica tube take-off pipe;
Embodiment 2
Silica tube in the preheating oven is got 1.5g purity and is 99.9% ferrocene and places a porcelain boat, is placed on air intake one end of silica tube, and closed quartz tube feeds argon gas with the air in the emptying silica tube.After treating that temperature in the silica tube is raised to 1000 ℃, open the valve of acetylene, argon gas and acetylene are mixed with 9: 1 ratio, Continuous Flow is through reaction chamber.Ferrocene in the heating porcelain boat, ferrocene is subjected to heat sublimation decompose to generate nano level small iron particle (catalyzer) and is blown in the stove by argon gas stream to react, acetylene forms carbon source in the catalyst surface cracking, and carbon source spreads by catalyzer, progressively generates onion-like fullerene.After ferrocene is exhausted, stop logical acetylene, treat that silica tube cool off in argon gas stream after, open the interior sedimentary onion-like fullerene black product that is rich in of silica tube take-off pipe;
Embodiment 3
Silica tube in the preheating oven is got 2g purity and is 99.9% ferrocene and places a porcelain boat, is placed on air intake one end of silica tube, and closed quartz tube feeds argon gas with the air in the emptying silica tube.After treating that temperature in the silica tube is raised to 1000 ℃, open the valve of acetylene, argon gas and acetylene are mixed with 8: 1 ratio, Continuous Flow is through reaction chamber.Ferrocene in the heating porcelain boat, ferrocene is subjected to heat sublimation decompose to generate nano level small iron particle (catalyzer) and is blown in the stove by argon gas stream to react, acetylene forms carbon source in the catalyst surface cracking, and carbon source spreads by catalyzer, progressively generates onion-like fullerene.After ferrocene is exhausted, stop logical acetylene, treat that silica tube cool off in argon gas stream after, open the interior sedimentary onion-like fullerene black product that is rich in of silica tube take-off pipe;
Embodiment 4
Silica tube in the preheating oven is got 2.5g purity and is 99.9% ferrocene and places a porcelain boat, is placed on air intake one end of silica tube, and closed quartz tube feeds argon gas with the air in the emptying silica tube.After treating that temperature in the silica tube is raised to 1200 ℃, open the valve of acetylene, argon gas and acetylene are mixed with 10: 1 ratio, Continuous Flow is through reaction chamber.Ferrocene in the heating porcelain boat, ferrocene is subjected to heat sublimation decompose to generate nano level small iron particle (catalyzer) and is blown in the stove by argon gas stream to react, acetylene forms carbon source in the catalyst surface cracking, and carbon source spreads by catalyzer, progressively generates onion-like fullerene.After ferrocene is exhausted, stop logical acetylene, treat that silica tube cool off in argon gas stream after, open the interior sedimentary onion-like fullerene black product that is rich in of silica tube take-off pipe;
After product in the silica tube ground with mortar, get a little ultra-sonic dispersion in ethanol, with hanging drop on little grid copper mesh, use H-800 type transmission electron microscope (TEM) and JEM-2010 type high-resolution-ration transmission electric-lens (HRTEM after dry, acceleration voltage is 200kV, and point resolution is 0.19nm) it is observed sign.Discovery has the nano-onions shape soccerballene of monomeric nano-onions shape soccerballene and interior iron clad particulate to form.
Claims (1)
1. a chemical Vapor deposition process prepares the method for onion-like fullerene, it is characterized in that, be a kind of catalyzer that need not to prepare, directly adopt acetylene pyrolysis organo-metallic primitive reaction thing ferrocene to prepare the method for the onion-like fullerene that comes in every shape, the processing step of concrete preparation process is:
I. the silica tube in the preheating oven is at first got 1-2.5g purity then and is 99.9% ferrocene and places a porcelain boat, is placed on air intake one end of silica tube;
II. closed quartz tube feeds argon gas with the air in the emptying silica tube;
III. after treating that temperature in the silica tube is raised to 900-1200 ℃, open the valve of acetylene, make argon gas and acetylene with 8-10: 1 ratio mixes, and Continuous Flow is through reaction chamber;
IV. heat the ferrocene in the porcelain boat, ferrocene is subjected to heat sublimation decompose to generate nano level small iron particulate catalyzer and is blown in the stove by argon gas stream to react, acetylene forms carbon source after the catalyst surface cracking, carbon source spreads by catalyzer, progressively generates onion-like fullerene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410012502 CN1266307C (en) | 2004-08-25 | 2004-08-25 | Preparing onion shape fulven by chemical vapour phase deposition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410012502 CN1266307C (en) | 2004-08-25 | 2004-08-25 | Preparing onion shape fulven by chemical vapour phase deposition |
Publications (2)
| Publication Number | Publication Date |
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| CN1598046A CN1598046A (en) | 2005-03-23 |
| CN1266307C true CN1266307C (en) | 2006-07-26 |
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| CN 200410012502 Expired - Fee Related CN1266307C (en) | 2004-08-25 | 2004-08-25 | Preparing onion shape fulven by chemical vapour phase deposition |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1318294C (en) * | 2005-05-10 | 2007-05-30 | 太原理工大学 | Catalytic pyrolysis method for preparing metal particle-encapsulating onion-like Fullerene |
| CN100368080C (en) * | 2005-08-29 | 2008-02-13 | 天津大学 | Process for preparing carbon nano tube and carbon onion by Ni/Al catalyst chemical gas phase deposition |
| CN100341778C (en) * | 2006-02-23 | 2007-10-10 | 上海交通大学 | Solid process of preparing great diameter thin wall fullerene |
| CN101941077B (en) * | 2010-09-02 | 2013-09-18 | 太原理工大学 | Method for preparing magnetic metal iron-encapsulated fullerene carbon spheres |
| CN102568838A (en) * | 2011-11-30 | 2012-07-11 | 北京信息科技大学 | Onion-like graphite nanosphere counter electrode of sensitized solar cell and preparation method of onion-like graphite nanosphere counter electrode |
| CN110255626B (en) * | 2019-07-08 | 2020-03-03 | 太原理工大学 | Method for preparing surface-active onion-shaped carbon nanospheres based on vapor deposition |
| CN112791225A (en) * | 2019-11-14 | 2021-05-14 | 美国发现集团有限公司 | Nano robot for tumor treatment and preparation method thereof |
| EP4098612A4 (en) * | 2020-01-28 | 2024-02-07 | Univ Electro Communications | Fullerene structure, method for producing same, and device for producing same |
| CN112247153B (en) * | 2020-10-12 | 2023-04-21 | 内蒙古碳谷科技有限公司 | Preparation method of metal-fullerene composite nano powder |
| CN112758915B (en) * | 2020-12-30 | 2022-11-22 | 温州大学 | Preparation method of highly-graphitized mesoporous-rich nano-carbon onion |
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- 2004-08-25 CN CN 200410012502 patent/CN1266307C/en not_active Expired - Fee Related
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| CN1598046A (en) | 2005-03-23 |
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