CN101585531B - Preparation method of carbon nano cage - Google Patents
Preparation method of carbon nano cage Download PDFInfo
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- CN101585531B CN101585531B CN2009100533147A CN200910053314A CN101585531B CN 101585531 B CN101585531 B CN 101585531B CN 2009100533147 A CN2009100533147 A CN 2009100533147A CN 200910053314 A CN200910053314 A CN 200910053314A CN 101585531 B CN101585531 B CN 101585531B
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- nano cages
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Abstract
The invention provides a preparation method of carbon nano cage belonging to the field of nano technique, which includes the following steps: the steps one, heating copper acetate; the steps two, infusing the mixture gas and copper acetate into the environment at 600-900 DEG C, reacting, collecting product, purifying and obtaining carbon nano cage; the mixture is composed of acetylene and indifferent gas, and the flow quantity of acetylene is 20-80 ml/min. The carbon nano cage with a well-regulated external shape provided by the invention, compared with nano cages of other shapes, is easy to realize self-assembly and large-scale production with very low preparation cost.
Description
Technical field
The present invention relates to a kind of preparation method of field of nanometer technology, specifically is a kind of preparation method of nano cages.
Background technology
Nano cages and CNT (carbon nano-tube), diamond are the same, are a kind of thermodynamic instability of carbon but the more stable metastable state material of kinetics.Nano cages is made up of the multilayer graphite linings, and its aperture is between 2～100nm, and surface tissue is similar to porous carbon, has bigger specific surface area.The unique texture of nano cages has determined them to have colourful physics, chemical property.At present, it demonstrates great application prospect as a kind of novel low-dimensional nano-functional material in fields such as superconduction, semi-conductor, catalyzer, biology, medical science.
Up to the present, many relevant methods that prepare nano cages have been reported, wherein more common method has: (1) carbon method of evaporation, as arc process, electrical resistance heating, electron beam irradiation method, laser evaporation graphite method, vacuum heat treatment method, plasma method etc.; (2) catalytic pyrolysis method is comprising the disproportionation of CO, C
2H
2, propylene etc. vapour-phase pyrolysis, the pyrolysis of ferrocene; The normal metals such as Fe, Co, Ni that use are made catalyzer in these class methods; (3) benzene flame combustion process, the benzene that diluted in hydrogen is crossed are burnt in oxygen can make nano cages, adopts the productive rate of different experiment condition may command nanocages; (4) conversion of carbon containing inorganics, SiC is only binary compound in the SiC-C phasor, when base reservoir temperature is 600 ℃, uses the laser direct irradiation, can be at big, the less nano cages of defective of SiC the inside generation size of crystallization.Other method such as explosion method, the hybrid gel that is mixed and made into pitch and iron nitrate is a raw material, can prepare the nano cages with good electrical magnetic property.In order to last method, comprise the nano cages of United States Patent (USP) the 6063243rd, Chinese patent 1454839A, No. 19740389 disclosed preparation of German Patent, be the spheric nano material, do not obtain the nano cages of other shapes.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of nano cages is provided.The nano cages of the present invention's preparation has regular profile, compare the easier realization self-assembly of nanocages of other shape, and preparation cost is very low, easily accomplishes scale production.
The present invention is achieved by the following technical solutions, the present invention includes following steps:
Step 1, heating copper acetate;
Step 2 feeds mixed gas and venus crystals in 600 ℃～900 ℃ the environment, and product is collected in reaction, and purifying obtains nano cages;
Described gas mixture is made up of acetylene and rare gas element, and the flow of acetylene is 20～80ml/min.
In the step 1, described 100 ℃～140 ℃ following insulations 20～40 minutes that are heated to be.
In the step 2, the flow of described rare gas element is 20～60l/h.
In the step 2, described purifying adopts the salpeter solution oxidation style: reaction product is imported in the salpeter solution of 1.2g/ml, ultrasonic vibration 3 hours is heated to the solution boiling then, is aided with magnetic in the heat-processed and stirs.
The present invention makes catalyzer become powder by macrobead by the crystal water in the heat treated removal catalyzer, to improve the transformation efficiency and the flowability of catalyzer in the subsequent reactions step; The gas mixture of forming with the catalyzer handled with by the gas and the rare gas element of carbonaceous sources is during by the high-temperature zone, catalytic cracking reaction can take place, generate nano cages, the height direct relation of temperature of reaction the grain fineness number size that forms nanometer copper, it will determine the size of nano cages, by the flow of control acetylene and other gases, the wall thickness of may command nano cages.
Compared with prior art; the present invention has following beneficial effect: the nano cages of the present invention's preparation has regular profile; compare the easier realization self-assembly of nanocages of other shape; and preparation cost is very low; easily accomplish scale production, have more advantage and potentiality in nano electron device design and manufacture view.
Embodiment
Embodiment 1
Step 1,100 ℃ of following heating copper acetate 40 minutes, cooling afterwards, venus crystals becomes fine powdered;
Step 2 is packed the venus crystals powder in the funnel into, is placed into the quartz glass tube top of setting; The temperature of quartz glass tube is 900 ℃, feeds mixed gas, and the flow of acetylene is 20ml/min, and the flow of argon gas is 60l/h; Open the valve of funnel, make the venus crystals powder pass quartz glass tube from top to down, product is collected in reaction; Reaction product is imported in the salpeter solution of 1.2g/ml, ultrasonic vibration 3 hours is heated to the solution boiling then, is aided with magnetic in the heat-processed and stirs; Obtain the product of purifying at last, i.e. nano cages.
The nano cages that present embodiment obtains is the cubes of rule, about 280 nanometers of the length of side, about 30 nanometers of the wall thickness of nano cages.
Embodiment 2
Step 1,140 ℃ of following heating copper acetate 20 minutes, cooling afterwards, venus crystals becomes fine powdered;
Step 2 is packed the venus crystals powder in the funnel into, is placed into the quartz glass tube top of setting; The temperature of quartz glass tube is 600 ℃, feeds mixed gas, and the flow of acetylene is 80ml/min, and the flow of nitrogen is 20l/h; Open the valve of funnel, make the venus crystals powder pass quartz glass tube from top to down, product is collected in reaction; Reaction product is imported in the salpeter solution of 1.2g/ml, ultrasonic vibration 3 hours is heated to the solution boiling then, is aided with magnetic in the heat-processed and stirs; Obtain the product of purifying at last, i.e. nano cages.
The nano cages that present embodiment obtains is the cubes of rule, about 30 nanometers of the length of side, about 3 nanometers of the wall thickness of nano cages.
Embodiment 3
Step 1,120 ℃ of following heating copper acetate 30 minutes, cooling afterwards, venus crystals becomes fine powdered;
Step 2 is packed the venus crystals powder in the funnel into, is placed into the quartz glass tube top of setting; The temperature of quartz glass tube is 750 ℃, feeds mixed gas, and the flow of acetylene is 50ml/min, and the flow of argon gas is 40l/h; Open the valve of funnel, make the venus crystals powder pass quartz glass tube from top to down, product is collected in reaction; Reaction product is imported in the salpeter solution of 1.2g/ml, ultrasonic vibration 3 hours is heated to the solution boiling then, is aided with magnetic in the heat-processed and stirs; Obtain the product of purifying at last, i.e. nano cages.
The nano cages that present embodiment obtains is the cubes of rule, about 200 nanometers of the length of side, about 20 nanometers of the wall thickness of nano cages.
Embodiment 4
Step 1,130 ℃ of following heating copper acetate 25 minutes, cooling afterwards, venus crystals becomes fine powdered;
Step 2 is packed the venus crystals powder in the funnel into, is placed into the quartz glass tube top of setting; The temperature of quartz glass tube is 680 ℃, feeds mixed gas, and the flow of acetylene is 40ml/min, and the flow of helium is 30l/h; Open the valve of funnel, make the venus crystals powder pass quartz glass tube from top to down, product is collected in reaction; Reaction product is imported in the salpeter solution of 1.2g/ml, ultrasonic vibration 3 hours is heated to the solution boiling then, is aided with magnetic in the heat-processed and stirs; Obtain the product of purifying at last, i.e. nano cages.
The nano cages that present embodiment obtains is the cubes of rule, about 150 nanometers of the length of side, about 15 nanometers of the wall thickness of nano cages.
Embodiment 5
Step 1,110 ℃ of following heating copper acetate 35 minutes, cooling afterwards, venus crystals becomes fine powdered;
Step 2 is packed the venus crystals powder in the funnel into, is placed into the quartz glass tube top of setting; The temperature of quartz glass tube is 820 ℃, feeds mixed gas, and the flow of acetylene is 65ml/min, and the flow of argon gas is 50l/h; Open the valve of funnel, make the venus crystals powder pass quartz glass tube from top to down, product is collected in reaction; Reaction product is imported in the salpeter solution of 1.2g/ml, ultrasonic vibration 3 hours is heated to the solution boiling then, is aided with magnetic in the heat-processed and stirs; Obtain the product of purifying at last, i.e. nano cages.
The nano cages that present embodiment obtains is the cubes of rule, about 250 nanometers of the length of side, about 10 nanometers of the wall thickness of nano cages.
Claims (2)
1. the preparation method of a nano cages is characterized in that, comprises the steps:
Step 1, heating copper acetate;
Step 2 feeds mixed gas and venus crystals in 600 ℃～900 ℃ the environment, and product is collected in reaction, and purifying obtains nano cages;
Described gas mixture is made up of acetylene and rare gas element, and the flow of acetylene is 20～80ml/min;
Described 100 ℃～140 ℃ following insulations 20～40 minutes that are heated to be;
The flow of described rare gas element is 20～60l/h.
2. the preparation method of nano cages according to claim 1 is characterized in that, in the step 2, described purifying adopts the salpeter solution oxidation style: reaction product is imported in the salpeter solution of 1.2g/ml, ultrasonic vibration 3 hours is heated to the solution boiling then, is aided with magnetic in the heat-processed and stirs.
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| CN2009100533147A CN101585531B (en) | 2009-06-18 | 2009-06-18 | Preparation method of carbon nano cage |
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| CN2009100533147A CN101585531B (en) | 2009-06-18 | 2009-06-18 | Preparation method of carbon nano cage |
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| CN101585531A CN101585531A (en) | 2009-11-25 |
| CN101585531B true CN101585531B (en) | 2010-12-08 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103787305B (en) * | 2014-02-19 | 2015-11-18 | 中国科学院上海硅酸盐研究所 | Combustion method prepares the method for hollow nano cages |
| CN104961119A (en) * | 2015-05-26 | 2015-10-07 | 南京大学（苏州）高新技术研究院 | Preparation method of boron and nitrogen co-doped hollow carbon nanocage |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040258603A1 (en) * | 1998-09-18 | 2004-12-23 | William Marsh Rice University | High-yield method of endohedrally encapsulating species inside fluorinated fullerene nanocages |
| CN1751989A (en) * | 2004-09-20 | 2006-03-29 | 三星Sdi株式会社 | Method of preparing carbon nanocages |
| CN1872675A (en) * | 2006-06-22 | 2006-12-06 | 上海交通大学 | Method for preparing hollow Nano carbon balls in graphite structure under solid state |
-
2009
- 2009-06-18 CN CN2009100533147A patent/CN101585531B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040258603A1 (en) * | 1998-09-18 | 2004-12-23 | William Marsh Rice University | High-yield method of endohedrally encapsulating species inside fluorinated fullerene nanocages |
| CN1751989A (en) * | 2004-09-20 | 2006-03-29 | 三星Sdi株式会社 | Method of preparing carbon nanocages |
| CN1872675A (en) * | 2006-06-22 | 2006-12-06 | 上海交通大学 | Method for preparing hollow Nano carbon balls in graphite structure under solid state |
Non-Patent Citations (2)
| Title |
|---|
| A.K.SCHAPER et al.Copper nanoparticles encapsulated in multi-shell carbon cages.《Applied Physics A》.2003,第78卷73-77. * |
| XU Bing-she.Prospects and research progress in nano onion-like fullerenes.《新型炭材料》.2008,第23卷(第4期),289-301. * |
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