Method of spinning fibres from graphene ribbons

FIELD: chemistry.

SUBSTANCE: invention relates to chemical fibre technology and a method of spinning fibres from graphene ribbons. The method of spinning fibres from graphene ribbons begins with unfolding carbon nanotubes to form graphene ribbons, cleaning and drying the graphene ribbons and dissolving the graphene ribbons in a suitable solvent, preferably a superacid, to form a spinning solution. The spinning solution is used to spin such that spliced fibres are fed into a coagulation medium, also known as an anti-solvent, where spun or spliced fibres undergo coagulation. The coagulation medium flows in the same direction as the orientation of fibres formed from the graphene ribbons. The coagulated fibres, formed from the graphene ribbons, are pulled off, neutralised and washed and then wound on a spool.

EFFECT: invention enables to produce fibres from graphene ribbons.

15 cl, 7 dwg

 

The invention belongs to a method for spinning graphene ribbon with the formation of fibers.

A spinning solution containing graphene ribbons, served in a die, and spinning solution spun fiber is spliced graphene ribbons, which is directed into the coagulation medium, also known as anti-solvent, where it is spun or spliced fiber coagulents. Coagulated filaments formed from graphene ribbons, pull to remove the excessive coagulation of the medium, neutralized (optional) and washed, and then is wound on the reel.

Spinning solution can be created by dissolving graphene ribbons in a suitable solvent, preferably in swarkestone. Way to create a spinning solution (optional) may include one or more of the following stages of purification of carbon nanotubes, unwinding of carbon nanotubes into graphene ribbons, cleaning of graphene ribbons and drying of graphene ribbons.

The invention is illustrated in the drawings, where:

Fig.1 schematically represents a variant of an embodiment of a method of manufacturing fibers from graphene ribbons according to the invention, including the availability of transport tubes, consisting of vertical and horizontal parts.

Fig.2 schematically represents an alternative GP�of osenia method for the manufacture of fibers from graphene ribbons according to the invention, including the presence of a transport tube, wherein the conveying portion of the tube is movable, that is used to modify the height of the outlet of the transporting pipe, to adjust the level of coagulation medium in the coagulation bath and, thus, to increase or decrease the length of the air gap and to control the rate of flow of coagulation fluid through the conveying tube.

Fig.3 schematically represents a method for the manufacture of fibers from graphene ribbons according to the invention, and coagulated fiber out of the coagulation bath down through the vertical pipe.

Fig.4 schematically represents a method for the manufacture of fibers from graphene ribbons according to the invention, and spliced fiber wipedout directly in the transport pipe containing a coagulation medium in the direction vertically upwards.

Fig.5 schematically represents a method for the manufacture of fibers from graphene ribbons according to the invention, and spliced fiber wipedout directly into a transport tube containing a coagulation medium in the horizontal direction, and wherein the flow velocity of the coagulation medium in the transporting pipe is determined by the difference in elevation between the liquid level in the coagulation bath and o�house of distributor pipes.

Fig.6 schematically represents a method for the manufacture of fibers from graphene ribbons according to the invention, and spliced fiber wipedout with the formation of a liquid curtain of coagulation environment.

Fig.7 schematically represents a nozzle suitable for spinning fibers from graphene ribbons in the coagulation medium.

Currently the latest high-performance fibers are composed primarily of carbon, such as a brand Kevlar®, Twaron®, Zylon®, or represent solely carbon, for example, polyacrylonitrile carbon fiber or carbon fiber-based resin. In addition, due to structural shortcomings of the current fibers have a strength that makes up only a small proportion, typically below 10%, on the strength of the molecular bonds of carbon-carbon. Control of nanostructures, starting from the receipt of the material predecessor and up to the end of the fiber, is a key challenge, which needs to improve high-performance fibers. In addition to carbon nanotubes, for spinning of high-performance fibers are also well suited graphene ribbons. Graphene ribbons are more flexible than carbon nanotubes, which is an advantage in the method of production, as well as for final products. Such �isoeffective graphene ribbon fibers can be used, for example, yarns, nonwovens, membranes and films.

Graphene ribbons can be produced in alternative ways, for example, by cutting the graphene ribbons from larger graphene sheets using chemical methods. However, the cutting of graphene ribbons according to these methods only allows for limited control of the width of the graphene ribbons. The deployment of carbon nanotubes by spinning along the length of the carbon nanotubes contributes to the achievement of full control of the width of the resulting graphene ribbons.

Invented method for spinning graphene ribbon with the formation of fibers includes the steps of supplying a spinning solution containing graphene ribbons, a die and spinning from a spinning solution with the formation of the beam spliced fibers formed from graphene ribbons. The beam spliced fibers can consist of any number of fibers in the range from one fiber to obtain a monofilament to several thousand fibers to obtain multifilament yarns of graphene ribbons. Spliced fiber is subjected to coagulation in the coagulation medium, preferably, sulfuric acid or trichloromethane, and coagulated fiber mechanical pull to remove the excessive coagulation of the medium, is subjected to neutralization (optional), and washed and wound on a bobbin. It is preferred that the coagulated fibers were subjected to neutralization and washing.

Spinning solution can be created by dissolving graphene ribbons, cutting of graphene ribbons from large-sized graphene sheets using chemical methods, in a suitable solvent, preferably in supercyclone, more preferably in chlorosulfonic acid or oleum, with the formation of the spinning solution. It is preferred that the spinning solution was formed by purification of carbon nanotubes (carbon nanotubes, CNT) to remove components that is different from the CNT, such as amorphous carbon, graphite and catalyst residues, the deployment of carbon nanotubes with the formation of graphene ribbons, drying (optional) graphene ribbons and subsequent dissolution of graphene ribbons in a suitable solvent, preferably in supercyclone, more preferably in chlorosulfonic acid or oleum, with the formation of the spinning solution.

Spinning solution wipedout so that spliced fiber had been sent to the coagulation medium, also known as antibacterial where or spun from spliced fibers undergo coagulation. Suitable antibacterial, used as a coagulation medium, represent, e.g.�, sulfuric acid, PEG-200, dichloro methane, trichloromethane, carbon tetrachloride, ether, water, alcohols such as methanol, ethanol and propanol, acetone, n-methylpyrrolidone (NMP) or dimethyl sulfoxide (DMSO).

It is preferred that the fibers from graphene ribbons were spun from from spinning solution containing as a solvent oleum in water, used as a coagulation medium.

Spliced fibers can be vypadate directly to the coagulation environment, but it is preferred that the fibers have been spun from going to the coagulation medium through an air gap. In this air gap spliced fibers from graphene ribbons may increase with increasing orientation of the fibers, and the presence of the air gap prevents direct contact between Villeroy and coagulation medium.

The coagulation spliced fibers from graphene ribbons influenced by many different factors, such as the concentration of graphene ribbons in the spinning solution additives, added to the spinning solution, the temperature of the spinning solution, the amount of spliced fibers formed from graphene ribbons, and the diameter of the spliced fibers from graphene ribbons.

The composition and concentration of coagulation medium and/or the temperature of the coagulation bath can be used for debugging speed Koa�ulali and ability to control the spliced fibers formed from graphene ribbons, to stretching and orientation of graphene ribbons in the resulting fiber.

Know the use of 96% sulfuric acid as a coagulation medium in the field of spinning fibers from carbon nanotubes (CNT) in a very small experimental equipment and use only very small amounts of solvent. Currently, it was found that the concentration of sulfuric acid in the coagulation medium affects the reaction of chlorosulfonic acid in sulfuric acid. At high concentration of sulfuric acid in the coagulation medium, for example, when the concentration of sulfuric acid of 96%, the reaction will be slow. The lower the concentration of sulfuric acid in the coagulation medium, the faster will be the reaction of chlorosulfonic acid, for example, when the coagulation medium was used 70% sulfuric acid, the reaction proceeded much faster than 96% sulfuric acid, but still uncontrollable. The reaction of chlorosulfonic acid with coagulation medium containing only water, i.e. 0% sulfuric acid, proceeded very rapidly.

Coagulation medium with different concentrations can be used to control the rate of coagulation spliced fibers formed from graphene ribbons, coagulation environment. It is preferred that the coagulation medium performance�allala a sulfuric acid concentration in the range of 70-100%, and more preferably in the range of 90-100%.

At high concentrations of sulfuric acid in the coagulation medium, the coagulation reaction will be slow, and spliced fibers from graphene ribbons will be easy to pull. At relatively low concentrations of sulfuric acid in the coagulation medium, the coagulation reaction will be fast, which will reduce the ability of the spliced fibers formed from graphene ribbons, to stretching. Therefore, by changing the concentration of the coagulant is possible to adjust the ability to stretch spliced fibers formed from graphene ribbons.

Increased ability to extrude spliced fibers formed from graphene ribbons, has special advantages for fibers containing long graphene ribbons. The increased speed of spliced fibers formed from graphene ribbons, leads to an increased orientation of graphene ribbons in the fibers, and hence to achieve high strength in the fibers formed from graphene ribbons.

Alternatively, the temperature of the coagulation medium can be used to control the speed of the reaction solvent in the coagulation medium and to control the rate of coagulation spliced fibers formed from graphene ribbons, and, thus, the ability to extrude spliced fibers, educated� of graphene ribbons.

The reaction of the coagulation of the spinning solution containing graphene ribbons in chlorosulfonic acid in the coagulation medium containing sulfuric acid, can be highly exothermic. It is preferred that the heat coagulation of the medium was large enough to prevent boiling of coagulation environment. Heat coagulation bath containing sulfuric acid as a coagulation medium depends both on the concentration of sulfuric acid, and the temperature of the coagulation bath. The temperature of the coagulation bath should be below 0°C to prevent ice formation on the equipment. The temperature of the coagulation bath should be above the melting temperature of the coagulation medium. When coagulation medium is water, the temperature of the coagulation bath should be above 0°C to prevent ice formation in the coagulation bath. When using sulfuric acid as a coagulation medium the temperature of the coagulation bath should be maintained carefully, since the melting point of sulfuric acid is strongly dependent on its concentration. It is preferred that the temperature of the coagulation bath were in the range of 0-10°C, and more preferably, the temperature of the coagulation bath was 5°C for maximum heat � environment coagulant without the formation of ice on the equipment and/or coagulation tub.

The rate of formation of fibers from graphene ribbons and thus, its acceleration is in the air gap or in the coagulation medium is usually set by the speed of high-speed spinning of the disc, which is preferably installed in a location where fibers from graphene ribbons were neutralized and washed. However, the rate of spliced fibers can also be enhanced by the flow velocity of the coagulation medium in wypadanie spliced fibers directly into the coagulation medium or slow coagulation spliced fibers formed from graphene ribbons, selected coagulation environment.

In the methods according to the invention the coagulation medium preferably flows in the same direction in which the oriented fibers of graphene ribbons. The flow velocity of the coagulation medium can be chosen in such a way that it was below, equal to or higher than the speed of the fibers formed from graphene ribbons. The flow velocity of the coagulation medium can be used to further adjust the speed of coagulation of spliced fibers formed from graphene ribbons, when the rate of coagulation is relatively small, for example, using a coagulation medium with a high concentration of sulfuric acid, for example, 96% sulfuric acid, or by using a coagulation medium with moderate concentrations�radiation sulfuric acid, for example, 70% sulfuric acid. Sulfonic acid in the coagulation reacts with water present in sulphuric acid, with formation of HCl in the form of steam and sulfuric acid, which increases the concentration of sulfuric acid in the coagulation medium. The contents of the coagulation medium to the content of the spinning solution, therefore, must be large in order to avoid a significant increase in the concentration of sulfuric acid.

When the flow velocity of the coagulation medium and the speed of the fibers formed from graphene ribbons, equal, affect the rate of coagulation will be limited because of coagulation of the medium will be difficult to penetrate the bundle of spliced fibers and the coagulation medium on the border of the fibers and the coagulation medium is not updated. When the flow velocity of the coagulation medium is less than the rate of fibers formed from graphene ribbons, the effect of coagulation will be improved because of the speed differential provides the ability for coagulation medium to penetrate into the bundle of spliced fibers. However, the regeneration rate of the coagulation medium on the border between the spliced fibers from graphene ribbons and coagulation environment will be limited due to the formation of the boundary layer. Generally, it is preferred that the flow velocity of the coagulation medium was higher than the speed of fiber into�on from graphene ribbons, to ensure that the coagulation medium can penetrate into the bundle of spliced fibers, and on the border between the fibers and the coagulation medium had a high regeneration rate of the coagulation medium. However, the flow velocity of the coagulation medium, smaller or equal to the speed of the fibers from graphene ribbons can be desirable when speed increases, the fibers from graphene ribbons can not be achieved due to the sudden increase in speed of the fiber, as, for example, in the air gap, but can be achieved by the slow increase in speed of the fiber. The rate of coagulation should correspond to the time during which the spliced fibers formed from graphene ribbons, undergo acceleration.

When using a coagulation medium, low concentration of sulfuric acid, at the very least - 0% sulfuric acid, coagulation occurs instantly, and the flow velocity of the coagulation medium cannot be used to adjust the speed of coagulation of spliced fibers formed from graphene ribbons.

It is preferred that the coagulation medium flowed through the transport tube along with fibers formed of graphene ribbons. The length of the transport pipe depends on the speed of the fibers formed from graphene ribbons, and the time required for the implementation of coagul�tion of fibers, formed from graphene ribbons. The height difference between the level of the coagulation bath to the outlet of the transporting pipe can be used for adjusting the frictional force of coagulation of the medium about the fiber from graphene ribbons to achieve the required level. It is preferred that the fibers from graphene ribbons fell into the transporting pipe directly after getting there coagulation environment to facilitate the free activation method.

Alternatively, spliced fibers formed from graphene ribbons, wipedout directly, or through an air gap, a coagulation bath in which the environment of the coagulant is basically a constant liquid. In the coagulant bath may occur minimum displacement environment of the coagulant, as part of the fluid coagulant may be fascinated by the fibers formed from graphene ribbons that are moved through the bath of coagulant, and/or a small flow of coagulant to be added to the bath of coagulant, to replenish a bath of coagulant, as part of the environment of coagulant will be fascinated by the fibers formed from graphene ribbons that are extracted from the coagulant bath. However, regarding the speed of the fibers formed from graphene ribbons, the coagulant bath for in this respect rassmatrivat� as stationary.

It is preferred that the coagulation medium flowed through the transport tube along with fibers from graphene ribbons. The use of distributor pipes allows actuation method for spinning fibers from graphene ribbons. Spinning of fibers from the spinning solution is carried out in such a way that the spliced fiber was directed to the coagulation bath. The coagulation medium flowing in a transportation pipe and leads the spliced fiber in the shipping tube. When coagulated filaments formed from graphene ribbons, and the coagulation medium are leaving the transport pipe at the outlet of the transporting pipe, filaments formed from graphene ribbons can be captured with the basket, attaching them to the trap for yarn, at start-up and transportation of the fibers formed from graphene ribbons, to the winding machine.

Is preferable to die, coagulation coagulation bath or the veil and the section of the neutralization/washing contained within a single housing, for example, a closed vessel. Any gaseous environment arising from the reaction solvent and coagulation medium, such as SO3and HCl generated by the reaction of chlorosulfonic acid used as the solvent, with water present in to�gostinnoj environment of sulfuric acid, can be easily removed from the housing through the controlled outputs, and then process in the scrubber. Filaments formed from graphene ribbons, leaving the casing through the seal or the cover that holds any gaseous environment inside the body.

The remnants of the coagulation medium, after they leave the transport pipe partly can mechanically scraped, and fibers from graphene ribbons before winding can be washed and subjected to neutralization, for example, a mixture of water/NaOH.

It should be understood that graphene ribbons used in this invention means a graphene ribbon, consisting of a single layer of carbon atoms arranged in a honeycomb manner, with any ratio of length to width. When the ratio of length to width of graphene ribbons is less than 1.5, the graphene ribbon is also sometimes called graphene sheets. Graphene ribbons with a ratio of length to width of more than 1.5 is usually called graphene ribbons. To obtain graphene sheets having a ratio of length to width of less than 1.5, carbon nanotubes, carbon nanotubes, i.e. ratio of length to diameter of carbon nanotubes, shall be less than the 4.7. For obtaining of carbon nanotubes, graphene ribbons with a ratio of length to width of more than 1.5, the aspect ratio of carbon nanotubes should comp�incumbent more than 4.7. Alternatively, graphene sheets, having the relationship of length to width of less than 1.5, can be obtained by cutting the larger graphene sheets using chemical means.

Graphene ribbons with a monodisperse distribution, i.e. all graphene ribbons with the same length and the same width, you can get through the deployment of single-walled carbon nanotubes (SWNT) and all individual SWNT before deployment have the same length.

When you deploy dolostone carbon nanotubes (single wall carbon nanotubes, DWNT), all of which have the same length, are obtained graphene ribbons with bidisperse distribution, i.e., graphene ribbons, all of which have the same length, and the outer wall of the DWNT is deployed in a wider graphene ribbon than the inner wall. Both types of graphene ribbons are present in equal amounts.

When deploying multi-walled carbon nanotubes (MWNT), all of which have the same length, are obtained graphene ribbons with a polydisperse distribution, i.e., graphene ribbons, all of which have the same length, but the obtained graphene ribbons with different width, because each wall of the MWNT is deployed in a graphene ribbon with a width that is different from others. All types of graphene ribbons with different widths of the Pris�point to the same amounts. MWNT can be formed from multiple concentric nanotubes, for example, MWNT can consist of 20 concentric nanotubes, which gives a mixture of graphene ribbons 20 different types present in equal amounts, and graphene ribbons - each of these 20 types have different width.

When you deploy a mixture of carbon nanotubes with different length, different diameter and/or different number of walls, it is possible to obtain any desired distribution of graphene ribbons.

The term "filaments formed from graphene ribbons" used in this invention should be understood as including the final product and any intermediate product spun from graphene ribbons. It covers the fibers, fibrils, fiber-binder film, tapes and membranes. It covers the liquid flow of the spinning solution spun from from spinning holes of a Spinneret, partially and fully coagulated fibers are present in the coagulation bath or coagulation of the veil and/or in the transport pipe, and it covers separated, neutralized and/or washed fibers constituting the final product.

Fig.1 schematically represents a method for the manufacture of fibers from graphene ribbons according to the invention. Graphene ribbons are dried and subsequently dissolved� in a solvent preferably, in supercyclone, most preferably, chlorosulfonic acid, to create a spinning solution. The spinning solution is supplied to a Spinneret for forming a beam of spliced fibers. Spliced fibers can be vypadate directly into the coagulation bath, but it is preferred that the fibers were spliced directed to the coagulation bath through an air gap. In this air gap and/or the coagulation bath spliced fibers formed from graphene ribbons, undergo acceleration with increasing orientation in the fibers. The air gap prevents direct contact between Villeroy and coagulation medium. The concentration of sulfuric acid and/or the temperature of the bath of coagulant can be used to adjust the speed of coagulation and to regulate the ability to stretch spliced fibers from graphene ribbons and orientation of graphene ribbons in the final fiber. The speed of the fibers from graphene ribbons is mostly determined by the speed of the spinning disk, once fibers from graphene ribbons were neutralized and washed. Coagulation Wednesday and spliced fiber is directed into the transport pipe, and at least part of the conveying pipe is at an angle to the direction of gravity. Tha� preferred to transport the pipe consisted of a horizontal part that no undesirable influence of gravity, and the vertical part intended for the collection of spliced fibers, at its introduction into the coagulation bath. Coagulated fiber mechanical pull away from excessive coagulation of the environment and neutralize (optional) and washed before winding fibers formed from graphene ribbons.

Is preferable to transport the pipe contained a vertical portion and a horizontal portion. The horizontal length of the conveying tubes is dependent on the spinning speed and the time required for coagulation of the fibers from graphene ribbons. The length of the vertical portion of the transporting pipe is dependent on the height difference between the level of the coagulation bath to the outlet of the transporting pipe to ensure that the friction force of coagulation of the medium about the fiber from graphene ribbons has reached the desired value. Is preferable that the vertical portion is started just below the level of the liquid coagulation bath to optimize friction forces of coagulation medium on the fiber from graphene ribbons and to facilitate the free activation method.

The use of distributor pipes allows actuation method �La spinning fibers from graphene ribbons. Fibers are spun from a spinning solution in such a way that the spliced fiber had been sent, preferably through an air gap, a coagulation bath. The coagulation medium flowing in a transportation pipe and leads the spliced fiber in the shipping tube. When coagulated fibers from graphene ribbons and the coagulation medium are leaving the transport pipe at the outlet of the transporting pipe, fibers from graphene ribbons can pick through baskets attach to the trap for the yarn during launch and transport of fibers formed from graphene ribbons, to the winding machine.

Alternatively, spliced fibers formed from graphene ribbons, wipedout directly, or through an air gap, a coagulation bath, and the environment coagulant is mostly stationary liquid. In the coagulant bath may occur minimum flow of coagulant, because some portion of the fluid coagulant may be stretched out fibers from graphene ribbons that are moved through the bath of coagulant, and/or a small flow of coagulant that is added to the bath of coagulant, to replenish a bath of coagulant, because some part of the environment of coagulant will stretch out the fibers formed from graphene ribbons when�and leave the coagulant bath. However, regarding the speed of the fibers from graphene ribbons, the bath of coagulant in this respect can be considered stationary.

Fig.2 represents an alternative embodiment of the invention. The spinning solution is supplied to a Spinneret or spinning kit with the formation of the beam spliced fibers. Spliced fibers can be spun from directly in the coagulation bath, but is preferred to be spliced fiber had been sent to the coagulation bath through an air gap. In this air gap and/or the coagulation bath spliced fibers formed from graphene ribbons, undergo acceleration with increasing orientation in the fibers. The air gap prevents direct contact between Villeroy and coagulation medium. The concentration of sulfuric acid and/or the temperature of the bath of coagulant can be used to debug the rate of coagulation and the ability to control pulling the spliced fibers formed from graphene ribbons, and orientation of graphene ribbons in the final fiber. Coagulation environment and spliced fiber is directed into the transport pipe containing at least two sections, of which at least one section of the transport pipe can be movable to change the height of the output Tran�portirovochnaya pipe. Thus, the level of coagulation medium in the coagulation bath can be adjusted to increase or decrease the length of the air gap to influence the orientation of the fibers formed from graphene ribbons, and to increase or decrease the flow velocity of the coagulation medium during transport of the pipe. Alternatively, the length of the last section of the conveying pipe can be changed for adjusting the height of the outlet of the transporting pipe and, thus, to increase or decrease the length of the air gap and to change simultaneously the residence time, which usually will take at least the time during which achieved complete coagulation of the fibers from graphene ribbons. The flow velocity of the coagulation medium on a conveying pipe can be adjusted by varying the amount of coagulation of the medium supplied to the coagulation bath, and, thus, in the shipping tube. The total length of the conveying tubes is determined by the speed of coagulation of spliced fibers in selected coagulation environment. Typically, the length of the transport pipe can be adjusted to achieve at least a minimum length to achieve complete coagulation spliced fibers formed from graphene ribbons.

The flow velocity COA�elezioni environment, you can choose so she was less than, equal to or greater than the speed of fibers formed from graphene ribbons. When the flow velocity of the coagulation medium and the speed of the fibers from graphene ribbons are equal, the effect of coagulation will be limited, as the coagulation medium is difficult to penetrate into the beam spliced fibers and the coagulation medium is not renewed at the border of the fibers and the coagulation medium. When the flow velocity of the coagulation medium is lower than the speed of the fibers formed from graphene ribbons, the effect of coagulation will increase, as the speed differential provides the opportunity for penetration of the coagulation medium in the beam spliced fibers. However, the update rate of coagulation medium on the border of the spliced fibers formed from graphene ribbons, and coagulation of the environment is limited due to the formation of the boundary layer. Usually it is preferred that the flow velocity of the coagulation medium was higher than the speed of the fibers formed from graphene ribbons, to ensure that the coagulation medium can penetrate into the bundle of spliced fibers, and to any high speed exchange of coagulation medium on the border of the fibers and the coagulation medium. However, the flow velocity of the coagulation medium, smaller or equal to the speed of the fibers formed from graphene ribbons can be� desirable when the acceleration of the fibers formed from graphene ribbons, can not be achieved due to the sudden increase of the speed of the fibers, as, for example, in the air gap, and should be achieved by the slow increase in the speed of the fibers. The rate of coagulation should correspond to the time during which the spliced fibers formed from graphene ribbons, undergo acceleration.

The method according to this variant embodiment can be used successfully at low speeds of the fibers, for example, of the order of 1 m/min, for ways of slow coagulation, since the flow velocity of the coagulation medium and, consequently, the difference between flow rate and speed of the fibers can be easily adjusted by supplying a flow of coagulation environment.

Fig.3 is a method for the manufacture of fibers from graphene ribbons according to the invention. The spinning solution is supplied to a Spinneret to create a beam of spliced fibers. Spliced fibers can be vypadate directly into the coagulation bath, but is preferred to be spliced fiber was directed to the coagulation bath through an air gap. In this air gap and/or the coagulation bath spliced fibers formed from graphene ribbons, undergo acceleration with increasing orientation of the fibers. Air gap predotvrashteniya direct contact between Villeroy and coagulation medium. The concentration of sulfuric acid and/or the temperature of the bath of coagulant can be used to debug the rate of coagulation and the ability to regulate spliced fibers to stretching of graphene ribbons and orientation of graphene ribbons in the final fiber. Coagulation Wednesday and spliced fiber leaving the coagulation bath through a pipe in the bottom of the coagulation bath and moved in the direction of gravity vertically downward. The flow velocity of the coagulation medium is determined mainly by gravity and to a lesser extent by the friction forces between the pipe wall and coagulation environment, as well as between the fibers of graphene ribbons and coagulation medium. The flow velocity of the coagulation medium in this embodiment will be approximately 100 m/min

The method according to this variant embodiment is generally safe, when the speed of the fibers is higher than the flow velocity of the coagulation medium, which is mainly determined by gravity.

Fig.4 is a method for the manufacture of fibers from graphene ribbons according to the invention. Spliced fiber wipedout directly into the coagulation bath in the vertically upward direction, i.e. in the direction against gravity. Air gap to influence the orientation of the fibers formed from graphene ribbons, does not apply in �ƈ embodiment. However, the concentration of sulfuric acid and/or the temperature of the bath of coagulant can be used to debug the rate of coagulation and the ability to regulate spliced fibers to stretching of graphene ribbons and orientation of graphene ribbons in the final fiber. Spinning spliced fibers from graphene ribbons in the vertically upward direction is particularly preferred when the density of the spliced fibers from graphene ribbons is lower than the density of the coagulation medium. When actuation method spliced fiber will float to the upper end of the pipe, where the coagulated filaments formed from graphene ribbons can be removed from the surface. The flow velocity of the coagulation medium is determined by the fluid flow environment coagulant is fed into a conveying pipe, and the diameter of the transporting pipe and the flow rate can be set at a desired level relative to the speed of the fibers, made of graphene ribbons.

Spinning spliced fibers in a vertically upward direction is preferred at low speed coagulation spliced fibers in selected coagulation environment. When wypadanie in the air gap of such slowly coagulasa fibers formed from graphene ribbons, there is a risk that the spliced fiber b�FLS to disintegrate into small pieces because of gravity, due to their own weight, are higher than the tensile strength of the spliced fibers formed from graphene ribbons. Spliced fiber formed of graphene ribbons, spun from directly in the coagulation medium in the direction vertically upwards, are held liquid coagulation medium, and therefore will not be torn to pieces because of its own weight. The speed of the fibers formed from graphene ribbons, is mainly determined by the speed of the spinning disc after neutralization and washing of the fibers formed from graphene ribbons, but in this embodiment the speed of the spliced fibers may also increase due to the upward flow velocity of the coagulation medium, affecting the orientation of the fibers from graphene ribbons.

The method according to this variant embodiment can be used successfully at low speeds of the fibers, for example, of the order of 1 m/min for ways of slow coagulation, since the flow velocity of the coagulation medium, and therefore, the difference between flow rate and speed of the fibers, can be easily regulirovanie by supplying a flow of coagulation environment.

Fig.5 is a method for the manufacture of fibers from graphene ribbons according to the invention. Spliced fiber wipedout NEP�directly in the coagulation bath in a horizontal direction. Air gap, affecting the orientation of the fibers formed from graphene ribbons, which in this embodiment is not used. However, the concentration of sulfuric acid and/or the temperature of the bath of coagulant can be used to debug the rate of coagulation and to regulate the ability to stretch spliced fibers formed from graphene ribbons, and orientation of graphene ribbons in the final fiber. Spliced fiber formed from graphene ribbons, less exposed to the forces of gravity, since the fibers rely on coagulation liquid environment, and therefore they do not break into small pieces under the action of its own weight. In the absence of yarn the flow velocity of the coagulation medium in the transporting pipe is determined by the difference in elevation between the liquid level of the coagulation bath to the outlet of the transporting pipe. Use this position to set the height of the inlet of the overflow hole can be used to regulate the liquid level in the coagulation bath and for the regulation of the friction forces between the coagulation medium and the fibers formed from graphene ribbons, during coagulation in the transport pipe and before. This variant embodiment is particularly suitable for generating, if necessary, laminar flow coagu�ational environment in the transport pipe.

Spinning spliced fibers from graphene ribbons directly into a coagulation medium in the horizontal direction or the vertically upward direction or a vertically downward direction, is particularly suitable for slow coagulation spliced fibers formed from graphene ribbons, selected coagulation environment. When spliced fibers formed from graphene ribbons can have a high speed coagulation coagulation in selected environment, there is a risk that the spliced fibers formed from graphene ribbons, will coagulopathic directly to the output, or even in the spinning holes of a Spinneret, which will lead to blockage of the spinning holes.

The method according to this variant embodiment can be used successfully at low speeds of the fibers, for example, of the order of 1 m/min at slow methods of coagulation, since the flow velocity of the coagulation medium, and hence the difference between flow rate and speed of the fibers can be easily controlled by feeding a stream of coagulation environment.

Fig.6 is a method for the manufacture of fibers from graphene ribbons according to the invention. The spinning solution is supplied to a Spinneret or spinning kit to create a beam of spliced fibers. Spliced fibers can be vypadate directly to the head of�su from a liquid coagulation medium, but is preferred to be spliced fiber was heading in a veil of coagulation environment through an air gap. In this air gap and/or in the veil of liquid coagulation medium spliced fibers formed from graphene ribbons, undergo acceleration with increasing orientation of graphene ribbons in the fibers. The air gap prevents direct contact between Villeroy and coagulation medium. The concentration of sulfuric acid and/or the temperature of the bath of coagulant can be used to debug the rate of coagulation and to regulate the ability to stretch spliced fibers formed from graphene ribbons, and orientation of graphene ribbons in the final fiber. The veil of coagulation medium can be easily created using the system overflow.

The flow velocity of the coagulation medium in this embodiment is determined mainly by gravity and to a lesser extent by the friction forces between the fibers of graphene ribbons and coagulation medium. The flow velocity of the coagulation medium in this embodiment will be approximately 100 m/min

The method according to this variant embodiment is generally safe, when the speed of the fibers is higher than the flow velocity of the coagulation medium, which is mainly determined by the force t�sheet.

Fig.7 in the methods according to the invention schematically represents a spinning kit suitable for wypadanie fibers formed of graphene ribbons. Die contains spinning kit with dual casing having an inlet and outlet for the liquid coolant, to provide heating of the spinning solution to the optimal temperature. Spinning solution prior to contact with a die is filtered to avoid clogging of the spinning holes in applicator. Is preferable to die that contains a spinning hole, protrudes from spinning kit to avoid direct contact between the heated spinning kit with double casing and coagulation environment to ensure that the coagulation medium in the spinning set double mantle is not heated by the coolant. In addition, the prevention of direct contact of coagulation medium with a spinning set of double mantle is desirable as coagulation medium can possess corrosive properties, as, for example, a medium containing sulfuric acid with high concentrations. Material Spinneret containing spinning holes, protruding from spinning set can be selected so as to withstand the corrosive properties of coagulase�environment by the auditors, and is preferable to represent a ceramic material, e.g., glass, or metal such as platinum, gold or tantalum, or an alloy of platinum, gold and/or tantalum.

1. Spinning of graphene ribbons with the formation of fibers, which includes the stages at which serves a spinning solution containing graphene ribbons, a die, shall wypadanie from spinning solution spliced fibers formed from graphene ribbons, carry out the coagulation of spliced fibers formed from graphene ribbons in the coagulation medium getting coagulated fibers formed from graphene ribbons, puke, neutralized (optional) and washed coagulated filaments formed from graphene ribbons, and wound coagulated filaments formed from graphene ribbons.

2. Spinning of graphene ribbons with the formation of fibers according to claim 1, characterized in that the spinning solution is generated by dissolving graphene ribbons in a solvent.

3. Spinning of graphene ribbons with the formation of fibers according to claim 1 or 2, characterized in that the coagulation medium flows in the same direction, which is oriented spliced fibers from graphene ribbons.

4. Spinning of graphene ribbons with the formation of fibers according to claim 3, characterized in that the spliced fibers formed from g�Apanovich tapes, and the coagulation medium is moved in the vertical direction.

5. Spinning of graphene ribbons with the formation of fibers according to claim 4, characterized in that the spliced fibers formed from graphene ribbons, and the coagulation medium is moved in the direction vertically upwards.

6. Spinning of graphene ribbons with the formation of fibers according to claim 4, characterized in that the spliced fibers formed from graphene ribbons, and the coagulation medium is moved in the vertically downward direction.

7. Spinning of graphene ribbons with the formation of fibers according to claim 3, characterized in that the spliced fibers formed from graphene ribbons, and the coagulation medium is moved in the horizontal direction.

8. Spinning of graphene ribbons with the formation of fibers according to claim 6, characterized in that the spliced fibers formed from graphene ribbons, and the coagulation medium is moved in the vertically downward direction and at least one other direction at an angle to the vertical direction.

9. Spinning of graphene ribbons with the formation of fibers according to claim 8, characterized in that at least one other direction is the horizontal direction.

10. Spinning of graphene ribbons with the formation of fibers according to claim 8, characterized in that at least one other direction is to limit�x the angle between the horizontal direction and a vertically upward direction.

11. Spinning of graphene ribbons with the formation of fibers according to claim 1, characterized in that the coagulation medium is sulfuric acid having a concentration in the range of 70-96%.

12. Spinning of graphene ribbons with the formation of fibers according to claim 11, characterized in that the coagulation medium is sulfuric acid having a concentration in the range of 90-100%.

13. Spinning of graphene ribbons with the formation of fibers according to claim 1, characterized in that the temperature of the coagulation bath is in the range of 0-10°C.

14. Spinning of graphene ribbons with the formation of fibers according to claim 13, characterized in that the temperature of the coagulation bath is 5°C.

15. Spinning of graphene ribbons with the formation of fibers according to claim 6, characterized in that the spliced fibers formed from graphene ribbons, wipedout coagulation in the environment through an air gap.



 

Same patents:

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

FIELD: nanotechnology.

SUBSTANCE: invention relates to a method of production of carbon nanofibres and/or carbon nanotubes. The method comprises the pyrolysis of dispersed cellulosic and/or carbohydrate substrate impregnated with a compound of the element or elements, which metal or alloy, respectively, is able to form carbides in the substantially oxygen-free atmosphere comprising a volatile silicon compound, optionally in the presence of carbon compound.

EFFECT: invention enables to obtain carbon nanotubes or nanofibres of a certain shape.

15 cl, 4 dwg

FIELD: chemistry.

SUBSTANCE: apparatus for thermal treatment of carbon-containing fibrous materials includes a carbonisation device and a graphitation device insulated from the carbonisation device, between which is integrated a device for accumulating and cooling carbonised material and/or washing and drying thereof. The graphitation device can be in the form of two identical electro-graphite furnaces which are not linked with each other and arranged in parallel one over the other. The electro-graphite furnace includes a heating element, a pipe for removing volatile products, a valve at the outlet for preventing entry of gaseous medium into the furnace, pipes for feeding an inert gas, a drive mechanism for transporting the material to be thermally treated, and a cooled metal housing with a heat insulation unit, in which there are horizontal slit-type channels for transporting material. The inlet channel is in the form of a pipe with a rectangular cross-section for removing volatile products, and between its upper and lower inner surfaces over the transported material at an inclination to said surfaces there is a graphite screen with gaps between the upper surface of the channel and the upper end of the screen, and between the lower surface of the channel and the lower end of the screen. The screen divides the heating chamber into a maximum temperature area, having a heater, and a medium temperature area.

EFFECT: high efficiency and stability of the process of thermal treatment of carbon-containing fibrous materials, high quality of the end product.

4 cl, 5 dwg

FIELD: electricity.

SUBSTANCE: nanoobjects sorting method (objects with at least one spatial dimension within the range from ~0.05 nm up to ~500 nm) wherein a) the initial mix with any primary content of electrically conductive nanoobjects and more electrically conductive nanoobjects contact any part of liquid substance surface; b) energy of the above mix of nanoobjects is transmitted so that different nanoobjects depending on degree of their conductivity are subjected to different degree of heating (per time unit), at that during any non-zero period of time upon beginning of the energy transmission T temperature is maintained in any part of the above contact substance surface at the level sufficient for compliance with at least one of the following conditions: (1) temperature T differential module for any part of the above surface of the contact substance and temperature of its active evaporation (Te) is less than ΔTn (i.e. |Te-T|<ΔTn), (2) temperature T differential module for any part of the above surface of the contact substance and temperature of the active chemical reaction threshold with the above substance (Tcs) is less than ΔTn (i.e. |Tcs-T|<ΔTn), (3) temperature T differential module for any part of the above surface of the contact substance and temperature of the active chemical reaction threshold with nanoobjects (Tcn) is less than ΔTn (i.e. |Tcn-T|<ΔTn)), and moreover it is provided that nanoobjects heated up to different temperature (Tn) are subjected to different degree of fixation with the contact surface (up to failure to fix), c) non-fixed and weakly fixed nanoobjects are separated from the surface and d) at least one spatially separated object is received out of pluralities of nanoobjects, which contains nanoobjects with the average conductivity differing from the average conductivity of nanoobjects in the initial mix.

EFFECT: improving the efficiency of sorting.

7 cl, 1 dwg, 12 ex

FIELD: chemistry.

SUBSTANCE: invention relates to chemical technology, in particular to processes of carbonisation of fibrous viscose materials, and can be used in production of graphitised fibrous materials, used as filling agents of composite materials; electrodes; flexible electric heaters; filters of aggressive media; in products for sport and medical purposes, etc. The material is preliminarily subjected to relaxation processing. The obtained material, which contains a pyrolysis catalyst, is continuously transported through zones of carbonisation heating. Carbonisation is carried out to 320-360°C in not less than three zones of heating, heat- and gas-isolated one from another by transporting material with inclination from bottom to top, with increase of heating temperature from 160-200°C in the first zone by 40-60°C in each next zone of heating, in comparison with the previous one. Volatile products are simultaneously removed from the said zones into the evacuation zone, heat- and gas-isolated from the external environment and located above the heating zones and connected with them via a perforated wall. Temperature in the evacuation zone of volatile substances is set by 5-15°C higher than temperatures of the respective heating zones, temperature of the output branch piece being 5-15°C above the maximum temperature of carbonisation.

EFFECT: invention ensures increase of the process efficiency and improvement of quality of the obtained carbon fibrous materials.

2 dwg, 1 tbl, 5 ex

FIELD: chemistry.

SUBSTANCE: method involves treating viscose fibre material with pyrolysis catalysts, heating to carbonisation temperature and subsequent graphitation to temperature of 3000°C in an inert medium. Carbonisation is preceded by preparation of precursor by preliminary washing of the starting material with water and/or 5-10% sodium hyposulphite solution with heating and drying, and/or ionising irradiation with a beam of fast electrons during transportation through the irradiation chamber of an electron accelerator, and/or warm-wet synthesis of a complex catalyst on the surface of viscose fibres and in the pore system thereof in boiling 10-20% aqueous ammonium chloride solution and with addition of diammonium phosphate in ratio of 0.5-4.0, followed by steaming in hot steam and final ventilated drying with constant transportation, which enables to deposit the catalyst in form of an amorphous film.

EFFECT: high stability of the process of carbonising viscose fibre material and improved physical and mechanical properties of the obtained carbon material.

6 cl, 7 dwg, 1 tbl, 12 ex

FIELD: chemistry.

SUBSTANCE: invention relates to modification of the surface of inorganic fibre by forming a highly developed surface of inorganic fibre used as filler by forming carbon nanostructures on the surface of the fibres and can be used in producing high-strength and wear-resistant fibre composite materials. The method of modifying the surface of inorganic fibre involves the following steps: (a) soaking inorganic fibre with a solution of an α2 sinter fraction in organic solvents; (b) drying the soaked fibre; (c) heat treatment of the soaked inorganic fibre at 300-600°C; (d) depositing a transition metal salt onto the surface of the fibre heat treated according to step (c); (e) reducing the transition metal salt to obtain transition metal nanoparticles; (f) depositing carbon onto the transition metal nanoparticles to obtain carbon nanostructures on the surface of the fibre. The composite material contains modified fibre made using the method given above and a matrix of polymer or carbon.

EFFECT: high strength of the composite material in the cross direction relative the reinforcement plane by preventing surface deterioration when modifying with carbon nanostructures.

9 cl, 3 ex, 1 tbl, 5 dwg

FIELD: process engineering.

SUBSTANCE: proposed method comprises processing initial cellulose fibrous material by liquid-phase composition containing silanol groups with molecular weight varying from 900 to 2400 and viscosity varying from 520 to 1700 cPs, and 2-7%-water solution of fire retardant. Processed material is dried to 105-125°C for 60-120 min. Then, carbonisation is performed in air at 140-170°C for 25-40 min. Carbonisation is terminated at 700°C to proceed with high-temperature processing at, at least, 2200°C.

EFFECT: high physical properties and yield.

4 cl, 6 ex

FIELD: chemistry.

SUBSTANCE: invention relates to heterogeneous catalysis and can be used to recycle hydrocarbons and halogen-substituted hydrocarbons when producing composite materials, catalysts, sorbents and filters. Catalytic pyrolysis of hydrocarbons is carried out at 500-700°C on a catalyst obtained by dispersing articles of solid nickel and alloys thereof with other metals, e.g., iron, chromium, as a result of reaction with 1,2-dichloroethane vapour. The catalyst contains dispersed active nickel particles attached to carbon nanofibres with diameter 0.1-0.4 mcm. The starting material used is bromine- or chlorine-containing hydrocarbons, alkanes, olefins, alkynes or aromatic hydrocarbons, e.g., ethane, propane, acetylene, benzene. Output of carbon nanofibres is equal to or more than 600 g per 1 g metal.

EFFECT: high efficiency of the method.

5 cl, 2 dwg, 9 ex

FIELD: chemistry.

SUBSTANCE: dust-like or granular solid substance is continuously sprayed onto the outer surface of a hollow drum substrate 2. After deposition, the catalyst on the revolving substrate enters reaction zone 3, into which carbon-containing gas is continuously fed through a gas-distributing collector 17, and gaseous pyrolysis products are continuously output through a nozzle 18. The reaction zone is heated with infrared heaters 7. The end product is removed from the substrate using a blade 9 and a cylinder brush 10, and then unloaded from the apparatus by an auger 14.

EFFECT: invention enables continuous synthesis of carbon fibre materials.

5 cl, 2 dwg, 2 ex

FIELD: chemistry.

SUBSTANCE: method includes fractionating feed stock, steaming fractions with fourfold washing, first acid hydrolysis with threefold washing, second acid hydrolysis with threefold washing, third acid hydrolysis with threefold washing, first bleaching with threefold washing and second bleaching with fourfold washing.

EFFECT: improved quality of the end product and optimisation of the process.

1 ex

FIELD: metallurgy.

SUBSTANCE: invention can be used for powder metallurgy. Method of production of the titanium carbide includes heating of the charge containing titanium dioxide and powder of nanofibrous carbon with specific surface 138…160 m2/g at weight ratio of titanium dioxide and powder of nanofibrous carbon 68.5:31.5, at temperature 2250°C.

EFFECT: invention reduces content of free carbon in the titanium carbide to below 1,5%.

3 ex

FIELD: nanotechnologies.

SUBSTANCE: inventions relate to nanotechnology and may be used to manufacture catalysts and sorbents. Graphene pumice contains graphenes arranged in parallel at distances of more than 0.335 nm, and amorphous carbon as a binder at their edges, with the graphene-binder ratio from 1:0.1 to 1:1 by mass. The specific area of the surface is more than 1000 m2/g. The absolute hardness is 1 unit by the Mohs scale and less, specific density is 0.008-0.3 g/cm3 for solids, loose specific density of 0.005-0.25 g/cm3 for granules. The composition is produced by burning of a homogeneous powder mix of graphite oxide, unstable organic material and organic and inorganic metal salts with the moisture of all components of 10-15% in a heat-resistant open or tight mould. The source material for the binder is represented by chemical compounds capable of being in a liquid state up to 180°C, not soaking the graphite/graphene surface and damaged at a temperature of not more than 800°C. Graphene pumice is activated by restoration in hydrogen at 400-450°C and pressure of 0.05-0.11 MPa for 10-30 min or in methane at 800-950°C for at least 1 hour at atmospheric pressure with subsequent cooling.

EFFECT: produced sorbents make it possible to multiply increase the capacity of reservoirs for the storage and transportation of natural gas.

15 cl, 8 dwg, 2 tbl, 4 ex

FIELD: process engineering.

SUBSTANCE: invention relates to machine building, particularly, to making of protective coating on parts subjected to high temperatures and mechanical stresses. Proposed method comprises cleaning of parts and vacuum chamber in glow discharge in inert gas atmosphere, ionic etching and coat application by deposition from vapour phase. Note here that prior to coat application the ion-plasma cementation is executed along with ionic etching. This is performed by feed of carbon-containing gas into the chamber and part heating with the help of two magnetrons operated in dual mode. Cementation is alternated with ionic etching in N steps, where N ≥ 1, while application of coating is executed by sequential forming of consecutive alternating plies of at least one micro ply consisting of chromium and the alloy of aluminium with silicon of total depth of 1.9-2.8 mcm and at least one micro ply consisting of chromium, aluminium and silicon oxides of total depth of 0.4-1.6 mcm produced at oxygen feed into said chamber. Note here that said micro plies consist of nano plies of said materials of 1-100 nm depth composed at part feed by magnetrons with targets of chromium and alloy of aluminium with silicon.

EFFECT: longer life, higher heat resistance at high-temperature oxidation and erosion.

1 ex, 1 tbl

FIELD: medicine.

SUBSTANCE: method for producing an agent for stimulating body cells involving preparing a mixture of aqueous solution of selenious acid and PEG 400; that is followed by preparing a mixture of hydrazine hydrochloride and PEG 400; the prepared mixtures are combined; the solution is put to dialyse against distilled water; surplus of water is driven off; the produced solution is added with hexamethylene tetramine; pH is reduced to 7.2-7.4; the method is implemented in certain circumstances.

EFFECT: producing high-effective, ecologically safe agent by the synergism of colloidal selenium and hexamethylene tetramine on body cell stimulation.

1 dwg, 2 tbl, 4 ex

FIELD: medicine.

SUBSTANCE: method for producing an agent inhibitory the tumour cell growth, involving preparing a mixture of aqueous solution of selenious acid and PEG 400; that is followed by preparing a mixture of aqueous solution of hydrazine hydrochloride and PEG 400; the produced mixtures are combined; the solution is put to dialyse against distilled water; surplus of water is driven off in a rotary evaporator; the produced solution is added with silymarin dissolved in Solufor with dialysis against distilled water; pH is reduced to 7.2-7.4; the method is implemented in certain circumstances.

EFFECT: agent produced by the given method possesses high inhibitory action on the tumour cell growth.

4 dwg, 2 tbl, 2 ex

FIELD: chemistry.

SUBSTANCE: invention can be applied in the production of a cathode material for chemical current sources, as well as thermistors, resistors, devices for information recording and storing. The method of obtaining nanoneedles of sodium vanadium oxide bronze with the composition α'-NaV2O5 includes obtaining a reaction mixture, which contains sodium metavanadate hydrate NaVO3·2H2O, and addition of sodium hydroxide to the mixture until pH 7.5-9.5 is set. The reaction mixture is placed into the autoclave and hydrothermal processing, heating to 140-180°C and exposure at the said temperature for 24-48 hours are carried out. The reaction mixture additionally contains vanadium sulphate hydrate with the composition VOSO4·3H2O, taken in an equimolar quantity relative to sodium metavanadate hydrate. The obtained product is filtered, washed and dried.

EFFECT: invention makes it possible to exclude the application of harmful or toxic substances, included into the reaction mixture composition.

2 dwg, 3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to chemistry and can be used in producing nanoelectronic, optoelectronic, sensor and photovoltaic devices, as well as for storing energy. The method includes depositing an aluminium film with thickness of 1-100 nm on an insulated substrate, sputtering thereon a film of a transition metal, e.g. Fe, Co or Ni, with thickness of 0.1-10 nm, annealing in air at temperature of 200-950°C for 0.1-10 min, heating to temperature of 700-1000°C in a reactor which is evacuated to pressure of 10-4-10-10 Torr. The method further includes successively releasing a carbon-containing gas to pressure of 1-10-4 Torr and evacuating the reactor every 1-30 s while simultaneously cooling to room temperature at a rate of 1-100°C/min.

EFFECT: invention enables to obtain films of hybrid graphene and carbon nanotubes with a given configuration at predetermined places using a simple and technologically effective method.

5 cl, 5 dwg, 5 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention can be used in the chemical industry, cosmetics and medicine in making cosmetic products, therapeutic agents, antioxidants, antimicrobial agents, radioprotective substances, compounds for gene material delivery. An aqueous nanodispersion of fullerene is produced by solving C60 fullerite crystals in N-methylpyrrolidone. The prepared solution is mixed with water and a stabilising agent, which is presented by amino acid, monosaccharide, peptide, polyvinylpyrrolidone or glycerol. That is followed by the dialysis of the prepared mixture. After the dialysis, the solution can be concentrated, e.g. by vacuum vaporisation. The process is safe as uses no toxic solvents.

EFFECT: simplifying the process by eliminating the use of pre-milled fulleren crystals, ultrasonic treatment and heating.

2 cl, 26 dwg, 4 ex

FIELD: physics.

SUBSTANCE: photolithographic interference method includes generating three coherent light beams and obtaining a two-dimensional periodic interference pattern thereof; the first two coherent beams are generated in the same plane of incidence and the third beam is generated in a plane perpendicular to the first; the first two beams have the same intensity and the third beam has intensity double that of the first beam.

EFFECT: obtaining non-defective nanosized two-dimensional periodic structures.

5 cl, 4 dwg

FIELD: carbon materials.

SUBSTANCE: weighed quantity of diamonds with average particle size 4 nm are placed into press mold and compacted into tablet. Tablet is then placed into vacuum chamber as target. The latter is evacuated and after introduction of cushion gas, target is cooled to -100оС and kept until its mass increases by a factor of 2-4. Direct voltage is then applied to electrodes of vacuum chamber and target is exposed to pulse laser emission with power providing heating of particles not higher than 900оС. Atomized target material form microfibers between electrodes. In order to reduce fragility of microfibers, vapors of nonionic-type polymer, e.g. polyvinyl alcohol, polyvinylbutyral or polyacrylamide, are added into chamber to pressure 10-2 to 10-4 gauge atm immediately after laser irradiation. Resulting microfibers have diamond structure and content of non-diamond phase therein does not exceed 6.22%.

EFFECT: increased proportion of diamond structure in product and increased its storage stability.

2 cl

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