CN102779986A - Preparation method of nanocomposite material with core shell structure - Google Patents
Preparation method of nanocomposite material with core shell structure Download PDFInfo
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- CN102779986A CN102779986A CN2012102362309A CN201210236230A CN102779986A CN 102779986 A CN102779986 A CN 102779986A CN 2012102362309 A CN2012102362309 A CN 2012102362309A CN 201210236230 A CN201210236230 A CN 201210236230A CN 102779986 A CN102779986 A CN 102779986A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a nanocomposite material with a core shell structure. According to the preparation method, alcoholic solution of copper-containing precursors is atomized and is then introduced into a burning reactor for carrying out hydrolysis reaction, and meanwhile, acetylene gas diluted by nitrogen gas is introduced into the burning reactor. In the flame, nano-copper particles are firstly generated, then, acetylene is resolved on the surfaces of the nano-copper particles to generate nanometer carbon tubes, and finally, the nanometer copper/nanometer carbon tube composite material with the core shell structure is obtained. The method has the advantages that the equipment and process are simple, the continuous production can be realized, the industrial implementation is easy, and the preparation method can be applied to fields of lithium ion batteries, conducting materials, field emission reinforcing material and the like.
Description
Technical field
The present invention relates to a kind of preparation method with nano composite material of nucleocapsid structure, particularly, relate to the preparation method of copper/CNT composite material, it can be applicable to fields such as lithium ion battery, electric conducting material, an emission reinforcing material.
Background technology
Nano copper particle is because its unique physics and chemical property are applied in fields such as catalysis, optics, electronics widely.But, oxidized inevitably at air owing to be nano-scale, from limit largely its further development.In order to reduce even to stop the aerial oxidation of copper nano particles, a feasible approach is that it is carried out finishing, as carries out the coating of carbon or silicon dioxide, and the carbon coating is the choosing of the best.At present, the method for preparing carbon-coated nano copper particle mainly contains liquid chemical method, arc discharge method, spray pyrolysis, chemical gaseous phase chemical deposition etc.Said method receives many conditions to a certain extent for example need be to the multistep processing of product, high equipment requirements and high energy consumption, and particularly the mode of operation at intermittence has seriously restricted its suitability for industrialized production.The spray burning method has that simple fast and the product purity advantages of higher reaction simultaneously itself is to react energy is provided by the burning of solvent, has reduced energy consumption effectively, is one of preparation method of nano material of tool industrial prospect.
Summary of the invention
The object of the present invention is to provide the preparation method that a kind of technology is simple, be easy to the nanometer copper/CNT composite material with nucleocapsid structure of industrializing implementation
The design of patent of the present invention is following:
The present invention adopts the spray burning reactor, and the alcoholic solution of cupric presoma atomizing back is fed combustion reactor be hydrolyzed reaction, the acetylene gas of feeding nitrogen dilution in reactor simultaneously.Nano copper particle at first generates in flame, and acetylene decomposes the generation CNT on the surface of nano copper particle then, finally obtains a kind of nanometer copper/CNT composite material with nucleocapsid structure.This method apparatus and process is simple, can be continuously produced, and is easy to industrializing implementation.
Concrete technical scheme is following:
A kind of preparation method with nano composite material of nucleocapsid structure comprises the steps:
Cupric presoma and solvent are mixed with solution, feed combustion reactor be hydrolyzed reaction, the acetylene gas of feeding nitrogen dilution in said combustion reactor simultaneously behind the said solution atomization; In the flame of said combustion reactor, at first generate nano copper particle, said acetylene gas decomposes the generation CNT on the surface of said nano copper particle, finally obtains a kind of nanometer copper/CNT composite material with nucleocapsid structure;
Wherein,
The molar concentration of said cupric precursor solution is at 0.1～0.5 mol/L, and inlet amount is 3～10 ml/min;
The inlet amount of said combustion reactor air is 1.0～3.0 m
3/ h;
The flow of said acetylene gas is 0.02～0.1 m
3/ h, the flow of said nitrogen are 0.3～1.0 m
3/ h;
The reaction temperature of said hydrolysis is 1200～1800 ℃.
The inorganic salts compound that said cupric presoma is a copper, said solvent are flammable liquid alcohols.
Said cupric presoma copper chloride, copper nitrate or copper sulphate, said solvent is methyl alcohol or ethanol.
The particle diameter of nano copper particle is 20～50nm in the nanometer copper/CNT composite material of said nucleocapsid structure, and the length of CNT is 200～500nm.CNT is coated on the surface of nano copper particle.
Preparation method's technology of the nanometer copper/CNT composite material with nucleocapsid structure of the present invention is simple, and operation need not reprocessing easily, and material structure is stable, can be applicable to fields such as lithium ion battery, electric conducting material, an emission reinforcing material.
Description of drawings
Fig. 1 is the transmission electron microscope photo of embodiment 1 product;
Fig. 2 is the transmission electron microscope photo of embodiment 2 products;
Fig. 3 is the XRD spectra of embodiment 1 product.
Embodiment
For example the present invention is specifically described through enforcement below.Be necessary to be pointed out that at this; Following examples only are used for the present invention is described further; Can not be interpreted as the restriction to protection range of the present invention, some nonessential improvement and adjustment that the professional and technical personnel in this field content according to the present invention is made still belong to protection scope of the present invention.
Each response parameter is following:
The molar concentration of cupric precursor solution is at 0.1～0.5mol/L, and inlet amount is 3～10 ml/min;
The inlet amount of combustion reactor air is 1.0～3.0 m
3/ h;
The flow of acetylene gas is 0.02～0.1 m
3/ h, the flow of nitrogen are 0.3～1.0 m
3/ h;
Reaction temperature is 1200～1800 ℃.
Embodiment 1
Utilize the spray burning reactor, copper chloride and ethanol are mixed with solution, the atomizing back feeds combustion reactor and carries out combustion reaction, and wherein, the molar concentration of copper chloride is 0.5mol/L, and feed rate is 3ml/min, and the inlet amount of combustion air is 3.0 m
3/ h, reaction temperature is 1200 ℃.In reactor, feeding the acetylene gas of nitrogen dilution simultaneously, is 1 m in order to the nitrogen flow that dilutes acetylene
3/ h, acetylene 0.02 m
3/ h.Nano copper particle generates earlier in flame; Acetylene decomposes the generation CNT on the surface of nanometer copper; Finally obtain a kind of nanometer copper/CNT composite material with nucleocapsid structure, the electromicroscopic photograph of product is as shown in Figure 1, the XRD photo is as shown in Figure 3, wherein; Nano copper particle particle diameter as nuclear is 50nm, and the carbon length of tube of clad nano copper particle is 200nm.
Utilize the spray burning reactor, copper nitrate and methyl alcohol are mixed with solution, the atomizing back feeds combustion reactor and carries out combustion reaction, and wherein, the molar concentration of copper nitrate is 0.1mol/L, and feed rate is 10 ml/min, and the inlet amount of combustion air is 1.0 m
3/ h, reaction temperature is 1800 ℃.In reactor, feeding the acetylene gas of nitrogen dilution simultaneously, is 0.3m in order to the nitrogen flow that dilutes acetylene
3/ h, acetylene 0.1 m
3/ h.Nano copper particle generates earlier in flame, and acetylene decomposes the generation CNT on the surface of nanometer copper, finally obtains a kind of nanometer copper/CNT composite material with nucleocapsid structure, and the electromicroscopic photograph of product is as shown in Figure 2.Wherein, the nano copper particle particle diameter is 20nm, and the carbon length of tube is 500nm.
Embodiment 3
Utilize the spray burning reactor, copper sulphate and ethanol are mixed with solution, the atomizing back feeds combustion reactor and carries out combustion reaction, and wherein, the molar concentration of copper sulphate is 0.3mol/L, and feed rate is 7 ml/min, and the inlet amount of combustion air is 2.0m
3/ h, reaction temperature is 1500 ℃.In reactor, feeding the acetylene gas of nitrogen dilution simultaneously, is 0.5m in order to the nitrogen flow that dilutes acetylene
3/ h, acetylene 0.05 m
3/ h.Nano copper particle generates earlier in flame, and acetylene decomposes the generation CNT on the surface of nanometer copper, finally obtains a kind of nanometer copper/CNT composite material with nucleocapsid structure, and wherein, the nano copper particle particle diameter is 30nm, and the carbon length of tube is 400nm.
Claims (4)
1. the preparation method with nano composite material of nucleocapsid structure is characterized in that, comprises the steps:
Cupric presoma and solvent are mixed with solution, feed combustion reactor be hydrolyzed reaction, the acetylene gas of feeding nitrogen dilution in said combustion reactor simultaneously behind the said solution atomization; In the flame of said combustion reactor, at first generate nano copper particle, said acetylene gas decomposes the generation CNT on the surface of said nano copper particle, finally obtains a kind of nanometer copper/CNT composite material with nucleocapsid structure;
Wherein,
The molar concentration of said cupric precursor solution is at 0.1～0.5 mol/L, and inlet amount is 3～10 ml/min;
The inlet amount of said combustion reactor air is 1.0～3.0 m
3/ h;
The flow of said acetylene gas is 0.02～0.1 m
3/ h, the flow of said nitrogen are 0.3～1.0 m
3/ h;
The reaction temperature of said hydrolysis is 1200～1800 ℃.
2. preparation method according to claim 1 is characterized in that, the inorganic salts compound that said cupric presoma is a copper, said solvent are flammable liquid alcohols.
3. preparation method according to claim 2 is characterized in that, said cupric presoma is copper chloride, copper nitrate or copper sulphate, and said solvent is methyl alcohol or ethanol.
4. preparation method according to claim 1 is characterized in that, the particle diameter of nano copper particle is 20～50nm in the nanometer copper/CNT composite material of said nucleocapsid structure, and the length of CNT is 200～500nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104637569A (en) * | 2013-11-07 | 2015-05-20 | 爱迪克科技股份有限公司 | Lead-free nano conductive paste material |
| CN104841924B (en) * | 2014-02-19 | 2017-11-21 | 中国科学院大连化学物理研究所 | A kind of preparation method of the fully enclosed metal nanoparticle of carbon |
| CN110697686A (en) * | 2019-09-17 | 2020-01-17 | 北京化工大学 | Method for preparing carbon nano tube by heating powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101954480A (en) * | 2010-11-08 | 2011-01-26 | 华东理工大学 | Method for preparing carbon-coated core-shell nanoparticles continuously |
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2012
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101954480A (en) * | 2010-11-08 | 2011-01-26 | 华东理工大学 | Method for preparing carbon-coated core-shell nanoparticles continuously |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104637569A (en) * | 2013-11-07 | 2015-05-20 | 爱迪克科技股份有限公司 | Lead-free nano conductive paste material |
| CN104841924B (en) * | 2014-02-19 | 2017-11-21 | 中国科学院大连化学物理研究所 | A kind of preparation method of the fully enclosed metal nanoparticle of carbon |
| CN110697686A (en) * | 2019-09-17 | 2020-01-17 | 北京化工大学 | Method for preparing carbon nano tube by heating powder |
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Inventor after: Li Chunzhong Inventor after: Hu Yanjie Inventor after: Qian Qi Inventor after: Wang Yundong Inventor before: Li Chunzhong Inventor before: Hu Yanjie Inventor before: Qian Qi Inventor before: Wang Yundong |
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Application publication date: 20121114 |