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Method of diamond processing

Method of diamond processing
IPC classes for russian patent Method of diamond processing (RU 2451774):
Another patents in same IPC classes:
Method of producing fluoride nanoceramic / 2436877
Method involves thermomechanical processing of initial crystalline material made from metal halides at plastic deformation temperature, obtaining a polycrystalline microstructured substance characterised by crystal grain size of 3-100 mcm and intra-grain nanostructure, where thermomechanical processing of the initial crystalline material is carried out in vacuum of 10-4 mm Hg, thus achieving degree of deformation of the initial crystalline material by a value ranging from 150 to 1000%, which results in obtaining polycrystalline nanostructured material which is packed at pressure 1-3 tf/cm2 until achieving theoretical density, followed by annealing in an active medium of a fluorinating gas. The problem of obtaining material of high optical quality for a wide range of compounds: fluoride ceramic based on fluorides of alkali, alkali-earth and rare-earth elements, characterised by a nanostructure, is solved owing to optimum selection of process parameters for producing a nanoceramic, which involves thermal treatment of the product under conditions which enable to increase purity of the medium and, as a result, achieve high optical parameters for laser material.
Procedure for surface of diamond grains roughing Procedure for surface of diamond grains roughing / 2429195
Procedure for surface of diamond grains roughing consists in mixing diamond grains with metal powder and in heating obtained mixture to temperature of 800-1100°C in vacuum as high, as 10-2-10-4 mm. As metal powders there are taken powders of iron, nickel, cobalt, manganese, chromium, their alloys or mixtures. Powders not inter-reacting with diamond grains at heating can be added to the mixture.
Method of annealing crystals of group iia metal fluorides / 2421552
Method involves subjecting a grown and hardened, i.e. correctly annealed crystal, to secondary annealing which is performed by putting the crystal into a graphite mould, the inner volume of which is larger than the crystal on diameter and height, and the space formed between the inner surface of the graphite mould and the surface of the crystal is filled with prepared crumbs of the same material as the crystal. The graphite mould is put into an annealing apparatus which is evacuated to pressure not higher than 5·10-6 mm Hg and CF4 gas is then fed into its working space until achieving pressure of 600-780 mm Hg. The annealing apparatus is then heated in phases while regulating temperature rise in the range from room temperature to 600°C, preferably at a rate of 10-20°C/h, from 600 to 900°C preferably at a rate of 5-15°C/h, in the range from 900 to 1200°C preferably at a rate of 15-30°C/h, and then raised at a rate of 30-40°C/h to maximum annealing temperature depending on the specific type of the metal fluoride crystal which is kept 50-300°C lower than the melting point of the material when growing a specific crystal, after which the crystal is kept for 15-30 hours while slowly cooling to 100°C via step-by-step regulation of temperature decrease, followed by inertial cooling to room temperature.
Method of thermal treatment of single-crystal substrate znte and single-crystal substrate znte Method of thermal treatment of single-crystal substrate znte and single-crystal substrate znte / 2411311
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Method of growing heat resistant monocrystals Method of growing heat resistant monocrystals / 2404298
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Method of producing monocrystals of calcium and barium flourides / 2400573
Method involves crystallisation from molten mass through Stockbarger method and subsequently annealing the crystals through continuous movement of the crucible with molten mass from the upper crystallisation zone to the lower annealing zone while independently controlling temperature of both zones which are separated by a diaphragm. The crucible containing molten mass moves from the crystallisation zone to the annealing zone at 0.5-5 mm/h. Temperature difference between the zones is increased by changing temperature in the annealing zone proportional to the time in which the crucible moves from the beginning of crystallisation to its end, for which, while maintaining temperature in the upper crystallisation zone preferably at 1450-1550°C, in the lower annealing zone at the beginning of the crystallisation process temperature is kept at 1100-1300°C for 30-70 hours, thereby ensuring temperature difference of 450°C between the zones at the beginning. Temperature of the annealing zone is then lowered to 500-600°C in proportion to the speed of the crucible with the growing crystal. Temperature of the annealing zone is then raised again to 1100-1300°C at a rate of 20-50°C/h, kept for 18-30 hours after which the zone is cooled to 950-900°C at a rate of 2-4°C/h, and then at a rate of 5-8°C/h to 300°C. Cooling to room temperature is done inertially. Output of suitable monocrystals of calcium and barium fluorides with orientation on axes <111> and <001>, having high quality of transparency, uniformity, refraction index and double refraction is not less than 50%.
Superstrong single crystals of cvd-diamond and their three-dimensional growth Superstrong single crystals of cvd-diamond and their three-dimensional growth / 2389833
Method includes placement of crystalline diamond nucleus in heat-absorbing holder made of substance having high melt temperature and high heat conductivity, in order to minimise temperature gradients in direction from edge to edge of diamond growth surface, control of diamond growth surface temperature so that temperature of growing diamond crystals is in the range of approximately 1050-1200°C, growing of diamond single crystal with the help of chemical deposition induced by microwave plasma from gas phase onto surface of diamond growth in deposition chamber, in which atmosphere is characterised by ratio of nitrogen to methane of approximately 4% N2/CH4 and annealing of diamond single crystal so that annealed single crystal of diamond has strength of at least 30 MPa m1/2.
Ceramic laser microstructured material with twinned nanostructure and method of making it Ceramic laser microstructured material with twinned nanostructure and method of making it / 2358045
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Method for thermal processing of semi-finished abrasive tools on organic thermosetting binding agents / 2351696
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Method for thermal treatment of half-finished abrasive tools on organic thermosetting binders / 2349688
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Method of producing diamond structure with nitrogen-vacancy defects Method of producing diamond structure with nitrogen-vacancy defects / 2448900
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Method of cleaning large crystals of natural diamonds Method of cleaning large crystals of natural diamonds / 2447203
Method involves step-by-step treatment of diamonds in an autoclave at high temperature and pressure, including a step for cleaning with a mixture of nitric acid and hydrogen peroxide and a step for cleaning with a mixture of concentrated nitric, hydrochloric and hydrofluoric acids under the effect of microwave radiation. After the step for cleaning with nitric acid and hydrogen peroxide, the diamonds are treated under the effect of microwave radiation with hydrochloric acid in gaseous phase at temperature 215-280°C for 15-300 minutes. Further, the diamonds are treated with distilled water at temperature 160-280°C for 5-30 minutes in an autoclave in liquid phase. At the step for cleaning with a mixture of nitric acid and hydrogen peroxide, treatment is carried out with the following volume ratio of components: nitric acid and hydrogen peroxide 4-10:1-3, respectively, at temperature 215-280°C for 15-540 minutes in liquid phase in a system with external heating or in a gaseous phase under the effect of microwave radiation. At the step for cleaning with a mixture of concentrated nitric, hydrochloric and hydrofluoric acids, treatment under the effect of microwave radiation is carried out with the following volume ratio of components: nitric, hydrochloric and hydrofluoric acid 1-6:1-6:1-3, respectively, in gaseous phase at temperature 215-280°C for 15-300 minutes.
Method of producing fluoride nanoceramic / 2436877
Method involves thermomechanical processing of initial crystalline material made from metal halides at plastic deformation temperature, obtaining a polycrystalline microstructured substance characterised by crystal grain size of 3-100 mcm and intra-grain nanostructure, where thermomechanical processing of the initial crystalline material is carried out in vacuum of 10-4 mm Hg, thus achieving degree of deformation of the initial crystalline material by a value ranging from 150 to 1000%, which results in obtaining polycrystalline nanostructured material which is packed at pressure 1-3 tf/cm2 until achieving theoretical density, followed by annealing in an active medium of a fluorinating gas. The problem of obtaining material of high optical quality for a wide range of compounds: fluoride ceramic based on fluorides of alkali, alkali-earth and rare-earth elements, characterised by a nanostructure, is solved owing to optimum selection of process parameters for producing a nanoceramic, which involves thermal treatment of the product under conditions which enable to increase purity of the medium and, as a result, achieve high optical parameters for laser material.
Procedure for production of diamonds of fantasy yellow and black colour Procedure for production of diamonds of fantasy yellow and black colour / 2434977
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Procedure for simultaneous production of several faceted valuable stones of synthetic silicon carbide - moissanite / 2434083
Procedure consists in simultaneous growth of multitude of work pieces of moissanite crystals in cellular mould of forming graphite, in dividing them to separate crystals, in faceting, grinding and in polishing. Before faceting, grinding and polishing work pieces are first glued on a mandrel, then they are re-glued on a back side. Moissanite is polished on a ceramic polisher rotating at rate from 200 to 300 rpm with utilisation of diamond powder (spray) with dimension of a grain from 0.125 to 0.45 mcm, facilitating depth of grooves less, than length of light wave of a visible part of spectre. Also, cut and chipped edges of the work piece with defects not suitable for faceting, are crumbled and returned to a stage of growth. Grinding paste with size of a grain 0.25 mcm can be used for grinding.
Procedure for radiation of minerals Procedure for radiation of minerals / 2431003
Procedure for radiation of minerals in neutron flow of reactor in container consists in screening radiated minerals from heat and resonance neutrons. Composition of material and density of the screen is calculated so, that specific activity of radiated minerals upon completion of radiation and conditioning does not exceed 10 Bq/g. Before radiation contents of natural impurities in radiated minerals can be analysed by the method of neutron activation analysis. Only elements activated with resonance neutrons are chosen from natural impurities of radiated minerals. Tantalum and manganese or scandium and/or iron or chromium are used as elements of the screen. Chromium-nickel steel alloyed with materials chosen from a row tantalum, manganese and scandium are used in material of the screen.
Procedure for surface of diamond grains roughing Procedure for surface of diamond grains roughing / 2429195
Procedure for surface of diamond grains roughing consists in mixing diamond grains with metal powder and in heating obtained mixture to temperature of 800-1100°C in vacuum as high, as 10-2-10-4 mm. As metal powders there are taken powders of iron, nickel, cobalt, manganese, chromium, their alloys or mixtures. Powders not inter-reacting with diamond grains at heating can be added to the mixture.
Method of annealing crystals of group iia metal fluorides / 2421552
Method involves subjecting a grown and hardened, i.e. correctly annealed crystal, to secondary annealing which is performed by putting the crystal into a graphite mould, the inner volume of which is larger than the crystal on diameter and height, and the space formed between the inner surface of the graphite mould and the surface of the crystal is filled with prepared crumbs of the same material as the crystal. The graphite mould is put into an annealing apparatus which is evacuated to pressure not higher than 5·10-6 mm Hg and CF4 gas is then fed into its working space until achieving pressure of 600-780 mm Hg. The annealing apparatus is then heated in phases while regulating temperature rise in the range from room temperature to 600°C, preferably at a rate of 10-20°C/h, from 600 to 900°C preferably at a rate of 5-15°C/h, in the range from 900 to 1200°C preferably at a rate of 15-30°C/h, and then raised at a rate of 30-40°C/h to maximum annealing temperature depending on the specific type of the metal fluoride crystal which is kept 50-300°C lower than the melting point of the material when growing a specific crystal, after which the crystal is kept for 15-30 hours while slowly cooling to 100°C via step-by-step regulation of temperature decrease, followed by inertial cooling to room temperature.
Sic crystal with diametre of 100 mm and method of its growing on off-axis seed Sic crystal with diametre of 100 mm and method of its growing on off-axis seed / 2418891
Semiconductor crystal of silicone carbide includes monocrystal seed part 21 and monocrystal grown part 22 on the above seed part 21; at that, seed 21 and grown 22 parts essentially form regular cylindrical monocrystal of silicone carbide 20; at that, boundary between grown and seed part shall be determined by seed part 23 which essentially is parallel to bases of the above regular cylindrical monocrystal 20 and has deviation from axis approximately through 0.5°-12° relative to base plane 26 of monocrystal 20, and the above monocrystal grown part reproduces polytype of the above monocrystal seed part and has the diametre at least of 100 mm.
Method of producing diamond structure with nitrogen-vacancy defects Method of producing diamond structure with nitrogen-vacancy defects / 2448900
Invention can be used in magnetometry, quantum optics, biomedicine and information technology. Cleaned detonation nanodiamonds are sintered in a chamber at pressure 5-7 GPa and temperature 750-1200°C for a period time ranging from several seconds to several minutes. The obtained powder of diamond aggregates is exposed to laser radiation with wavelength smaller than 637 nm and diamond aggregates with high concentration of nitrogen-vacancy (NV) defects are selected based on the bright characteristic luminescence in the red spectral region. In the obtained diamond structure, about 1% of carbon atoms are substituted with NV defects and about 1% of carbon atoms are substituted with single nitrogen donors.

FIELD: process engineering.

SUBSTANCE: invention relates to diamond processing, in particular, by thermochemical process. Proposed method comprises applying layer of spirit glue composition onto diamond surface, said composition containing transition metal, for example, Fe, Ni or Co, and processing diamond thermally at temperature not exceeding 1000°C. To prepare spirit glue composition, powder of water-soluble salt of transition metal is used. Said powder in amount of 1-10 wt % of water solution is mixed with spirit solution of glue at salt water solution-to-glue spirit solution ratio of 1:1. Prepared mix is applied on diamond surface in 10-20 mcm-thick layer to be dried. Thermal processing of diamond is performed in two steps. Note here that, at first step, diamond is processed at 600-700°C for 1-2 min, while, at second step, it is processed at 800-1000°C for 15-30 min.

EFFECT: superhigh specific surface with nano-sized (100-200 nm) relief, expanded applications.

2 dwg, 7 ex

 

The invention relates to the field of non-abrasive processing methods of the diamond, in particular to thermochemical processing of diamond, providing diamond ultra-high specific surface area and nanoscale topography (pores, rough surface, channels, grooves and similar patterns).

Creating on the diamond surface nanostructures in the form of pores, channels, etc. can be used to introduce or deposition of nanoparticles of active metal (Ni, Co, Pt and others) with their reliable fixation on the diamond. When this diamond is inert chemically and electrochemically stable substrate, useful for holding and retaining a long time of metal nanoparticles, such as catalysts. Modified diamond materials with high specific surface promising for use as adsorbents and conveyors of a number of substances, as well as for the analysis of organic, inorganic compounds (phenols, medicinal materials, nitrates, metal ions and many others). Large specific surface of the diamond powder used in the manufacture of diamond electrodes. Currently, various research organizations and private companies conducted research on the development and use of electrodes for electrochemistry and catalysis (for water purification, electrosynthesis, electroanalysis, sensors) OS is ove diamond materials, which are more promising than electrodes made of traditional materials. To the disadvantage of the diamond electrodes include the lack of suitable methods of etching of the surface.

Known abrasive and laser processing of diamond does not provide diamonds with high specific surface area. Chemical etching of the diamond surface, for example, in the melt nitrate can increase the specific surface of the diamond, but the achievable pore size is more than 1 μm [Brisk G.P., Epishin NI, Semenov-Tian-Shansky A.S. Etching octahedral faces Yakut diamonds with the aim of podset densities of dislocations. - Diamonds, 1968, 4, p.3-5; Zhikhareva, V.P. experiments on the etching of synthetic diamonds. - Min. Proc. of Lvovski. University, 1980, 34, issue 1, s-76].

There is a method of etching the surface of the diamond in an oxygen plasma, which allows to obtain nanostructured surface of the diamond-type honeycomb with a cell size of 60-300 nm and a depth of from 500 nm to 3.5 μm [K. Honda, T.N. Rao, D. A. Tryk et al. Electrochemical Characterization of the Nanoporous Honeycomb Diamond Electrode as an Electrical Double-Layer Capacitor - J.Electrochem. Soc., 2000, 147, p.659-664]. The disadvantages of the method of etching the surface of the diamond in an oxygen plasma includes the following: part of the diamond on its surface graffitied, pores are isometric in shape with smooth walls, it is difficult to carry out bulk etching of diamond powder with a specified pore size

When the etching of the diamond surface using known methods is achieved by the shape of the pore cell, conical, spherical, which allows you to get a diamond with sverhchudesnoe surface.

The closest technical solution is the method of processing diamonds, based on the catalytic hydrogenolysis of diamond using as catalysts powders of transition metals of the iron group (Fe, Co or Ni) [Chepurov A.I., Sonin V.M., Shamayev P.P. mechanical engineering. 2002, 3, s-27]. The method used for the soldering of diamonds with metals in the manufacture of single crystal of the instrument and include heat treatment of the diamond surface with a deposited alcohol adhesive mixture powder of the transition metal particle size of about 10 μm in a stream of hydrogen at high temperatures (600-1200°C) for 5-30 minutes While ensuring etching (roughness) of the surface of the crystal required for further strong connection diamond with metal materials in the manufacture of diamond tools.

However, this method of processing diamonds provides the etching of the diamond surface with pore size > 1 µm).

The technical result of the invention to provide ultra-high specific surface area and nanoscale topography of the diamond, which provides enhanced functionality Alma is A.

This result is achieved in that in the processing method of a diamond, comprising coating the surface of the diamond layer alcohol adhesive mixture containing a transition metal such as Fe, Ni or Co, and heat treatment of diamond in a stream of hydrogen at a temperature of not more than 1000°C, for the preparation of the adhesive solution use powder water-soluble salt of the transition metal, which is in the form of 1-10 wt.% the aqueous solution is mixed with an alcoholic solution of glue with a volumetric ratio of the aqueous solution of the salt/alcohol solution of glue, equal to 1/1, put the mixture on the diamond layer thickness of 10-20 μm and dried, and heat treated diamond is carried out in two stages, the first stage of the diamond is treated in a stream of hydrogen at a temperature of 600-700°C for 1-2 min, and the second stage heat treatment is carried out at 800-1000°C for 15-30 minutes

The use of water-soluble transition metal salts, such as chlorides, sulphates and any other water-soluble salts of Fe, Ni or Co, unlike the prototype, which uses powders of the metal-catalyst is Fe, Ni or Co, provides education on the diamond surface at the first stage of processing particles of these metals the size of 20-100 nm, in the following and create the desired surface topography of the diamond. Thus, the process of interaction restored hour the CI transition metal with the surface of the diamond heat-treated diamond in the stream of hydrogen. According to the method, when applied to nanoparticles of metal powder on the surface of the diamond, is their agglomeration (clumping together) with enlargement of the particles of metal, and the diamond will infect nanoparticles and larger agglomerates. In addition, it is technically impractical to use metal powder particle size of 10-100 nm. When the concentration of the water-soluble salts of transition metals less than 1 wt.% and the thickness of the adhesive is less than 10 μm on the surface of the diamond does not form a sufficient amount of nanoparticles of transition metals, and at salt concentrations of more than 10 wt.% and the layer thickness of more than 10 μm particles glomerida that prevents the formation of nanopores. Drying adhesive for fastening salt layer of the transition metal on the diamond. The method of any drying that removes moisture. The first stage heat treatment at temperatures below 600°C does not restore the transition metal in a flow of hydrogen and at temperatures above 700°C. the recovered nanoparticles of transition metal can aglomerirovanie. When carrying out the second stage heat treatment at temperatures below 800°C does not occur, the introduction of nanoparticles of transition metal in the diamond, and at temperatures above 1000°C, the implementation process of the nanoparticles of the transition metal becomes unmanageable and particles glomerida the formation of pores of large size, and, in addition, graphitization of the diamond surface. While the first and second stages of the heat treatment are separated in time, the first stage is carried out within 1-2 min, time, ensuring the formation on the surface of the diamond recovered nanoparticles of a transition metal, and the second stage is within 15-30 min, time, ensuring the implementation of the surface of the diamond particles of the metal with the formation of nanopores.

For explanation of the present invention proposed illustration characterizing obtaining porous surface of the diamond. Figure 1 shows the formation of Fe particles after the first stage heat treatment. The main interval of particle size of 20-100 nm. Figure 2 shows the surface on the diamond after the second stage of treatment with 200 nm pore size.

Examples of specific performance

Example 1

On the surface of the octahedral faces of the diamond size 4x4 mm or an area of 15 mm2or crystal weight of 0.5 carats put thinset thickness of 15 μm, consisting of glue BF-6, diluted with ethyl alcohol, and a solution obtained by dissolving 1.5 g of powder FeCl3·6H2O in 100 ml of distilled water at a ratio of 50% by volume of an alcohol solution of glue and 50% by volume of the salt solution FeCl3·6H2O. Dried to remove moisture, then placed in the installation, created on the basis of the tubular electro is ECI "COOL" seated tube made of quartz glass [Sonin V.M., Chepurov A.I. Inorganic materials. 1994, 30, 4, s-438], through which is passed a hydrogen flow rate of hydrogen of 3 l/hour), and conducting heat treatment in two stages. At the first stage of the diamond with the dried adhesive composition is treated at a temperature of 600°C in a stream of hydrogen for 2 minutes, which provides education on the surface of the diamond recovered Fe nanoparticles (Figure 1), and the second stage heat treatment is carried out in a stream of hydrogen at 800°C for 15 minutes, time, ensuring the implementation of the Fe particles in the surface of the diamond with the formation of a relief with a pore size of 200 nm (Figure 2).

Example 2

As in example 1, but at the first stage heat treatment, the diamond with the dried adhesive composition is treated at a temperature of 700°C in a stream of hydrogen for 1 minute, the surface on the diamond represents the terrain with pore size less than 100 nm.

Example 3

As in example 1, but in the second stage heat treatment is carried out in a stream of hydrogen at 1000°C for 10 minutes, time, ensuring the implementation of the Fe particles in the surface of the diamond with the formation of nanopores. The obtained surface on the diamond represents the terrain with pore size less than 100 nm.

Example 4

As in example 1, but the adhesive mixture of the alcohol solution of glue BF-6, and a solution obtained by dissolving 5 g of the powder NiCl2·6H2O in 100 ml of dist is therouanne water. The obtained surface on the diamond represents the terrain with pore size less than 150 nm.

Example 5

As in example 1, but the adhesive mixture of the alcohol solution of glue BF-6, and a solution obtained by dissolving 7 g of powder CoCl2·6N2About 100 ml of distilled water. The obtained surface on the diamond represents the terrain with pore size less than 200 nm.

Example 6

As in example 1, but the adhesive mixture is applied to the diamond powder particle size of 0.1 to 0.2 mm, the surface on the diamond grains is relief with pore size of 120 nm.

Example 7

As in example 1, but the adhesive mixture is applied on different crystallographic faces of the crystal diamond: the octahedron {111}, cu {100} and rhombododecahedral {110}. All faces received an identical surface representing the terrain with a pore size of 200 nm or less.

Thus, the present invention allows to obtain nano-sized (100-200 nm) relief on the diamond for any crystallographic direction: the etched surface normal, i.e. perpendicular to the surface, and the metal particles are immersed vertically. This allows for a comprehensive treatment of diamond powders. With the resulting surface nanostructures are composed entirely of diamond, you have the ability to handle 3D objects, such as diamond powder. The quality is improved and so is the durability of fastening of diamond crystals in metal Kristallografiya in the manufacture of diamond tools and equipment with diamond detail. In addition, diamonds, obtained by the proposed method can be used for production of sorbents and catalysts, where the diamond is the frame material; in the manufacture of filters and causes; when creating a metal-diamond composites, heat sinks in electronic devices.

The processing method of a diamond, comprising coating the surface of the diamond layer alcohol adhesive mixture containing a transition metal such as Fe, Ni or Co, and heat treatment of diamond in a stream of hydrogen at a temperature of not more than 1000°C, characterized in that for the preparation of alcohol adhesive mixture used powder water-soluble salt of the transition metal, which is in the form of 1-10 wt.% the aqueous solution is mixed with an alcoholic solution of glue with a ratio of aqueous solution of salt/alcohol solution of glue, equal to 1/1, put the mixture on the diamond layer thickness of 10-20 μm and dried, and heat treated diamond is carried out in two stages, the first stage of the diamond is treated at a temperature of 600-700°C for 1-2 min, and the second stage heat treatment is carried out at 800-1000°C for 15-30 minutes

 

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