Method for production of coatings from carbon nanomaterials and device for its realisation

FIELD: nanotechnologies.

SUBSTANCE: invention relates to nanotechnologies and may be used to produce coatings from nanodiamonds, fullerenes and carbon nanotubes, operating under extreme conditions. Mixture with negative oxygen balance, made of carbon-containing substance and oxidant, is prepared in half-closed resonant detonation chamber 2, which is part of case 1. Carbon-containing substance is produced by ethylene bubbling in bubbler 7 through kerosene heated by means of electric heater 8 in the temperature range from 500 to 750°K. Carbon-containing substance is supplied into half-closed resonant detonation chamber 2 via porous end wall 4, and oxidant - via circular slot supersonic nozzle 3, formed by internal walls 5 and porous wall 4. Then mixture detonation is periodically initiated with frequency of 100-20000 Hz with the help of detonation initiator 6 in medium inertial towards carbon. After detonation, produced flow of carbon nanoclusters from detonation chamber 2 is sent to item 15 with processed surface 16, heated by source of radiant energy 17 to temperature of 550-1300 K. At the same time with the help of drive 13 and control system 14, processed surface 16 is periodically displaced with frequency of at least 1 Hz relative to vector of carbon nanoclusters flow speed in the range of angles from -45 to 45 degrees. Speed of detonation products cooling is maintained in the range from 5·103 to 2·106 K/s.

EFFECT: invention makes it possible to produce coats from carbon nanomaterials on surfaces of bulk products of complex shape and to do fine adjustment of coats parametres.

2 cl, 1 dwg

 

The invention relates to nanotechnology and can be used for processing products and coatings for operation in hazard conditions.

There is a method of hardening of parts (EN 2194796 C1 IPC SS 12/02, 2001), based on the application of the surface additives of graphite and carbon-silicon-titanium-aluminium-containing material and heating the additive and hardened seats to a temperature not lower than 700°C currents or high frequency electric arc, plasma or gas burner.

The disadvantage of this method is the low quality of the material additives and insignificant effect hardening of the workpiece.

A method of obtaining coatings of powder materials and device for its implementation (EN 2145644 C1 IPC SS 4/12, 1998), including the formation of accelerating the flow of carrier gas, the introduction of particles of the powder material in the pulse mode, the supply of gas-powder mixture obtained in accelerating supersonic nozzle and applying the powder material on the pre-heated surface. A device for receiving the coating from the powder material spray contains the node in the form of accelerating supersonic nozzle, means for supplying a carrier gas and enter the gas-powder mixture in the spray unit and metering unit, the processing unit powder mother of the La to activate and clean the surface of the particles and the pulsator, coupled with a means of entering the gas-powder mixture.

The disadvantage of this method and device is that they do not provide create mode nanocoatings.

The known method of forming the nano(micro)systems of carbon nanotubes (EN 2306257, IPC WV 3/00, 2007), comprising applying to the substrate a multilayer coating containing catalytic layer and the carbon layer nanoscale thickness and performing the catalytic layer of the specified picture under electrical influence of constant or pulsed mode with a location of the sample in the growth chamber, heated to a temperature of 350...600°C in the presence of the reactant gases and RF or microwave radiation.

The disadvantage of this method is its low productivity.

There is a method for plasma coating (EN 2155822 C1 IPC SS 4/12, 1999), including the input of the sprayed powder into the plasma jet, thermal activation of the processed surface of the external excitation of the electric arc, combined with the plasma jet, and transportation of powder plasma jet to the treated surface. When this external electric arc is fed by a pulsed current with a pulse repetition rate of 25-100 Hz average power pulse arc 1-8,5 kW.

The disadvantage of this method is that it does not get manorism rye coating of carbon nanomaterials.

A method of obtaining coatings (EN 2146302 C1 IPC SS 4/12, 1997), including the process of spraying at an angle of particle collisions with the substrate in two stages: in the first stage, the plating lead angle of particle collisions with the substrate, a large 45°, in the second phase - angle of particle collisions with the substrate 0-45°.

The disadvantage of this method is the lack of coating uniformity, especially for nanoscale thickness.

Known methods for producing nano-carbon (variants) and a device for implementing them (patent RU №2344074 C1 IPC SW 31/00, WV 3/00, 2009).

Methods of obtaining nanosized carbon-based mixture with a negative oxygen balance, which includes carbon-containing substance in the starting mixture in a resonant half-closed detonation chamber into two streams with different coefficient of excess oxidant through the porous wall and through the annular slit supersonic nozzle, periodic detonation frequency 100-20000 Hz in an environment inert to carbon, and subsequent cooling of detonation products at the rate of 2·105-106K/S. a Device for obtaining nanosized carbon includes a housing with a semi-closed resonant detonation chamber, the entrance of which is mounted an annular slit supersonic nozzle, sformirovann the e porous end and the inner walls of the resonance chamber.

A disadvantage of the known technical solutions are limited technological capabilities for the preparation of a mixture of carbon-containing substances with negative oxygen balance to create a flow of carbon nanoclusters and coatings of carbon nanomaterials.

The closest of the technical solutions proposed method and device coatings of carbon nanomaterials are the method and the device described in patent RU No. 2218299 C1 IPC SS 14/25, WV 3/00, 2003

A method of producing coatings of carbon nanomaterials based on the use of carbon-containing substances and the workpiece, pre-trained for applying a carbon coating. Device for obtaining coatings of carbon nanomaterials includes a housing, a heater and a product with the workpiece surface.

A disadvantage of the known technical solution is small size products with the treated surface and the limited possibility to control the parameters of the sprayed coating of carbon nanomaterials.

The objective of the invention is the improvement of coating properties of carbon nanomaterials on the treated surface.

The technical result obtained by the invention is the ability to create p the closure of the carbon nanomaterials, including fullerenes, nanodiamonds and carbon nanotubes on the surface of treated dimensional complex-shaped products and to further adjust the parameters of such coatings.

The solution of the problem and the technical result is achieved by the fact that in the method of producing coatings of carbon nanomaterials using carbon-containing substance and the workpiece, pre-trained for applying a carbon coating, the carbonaceous substance use ethylene gas that is bubbled through the kerosene at a temperature in the range from 500 to 750 K, the mixture with negative oxygen balance is prepared in resonant half-closed detonation chamber, feeding carbonaceous substance through a porous wall, and the oxidizer through an annular slit supersonic nozzle, carry out periodic detonation cooked mixture with a frequency of 100-20000 Hz in an environment inert to the carbon, after detonation the resulting stream of carbon nanoclusters of the resonance chamber is directed to the workpiece surface, which is heated by the radiant energy flux to a temperature in the range from 550 to 1300 K, and periodically with a frequency less than 1 Hz to carry out the angular displacement of the treated surface relative to the velocity of flow of carbon nanoclustered range of angles from -45 to 45 degrees, at the same time supporting the cooling rate of detonation products in the range of 5·103up to 2·106K/s by adjusting the radiant heating of the workpiece and the environment settings flooded space, which expires in the flow of carbon nanoclusters of resonant half-closed detonation chamber.

The solution of the problem and the technical result is achieved that the device for producing coatings of carbon nanomaterials, including the housing, the heater and the product with the treated surface, equipped with a detonation initiator, the body is equipped with resonant half-closed detonation chamber, the porous end and the inner wall of which is formed an annular slit supersonic nozzle, at the entrance to the resonant half-closed detonation chamber before the porous end wall installed bubbler with heater, temperature controller, gas mixer, metering and shut-off valve, and the output resonant detonation chamber on the rotary platform with drive and control system fixed product with the treated surface, heated by the source radiant energy.

Diagram of the device for obtaining coatings of carbon nanomaterials on the proposed method is shown in the drawing.

According to the claimed invention offer aemy a method of producing coatings of carbon nanomaterials using carbon-containing substance and the workpiece, pre-trained for applying a carbon coating, is to use ethylene as a carbon-containing substance, which is bubbled through the kerosene at a temperature in the range from 500 to 750 K, the mixture with negative oxygen balance is prepared in resonant half-closed detonation chamber, feeding carbonaceous substance through a porous wall, and the oxidizer through an annular slit supersonic nozzle, carry out periodic detonation cooked mixture with a frequency of 100-20000 Hz in an environment inert to the carbon, after the detonation of the received stream of carbon nanoclusters of the resonance chamber is directed to the workpiece surface, which is heated by the radiant energy flux to a temperature in the range from 550 to 1300 K, and periodically with a frequency less than 1 Hz to carry out the angular displacement of the treated surface relative to the velocity of flow of carbon nanoclusters in the range of angles from -45 to 45 degrees, supporting the cooling rate of detonation products in the range of 5·103up to 2·106K/s by adjusting the radiant heating of the workpiece and the environment settings flooded space, which expires in the flow of carbon nanoclusters of resonant half-closed detonation chamber.

According to the implemented invention proposed a method of producing coatings of carbon nanomaterials is implemented using a device, shown in the drawing and comprising a housing 1 with a resonant half-closed detonation chamber 2, a porous face 4 and 5 internal wall of which is formed an annular slit supersonic nozzle 3, the initiator 6 detonation, the heater 8 and the workpiece 15 with the workpiece surface 16. At the entrance to the resonant half-closed detonation chamber 2 before the porous end wall 4 has a bubbler 7 heater 8, a controller 9 temperature, the mixer 10 gas, metering and shut-off valve 11, and the output resonant detonation chamber 2 on the rotary platform 12 with the actuator 13 and 14 control the pinned item 15 with the workpiece surface 16, heated by the source 17 of radiant energy.

The device operates as follows: the mixture with a negative oxygen balance for detonation synthesis of carbon nanomaterials prepared in resonant half-closed detonation chamber 2, which serves carbonaceous substance through the porous end wall 4 and the oxidant through the annular slit supersonic nozzle 3. The carbonaceous substance use ethylene gas that is bubbled through the kerosene at a temperature in the range from 500 to 750 K, and the oxidizer is a mixture of oxygen with nitrogen, helium or argon. In semi-closed resonant detonat the Onna camera 2 carry out periodic detonation cooked mixture with a frequency of 100-20000 Hz in the environment, inert to carbon. After the detonation of the received stream of carbon nanoclusters of resonance detonation chamber 2 is directed onto the surface 16, which is heated by the radiant energy flux to a temperature in the range from 550 to 1300 K, and periodically with a frequency less than 1 Hz to carry out the angular displacement of the treated surface 16 relative to the velocity of flow of carbon nanoclusters in the range of angles from -45 to 45 degrees. At the same time supporting the cooling rate of detonation products in the range of 5·103up to 2·106K/s by adjusting the radiant heating of the treated surface 16 and environments flooded space, which expires in the flow of carbon nanoclusters of resonant half-closed detonation chamber 2.

The advantage of the proposed method of producing coatings of carbon nanomaterials, including fullerenes, nanodiamonds and carbon nanotubes, is:

radical reduction of the residence time of detonation products in resonant half-closed detonation chamber, eliminating overheating, graphitization and pollution of detonation products;

- the possibility of fine adjustment of the composition of the working mixture and environment detonation synthesis of determining the quality of carbon nanomaterials;

- obtaining fullerene is in, nanodiamonds and carbon nanotubes and coatings based on them in fast processes of detonation synthesis without the use of catalysts;

- the opportunity to create a special coating on the dimensional complex-shaped products, giving them a new consumer properties.

To create and implement new technologies, services and products on the basis of the claimed group of inventions is expected to actively attract investments on favorable terms.

1. A method of producing coatings of carbon nanomaterials using carbon-containing substance and the workpiece, pre-trained for applying a carbon coating, characterized in that the carbonaceous substance use ethylene gas that is bubbled through the kerosene at a temperature in the range from 500 to 750 K, the mixture with negative oxygen balance is prepared in resonant half-closed detonation chamber, feeding carbonaceous substance through a porous wall, and the oxidizer through an annular slit supersonic nozzle, carry out periodic detonation cooked mixture with a frequency of 100-20000 Hz in an environment inert to the carbon, after the detonation of the received stream of carbon nanoclusters of resonance the camera is directed to the workpiece surface, which is heated beam is stim energy flow to a temperature in the range from 550 to 1300 K, and periodically with a frequency less than 1 Hz to carry out the angular displacement of the treated surface relative to the velocity of flow of carbon nanoclusters in the range of angles from -45°to 45°, supporting the cooling rate of detonation products in the range of 5·103up to 2·106K/s by adjusting the radiant heating of the treated surface.

2. Device for obtaining coatings of carbon nanomaterials, including the housing, the heater and the product with the treated surface, characterized in that it is equipped with a detonation initiator, the body is equipped with resonant half-closed detonation chamber, the porous end and the inner wall of which is formed an annular slit supersonic nozzle, at the entrance to the resonant half-closed detonation chamber before the porous end wall installed bubbler with heater, temperature controller, gas mixer, metering and shut-off valve, and the output resonant detonation chamber on the rotary platform with drive and control system fixed product with the treated surface, heated by the source of radiant energy.



 

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FIELD: technological processes.

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3 ex

FIELD: chemistry.

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2 ex

FIELD: chemistry.

SUBSTANCE: invention can be used to make carbonaceous adsorbents. Iodine heptafluoride is frozen onto a graphite-containing powdered material from a gas phase with pressure lower than equilibrium pressure over liquid-phase iodine heptafluoride. The graphite-containing powdered material is then treated with liquid-phase iodine heptafluoride to obtain an intercalation compound of fluorinated graphite by defrosting the two-component mixture to temperature of 7-25°C and then holding at equilibrium pressure of iodine heptafluoride vapour over the liquid phase. The remaining liquid phase is frozen out from the graphite-containing powdered material. The obtained powdered intercalation compound of fluorinated graphite is thermally treated in a muffle furnace.

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1 tbl, 4 dwg

FIELD: chemistry.

SUBSTANCE: method relates to nanotechnology of layered materials and is meant for obtaining nanosized carbon layers on non-conducting substrates for mass production of devices using planar technology. The method of obtaining a carbon layer on a non-conducting substrate involves oxidation of a graphite substrate through fluorination under conditions which provide dielectric properties of the substrate. An intercalation compound based on graphite fluoride C2FX with x≤1 is obtained, wherein the introduced component can be substituted. Fluorine-oxidising agent is used: BrF3 vapour or BrF3 solution to Br2. Fluorine atoms are then removed from the surface layer of the required thickness of 1-4 nm under conditions which facilitate formation of a carbon layer of controlled thickness on the dielectric substrate. Defluorination is carried out via chemical reduction in water vapour or hydrasine hydrate vapour or through exposure to ionising particles - electron beam. Due to the purely chemical and/or radiation-chemical nature of the main operations, as well as initiation of formation of the carbon layer during defluorination from the surface with distribution deep into the substrate, with achievement of the required thickness of the formed carbon layer through chemical reduction conditions - concentration and temperature of the vapour of reagents and in case of reduction with an electron beam - kinetic energy of electrons, increase in the area of the solid carbon layer and possibility of controlling its thickness are achieved.

EFFECT: increased area of the solid carbon layer and possibility of controlling its thickness.

11 cl, 4 dwg, 5 ex

FIELD: chemistry.

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1 tbl, 10 ex

FIELD: chemistry.

SUBSTANCE: invention can be used in production of semiconductors and in microelectronics. Grinding powder which contains silicon carbide, silicon oxide, silicon and metallic impurities is treated with organic solutions and/or dried. The powder is then treated with bromoform and/or dibromomethane in airtight conditions at pressure over 0.2 atm with mechanical agitation. Silicon carbide separated as a heavy fraction contains 95-98% of the main product, while the initial treated powder contains 3-55 wt % silicon carbide.

EFFECT: improved properties of the grinding powder.

3 cl

FIELD: chemistry.

SUBSTANCE: invention relates to technology of producing fibrous carbon materials through pyrolysis of aromatic and non-aromatic hydrocarbons. A catalyst 9 is deposited on the top surface of a container 8. After sealing the reactor, inert gas is blown inside and heating elements 5 and the disc 6 rotary actuator 7 are switched on. Carbon-bearing gas is fed into the cavity between the cap 10 and the container 8 and the catalyst 9 is heated. Heating is then stopped and a forced cooling system is switched on. After lowering temperature in the reactor, the disc 6 rotary actuator 7 is switched off, the reactor is opened and the container 8 with nanotubes is removed.

EFFECT: invention enables to obtain multilayer carbon nanotubes with diametre of 15-50 nm.

3 cl, 8 dwg, 2 ex

FIELD: machine building.

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EFFECT: higher quality of products, synthesis of nanotube with OD varying from 3 to 10 nm.

5 cl, 8 dwg, 1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to production of low-density carbon-graphite heat-insulating materials for high-temperature vacuum furnaces or non-oxidising atmosphere furnaces and can be used in production of carbon-carbon composite materials. Oxidised graphite obtained using nitrate or bisulphate technology is exposed to a thermal shock. Carbon fibre is added to particles of thermally expanded graphite. A workpiece with density of not more than 0.07 g/cm3 is formed. The moulded porous workpiece undergoes pyrolytic saturation in cyclic mode through deposition of pyrolytic carbon on the entire volume until attaining pyrolytic saturation between 5 and 100%. A layer of graphite foil is glued on the other side of the obtained material. The material is carbonised.

EFFECT: invention simplifies technology, enables to obtain high-temperature heat-insulating material with low heat-conductivity and sufficient strength.

11 cl, 1 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to chemical methods of functionalising nano-sized objects for endowing their surface with certain properties. Nanopowder of metals or metal oxides in a carbon shell or without a carbon shell, or nanocarbon, or nanodiamond, react with a water-soluble arenediazonium tosylate salt for formation of covalent bonds of organic functional groups with the surface of the powder.

EFFECT: simplification of synthesis conditions with possibility of obtaining double-layer and single-layer particles having a surface with selective capacity to react with organic, bioorganic and inorganic substances or metal ions or their stabilisation in corresponding media during use.

17 ex, 5 dwg

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