CN105642917A - Preparation method for metal-clad carbon nano tube - Google Patents
Preparation method for metal-clad carbon nano tube Download PDFInfo
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- CN105642917A CN105642917A CN201610146466.1A CN201610146466A CN105642917A CN 105642917 A CN105642917 A CN 105642917A CN 201610146466 A CN201610146466 A CN 201610146466A CN 105642917 A CN105642917 A CN 105642917A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F9/26—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions using gaseous reductors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0549—Hollow particles, including tubes and shells
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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
Abstract
The invention discloses a preparation method for a metal-clad carbon nano tube. The preparation method includes the steps that (1) carbon source materials and a catalyst source are sprayed into a high-temperature reactor cavity full of reducing atmosphere from the top of a carbon nano tube synthesis furnace in the direction from top to bottom, and the catalyst source is subjected to pyrolysis and reduced by the reducing atmosphere, so that nano metal particles Ma are formed; the carbon source materials are subjected to pyrolysis to form highly active carbon atoms, and a carbon nano tube is formed under the catalysis of the Ma; and (2) at the same time of the reaction, a metal source solution is sprayed into the high-temperature reactor cavity full of the reducing atmosphere from the bottom of the carbon nano tube synthesis furnace in the direction from bottom to top, and the metal source forms nano metal particles Mb which deposit on the surface of the carbon nano tube, so that the metal-clad carbon nano tube is generated. By means of the preparation method, the self-agglomeration of the carbon nano tube after generation is avoided, and uniform dispersion of the metal and the carbon nano tube at the nanoscale is realized.
Description
Technical field
The present invention relates to field of material technology, be specifically related to the preparation method that a kind of original position (in-situ) synthesizes metallic cover CNT.
Background technology
CNT is the body of seamless, the hollow that the graphene sheet layer formed by carbon atom is rolled into, it has high axial strength and significantly high elastic modelling quantity, draw ratio is big, specific surface is big, high-temperature stable, anti-friction wear-resistant are good, heat conductivity is good, therefore can be used to the nano novel composite being widely used in manufacturing high intensity, good stability. In order to give full play to CNT excellent properties in the composite, it is necessary to CNT is effectively disperseed.
In recent years, the research for improving the dispersibility of CNT is concentrated mainly in post processing, by including the means such as ball milling mixing, surface chemical plating, alleviates the reunion degree of CNT self, and is uniformly dispersed in matrix material. And the potentiation that relatively uniform scattered CNT is in metallic matrix is clearly, the performance such as the tensile strength of material, yield strength, hardness, wearability is all obviously improved. But high speed ball milling easily damages carbon nano tube structure, low speed ball milling is opened CNT and is reunited inefficient, and Electroless Plating Procedure is complicated, coating inevitably contains other impurity (such as palladium etc.), and owing to processing cost is high, the reasons such as difficult quality control, above method all fails large-scale application in industrialized production.
Summary of the invention
The present invention is directed to the technical problem that prior art exists, it is provided that a kind of original position (in-situ) synthesizes metallic cover CNT and preparation method thereof. In CNT synthetic furnace, while synthesizing carbon nanotubes, generate vapor phase metal atom uniform deposition in carbon nano tube surface, forming metallic cover CNT, it is dispersed with the nanoscale of metal that original position (in-situ) realizes CNT.
For solving above-mentioned technical problem, the preparation method that a first aspect of the present invention provides a kind of metallic cover CNT, it comprises the steps:
(1) carbon source material and catalyst source from CNT synthetic furnace top, from up to down spray into the high-temperature reactor intracavity 800��1500 DEG C of full reducing atmosphere, catalyst source pyrolysis being reduced property atmosphere is reduced, and forms nano-metal particle Ma;Carbon source material pyrolysis becomes high-activity carbon atom, forms CNT under the catalysis of metallic particles Ma;
(2) while above-mentioned course of reaction carries out, by source metal solution from bottom CNT synthetic furnace, the bottom-up high-temperature reactor intracavity spraying into above-mentioned full reducing atmosphere, source metal forms nano-metal particle Mb and is deposited in step (1) carbon nano tube surface generated, and original position (in-situ) generates metallic cover CNT.
The thickness (and weight) of carbon nano tube surface metallic cover can be regulated by material charging rate (mol/hr) ratio of upper and lower jet pipe.
Preferably, in above-mentioned steps (1) and step (2), the temperature in reactor cavity is preferably 1000��1200 DEG C.
Preferably, described carbon source material is hydrocarbon selected from methanol, ethanol, benzene or toluene etc. or one or more mixing in hydrocarbon oxygen compound.
Preferably, one or more in hydrogen, carbon monoxide or ammonia gas of described reducing atmosphere; Or the gaseous mixture of above-mentioned reducibility gas and noble gas, wherein indifferent gas is the one in argon or nitrogen or gaseous mixture.
Preferably, described catalyst source is selected from metal inorganic salt or metallo-organic compound. One or more the mixing in ferrous sulfate, nitric acid molybdenum or tungsten chloride of the described metal inorganic salt; One or more the mixing in cobalt oxalate, nickel acetylacetonate or ferrocene of the described metallo-organic compound.
Preferably, described source metal is selected from metal inorganic salt or metallo-organic compound, one or more the mixing in copper sulfate, nickel nitrate, silver nitrate or aluminum chloride of the described metal inorganic salt; One or more the mixing in Schweinfurt green, nickel acetylacetonate or ferrocene of the described metallo-organic compound.
Preferably, described metallic element Ma and Mb, can be identical element or different element.
Preferably, described metallic cover CNT, carbon pipe diameter is 5��100nm, and the metal thickness in its coated with uniform is 1��100nm, and nanocarbon/metal weight ratio is 0.1��1.0.
Preferably, after described carbon source material mixes with catalyst source, from up to down spray into the high-temperature reactor intracavity of full reducing atmosphere from the same pipeline at CNT synthetic furnace top.
A second aspect of the present invention provides a kind of metallic cover CNT, and it prepares by the following method:
(1) carbon source material and catalyst source from CNT synthetic furnace top, from up to down spray into the high-temperature reactor intracavity 800��1500 DEG C of full reducing atmosphere, catalyst source pyrolysis being reduced property atmosphere is reduced, and forms nano-metal particle Ma; Carbon source material pyrolysis becomes high-activity carbon atom, forms CNT under the catalysis of Ma;
(2) while above-mentioned course of reaction carries out, by source metal solution from bottom CNT synthetic furnace, the bottom-up high-temperature reactor intracavity spraying into above-mentioned full reducing atmosphere, source metal forms nano-metal particle Mb and is deposited in step (1) carbon nano tube surface generated, in-situ preparation metallic cover CNT.
Preferably, described metallic element Mb is selected from nickel, copper, ferrum, silver.
Preferably, the carbon pipe diameter of described metallic cover CNT is 5��100nm, and the metal thickness in its coated with uniform is 1��100nm, and nanocarbon/metal weight ratio is 0.1��1.0.
The preparation method of the fabricated in situ metallic cover CNT of the present invention. In same reactor, by while CVD synthesizing carbon nanotubes, by metal (nickel, copper, ferrum, silver etc.) atomic deposition in carbon nano tube surface, form equally distributed metal coating.
Prepared by the preparation method of metallic cover CNT provided by the invention, both avoided self reuniting after CNT generates, and achieves again dispersed at nanoscale of metal and CNT. Compare the CNT post-processing approach such as ball milling and chemical plating, original position (in-situ) the synthetic method production efficiency that the present invention adopts is higher, newborn metallic atom is combined more firm with newborn CNT, building-up process does not use the heavy metals such as palladium, does not introduce other impurity yet, and the more readily dispersible use of the CNT of metallic cover, process without postorder and processing, be conducive to keeping structure and the feature of primary CNT.
Accompanying drawing explanation
Fig. 1 is the synthetic method schematic diagram that the present invention prepares metallic cover CNT
Fig. 2 is the XRD curve of metallic cover carbon nanotube product shown in the embodiment of the present invention 1,
Fig. 3 is the SEM photograph of metallic cover CNT shown in the embodiment of the present invention 1 (carbon content 50%).
Wherein, 1 is synthetic furnace, and 2 is rewinding mouth.
Detailed description of the invention
Below in conjunction with accompanying drawing, the specific embodiment of the invention is described.
Embodiment 1
Under hydrogen, nitrogen mixed gas protection; stove is warming up to 800��1500 DEG C; the methanol solution (0.10mol/L ferrum) of ferrocene is sprayed into synthetic furnace from synthetic furnace top; the tetrahydrofuran solution (1.0mol/L nickel) of nickel acetylacetonate is sprayed into synthetic furnace from spout bottom synthetic furnace simultaneously; the charging rate of the tetrahydrofuran solution of the charging rate/nickel acetylacetonate of the methanol solution of ferrocene is 1/7; put into synthetic furnace, the nickel coated CNT that nickel carbon weight ratio is 1 can be obtained.
Fig. 2 is the XRD testing result of the said goods, it was demonstrated that nickel metal about 50% in product, carbon nanotubes about 50%, the grain size 20��50nm of nickel.
Fig. 3 is product scanning electron microscope testing result, and diameter is the carbon nano tube surface that 20��50nm metallic nickel granule is evenly distributed on that diameter is 50��100nm, without substantially reuniting between CNT.
Embodiment 2
Under hydrogen, nitrogen mixed gas protection; stove is warming up to 800��1500 DEG C; the alcoholic solution (0.10mol/L ferrum) of ferrous sulfate is sprayed into synthetic furnace from synthetic furnace top; the aqueous solution (1.0mol/L nickel) of nickel nitrate is sprayed into synthetic furnace from spout bottom synthetic furnace simultaneously; the charging rate of the aqueous solution of the charging rate/nickel nitrate of the alcoholic solution of ferrous sulfate is 1/7; put into synthetic furnace, the nickel coated CNT that nickel carbon weight ratio is 1 can be obtained.
Embodiment 3
Under hydrogen, nitrogen mixed gas protection; stove is warming up to 800��1500 DEG C; the toluene solution (0.10mol/L molybdenum) of nitric acid molybdenum is sprayed into synthetic furnace from synthetic furnace top; the aqueous solution (1.0mol/L copper) of copper sulfate is sprayed into synthetic furnace from spout bottom synthetic furnace simultaneously; the charging rate of the aqueous solution of the charging rate/copper sulfate of the toluene solution of nitric acid molybdenum is 1/7; put into synthetic furnace, the nickel coated CNT that nickel carbon weight ratio is 1 can be obtained.
The ultimate principle of the present invention, principal character and advantages of the present invention have more than been shown and described. Skilled person will appreciate that of the industry; the present invention is not by the restriction of examples detailed above; described in examples detailed above and description is that principles of the invention is described; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements both fall within the claimed scope of the invention. Claimed scope is defined by appending claims and equivalent thereof.
Claims (10)
1. the preparation method of a metallic cover CNT, it is characterised in that it comprises the steps:
(1) carbon source material and catalyst source from CNT synthetic furnace top, from up to down spray into the high-temperature reactor intracavity 800��1500 DEG C of full reducing atmosphere, catalyst source pyrolysis being reduced property atmosphere is reduced, and forms nano-metal particle Ma;Carbon source material pyrolysis becomes high-activity carbon atom, forms CNT under the catalysis of metallic particles Ma;
(2) while above-mentioned course of reaction carries out, by source metal solution from bottom CNT synthetic furnace, the bottom-up high-temperature reactor intracavity spraying into above-mentioned full reducing atmosphere, source metal forms nano-metal particle Mb and is deposited in step (1) carbon nano tube surface generated, in-situ preparation metallic cover CNT.
2. preparation method according to claim 1, it is characterised in that the described carbon source material one or more mixing in methanol, ethanol, benzene or toluene; One or more in hydrogen, carbon monoxide or ammonia of described reducing atmosphere.
3. preparation method according to claim 1 or claim 2, it is characterised in that described catalyst source is selected from metal inorganic salt or metallo-organic compound; Described reducing atmosphere is the mixing gas of reducibility gas and noble gas.
4. preparation method according to claim 3, it is characterised in that the described metal inorganic salt one or more mixing in ferrous sulfate, nitric acid molybdenum or tungsten chloride; One or more the mixing in cobalt oxalate, nickel acetylacetonate or ferrocene of the described metallo-organic compound.
5. preparation method according to claim 1, it is characterised in that described source metal is selected from metal inorganic salt or metallo-organic compound.
6. preparation method according to claim 5, it is characterised in that the described metal inorganic salt one or more mixing in copper sulfate, nickel nitrate, silver nitrate or aluminum chloride; One or more the mixing in Schweinfurt green, nickel acetylacetonate or ferrocene of the described metallo-organic compound.
7. preparation method according to claim 1, it is characterised in that described metallic element Ma and Mb is identical element or different element.
8. a metallic cover CNT, its method described in any one of claim 1-7 prepares.
9. metallic cover CNT according to claim 8, it is characterised in that described metal is selected from nickel, copper, ferrum, silver.
10. metallic cover CNT according to claim 8, it is characterised in that the carbon pipe diameter of described metallic cover CNT is 5��100nm, the metal thickness in carbon nano tube surface cladding is 1��100nm, and nanocarbon/metal weight ratio is 0.1��1.0.
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| CN201610146466.1A CN105642917A (en) | 2016-03-15 | 2016-03-15 | Preparation method for metal-clad carbon nano tube |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108213447A (en) * | 2016-12-12 | 2018-06-29 | 湖南久泰冶金科技有限公司 | A kind of metal atomization powder chemical combination tower room |
| CN109148905A (en) * | 2018-09-30 | 2019-01-04 | 北京海得利兹新技术有限公司 | A kind of polymer dielectric film fuel cell high activity elctro-catalyst and preparation method thereof |
| CN110586153A (en) * | 2019-08-27 | 2019-12-20 | 浙江工业大学 | Application of carbon nano tube embedded metal particle catalyst in ammonia decomposition reaction |
| CN112938936A (en) * | 2021-03-17 | 2021-06-11 | 西安交通大学 | Metal atom loaded nano composite material and preparation method thereof |
| CN113026351A (en) * | 2021-03-09 | 2021-06-25 | 常州大学 | Preparation method of carbon nanotube metal composite conductive fiber, product and application thereof |
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| CN113026351A (en) * | 2021-03-09 | 2021-06-25 | 常州大学 | Preparation method of carbon nanotube metal composite conductive fiber, product and application thereof |
| CN112938936A (en) * | 2021-03-17 | 2021-06-11 | 西安交通大学 | Metal atom loaded nano composite material and preparation method thereof |
| CN112938936B (en) * | 2021-03-17 | 2023-08-15 | 西安交通大学 | Metal atom loaded nanocomposite and preparation method thereof |
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