Method of carbonaceous material receiving, consisting metal

FIELD: nanotechnology.

SUBSTANCE: invention relates to nanotechnology and nanostructures, particularly carbon-base materials and can be used in different field of engineering and energetics. In vacuum on substrate made of dielectric material it is sediment evaporated in vacuum silver by means of plasma carbon-base material. Silver sedimentation is implemented before the sedimentation of carbon-base material. Evaporation of carbon-base material, in the capacity of which it is used graphite, is implemented by pulsed arc discharge. Plasma for sedimentation of carbon-base material is created outside the discharge gap area of voltaic arc in the form of compensated currentless for-coagulates of carbonaceous plasma with density 5-1012-1·1013 cm-3, duration 200-600 mcs, recurrence rate 1-5 Hz. During the sedimentation process of carbon-base material it is implemented stimulating effect of carbonaceous plasma by inert gas in the form of ion flow with energy 150-2000 eV, which is directed perpendicularly to carbonaceous plasma stream. Then substrate with sediment on it silver and carbon-base material is extracted from vacuum chamber and annealed on air at temperature 400°C during 10 minutes.

EFFECT: it is manufactured carbon-base material, containing metal, with new properties, for instance electrical conductance and transparency.

11 dwg

 

The invention relates to nanotechnology and nanostructures, particularly carbon nanomaterials, and can be used to obtain materials for machinery, and energy. In particular, for the production of parts, which have, for example, conductive or transparency properties. Such materials can be used in the manufacture of electrodes, protective coatings, etc.

One of the common ways of obtaining carbon and metal nanomaterials is a method of laser ablation of carbon or metal target (Kozlov GI // technical physics Letters, 2003, vol. 29, VIP, p.88-94). The material is exposed to laser radiation of high power, resulting in the evaporation of atoms and clusters from the surface and their subsequent condensation in the nanoparticles.

A method of obtaining carbon and metallic materials in the process of dissociation of the source of the carbon and metal-containing molecules using electric arc discharge with subsequent cooling of the products of dissociation and their condensation (Zeng H, Zhu L, Hao G.M, Sheng RS // Carbon 1998, 36 (3), 259-61). The disadvantage of these methods of nanomaterials is the uncertainty of the concentrations and composition of ablation products, which leads to uncertainty in the properties of the material obtained.

There is a method of extracting the Oia nanomaterial in the combustion of hydrocarbons in flames (P.Minutolo, G.Gambi and A.D'Alessio // Twenty-Seventh Symposium (International) on Combustion, The Combustion Institute, 1998, pp.1461-1469). Adding various additives and varying characteristics of the flame, you can get a wide range of nanomaterials. However, for this method it is possible to note the disadvantages of the aforementioned methods. Besides, the presence of oxygen in the combustion process leads to partial oxidation of the carbon and especially metals.

A known method of manufacturing a carbon nanomaterial containing metal, in the form of a film having in its composition as the main elements carbon, silicon, metal, oxygen and hydrogen. The method consists in the fact that in the vacuum chamber place the holder with the substrate of dielectric material, is served on the holder substrate voltage of 0.3-5.0 kV with a frequency in the range from 1 to 25 MHz and keep the temperature of the substrate ranging from 200 to 500°C., in a vacuum chamber to create a gas discharge plasma, which uses argon, with an energy density of more than 5 kW·hour/gram-atom of carbon particles in the generated gas discharge plasma is vaporized carbonaceous material, which is used as organosiloxane heated to a temperature of 500-800°C, the decomposition in the plasma serves as a source of carbon, silicon, oxygen, and hydrogen, and then in a vacuum chamber with a gas discharge plasma is injected beam particles of the alloying Mat is the Rial, for example of metal, in the form of atoms or ions, carry out the deposition on the substrate atoms or ions of carbon, silicon, oxygen, and hydrogen, as well as atoms or metal ions and obtain a conductive carbon nanocomposite film (see patent RU 2118206, 1998).

The closest technical solution is a method of manufacturing a carbon - and metal-containing nanomaterial in the form of a film having in its composition as the main elements carbon, silicon, metal, oxygen, hydrogen and located on the dielectric substrate (see, for example, U.S. patent 5352493, 1994). The method involves deposition in vacuum on a substrate of dielectric material evaporated in vacuum and silver using plasma evaporated in vacuum carbon material.

The obtained film is an amorphous isotropic structure, which includes three network. The main matrix of the chain is a diamond-like carbon film. However, the films obtained have a high electrical resistance, higher values mentioned in the description to the specified patent, possibly due to the barrier resistance at interfaces between clusters. In the film structure manufactured by the above method, there are nanoclusters size (30-500) As determined by studies in tunneling microscope. Obviously, because of the emerging when this is istoty film in high temperatures in the presence of atmospheric oxygen is increased diffusion of oxygen into the film, followed by the burning of carbon at high temperatures.

The method aims to obtain films with uniform composition. The choice of the alloying material is dictated by the set by the qualities of the film that you want to retrieve.

However, the properties obtained in this way material containing the composition of the metal, mainly due to the properties of this metal in combination with a carbon material, such as electrical conductivity.

The task of the claimed invention is to provide a method of manufacturing a carbon nanomaterial containing metal, in the form of a film having new properties that extend the range of industrial applications such material.

The technical result of the claimed invention to provide a new property of the carbon material containing the metal.

This result is achieved by the fact that when the production of carbon nanomaterial containing metal, including deposition in vacuum on a substrate of dielectric material evaporated in vacuum and silver using plasma evaporated in vacuum carbon material according to the invention the deposition of silver is carried out before the deposition of the carbon material, the evaporation of the carbon material, which is used as graphite, perform pulsed arc discharge plasma for about what adenia carbon material create outside the scope of the bit period of the arc discharge in the form of compensated current-free forshadow carbon plasma density of 5·10 12-1·1013cm-3duration between 200 and 600 μs, a repetition rate of 1-5 Hz, while in the process of deposition of the carbon material are stimulation carbon plasma with an inert gas in the form of a stream of ions with energy of 150-2000 eV, which is directed perpendicular to the stream of carbon plasma, after which the substrate with the deposited it with silver and carbon material is removed from the vacuum chamber and annealed in air at 400°C for 10 minutes.

The method is as follows. On a substrate made of material (for example, mica brand COULD GOST 13752-86, Quartz, K-8, Sitall brand CT-50-1, polikor brand VK-100), which is not destroyed, does not decompose and does not emit gaseous products when heated in air to 500°C. is applied in the vacuum thermal evaporation film of silver, for example, brands SR,9 or SR. On top of this film synthesized ion-plasma method, a carbon film. This process, figure 1, is carried out in a vacuum chamber 1, in the case where the lateral flange axes are mutually perpendicular, inside one of them posted in the form of cylinder cathode of main discharge 5 and the anode of the auxiliary discharge 4 covering a gap cathode of main discharge 5, and the inner surface of the anode auxiliary discharge 4 is made with a tapered cut, drawn from one of the tor the extract cathode of main discharge 5 in the direction of the main discharge anode 3, made in the form of two rings rigidly connected by metal rods, with equal increments around the circumference, while the control electrode 6, the dielectric insert 8, the cathode of the auxiliary discharge 7 is made in the form of a disk, rigidly connected and installed between the main anodes 3 and 4 auxiliary discharge inside the vacuum chamber 1 is installed with the possibility of planetary rotation around the vertical axis and electrically coupled to the housing of the vacuum chamber 1 polictial 2. The substrate is isolated from podarkticules. Condensation of carbon is produced from the no-current carbon plasma supplied to the substrate in vacuum at a pressure of 1·10-1-1·10-2PA. Between the cathode of the main discharge 5 and the main discharge anode 3 under capacity 200 through an auxiliary discharge between the cathode of the auxiliary discharge 7, which is located at a distance L from the cathode of the main discharge 5, and the anode of the auxiliary discharge 4 covering the cathode of the main discharge 5, ignited arc discharge. The auxiliary discharge is ignited by a control electrode 6 made in the form of a ring located between the anode 4 and cathode 5 of the auxiliary discharge. Forming a film of carbon is achieved by the fact that at the time of formation of the plasma forsgate is isarene the graphite cathode of main discharge 5 in the pulse heating of the surface of the graphite to a temperature of 3000°C. Evaporation of carbon occurs in the form of chains Cn (where n 1, 2, 3, 5, 7). The resulting chain is coming to the surface of the substrate, where they polycondensation, i.e. the formation of longer due to their Association chains. Electronic temperature of the plasma must not exceed the energy of breaking bonds in the carbon chain, as it leads to the "merging" of these chains and the formation of amorphous carbon with a short-range order of the diamond or graphite type.

In the electric circuit of the main discharge is in series connected capacitor 11 and inductor 12, limiting the slew rate pulse discharge current. The capacitor 11 is charged by the power source 10 connected in parallel to the respective capacitor plates 11, to a voltage of 200 C. the main discharge Anode 3 has a very extensive internal surface, for which he may be made in the form of a "squirrel" wheels, that is, in the form of two rings rigidly connected by metal rods that are installed with equal pitch in the circumferential direction. The main discharge anode 3, the anode of the auxiliary discharge 4, the cathode of the main discharge 5, control electrode 6, the cathode of the auxiliary discharge 7, the dielectric insert 8 is installed coaxially.

The substrate on which is formed condensate is seanodes space R which is 20 - 30 cm from the main discharge) and may be made of any material, in particular ceramic, metal, polymer, silicone rubber, alloy, etc. may be of any shape and geometry. The coating is applied with high adhesion, uniformly on any form of surface depressions, the projections smaller than the Debye radius equal to 10 μm. The substrate is mounted on poblagodarite that during the coating process performs a planetary motion, that is, simultaneously rotates around its axis and the vertical axis of the vacuum chamber. During the entire cycle of formation of a film of carbon substrate with increasing the film is irradiated with ions of inert gas, for example argon. Inert gas ions formed in the ion source of radiation 9, located at the other lateral flange of the vacuum chamber 1 is communicated with the vacuum chamber an annular opening for passage of the ion beam. The source of ion irradiation can be a two-electrode system consisting of a cylindrical cathode with an annular gap for the passage of the ion beam and the annular anode. The energy of the ion beam of an inert gas, irradiating the film perpendicular to the flow compensated current-free plasma forshadow varies in the range of 150-2000 eV. Formed in the region of the discharge gap of the arc discharge compensated during PLA is Menno forgucci have a density of 5·10 12-1·1013cm-3the duration between 200 and 600 μs, a repetition rate of 1-5 Hz.

These parameters can be provided by specially selected geometry of the ignition electrodes, the electrical circuit of the plasma generator, comprising a storage capacitor, limiting inductance, a three-stage schema of the ignition. The result is a film consisting of a layer of silver and a layer representing a linear carbon chain.

The sample obtained was placed in a muffle furnace, for example, PM-8, and annealed in air at 400°C for 10 minutes (for silver). As the distance between the carbon chains in the hexagonal structure of the film is 5Å. (see figure 2), in film of linear-chain carbon intercalary silver atoms whose radius is less than 2Å.

Figure 2 presents the structure of the sample prepared by annealing.

The structure of the surface before the heat treatment was investigated on the microscope Femtoscan in atomic force mode, shown in figure 3.

Figure 4 shows the transmission spectra systems LTD - silver (when the film thickness of the silver 600Å) before heat treatment on - line in the form of a square characters, after heat treatment is in the form of a round character. From this figure it follows that after the heat treatment system became more transparent.

The volt-ampere characteristic obtained by the microscope is Femtoscan tunnel mode before annealing, presented in figure 5. It shows metallic character of conductivity.

After annealing in a muffle furnace PM-8 in air at 400°C for 10 minutes received the following changes:

1. Change the appearance of a - 6. There is a lamp mounted behind a film.

2. The surface topography - 7. Compared with figure 3 topography has changed towards integration cluster.

3. The volt-ampere characteristic of the resulting nanomaterial - Fig.

This current-voltage characteristic shows that the tunneling transition corresponds to a transition metal - semiconductor. Metal is the needle microscope, semiconductor - surface of the heat-treated film silver - pointers. With needles in the surface takes more electrons than with the film surface on the needle. The resulting material belongs to the class of p-semiconductors.

It is obvious that the claimed method received a new substance composed of atoms of silver and polymer molecules of carbon. In the world practice it is known that the use of silver in contact with the carbon materials even at temperatures of 1100°C does not give such a result. The proof of this is the known phase diagram of the system silver - graphite, which is shown in Fig.9.

The thickness of the deposited films plays an important role for the degree transparently the ti film.

Figure 10 presents electronography of the heat-treated film Ag++, where in the center of the visible 6 reflexes, characterize, as it is known (see, for example, Amelda. Conjugated polymers. Moscow, Nauka, 1989), the hexagonal structure of linear-chain carbon. On the periphery of the visible reflexes silver rings.

The resulting electronography figure 10 suggests that the hexagonal structure pointers are not destroyed when annealing with silver. This is evidenced by the absorption spectrum obtained by using infrared Fourier-transform spectrometer. This spectrum is shown in 11.

Method for the production of carbon nanomaterial containing metal, including deposition in vacuum on a substrate of dielectric material evaporated in vacuum and silver using plasma evaporated in vacuum carbon material, characterized in that the deposition of silver is carried out before the deposition of the carbon material, the evaporation of the carbon material, which is used as graphite, perform pulsed arc discharge plasma for deposition of the carbon material create outside the scope of the bit period of the arc discharge in the form of compensated current-free forshadow carbon plasma density of 5·1012-1·1013cm-3duration between 200 and 600 μs, a repetition rate of 1-5 Hz, the ri in the process of deposition of the carbon material are stimulation carbon plasma with an inert gas in the form of a stream of ions with energy of 150-2000 eV, which is directed perpendicular to the stream of carbon plasma, after which the substrate with the deposited it with silver and carbon material is removed from the vacuum chamber and annealed in air at 400°C for 10 minutes



 

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1 tbl

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11 cl, 1 dwg, 5 ex

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