Synthetic diamond-containing substances and a method for separation thereof

FIELD: carbon materials.

SUBSTANCE: invention relates to inorganic chemistry of carbon and can be utilized when obtaining stable nano-diamond sols. According to an embodiment of invention, synthetic diamond-containing substance contains 82-91% carbon, 0.8-1.5% hydrogen, 1.1-2.2% oxygen, and 1.1-1.3% metallic impurities with content of non-diamond carbon 2-25% based on total weight of carbon. diamond-containing substance is characterized by ζ(zeta) potential from -40 to -85 mV. According to second embodiment, substance contains 97.5-98.5% carbon, 0.09-0.2% hydrogen, 0.3-0.5% oxygen, and 0.5-0.8% metallic impurities with content of non- diamond carbon 0.2-5% and zeta potential from 0 to -75 mV. Synthetic diamond-containing substance according to invention manifest high colloidal particle stability and are susceptible to be fractioned with narrow particle size distribution: 3 to 1700 nm and 3 to 8000 nm, respectively. Present substances are recovered by treating dry nano-diamond powder obtained from mixture of explosives (trinitrotoluene-hexogen or graphite-hexogen) in boiled organic solvents, succession of solvents going from hydrophobic solvents to hydrophilic ones so that each precedent solvent dissolves well in subsequent one.

EFFECT: increased economical efficiency and commodity of transportation of raw material and diamond-containing substances obtained thereof.

3 cl, 9 dwg, 4 ex

 

The invention relates to the field of inorganic chemistry of carbon, namely, nano-carbon materials and the method of their isolation, and can be used in various fields of industry and science of using powders of detonation nanodiamonds or sols.

Known synthetic diamond carbon material [p. RF 2046094, IPC SW 31/04,06, publ. 20.10.95,, bull.№29]. Specified material contains elements in the following ratio, wt. %:

Carbon65-80
Hydrogen0,6-3,3
Nitrogen1,4-3,4
Oxygena 13.3-33,0,

when this carbon contains 8-40 wt.% non-diamond forms.

Closest to the claimed is amaturenude substance [p. RF 2183583, IPC SW 31/06, publ. 20.06.2002,, bull.№22]. This substance contains elements in the following ratio, wt. %:

Carbon89-93
Silica particles, metal1.5
Hydrogen, oxygen and nitrogenrest

this 96,0-a 99.6 wt. % of carbon contained in a diamond shape, and the specific surface of the powder obtained substance is within 400-500 m2/year

Weeks is the action known diamond-bearing substances, synthesized by the detonation of explosive substances in various media, are numerous organic ligands due to incomplete oxidative destruction of organic products of the explosion, a high content of non-diamond forms of carbon impurities of metals and non-combustible impurities, which reduces the Zeta-potential of the particles affects the hydrophilicity of the surface of nanodiamonds and, accordingly, the colloidal stability of their hydrosols.

The closest way to the claimed method is [p. the Russian Federation, 2183583, IPC SW 31/06, publ. 20.06.2002,, bull. No. 22], where the diamond-containing substance high purity receive additional cleaning of the primary powder, which is carried out in several successive stages by treatment with a solution of alkali, hydrochloric or nitric acid, washing the precipitate with distilled water to pH 7 after each stage and the subsequent washing in perchloric acid. Next, the precipitate is washed with distilled water to a pH of 6.5 to 7.0, the water is drained by the method of decanting, the residue is concentrated in a centrifuge and dried at a temperature of +100 -120°to a moisture content of 1-2%.

The disadvantage of this method is the complexity of the method, requiring the use of containers made of different materials (stainless steel - processing alkalis, porcelain or glass - nitric, hydrochloric acid), costs associated with a large number of distillers the authorized water for washing powder from a strong acid to a pH of 7, and time for sediment (required for decanting solutions). As well as a low degree of surface cleaning amatooriradio substances from oxidized organic matter and its associated metal impurities, so it does not acquire advantages, for example, colloidal stability, size of units and hydrophilicity of the surface.

The main task, which is directed to the claimed technical solution is to obtain a synthetic diamond-containing substances with properties to repeatedly reproduce a stable colloidal system and the ability to fractionation.

The technical result achieved in the implementation of the claimed group of inventions is:

- synthetic diamond-containing substances of high purity, forming svobodnodispersnye system with high colloidal stability and ability to fractionation;

- use as raw material dry substance (powder) nanodiamonds obtained not only in the process of synthesis of a mixture of explosives trinitrotoluene-hexagon (TNT-G)and a mixture of graphite-hexagon (G-G);

- savings and convenience when transporting raw materials and obtained from him a diamond-containing substances.

Specified single technical result in the exercise of invention the object - substance d is attained, however, synthetic diamond-containing substance containing carbon, hydrogen, nitrogen and oxygen, contains elements in the following ratio, wt. %:

Carbon82-91
Hydrogen0,8-1,5
Nitrogen1,1-2,2
Oxygen6,0-13,0,

including Almazny carbon in the range of 2-25%, and impurity metals of 1.1-1.3%, the Zeta-potential of -40 to -85 mV, and which has the ability to form svobodnodispersnye systems with high colloidal stability of the particles and capable of fractionation with a narrow distribution of particle sizes from 3 to 1700 nm.

Unified technical result is also achieved by the fact that synthetic diamond-containing substance containing carbon, hydrogen, nitrogen and oxygen, contains elements in the following ratio, wt.%:

Carbon97,5-98,5
Hydrogen0,09-0,2
Nitrogen0,3-0,5
Oxygen0,6-1,0,

including Almazny carbon in the range of 0.2 to 5%, and impurity metals from 0.5 to 0.8%, the Zeta-potential of from 0 to -75 mV, and which has the ability to form svobodnodispersnye systems with high colloi the Noah resistant particles and capable of fractionation with a narrow distribution of particle sizes from 3 to 8000 nm.

Specified single technical result in the exercise of invention the object of the method is achieved by the fact that the method of selection of synthetic diamond-bearing substances, including the processing of nanodiamond powders consistently in several stages boiling solvents, with the subsequent removal of solvent and drying of the powder, what's new is that the processing is subjected to the dry powder of nd obtained from a mixture of explosives "TNT-RDX" or "graphite-RDX and use of organic solvents in sequence of processing from hydrophobic to hydrophilic so that the previous solvent was well dissolved in later.

The claimed group of inventions to meet the requirement of unity of invention, since the group runobject inventions form a single inventive concept, one of the declared objects of the group allocation method, is designed to receive the other of the declared objects of the group - synthetic diamond-containing substances, all group objects of the invention aimed at solving the same problem for a single technical result.

It is known that variations in the properties of nanodiamonds extracted from the fusion products in a variety of ways, determined by the differences of their poverhnostnogo the composition. As a result of implementation of this method under the influence of the organic solvent is further removed from the surface of the particles of the organic components formed during the synthesis process, and the subsequent allocation of the burden and associated metal impurities. Thus, additional cleaning nanodiamond powders, the resulting explosive synthesis injection of charges TNT-G, or nanodiamonds obtained in the synthesis of G-D, are synthetic diamond-containing substances of high purity, forming svobodnodispersnye system (hydrosols with high colloidal stability and liseli).

The analysis of the prior art, including searching by the patent and scientific and technical information sources and identify sources that contain information about the equivalents of the claimed group of inventions for object - method and object - matter has allowed to establish that the applicant had not discovered analogues as for the method, and group claimed substances having characteristics identical with all the essential features of the method and of the inventive substances. The definition of the list of identified unique prototype for method and substances as the most similar set of features analogues revealed a combination of) the public against perceived by the applicant to the technical result of the distinctive features for each of the declared objects of the group, set forth in formulas. Therefore, each of the objects of invention meets the condition of "novelty". The features distinguishing the claimed technical solution from the prototypes that have been identified in other technical solutions in the study data and related areas of technology and, therefore, provide the proposed solutions meet the criterion of "inventive step".

As highlighted by this method of synthesis products of TNT-G or G-G diamond-containing substances have a number of General properties and characteristics, then the description of such properties does not make sense to duplicate the illustration, therefore, they are presented for one of the substances. This implies that the second substance has similar options. Figure 1 presents the size of nanoparticles and their clusters, determined by the scattering indicatrix in the Hydrosol forming svobodnodispersnye system for synthesis of TNT-G: 1 - nefrackzionirovannam substance; 2 - the simple addition of water to the fraction of large particles; 3 - the simple addition of water to the fraction of fine particles; 4 - ultrasonic treatment of the fraction of fine particles; 5 - lozol size less than 100 nm (additional fractionation fraction of fine particles). Figure 2 gives the sizes of the nanoparticles and their clusters forming svobodnodispersnye system, determined by the scattering indicatrix in the Hydrosol device - Coulter No. 5), for synthesis of G-D: 1 - nefrackzionirovannam substance; 2 - fraction of small particles; 3 - fraction of large particles. Figure 3 given the distribution nefrackzionirovannam nanoparticles and their clusters forming svobodnodispersnye system for synthesis of G-D, recorded on the system "Videotest". 4 shows the Auger spectrum of the fraction of fine particles forming svobodnodispersnye system for synthesis of TNT, figure 5 gives the radiograph (device DRON - 3) feedstock (1) and emissions from it are small fractions (2) and large (3) nanoparticles, forming svobodnodispersnye system. Figure 6 presents the EPR spectra (radiospectrometer RE 1307) feedstock (1) and the allocation of large fractions (2, 4) and small (3, 5) nanoparticles, forming svobodnodispersnye system. Figure 7 presents the IR spectra of (spectrometer firm Broker) raw materials (1) and obtained from him the substance that forms svobodnodispersnye system (2). On Fig presents the IR spectrum (spectrometer firm Broker) impurities that are removed in this way from the surface of the nanoparticles. Figure 9 shows a histogram reflecting the change in optical density hydrosols in ten cycles, drying and then adding water to the dry powder (spectrophotometer UV-300, Shimadzu).

Cleaning is performed in several stages, successively washing powder almatadema the th substances organic solvents: chloroform, benzene, acetone and alcohol. Powder, synthetic diamond-containing substance in an amount of 3 g was placed in a glass flask from heat-resistant glass, pour 50-100 ml of chloroform, set the reflux condenser and heated in a sand bath for 10-15 minutes and should be followed two main principles: a sequence of solvents must be from hydrophobic to hydrophilic; previous liquid should be well soluble (mixed followed, such as chloroform, benzene, acetone, alcohol). But can be used other combinations of other organic solvents, such as 1,2-dichloroethane, benzene, dimethylformamide, dimethylsulfoxide. Depending on the equipment used (techniques) there are various options for implementation of the method. Variants of technological methods and sequences of organic solvents is given in the examples. After completion of the cleaning process, the solvent is removed (for example by decantation), the powder is dried at a temperature of 80-100°to a moisture content of 1-2%.

Synthetic diamond-containing substance, obtained by the claimed method of fusion products of TNT-G, has the following elemental composition in wt. %: carbon 82-91; hydrogen 0,8-1,5; nitrogen 1,1-2,2; oxygen 6,0-13,0 and Almazny carbon in the range of 2-25%, and impurity metals of 1.1-1.3%, Zeta-what otential -40 to -85 mV (measured in the area of the positive electrode, the electrolyte KCI) and represents the powder from light gray to black, depending on the fractional composition.

Dimensions nefrackzionirovannam nanoparticles and their clusters in the Hydrosol, as defined by the indicatrix of scattering or sedimentation method for synthesis of TNT-G are in the range 3-1700 nm (figure 1, curve 1), the sizes of clusters fractionated particles in the Hydrosol enable liseli with dimensions less than 100 nm (figure 1, curve 5), and the range of values of specific surface area, determined by adsorption of Argos on the Gasometer GC-1, ranges from 300 m2/g with an average value of sizes of clusters of 300-400 nm (figure 1, curve 2) and 420 m2/g with the average cluster sizes of 30-50 nm (figure 1, curves 3,4).

Synthetic diamond-containing substance, obtained by the claimed method to produce the synthesis of G-D, has the following elemental composition, wt. %: carbon 97,5-98,5; hydrogen 0,09-0,2; nitrogen 0.3 to 0.5; the oxygen of 0.6-1.0 and not diamond carbon in the range of 0.2 to 5%, and impurity metals from 0.5 to 0.8%, the Zeta-potential of from 0 to -75 mV (measured in the area of the positive electrode, the electrolyte KCI) and represents the powder from light gray to black, depending on the fractional composition.

Dimensions nefrackzionirovannam nanoparticles and their clusters in the Hydrosol (presume the indicatrix of scattering on the device Coulte No. 5 (figure 2) or the "Videotest" (figure 3), for synthesis of G-D are in the range 3-8000 nm, and specific surface area measured by BET method (Brunauer - Emmet - Teller)is for fractions of diamond-containing material size 50-300 nm, 40-55 m2/g for fractions 80-1000 nm, 30-35 m2/g for fractions 2000-4000 nm, 23-27 m2/year

Proportion of chemical elements entering into the composition of the obtained synthetic diamond-bearing-forming substances svobodnodispersnye system, was determined by different methods. In figure 4, as an example, presents the results of Auger spectroscopy for the fraction of fine particles of the product of the synthesis of TNT,

Compositions of synthetic diamond-bearing-forming substances svobodnodispersnye system, presented in the table.

Party substancesView synthesisTotal mass fraction of hydrocarbon, %Mass fraction of hydrogen, %Mass fraction of nitrogen in %Mass fraction of oxygen in %Mass fraction of impurity metals, %The average particle size, D50nmZeta-potential, mV
TNT-G
182 1,52,2131,340-85
2851,21,611,01,2160-46
3910,81,16,01,1650-40
G-G
497,50,20,51,00,8750-75
598,10,10,40,80,62500-23
698,50,090,30,60,5140000

Along with the above properties, the selected data by way of the products of the synthesis of TNT-G or G-G diamond-containing substances have a number of General properties and characteristics.

Since when obtaining substances are not carried out the action on the diamond core particles, the parameters of the crystal is practical gratings and the size of the primary particles (crystallites) correspond to the parameters of the lattices and the size of the primary particles of the raw materials used and do not depend on the fractional composition. According to the radiograph (figure 5)obtained on the instrument DRON - 3, secreted fraction of the nanoparticles, forming svobodnodispersnye system are diamonds spades(111), (220), (311)). Comparative x-ray diffraction analysis of the diamond component suggest that the raw materials and selected fractions consist of identical diamond nanocrystallites. For the samples presented in figure 5, the characteristic size of the nanocrystallites, determined by the method of Hall-Williamson [Williamson O.K., W.H. Hall X-ray line broadening filed aluminium and wolfram. Acta Metallurgica, 1953, 1, 22-31], equal to 3.5 nm, and the level of microstrains insignificant and does not exceed 0.06 percent. The lattice parameter equal 0,3561±0,0007 nm, which corresponds to theoretical density nd of 3.56 g/cm3. On the surface of the nanoparticles, there is an admixture of non-diamond carbon in the range of 2-25% (peak (002)), the number of which depends on the fractional composition.

Registration spectra EPR (electron paramagnetic resonance) using RF RE 1307 showed the presence of all samples of diamond-containing substances, regardless of their fractional composition and method of synthesis (TNT-G, G-G)signal which is characteristic of nanodiamonds explosive synthesis (6, curves 1, 2, 3). The spectra are also logged signals from impurities of iron, the amplitude of which depends on the fractional composition of the sample. Kolichestvennoi impurities for the fraction of particles with small sizes can be 3-4 times more than for the fraction of particles of large size (6, curves 4, 5).

Comparison of the IR spectra of the original and derived substances registered in the IR spectrometer (Bruker), shows that as a result of implementation of the proposed method is essential to clean the surface of the nanoparticles (Fig.7).

Removed in this way from the surface of the nanoparticles pollution have a brown color and evaporation of organic solvents to form a glassy mass. According to IR-spektroskopie composition of removing impurities (Fig) presents: -och3; -CH3; =C=O; N-C=O; -O-C-O-C-; -C=C-C=C-C-, -IT, =NH, -SH. According to the data obtained using atomic absorption spectrometer quantum-2A, contains (mg/kg): Fe - 23960; Sa - 21180; Na - 19020; K - 1650; Cu - 1241,02; Mg - 1170; Cr - 509,18; Zn - 328,69; Ni - 283,61; Mn - 7,526; Co - 5,38. Using volumetric titration is determined by the S - 10800 mg/kg According to the data obtained using emission spectroscopy (spectrograph PGS-2 Karl Zeis Jena), contains (%): Ti - 4,7; Al - 1,28; Sr - 0,46; V - 0,07; Mo - 0,0152; 0,0034.

It is known that the ability to form svobodnodispersnye systems associated with the reduction of surface impurities and higher Zeta-potential, which is an important parameter in determining the stability of the nanoparticles in the Hydrosol. According to theory DLFO [BV Deryagin. To the question about the definition and value of RA is convego pressure and its role in statics and kinetics of thin layers of liquids, Colloid journal, 1955, V.17, V. 3], satisfactorily describes the aggregate behavior of the Hydrosol nanodiamonds (taking into account the small size of the particles of nanodiamond) [Gaisanova. Colloid journal, 2000, 62, 2, 272] for raw TNT-G depending on the pH of the Hydrosol, values of Zeta-potential are typically in the range of -30 ÷ -38 mV [Gaisanova. Colloid journal, 1994, 56, 2, 266. Gaisanova. Colloid journal, 2000, 62, 2, 272]. For the inventive diamond-containing substances synthesis TNT-G Zeta-potential is within -40 ÷ -85 mV, and for particle synthesis Yoy Zeta-potential is determined in the range from 0 to -75 mV. The observed low value of Zeta-potential (for parties of substances 5-6, PL.) associated with large clusters of nanodiamonds, are not applicable calculations on theory of DFLE and additional counter the gravitational forces due to the large number of clusters. The high value of Zeta-potential (for parties of substances 1-4, table). talks about the increasing energy of the electrostatic repulsion of the particles is proportional to the square of the diffuse layer potential, amounting in dilute solutions of electrolytes to the electrokinetic potential, and in combination with high surface cleanliness contributes towards the inventive diamond-containing substances properties to education svobodnodispersnye systems.

Examples of what sushestvennee way

Example 1.

Raw material (powder nanodiamonds party No. 11, synthesized according to the method of TNT-G in IWDM KSC, Krasnoyarsk) in an amount of 3 g was placed in a glass flask from heat-resistant glass with a volume of 100-150 ml, pour 50 ml of chloroform, set the reflux condenser and the sand bath is brought to a boil and boil for 10-15 minutes. After cooling, the mixture liquid is removed by decantation, and the flask with 50 ml of benzene. The process of heating, boiling and removal of the benzene solution is repeated. Such procedures are conducted sequentially with acetone and alcohol. After completion of the cleaning process, the solvent is removed by decantation, the powder is dried at a temperature of 100°to a moisture content of 1-2%. After this processing get the gray powder in the amount of 2.76 g (weight loss of 8%) in the following ratio of elements, wt. %: carbon 82-91, including Almazny carbon in the range of 2-25%; hydrogen 0,8-1,5; nitrogen 1,1-2,2; oxygen 6,0-13,0 and impurity metals of 1.1-1.3%. Then by simply adding water to the obtained powder (without application of ultrasonic treatment) receive Hydrosol, allowing fractionation by any known method (in this case by centrifugation; the centrifugation get powders with characteristics that depend on the fractional composition of which is given in table. (the party of substances 1, 2, 3). Mnogoe the Noah drying and easy addition of water as to not fractionated powder, and to separate the fractions again allows to obtain a stable hydrosols that speaks of making nanoparticles svobodnodispersnye properties.

Example 2.

The polycrystalline powder of nanodiamonds produced by LLC "real-Dzerzhinsk", obtained by blowing G-G, which is the raw material, in an amount of 5 g was placed in a glass flask from heat-resistant glass, pour organic solvent in the amount of 50-100 ml and on a sand bath for 10-15 min refluxed. After cooling, the mixture liquid is removed in any way (except for evaporation) and substitute the following solvent. Observed sequence of hydrophobic solvents hydrophilic. Recommended fluids and their sequence - chloroform, benzene, acetone, dimethylformamide, alcohol. After the cleaning process auctorial removed by decantation, the powder is dried at a temperature of 80°to a moisture content of 1-2%. After this processing get the gray powder in the amount of 4.75 g (weight loss of 5%) in the following ratio of elements, wt. %: carbon 97,5-98,5, including Almazny carbon in the range of 0.2-5%; hydrogen 0,09-0,2; nitrogen 0.3 to 0.5; the oxygen of 0.6-1.0 and impurity metals of 0.51 to 0.8. Then by simply adding water to the obtained powder (without application of ultrasonic treatment) receive Hydrosol, allowing practionier the W by any known method (in this case - by centrifugation). In the centrifugation get powders with characteristics that depend on the fractional composition of which is given in table. (party substances 4, 5, 6). Repeated drying and easy addition of water as nefrackzionirovannam powder, and a separate factions allows you to regain a stable hydrosols that speaks of making nanoparticles svobodnodispersnye properties.

Example 3.

The nanodiamond powder batch No. 11, synthesized in IWDM transmission (Krasnoyarsk) when the detonation TNT-G, which is the raw material, in the amount of 2 g is placed in the to conventional Soxhlet extractions. Regular washing powder organic solvents (chloroform, benzene, acetone, alcohol) for 10 cycles of change of each solvent in the amount of 100 ml After completion of the cleaning process, the solvent is removed by decantation, the powder is dried at a temperature of 100°to a moisture content of 1-2%. After this processing get the gray powder in the amount of 1.86 g (weight loss of 7%in the following ratio of elements, wt.%: carbon 82-91, including Almazny carbon in the range of 2-25%; hydrogen 0,8-1,5; nitrogen 1,1-2,2; oxygen 6,0-13,0 and impurity metals of 1.1-1.3%. Then by simply adding water to the obtained powder (without application of ultrasonic treatment) receive Hydrosol, allowing fractionation by any known method (Yes in the nom case - by centrifugation). In the centrifugation get powders with characteristics that depend on the fractional composition of which is given in table. (the party of substances 1, 2, 3). Repeated drying and easy addition of water as nefrackzionirovannam powder, and a separate factions allows you to regain a stable hydrosols that speaks of making nanoparticles freely dispersed properties.

Example 4.

Powder of nanodiamonds produced by LLC "real-Dzerzhinsk", obtained by blowing G-G, which is the raw material, in the amount of 2 g is placed in the to conventional Soxhlet extractions. Regular washing powder organic solvents (1,2-dichloroethane, benzene, dimethylformamide, dimethyl sulfoxide) for 10 cycles of change of each solvent in the amount of 100 ml After completion of the cleaning process, the solvent is removed by decantation, the powder is dried at a temperature of 80°to a moisture content of 1-2%. After this processing get the gray powder in the amount of 1.93 g (weight loss of 3.5%) in the following ratio of elements, wt.%: carbon 97,5-98,5, including Almazny carbon; in the range of 0.2-5%; hydrogen 0,09-0,2; nitrogen 0.3 to 0.5; the oxygen of 0.6-1.0 and impurity metals of 0.51 to 0.8. Then by simply adding water to the obtained powder (without application of ultrasonic treatment) receive Hydrosol, allowing fractionation lubesite method (in this case by centrifugation). In the centrifugation get powders with characteristics that depend on the fractional composition of which is given in table. (party substances 4, 5, 6). Repeated drying and easy addition of water as nefrackzionirovannam powder, and a separate factions allows you to regain a stable hydrosols that speaks of making nanoparticles svobodnodispersnye properties.

The inventive method allows to obtain well-treated diamond material with high Zeta-potential, ability to levy education svobodnodispersnye systems, which by simple addition of water (without the use of ultrasonic treatment) form a Hydrosol with high colloidal stability of the nanoparticles, allowing for fractionation by any known method, for example by centrifugation. Repeated drying and easy addition of water as nefrackzionirovannam the powders and to separate the fractions again allows to obtain a stable hydrosols that speaks of making nanoparticles as nefrackzionirovannam diamond-containing substances, and their individual factions ability to education svobodnodispersnye systems, this property is illustrated in the histogram (figure 9).

Received diamond-containing substances, protecting characteristics in dry form (powder is OK) convenient and economic transportation. The use as raw materials of nanodiamonds obtained as in the synthesis of TNT-G and G-G, in the form of the original dry matter, not hydrosols nanoparticles, it is also very convenient and economical to transport.

The inventive diamond-containing compounds having the ability to form svobodnodispersnye systems, can be used in biomedical research for the preparation of stable sterile colloidal solution with a certain weight concentration of particles intended for oral administration and all kinds of injections. After freezing - thawing them, nanoparticles hydrosols do not form aggregates, nanoparticles can be distributed evenly in agar gel.

In the technical fields of synthetic diamond-containing compounds having the ability to form svobodnodispersnye systems, can be used to obtain colloidal systems with increased stability of the nanoparticles in oils, organic solvents and other liquids, which allows their use in lubricating oils to improve the performance of engines, polishing pastes for processing substrates, media, polishing precious stones, etc.

1. Synthetic diamond-containing substance containing carbon, hydrogen, nitrogen and oxygen, characterized in that it contains elements ol the following ratio, wt.%:

Carbon82-91
Hydrogen0,8-1,5
Nitrogen1,1-2,2
Oxygen6,0-13,0

including Almazny carbon in the range of 2-25%, and impurity metals of 1.1-1.3%, the Zeta-potential of -40 to -85 mV, and which has the ability to form svobodnodispersnye systems with high colloidal stability of the particles and capable of fractionation with a narrow distribution of particle sizes from 3 to 1700 nm.

2. Synthetic diamond-containing substance containing carbon, hydrogen, nitrogen and oxygen, characterized in that it contains elements in the following ratio, wt.%:

Carbon97,5-98,5
Hydrogen0,09-0,2
Nitrogen0,3-0,5
Oxygen0,6-1,0

including Almazny carbon in the range of 0.2 to 5%, and impurity metals from 0.5 to 0.8%, the Zeta-potential of from 0 to -75 mV and which has the ability to form svobodnodispersnye systems with high colloidal stability of the particles and capable of fractionation with a narrow distribution of particle sizes from 3 to 8000 nm.

3. The method of selection of synthetic ALM is soderjaschih substances, including the processing of nanodiamond powders consistently in several stages boiling solvents with subsequent removal of solvent and drying of the powder, characterized in that the processing is subjected to the dry powder of nd obtained from a mixture of explosives "TNT-RDX" or "graphite-RDX and use of organic solvents in sequence of processing from hydrophobic to hydrophilic so that the previous solvent was well dissolved in later.



 

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EFFECT: increased degree of removing residual graphite under relatively low temperature preventing oxidation of diamond.

1 tbl, 7 ex

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EFFECT: simplified method allowing stability of nanodiamond suspension in various media to be improved.

3 ex

FIELD: chemical industry; cutting tool industry; mechanical engineering; methods of the production of the artificial highly rigid materials.

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2 cl, 2 ex

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1 tbl, 6 ex

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46 cl, 4 dwg, 1 ex

FIELD: treatment of diamonds.

SUBSTANCE: proposed method includes the following stages: (i) forming of reaction mass at presence of diamond in pressure-transmitting medium fully surrounding the diamond and (ii) action of reaction mass by high temperature and pressure during required period of time; diamond is of IIb type and its color is changed from gray to blue or dark blue or is enriched by action on reaction mass of temperature from 1800°C to 2600°C at pressure of from 6.7 GPa to 9 GPa (first version). Diamond of type II may be also proposed which contains boron and its color is changed to blue or dark blue by action on reaction mass by the same temperature and pressure (second version).

EFFECT: improved color of diamond by changing it from gray (brown-gray) to blue or dark blue.

31 cl, 4 dwg, 2 ex

FIELD: treatment of natural diamond for change of its color.

SUBSTANCE: proposed method includes the following stages: (i)forming of reaction mass at presence of diamond pressure-transmitting medium which fully surrounds it; (ii) action on reaction mass by high temperature and pressure during required period of time; proposed diamond is brown diamond, type IIa; its color is changed from brown to rose by action on reaction mass by temperature from 1900°C to 2300°C at pressure from 6.9 GPa to 8.5 GPa.

EFFECT: enhanced efficiency of enriching diamond color keeping its crystals intact.

30 cl, 4 dwg, 1 ex

FIELD: processes and equipment for working natural and artificial origin diamonds, possibly in jewelry for refining diamonds and for imparting to them new consumer's properties.

SUBSTANCE: method comprises steps of acting upon crystal with electron beam whose integral flux is in range 5 x 1015 - 5 x 1018 electron/cm2; annealing crystal in temperature range 300 - 1900°C and acting with electron beam in condition of electric field having intensity more than 10 V/cm at least upon one local zone of crystal for imparting desired color tone to said zone. Local action of electron beams is realized through protection mask. As irradiation acts in condition of electric field local flaws such as bubbles or micro-inclusions are effectively broken.

EFFECT: possibility for producing diamonds with different local three-dimensional colored images such as letters or patterns of different tints and color ranges.

2 dwg

FIELD: advanced techniques for creating diamonds, possibly micro- and nano-electronics for creating new super-strength construction materials widely used in different branches of industry, for producing semiconductor diamond base light emitting diodes, jewelry articles.

SUBSTANCE: diamond synthesis method comprises steps of irradiating carbon-containing materials with fluxes of magnetic mono-fields generated from plasma for time period determined by motion speed of magnetic mono-fields through irradiated material. Such process does not need high-pressure chambers, special heating members and it is possible to realize it at atmospheric pressure and room temperature or in vacuum.

EFFECT: possibility for producing high-purity diamonds of predetermined size and shapes.

8 dwg

FIELD: mineral dressing.

SUBSTANCE: method comprises charging, chemically enriching concentrate, cleaning, and discharging desired product. Chemical enrichment is carried out by way of single or multiple processing in acid or in acids and then in alkali or alkali mixture, while heating material to 900-1000°C and holding it at this temperature in inert gas medium at stirring.

EFFECT: enhanced diamond cleaning efficiency.

6 cl, 1 tbl

FIELD: carbon materials.

SUBSTANCE: invention concerns manufacture of diamond films that can find use in biology, medicine, and electronics. Initial powder containing superdispersed diamonds with level of incombustible residue 3.4 wt %, e.g. diamond blend, is placed into quartz reactor and subjected to heat treatment at 600-900оС in inert of reductive gas medium for 30 min. When carbon-containing reductive gas medium is used, heat treatment is conducted until mass of powder rises not higher than by 30%. After heat treatment, acid treatment and elevated temperatures is applied. Heat treatment and acid treatment can be repeated several times in alternate mode. Treated powder is washed and dried. Level of incombustible impurities is thus reduced to 0.55-0.81 wt %.

EFFECT: reduced level of incombustible impurities.

4 cl, 3 ex

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

FIELD: chemical industry and electronics; production of diamonds.

SUBSTANCE: the invention is intended for chemical industry and electronics. The chemical product is prepared out of the following organic compounds (in weight %): acetamide - 6.7; carbamide - 0.8; ethylene glycol - 2.0; glycolic acid - 11.7; lactamide - 8.8; glycerine - 2.3; hexamethylenetetramine - 11; indene - 7.6; 1,2-dimethylnaftaline - 2.6; 1,4 -diisopropenylbenzol - 3.3; cyclohexylphenylketon - 8.1; 4'-cyclohexylacetophenone - 7.2; 4-(1-adamantyl)phenol - 2.1; 4,4'-methylenebis (2,6-dimethyl phenol) - 2.3; α,α'- bis (4-hydroxyfenyl)-1.4-diisopropylbenzol - 0.2; phenanthrene - 11.0; lauric acid - 6.2; sebacic acid-6.3; eicosanic acid - 9.7. The indicated components are mixed with water in the ratio of 1:(1-2). The mixture is heated up to 150-200°С in vacuum of 10-1-10-6Pa. A reaction sample formed this way is refrigerated in conditions of vacuum and dried for removal of water and the volatile organic substances. The dried reaction sample is heated in vacuum up to 200-400°С for 80 hours. The invention allows to use the raw material being in lower power state as compared with the known methods and to produce the high-clean diamonds.

EFFECT: the invention ensures production of the high-clean diamonds from the raw material of the lower power state.

16 cl, 1 tbl, 1 ex, 4 dwg

FIELD: production of color diamonds.

SUBSTANCE: the invention is pertaining to the field of production of fantasy neon yellow-green diamonds of precious quality produced from the pale (discolored) or so-called "brown" diamonds of the lowest quality. The method provides for placement of a pale natural diamond in the medium capable to transfer the pressure, which then is mold into a "tablet". Then the tablet is placed in the high-pressure press (HP/HT) and exposed to machining at an increased pressure and temperature being within the range of graphite stability or a diamond being on the phase diagram of carbon for the period of time necessary for improvement of a color of the mentioned diamond. In the end the diamond is removed from press. The indicated method ensures production of diamonds of an attractive yellowish-green or yellow-green and neon yellow-green colors.

EFFECT: the invention ensures production of diamonds of attractive yellow-green colors.

22 cl, 4 ex, 2 dwg

FIELD: chemical industry.

SUBSTANCE: the invention is intended for chemical industry. To 1 g of a powder of nanodiamonds of an explosive synthesis add 100 ml deionized water. The mixture is treated with the ultrasonic dispersant for 5 minutes. The produced suspension is added with an electrolyte - NaCl solution in the quantity exceeding sorptive capacity of nanoparticles by ions of sodium, for example, 20 ml of 0.9 M solution. Then separate the disperse medium and the settling. The disperse medium is removed. The settling is added with 100 ml of deionized water and is intensively agitated. The supernatant - hydrosol of nanodiamonds is separated and dried. At multiple add-on of water to the produced powder a stable nanodiamond hydrosol is formed. The share of the surface impurities in the produced nanodiamond is reduced. Simultaneously the share of sodium ions is increased.

EFFECT: the invention allows to reduce the share of the surface impurities in the produced nanodiamond and simultaneously to increase the share of sodium ions.

1 dwg, 1 tbl

FIELD: carbon materials.

SUBSTANCE: invention is designed for use in manufacture of hydrosols, organosols, and suspensions in oils. Nano-size diamond powder is charged into ultrasonic disperser and water and modifier, in particular organic ligand such as EDTA or ethylenebis(oxyethylenenitrilo)tetraacetic acid are then added. Resulting suspension is separated on centrifuge into dispersion medium and precipitate. The latter is treated with water to form suspension, which is centrifuged to give precipitate and hydrosol, which are concentrated separately by heating in vacuum into powderlike form. When concentrating hydrosol, depending on desire, following finished products may be obtained: concentrated hydrosol, cake, or dry black powder. When concentrating precipitate, clear nano-size diamond powder is obtained. Thus obtained products are appropriate to prepare sedimentation-resistant hydrosols and organosols with no ultrasound utilized, which products have no tendency to aggregate upon freezing and thawing, boiling and autoclaving, and which can be repetitively dried and reconstituted. Surface pollution of nanoparticles is reduced.

EFFECT: enabled preparation of hydrosols with precise concentration of nano-size diamonds.

3 cl, 1 tbl, 5 ex

FIELD: chemistry.

SUBSTANCE: method comprises filling tank (11) with coolant (12) and igniting heating mixture (3) say silicon boride. At the moment of maximum heating of the graphite (5) to be processed, explosive (1), say trinitrotoluene, is initiated. The propagating explosion wave set heated mixture (3) and agent (5) to be processed into motion, and agent (5) enters closed passage between the cooled separated substrate (8) and rod (9). The passage can be diverging to provide additional compression of agent (5) and pressing substrate (8) into conical mandrel (1) under the action of shock wave. Deflecting diaphragm (7) is an insulator, and insulating layer (2) prevents agent (5) to be ignited up to the moment of its maximum heating.

EFFECT: enhanced efficiency and reduced power consumption.

1 cl, 2 dwg

FIELD: power industry, mechanical engineering and environmental control.

SUBSTANCE: the invention is pertaining to the field of high power industry, mechanical engineering and environmental control. In a explosion-proof chamber 1 with double-walls simultaneously feed a gaseous explosive mixture using pipeline 4 through channels 5 and inject hydrocarbons with the nucleuses of carbon crystallization using a pipeline 6 through an injector 7 with formation of a cone-shaped shell 8 with an inert cavity in the central zone. The shell 8 and the explosive mixture 9 form a cumulative charge. Conduct initiation of undermining of an explosive mixture 9, as a result of which the cumulative charge forms a cumulative spray 10 moving at a high speed along the axis of the cumulation. The gaseous products withdraw through pipeline 17. At collision of the cumulative spray 10 with a barrier having channels 11 of the cooling unit 2 the pressure and temperature there sharply increase ensuring growth of the formed crystals of diamond. Simultaneously conduct cooling with the help of pipelines 12 located in metal filings and granules 13. The atomized and cooled cumulative spray gets into the auxiliary chamber 3, where the diamonds 14 are separated, feed through the pipeline 15 to a power accumulator 16, in which they are settling. Separated hot hydrogen is removed for storing or utilization. The invention allows to magnify the sizes of dimensions crystals of diamond up to 800 microns and more, to decrease atmospheric injections, to reduce the net cost of the diamonds, to increase effectiveness of the device.

EFFECT: the invention ensures growth of sizes of diamonds crystals up to 800 microns and more, decrease of atmospheric injections, reduction of the net cost of the diamonds, increased effectiveness of the device.

2 cl, 2 dwg

FIELD: methods and devices used for production of diamonds.

SUBSTANCE: the invention is pertaining to methods and devices for production of diamonds and may be used in materials technology. Assemble a mold. Ignite a thermit grain and heat up the powdered graphite. After that they initiate explosion of a charge. The explosion energy sets in motion a striker, which is directly caulking the powder graphite in the capsule. After that disassemble the mold, extract the produced diamond. The invention allows to miniaturize the sizes of the charge and the mold, to simplify the production process and to use such a mold multiply.

EFFECT: the invention allows to miniaturize the charge and the mold sizes, to simplify the process of diamonds production and to use such a mold multiply.

2 dwg

FIELD: production of the jewelry quality diamonds from the natural low-grade undecoratively colored diamonds.

SUBSTANCE: the invention is pertaining to production of the diamonds of the jewelry quality from the natural low grade undecoratively colored so-called "brown" diamonds, especially from the diamonds of IIa type and IaA/B type, in which nitrogen forms predominantly B-center for improvement of heir color. The invention provides for realization of the rough faceting and molding of the undecoratively colored natural diamond for giving it the streamline form to avoid its breakup in the press of the high-pressure and heating (HP/HT press). The indicated undecoratively colored natural diamond is put in the pressure transferring medium, which then is compacted into the tablet. Then the tablet is put in the HP/HT squeezer under the high pressure and temperature kept in the field of stability of the blacklead or the field of stability of the diamond of the phase diagram of carbon for the time duration sufficient for improvement of the color of the diamond. After the operation is terminated extract the diamond from the squeezer. The method ensures production of the colorless and decoratively colored diamonds.

EFFECT: the invention ensures production of the colorless and decoratively colored diamonds.

25 cl, 6 ex, 2 dwg

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