Hollow carbon nanoparticles, carbon nanomaterial and method for its production

FIELD: nanotechnology.

SUBSTANCE: group of inventions relates to the field of nanotechnologies, in particular to the technologies of production of carbon nanostructures and nanomaterials for use as substrates for applied catalysts, high-strength fillers, and relates to hollow carbon nanoparticles, carbon nanomaterial and method of its preparation. The carbon nanoparticle has an average size of not less than 5 nm, and comprises a central inner cavity and an outer closed casing enclosing the inner cavity on all sides. At that the outer casing comprises at least a pair of separate carbon layers. The carbon material comprises a mixture of hollow carbon nanoparticles comprising a central inner cavity and an outer closed casing enclosing the inner cavity on all sides. At that the outer casing comprises at least a pair of separate carbon layers, and the single-walled and double-walled carbon nanotubes. The method of producing the carbon material comprising a mixture of hollow carbon nanoparticles and single-walled and double-walled carbon nanotubes comprises catalytic decomposition of hydrocarbons at a temperature of 600-1200°C with obtaining a mixture of carbon nanoparticles, which is separated from the gaseous products and annealed at 1700-2400°C in the atmosphere of inert gas.

EFFECT: invention provides obtaining of novel carbon nanoparticles and nanomaterials having high strength at low weight, which can be used to create new composite light and high strength materials.

4 cl, 2 dwg, 3 ex

 

The invention relates to carbon nanostructures, carbon nanomaterials based on carbon nanostructures, technology for the production of carbon nanomaterials, and can be used for the production of carbon nanostructures and materials, which in turn can be used as substrates for supported catalysts, high-strength fillers and other

The first information about these nanostructures, such as nanotubes, first appeared in 1991, and now we already know quite a large number of carbon nanostructures.

Thus, the known carbon nanofibres is a nanostructure consisting of thin filaments with a diameter of 3-15 microns, formed of carbon atoms [U.S. Patent No. 4 663 230, IPC D01F 9/127, D01F 9/12].

Also known carbon nanotube - carbon fiber with a hole where the wall is, basically, a single layer of carbon atoms [U.S. Patent No. 5 424 054, IPC D01F 9/127, D01F 9/12].

Known carbon nanostructures onion shape - neolocality formed nested in one another carbon spheres [RF Patent №2094370].

Known fullerene - molecular compound belonging to the class of allotropic forms of carbon, representing a closed convex polyhedra composed of an even number tricoordinated carbon atoms [Sokolov, C. I., Stankevich is.In. Fullerenes - new allotropic forms of carbon: structure, electronic structure and chemical properties//USP, T. 62 (5), S. 455, 1993].

Known and others not mentioned here, carbon nanostructures and their number is constantly growing. Part of the carbon nanostructures have already found application in several industries as additives to various materials that change properties of these materials. For example, carbon nanofibres give composite materials properties such as high strength, high electrical and thermal conductivity, high impact strength, and containing polymers are used for parts of automobiles, airplanes, shielded from electromagnetic radiation, etc. In connection with the special properties of carbon nanostructures is projected to expand their scope in the future.

Because the use of different carbon nanostructures in various sectors of human activity allows you to get extremely good results that it was impossible to foresee, there is an urgent need for new carbon nanoparticles and nanomaterials, in particular nanoparticles having high strength at low weight.

The invention solves the problem of obtaining new high-strength carbon nanoparticles and nanomaterials with high coloring strength is firm at low weight, which can be used to create new composite light and high-strength materials.

The problem is solved in that the proposed carbon nanoparticles with an average size of not less than 5 nm, includes an internal Central cavity and the outer closed shell covering called an internal cavity on all sides, and named the outer shell comprises at least a pair of individual carbon layers.

The thickness of the outer shell carbon nanoparticles, mainly, does not exceed 20% of its size.

It is also proposed carbon nanomaterial containing the above-described nanoparticles in a mixture of single-walled and multiwalled nanotubes.

The proposed carbon nanoparticles is shown in Fig.1, where: 1 - the Central internal cavity, 2 - closed shell, 3 - layers of the shell.

The particle in Fig.1 has an empty interior cavity 1 and the shell 2. The cavity is shown quite large, and the shell 2 consists of two layers of carbon, arranged almost concentrically. However, the particles may have a Central cavity smaller in larger shell thickness, consisting of multiple layers of carbon. Its thickness can reach up to 20% of the particle size.

Photograph of the proposed carbon nanomaterial is shown in Fig.2, you can see the hollow coal is native nanoparticles mixed with nanotubes.

Hollow carbon nanoparticles get in the composition of the carbon nanomaterial, mainly by catalytic decomposition of gaseous hydrocarbons with subsequent high-temperature annealing poluchennogo carbon nanomaterial.

For example, there is a method of producing carbon nanotubes, in accordance with which in the reaction chamber maintain the temperature of 500-1200°C and generate catalytic material in the form of vapor, which then condenses in the volume of the reaction chamber with the formation of free nanoparticles of the catalyst, the surface of which carbon nanostructures are formed by decomposition of gaseous hydrocarbons [U.S. Patent No. 8137653, IPC B01J 19/08, D01F9/127]. In this way the formation of vapor of the substance containing the catalyst, and the catalyst nanoparticles takes place directly in the volume of the reaction chamber. In this same chamber occurs and the formation of carbon nanostructures. The course of such different nature of the processes in a single volume makes them difficult to control, and optimization. Accordingly, the problem arises to control the properties of the resulting carbon nanostructures. This method are mainly carbon nanotubes.

Carbon hollow nanoparticles and carbon nanomaterial can be obtained by decomposition in the reaction chamber a gaseous hydrocarbon is in the presence of a catalyst at a temperature of 600-1200°C and the formation of carbon nanostructures on the surface of the aforementioned catalyst. To do this, in the reaction chamber and injected a mixture of gaseous hydrocarbons and catalyst in the form of free nanoparticles in the flow of carrier gas. Formed on the surface of free nanoparticles of catalyst carbon nanostructures are removed from reaction chamber in the gas stream and separate them from the named gas. Thus obtained carbon material comprises carbon nanotubes, single-walled and double-walled, and the catalyst nanoparticles coated with amorphous carbon in the form of carbon capsules. This material is then subjected to high temperature annealing at a temperature of 1700-2400°C. the Annealing may be conducted in vacuum or in an atmosphere of inert gas from a number of: helium, argon, peony, xenon, etc. When annealing is burning substances catalyst of the carbon capsules. After burning receive carbon nanoparticles of a size not less than 5 nm with an empty Central cavity, which from all sides covers carbon shell, consisting of layers of carbon. The Central part of the particle - empty, which distinguishes it from neolocality and gives it a little weight. The shell may consist of two, three, four, five or more layers of carbon. Each layer of the shell or part of them in its structure is similar to a sheet of graphene, who closed form.

Because of the hollow particles and the shell thickness is not more the 20% of their size, they are light, and their strength is quite large.

As mentioned above, the carbon material, which is subjected to annealing, initially contains, in addition to the closed carbon capsules, single-walled and double-walled carbon nanotubes. Accordingly, annealed nanomaterial contains hollow carbon nanoparticles and single-walled and double-walled nanotubes, as shown in Fig.2. Their proportion in the composition of the material can vary and depends on the parameters of the catalytic decomposition of gaseous hydrocarbons. It is possible to choose the parameters of the process, so that the content of the hollow carbon nanoparticles in the material is high - up to 90%, and may be low - less than 10%.

Obtain hollow particles containing material characterized by high strength and low weight.

Example 1

In the evaporation chamber pre-receive nanoparticles containing the substance of the catalyst. The evaporation chamber is the volume at the bottom of which are two electrodes, made in the form of tanks filled with a material containing in its composition ingredient of the catalyst is iron (steel type Art.3). Between the electrodes there is a wall in which the bit of the channel, the ends of which are suitable to these electrodes.

When applying to the electrodes a voltage occurs arc R which would be loaded on the, passing into the discharge canal, through which is passed a plasma-forming gas is nitrogen in the form of a whirlwind, obtained with the help of the vortex chamber, and in which support current of 90 A. When this occurs, the melting of steel in the tanks of the electrodes and its evaporation from the formation of vapor iron. At the same time in the camera serves a carrier gas composed of a mixture of hydrogen and nitrogen in a molar ratio 3/40. Pair of iron in the stream of carrier gas condensed into nanoparticles. Then the carrier gas with iron nanoparticles served at the site of mixing, which also serves gaseous hydrocarbon is methane, which is preheated to a temperature of 400°C. In the mixing node mixing receive the working mixture.

Working the mixture is heated to a temperature of 1100°C and served in a reaction chamber, having a volume of 1 m3and a diameter of 1 m In the reaction chamber maintain the temperature of 945°C. In the catalytic decomposition of methane on the iron nanoparticles, the growth of carbon nanotubes. The reaction products pass through the filter, where the separated carbon nanomaterial from the gas. The resulting nanomaterial contains iron nanoparticles in the carbon shells of amorphous carbon and single-walled and double-walled nanotubes. Further, this material is subjected to annealing at 2000°C in an argon atmosphere. Obtained after annealing the carbon Mat is Rial consists of a hollow carbon particles with a size of 5-7 nm - 31% and the above-mentioned single-walled and double-walled nanotubes - the rest.

Example 2

Same as in example 1, but in the reaction chamber maintain the temperature of 600°C. In the catalytic decomposition of methane on one part of iron nanoparticles is the growth of carbon nanotubes, on the other - formed shell of amorphous carbon. The reaction products are removed from reaction chamber and passed through the filter, where the separated carbon nanostructures from the exhaust gas. The resulting nanomaterial contains iron nanoparticles in the membranes of amorphous carbon and single-walled and double-walled nanotubes. Further, this material is subjected to annealing at 1700°C in argon atmosphere. Obtained after annealing the carbon material consists of hollow carbon particles size 5-12 nm - 76% and the above-mentioned single-walled and double-walled nanotubes - the rest.

Example 3

Same as in example 1, but in the reaction chamber maintain the temperature of 1200°C. In the catalytic decomposition of methane on one part of iron nanoparticles is the growth of carbon nanotubes, while the other formed a shell of amorphous carbon. The reaction products are removed from reaction chamber and passed through the filter, where the separated carbon nanostructures from the exhaust gas. The resulting nanomaterial contains iron nanoparticles in the membranes of amorphous carbon is kind and single-walled and double-walled nanotubes. Further, this material are annealed at 2400°C in argon atmosphere. Obtained after annealing the carbon material consists of hollow carbon particles with a size of 5-7 nm - 12% and the above-mentioned single-walled and double-walled nanotubes - the rest.

1. Carbon nanoparticles, characterized in that it has an average size of at least 5 nm and includes a Central inner cavity and the outer closed shell covering called an internal cavity on all sides, and named the outer shell comprises at least a pair of individual carbon layers.

2. Carbon nanoparticles under item 1, characterized in that the thickness of the outer shell does not exceed 20% of its size.

3. Carbon material, characterized in that it contains a mixture of hollow carbon nanoparticles with an average size of not less than 5 nm, includes a Central inner cavity and the outer closed shell covering called an internal cavity on all sides, which is called the outer shell comprises at least a pair of individual carbon layers, and single-walled and double-walled carbon nanotubes.

4. A method of obtaining a carbon material containing a mixture of hollow carbon nanoparticles with an average size of not less than 5 nm, includes a Central inner cavity and the outer closed shell covering the title is ing the inner cavity on all sides, have called the outer shell comprises at least a pair of individual carbon layers, and single-walled and double-walled carbon nanotubes, comprising the catalytic decomposition of hydrocarbons at a temperature of 600-1200°C with a mixture of carbon nanostructures, which is separated from the gaseous decomposition products and are annealed at a temperature of 1700-2400°C in an atmosphere of inert gas.



 

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