CA2349597A1 - Method for producing a coating made of powdered materials and device for realising the same - Google Patents
Method for producing a coating made of powdered materials and device for realising the same Download PDFInfo
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- CA2349597A1 CA2349597A1 CA002349597A CA2349597A CA2349597A1 CA 2349597 A1 CA2349597 A1 CA 2349597A1 CA 002349597 A CA002349597 A CA 002349597A CA 2349597 A CA2349597 A CA 2349597A CA 2349597 A1 CA2349597 A1 CA 2349597A1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
- C23C24/04—Impact or kinetic deposition of particles
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- Other Surface Treatments For Metallic Materials (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Junction Field-Effect Transistors (AREA)
Abstract
The purpose of the present invention is to improve the physical and chemical properties of a coating made of various powdered materials and to improve the application process efficiency. This method is characterised in that, before supplying a gas-powder mixture to the acceleration nozzle, said mixture is previously accelerated to a predetermined speed using a gas which is inert relative to the starting powdered material, and further fed into the core of the working-gas acceleration flow. The device includes a pulverisation unit in the form of a supersonic acceleration nozzle comprising a linear section, at its outlet, which turns into a curved-surface section. The device also includes an intermediate supersonic nozzle which is arranged coaxially relative to the acceleration nozzle and is capable of reciprocating movement in the subsonic portion thereof.
Description
METHOD FOR PRODUCING A COATING MADE OF POWDERED MATERIALS
AND DEVICE FOR REALISING THE SAME
Technical Field The present invention relates to the field of applying and producing coatings from powder materials and more par-ticularly to a method of producing a coating from powder ma-terials and to a device for carrying out said method.
Background of the Invention Known in the art is a method of producing a coating from powder materials, which comprises introducing a start ing powder material into a gas stream which accelerates ma terial particles, shaping a high-velocity gas-and-powder jet, and applying the powder material to the surface of an article (Inventor's Certificate RU No. 1618778, C1. C23C
4/00, 1991).
This method suffers from the following disadvantages:
particles of a coating material cannot be accelerated by a gas stream up to velocities close to those of the gas accel-erating thereof, and the process of forming a coating cannot be effected with relatively not high parameters of the work-ing gas (air) with the pressure P < 10*105 N/mz.
Said disadvantages restrict the technological possi-bilities of the method and involve considerable power in-puts.
Also known in the art is a method of producing a coat-ing from powder materials on the surface of an article whose material is selected from the group consisting of metals, alloys, dielectrics, which method comprises the steps of forming an accelerating flow of a working carrier gas, in-troducing particles of a powder material into this flow, seeding the resulting gas-and-powder mixture into an accel-erating supersonic nozzle, and applying the powder material to the surface of an article by the gas flow (International Application WO 91/19016, C1. C23C 4/00, B05B 7/24, B05C
19/00, 1991).
For carrying this method into effect, a device is used, comprising a spraying unit made as a supersonic nozzle with a subsonic converging and a supersonic parts and an interme diate nozzle, a means for feeding a compressed working car-rier gas, and a means for introducing a gas-and-powder mix-ture into the spraying unit (International Application WO
91/19016, C1. C23C 4/00, B05B 7/24, B05C 19/00, 1991).
The disadvantages of the known method and device are as follows: limited possibilities of producing an adequate-quality coating material due to the presence of a superfi-cial oxide film on particles of the employed powder materi-als and, as a result, the presence of oxides in the struc-ture of the coating material; an insufficient effectiveness of the particle acceleration process due to the deceleration of particles in the compressed wall layer of gas at the sur-face of the article being treated; insufficiently high phys-icochemical properties of produced coatings; limited possi-bilities of controlling the velocity of the gas flow and the particles of the powder material from which the coating is formed; the presence of friction and of the deceleration of particles along the walls of the acceleration channel of the supersonic nozzle, which lead to reducing the effectiveness of the coating application process and the service life of the spraying system. Said disadvantages interfere with pro-ducing coatings having high physico-mechanical properties, restrict the technological possibilities of producing a high-quality coating from powder materials, and also inter-fere with the provision of a high effectiveness of the coat-ing application process and with the provision of a long service life of the spraying system.
AND DEVICE FOR REALISING THE SAME
Technical Field The present invention relates to the field of applying and producing coatings from powder materials and more par-ticularly to a method of producing a coating from powder ma-terials and to a device for carrying out said method.
Background of the Invention Known in the art is a method of producing a coating from powder materials, which comprises introducing a start ing powder material into a gas stream which accelerates ma terial particles, shaping a high-velocity gas-and-powder jet, and applying the powder material to the surface of an article (Inventor's Certificate RU No. 1618778, C1. C23C
4/00, 1991).
This method suffers from the following disadvantages:
particles of a coating material cannot be accelerated by a gas stream up to velocities close to those of the gas accel-erating thereof, and the process of forming a coating cannot be effected with relatively not high parameters of the work-ing gas (air) with the pressure P < 10*105 N/mz.
Said disadvantages restrict the technological possi-bilities of the method and involve considerable power in-puts.
Also known in the art is a method of producing a coat-ing from powder materials on the surface of an article whose material is selected from the group consisting of metals, alloys, dielectrics, which method comprises the steps of forming an accelerating flow of a working carrier gas, in-troducing particles of a powder material into this flow, seeding the resulting gas-and-powder mixture into an accel-erating supersonic nozzle, and applying the powder material to the surface of an article by the gas flow (International Application WO 91/19016, C1. C23C 4/00, B05B 7/24, B05C
19/00, 1991).
For carrying this method into effect, a device is used, comprising a spraying unit made as a supersonic nozzle with a subsonic converging and a supersonic parts and an interme diate nozzle, a means for feeding a compressed working car-rier gas, and a means for introducing a gas-and-powder mix-ture into the spraying unit (International Application WO
91/19016, C1. C23C 4/00, B05B 7/24, B05C 19/00, 1991).
The disadvantages of the known method and device are as follows: limited possibilities of producing an adequate-quality coating material due to the presence of a superfi-cial oxide film on particles of the employed powder materi-als and, as a result, the presence of oxides in the struc-ture of the coating material; an insufficient effectiveness of the particle acceleration process due to the deceleration of particles in the compressed wall layer of gas at the sur-face of the article being treated; insufficiently high phys-icochemical properties of produced coatings; limited possi-bilities of controlling the velocity of the gas flow and the particles of the powder material from which the coating is formed; the presence of friction and of the deceleration of particles along the walls of the acceleration channel of the supersonic nozzle, which lead to reducing the effectiveness of the coating application process and the service life of the spraying system. Said disadvantages interfere with pro-ducing coatings having high physico-mechanical properties, restrict the technological possibilities of producing a high-quality coating from powder materials, and also inter-fere with the provision of a high effectiveness of the coat-ing application process and with the provision of a long service life of the spraying system.
Disclosure of the Invention The problem underlying the described invention is the provision of a method of preparing a coating from powder ma-terial and a device for carrying this method into effect, which would make it possible to broaden the technological possibilities of producing coatings from various powder ma-terials and from their mixtures, to improve the physico-chemical properties of the resulting coating material, to raise the effectiveness of the process of applying and form-ing the coating, and to prolong the service life of the spraying system.
The indicated technical result is attained owing to the use of method of producing a coating from powder materials and of a device for carrying this method into effect, the essence of which is as follows:
The herein-proposed method of producing a coating from powder materials, comprising the steps of forming an accel-erating flow of a carrier gas, introducing particles of a powder material thereinto, feeding the resulting gas-and-powder mixture into an accelerating supersonic nozzle, and applying the powder material by means of the gas flow to the surface of an article, envisages that before feeding the gas-and-powder mixture into the supersonic nozzle the mix-ture is pre-accelerated by a gas inert with respect to the starting powder material to a velocity defined by the number 0.3 < M <_ 1.0, where M is the Mach number, and accelerated additionally by introducing the gas-and-powder mixture into the core of the accelerating flow of the carrier gas, and that before applying the coating powder material to the sur-face of an article the powder particles are separated from the gas. The accelerating flow of the working carrier gas is formed in accordance with the square law of variation of the profile of the accelerating supersonic nozzle area. This provides a possibility for a more effective utilization of the gas flow energy.
It is reasonable to effect feeding of the gas-and powder mixture into the accelerating nozzle with the cumula tive flow of the accelerating carrier gas and of the gas in ert to the powder material set in accordance with the rated conditions of the accelerating nozzle.
The method envisages the use of air or of a mixture of gases as the working carrier gas and the use of a gas or a mixture of gases not reacting with the powdered components of the powder material as the gas inert with respect to this material.
Before the preliminary acceleration of the powder mate rial, it is subjected to mechanical, electrochemical or chemical treatment in a gaseous medium inert to the starting powder material, and the powder material is supplied in a flow of this medium into a metering feeder.
It is desirable that a gas with the temperature T <_ 300 K should be used as the gas inert to the powder material.
The gas-and-powder mixture may be introduced into the core of the accelerating flow from the metering feeder in a pulsed mode.
When applying the powder material to the surface of an article, the latter may be brought in vibratory motion coax Tally to the incident two-phase supersonic flow.
For enhancing the plasticity of the surface to be coated, the article is subjected to superficial heating.
In the course of applying a coating, a potential may be supplied to the article to be coated, the sign of this po tential being opposite to that of the particles in the two phase flow of the gas-and-powder mixture.
The essence of the invention, as regards the herein-proposed device, is that the device for producing coatings from powder materials, comprising a spraying unit made as an accelerating supersonic nozzle with a subsonic converging and a supersonic parts and an intermediate nozzle, a means for feeding a compressed working carrier gas, and a means for introducing a gas-and-powder mixture into the spraying 5 unit, and a metering feeder, is provided with a means for supplying an additional compressed gas inert to the powder material, the intermediate nozzle is made as a supersonic one, with the diameter of the nozzle exit section dsect.
smaller than the diameter of the critical section D~rit. of the accelerating nozzle, and is arranged coaxially with the possibility of translational displacement in the subsonic converging part, the accelerating supersonic nozzle having at the outlet of the supersonic part a linear portion which passes into a portion with a curvilinear surface of a radius R.
The device is provided with a unit for treating the powder material with a view to activating and cleaning the surface the particles of the coating material, with a gas pulser connected to the means for introducing the gas-and-powder mixture, with a vibrator for imparting vibrations to the article being coated, and with a power supply source for supplying a potential to the article.
Brief Description of Drawings The invention is further explained by a particular ex ample of its embodiment and by the accompanying drawings, in which:
Fig. 1 shows a general view of a device for producing a coating from powder materials;
Fig. 2 shows a spraying unit of the proposed device with a means for introducing a gas-and-air mixture and sepa-rating a two-phase flow into fractions.
Best Mode of Carrying the Invention into Effect The device of the invention comprises a means 1 for feeding a compressed gas inert to a coating material (to a mixture of powdered components), a shutoff valve 2, a unit 3 for the pretreatment of a powder material to remove an oxide film from and to activate particles of the powder material, a unit 4 for collecting the oxide film and the fine-s dispersed fraction of the powder, a unit 5 for feeding the treated powder material to a metering feeder 6, a shutoff valve 7, a pulser 8 of the gas inert to the powder material, a means 9 for feeding a working carrier gas (for instance, air), a system 10 for controlling the working process of ap-plying coatings, a heater 11 of the working carrier gas, a unit 12 for the provision of translational axial displace-ment of an intermediate supersonic nozzle 13, a chamber 14 for adjusting the carrier-gas flow, a centering perforated sleeve 15, an accelerating nozzle 16 with a linear portion 17 which passes into a portion with a curvilinear surface 18 for varying the direction of motion of the gas flow, a means 19 for turning the gas flow away from the article being coated 20, a means 21 for securing and rotating the article being coated, a unit 22 for the translational displacement of the article being coated, a vibrator 23, a power supply source 24, a tube 25 for feeding 'the gas-and-powder mixture, a tube 26 for feeding the working carrier gas.
The method of the invention is carried into effect and the device of the invention operates in the following man-ner.
A gas inert to the coating material (to a mixture of powdered components) is fed under a pressure, with the shut-off valve open, from the means 1 to the unit 3 for the pre-treatment of the powder coating material, said unit being preliminarily filled with a required amount of a powder (a mixture of powders). When the unit 3 for the pretreatment of the powder material is thrown into action, oxide film is re-moved from the surface of the powder material particles therein by a mechanical or any other method. After the pre-treatment, waste substances in the form of oxide'film parti-cles and non-calibrated fine-dispersed fraction of the pow-der come to the unit 4. Then the particles of the powder coating material are activated by an electromagnetic, ther-mal, chemical or any other method, depending on the chemical composition and physical properties of the powder material (the mixture of powdered components). The activated parti-cles are supplied with the help of the unit 5 into the me-tering feeder 6. After filling the metering feeder 6 with the powder material and with the gas inert to the powder ma-terial, the units 3, 4, 5 are switched off, and the shutoff valve 2 is closed, whereby supplying the gas inert to the powder material is stopped.
For the process of producing a coating from powder ma terials, a working carrier gas (for instance, air, nitrogen) is supplied under a pressure from the feeding means 9 to the system 10 for controlling the working process of applying coatings, wherein the pressure is reduced to the required working value. The gas whose pressure reduced to the re quired value comes to the heater 11 of the gas, where the gas is heated to a temperature corresponding to the rated operating conditions. The heated working carrier gas comes along the tube 26 for feeding the working carrier gas to the chamber 14 for adjusting the carrier-gas flow, and then through profiled apertures in the centering sleeve the work-ing carrier gas is fed to the accelerating supersonic nozzle 16, wherein the carrier gas is accelerated to the velocity required for applying and forming a coating. When the re-quired parameters of the working carrier gas are reached, the shutoff valve 7 is opened, whereby feeding of the gas inert to the powder material is effected, which gas first comes to the pulser 8, where it acquires a pulsating compo-nent having a required frequency. From the pulser 8 the gas inert to the powder material with the required frequency comes to the metering feeder 6 wherein, as the gas under variable pressure is mixed with the particles of the powder coating material, a gas-and-powder mixture is formed, in which the powder particles are in the form of a suspension.
The resulting gas-and-powder mixture is fed in the form of a two-phase flow through the tube 25 into the intermediate su-personic nozzle 13 and then into the core of the accelerat-ing flow of the carrier gas into the area of the critical section of the accelerating supersonic nozzle 16. The re-quired rated thermo- and gasdynamic parameters of the work-ing carrier gas and of the pulsating gas-and-powder mixture in the area of the critical section of the accelerating noz-zle 16 are attained by displacing the intermediate super-sonic nozzle 13. This displacement is performed in a trans-latory manner along the axis of the nozzles, with the help of the unit 12 for the provision of translational axial dis-placement, for a distance depending on the velocity of flow and the frequency of pulsations of the gas-and-powder mix-ture in the area of the critical section of the accelerating supersonic nozzle 16. When the required displacement is achieved, the unit 12 for'the provision of axial displace-ment of the intermediate supersonic nozzle 13 is switched off. The pulsating mixture of particles with the gas inert to them, issuing from the intermediate supersonic nozzle 13, having the initial axial velocity 0.3 _< M _< 1.0 (where M is the Mach number) , is mixed in the area of the critical sec-tion of the accelerating supersonic nozzle 16 with the work-ing carrier gas, and in this area the main acceleration of the gas-and-powder mixture takes place. Having acquired the required velocity along the channel of the accelerating su-personic nozzle 16, the flow of the gas-and-powder mixture adjusts the direction of its motion within the linear por-tion 17, then the main part of the gas flow turns within the portion with a curvilinear surface 18 and gets into . the en-trance portion of the means 19 for turning off the gas flow.
The powder particles of the coating material, having a large mass and sluggishness, continue their rectilinear motion till they collide with the surface of the article being coated. When the necessary thermo- and gasdynamic conditions for applying the coating are attained, the article 20 to be coated, which is secured in the means 21 for securing the article, is set in (back-and-forth or rotary) motion. Then the vibrator 23, connected with the unit 22 for the dis-placement of the article, and the power supply source 24, which feeds to the article 20 a potential whose sign is op-posite to that of the moving particles, are switched on.
This is how the process of applying a coating to and forming a coating on the surface of an article occurs.
As the gas inert to the powder material, a gas (a mix-ture of gases) may be chosen, which does not react chemi-cally with the powder material of the coating, for instance, nitrogen, argon, helium, krypton, and others. The choice is determined by particular requirements to the properties of the resulting coating, its structure, and the composition of the material of the latter.
Removal of the oxide film from the surface of the pow-der particles of the coating material, activation of the particles, and their preliminary acceleration by the gas in-ert to the particles, prevent oxidation of the coating mate-rial and make it possible, when applying and forming a coat-ing, to obtain chemically pure materials, without oxides in their structure, to improve substantially their structure, physicochemical and technological properties.
The coefficient of utilization of the coating material being applied, the adhesion, cohesion and its structure de-pend on the impact velocity of the coating particles being applied with the surface of the material.
Preliminary acceleration of the particles of the coat-ing material by the gas inert to them at a temperature T 5 <_ 300 K, with the velocity of the accelerating gas of 0.3 5 < M 5 1.0, and introducing the gas-and-powder mixture into 5 the core of the carrier gas accelerating the particles make it possible to increase substantially the velocity of the particles of the coating material to a velocity close to that of the accelerating gas and thereby to make maximum use of the energy of the gas jet accelerating the particles. In-10 troducing the powder mixture into the core of the accelerat-ing flow of the carrier gas eliminates the effect of decel-eration of the particles by the walls of the flow-through part of the supersonic accelerating nozzle, prolongs the service life of the device, increases the coefficient of utilization of the coating material being applied. For eliminating the effect of decelerating the coating particles in the compressed near-wall gas layer, which originates as the supersonic gas jet falls upon the surface of the arti-cle, in the method of the invention the gas flow is turned and moved away from the surface of the article being treated. Turning of the gas flow is brought about by the physical effect which originates as the plane-parallel flow of gas flows around the curvilinear surface of radius R.
Thus, turning of the gas flow and moving it away from the surface of the surface of the article being treated elimi-nate the appearance of the compressed near-wall gas layer on the surface of the article, and the coating particles con-tinue their rectilinear motion, reach the surface of the ar-ticle with the velocity which they acquired in their inter-action with the gas flow accelerating them. Thereby, it be-comes possible, with smaller energy parameters of the gas flow, to apply particles of the of the coating material with higher impact velocities with the surface of the material of the article. As a result, the power inputs are reduced, the coefficient of utilization of the coating material is in-creased, and the structure, quality and properties of the coating material are improved.
Setting the cumulative rate of flow of the working car s rier gas and of the gas inert to the powder coating material in accordance with the calculated conditions of the gas flow issue from the accelerating nozzle is the regime in which the pressure in the exit section of the accelerating super sonic nozzle corresponds to the pressure of the ambient me dium. Under this condition the velocity of the gas flow is-suing from the supersonic nozzle will be maximum. Any changes in the parameters of the carrier gas, such as tem-perature, pressure, kind of gas, lead to off-design condi-tions of the issue, i.e., to a loss of the gas flow velocity and, consequently, of the velocity of particles of the coat-ing material being applied.
Vibratory motions of the article being treated in the case of synchronous introducing in the pulsed mode of the gas-and-powder mixture into the core of the accelerating flow of the carrier gas are effected in such a manner that feeding the gas-and-powder mixture occurs at the moment when the article being treated moves in a direction opposite to that of the flow of particles of the coating material. In this case the velocity of moving particles of the coating material and the velocity of displacing the article being treated are added together. As a result, the velocity of collision of the particles with the surface increases. This leads to an increase in the depth of penetration of the par-ticles into the surface of the material of the article, in the extent of their plastic deformation, in the coefficient of utilization of the coating material, to an improvement in the structure of the coating and its technological proper-ties.
The indicated technical result is attained owing to the use of method of producing a coating from powder materials and of a device for carrying this method into effect, the essence of which is as follows:
The herein-proposed method of producing a coating from powder materials, comprising the steps of forming an accel-erating flow of a carrier gas, introducing particles of a powder material thereinto, feeding the resulting gas-and-powder mixture into an accelerating supersonic nozzle, and applying the powder material by means of the gas flow to the surface of an article, envisages that before feeding the gas-and-powder mixture into the supersonic nozzle the mix-ture is pre-accelerated by a gas inert with respect to the starting powder material to a velocity defined by the number 0.3 < M <_ 1.0, where M is the Mach number, and accelerated additionally by introducing the gas-and-powder mixture into the core of the accelerating flow of the carrier gas, and that before applying the coating powder material to the sur-face of an article the powder particles are separated from the gas. The accelerating flow of the working carrier gas is formed in accordance with the square law of variation of the profile of the accelerating supersonic nozzle area. This provides a possibility for a more effective utilization of the gas flow energy.
It is reasonable to effect feeding of the gas-and powder mixture into the accelerating nozzle with the cumula tive flow of the accelerating carrier gas and of the gas in ert to the powder material set in accordance with the rated conditions of the accelerating nozzle.
The method envisages the use of air or of a mixture of gases as the working carrier gas and the use of a gas or a mixture of gases not reacting with the powdered components of the powder material as the gas inert with respect to this material.
Before the preliminary acceleration of the powder mate rial, it is subjected to mechanical, electrochemical or chemical treatment in a gaseous medium inert to the starting powder material, and the powder material is supplied in a flow of this medium into a metering feeder.
It is desirable that a gas with the temperature T <_ 300 K should be used as the gas inert to the powder material.
The gas-and-powder mixture may be introduced into the core of the accelerating flow from the metering feeder in a pulsed mode.
When applying the powder material to the surface of an article, the latter may be brought in vibratory motion coax Tally to the incident two-phase supersonic flow.
For enhancing the plasticity of the surface to be coated, the article is subjected to superficial heating.
In the course of applying a coating, a potential may be supplied to the article to be coated, the sign of this po tential being opposite to that of the particles in the two phase flow of the gas-and-powder mixture.
The essence of the invention, as regards the herein-proposed device, is that the device for producing coatings from powder materials, comprising a spraying unit made as an accelerating supersonic nozzle with a subsonic converging and a supersonic parts and an intermediate nozzle, a means for feeding a compressed working carrier gas, and a means for introducing a gas-and-powder mixture into the spraying 5 unit, and a metering feeder, is provided with a means for supplying an additional compressed gas inert to the powder material, the intermediate nozzle is made as a supersonic one, with the diameter of the nozzle exit section dsect.
smaller than the diameter of the critical section D~rit. of the accelerating nozzle, and is arranged coaxially with the possibility of translational displacement in the subsonic converging part, the accelerating supersonic nozzle having at the outlet of the supersonic part a linear portion which passes into a portion with a curvilinear surface of a radius R.
The device is provided with a unit for treating the powder material with a view to activating and cleaning the surface the particles of the coating material, with a gas pulser connected to the means for introducing the gas-and-powder mixture, with a vibrator for imparting vibrations to the article being coated, and with a power supply source for supplying a potential to the article.
Brief Description of Drawings The invention is further explained by a particular ex ample of its embodiment and by the accompanying drawings, in which:
Fig. 1 shows a general view of a device for producing a coating from powder materials;
Fig. 2 shows a spraying unit of the proposed device with a means for introducing a gas-and-air mixture and sepa-rating a two-phase flow into fractions.
Best Mode of Carrying the Invention into Effect The device of the invention comprises a means 1 for feeding a compressed gas inert to a coating material (to a mixture of powdered components), a shutoff valve 2, a unit 3 for the pretreatment of a powder material to remove an oxide film from and to activate particles of the powder material, a unit 4 for collecting the oxide film and the fine-s dispersed fraction of the powder, a unit 5 for feeding the treated powder material to a metering feeder 6, a shutoff valve 7, a pulser 8 of the gas inert to the powder material, a means 9 for feeding a working carrier gas (for instance, air), a system 10 for controlling the working process of ap-plying coatings, a heater 11 of the working carrier gas, a unit 12 for the provision of translational axial displace-ment of an intermediate supersonic nozzle 13, a chamber 14 for adjusting the carrier-gas flow, a centering perforated sleeve 15, an accelerating nozzle 16 with a linear portion 17 which passes into a portion with a curvilinear surface 18 for varying the direction of motion of the gas flow, a means 19 for turning the gas flow away from the article being coated 20, a means 21 for securing and rotating the article being coated, a unit 22 for the translational displacement of the article being coated, a vibrator 23, a power supply source 24, a tube 25 for feeding 'the gas-and-powder mixture, a tube 26 for feeding the working carrier gas.
The method of the invention is carried into effect and the device of the invention operates in the following man-ner.
A gas inert to the coating material (to a mixture of powdered components) is fed under a pressure, with the shut-off valve open, from the means 1 to the unit 3 for the pre-treatment of the powder coating material, said unit being preliminarily filled with a required amount of a powder (a mixture of powders). When the unit 3 for the pretreatment of the powder material is thrown into action, oxide film is re-moved from the surface of the powder material particles therein by a mechanical or any other method. After the pre-treatment, waste substances in the form of oxide'film parti-cles and non-calibrated fine-dispersed fraction of the pow-der come to the unit 4. Then the particles of the powder coating material are activated by an electromagnetic, ther-mal, chemical or any other method, depending on the chemical composition and physical properties of the powder material (the mixture of powdered components). The activated parti-cles are supplied with the help of the unit 5 into the me-tering feeder 6. After filling the metering feeder 6 with the powder material and with the gas inert to the powder ma-terial, the units 3, 4, 5 are switched off, and the shutoff valve 2 is closed, whereby supplying the gas inert to the powder material is stopped.
For the process of producing a coating from powder ma terials, a working carrier gas (for instance, air, nitrogen) is supplied under a pressure from the feeding means 9 to the system 10 for controlling the working process of applying coatings, wherein the pressure is reduced to the required working value. The gas whose pressure reduced to the re quired value comes to the heater 11 of the gas, where the gas is heated to a temperature corresponding to the rated operating conditions. The heated working carrier gas comes along the tube 26 for feeding the working carrier gas to the chamber 14 for adjusting the carrier-gas flow, and then through profiled apertures in the centering sleeve the work-ing carrier gas is fed to the accelerating supersonic nozzle 16, wherein the carrier gas is accelerated to the velocity required for applying and forming a coating. When the re-quired parameters of the working carrier gas are reached, the shutoff valve 7 is opened, whereby feeding of the gas inert to the powder material is effected, which gas first comes to the pulser 8, where it acquires a pulsating compo-nent having a required frequency. From the pulser 8 the gas inert to the powder material with the required frequency comes to the metering feeder 6 wherein, as the gas under variable pressure is mixed with the particles of the powder coating material, a gas-and-powder mixture is formed, in which the powder particles are in the form of a suspension.
The resulting gas-and-powder mixture is fed in the form of a two-phase flow through the tube 25 into the intermediate su-personic nozzle 13 and then into the core of the accelerat-ing flow of the carrier gas into the area of the critical section of the accelerating supersonic nozzle 16. The re-quired rated thermo- and gasdynamic parameters of the work-ing carrier gas and of the pulsating gas-and-powder mixture in the area of the critical section of the accelerating noz-zle 16 are attained by displacing the intermediate super-sonic nozzle 13. This displacement is performed in a trans-latory manner along the axis of the nozzles, with the help of the unit 12 for the provision of translational axial dis-placement, for a distance depending on the velocity of flow and the frequency of pulsations of the gas-and-powder mix-ture in the area of the critical section of the accelerating supersonic nozzle 16. When the required displacement is achieved, the unit 12 for'the provision of axial displace-ment of the intermediate supersonic nozzle 13 is switched off. The pulsating mixture of particles with the gas inert to them, issuing from the intermediate supersonic nozzle 13, having the initial axial velocity 0.3 _< M _< 1.0 (where M is the Mach number) , is mixed in the area of the critical sec-tion of the accelerating supersonic nozzle 16 with the work-ing carrier gas, and in this area the main acceleration of the gas-and-powder mixture takes place. Having acquired the required velocity along the channel of the accelerating su-personic nozzle 16, the flow of the gas-and-powder mixture adjusts the direction of its motion within the linear por-tion 17, then the main part of the gas flow turns within the portion with a curvilinear surface 18 and gets into . the en-trance portion of the means 19 for turning off the gas flow.
The powder particles of the coating material, having a large mass and sluggishness, continue their rectilinear motion till they collide with the surface of the article being coated. When the necessary thermo- and gasdynamic conditions for applying the coating are attained, the article 20 to be coated, which is secured in the means 21 for securing the article, is set in (back-and-forth or rotary) motion. Then the vibrator 23, connected with the unit 22 for the dis-placement of the article, and the power supply source 24, which feeds to the article 20 a potential whose sign is op-posite to that of the moving particles, are switched on.
This is how the process of applying a coating to and forming a coating on the surface of an article occurs.
As the gas inert to the powder material, a gas (a mix-ture of gases) may be chosen, which does not react chemi-cally with the powder material of the coating, for instance, nitrogen, argon, helium, krypton, and others. The choice is determined by particular requirements to the properties of the resulting coating, its structure, and the composition of the material of the latter.
Removal of the oxide film from the surface of the pow-der particles of the coating material, activation of the particles, and their preliminary acceleration by the gas in-ert to the particles, prevent oxidation of the coating mate-rial and make it possible, when applying and forming a coat-ing, to obtain chemically pure materials, without oxides in their structure, to improve substantially their structure, physicochemical and technological properties.
The coefficient of utilization of the coating material being applied, the adhesion, cohesion and its structure de-pend on the impact velocity of the coating particles being applied with the surface of the material.
Preliminary acceleration of the particles of the coat-ing material by the gas inert to them at a temperature T 5 <_ 300 K, with the velocity of the accelerating gas of 0.3 5 < M 5 1.0, and introducing the gas-and-powder mixture into 5 the core of the carrier gas accelerating the particles make it possible to increase substantially the velocity of the particles of the coating material to a velocity close to that of the accelerating gas and thereby to make maximum use of the energy of the gas jet accelerating the particles. In-10 troducing the powder mixture into the core of the accelerat-ing flow of the carrier gas eliminates the effect of decel-eration of the particles by the walls of the flow-through part of the supersonic accelerating nozzle, prolongs the service life of the device, increases the coefficient of utilization of the coating material being applied. For eliminating the effect of decelerating the coating particles in the compressed near-wall gas layer, which originates as the supersonic gas jet falls upon the surface of the arti-cle, in the method of the invention the gas flow is turned and moved away from the surface of the article being treated. Turning of the gas flow is brought about by the physical effect which originates as the plane-parallel flow of gas flows around the curvilinear surface of radius R.
Thus, turning of the gas flow and moving it away from the surface of the surface of the article being treated elimi-nate the appearance of the compressed near-wall gas layer on the surface of the article, and the coating particles con-tinue their rectilinear motion, reach the surface of the ar-ticle with the velocity which they acquired in their inter-action with the gas flow accelerating them. Thereby, it be-comes possible, with smaller energy parameters of the gas flow, to apply particles of the of the coating material with higher impact velocities with the surface of the material of the article. As a result, the power inputs are reduced, the coefficient of utilization of the coating material is in-creased, and the structure, quality and properties of the coating material are improved.
Setting the cumulative rate of flow of the working car s rier gas and of the gas inert to the powder coating material in accordance with the calculated conditions of the gas flow issue from the accelerating nozzle is the regime in which the pressure in the exit section of the accelerating super sonic nozzle corresponds to the pressure of the ambient me dium. Under this condition the velocity of the gas flow is-suing from the supersonic nozzle will be maximum. Any changes in the parameters of the carrier gas, such as tem-perature, pressure, kind of gas, lead to off-design condi-tions of the issue, i.e., to a loss of the gas flow velocity and, consequently, of the velocity of particles of the coat-ing material being applied.
Vibratory motions of the article being treated in the case of synchronous introducing in the pulsed mode of the gas-and-powder mixture into the core of the accelerating flow of the carrier gas are effected in such a manner that feeding the gas-and-powder mixture occurs at the moment when the article being treated moves in a direction opposite to that of the flow of particles of the coating material. In this case the velocity of moving particles of the coating material and the velocity of displacing the article being treated are added together. As a result, the velocity of collision of the particles with the surface increases. This leads to an increase in the depth of penetration of the par-ticles into the surface of the material of the article, in the extent of their plastic deformation, in the coefficient of utilization of the coating material, to an improvement in the structure of the coating and its technological proper-ties.
In order to intensify the course of mechanical and chemical processes in the superficial layer of the material of the article on collision of particles of the coating ma-terial with the surface of the article in the method of the invention, the article is subjected to surface heating to a temperature at which the plasticity of the surface of the material of the article is close to the plasticity of the coating material. This makes it possible to apply coatings having a smaller hardness to harder and less plastic sur-faces of articles. In this case the properties of the tran-sition zone (material of the particles and material of the article) change sharply, the structure of this zone and, as a consequence, adhesion of the coating, becomes improved. In the transition zone there is also formed an intermetallic compound on application of a metal to a metal, consisting of the material of the coating particles being applied and of the material of the article. Solid particles, while moving in the gas flow, acquire a charge having a definite value and sign due to friction with gas, against each other, and on the walls of the flow-through part of the gas channel.
The value and sign of the charge depend on the material of the particles. When in the method of the invention an oppo-site-sign potential is fed to the surface of the article be-ing coated, there occurs an increase in the velocity of the charged particles as they approach to the surface of the ar-ticle, and a micro-arc discharge originates on collision.
Acting on the moving flow of charged particles by dif-ferent electromagnetic methods and by the value of the po tential fed to the article, it is possible to regulate the process of applying and forming the coating.
This makes it possible to vary the structure, proper-ties and quality of the coating in the course of applying thereof.
The value and sign of the charge depend on the material of the particles. When in the method of the invention an oppo-site-sign potential is fed to the surface of the article be-ing coated, there occurs an increase in the velocity of the charged particles as they approach to the surface of the ar-ticle, and a micro-arc discharge originates on collision.
Acting on the moving flow of charged particles by dif-ferent electromagnetic methods and by the value of the po tential fed to the article, it is possible to regulate the process of applying and forming the coating.
This makes it possible to vary the structure, proper-ties and quality of the coating in the course of applying thereof.
The structural feature of the means for introducing the gas-and-powder mixture make it possible to effect axial in-troducing of the coating particles with the starting eeloc-ity into the core of the working carrier-gas flow accelerat-ing said particles, obviating the interaction of particles of the coating material with the walls of the accelerating nozzle 16 under the conditions of dsect. ~
Thereby it becomes possible to prolong the service life of the device, to make maximum use of the energy of the gas flow for increasing the kinetic energy of the particles of the coating material, to carry into effect the process of coating formation with relatively not high starting parame-ters of the carrier gas, to increase the coefficient of utilization of the material being applied.
The device of the invention may be used for producing multifunctional coatings and materials from various powdered components selected from the group comprising metals, alloys or mechanical mixtures thereof, as well as dielectrics and organic compounds.
Owing to the provision of conditions which allow acti-vating the particles and rule out the presence of an oxide film on their surface, the range of materials used for the application of coatings by the method of the invention may be substantially broadened.
So, the described method and device for producing coat-ings from powder materials make it possible to intensify the process of applying and forming coatings from various pow-ders and their mixtures, to obtain a coating material with-out the presence of oxide inclusions in its structure, to improve the structure and physicochemical properties of the coating material, to increase the coefficient of utilization of the coating material, to reduce the energy parameters of the gas flow, to broaden the possibility of controlling the process of applying and forming coatings, to obtain materi-als in coatings with unique properties, to broaden the tech-nological and functional possibilities of the process for producing coatings.
Industrial Applicability The present invention may be used in metallurgy, me-chanical engineering, radio- and electronic engineering and other industries for improving the technological and phys-5 icochemical properties of articles, for restoring various worn-out parts, and for imparting specific properties to the surface of articles.
Thereby it becomes possible to prolong the service life of the device, to make maximum use of the energy of the gas flow for increasing the kinetic energy of the particles of the coating material, to carry into effect the process of coating formation with relatively not high starting parame-ters of the carrier gas, to increase the coefficient of utilization of the material being applied.
The device of the invention may be used for producing multifunctional coatings and materials from various powdered components selected from the group comprising metals, alloys or mechanical mixtures thereof, as well as dielectrics and organic compounds.
Owing to the provision of conditions which allow acti-vating the particles and rule out the presence of an oxide film on their surface, the range of materials used for the application of coatings by the method of the invention may be substantially broadened.
So, the described method and device for producing coat-ings from powder materials make it possible to intensify the process of applying and forming coatings from various pow-ders and their mixtures, to obtain a coating material with-out the presence of oxide inclusions in its structure, to improve the structure and physicochemical properties of the coating material, to increase the coefficient of utilization of the coating material, to reduce the energy parameters of the gas flow, to broaden the possibility of controlling the process of applying and forming coatings, to obtain materi-als in coatings with unique properties, to broaden the tech-nological and functional possibilities of the process for producing coatings.
Industrial Applicability The present invention may be used in metallurgy, me-chanical engineering, radio- and electronic engineering and other industries for improving the technological and phys-5 icochemical properties of articles, for restoring various worn-out parts, and for imparting specific properties to the surface of articles.
Claims (17)
1. A method of producing a coating from powder materi-als, comprising the steps of forming an accelerating flow of a working carrier gas, introducing particles of a powder ma-terial thereinto, feeding the resulting gas-and-powder mix-ture into an accelerating supersonic nozzle (16), and apply-ing the powder material to the surface of an article with the help of the gas flow, characterized in that before feeding the gas-and-powder mixture into the super-sonic nozzle (16), the mixture is subjected to preliminary acceleration by a gas inert to the starting powder material to a velocity defined by the number 0.3 ~ M ~ 1.0, wherein M
is the Mach number, and to additional acceleration by intro-ducing the gas-and-powder mixture into the core of the ac-celerating flow of the working carrier gas, and in that be-fore applying the powder material to the surface of the ar-ticle the powder particles are separated from the gas.
is the Mach number, and to additional acceleration by intro-ducing the gas-and-powder mixture into the core of the ac-celerating flow of the working carrier gas, and in that be-fore applying the powder material to the surface of the ar-ticle the powder particles are separated from the gas.
2. A method according to claim 1, character-ized in that forming said accelerating flow of a working carrier gas is effected in accordance with the square law of variation of the profile of the accelerating supersonic noz-zle area.
3. A method according to any of claims 1, 2, char-acterized in that feeding the gas-and-powder mix-ture into the accelerating nozzle (16) is effected with the cumulative flow of the accelerating carrier gas and of the gas inert to the powder material set in accordance with the rated conditions of the accelerating nozzle (16).
4. A method according to any of claims 1-3, char-acterized in that air is used as the working car-rier gas and a gas or a mixture of gases which do not react with the powder material is used as the gas inert to the powder material.
5. A method according to any of claims 1-4, char-acterized in that before the preliminary accelera-tion the powder material is subjected to treatment in a gaseous medium inert to the powder material for activating the powder particles and removing an oxide film from the surface of the powder particles, and in that the powder ma-terial is fed in a flow of this medium into a metering feeder (6).
6. A method according to claim 5, character-ized in that the treatment of the powder material is ef-fected by mechanical, electrochemical or chemical methods.
7. A method according to any of claims 1-6, char-acterized in that the gas inert to the powder mate-rial is used at a temperature T ~ 300 K.
8. A method according to any of claims 1-7, char-acterized in that introducing the gas-and powder mixture into the core of the accelerating flow of the work-ing carrier gas is effected in a pulsed mode.
9. A method according to any of claims 1-8, char-acterized in that in applying the powder coating material to the surface of an article, the latter is sub-jected to a vibratory displacement coaxially to an incident two-phase flow.
10. A method according to any of claims 1-9, char-acterized in that in applying the powder coating material a surface heating of the material is effected.
11. A method according to any of claims 1-10, char-acterized in that applying the powder material to the surface to be coated is carried out with feeding a po-tential to the article, the sign of the potential being op-posite to that of the particles of the flow of the gas-and-powder mixture.
12. A device for producing a coating from powder mate-rials, comprising a spraying unit made as an accelerating supersonic nozzle (16) with a subsonic converging part and a supersonic diverging part and an intermediate nozzle (13), a means (9) for feeding compressed working carrier gas, a means for introducing the gas-and-powder mixture into the spraying unit and a metering feeder (6), character-ized in that it is provided with a means for feeding ad-ditional compressed gas, inert to the powder coating mate-rial, the intermediate nozzle (13) is made as a supersonic one, with the diameter of the nozzle exit section d sect.
smaller than the diameter of the critical section D crit. of the accelerating nozzle, and is arranged coaxially with the possibility of translational displacement in the subsonic converging part, and the accelerating supersonic nozzle (16) has at the outlet of its supersonic part a linear portion (17) which passes into a portion with a curvilinear surface (18) of a radius R.
smaller than the diameter of the critical section D crit. of the accelerating nozzle, and is arranged coaxially with the possibility of translational displacement in the subsonic converging part, and the accelerating supersonic nozzle (16) has at the outlet of its supersonic part a linear portion (17) which passes into a portion with a curvilinear surface (18) of a radius R.
13. A device according to claim 12, character-ized in that it is provided with a unit (3) for treating the powder material for activating and cleaning the surface of the particles, which is connected with a means for intro-ducing the gas-and-powder mixture.
14. A device according to any of claims 12-13, cha-racterized in that is provided with a pulser (8) connected with the means for introducing the gas-and-powder mixture.
15. A device according to any of claims 12-14, cha-racterized in that the pulser (8) is arranged ahead of the metering feeder (6).
16. A device according to any of claims 12-15, cha-racterized in that it is provided with a vibrator (23) for imparting vibrations to the article being coated.
17. A device according to any of claims 12-16, cha-racterized in that it is provided with a power supply source (24) for feeding a potential to the article.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU98119848/02A RU2145644C1 (en) | 1998-11-05 | 1998-11-05 | Method and device for producing coat from powder materials |
| RU98119848 | 1998-11-05 | ||
| PCT/RU1999/000262 WO2000028110A1 (en) | 1998-11-05 | 1999-07-29 | Method for producing a coating made of powdered materials and device for realising the same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2349597A1 true CA2349597A1 (en) | 2000-05-18 |
Family
ID=20211902
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002349597A Abandoned CA2349597A1 (en) | 1998-11-05 | 1999-07-29 | Method for producing a coating made of powdered materials and device for realising the same |
Country Status (7)
| Country | Link |
|---|---|
| EP (1) | EP1132497A4 (en) |
| KR (1) | KR20010085999A (en) |
| CN (1) | CN1332811A (en) |
| AU (1) | AU1087500A (en) |
| CA (1) | CA2349597A1 (en) |
| RU (1) | RU2145644C1 (en) |
| WO (1) | WO2000028110A1 (en) |
Families Citing this family (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1031388B1 (en) | 1999-02-26 | 2012-12-19 | Hitachi Metals, Ltd. | Surface-treatment of hollow work, and ring-shaped bonded magnet produced by the process |
| US6641778B2 (en) | 2001-05-17 | 2003-11-04 | National Research Council Of Canada | Device and method for regulating flow of particulate material, especially small flows of fine powder |
| DE10158622A1 (en) * | 2001-11-29 | 2003-06-12 | Benteler Automobiltechnik Gmbh | Removing oxide layers from steel component and simultaneously coating them, jet blasts them with particles at just under mach one |
| GB0130782D0 (en) * | 2001-12-21 | 2002-02-06 | Rosti Wembley Ltd | Applying metallic coatings to plastics materials |
| US7125586B2 (en) * | 2003-04-11 | 2006-10-24 | Delphi Technologies, Inc. | Kinetic spray application of coatings onto covered materials |
| DE102004059716B3 (en) * | 2004-12-08 | 2006-04-06 | Siemens Ag | Cold gas spraying method uses particles which are chemical components of high temperature superconductors and are sprayed on to substrate with crystal structure corresponding to that of superconductors |
| KR100691161B1 (en) * | 2005-05-12 | 2007-03-09 | 삼성전기주식회사 | Fabrication method of field emitter electrode |
| EP1806183A1 (en) | 2006-01-10 | 2007-07-11 | Siemens Aktiengesellschaft | Nozzle arrangement and method for cold gas spraying |
| DE502006001063D1 (en) | 2006-01-10 | 2008-08-21 | Siemens Ag | Cold spraying and cold spraying with modulated gas flow |
| DE102006027754A1 (en) * | 2006-06-09 | 2007-12-13 | Siemens Ag | Arrangement and method for accelerating particles |
| DE102006029619B3 (en) * | 2006-06-23 | 2007-07-26 | Siemens Ag | Process to vary the thickness of coating applied to metal component by generation of standing, acoustic transverse surface wave during exposure to cold gas |
| KR101020042B1 (en) * | 2008-11-11 | 2011-03-09 | 주식회사 펨빅스 | Deposition apparatus of solid powder with thermal shock control units ? Temperature control method for eliminating thermal shock in solid powder spray deposition |
| KR101038187B1 (en) * | 2008-11-05 | 2011-06-01 | 주식회사 펨빅스 | Vacuum deposition apparatus with temperature control units and Method of vacuum fixing solid powder on substrates and bodies |
| KR101065271B1 (en) * | 2009-04-30 | 2011-09-20 | 주식회사 펨빅스 | Powder coating apparatus |
| JP5852131B2 (en) * | 2010-12-15 | 2016-02-03 | スルザー メテコ（ユーエス）インコーポレイテッド | Pressure liquid supply system for suspension plasma spraying |
| CN104372332B (en) * | 2013-08-13 | 2017-06-06 | 宝山钢铁股份有限公司 | Crystallizer cold spraying integral restoration method and corner treatment Special clamping device |
| CN104624428B (en) * | 2015-02-11 | 2017-01-25 | 普利瑞医疗科技（苏州）有限公司 | Full-angle ultrasonic spraying operation system |
| CN104607335B (en) * | 2015-02-11 | 2017-11-21 | 苏州微赛智能科技有限公司 | A kind of full angle ultrasound spraying operation system |
| CN109500488B (en) * | 2019-01-12 | 2024-02-13 | 锦州汉拿电机有限公司 | Ultrasonic vibration-based powder coating device and process |
| CN114875351A (en) * | 2022-05-13 | 2022-08-09 | 中国舰船研究设计中心 | Device for reducing oxidation of thermal spraying amorphous alloy coating |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5933670B2 (en) * | 1981-11-04 | 1984-08-17 | 敞 井出 | Solid thin film production device on the surface of the workpiece |
| LU85363A1 (en) * | 1984-05-15 | 1986-01-29 | Arbed | ADAPTER DEVICE FOR SOLID PARTICLE ACCELERATION NOZZLE |
| WO1991019016A1 (en) * | 1990-05-19 | 1991-12-12 | Institut Teoreticheskoi I Prikladnoi Mekhaniki Sibirskogo Otdelenia Akademii Nauk Sssr | Method and device for coating |
| RU2082823C1 (en) * | 1991-06-17 | 1997-06-27 | Московский авиационный институт им.Серго Орджоникидзе | Method of preparing coatings |
| US5779523A (en) * | 1994-03-01 | 1998-07-14 | Job Industies, Ltd. | Apparatus for and method for accelerating fluidized particulate matter |
| RU2062820C1 (en) * | 1994-05-20 | 1996-06-27 | Иосиф Сергеевич Гершман | Method of application of coatings |
| US5795626A (en) * | 1995-04-28 | 1998-08-18 | Innovative Technology Inc. | Coating or ablation applicator with a debris recovery attachment |
| RU2081202C1 (en) * | 1995-06-28 | 1997-06-10 | Научно-исследовательский институт низких температур при МАИ (Московском государственном авиационном институте-техническом университете) | Method of coating application, its versions |
| RU2100474C1 (en) * | 1996-11-18 | 1997-12-27 | Общество с ограниченной ответственностью "Обнинский центр порошкового напыления" | Apparatus for gasodynamically applying coatings of powdered materials |
-
1998
- 1998-11-05 RU RU98119848/02A patent/RU2145644C1/en not_active IP Right Cessation
-
1999
- 1999-07-29 KR KR1020017005660A patent/KR20010085999A/en not_active Application Discontinuation
- 1999-07-29 AU AU10875/00A patent/AU1087500A/en not_active Abandoned
- 1999-07-29 EP EP99954555A patent/EP1132497A4/en not_active Withdrawn
- 1999-07-29 CN CN99815192A patent/CN1332811A/en active Pending
- 1999-07-29 CA CA002349597A patent/CA2349597A1/en not_active Abandoned
- 1999-07-29 WO PCT/RU1999/000262 patent/WO2000028110A1/en not_active Application Discontinuation
Also Published As
| Publication number | Publication date |
|---|---|
| EP1132497A4 (en) | 2002-03-27 |
| WO2000028110A1 (en) | 2000-05-18 |
| KR20010085999A (en) | 2001-09-07 |
| EP1132497A1 (en) | 2001-09-12 |
| AU1087500A (en) | 2000-05-29 |
| CN1332811A (en) | 2002-01-23 |
| RU2145644C1 (en) | 2000-02-20 |
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