Method of receiving of carbon-bearing nano-materials

FIELD: nanotechnology.

SUBSTANCE: invention is provided for nanoelectronics, analytical chemistry, biology and medicine and can be used for manufacturing of sensors, polymers and liquid crystals. Between volumes of liquid hydrocarbon composition and electrically conducting liquid it is formed boundary, on which there are actuated microplasmous discharges by means of voltage application between electrodes, located in these volumes. Using power supply with frequency 50 Hz, providing smoothly varying of preset voltage from 0 up to 4000 V, it is implemented anodic or cathodic high-voltage polarisation of boundary and high-temperature electrochemical conversion with formation of carbon-bearing nano-materials. In the capacity of liquid hydrocarbon compound can be used, for instance, benzol or octane; in the capacity of electrically conducting liquid - solution of potassium hydroxide, solutions of halogenides of alkaline metals. On boundary it can be located diaphragm, implemented of glass or from aluminium foil with oxide coating.

EFFECT: receiving the ability to implement controllable synthesis of carbon-bearing nano-materials.

8 cl, 6 dwg, 3 tbl

 

The invention relates to a process for the synthesis of carbonaceous materials and can be used for the production of fullerenes, nanotubes and other nanomaterials and their derivatives, which find wide application in nanoelectronics in analytical chemistry to obtain sensors and nanochemistry, biology and medicine, to obtain fullerensoderzhashchikh polymers and liquid crystals.

Traditional methods of production of fullerenes, for example, include a method of laser evaporation, arc evaporation, the method of high-frequency induction heating, the method of combustion, pyrolysis, etc.

A known method of producing fullerenes using arc evaporation of graphite electrodes in a helium atmosphere [W. Kratschmer Nature. 347, s-358. 1991].

Known methods for producing fullerenes [RU No. 2178766 C1 and 2186022 C1, year], in which the fullerenes produced by sublimation of carbon-containing material by exposing it to high-temperature fields. In these ways carbonaceous material such as graphite 14, served in the reaction zone of the apparatus and the influence of high-temperature field at T=3×103-9×103°C. the Box is formed from a flowing stream or plasma by electric discharge at a voltage of 15-25 kV.

In the above methods the starting material to obtain fullerenes is graphite. IU the od requires more power consumption. Moreover, it is difficult to extract fullerensoderzhashchie soot from the reaction zone.

A known method of producing fullerenes [WO 9506001, 1995] the pyrolysis of a number of aromatic hydrocarbon compounds. The pyrolysis is performed in the gas phase at temperatures up to 3000°C With subsequent condensation of the vaporized hydrocarbon source.

The disadvantages of this method include complex hardware performance and high energy to create a high temperature.

All of the above methods for the synthesis is carried out in an atmosphere of inert gas, which requires sealed equipment.

Known method for synthesis of carbon nanomaterials, including fullerenes [US 2003049195 A, 2003] by burning in the flame aromatic hydrocarbon fuels, which leads to their conversion and obtaining of extractable fullerenes. In the incinerator [US 2003143151 A, 2003] introduce oxygen-containing gas, a hydrocarbon gas fuel and carry out the drip feed of hydrocarbon fuel.

The disadvantages of this method include the explosion.

The known method [US 2004258604 A, 2004], in which receive the mixture from C60with hydrogen with the lowest (36With40With42With44C48C50C52C54C58) or higher (C72With76) fullerenes by using high voltage AC arc discharge in fluid is th bengalboy or toluene environment. The electric field of the order of 15-20 kV passes through graphite electrodes, whose pointed ends introduced into the liquid. After removal nerastvorim of soot particles by filtering spend vacuum evaporation of the treated liquid and rinse (HPLC) and the analysis of the obtained particles by the method of mass spectrometry, showing the presence of fullerenes from C50to C76.

The disadvantages of this method include the explosion.

The known method [US 5876684 A, 1999], which proposed a number of systems in which the hydrocarbons in liquid or gaseous form are used as a carbon source and to this end are subjected to high temperature heating due to discharge between graphite electrodes.

This method is chosen as a prototype.

Its disadvantages are that the method requires a high energy consumption and is explosive.

The present invention is to develop a new method of obtaining a carbon-containing compounds based on the method of excitation of microplasma discharges at the interface of two immiscible liquids.

The technical result - controlled synthesis of carbon nanomaterials.

The problem is solved in that, as known, in a method of producing carbon nanomaterials high-temperature conversion is subjected to fluid the e hydrocarbon compounds.

What's new is that high-temperature electrochemical conversion is carried out by high-voltage polarization boundary which is formed by the displacement of liquid hydrocarbon compounds with a volume of conductive liquid, and excitation mentioned on the boundary of the microplasma discharges.

In addition, as a liquid hydrocarbon compounds using an aromatic or saturated hydrocarbons, for example benzene or octane.

In addition, as the conductive liquid, using an aqueous solution of a conductive liquid such as potassium hydroxide or alkali metal halides or any other conductive liquid.

In addition, microplasma discharges at the interface excite by application of voltage between electrodes placed in the liquid hydrocarbon compounds and the amount of conductive liquids.

In addition, carry out either anodic or cathodic high-voltage polarization boundary using a pulsed power source with a frequency of 50 Hz, which allows you to smoothly change the setpoint voltage from 0 to 4000 Century

In addition, at the interface of host membrane, or glass, or made of aluminum foil coated with an oxide coating.

In addition, the border section which may be natural, horizontal without a membrane.

In addition, to increase the duration of the microplasma process continuously replenishing amounts of the phases, or use a flow-through cell.

In addition, the product obtained after the initial high-temperature electrochemical conversion, containing a small amount of fullerenes or predecessors of fullerenes, repeatedly subjected to high-temperature electrochemical conversion to increase the output of fullerenes.

The advantage of this method is the use of high-voltage electrochemical synthesis, which is compared with the chemical synthesis of more powerful tool because it allows you to control the synthesis process by using the changes of electric parameters. Selection as a method of high-temperature electrochemical conversion method of excitation of plasma processes in solutions of electrolytes caused by high-voltage polarization phase boundary, due to the fact that it is a rapid non-equilibrium processes, followed by a local high-temperature plasma discharges, glow and ionization. Most electrochemical reactions of this process comes with stress and is a nonequilibrium high-energy processes.

Consider the necessary conditions, in nikeysha at the interface of two liquid phases, which lead to the synthesis of new organic compounds. First, in the process of high-voltage polarization of the boundary between the liquid phase and the occurrence of microplasma discharges are formed valent unsaturated radicals, which are extremely active. The existence of active valent unsaturated groups and radicals leads to the appearance of new chemical compounds with microplasma processes at the interface of liquid phases. Secondly, the high temperature and high pressure, resulting in the formation of microplasma processes at the interface, create the conditions for disconnection and high-temperature synthesis. Thirdly, the composition of the aqueous phase, the presence of anions and cations provide their influence on the products of the electrochemical synthesis. Fourth, high temperature and high pressure accompanying microplasma processes at the interface of two liquid phases, lead to the destruction and burning of the organic phase to the carbon powder. The formation of cyclic organic compounds containing five - and six-membered rings, which represent intermediate products for the synthesis of fullerenes, which at high temperature microplasma discharges at the phase boundary to form fullerenes.

With the aim of exploring the capabilities of organic synthesis, e.g. is the halogenation of organic substances microplasma processes at the interface of two liquid phases in its high-voltage polarization, following studies were conducted.

As the organic phase was chosen such solvents as aromatic solvents are benzene, toluene, and to compare unsaturated hydrocarbon octane.

As the aqueous phase used aqueous 1 M solution of potassium halides, for comparison, solutions of acids and alkalis.

In turn, the phase boundary can be polarized as a cathode and an anode, that is, the electrodes that are in different phases, can be charged both positively and negatively. In accordance with this, the phase boundary flow in a variety of electrochemical processes with the formation of different reaction products, depending on the sign of the polarization.

Expected if the phase boundary from the organic phase is charged positively, the anions of the aqueous phase with the motion of the phase boundary will cause halogenoalkane products resulting from benzene in the microplasma processes at the interface of liquid phases. When the reverse polarization of the anions of Halogens should move to a platinum electrode in aqueous phase with the formation of halogen-free. I.e. the product of synthesis at different polarization boundary liquid phases must be different.

The invention is illustrated in the following graphics:

Figure 1 shows the electrochemical cell DL is holding synthesis of organic compounds.

Figure 2 shows pictures of carbonaceous particles obtained by high-voltage cathodic polarization boundary benzene - water 1 M solution of KOH, followed microplasma processes. An increase of 100,000.

Figure 3 shows pictures of the carbon particles, obtained by high-voltage anodic polarization boundary benzene - water 1 M solution of KOH, followed hard microplasma processes. An increase of 100,000.

Figure 4 shows pictures of the carbon particles, obtained by high-voltage anodic polarization boundary benzene - water 1 M solution of KOH, followed microplasma processes. An increase of 100,000.

Figure 5 shows pictures of the carbon particles, obtained by high-voltage cathodic polarization boundary octane - water 1 M solution of KOH, followed microplasma processes. An increase of 100,000.

Figure 6 shows the surface of the oxide coating of the foil between the two pores, which were obtained fullerenes, increase a, b) 10000 C) 20000.

Further, the invention is illustrated by examples of its specific implementation.

For carrying out the synthesis of organic compounds was established electrochemical cell, shown in figure 1. For HV polarization used switching power supply with a frequency of 50 Hz, which poses which enables you to smoothly change the setpoint voltage from 0 to 4000 Century

The material of the electrodes were chosen for their insolubility in these conditions, as the soluble electrodes lead to changes in ion concentration in the aqueous and organic phases.

The first electrode is a titanium needle with the working surface of 0.8 cm2is disposed as close as possible to the boundary in the organic liquid (a liquid hydrocarbon compound)to reduce the voltage drop. The second electrode was an aluminum plate with a surface equal to 4 cm2. It was posted in the aqueous phase (aqueous solution of conductive liquids) with a volume of 30 ml.

Example 1

As the organic phase used benzene (volume 30 ml)

As the aqueous phase used aqueous 1 M solution of potassium hydroxide by volume of 3 ml.

Created the phase boundary benzene - water 1 M solution of potassium hydroxide and subjected to its high-voltage cathodic or anodic polarization.

Figure 2 shows pictures of carbonaceous particles obtained by high-voltage cathodic polarization boundary benzene - water 1 M solution of KOH, followed microplasma processes. The size of the carbon particles is from 7 to 15 nm.

Figure 3 shows pictures of the carbon particles, obtained by high-voltage anodic polarization boundary benzene - water 1 M RA is a creation CON, accompanied by hard microplasma processes. The size of the carbon particles is 50 nm.

Figure 4 shows pictures of the carbon particles, obtained by high-voltage anodic polarization boundary benzene - water 1 M solution of KOH, followed microplasma processes. The size of the carbon particles comprise from 10 to 40 nm.

Example 2.

The purpose of the research of halogenation of organic substances microplasma discharges at the interface of two liquid phases at high-voltage polarization phase boundary - aqueous 1 M solution of potassium fluoride (potassium chloride, potassium iodide) conducted the following study.

Forming a phase boundary benzene - water 1 M solution and subjected to its high-voltage cathodic or anodic polarization.

Products microplasma synthesis, mass, time, output and content percentage at the boundary between the benzene - water solutions of potassium fluoride, potassium chloride, potassium iodide, are presented in table 1. The sign "+" denotes anode polarization boundary liquid phases, the sign "-" as the cathode. For a more visual representation of the data in table 1 has left a number of products of the synthesis of more than 5%.

Gas chromatography-mass spectral analysis of the products of the microplasma synthesis at high voltage polarization borders the interface of two liquid phases are presented in Table 1.

According to table 1, when the cathodic polarization of the boundary between the benzene - water solution

1. Potassium fluoride synthesized three main products:

benzo[a]azulene, phenanthrene, fluoranthene.

2. Potassium chloride has four main product:

Acenaphthylene, biphenyl, phenanthrene, fluoranthene.

3. Potassium iodide - eight main products:

Acenaphthylene, biphenyl, benzo[a]azulene, phenanthrene, fluoranthene, pyrene, benzo[ghi]fluoranthene.

4. Potassium hydroxide -11 main products: biphenylene, acenaphthylene, biphenyl, benzo[a]azulene, diphenylacetylene, phenanthrene, fluoranthene, pyrene, benzo|ghi]fluoranthene, aapirin.

Under cathodic polarization, the phase boundary is charged negatively, as a consequence of the studied anions do not approach the phase boundary, and under the influence of an electric field suited to the positively charged electrode in the aqueous phase and are oxidized to free of Halogens. To neg the adverse charged boundary moving cations of hydrogen and processes with their participation, as suggested from the analysis of the fusion products, processes dehydrogenation.

When high-voltage anode polarization processes microplasma synthesis of the most favorable conditions create the iodine anions, less chlorine ions and weak synthesis is in the presence of fluoride ions and hydroxyl. As products of the halogenation is not formed, and the liberation of gas bubbles on the phase boundary occurs at anodic polarization of the anions under the influence of an electric field suited to the positively charged phase boundary, apparently, interact with cations of hydrogen and are in the form of volatile hydrogen halides). In addition, under the action of microplasma processes produced many radicals due to the high energy and the temperature of the phase boundary, is the destruction of chemical bonds formed cyclic compounds consisting of five and six-membered carbon rings.

Example 3.

As the organic phase used octane.

As the aqueous phase used aqueous 1 M solution of potassium hydroxide.

Formed the boundary of the phase boundary octane - water 1 M solution and subjected to its high-voltage cathodic or anodic polarization.

The products of the process of microplasma synthesis at the interface of these liquid phases were progulivali in a muffle furnace in a quartz am the OLE for separation of fullerenes, then was dissolved in benzene and photographed by scanning electron microscope at magnification of 100,000.

Figure 5 shows pictures of the carbon particles, obtained by high-voltage cathodic polarization boundary octane - water 1 M solution of KOH, followed microplasmin processes. The size of the carbon particles is from 7 to 30 nm.

Example 4. As the organic phase used benzene.

As the aqueous phase used aqueous 1 M solution of N3RHO4.

Forming a phase boundary benzene - water 1 M solution of N3RHO4and subjected to its high-voltage cathodic or anodic polarization.

The results of synthesis example 3 and 4 are shown in table 2.

Table 2
Gas chromatography-mass spectral analysis of the products of electrochemical synthesis at HV polarization of the interface between two liquid phases.
MConnectionTime out9-H3RHO410+H3RHO411-CON12+CON13-
KON
14+CON
benzeneoctane
135toluene6.134.92
152biphenylene11.41-12.772.321.672.151.06
152acenaphthylen12.366.45
154b is phenyl 10.734.735.0013.06
178the phenanthrene21.23-23.802.104.254.832.136.21
178anthraceneAt 23.434.198.846.121.20
202pyrene33.56-at 36.561.402.502.076.84
1.48
202fluoranthene33.0057.233.801.153.078.97
At 33.546.983.193.86
3.81
2206,7,8,9,-benzo[6]fluoren46.29-53.551.382.0024.279.15
230p-terphenyl34.98-36.040.464.2329.186.59
3.02
4-ethyl-octane48.785.536.941.30
4.92
pentacosane51.17 9.05
9-octadecenamideAt 51.6711.36
1-hepten52.145.43
2 methyl-octadecan53.485.63
9-octadecene55.70-57.876.92
is the 6.21
2201H-pyrazole, 3,4-diphenyl53.67-at 53.7013.9738.106.62
6.575.07
252benzo[K]fluoranthene52.646.212.09

The main products of synthesis during the cathodic polarization boundary benzene - N3RHO4according to the results of gas chromatography-mass spectral analysis are fluoranthene, benzo-K-fluoranthene, anthracene and biphenyl, when anodic polarization - biphenyl, anthracene, fluoranthene, but the intensity of the spectra at the cathodic polarization above.

Main products microps semennogo synthesis in the system Octan-CON at the cathodic polarization is p-terphenyl, and when anodic polarization - fluoranthene, phenanthrene, pyrene and p-terphenyl.

Example 5

To obtain carbon (fullerenes and nanotubes) on the surface of solids used boundary of two liquids separated by a membrane, carried out its high-voltage polarization and passing it microplasma processes.

Used glass membrane or aluminum foil coated with an oxide coating in microplasma mode.

On the glass membrane are formed of carbon deposits in the form of "carbon tracks that facilitate the initiation of microplasma discharges in high-voltage polarization phase boundary, i.e. microplasma discharges appear when less high voltages.

Aluminum foil coated with the oxide coating in the plasma mode is placed at the interface of the aqueous and organic phases, served on it (the interface) reference voltage. Microplasma process begins at the interface of liquid phases at high voltage its polarization is of the order of 3000 generated by the microplasma process carbon deposited on the aluminum oxide, filling the pores and forming a carbon nanotube.

Figure 6 shows the surface of the oxide coating of the foil between the two pores, which were obtained the fullerenes, increase a, b) 10000 C) 20000. See also the surface of the glass membrane d)separating the two liquid during the flow on the phase boundary microplasma processes (10000).

Example 6. For a quantitative assessment of plasma exposure on the boundary of the liquid phase was taken in 100 ml of organic liquid (benzene, or octane) and 10 ml of 1 M aqueous solutions of electrolytes, held microplasma processing boundaries of these fluids within 15 minutes, spent the extraction of fullerenes from soot, benzene, separated soot and have determined the mass of coal and dry residue. It is known that fullerenes dissolved in benzene, but their solubility is limited, so part of them is in a solution of benzene, and the part is deposited together with soot. To extract fullerenes from the soot, it is necessary to conduct multiple processing carbon black with a small amount of benzene. The dry residue after removal of benzene was analyzed by the method of mass spectrometry gas chromatography-mass spectrometer, the results are presented in table 1 and 2. The most diverse products microplasma synthesis quality and quantity are obtained by cathodic polarization "-" studied systems.

Table 3 shows data on the quantification of soot (carbon) and the dry residue for the studied systems.

Table 3
The coal mass and the mass of the dry residue in the products microplasma synthesis
PolarizationNo.The organic phaseThe aqueous phaseThe coal mass, mgThe mass of dry residue mgThe dry weight of residue/coal Mass, %
cathode1benzeneKl1823519,2
anodic2benzeneKl902022,2
cathode3benzeneKON2124018,9
anodic4benzeneKON13023 17,8
anodic5benzeneKF401025,0
cathode6benzeneKF175169,1
cathode7benzeneKI1103027,2
anodic8benzeneKI652030,8
cathode9benzeneH3RHO4451022,2
anodic10benzeneH3RHO420 420,0
cathode11benzeneKON3511of 31.4
anodic12benzeneKON481020,8
cathode13octaneKON291344,8
anodic14octaneKON5120,0
cathode15hexaneKl381539,0
anodic16hexaneKl27 1244,4

Analysis of the results shows that most of the carbon particles obtained by high-voltage polarization boundary of the system benzene-CON, and at the cathodic polarization of the particle size is slightly smaller than during anodic polarization. The size of the carbon particles is from 7 to 30 nm (figure 2). For this system obtained MALDI spectra.

The most diverse products microplasma synthesis quality and quantity are obtained by cathodic polarization "-" studied systems. For the discovery of fullerenes analysis of direct input products microplasma synthesis method ionization, laser desorption in a matrix, the so-called method of MALDI (matrix Assistant Laser Desorption Ionization"), two matrices with trihydroxyanthracene (TNA) and nitroaniline (NA), UV laser, the pulse duration is 0.5-10 NS. The radiation energy of one pulse per unit area is approximately 30-600 j/m2. The radiation intensity 1.106-5.107W/cm2. MALDI spectra showed that the formed carbon mass 792, which corresponds to the fullerene C66and a lot 840, which corresponds to the fullerene C70.

1. A method of obtaining a carbon-based nanomaterials, in which high-temperature conversion is subjected to W is dcie hydrocarbon compounds, characterized in that the high-temperature electrochemical conversion is carried out by high-voltage polarization boundary which is formed by the displacement of liquid hydrocarbon compounds with a volume of conductive liquid, and excitation mentioned on the boundary of the microplasma discharges.

2. The method according to claim 1, characterized in that as the liquid hydrocarbon compounds using an aromatic or saturated hydrocarbons, for example benzene or octane.

3. The method according to claim 1 or 2, characterized in that a conductive liquid is used, for example, a solution of potassium hydroxide, or solutions of alkali metal halides, or any other conductive liquid.

4. The method according to claim 1, wherein the microplasma discharges at the interface excite by application of voltage between electrodes placed in the liquid hydrocarbon compounds and the amount of conductive liquids.

5. The method according to claim 1 or 4, characterized in that exercise either anodic or cathodic high-voltage polarization boundary using a pulsed power source with a frequency of 50 Hz, which allows you to smoothly change the setpoint voltage from 0 to 4000 Century

6. The method according to claim 1, characterized in that the boundary is placed a membrane or glass, whether what about the made of aluminum foil coated with an oxide coating.

7. The method according to claim 1, characterized in that the boundary may be a natural horizontal formed without a membrane.

8. The method according to claim 1, characterized in that it further obtained during high-temperature electrochemical conversion of carbonaceous nanomaterials calcined in a muffle furnace in a quartz ampoule for separation of fullerenes, and then dissolved in benzene.



 

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1 cl, 1 tbl, 14 ex

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

FIELD: production processes.

SUBSTANCE: invention refers to obtaining of wear-resisting ultra-hard coatings, namely, to forming of diamond-type coatings and can be used in metalworking, engineering industry, nanotechnologies, medicine and electronics. Preliminary there performed is product surface plasma stripping by accelerated ions in vacuum chamber at pressure of 10-3 - 10 Pa. Then adhesion layer is applied by plasma method. The thickness is 1-500 nm. The layer is made from metal that belongs to the group of aluminium, chrome, zirconium, titanium, germanium or silicone or their alloys. At the same time the product receives direct or pulse negative voltage of 1-1500 V. Then there applied is intermediate layer with thickness of 1-500 nm. It consists of carbon and metal mixture. Metal belongs to the group of aluminium, chrome, zirconium, titanium, germanium or silicone or their alloys. Intermediate layer is applied at ascending changing of carbon concentration in this mixture from 5 to 95 at.%. At the same time the product receives direct or pulse negative voltage of 1-1500 V. Then there applied is at least one layer of carbon diamond-type film by graphite cathode or laser spraying or by plasma destruction of carbon-bearing gases or carbon-bearing liquid vapours.

EFFECT: increase of adhesion, wear resistance and temperature stability of diamond-type coating.

11 cl, 1 dwg, 5 ex

FIELD: metallurgy.

SUBSTANCE: invention relates to metallurgy field and can be used for manufacturing of high-duty cast iron with globular graphite. For receiving of magnesium-bearing nano- modifying agent is blended with water solution of polyvinyl alcohol, chloride of magnesium and iron in molar correlation (10-5):1:1, agreeably, it is evaporated specified mixture before gel formation after what it is implemented carbonation at temperature 350-500°C in atmosphere of inert gas with formation of carbon nanotube, filled by chloride of magnesium and iron.

EFFECT: invention decrease magnesium losses 1,5-2 times with introduction of nano- modifying agents into the cast iron.

6 ex, 1 tbl, 6 dwg

FIELD: chemistry.

SUBSTANCE: invention can be used at production of finishing compositions, film coatings, radiation-resistant materials. The diamond-carbon material contains the carbon in the form of diamond cubic modification and the X-ray amorphous phase in the mass ratio (40-80):(60-20) respectively; the content of said material is as follows (wt %): carbon 89.1-95.2; hydrogen 1.2-5.0; nitrogen 2.1-4.8; oxygen 0.1-4.7; non-combustible admixtures 1.4-4.8. This material is obtained in enclosed volume, in the gas phase inert to carbon by the detonation of carbon-containing explosive with oxygen deficiency placed into the shell of deoxidant-containing condensed phase with deoxidant/carbon-containing explosive mass ratio not less than 0.01:1. The samples of the obtained diamond-carbon material are prepared for elemental analysis by exposition at 120-140°C under vacuum 0.01-10.0 Pa during 3-5 hrs and following treatment at 1050-1200°C by the oxygen flow with the rate providing their combustion during 40-50 s.

EFFECT: invention allows to obtain the product with high carbon content, predictable properties and ultimate composition in the desired phase state.

4 cl, 1 tbl, 25 ex

FIELD: chemistry.

SUBSTANCE: invention refers to the catalytic systems based on gold; usage of nanometric gold precipitation by the condensation from vapour phase to the activated carrier; system of breathing organs defence using aforesaid catalytic systems. The method of heterogenous catalytic system making is described including: 1) condensation from vapour phase of the catalytically active gold clusters with dimensions in the range from 0.5 to 50 nm to the nanoporous carrier; 2) the following stages: (a) impregnation of water-soluble salt to the catalyst nanoporous carrier; (b) thermic treatment of the said impregnated carrier at temperature more than approximately 200°C; (c) condensation from vapour phase of the catalytically active gold clusters with dimensions in the range from 0.5 to 50 nm to the said thermically treated nanoporous carrier; 3) following stages: a) aggregation of the relatively small particles multifold and of the relatively large particles multifold to the multifold of nanoporous composite particles; b) precipitation of catalytically active gold clusters with dimensions in the range from 0.5 to 50 nm gold clusters to the said composite particles by the condensation from vapour phase. The described heterogenous catalytic system contain: 1) nanoporous carrier; at least one water-soluble salt impregnated to the said carrier; clusters of catalytically active gold with dimensions in the range from 0.5 to 50 nm precipitated on the said carrier with the penetration depth index in the range from ca 1×10-9 to ca 0.1; 2) multifold of the composite catalytically active particles characterised in that said catalytically active particles are obtained from the components containing relatively small particles and relatively large particles with said composite particles containing catalytically active gold precipitated on the relatively small particles by the condensation from vapour phase. The system of breathing organs defence including any of aforesaid heterogenous catalytic systems is described.

EFFECT: invention provides essential improvement of the method of gold-containing catalytic systems preparation and enhancing of their characteristics.

22 cl, 71 ex, 4 tbl, 58 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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