Method of producing fluoride nanoceramic

IPC classes for russian patent Method of producing fluoride nanoceramic (RU 2436877):

C30B33/02 - Heat treatment (C30B0033040000, C30B0033060000 take precedence);;

C30B28/02 - directly from the solid state

C04B35/622 -

C04B35/553 -

B82B3 - Manufacture or treatment of nano-structures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units

Another patents in same IPC classes:

Polycrystalline laser material / 2431910

Polycrystalline laser material is a microstructured substance with grain size from 3 mcm and consists of calcium and ytterbium fluorides. The material is a solid solution of calcium fluoride and ytterbium fluoride. Content of ytterbium fluoride is less than 5 mol %. The base of the structure of the material is composed of layered grains in which layer thickness ranges from 30 to 100 nm, and the size of separate grains ranges from 30 to 150 mcm.

Laser gain medium and laser generator (versions) using said medium / 2427061

Laser medium includes an optical medium which can transmit a laser beam and having an input surface, a first surface and a second surface opposite the first surface. At least one of the gain media is connected to the first surface of the optical medium and at least one of the gain media is connected to the second surface. The gain media are pumped by an optical pumping beam and amplify the laser beam during its successive reflection. The gain media are made from the same optical material and are doped with at least one active element. The amount of the doping active element in the gain media and/or thickness of the gain media in the direction perpendicular to the first or second surfaces is chosen such that the amount of heat released during absorption of the optical pumping beam is the same for the said gain media.

Laser material / 2395883

Proposed laser material features garnet structure R₃T₅O₁₂, where R is ions selected from the group Y, La, Ce, Gd, Sc, Lu; T is ions selected from the group Al, Ga, Sc, Lu. Laser material comprises ion of trivalent hafnium as activator. Activator concentration varies from 0.05 to 5 % by weight in terms of hafnium dioxide in excess of garnet stoichiometric formula. Said laser material can represent an optical ceramic, monocrystal or monocrystalline film.

Laser material / 2391754

Laser material has a garnet structure R₃T₅O₁₂. R denotes ions selected from Y, La, Ce, Gd, Sc, Lu. T denotes ions selected from Al, Ga, Sc, Lu. The laser material contains active ions of trivalent neodymium and a sensitising agent. The sensitising agent used is at least one ion selected from a group of trivalent ions of titanium, zirconium and hafnium.

Laser material / 2369670

Invention relates to electronic engineering material and can be used in making new devices in photonics, quantum electronics and ultraviolet optics. The laser material, based on barium and yttrium fluoride crystal, activated by trivalent ions of cerium BaY₂F₈:Ce³⁺, additionally contains ytterbium and lutetium ions in concentration of 0.5-5.0 at % and 1-5 at %, respectively.

Method of receiving of optical material for quantum electronics on basis of crystals of double fluorides / 2367731

Invention relates to crystal growth process and can be used at creation of activated crystalline materials with predicted properties for needs of photonics, quantum electronics and optics. Optical material on the basis of crystals of double fluorides of scheelite structure is received by means of crystal growth from melt of ingredients LiF, YF₃, LuF₃, LnF₃, where Ln - trivalent ions of cerium subgroup of lanthanide row, herewith into charge for preparation of melt it is introduced lutetia fluoride in amount from 50 mole % up to 90 mole % relative to yttrium fluoride.

Laser material / 2362844

Invention relates to materials for electric engineering; it can be used for creation of new devices in the area of photonics, quantum electronics and UF-band optics. Based on crystals of lithium and lutetium fluorides activated by trivalent cerium ions laser material contains additionally yttrium and ytterbium fluorides in compliance with chemical formula LiLu_1-xY_xYb_yF₄:Ce, where x=0.5÷0.8, y=0-0.05.

Quasi three-level solid laser and method of operation / 2360341

Invention relates to solid laser, namely to lasers with laser diode pumping. The invention can be applied in medicine and cosmetology in industrial scope. Quasi three-level solid laser includes laser diode, active element, laser diode radiation focusing device and laser resonator. The laser contains laser diode temperature sensor, current and laser diode temperature control unit having electrical connection with laser diode, thermal stabilisation unit and diode temperature sensor. The laser diode control unit is designed so that it can control various currents and laser diode temperatures. Method of quasi three-level solid laser operation provides for transmitting current via laser diode. The laser diode radiation is focused inside the above-mentioned active element placed between input and output mirrors. After that the radiation is reflected from the output surface of active element. Radiation from the active element is transmitted though input and output surfaces of the active element. In addition, the radiation falling on the output mirror of resonator is partially transmitted through it whereas radiation from laser diode reflected from the laser elements is simultaneously reduced during transients related to laser diode switching on or changing diode radiation power. The current flowing through laser diode is changed so that the length of laser diode radiation wave coincides with the centre of active element absorption line.

Ceramic laser microstructured material with twinned nanostructure and method of making it / 2358045

Proposed laser material is a ceramic polycrystalline microstructure substance with particle size of 3-100 mcm, containing a twinned nanostructure inside the particles with size of 50-300 nm, made from halides of alkali, alkali-earth and rare-earth metals or their solid solutions, with vacancy or impurity laser-active centres with concentration of 10¹⁵-10²¹ cm^-3. The method involves thermomechanical processing a monocrystal, made from halides of metals, and cooling. Thermomechanical processing is done until attaining 55-90% degree of deformation of the monocrystal at flow temperature of the chosen monocrystal, obtaining a ceramic polycrystalline microstructure substance, characterised by particle size of 3-100 mcm and containing a twinned nanostructure inside the particles with size of 50-300 nm.

Infrared potassium and rubidium pentobromplumbite crystal laser array / 2354762

There is disclosed infrared potassium and rubidium pentobromplumbite crystal laser array as described by formula K_XRb_1-XPb₂Br₅ where x changes within 0.2≤x≤0.5.

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 / 2411311

Method includes the first stage of increasing temperature of single-crystal substrate ZnTe up to the first temperature of thermal treatment T1 and maintenance of substrate temperature within specified time; and the second stage of gradual reduction of substrate temperature from the first temperature of thermal treatment T1 down to the second temperature of thermal treatment T2, lower than T1 with specified speed, in which T1 is established in the range of 700°C≤T1≤1250°C, T2 - in the range of T2≤T1-50, and the first and second stages are carried out in atmosphere of Zn, at the pressure of at least 1 kPa or more, at least 20 cycles or at least 108 hours.

Method of growing heat resistant monocrystals / 2404298

Crystals are grown using the Kyropoulos method with an optimum annealing mode, carried out while lowering temperature of the grown monocrystal to 1200°C at a rate of 10-15°C/hour and then cooling to room temperature at a rate of 60°C/hour.

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 / 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 m^1/2.

Ceramic laser microstructured material with twinned nanostructure and method of making it / 2358045

Method for thermal processing of semi-finished abrasive tools on organic thermosetting binding agents / 2351696

Invention is related to the field of abrasive processing and may be used in production of abrasive tools for polishing of blanks from different metals and alloys. Full cycle of thermal processing of semi-finished abrasive tools on organic thermosetting binding agents includes stages of preliminary heating and hardening in microwave field of SHF- chamber with frequency of 2450 MHz for abrasive tool with thickness of up to 100 mm and with frequency of 890 - 915 MHz for abrasive tool with thickness of more than 100 mm. Prior to SHF-thermal processing semi-finished abrasive tools are placed into radio transparent steam-and-gas permeable container-thermostat. After temperature of thermosetting binding agent complete polymerization has been achieved, and after pause at this temperature, thermostat is withdrawn from SHF-chamber, and semi-finished abrasive tools are kept in thermostat until their temperature drops at least by 80°C. After that thermostat is opened, semi-finished products are cooled in open air and then withdrawn from thermostat.

Method for thermal treatment of half-finished abrasive tools on organic thermosetting binders / 2349688

Group of half-finished abrasive tools prior to thermal treatment is placed into thermally insulated steam and gas permeable radiolucent thermostat. Full cycle of mentioned half-finished articles thermal treatment is carried out. Cycle includes stages of preliminary heating and hardening of half-finished items group in microwave field of SHF-chamber with frequency of 2,450 MHz for abrasive tools with thickness of up to 100 mm and frequency of 890...915 MHz for abrasive tools with thickness of more than 100 mm to achieve temperature of organic thermosetting binder complete polymerisation with further maintenance at this temperature. In process of SHF thermal treatment volatile substances are forcedly and uniformly removed from free volume of thermostat through slots arranged in front and back walls of thermostat. Possibility for vapours of volatile substances to be saturated is eliminated with preservation of maximum possible effect of thermostat working area thermal insulation effect and provision of half-finished items temperature difference that does not exceed ±10% of its average level inside thermostat.

Method of obtaining synthetic minerals / 2346887

Invention concerns obtaining synthetic minerals and can be applied in technics and jewellery. Method of artificial mineral synthesis is implemented by crucible method involving blend processing in plasma torch of plasmotron to obtain melt, melt drop feeding into crucible by plasma-forming gas flow with further crystallisation. Seeding agent is placed at crucible bottom in advance, and synthesis is performed at plasmotron output of 12 kW and blend feed rate of 2-3 g/min with simultaneous annealing of the melt crystallised on seeding agent in annular furnace for 2-3 hours at 1000°C. Preliminary placement of seeding agent to crucible bottom ensures accelerated crystal growth and higher process performance. Simultaneous annealing of artificial minerals reduces tension in end product significantly.

Inorganic scintillation material, crystalline scintillator and radiation detector / 2426694

Invention relates to novel inorganic scintillation materials, a novel crystalline scintillator, especially in form of a monocrystal, and can be used to detect ionising radiation in form of low-energy electromagnetic waves, gamma radiation, X-rays, cosmic rays and particles in fundamental physics, computerised tomography devices, PET tomographic scanners, new-generation tomographic scanners, gamma spectrometres, cargo scanners, well logging systems, radiation monitoring systems, etc. The halide-type scintillation material has the formula Ln_(1-m-n)Hf_nCe_mA_(3+n), where A is either Br, Cl or I or a mixture of at least two halogens from this group, Ln is an element selected from: La, Nd, Pm, Sm, Eu, Gd, Tb, Lu, Y; m is molar fraction of substitution of Ln with cerium, n is the molar fraction of substitution of Ln with hafnium, m and n is a number greater than 0 but less than 1, (m+n) is less than 1. The crystalline scintillator has formula Ln_(1-m-n)Ce_mA₃:n-Hf⁴⁺, where Ln_(1-m)Ce_mA₃ is the formula of the matrix of the material, A is Br, O or I or a mixture of at least two halogens from this group, Ln is an element selected from: La, Nd, Pm, Sm, Eu, Gd, Tb, Lu, Y; Hf⁴⁺ is a dopant, m is a number greater than 0 but less than or equal to 0.3, n is content of the Hf⁴⁺ dopant (mol %) which is preferably between 0.05 mol % and 1.5 mol %. The radiation detector has a scintillation element based on the novel inorganic scintillation material.

FIELD: physics.

SUBSTANCE: 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.

EFFECT: nanosize structure of the ceramic and improved optical, laser and generation characteristics.

3 cl, 3 ex

The invention relates to a technology for optical polycrystalline materials, namely, to a method for fluoride ceramics with nano-sized structure and improved optical, laser and laser characteristics.

Optical ceramics with improved compared to single crystals and glasses, mechanical and thermomechanical properties found its use as structural elements of optics, which during operation are subjected to mechanical loads, temperature changes and contact with atmospheric moisture. Uniform distribution of the various components in the composition of the ceramic gives you the ability to synthesize a variety of compounds, including a high content of laser ion that is unattainable for crystals. The most widely fluoride ceramics on the basis of fluorides of alkali, alkaline earth and rare earth metals.

Obtaining ceramics by hot recrystallization pressing powders of fluoride is not possible to synthesize a material with high transparency and optical homogeneity, and in the case of ceramics, assisted laser ions cannot reach the low threshold and high efficiency generation of laser radiation.

Poor transparency and optical homogeneity ceramics are the result of the atom in the presence of microscopic pores and voids, educated at the grain boundaries of the crystallites on the surface of which is localized various impurities (CO₂, OH^-H₂O).

To improve the optical characteristics of fluoride ceramics using such techniques as the heat treatment of the raw powder by gas-reducing agent or gas-fluorinating agent, using as raw material powders gidrohloridu alkali and alkaline earth metals, conducting secondary annealing the material in a gaseous atmosphere CF₄.

Famous U.S. patent No. 4089937 published 16.05.1978 index IPC C01F 11/22, C01F 17/00, C01F 5/28, SW 9/08 "hot-pressed fluoride ion optical ceramic materials without absorption bands and methods of their manufacture". On the mentioned patent get hot-pressed ceramics on the basis of fluorides of alkali, alkaline earth and rare earth elements, free from absorption bands belonging to the impurities CO₂N₂Oh, HE^-. Receiving material are as follows. The raw material powder is placed in a mold for hot pressing and set in the oven, raise the temperature to 400-600°C and passed within a few hours through a system of gas-reducing agent (H₂N₂N₂+H₂N₂+Not) or gaseous hydrogen fluoride (HF). When this noise is through the system, the gas interacts with the raw powder fluoride, removing from its surface impurities. After processing gas to provide hot pressing the powder at temperatures of 400-800°C and the pressure 70-300 MPa.

The above-described method are transparent optical ceramics for the entrance optics that are free from absorption bands of impurity bands HE^-N₂And CO₂in the range of 1-7 μm. The disadvantages of the invention include: low temperature process and the absence of vacuum in the system that does not allow to obtain dense samples of optical ceramics, free from pores with high transmittance in the working range of 0.2 to 7 microns.

In the method of obtaining laser fluoride ceramics according to the patent of Russian Federation №2321120 published 27.03.2008 IPC index H01S 3/16, as the source materials used powders fluoride and gidrohloridu alkali and alkaline earth metals and/or complex compounds of rare earth elements containing excess fluoride ion. Source powders are placed in the mold, which is established in the vacuum oven for pressing, oven create a vacuum of 1 PA (7.5·10^-3mm Hg), heat up and make the isothermal aging process, during which hydrohloride alkali and alkaline earth metals and/or complex compounds of rare earth elements disintegrate, forming the corresponding metal fluoride, hydrogen fluoride and fluoride and mania (decomposition of complex compounds). The latter two compounds are fluorinating agents, cleansing the source powders from oxydiesel. In this way it is also proposed the implementation of fluoridation powder throughout the process of hot pressing. To do this, before heating in a vacuum furnace with the raw material powder sleuth of tetraploid carbon and do not stop the flow of gas throughout the process of obtaining ceramics. Thus, to prevent contamination of the synthesized material impurities from the used tooling.

The processing efficiency of the active material of fluorine in the above method may not be high enough. When a source of active fluoride are used as starting powders, such as hydrohloride, the processing of the material in fluorinating environment is limited by the duration of isothermal soaking prior to extrusion. However, after decomposition hydrohloride at the stage subsequent hot pressing of the powder does not exclude the contamination of the compression of the material of unwanted impurities. In the case of processing of the compression of the powder gas CF₄the time of contact of the material with a fluorinating agent of the limited duration of the process of hot pressing, which may not be enough to remove from the material of all impurities.

Described you the e method allows to obtain samples of fluoride ceramics with small indicators absorption in the region of 1 μm. For example, the absorption of ceramics based on calcium fluoride activated with ytterbium, at a wavelength of 1.064 μm is equal to 0.003 cm^-1. However, this method of obtaining material provides high transparency fluoride ceramics in the UV, visible and IR region of the spectrum up to 1 micron.

Known invention "Ceramic laser microstructured material with twin nanostructure and method of its manufacture" (patent RF №2358045 published 27.02.2009 index IPC SW 28/00, 33/02, 29/12; H01S 3/16; VV 3/00). Here is a way to get laser ceramics on the basis of fluorides of alkali, alkaline earth and rare earth elements from the respective crystals, which consists in the following. The single crystal sample (fluoride of alkaline, alkaline earth or rare earth element or their solid solutions) is heated to temperatures from 2/3T_pl.to T_PLand above (depending on the specific case) and by uniaxial compression the sample to deform relative change in linear dimension of the crystal (degree of deformation) 55-90%. Deformation can occur either in vacuum (10^-2mm Hg) and a temperature below the melting temperature of the single crystal, or in the atmosphere gas of CF₄and a temperature above the melting point of the material. In the process of deformation of the original single crystal is not asaeda in the material with a polycrystalline structure and a grain size structure of the crystallites 3-100 μm, within the grains is twinned structure with a characteristic size of 50-300 nm.

This method allows you to get fluoride ceramics with improved compared with single crystals of mechanical characteristics and is capable of generating laser radiation. The microhardness of the synthesized material is higher by 10-15% compared with the corresponding single crystals, and fracture toughness above 2-6 times. The maximum generation efficiency was obtained for the ceramic samples obtained on the basis of LiF:F₂at the working wavelength 1.117 μm and amounted to a value of 26%.

The disadvantages of the considered method include the following. There is a low vacuum (10^-2mm Hg), which does not eliminate active impurities in the zone of the deformation of single crystal and makes it difficult to obtain polycrystalline material with high transparency and optical homogeneity. In these conditions, obtaining polycrystalline material with high transparency and optical homogeneity is impossible. The task of ensuring high optical quality of the environment can be solved by creating the conditions when there is a permanent removal of oxydiesel of the composition of the sample. This problem was solved only in the case when the sample was transferred into a liquid state. In subsequent inertial mode cooling was obtained odnorodny sample with a fissured structure. Low degree of deformation 50-90% does not allow to obtain a homogeneous finely structured ceramic material of optical quality. The higher the degree of deformation in this way is impossible due to the low purity of the working gas, which leads to disruption of the stoichiometric composition of the final product and unacceptably low level of optical quality.

The above method of obtaining fluoride ceramic material according to the patent of Russian Federation №2358045 is actually the closest to the proposed invention and is taken as a prototype of the proposed method.

The objective of our invention is to solve the problem of obtaining material of high optical quality for a wide class of compounds: fluoride ceramics on the basis of fluorides of alkali, alkaline earth and rare earth elements, characterized by the nanostructure and high optical, laser and laser characteristics.

The solution of this problem is due to the optimal selection of process parameters of the process of obtaining nanoceramics, which includes heat treatment of the product under conditions that allow to increase the purity of the environment and to achieve a high optical parameters of the laser material.

The objective of the invention is solved JV is a way to get fluoride nanoceramics, including thermomechanical processing of the original crystalline material made of metal halides, at a temperature of plastic deformation, obtaining polycrystalline microstructure of matter, characterized by a grain size of crystals of 3 to 100 μm and nanostructure inside the grains, which, unlike the prototype, thermomechanical processing of the original crystalline material is carried out at a vacuum of 10^-4mm Hg, reaching the degree of deformation of the original crystalline material from 150 to 1000%, resulting in a gain of polycrystalline nanostructured material, then hold his seal at a pressure in the range of 1-3 mV/cm²to achieve theoretical density, and then to remove the optically active impurities it is annealed in an active medium fluorinating gas.

As the source of crystalline material you can use fine powder that underwent heat treatment in a gaseous carbon tetrafluoride or without such treatment, if the source material has a specific degree of purity.

Another variation of the original crystalline material can be molded workpiece of a given size, obtained from a powder.

Source procurement may be a sintered billet milked spirtnogo powder, the last heat treatment in the atmosphere of carbon tetrafluoride.

As the source of crystalline material can be used crystalline form of the substance, including the single crystal of a given composition.

Heat treatment of the polycrystalline material is preferably carried out in an atmosphere of fluorinating gas, preferably carbon tetrafluoride, at a pressure of 800-1200 mm Hg However, there is another option of treatment with other fluorine-containing agents, such as other compounds of fluorine and carbon. Gaseous fluorinating agent may be the products of pyrolysis of PTFE-4, which occur in a vacuum at a temperature in excess of 400-600°C. Specific activity possesses gaseous sulfur hexafluoride or carbon tetrachloride is mixed with an inert carrier gas, as agent, active against hydrogeography and oxyconti basic substance.

To increase the purity and the forming of the source material being heat treated. The crystalline material of the desired composition is placed in a graphite form of a given size, which is established in the vacuum oven. In the furnace, vacuum is applied at the level of 10^-4mm Hg, after which filled with a gaseous CF₄to pressure 800-1200 mm Hg and maintained heating furnace to a temperature of 800-1400°C, depending on the composition of the mixture (without melting). What follows is an excerpt 10-30 hours, during which the active medium gaseous CF₄interacts with particles in the original sample, replacing the oxygen-containing impurities on fluoride. At the end of the exposure system is cooled to room temperature. After heat treatment under these conditions receive a molded sample in the form of a cylinder with dimensions suitable for receiving nanoceramics.

For the next stage of initial preparation of the crystalline material is placed in a mold and heat resistant metal alloy. Avoid interaction of the workpiece with a material form all its surface treated boron nitride, and the material in the mold is crimped at the top and bottom plates of the molybdenum foil and graphite gaskets. When this strip is placed so that the foil is in contact with the lower and upper ends of the workpiece. Then the mold is placed in a vacuum furnace for carrying out the process of deformation and compaction of the original sample. In the furnace, vacuum is applied at the level of 10^-4mm Hg and begin a slow heating to a temperature of 800-1400°C depending on the composition of the original product. After reaching the specified temperature level, doing isothermal exposure duration of 20-40 minutes. In this case, the billet remaining in the solid state, is able to deform, not adresas. Then using a hydraulic press exercise strain, slowly increasing the pressure to a value of 1-2 mV/cm². Pressure is applied to the upper end face of the workpiece so that when the strain was decreased its height. The ratio of the dimensions of the mold and preform are selected so that the relative change in height of the workpiece (degree of deformation) was higher than 150%. Once achieved, the pressure of 1-2 mV/cm²make Isobaric-isothermal exposure for 10-60 minutes to eliminate pores with sizes larger than the thickness of one layer of the grain, and make the material density close to theoretical. After exposure, the pressure is gradually reduced to 0 mV/cm²and slowly cooled in the furnace to a temperature of 25°C. the Rate of cooling and heating furnaces are chosen depending on the chemical composition of a deformable material and dimensions of the workpiece and must ensure the integrity of the workpiece and the absence of residual stresses. Throughout the process, maintain the vacuum level of 10^-4mm Hg, which allows to obtain the material in a clean environment.

The material acquires a unique nanocrystalline structure in the process of uniaxial deformation with a high degree of deformation over 90% and Isobaric-isothermal exposure on the Duma Deputy stage process for achieving maximum effort. Nanostructured material is constructed of tightly Packed grains up to 100 μm, which have a layered structure with the thickness of one layer of 30-100 nm. In addition to grains with a layered structure ceramics has pores, which are localized in the same layer and are a dead-end. The size of a single pore, located at the junction of the grains is substantially less than the thickness of one layer of grain. The presence of such pores causes light scattering in the VUV region of the spectrum that does not affect the generation characteristics of the material, but lead along with a layered nanostructure increase the operational stability of the working fluid device, mechanical properties, heat resistance, etc.

The choice of the degree of deformation of the workpiece more than 150%, because only under this condition the material acquires a characteristic layered structure of grains - nanostructure and receives necessary for use as a laser material properties: homogeneity of the composition and refractive index, high values of thermophysical and mechanical properties.

To achieve the highest possible optical characteristics of the ceramic workpiece is subjected to heat treatment in an atmosphere of gaseous carbon tetrafluoride, and for removing the resulting residual thermoelastic stress heat treatment is carried out in the mode of annealing when set to the higher speed of the heating and cooling of the material. Annealing in fluorinating environment carried out similarly to the above-described heat treatment of the source material. The difference is that the heating rate and cooling of the workpiece in this case are controlled by the parameters and the optimal value is 25°C per hour.

The result was obtained optical ceramics on the basis of fluorides of alkali, alkaline earth and rare earth elements having a new structure and with the best, in comparison with single crystals, mechanical and thermomechanical properties, with high transmittance in the range from 0.2 to 7 μm and an increased, in comparison with the prototype, the efficiency of generation of laser radiation (60%).

Specific examples of the method

Example No. 1. The fine powder of barium fluoride (BaF₂) annealed in fluorinating atmosphere at a temperature of 1300°C for 10 hours, the resulting sintered powder was placed in a mold and subjected to uniaxial deformation in vacuum 10^-4mm Hg at a temperature of 1150°C., applying a pressure of 2 mV/cm²within 30 minutes the Degree of deformation is 170%. Once achieved, the pressure value of 2 mV/cm²make Isobaric-isothermal exposure for 60 minutes.

Thus obtained ceramic material was further subjected to heat treatment in an atmosphere gas of CF₄at a temperature of 1300 the C for 20 hours. The result was obtained ceramic material, characterized by a tensile strength Flexural 3.5 kg/mm²that at least 30% higher than that of the single crystal, and temperature 30°C, which is 1.5 times higher in comparison with the single crystal of the same composition, for any crystallographic orientation of the latest types of these materials. In the spectral range from 0.2 to 7 μm, the material has a high transmittance at the level of theoretically possible (>90%).

Example No. 2. The single crystal structure of CaF₂:3 mol.% Yb is subjected to deformation at a temperature of 1150°C., a vacuum of 10 mm Hg, with a force of 1 mV/cm²within 20 minutes. The degree of deformation of the material is 550%.

Once achieved, the pressure value of 1 mV/cm²make Isobaric-isothermal exposure for 20 minutes to eliminate the pores and make the material density close to theoretical.

Then, similarly to the previous example, carry out the annealing of the material obtained in the environment of gas CF₄. Synthesized thus polycrystal consists of grains having a layered structure, and has high transparency in the field of 0.2 to 7 μm. This sample is used to study the possibility of lasing of the laser radiation at wavelengths of 1.025 and 1.040 μm, excitation radiation with a wavelength of 0.967 μm. While KP is the generation amounted to 45%.

Example No. 3. The crystal on the basis of calcium fluoride doped with fluoride, strontium and ytterbium, passes through a stage of deformation in vacuum at a temperature of 1150°C, with a maximum pressure of 2 mV/cm². Once reached the maximum pressure of 2 mV/cm²make Isobaric-isothermal exposure for 10-60 minutes to make the material homogeneity. The degree of deformation in this case amounted to 400%.

The obtained ceramic material was annealed in fluorinating atmosphere gaseous CF₄at 1300°C for 30 hours. The workpiece has a homogeneous structure with a grain size of 70 μm and a thickness of forming the seed layer 40 nm. Microhardness and Flexural strength of the obtained material were respectively 465 kg/mm²and 9.8 kg/mm². The polycrystal is able to generate laser radiation at wavelengths 1025, 1040 nm with an efficiency of 55%.

Example No. 4. The fine powder of barium fluoride qualifications of barium fluoride brand OFS annealed in an atmosphere of carbon tetrafluoride at a pressure of 1000 mm Hg and a temperature of 1300°C for 20 h, the obtained sintered powder was placed in a mold and subjected to uniaxial deformation in vacuum 10^-4mm Hg at a temperature of 1150°C., applying a pressure of 3 mV/cm²within 30 minutes the Degree of deformation was the amount of 150%. After to what it was reached the pressure of 2 mV/cm ²spent Isobaric-isothermal exposure for 60 minutes.

To increase the transmittance in the vacuum ultraviolet, visible and near IR region of the spectrum ceramic material was further subjected to heat treatment in an atmosphere gas of CF₄at a temperature of 1300°C for 20 hours.

Ceramic material obtained by the proposed method, the optical properties are not inferior to the single crystal of the same composition, but has better mechanical properties: hardness higher than 10-15%, tensile strength Flexural strength higher by 25-30% and the value of fracture toughness is above 2 times.

1. The method of obtaining fluoride nanoceramics, including thermo-mechanical processing of the original crystalline material made of metal halides, at a temperature of plastic deformation, obtaining polycrystalline microstructure of matter, characterized by a grain size of crystals of 3 to 100 μm and nanostructure inside the grains, wherein thermomechanical processing of the original crystalline material is carried out in a vacuum of 10^-4mm Hg, reaching the degree of deformation of the original crystalline material on a value of from 150 to 1000%, resulting in a gain of polycrystalline nanostructured material that is compacted at a pressure of 1-3 mV/cm²to achieve theoretical density, and then annealing the ut in the active medium fluorinating gas.

2. The method according to claim 1, characterized in that as the source of crystalline material used fine powder that has undergone a heat treatment in an environment of gaseous carbon tetrafluoride.

3. The method according to claim 1, characterized in that as the source of crystalline material used molded preparation of the crystalline material obtained from a powder, and heat in the environment of gaseous carbon tetrafluoride.