Method of determining angle of misorientation of diamond crystallites in diamond composite |
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IPC classes for russian patent Method of determining angle of misorientation of diamond crystallites in diamond composite (RU 2522596):
    
Pcd diamond / 2522028
Invention relates to PCD diamond to be used in production of water-jet ejectors, engraving cutters for intaglio, scribers, diamond cutters and scribing rollers. PCD diamond is produced by conversion and sintering of carbon material of graphite-like laminar structure at superhigh pressure of up to 12-25 GPa and 1800-2600°C without addition of sintering additive of catalyst. Note here that sintered diamond grains that make this PCD diamond feature size over 50 nm and less than 2500 nm and purity of 99% or higher. Diamond features grain diameter D90 making (grain mean size plus grain mean size × 0.9) or less and hardness of 100 GPa or higher.
 Method for preparing nanodiamonds with methane pyrolysis in electric field / 2521581
Invention may be used in medicine in producing preparations for a postoperative supporting therapy. What is involved is the high-temperature decomposition of methane on silicone or nickel substrate under pressure of 10-30 tor and a temperature of 1050-1150°C. The heating is conducted by passing the electric current through a carbon foil, cloth, felt or a structural graphite plate whereon the substrates are arranged. An analogous plate whereon a displacement potential from an external source is sent is placed above the specified plate. Nanodiamonds of 4 nm to 10 nm in size are deposited on the substrates.
 Device to produce diamonds / 2514869
Invention relates to blast processes of the synthesis of materials, in particular, diamonds. Proposed device comprises flow vessel 1 with tight cover 3, mix of explosive arranged inside said vessel that features a high specific energy and graphite or carbon-bearing explosive with negative oxygen balance, initiator 5, indestructible cylindrical barrier 6 composed by pipe arranged aligned with vessel 1 there inside. Note here that said mix of graphite and explosive and initiator 5 are placed at barrier 6 centre.
 Method for selective final purification of nanodiamond / 2506095
Present invention refers to pharmacology, nanomaterials and nanotechnology, and concerns a method for selective final purification of nanodiamonds to remove foreign nitrate ions and sulphur compounds to be used in pharmaceutics; the method implies that charge-free nanodiamond powder is treated with alkaline water of the concentration of 0.01-1 mole/l at 20-100°C; the prepared suspension is then decanted and centrifuged; the precipitation is washed with water using ultrasound, separated and dried.
 Method of diamond selective grinding / 2492138
Invention relates to diamond grinding in making diamond rock cutting tool. Proposed method comprises processing the diamonds in velocity layer of magnetic fields together with ferromagnetic particles. Mix composed of ferromagnetic particles and diamond grains fills the cylindrical case by 0.25-0.35 of its volume. Diamond magnetic susceptibility is defined by the relationship:
Method of producing superhard composite material / 2491987
Invention relates to production of carbon-based superhard composite to be used for making tools for mining, stone-working and metal working. Proposed method comprises applying high pressure and temperature to initial carbon component, a diamond, and binder. Note here that said carbon component comprises additionally fullerene and/or nanodiamond while said binder represents one or several components selected from the family including silicon bronze alloy, Monel metal, solid alloy. Superhard material is produced in two steps. At first step, the mix of initial components is subjected to dynamic pressure of 10-50 GPa at 900-2000°C. At second step, obtained material is placed in high-pressure vessel and subjected to static pressure of 5-15 GPa and heated to 700-1700°C for at least 20 seconds.
Method of producing diamonds with semiconductor properties / 2484189
Method involves decomposition of solid carbonyl compounds of platinum metals in a gaseous medium at high temperature in a sealed container to form diamonds and doping said diamonds with boron at temperature of 150°C-500°C for 2-5 hours in a gaseous medium which contains carbon monoxide CO and diborane B2H6 with weight ratio of boron to carbon in the gaseous mixture of 1:100-1000.
 Method of producing synthetic diamonds and apparatus for realising said method / 2484016
Invention relates to chemical and jewellery industry. Diamonds are synthesised in a high-frequency induction crucible furnace with frequency range of 60-100 kHz. A ceramic crucible 1 is fitted with a ceramic grid 2 with holes with diameter of 0.3-0.5 mm, lying at a height of 20 mm from its bottom, and a ceramic pipe 3 with inner diameter of 15-20 mm for feeding a mixture of methane and carbon dioxide with specific volume rate of 60-70 h-1. Sodium carbonate and potassium carbonate are fed into the crucible 1, said carbonates being mixed in equimolecular ratio and heat treated at 400-450°C for 2 hours. Diamond synthesis is carried out in one day at temperature of 700-900°C in a melt of said salts in the presence of a catalyst - powdered iron with granule size of 3-5 mm in amount of 5-10% of the molten mass. Gas supply is cut at the end of the process. The molten salts, along with the catalyst and diamonds, are poured into moulds. The cooled down ingots are fed into a reactor - crystalliser 5. After dissolving the sodium carbonate and potassium carbonate, the suspension of catalyst and diamonds is fed onto a filter 6.The obtained filtrate is used in the reactor-crystalliser 5, and the diamond crystals are separated from the catalyst by a magnet.
 Method of producing carbon-containing nanoparticles / 2484014
Invention can be used in plasma chemistry and pharmacology. A vapour-liquid plasmatron is used to form a plasma jet from alcohol or aqueous solution thereof. The plasma jet is fed into a volume of water by dipping the nozzle of the plasmatron 10-20 mm into the water perpendicular to the water surface.
 Method for industrial production of diamonds and other solid-phase nanostructured graphite formations, apparatus and charge for production thereof / 2483023
Invention relates to detonation synthesis of nanostructured graphite formations, particularly diamonds, for use in chemical and electrochemical industry, in pharmacology, for conducting biomedical researches, for producing growth catalysts, diamond and diamond-like films, as a base for optical gates - laser radiation intensity limiters, as additives for rocket fuel, lubricant material, nano-modifier for concrete, antifriction additive for structural materials and lubricants, cold cathode element, nonlinear optical system element, including wide-band laser radiation limiters. The method for industrial production of diamonds and other solid-phase nanostructured graphite formations by blowing an explosive charge in an ice cover, said charge having oxygen deficiency and a shape elongated along the axis, composed of two or more cylindrical elements obtained by cold moulding from hexogene and fine trinitrotoluene, in a sealed explosion chamber in a medium which is inert towards condensed detonation products, with subsequent cleaning thereof, wherein a preliminary trigger discharge is formed by blowing an additional detonator. The apparatus for realising said method further comprises an electric detonator placed in a cut on the additional detonator.
 Method of modifying envelopes of polyelectrolyte capsules with magnetite nanoparticles / 2522204
Invention relates to a method of modifying envelopes of polyelectrolyte capsules with magnetite nanoparticles. The disclosed method involves producing a container matrix in form of porous calcium carbonate microparticles, forming envelopes of polyelectrolyte capsules by successive adsorption of polyallyl amine and polystyrene sulphonate and modifying with magnetite nanoparticles on the surface of the container matrix or after dissolving the matrix through synthesis of magnetite nanoparticles via chemical condensation.
 Method of producing nanostructured metal oxide coatings / 2521643
Method comprises preparing an alcohol solution of β-diketonates of one or more p-, d- or f-metals with concentration 0.001h2 mol/l; heating the solution to 368-523 K and holding at said temperature for 10-360 minutes to form a metal alkoxo-β-diketonate solution; depositing the obtained solution in droplets at the centre of a substrate being rotated at a rate of 100-16000 rpm, or immersing the substrate into said solution at a rate of 0.1-1000 mm/min at an angle of 0-60° to the vertical; holding the substrate with a film of the alkoxo-β-diketonate solution at 77-523 K until mass loss ceases, to form xerogel on the surface of the substrate; crystallising oxide from the xerogel at 573-1773 K.
Method for preparing nanodiamonds with methane pyrolysis in electric field / 2521581
Invention may be used in medicine in producing preparations for a postoperative supporting therapy. What is involved is the high-temperature decomposition of methane on silicone or nickel substrate under pressure of 10-30 tor and a temperature of 1050-1150°C. The heating is conducted by passing the electric current through a carbon foil, cloth, felt or a structural graphite plate whereon the substrates are arranged. An analogous plate whereon a displacement potential from an external source is sent is placed above the specified plate. Nanodiamonds of 4 nm to 10 nm in size are deposited on the substrates.
 Agent with anti-stroke action, and method for preparing it / 2521404
Invention concerns an agent having an anti-stroke action and representing the amino acid glycine immobilised on the detonation-synthesised nanodiamond particles of 2-10 nm in size, and a method for preparing it.
Polymer nanocomposite with controlled anisotropy of carbon nanotubes and method of obtaining thereof / 2520435
Invention relates to the field of polymer materials science and can be used in aviation, aerospace, motor transport and electronic industries. Nanotubes are obtained by a method of pyrolytic gas-phase precipitation in a magnetic field from carbon-containing gases with application of metals-catalysts in the form of a nanodisperse ferromagnetic powder, with the nanotubes being attached with their butt ends to ferromagnetic nanoparticles of metals-catalysts. Magnetic separation of the powder particles with grown on them nanotubes, used in obtaining a polymer-based composite material, is carried out. After filling with a polymer, a constant magnetic field is applied until solidification of the polymer takes place. The material contains carbon nanofibres and/or a gas-absorbing sorbent, for instance, silica gel, and/or siliporite, and/or polysorb as a filling agent.
 Test object for calibrating microscopes in micrometer and nanometer ranges / 2519826
Test object for calibrating microscopes is in form of groove structures whose walls have an inclined profile, a flat base and a different width on the surface and at the bottom. A constant angle between the side wall and the bottom plane is maintained for all elements. Linear dimensions of at least part of the elements differ from each other by a certain number of times, and linear dimensions of the largest element can be measured with high accuracy on calibrated measuring equipment used when taking measurements.
 Antipsychotic agent and method for preparing it / 2519761
Invention concerns an antipsychotic agent representing the amino acid glycine immobilised on the detonation-synthesised nanodiamond particles of 2-10 nm in size, and a method for preparing it.
 Antioxidant and method for preparing it / 2519760
Invention concerns an antioxidant representing the amino acid glycine immobilised on the detonation-synthesised nanodiamond particles of 2-10 nm in size.
 Antidepressant drug and method for preparing it / 2519759
Invention concerns an antidepressant drug representing the amino acid glycine immobilised on the detonation-synthesised nanodiamond particles of 2-10 nm in size, and a method for preparing it.
 Anxiolytic and method for preparing it / 2519755
Invention concerns an anxiolytic representing the amino acid glycine immobilised on the detonation-synthesised nanodiamond particles of 2-10 nm in size, and a method for preparing it.
 Nanoliposome with application of etherificated lecitin and method of obtaining such, as well as composition for prevention or treatment of skin diseases including such liposomes / 2418575
Invention relates to medicine and deals with nanoliposome which includes liposomal membrane, contains ethgerificated lecitin and one or more physiologically active ingredients, incorporated in the internal space of liposomal membrane, method of obtaining such, as well as composition for prevention or treatment of skin diseases, containing nanoliposome.
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FIELD: chemistry. SUBSTANCE: invention can be used in the field of elaboration of diamond-based materials for magnetic therapy, quantum optics and medicine. A method of determining an angle of misorientation of diamond crystallites in a diamond composite includes placement of the diamond composite into a resonator of an electronic paramagnetic resonance (EPR) spectrometer, measurement of EPR spectrums of nitrogen-vacancy NV-defect in the diamond composite with different orientations of the diamond composite relative to the external magnetic field, comparison of the obtained dependences of EPR lines with the calculated positions of EPR lines of NV-defect in the diamond monocrystal in the magnetic field, determined by the calculation. After that, the angle of misorientation of the diamond crystallites is determined by an increase of width of EPR line in the diamond composite in comparison with the width of EPR line in the diamond monocrystal. EFFECT: invention ensures higher accuracy of measurements. 3 cl, 6 dwg
The invention relates to nanotechnology and can be used in the development of materials based on diamond for magnetometry, quantum optics, Biomedicine, as well as in information technology, based on the quantum properties of spins and single photons. Various physical effects on polycrystalline system can lead to the formation of composite materials (composites), the microstructure consists of crystal grains that are not random, and some preferred orientation (see .J.Bunge, Texture Analysis in Materials Science: Mathematical Methods, translated by P.R.Morris (Butterworths, London, 1982). Such systems are characterized by the presence of preferred orientation, commonly referred to in the literature as "texture" (texture). Electronic properties of polycrystalline semiconductor materials greatly depend on the structural quality of these materials. Thus, studies of perfection (or imperfection) texture of the material are of great practical importance. The effects of texturing materials traditionally measured optical and diffraction methods. Diffraction methods based on the use of the diffraction of x-rays, neutrons, electrons, is also used probe microscopy. Application of the method of determining the angle risorante the gain of micro - and nanocrystals in the composite, based on the technique of electron paramagnetic resonance (EPR) (see L.A.Boatner, J.L.Boldu, and M.Abraham, Journal of the American Ceramic Society (J. Am. Ceram. Soc.) 73, 2333 (1990); G.Hendorfer, W.Jantsch, W.Helzel, J.H.Li, Z.Wilamowski, T.Widmer, D.Schikora, and K.Lischka, Mater. Sci. Forum 196-201, 561 (1995); T.A.Kennedy, E.R.Glaser, P.B.Klein, and R.N.Bhargava, Symmetry and electronic structure of the Mn impurity in ZnS nanocrystals, Phys. Rev. 52, 14356 (1995)), has proved to be extremely effective technique, because EPR is sensitive to the microscopic symmetry of the local structure near the paramagnetic center. The method is based on the EPR method has several advantages compared to traditional x-ray texture analysis. In particular, when using the technique of EPR degree of orientation of a system register in the entire volume, while x-ray analysis allows to obtain information about the angle of RetryInterval material only in the surface layer of several microns. Method of EPR is completely non-destructive and does not depend on the shape and size of samples. In the present invention as an object of study, we have considered the composite diamond, but EPR method is applicable to other materials. Diamond patterns are a promising material for applications in various electronic devices. However, the successful application of these materials requires the optimization of their structural and electronic properties. Optical technique for definition wide-angle the texture of polycrystalline diamond can be easily applied, but obtaining only semi-quantitative results. This technique is sensitive only to the surface and is not suitable for samples of arbitrary shape, especially for composites in the form of sintered under high pressure and high temperature micro - and nanodiamonds. A known method for determining the angle of RetryInterval polycrystalline materials by recording the EPR spectra of transition elements, specially introduced in the materials that examine the effects of texturing (see L.A.Boatner, J.L.Boldu, and M.Abraham, J.Am. Ceram. Soc. 73, 2333, 1990). In a known way in the polycrystalline material is injected ions of transition elements such as Mn, Cr, Fe EPR spectra which, due to the presence of fine structure, resulting in anisotropy of the EPR spectrum provide information about the angle of RetryInterval material. Then record the EPR spectra of these ions, which are compared with the spectra of EPR, calculated from the spin Hamiltonian for the corresponding single-crystal material (i.e., for fully oriented system). Next, determine the increase of the ESR line width in polycrystalline material in comparison with the width of the ESR line in the single-crystal material, and the amount of increase of the ESR line width calculated angle RetryInterval material. The disadvantage of this method is it is Timoti the introduction of additional impurities certain transition elements, having a sharply anisotropic EPR spectra that are almost impossible to implement in the material studied on the basis of the diamonds. There is a method of determining the position of an impurity in the nanocrystal, which is a structure in the form of a crystalline semiconductor fundamentals "SOG" and the crystalline semiconductor shell - shell (e.g., CdS/ZnSe core/shell nanocrystal) through registration of the EPR spectrum of manganese ions MP2+(see application US 20100055462, IPC WV 1/00; VV 3/00, published 04.03.2010), by determining the splitting of the hyperfine structure for ions MP2+in six lines (sextet) and comparing this decomposition with the value observed in the bulk crystal, the source of the core material and shell. The position of the ion MP2+within the framework or shell is determined by changing the width of the individual lines of the sextet. This fine structure in the EPR spectrum of the ion MP2+can provide information about the angle of RetryInterval of nanocrystals. The disadvantage of this method is the low value of the hyperfine splitting patterns MP2+in view of the weak dependence of this quantity from the position of the manganese in the nanocrystal, the large width of the individual lines of hyperfine sextet near the interface or in the shell. The isotropic hyperfine interaction is not possible to determine the extent of the Orient is rovannost system according to this feature, and fine structure, which is usually the most informative for determining the degree of orientation of a system, almost not visible in the EPR spectra due to line broadening caused by the effects of stress in the nanostructure. A known method for determining the angle of RetryInterval of diamond crystallites in the composite diamond in the form of polycrystalline diamond films (.F..Graeff, ..Nebel, .Stutzmann, A.Floeter and R.Zachai, Characterization of textured polycrystalline diamond by electron spin resonance spectroscopy, J. Appl. Phys. 81 (1), 234-237, 1997), which coincides with this decision on the greatest number of significant features and adopted for the prototype. In the method prototype is placed composite diamond in the form of a polycrystalline diamond film in the resonator spectrometer electron paramagnetic resonance (EPR)log EPR spectrum of N0-defects in composite diamond at different orientations of the composite diamond relative to the external magnetic field, the comparison of the obtained dependencies of the EPR lines with the calculated positions of the EPR lines N0-defect in the diamond single crystal in a magnetic field, determined from the relation: In=In0±[(A||2Cos2θ+A⊥2Sin2θ]1/2, where0=hf/geβethe magnetic field that specifies the center of gravity of the EPR spectrum, T; h=6,62606896·10-34is the Planck constant, j·s; f - frequency is of an EPR spectrometer, Hz; ge=2,0024 is a dimensionless quantity called the g-factor and characterizing the gyromagnetic ratio for the electron magnetic moment N0-defect; βe=9,2740·10-24- magneton Boron, j/T; A||=4,093·10-3- constant of the hyperfine interaction with the nucleus of nitrogen14N to N0-defect in the direction of the magnetic field parallel to the axis of symmetry of the defect, T; A⊥=2,920·10-3- constant of the hyperfine interaction with the nucleus of nitrogen14N to N0-defect in the direction of the magnetic field perpendicular to the axis of symmetry of the defect, T; θ is the angle between the direction of the external magnetic field and the axis <111> crystal diamond, which is oriented along the considered N0-the defect degrees; determine the increase of the ESR line width in the composite diamond compared to the width of the ESR line in single crystal diamond, and to increase the ESR line width calculated angle RetryInterval of diamond crystallites in the composite diamond. The prototype method is based on the use of electron paramagnetic resonance (EPR) to register the angle of RetryInterval of diamond crystallites in the composite diamond in the form of polycrystalline diamond films. From studies of natural and synthetic diamond is known that nitrogen is the dominant impurity in the diamond, when the nd in the crystal in many forms: from isolated atoms, replacement carbon to polyatomic units. Nitrogen in the form of atom replacing a carbon, is a deep donor level located below the conduction band at a depth of 1.7 eV and is characterized by a well identified by the EPR-signal, known as the P1 center. In the prototype as a measuring defect using P1 centre, which will be further denoted as N0-the defect. The EPR signal of N0-defects in the diamond represents the Central line and two satellites due to the hyperfine interaction of the unpaired electron with spin S=1/2 with the nucleus of nitrogen14N, with nuclear spin I=1. The unpaired electron can be in one of four C-N linkages and, therefore, the axis of symmetry of the center for the hyperfine interaction with the nucleus14N also parallel to one of four <111> directions in the crystal. Misorientation of the crystallites leads to broadening of the satellite lines, this broadening is used to quantify the angle of RetryInterval the crystal structure of the diamond film. Using the anisotropy of the provisions of the EPR lines N0-defect from the orientation of the individual crystallites of diamond. It should be emphasized that the range of the EPR textured material (partially oriented diamond crystallites) represents an intermediate with the standing between the two extremes in the form of a single crystal with one hand and fully averaged over the orientations of the system micro - or nanocrystals on the other. The shape of the broadened line of satellites allows to obtain the distribution function of orientation (FROH) of the crystallites forming the film. The disadvantage of this method is the weak anisotropy of the EPR spectra of N0-defects, insufficient accuracy of orientation determination, and the impossibility of optical detection of EPR spectra of these defects. The present invention is to provide such a method for determining the angle of RetryInterval of diamond crystallites in the composite diamond, which would ensure a higher accuracy of measurements, and the possibility of optical detection of magnetic resonance (ODMR), which increases the sensitivity of the measurements by more than five orders of magnitude. The problem is solved in that a method for determining the angle of RetryInterval of diamond crystallites in the composite diamond includes a composite diamond in the resonator spectrometer electron paramagnetic resonance (EPR), the measurement of the ESR spectra of nitrogen-vacancy (NV)defect in composite diamond at different orientations of the composite diamond relative to the external magnetic field, the comparison of the obtained dependencies of the EPR lines with the calculated positions of the EPR lines NV-defect in diamond single crystal in a magnetic field, determined from the relation: In=B0±1/2D(3Cos2θ-1), where0=hf/geβe- the magnetic field, determining the center of gravity of the EPR spectrum, T;h=6,62606896·10-34is the Planck constant, j·c; f - frequency EPR spectrometer, Hz; ge=2,0024 is a dimensionless quantity called the g-factor and characterizing the gyromagnetic ratio for the electron magnetic moment of the NV-defect in diamond. Ine=9,274010-24- magneton Boron, j/T; D=0.104 g - splitting of the fine structure for the NV defect in diamond, T; Θ is the angle between the magnetic field and the axis <111> crystal diamond, C; determination of the increase of the ESR line width in the composite diamond compared to the width of the ESR line in the diamond single crystal and the angle definition RetryInterval of diamond crystallites in the composite diamond to increase the ESR line width. Measurement of ESR spectra of NV-defect can be carried out by the method of optical detection of magnetic resonance (ODMR) NV-defects. The excitation of the n-V defects in diamond can be carried out using confocal optics. NV-defects, selected in this way as a measuring defects represent a vacancy carbon (V), in the nearest coordination sphere which one of the four carbon atoms are replaced by nitrogen atom (N). After opening a unique emitting properties of the NV-defect in Alma is e, allowing optical record magnetic resonance in the ground state NV-defects at room temperature and higher (up to 300°C) until the reception of the magnetic resonance on single defect (see A.Gruber, A.Drabenstedt, .Tietz, L.Fleury, J.Wrachtrup, .Von Borczyskowski, Scanning Confocal Optical Microscopy and Magnetic Resonance on Single Defect Centers, Science 1997, 276, 2012-2014; J.Wrachtrup, F.Jelezko, Processing quantum information in diamond, J.Phys.: Condens. Matter 18, S807, 2006), the opportunity absolute miniaturization of the element base of micro - and optoelectronics until the device based on a single defect. This opens up possibilities for application NV-defects in such promising areas as magnetometry, quantum optics, Biomedicine, as well as for the development of new information technologies, based on the quantum properties of spins and single photons. The use of confocal optics for excitation and measurement NV-defects in submicron volume of the material allows to determine the mutual orientation of the nanocrystals in optically excited small volume of material. When using this method the accuracy of determining the relative orientation of the crystallites of diamond increased by more than two orders of magnitude compared with the method of the prototype. The possibility of optical detection of magnetic resonance NV-defects, which cannot be implemented using the meter the CSO N 0-defect prototype, increases the sensitivity of the method when registering measuring NV-defects not less than five orders of magnitude, as recorded high-energy optical quantum, but not low-energy microwave quantum. The claimed technical solution is illustrated by drawings, where: figure 1 shows the calculated orientation dependence of the provisions of the EPR lines NV-defects and N0-defects. (Right orientational dependence is presented in enlarged 20 times the scale magnetic fields. The value of DV/D0 refers to the average value of the change in the magnetic field near the orientation of 45° when the orientation changes by one degree in units of Tesla. For NV-defects Δ/Δθ=2,68 MT/C, for N0-defects Δ/Δθ=0.02 MT/degree); figure 2 presents the experimental EPR spectra NV-defects (dyskobolia part) and N0-defects recorded at room temperature at a frequency of 94 GHz: (1) in the sintered composite BOTTOM size of about 10 μm, as shown in the figure, the orientation of the magnetic field close to the direction of one axis <111> oriented array of the composite; (2, 3) in a single synthetic microcrystal diamond the size of about 100 μm for the two orientations of the magnetic field relative to the crystal axes; figure 3 shows the comparison of line widths of EPR NV-defects, ZAR is registered in the sintered composite BOTTOM and single synthetic microcrystal diamond. (Marks indicated two satellites due to hyperfine interaction with the carbon nucleus13With specifying the absolute magnitude of the magnetic field, since the parameters of the hyperfine interaction with the carbon nucleus13With tabulated. The half width of the lines indicated by arrows); figure 4 presents the reference orientation dependence of the provisions of the line ODMR in a magnetic field for measuring n-V defects in diamond, calculated for two selected microwave frequency of 2.7 GHz and 3.0 GHz, which is smaller and more frequency splitting of the fine structure of the spin sublevels NV-defect equal 2,87 GHz (Value Δ/Δθ refers to the average value of the change in the magnetic field while changing the orientation of the crystal relative to the magnetic field of one degree in units of T/C); figure 5 shows the reference orientation dependence of the provisions of the lines ODMR in a magnetic field for measuring n-V defects in diamond monocrystal having four equivalent orientations in the crystal axis <111>, calculated for the selected microwave frequency 3.0 GHz, which is more than the frequency splitting of the fine structure of the spin sublevels NV-defect equal 2,87 GHz; figure 6 shows the experimental spectra ODMR NV-defects, registered at room temperature for two frequencies (greater than and less than the frequency 2,87 G is C) in a single synthetic microcrystal diamond the size of about 100 μm for the same orientation of the magnetic field relative to the crystal axes (Dotted line ODMR, registered in the sintered composite BOTTOM size of about 10 μm, the image of which is shown in figure 2). The present method for determining the angle of RetryInterval of diamond crystallites in the composite diamond is as follows. Place the composite diamond in the resonator spectrometer electron paramagnetic resonance (EPR) and measured EPR spectra of nitrogen-vacancy (NV) defect in composite diamond at different orientations of the composite diamond relative to the external magnetic field, as shown in figure 2, and the position of these lines is surely connected with the orientation of this NV-defect, that is, from a certain angle θ. Calculate the orientational dependence of the provisions of the EPR lines NV-defects in the diamond single crystal, proceeding from the known parameters of the spin Hamiltonian, which are used as calibration curves, as shown in the right part of figure 1. The position of the lines NV-defects in the magnetic field is determined from the relation: In=B0±1/2D(3Cos2θ-1), where0=hf/geβe- the magnetic field, determining the center of gravity of the EPR spectrum, T; h=6,b·10-34is the Planck constant, j·s; f - frequency EPR spectrometer, Hz; geis a dimensionless quantity called the g-factor and characterizing the gyromagnetic ratio for the electron is inanaga moment; β=9,2740·10-24- magneton Boron, j/T; D=0.104 g - splitting of the fine structure for the NV defect in diamond, T; θ is the angle between the magnetic field and the axis <111> crystal diamond, degrees. Value Δ/Δθ refers to the average amplitude changes of the magnetic field near the orientation of 45° when the orientation changes by one degree in units of Tesla. For NV-defects average value calculated from the deflection angle θ of 45° ±5°, Δ/Δθ=2,68 MT/degree. This value, as can be seen from the right part of figure 1 by more than two orders of magnitude greater than Δ/Δθ=0.02 MT/C for N0-defects, also calculated from the deflection angle θ of 45° ±5°. The width of the individual lines, the obtained EPR spectra, are compared with the corresponding widths of the lines known reference EPR spectra of n-V defects in diamond single crystal, is shown for two arbitrary orientation in the lower part of figure 2. Then determine the angle of RetryInterval of diamond crystallites in the composite diamond to increase the ESR line width NV-defects in the composite compared to the width of the ESR line NV-defects in the reference sample of single crystal diamond. In the preliminary analysis of the line width is simply divided into Δ/Δθ=2,68 MT/C, and the result is the angle RetryInterval crystallites in degrees. If a more accurate determination of the angle of RetryInterval is required each lnii NV defects in figure 2 to compare the angle θ between the axis of the NV defect and the external magnetic field, and then, according to figure 1 to determine the parameter Δ/Δθ for a given angle θ. The inventive method is illustrated on the example of determination of the angle of RetryInterval crystallites in the composite, manufactured by sintering detrazioni nanodiamonds (BOTTOM). The production of the diamond structure with NV-defects includes sintering the treated BOTTOM with the size of the diamond grains 4-5 nm in the high pressure chamber at a pressure of 5-7 GPA and a temperature of 750 to 1000°C in a period of time from several seconds to several minutes. Then made a selection from a powder of diamond aggregates with sizes in the field of 1-15 μm with quasicrystalline properties with a high concentration of NV-defects characterized by a bright luminescence in the red region when excited with their laser with a wavelength of 532 nm. The result is a composite in the form of a diamond structure with a high concentration of NV-defects and N0-defects. The resulting composite is placed in the cavity of an EPR spectrometer selected range. In this example, we used high-frequency spectrometer, operating at a frequency of 94 GHz, increased sensitivity which allows the use of a single composite sample of micron size. The image of this sample is shown in figure 2. Recorded EPR spectrum for an arbitrary orientation of the composite magnetic field. In this example, PU is eating the rotation of the sample was achieved orientation, when observed maximum cleavage between the extreme lines in the spectrum, this corresponds to the minimum magnetic field to the extreme line of the spectrum presented in figure 2. The establishment of a special orientation is not mandatory in this way, as the position of the EPR lines NV-defects always possible to accurately determine the angle θ for this NV-defect. In the EPR spectrum in figure 2 show several lines EPR belonging NV-defects that correspond to different angles of the magnetic field relative to the axis of the NV-defect. Then choose one line in the EPR spectrum of the composite and its width compared to the width of the ESR line NV-defects observed in the reference sample in the form of a diamond single crystal, as shown in figure 3. The line width in the composite to the magnitude of the AB/L for a given angle θ gives the angle of RetryInterval crystallites in the composite. If you take the average Δ/Δθ=2,68 MT/degree for orientation of about 45 degrees to get the angle RetryInterval crystallites in the composite is about 0.5 degrees. Unlike the prototype method, in this method EPR spectra NV-defects can be detected optically. Thus the sensitivity of detection of EPR spectra is increased by several orders of magnitude (at least five orders of magnitude). The present method for determining the angle RetryInterval the ti nanocrystals in the composite of micro - diamond nanocrystals with optical detection of EPR spectra is as follows. The sample is placed in a resonator system of the spectrometer is a low-frequency range, which represents a coil of wire. In turn serves the microwave with a given frequency and relieve spectra ODMR change characteristic luminescence of NV-defects in the red region when excited by a green laser (e.g., 532 nm) at the time of magnetic resonance, the terms of which are created by the sweep of an external magnetic field on the sample. Calculate the orientational dependence of the provisions of the EPR lines NV-defects in single crystal diamond, registered at microwave frequencies, slightly smaller or slightly larger frequency splitting of the fine structure of the spin sublevels NV-defects equal 2,87 GHz on known parameters of the spin Hamiltonian and is determined by the average Δ/Δθ. Then the width of the ESR line NV-defects obtained in the composite, compared to the width of the ESR line obtained in reference single crystal diamond. Then calculate the angle of RetryInterval crystallites of the composite to increase the line width ODMR NV-defects in the composite compared to the line width ODMR NV-defects in the reference sample of single crystal diamond. Figure 4 presents the reference orientation dependence of the provisions of the line ODMR in a magnetic field for measuring n-V defects in diamond, calculated for two selected microwave frequency of 2.7 GHz and 3.0 G is C, less and more the frequency splitting of the fine structure of the spin sublevels NV-defect equal 2,87 GHz. The value of DV/D0 refers to the average value of the change in the magnetic field while changing the orientation of the crystal relative to the magnetic field of one degree in units of T/C. Figure 5, in addition to figure 4, shows the reference orientation dependence of the provisions of the lines ODMR in a magnetic field for measuring n-V defects in diamond monocrystal having four equivalent orientations in the crystal axis <111>, calculated for the selected microwave frequency 3.0 GHz, which is more than the frequency splitting of the fine structure of the spin sublevels NV-defect equal 2,87 GHz. You can see that there are multiple lines EPR NV-defects, which indicates the execution of the resonance conditions for multiple NV-defects, characterized by different orientations in a magnetic field. Figure 6 as an example, the experimental spectra ODMR NV-defects, registered at room temperature for two frequencies greater than and less than the frequency 2,87 GHz in a single synthetic microcrystal diamond the size of about 100 μm for the same orientation of the magnetic field relative to the crystal axes. The dotted line ODMR registered in the sintered composite BOTTOM size of about 10 micrometers, the image of which is shown in figure 2. The line width in the composite to the magnitude of the Δ/Δθ calculated for a given angle θ uniquely determined from Petrov ODMR, gives the angle of RetryInterval crystallites in the composite. Angle RetryInterval crystallites in the composite is about 0.5 degrees, which is in good agreement with the results obtained using the standard method of EPR. The use of confocal optics for excitation and measurement NV-defects in submicron volume of material, allows to determine the mutual orientation of the nanocrystals in optically excited small volume of material, which is impossible without ODMR. 1. The method for determining the angle of RetryInterval of diamond crystallites in the composite diamond, including the location of the composite diamond in the resonator spectrometer electron paramagnetic resonance (EPR), the measurement of the ESR spectra of nitrogen-vacancy NV-defect in composite diamond at different orientations of the composite diamond relative to the external magnetic field, the comparison of the obtained dependencies of the EPR lines with the calculated positions of the EPR lines NV-defect in diamond single crystal in a magnetic field, determined from the relation: 2. The method according to claim 1, characterized in that the measurement of EPR spectra of NV-defect carried out by the method of optical detection of magnetic resonance NV-defects. 3. The method according to claim 2, characterized in that the excitation of the NV-defect diamond carried out using confocal optics.
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