EP2660004B1 - Diamond surface polishing method - Google Patents

Diamond surface polishing method Download PDF

Info

Publication number
EP2660004B1
EP2660004B1 EP11852528.6A EP11852528A EP2660004B1 EP 2660004 B1 EP2660004 B1 EP 2660004B1 EP 11852528 A EP11852528 A EP 11852528A EP 2660004 B1 EP2660004 B1 EP 2660004B1
Authority
EP
European Patent Office
Prior art keywords
polishing
diamond
polishing member
metal
laser beam
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
EP11852528.6A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP2660004A4 (en
EP2660004A1 (en
Inventor
Ryozo SHIROISHI
Kenichi Takao
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Toyo Seikan Group Holdings Ltd
Original Assignee
Toyo Seikan Group Holdings Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from JP2010292145A external-priority patent/JP5817116B2/ja
Application filed by Toyo Seikan Group Holdings Ltd filed Critical Toyo Seikan Group Holdings Ltd
Publication of EP2660004A1 publication Critical patent/EP2660004A1/en
Publication of EP2660004A4 publication Critical patent/EP2660004A4/en
Application granted granted Critical
Publication of EP2660004B1 publication Critical patent/EP2660004B1/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B1/00Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B19/00Single-purpose machines or devices for particular grinding operations not covered by any other main group
    • B24B19/22Single-purpose machines or devices for particular grinding operations not covered by any other main group characterised by a special design with respect to properties of the material of non-metallic articles to be ground
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B21/00Machines or devices using grinding or polishing belts; Accessories therefor
    • B24B21/04Machines or devices using grinding or polishing belts; Accessories therefor for grinding plane surfaces
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B21/00Machines or devices using grinding or polishing belts; Accessories therefor
    • B24B21/16Machines or devices using grinding or polishing belts; Accessories therefor for grinding other surfaces of particular shape
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B7/00Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor
    • B24B7/02Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor involving a reciprocatingly-moved work-table
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B7/00Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor
    • B24B7/20Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground
    • B24B7/22Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground for grinding inorganic material, e.g. stone, ceramics, porcelain
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B9/00Machines or devices designed for grinding edges or bevels on work or for removing burrs; Accessories therefor
    • B24B9/02Machines or devices designed for grinding edges or bevels on work or for removing burrs; Accessories therefor characterised by a special design with respect to properties of materials specific to articles to be ground
    • B24B9/06Machines or devices designed for grinding edges or bevels on work or for removing burrs; Accessories therefor characterised by a special design with respect to properties of materials specific to articles to be ground of non-metallic inorganic material, e.g. stone, ceramics, porcelain
    • B24B9/16Machines or devices designed for grinding edges or bevels on work or for removing burrs; Accessories therefor characterised by a special design with respect to properties of materials specific to articles to be ground of non-metallic inorganic material, e.g. stone, ceramics, porcelain of diamonds; of jewels or the like; Diamond grinders' dops; Dop holders or tongs
    • B24B9/166Machines or devices designed for grinding edges or bevels on work or for removing burrs; Accessories therefor characterised by a special design with respect to properties of materials specific to articles to be ground of non-metallic inorganic material, e.g. stone, ceramics, porcelain of diamonds; of jewels or the like; Diamond grinders' dops; Dop holders or tongs using heat
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24DTOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • B24D3/02Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
    • B24D3/04Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic
    • B24D3/06Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic metallic or mixture of metals with ceramic materials, e.g. hard metals, "cermets", cements

Definitions

  • This invention relates to a method of polishing the diamond-surface and, more specifically, to a method of polishing the various kinds of diamond product-surface.
  • the diamond which is a crystal of carbon has been used for a variety of applications owing to its very high hardness, excellent resistance against abrasion as well as excellent slipping property, heat conductivity and high refractive index.
  • the tools for cutting such as cutting tool, end mill and file, metal molds for plastic machining, such as punch and dies, sliding members such as valve lifter and bearing, heat-radiating members such as heat sink, electronic circuit boards and optical parts such as lens and window.
  • these diamond products In order for their properties to be exhibited to a sufficient degree, these diamond products must have the diamond-surface polished to assume smooth surface.
  • the diamond-surface had so far been mechanically polished by using grains or a grind stone of diamond requiring extended periods of time. Besides, since both of them are abraded, there occurred such problems as short life of the tool and not being suited for polishing rugged three-dimensional surfaces. In an effort to improving the above defects, therefore, various kinds of polishing methods have now been proposed.
  • a patent document 1 proposes a polishing method which conducts the polishing by using a polishing member constituted by a metal that easily reacts with carbon in the diamond crystals, applying ultrasonic waves onto the polishing member, and pushing the polishing member onto the surfaces of the diamond while the polishing member is undergoing ultrasonic oscillation.
  • a polishing member constituted by a metal that easily reacts with carbon in the diamond crystals
  • the metal that easily reacts with carbon include a ⁇ -Fe-containing stainless steel, titanium (Ti), zirconium (Zr) and tantalum (Ta).
  • a patent document 2 proposes a polishing method by using, as a grind stone, an intermetallic compound of at least one metal element selected from the group consisting of Al, Cr, Mn, Fe, Co and Ni and at least one metal element selected from the group consisting of Zr, Hf, V, Nb, MO, Ta and W, and pushing the grind stone onto the diamond-surface that is moving relative thereto while, as required, heating the grind stone at 100 to 800°C.
  • a patent document 3 proposes a method of polishing the diamond-surface by focusing the laser beam on the diamond-surface.
  • a patent document 4 proposes a method of polishing a diamond film by sliding a metal and the diamond relative to each other at a point where the two are contacting to each other while continuously varying the temperature over a range of 700°C to 1000°C at the portion where the metal and the diamond are contacting to each other.
  • JP H08 175826 proposes a method for polishing a diamond film by preforming a metallic thin film on a diamond surface, then bringing a metallic tool into contact with the metallic thin film and polishing.
  • Patent Documents
  • Patent document 1 JP-A-2005-231022 ; Patent document 2: JP-A-2001-198833 ; Patent document 3: JP-A-6-170571 ; Patent document 4: JP-A-7-314299
  • the method proposed by the patent document 1 executes the polishing by causing the metal constituting the polishing member to undergo chemical reaction with carbon on the diamond-surface by utilizing the heat of friction produced by ultrasonic oscillation.
  • the temperature must be controlled relying on the frequency and the pushing force involving great difficulty, and it is not easy to conduct the polishing maintaining stability and constant efficiency.
  • the polishing member Upon utilizing the heat of friction, further, the energy efficiency is low and to elevate the temperature, the polishing member must be pushed onto the diamond-surface with a considerable pushing force. Besides, the hardness of the metal constituting the polishing member is very lower than that of the diamond. Accordingly, the polishing member abrades conspicuously and has only a short life.
  • the polishing machine and, specifically, the surrounding of the polishing member must have an increased toughness resulting in an increase in the size of the apparatus.
  • the polishing is carried out by using a grind stone that contains as grains a very hard intermetallic compound.
  • use of the special intermetallic compound drives up the cost strikingly.
  • the polishing is conducted by pushing the hard intermetallic compound (hardness Hv of 500 to 1000) onto the diamond-surface, abraded powder generates much due to the abrasion of grains.
  • the surfaces of the powder are highly and chemically active and, therefore, the abraded powder that is generated much may cause ignition and explosion.
  • the mechanical polishing by pushing the grind stone onto the diamond-surface needs the apparatus that tends to become bulky.
  • the polishing is conducted by gasifying carbon in the diamond-surface by being heated by using a laser beam.
  • the laser beam must be emitted so as to be focused on a convex portion on the diamond-surface, and it is very difficult to control the emission of the laser beam. Therefore, there remains a problem in that a very extended period of time is required for polishing a material having an area that is wide to some extent (e.g., several tens of square centimeters or more).
  • the polishing is conducted by sliding the metal and the diamond relative to each other at a portion where they are contacting to each other while continuously varying the temperature over a range of 700°C to 1000°C at the portion where they are contacting to each other.
  • heating is conducted by a heater and the temperature cannot be instantaneously varied imposing limitation on adjusting the amount of polishing.
  • the polishing member is formed in a spherical shape to prevent deviated abrasion, and is rotated at a low speed.
  • an object of the present invention to provide a method of polishing the diamond-surface which generates less abraded powder, enables the polishing member to maintain an extended life and to be easily controlled, makes it possible to obtain the surface of a high degree of smoothness, and can be easily applied to polishing rugged three-dimensional surface, too.
  • Another object of the present invention is to provide a method of polishing the diamond-surface that is capable of conducting the polishing without using an expensive material obtained by a special production method, such as intermetallic compound but using a polishing member formed by using an inexpensive simple metal.
  • the metal that easily reacts with carbon is a metal having a temperature region in which a change in the Gibb's free energy ( ⁇ G) in the carbide-forming reaction assumes a negative sign and, particularly preferably, is a metal of which the amount of change in the free energy ( ⁇ G) in the carbide-forming reaction is not more than -20 kcal/mol in a temperature region that does not exceed the temperature (750 to 850°C) at which the diamond carbonizes.
  • Amounts of change in the Gibb's free energy of various metals in the carbide-forming reaction have been known as described, for example, in the Metals Data Book, 4th Edition (Edited by The Japan Institute of Metals, Maruzen Co. ).
  • the carburizing metal is a metal into which carbon can be diffused and permeated from the surface thereof.
  • the polishing is conducted by rubbing the diamond-surface with the polishing member-surface.
  • the polishing member-surface is formed of a metal that easily reacts with carbon or of a carburizing metal, and the polishing member or the diamond-surface is heated prior to polishing with the polishing member.
  • carbon on the diamond-surface reacts with the easily reacting metal that is forming the polishing member-surface, or diffuses and permeates in the layer of the carburizing metal-surface.
  • the diamond-surface is robbed of carbon and is effectively polished.
  • the polishing member that is used has a linear, belt-like or rod-like shape, and the polishing is conducted while continuously or intermittently varying the polishing member-surface formed of the above-mentioned metal material. That is, since the diamond-surface is slide-rubbed while varying the contacting portion, the reaction (reaction of the easily reacting metal with carbon on the diamond-surface, or diffusion and permeation of carbon) does not reach the saturated state, the surface pressure is not changed by abrasion, and the process continues maintaining stability at all times. Accordingly, the polishing can be continued maintaining stability for extended periods of time.
  • the metal that forms the polishing member-surface and easily reacts with carbon it is desired to use Zr, Ta, Ti or Al as the metal that forms the polishing member-surface and easily reacts with carbon.
  • These metals are all soft metals and have Vickers' hardnesses (Hv) which are all not higher than 200 and are not only very lower than that of the diamond-surface but also considerably lower than the hardness of 500 to 1000 of the grind stone of an intermetallic compound used in the above patent document 2. Since the diamond-surface is slide-rubbed by the metal of such a low hardness so as to be polished, generation of the abraded powder can be effectively suppressed as compared to when a highly hard metal or metal compound is used making it possible to lengthen the life of the polishing member, which is a great advantage of the present invention.
  • Fe, Ni or Co as the carburizing metal that forms the polishing member-surface.
  • These metals have a property that permits carbon to diffuse and permeate therein from the surface thereof.
  • the diamond-surface is heated by the laser beam-irradiation prior to polishing and to polish the laser beam-irradiated portion by using the polishing member.
  • laser beam-irradiation is simply for heating at such a temperature at which the metal of the polishing member-surface reacts with carbon or at such a temperature at which the polishing member-surface is carburized with carbon on the diamond-surface. It should be noted that the laser beam-irradiation is not for vaporizing or volatilizing the carbon on the diamond-surface.
  • the diamond-surface in heating the diamond-surface by the laser beam-irradiation, the diamond-surface is locally heated, i.e., a spot on the surface is heated instantaneously. Therefore, in polishing a diamond film formed on a predetermined substrate, the diamond film is not damaged by a difference in the thermal expansion between the diamond film and the substrate . Besides, since the heating is locally conducted, the energy can be utilized very highly efficiently.
  • the intensity of the laser beam can be varied instantaneously making it possible to adjust the amount of polishing by varying the temperature of heating.
  • the surface property is monitored and the data are fed back to improve the evenness of the surface or to form fine ruggedness on the surface.
  • the heating further accelerates the reaction of carbon on the diamond-surface with the metal forming the polishing member-surface or further accelerates carburization of the metal surface contributing to conducting the polishing efficiently and in a short period of time.
  • the polishing member is formed using an existing simple metal instead of using a special compound such as intermetallic compound offering advantage from the standpoint of cost, too.
  • the present invention is to polish a workpiece 1 that has a diamond-surface 1a.
  • the workpiece 1 may have any shape suited for the use so far as it has the diamond-surface 1a of a single crystal, polycrystals or a thin film.
  • the diamond-surface 1a of the workpiece 1 is polished by using a polishing device 3 equipped with a polishing member 3a that rubs the diamond-surface 1a sliding on it.
  • the surface 1a is irradiated with a laser beam 5 prior to polishing and after having been irradiated, the portion irradiated with the laser beam 5 is polished by the polishing device 3.
  • the polishing device 3 is equipped with the polishing member 3a that rubs the diamond-surface 1a sliding on it, the polishing member 3a being formed of a metal that easily reacts with carbon or of a carburizing metal.
  • the metal that easily reacts with carbon is a metal having a temperature region in which a change in the Gibb's free energy ( ⁇ G) in the carbide-forming reaction assumes a negative sign
  • its examples include Zr, Ta, Ti, W, Nb and Al.
  • Zr, Ta, Ti, and Al are preferred.
  • these metals have surface hardnesses Hv (Vickers' hardnesses) which are very low; e.g., Ta being about 100 to 150, Zr being about 120 to 200, Ti being about 100 to 200, and Al being about 15 to 50.
  • Zr, Ta and Ti are most desired. These metals have amounts of change in the Gibb's free energy ( ⁇ G) in the reaction for forming carbide (ZrC, TaC, TiC) of not more than -20 kcal/mol and, specifically, as small as about -30 to -45 kcal/mol in a temperature region that does not exceed the temperature (750 to 850°C) at which the diamond carbonizes. Due to the slide-rubbing after heated by the irradiation with the laser beam 5, therefore, the metal very easily reacts with carbon on the diamond-surface 1a and effectively polishes the diamond-surface 1a. For example, as demonstrated by the experimental results (see Fig.
  • a rough surface of a roughness Rz (maximum height) of about 1.5 ⁇ m can be polished into a smooth surface of a roughness of about 0.8 ⁇ m in a short period of time.
  • the carburizing metal there can be exemplified Fe, Ni and Co. Among them, it is desired to use Ni for forming the surface of the polishing member 3a. Namely, when the polishing member 3a having the carburizing metal-surface is used, carbon atoms on the diamond-surface 1a diffuse in the surface of the polishing member 3a at the time of polishing with the polishing member 3a, and the diamond-surface can be effectively polished.
  • Polishing with the polishing member 3a is conducted by rubbing the portion irradiated with the laser beam by using the polishing member 3a that slides thereon; i.e., no large pushing force is necessary for the slide-rubbing.
  • an appropriate pushing force may differ depending on the shape and material of the polishing member, it has been confirmed that the polishing can be conducted with a pushing force of about 5 N (0.5 kgf).
  • the true contact area increases with an increase in the pushing force, and the polishing tends to accelerate. Therefore, the pushing force may be suitably set depending on the shape of the workpiece, shape and material of the polishing member corresponding thereto, and rigidity of the apparatus.
  • the present invention does not require such a pushing force that causes an end of the polishing member to be greatly deformed. Therefore, the polishing member and the holding fitting can be realized in small sizes offering advantage from the standpoint of polishing the workpieces that have complex shapes and holes of small diameters therein.
  • the diamond-surface 1a is locally heated by being irradiated with the laser beam 5 so that the metal forming the surface of the polishing member 3a easily reacts with carbon, and the degree of heating is determined by the density of the laser irradiation energy and the energy absorbency of the diamond.
  • the laser output, width of irradiation (spot diameter) and rate of working are suitably set based on the energy absorbency of the diamond to the laser source used for the polishing.
  • Fig. 4 shows a relationship between the density of the energy of when a 10 ⁇ m-thick diamond coated on a super hard alloy is irradiated with a carbon dioxide gas laser and the temperature on the diamond-surface though it may really differ depending on the shape, thickness and the laser species.
  • the temperature was measured by using a radiation thermometer (FTK9-R220A-2.5B11) manufactured by Japan Sensor Co.
  • the temperature increases with an increase in the density of the irradiated energy. If the density of the irradiated energy increases too much, the diamond is carbonized at around 750 to 850°C, and the temperature does not rise any more.
  • the radiation conditions such as the density of the laser beam irradiation energy must be so set that the diamond-surface 1a is heated to a temperature range that does not exceed the temperature (750 to 850°C) at which the diamond carbonizes.
  • the temperature range is not lower than 200°C and, specifically, is from 220°C to 800°C and when a carburizing metal is used, the temperature range is not lower than 600°C and, specifically, is from 700°C to 800°C.
  • the irradiation condition may then be so set that the diamond-surface is heated at a temperature within the above range but does not exceed the melting point of the metal used for the polishing member 3a.
  • a variety of kinds of laser sources have been known for emitting the laser beam 5.
  • the level of heating is so low that the laser source is not limited, and any known laser can be used.
  • solid lasers have been widely used, such as YAG and fiber laser. According to the present invention, however, it is also allowable to use gas lasers such as carbon dioxide gas laser and excimer laser in addition to the solid lasers.
  • the width of irradiation (spot diameter) of the laser beam 5 it is desired that it is close to the width over which the polishing member 3a comes in contact with the diamond from the standpoint of energy efficiency of the laser beam and the efficiency of polishing. For example, if the width of irradiation is very smaller than the width of contact between the two, the polishing does not proceed on the portions where the temperature is low (portions that are not irradiated) and, as a result, an extended period of time is required for the polishing.
  • the width of irradiation is set to be too wide, on the other hand, then the portions that need not be heated (that are not polished) are heated resulting in a loss of energy and making it necessary to undesirably increase the output of the laser beam or to decrease the rate of machining.
  • the width in which the polishing member 3a comes in contact with the diamond can be roughly calculated in compliance with the widely known Hertz's law.
  • a portion is irradiated with the laser beam 5 and, thereafter, the irradiated portion is polished with the polishing member 3a.
  • the timing of polishing is that the surface of the irradiated portion is still maintained at about a temperature at which the metal of the polishing member 3a undergoes the reaction (or carburization) with carbon on the diamond-surface 1a.
  • the diamond since the diamond has a very high thermal conductivity (tends to be quickly cooled), it is desired to bring the irradiated portion as close to the polishing member 3a as possible so far as it is permitted by the installation space to shorten the time.
  • the present invention it is also allowable to heat the diamond-surface 1a by a known heating means such as various kinds of heaters, hot air, heating by flowing an electric current through a resistor, induction heating or high-energy beam instead of irradiation with the laser beam under a condition that the diamond is not carbonized.
  • a known heating means such as various kinds of heaters, hot air, heating by flowing an electric current through a resistor, induction heating or high-energy beam instead of irradiation with the laser beam under a condition that the diamond is not carbonized.
  • a known heating means such as various kinds of heaters, hot air, heating by flowing an electric current through a resistor, induction heating or high-energy beam instead of irradiation with the laser beam under a condition that the diamond is not carbonized.
  • a unit for irradiating the laser beam 5 and the polishing member 3a of the polishing device 3 are arranged in concentric, and the diamond-surface is polished by being rubbed with the polishing member 3a that slides on it while being irradiated with the laser beam 5 in a state where the workpiece 1 is being rotated. Further, the polishing device 3 (polishing member 3a) and the source of irradiating the laser beam 5 are caused to move intermittently or continuously in the radial direction of the diamond-surface 1 to polish the whole diamond-surface 1a.
  • polishing device 3 polishing member 3a
  • the source of irradiating the laser beam 5 instead of rotating the workpiece 1. It is, however, a generally accepted practice to rotate the workpiece 1 since it does not cause the apparatus to become bulky. If the polishing cannot be accomplished to a sufficient degree by the polishing of one time only, then the above-mentioned operation may be repeated a plurality of times to further continue the polishing.
  • the workpiece 1 or the polishing device 3 (polishing member 3a) and the source of irradiating the laser beam 5 may be caused to linearly slide to conduct the polishing.
  • a workpiece 35 is fixed on a table 31 that can slide on a rail 30, a laser source 37 is arranged over the table 31, and a polishing device 39 is provided in parallel with the laser source 37.
  • the polishing device 39 has a polishing member 40 attached to the lower end thereof.
  • the diamond-surface of the workpiece 35 is polished by being rubbed with the polishing member 40 that slides on it while being irradiated with a laser beam 37a as the table 31 moves a round trip. It is also allowable to place the workpiece 35 on a support member 33 and to fix the support member 33 onto the table 31.
  • the polishing member 3a has a linear shape (wire shape), belt-like shape or rod-like shape and, further, that the contacting portion of the polishing member is varied continuously or intermittently while conducting the polishing.
  • the polishing member-surface (contacting portion) that is in contact with the diamond-surface varies at all times, enabling the carbon atoms to react with the metal or enabling the carbon atoms to diffuse and permeate efficiently at all times and permitting the polishing to be stably conducted at all times without any change in the surface pressure that is caused by the abrasion.
  • the polishing can be conducted maintaining stability over extended periods of time.
  • Fig. 3 shows examples of the polishing members 3a of various shapes used in the invention.
  • an endless wire 15 is wound round a pulley 13 that is held by a predetermined support member 10.
  • the wire 15 serves as the polishing member 3a that is made from a metal that easily reacts with carbon (or is made from a carburizing metal).
  • an endless belt 19 is wound round a roller 17 held by the support member 10 and serves as the polishing member 3a.
  • a rod 21 is penetrating through the sleeve-like support member 10 and its lower end surface rubs the diamond-surface 1a sliding thereon. That is, the rod 21 serves as the polishing member 3a.
  • the endless wire 15 or the endless belt 19 polishes the diamond-surface 1a while continuously or intermittently varying its rubbing surface. Further, the rod 21 is continuously or intermittently delivered so as to conduct the polishing.
  • the surface thereof that contacts to the diamond is not worn out through the polishing and is not abraded. Therefore, the surface pressure does not change, and the polishing can be continued maintaining stability over extended periods of time.
  • the polishing member 3a has a spherical shape as described in, for example, the patent document 4, the same effect can be expected by rotating the sphere. If the axis of rotation is fixed, however, the polishing member can be used for only one turn. To make the axis of rotation free, however, the apparatus becomes complex.
  • the slide-rubbing surface of the polishing member 3a comes into point contact or line contact with the diamond-surface 1a to maintain a high polishing efficiency as well as to conduct the polishing with a new surface at all times. Therefore, the surface pressure is not changed by the abrasion, and the polishing can be continued maintaining stability over extended periods of time.
  • the polishing member 3a is heated in advance to attain a synergistic effect. This makes it possible to further elevate the temperature on the diamond-surface and to accelerate the reaction of carbon in the diamond-surface 1a with the metal on the surface of the polishing member 3a or to accelerate the carburization of the metal surface (diffusion of carbon). As a result, the output of the laser beam can be maintained low.
  • the diamond-surface can be polished maintaining a certain degree of efficiency relying only on the slide-rubbing with the polishing member 3a without being irradiated with the laser beam.
  • the above heating is effected such that the diamond-surface 1a or the surface of the polishing member 3a or the two are heated at a temperature of not lower than 200°C and, specifically, not lower than 220°C but that the temperature at which the diamond carbonizes is not exceeded.
  • heating means as various kinds of heaters, hot air, heating by flowing an electric current through a resistor, induction heating or high-energy beam depending upon the form of the polishing member 3a.
  • the above heating means can also be used as means for heating the diamond-surface instead of irradiating the laser beam.
  • the above polishing method of the present invention makes it possible to conduct the polishing without using a polishing member made of a particularly expensive compound but using a polishing member made of a simple metal, as well as to easily control the polishing. It is, therefore, allowed to effectively polish not only flat surfaces but also rugged three-dimensional surface and curved surface lending the polishing method well for polishing the workpieces having diamond surfaces of various shapes.
  • the polishing may be conducted while blowing an oxygen gas or the like gas.
  • the polishing may be conducted while effecting the evacuation or continuously or intermittently blowing the high-pressure air or a very small amount of washing solution to remove metal carbide or foreign matter produced by the polishing.
  • the surface roughness was measured by a method described below.
  • Shape flat plate measuring 13 mm x 13 mm (5 mm thick)
  • Substrate cemented carbide
  • Thickness of diamond 10 ⁇ m
  • Maximum height Rz 1.5 ⁇ m (diamond-surface)
  • Laser carbon dioxide gas laser
  • Evolution 100 W manufactured by Synrad Co.:
  • a Ta wire having a circular shape in cross section and a diameter of 1 mm was attached to the above polish tester (see Fig. 3(a) ), and a gap was set to be 2 mm between the position on where the laser is irradiated and the position where the polishing member comes in contact with the test piece.
  • the polishing member (Ta wire) was pushed onto the surface of the test piece with a load of 10 N, and the test piece was polished by being moved at 72 m/min while being irradiated with the laser beam. After every end of the polishing, the test piece was moved by 0.005 mm perpendicularly to the direction of slide-rubbing. This operation was repeated a plurality of number of times (about 100 times) to execute a planar polishing test.
  • the contacting portion of the wire was changed every after 5 times of slide-rubbing of the same portion of the test piece. Further, a maximum height Rz of the polished portion was measured. The results were as shown in Fig. 5 . The maximum height Rz decreased with an increase in the number of times of the slide-rubbing, from which it was confirmed that the polishing was conducted.
  • Table 1 shows the experimental conditions and the results of the following Experiments. Further, Fig. 5 shows relationships between the number of times of slide-rubbing and the maximum heights Rz like those of Experiment No. 1.
  • the polishing test was conducted in quite the same manner as in Experiment 1 but without irradiated with the laser beam.
  • the polishing test was conducted in quite the same manner as in Experiment 1 but decreasing the intensity of the laser beam down to 50 W.
  • the polishing test was conducted in quite the same manner as in Experiment 1 but without effecting the slide-rubbing with the polishing member.
  • the polishing test was conducted in quite the same manner as in Experiment 1 but increasing the pushing force to 20 N.
  • polishing tests were conducted in quite the same manner as in Experiment 1 but changing the polishing member to Ti, Zr and Al. As a result, it was confirmed that the polishing proceeded faster when Ti and Zr were used than when Ta was used, but the polishing did not much proceed when Al was used.
  • Table 2 shows the experimental conditions and the results of the following Experiments.
  • Fig. 6 shows relationships between the number of times of slide-rubbing and the maximum heights Rz like those of Experiment No. 1.
  • the polishing test was conducted in quite the same manner as in Experiment 1 but changing the movement of the test piece as described below, without irradiating the laser beam and heating the polishing member at 700°C by using a heater.
  • Test piece moving speed 18 m/min
  • Test piece slide-rub movement in the vertical direction 0.025 mm/rev
  • the polishing test was conducted in quite the same manner as in Experiment 9 but heating the polishing member at 800°C.
  • the polishing test was conducted in quite the same manner as in Experiment 9 but heating the polishing member at 500°C.
  • the polishing test was conducted in quite the same manner as in Experiment 9 but changing the polishing member to Fe.
  • the polishing test was conducted in quite the same manner as in Experiment 12 but heating the polishing member at 500°C.
  • the polishing test was conducted in quite the same manner as in Experiment 1 but changing the polishing member to Ni.
  • Fig. 7 shows relationships between the number of times of slide-rubbing and the maximum heights Rz like those of Experiment No. 1, and Fig. 8 shows relationships between the distances in the direction of outer diameter from the polishing start point and the maximum heights Rz after 50 times of slide-rubbing.
  • the polishing test was conducted in quite the same manner as in Experiment 1 but changing the conditions as described below, moving the polishing member from the inner diameter toward the outer diameter at a rate of 0.025 mm/rev while rotating the test piece, ending the polishing when the end point is reached, changing the contacting portion of the wire and, thereafter, starting again the polishing from the inner diameter.
  • Shape ring having an inner diameter of 33 mm and an outer diameter of 65 mm (12 mm thick)
  • Substrate cemented carbide
  • Thickness of diamond 20 ⁇ m
  • Maximum height Rz 1.8 ⁇ m (diamond-surface)
  • Circumferential speed 24 m/min
  • Load on polishing member 20 N Gap between the position on where the laser is irradiated and the position where the polishing member contacts to the test piece: 0.7 mm
  • a maximum height Rz of the polished portion was measured on the same portion of the test piece every after 5 times of slide-rubbing.
  • the polishing test was conducted in quite the same manner as in Experiment 13 but continuously feeding the Ta wire at 0.5 mm/s and changing the contacting portion.
  • Table 1 Experiment Polishing member Laser specifies Laser intensity W Irrad. Width mm Irrad. Time s Pushing force N Testing rate m/min Results 1 Ta carbon dioxide 100 ⁇ 0.2 0.00018 10 72 ⁇ 2 Ta none - - - 10 72 ⁇ 3 Ta carbon dioxide 50 ⁇ 0.2 0.00018 10 72 ⁇ 4 none carbon dioxide 100 ⁇ 0.2 0.00018 - 72 ⁇ 5 Ta carbon dioxide 100 ⁇ 0.2 0.00018 20 72 ⁇ 6 Ti carbon dioxide 100 ⁇ 0.2 0.00018 10 72 ⁇ 7 Zr carbon dioxide 100 ⁇ 0.2 0.00018 10 72 ⁇ 8 Al carbon dioxide 100 ⁇ 0.2 0.00018 10 72 ⁇ Table 2 Experiment Polishing member Heating temp. W Pushing force N Testing rate m/min Results of tests 9 Ta 700 10 18 ⁇ 10 Ta 800 10 18 ⁇ 11 Ta 500 10 18 ⁇ 12 Fe 700 10 18 ⁇ 13 Fe 500 10 18 ⁇ 14 Ni 700 10

Landscapes

  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Grinding And Polishing Of Tertiary Curved Surfaces And Surfaces With Complex Shapes (AREA)
  • Polishing Bodies And Polishing Tools (AREA)
  • Laser Beam Processing (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Grinding-Machine Dressing And Accessory Apparatuses (AREA)
EP11852528.6A 2010-12-28 2011-07-26 Diamond surface polishing method Active EP2660004B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2010292145A JP5817116B2 (ja) 2010-02-03 2010-12-28 ダイヤモンド表面の研磨方法
PCT/JP2011/066952 WO2012090540A1 (ja) 2010-12-28 2011-07-26 ダイヤモンド表面の研磨方法

Publications (3)

Publication Number Publication Date
EP2660004A1 EP2660004A1 (en) 2013-11-06
EP2660004A4 EP2660004A4 (en) 2017-11-22
EP2660004B1 true EP2660004B1 (en) 2021-07-14

Family

ID=46384055

Family Applications (1)

Application Number Title Priority Date Filing Date
EP11852528.6A Active EP2660004B1 (en) 2010-12-28 2011-07-26 Diamond surface polishing method

Country Status (5)

Country Link
EP (1) EP2660004B1 (zh)
KR (2) KR20130092606A (zh)
CN (1) CN103282157B (zh)
BR (1) BR112013015008B1 (zh)
WO (1) WO2012090540A1 (zh)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102013218446A1 (de) * 2013-09-13 2015-03-19 Cemecon Ag Werkzeug sowie Verfahren zum Zerspanen von faserverstärktenMaterialien
JP6488775B2 (ja) * 2015-03-09 2019-03-27 東洋製罐グループホールディングス株式会社 ダイヤモンド表面の研磨方法およびそれを実施する装置
CN107457616B (zh) * 2017-09-07 2019-07-26 哈尔滨工业大学 一种基于纳米镍粉的金刚石晶体表面机械化学抛光方法
CN110774153B (zh) * 2019-10-23 2022-02-08 华侨大学 一种大尺寸单晶金刚石的抛光方法
CN110774118B (zh) * 2019-10-23 2021-04-30 华侨大学 一种大尺寸单晶金刚石的磨削方法
CN114012512B (zh) * 2021-10-29 2022-08-16 哈尔滨工业大学 一种基于激光加热、水浴加热、化学作用共同辅助的小球头磁流变抛光方法
CN115229647B (zh) * 2022-07-20 2023-08-29 华侨大学 一种飞秒激光辅助抛光金刚石的装置及其抛光方法

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5858190B2 (ja) * 1981-11-10 1983-12-23 株式会社東芝 ダイヤモンド研摩方法
JPH0775818B2 (ja) * 1986-08-08 1995-08-16 株式会社東芝 ダイヤモンド部材の加工方法
JP3096943B2 (ja) 1992-12-07 2000-10-10 鋼鈑工業株式会社 ダイヤモンドのレーザ研磨方法および装置ならびにそれを利用したダイヤモンド製品
JP3144752B2 (ja) 1994-05-24 2001-03-12 キヤノン株式会社 ダイヤモンド膜の研磨方法
JPH08175826A (ja) * 1994-12-22 1996-07-09 Canon Inc ダイヤモンド膜の研磨方法
JPH09117852A (ja) * 1995-10-26 1997-05-06 Dainippon Printing Co Ltd 微細パターン部分研磨装置
JP3717046B2 (ja) * 2000-01-21 2005-11-16 独立行政法人産業技術総合研究所 ダイヤモンド研磨用砥石及びダイヤモンド研磨方法並びにダイヤモンド研磨用複合砥石
DE60018634T2 (de) * 1999-05-12 2005-08-04 National Institute Of Advanced Industrial Science And Technology Schleif- und Polierwerkzeug für Diamant, Verfahren zum Polieren von Diamant und polierter Diamant, und somit erhaltener Einkristalldiamant und gesintertes Diamantpresswerkstück
CN2561551Y (zh) * 2002-08-23 2003-07-23 郑州磨料磨具磨削研究所 金刚石锯片砂带抛光机
JP4222515B2 (ja) * 2004-01-22 2009-02-12 地方独立行政法人 東京都立産業技術研究センター ダイヤモンドの研磨方法と装置
CN101310923A (zh) * 2007-05-23 2008-11-26 房丰洲 一种新型的局部加热的金刚石研磨法

Also Published As

Publication number Publication date
WO2012090540A1 (ja) 2012-07-05
KR20130092606A (ko) 2013-08-20
EP2660004A4 (en) 2017-11-22
EP2660004A1 (en) 2013-11-06
BR112013015008B1 (pt) 2021-04-13
KR20150104214A (ko) 2015-09-14
CN103282157B (zh) 2016-05-18
BR112013015008A2 (pt) 2016-08-09
KR101785183B1 (ko) 2017-10-12
CN103282157A (zh) 2013-09-04

Similar Documents

Publication Publication Date Title
US9149901B2 (en) Method of polishing the diamond-surface
EP2660004B1 (en) Diamond surface polishing method
KR101552895B1 (ko) 워크의 절단방법
JP5185103B2 (ja) 変態を起こす金属の表面硬化処理方法
Tsai et al. Evaluation research of polishing methods for large area diamond films produced by chemical vapor deposition
JP2007230807A (ja) ダイヤモンド製品の製造方法
CN106078519A (zh) 一种采用金刚石纤维微切削进行砂轮形貌重构的方法
EP2040879A1 (en) Method and apparatus for polishing diamond and diamond composites
CN113355491A (zh) 一种减小激光淬火搭接软带宽度的激光淬火工艺
JP6481416B2 (ja) ダイヤモンド表面の研磨方法
JP6487644B2 (ja) 研磨装置
Chen et al. Dynamic friction polishing of diamond utilizing high reactive metallic tools
RU2734612C1 (ru) Способ полирования поверхности поликристаллического алмазного покрытия деталей
CN114340830A (zh) 刮削加工装置和刮削加工方法
JP2016055302A (ja) レーザフォーミング加工方法およびレーザフォーミング加工装置
JP2003117784A (ja) ワーク研削装置およびワーク研削方法
JP2007290052A (ja) 表面加工方法
Yakubovsky et al. Influence of laser beam treatment modes on the parameters of thermal impact zones and tribotechnical characteristics of steels
JP2016097466A (ja) 硬質表面の研磨方法
RU2107739C1 (ru) Способ поверхностной закалки и устройство для его осуществления
JP2020037718A (ja) めっき被膜の表面改質方法及び装置
CN105324182A (zh) 用于改善耐磨性的激光辅助间隙合金化
JP2021171811A (ja) 表面加工装置及び表面加工方法
JPH049425A (ja) 表面処理方法及びその装置
KR20040057337A (ko) 롤러의 표면 경화 열처리 방법

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: REQUEST FOR EXAMINATION WAS MADE

17P Request for examination filed

Effective date: 20130531

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

DAX Request for extension of the european patent (deleted)
RA4 Supplementary search report drawn up and despatched (corrected)

Effective date: 20171025

RIC1 Information provided on ipc code assigned before grant

Ipc: B24B 9/16 20060101ALI20171019BHEP

Ipc: B24B 1/00 20060101AFI20171019BHEP

Ipc: B24B 7/02 20060101ALI20171019BHEP

Ipc: B24B 21/04 20060101ALI20171019BHEP

Ipc: B24D 3/06 20060101ALI20171019BHEP

REG Reference to a national code

Ref country code: DE

Ref legal event code: R079

Ref document number: 602011071381

Country of ref document: DE

Free format text: PREVIOUS MAIN CLASS: B24B0001000000

Ipc: B24B0019220000

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: GRANT OF PATENT IS INTENDED

RIC1 Information provided on ipc code assigned before grant

Ipc: B24B 19/22 20060101AFI20210330BHEP

Ipc: B24B 21/04 20060101ALI20210330BHEP

Ipc: B24B 21/16 20060101ALI20210330BHEP

Ipc: B24B 1/00 20060101ALI20210330BHEP

Ipc: B24B 7/22 20060101ALI20210330BHEP

Ipc: B24D 3/06 20060101ALI20210330BHEP

Ipc: B24B 7/02 20060101ALI20210330BHEP

Ipc: B24B 9/16 20060101ALI20210330BHEP

INTG Intention to grant announced

Effective date: 20210429

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE PATENT HAS BEEN GRANTED

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: DE

Ref legal event code: R096

Ref document number: 602011071381

Country of ref document: DE

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: AT

Ref legal event code: REF

Ref document number: 1410269

Country of ref document: AT

Kind code of ref document: T

Effective date: 20210815

REG Reference to a national code

Ref country code: LT

Ref legal event code: MG9D

REG Reference to a national code

Ref country code: NL

Ref legal event code: MP

Effective date: 20210714

REG Reference to a national code

Ref country code: AT

Ref legal event code: MK05

Ref document number: 1410269

Country of ref document: AT

Kind code of ref document: T

Effective date: 20210714

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: HR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

Ref country code: AT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

Ref country code: BG

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211014

Ref country code: LT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

Ref country code: NO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211014

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211115

Ref country code: RS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

Ref country code: ES

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: PL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

Ref country code: LV

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20211015

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

REG Reference to a national code

Ref country code: BE

Ref legal event code: MM

Effective date: 20210731

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 602011071381

Country of ref document: DE

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20210731

Ref country code: DK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20210731

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SM

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

Ref country code: SK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

Ref country code: RO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

Ref country code: MC

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20210726

Ref country code: EE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

Ref country code: CZ

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

Ref country code: AL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

26N No opposition filed

Effective date: 20220419

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

Ref country code: IE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20210726

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20210731

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: HU

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT; INVALID AB INITIO

Effective date: 20110726

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20230720

Year of fee payment: 13

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20230725

Year of fee payment: 13

Ref country code: DE

Payment date: 20230719

Year of fee payment: 13

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210714