WO2004106587A1 - 放電表面処理用電極、放電表面処理用電極の製造方法、放電表面処理装置および放電表面処理方法 - Google Patents
放電表面処理用電極、放電表面処理用電極の製造方法、放電表面処理装置および放電表面処理方法 Download PDFInfo
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- WO2004106587A1 WO2004106587A1 PCT/JP2004/000742 JP2004000742W WO2004106587A1 WO 2004106587 A1 WO2004106587 A1 WO 2004106587A1 JP 2004000742 W JP2004000742 W JP 2004000742W WO 2004106587 A1 WO2004106587 A1 WO 2004106587A1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0433—Nickel- or cobalt-based alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
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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
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/044—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by jet milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
Definitions
- Discharge surface treatment electrode Discharge surface treatment electrode manufacturing method, Discharge surface treatment device, Discharge surface treatment method Technical field
- a pulse-like discharge is generated between an electrode for discharge surface treatment composed of a compact formed by compression-molding a powder of a metal, a metal compound or a ceramic, and a pulsed discharge.
- the present invention relates to a discharge surface treatment electrode used in a discharge surface treatment for forming a film made of an electrode material or a substance in which the electrode material reacts with discharge energy on a workpiece surface, and a method of manufacturing the same.
- the present invention also relates to a discharge surface treatment apparatus and a discharge surface treatment method using the discharge surface treatment electrode. Background technology ''
- FIG. 1 is a diagram schematically showing the structure of a turbine blade of an aircraft gas turbine engine. As shown in this figure, a plurality of turbine blades 100 are fixed in contact with each other, and the turbine blade 100 is configured to rotate around an axis (not shown). These contact portions P between the turbine blades 100 are violently rubbed or hit in a high temperature environment when the turbine blades 100 rotate.
- thermal spraying refers to a processing method in which powder with a particle size of about 50 m is ejected from a nozzle, a part of the powder is melted at the nozzle outlet, and a film is formed on the surface of a loe (hereinafter referred to as a workpiece).
- Welding means that an arc is generated between the electrode and the workpiece. ⁇ The heat of the arc melts part of the electrode and forms droplets, which are transferred to the surface of the workpiece to form a coating. Processing method.
- welding is a method in which heat concentrates on the work, so when processing materials with a small thickness, or when using materials that are fragile such as direction control alloys such as single crystal alloys and directionally solidified alloys. In the case of processing, welding cracks and deformation are liable to occur, and the yield is low.
- discharge surface treatment a method of forming a film on a work surface by pulsed discharge (hereinafter referred to as discharge surface treatment) is disclosed in Patent Document 1 and the like.
- this discharge surface treatment an arc discharge is generated between the electrode and the work made of a compact formed by compressing the powder to a hardness of about white, and thereby the constituent material of the melted electrode is formed on the work surface. It forms a film by solidification, and is attracting attention as a technology that can be used as a line of work instead of the above-mentioned methods such as welding and thermal spraying.
- conventional discharge surface treatments have formed a coating of a hard material such as TiC (titanium carbide) that has abrasion properties at room temperature.
- a hard material such as TiC (titanium carbide) that has abrasion properties at room temperature.
- electrodes formed by compressing WC (tungsten carbide) powder with an average particle size of about 1 are used. The film was formed of a hard material due to difficulty in shaking.
- Patent Document 1
- the supply of material from the electrode side and the manner in which the supplied material melts on the work surface may have the greatest effect on the coating performance. It is the strength or hardness of the electrode that affects the supply of the electrode material. Specifically, it is considered desirable that the electrode has a uniform hardness. However, in Patent Document 1, no consideration is given to uniformly molding the hardness of the electrode at the time of powder compression molding, and the hardness of the electrode itself may vary. As shown in Patent Document 1, when a thin film is formed, since the formed film is thin, even if the hardness of the electrodes is not uniform, it hardly affects the film.
- powders with a particle size of 3 ⁇ m or less are very expensive because only about a few percent of all processed powders can be collected.
- the sampling amount was affected by changes in the surrounding environment, and the yield was poor.
- the maximum diameter that can be manufactured by the atomization method is about 6 im, so that powder having a particle size of 3 m or less is obtained. It is very difficult.
- the powder produced by the atomization method is produced by evaporating the raw material and condensing it, and the resulting powder becomes spherical due to the effect of surface tension.
- an electrode is formed from such a spherical powder, there is also a problem that the interparticle bonding is weakened because the powder is in point contact, and the powder becomes brittle.
- the present invention has been made in view of the above, and has a uniform hardness, a uniform thickness at the time of discharge surface treatment, and a thick film having a thickness of about 100 m or more. It is an object of the present invention to obtain a discharge surface treatment electrode capable of performing the following.
- an electrode for electric discharge surface treatment is characterized in that a green compact obtained by compression-molding a powder containing a metal or a metal compound is used as an electrode in a working fluid or in air.
- a discharge surface treatment in which a discharge is generated between an electrode and a workpiece and the discharge energy forms a film made of an electrode material or a substance in which the electrode material has reacted with the discharge energy on the surface of the workpiece.
- the powder has an average particle diameter of 3 / m or less.
- the electrode for electric discharge surface treatment according to the next invention is characterized in that a green compact obtained by compression-molding a metal, a metal compound, or a ceramics powder is used as an electrode, and the electrode and the workpiece are processed in a working fluid or air. An electric discharge is generated between the electrodes, and the discharge energy is used to form an electrode surface or an electrode for discharge surface treatment used for the discharge surface treatment for forming a film made of the electrode material or a substance reacted by the discharge energy on the surface of the workpiece. Wherein the powder has a non-spherical shape.
- a discharge is generated between the electrode and the workpiece in a working fluid or in the air by using a green compact obtained by compression-molding a powder of a metal or a metal compound as an electrode.
- the discharge surface treatment electrode used for discharge surface treatment for generating a film made of an electrode material or a substance in which the electrode material reacts with the discharge energy by the discharge energy generated by the discharge energy. Is characterized by mixing a small-diameter powder having a small particle size distribution and a large-diameter powder having an average particle size more than twice as large as the small-diameter powder.
- the electrode for discharge surface treatment according to the next invention is characterized in that a green compact obtained by compression-molding a metal, metal compound, or ceramic powder is used as an electrode, and the electrode is formed in a working fluid or in the air. A discharge is generated between the workpieces, and the discharge energy is used for a discharge surface treatment for forming a film made of an electrode material or a substance in which the electrode material has reacted by the discharge energy on the surface of the workpiece.
- the powder has an average particle diameter of 1 / im or less.
- the method for producing an electrode for electric discharge surface treatment comprises the steps of pulverizing a metal, metal compound or ceramic powder into a non-spherical powder having a predetermined particle size by a pulverizer. 3 ⁇ 4A first step, and a second step of forming the crushed powder into a predetermined shape and compression-molding the powder so as to have a predetermined hardness.
- the present invention provides a discharge surface treatment method according to the present invention, wherein a green compact obtained by compression-molding a powder containing a metal or a metal compound is used as an electrode.
- the coating is formed using an electrode obtained by compression-molding a powder having an average particle size of 3 m or less. ' ⁇ .'
- the discharge surface treatment method according to the next invention is characterized in that a discharge is generated between the electrode and the workpiece by using a compact formed by compression-molding a powder of a metal or a metal compound as an electrode.
- the method is characterized in that a large-diameter powder having an average particle diameter more than twice that of the small-diameter powder is mixed, and the coating is formed using a compression-molded electrode.
- the discharge surface treatment method generates an electric discharge between the electrode and the workpiece made of a compact formed by compression-molding a powder having an average particle size of 1 ⁇ m or less,
- the discharge energy forms a film made of an electrode material or a substance reacted by the discharge energy on the surface of the workpiece.
- an electric discharge surface treatment apparatus comprises: an electrode made of a green compact obtained by compression-molding a powder containing a metal or a metal compound; and a workpiece on which a coating is formed.
- a pulsed discharge is generated between the electrode and the rotatable object by a power supply device that is disposed in the liquid or air and is electrically connected to the electrode and the rotatable object.
- the electrode has an average value of particle diameter of 3 ⁇ or less. It is characterized by being manufactured by compression molding of powder.
- the discharge surface treatment apparatus comprises: an electrode made of a compact formed by compression-molding a metal or metal compound powder; a roe on which a film is formed; and an electrical connection between the electrode and the gap. And a power supply device connected to the workpiece.
- the power supply device generates a pulse-like discharge between the electrode and the workpiece, and the discharge energy is applied to the surface of the workpiece.
- the electrode According to a discharge surface treatment apparatus for forming a film made of an electrode material or a substance in which the electrode material reacts with discharge energy, the electrode has a small diameter, a small-diameter powder having a particle size distribution, and twice as large as the small-diameter powder. It is characterized in that it is manufactured by compression molding a powder obtained by mixing a large-diameter powder having the above average particle size.
- the discharge surface treatment apparatus has an average particle diameter of 1 ⁇ m or less.
- An electrode made of a compact obtained by compression-molding the powder of (1), a coating on which a coating is formed, and a power supply device electrically connected to the electrode and the coating.
- a pulse-like electric discharge is generated between the electrode and the object by the apparatus, and a film made of an electrode material or a material in which the electrode material reacts with the discharge energy on the surface of the workpiece by its discharge energy. Is formed.
- FIG. 1 is a view schematically showing the structure of a turbine blade of an aircraft gas turbine engine
- FIG. 2 is a view schematically showing a discharge surface treatment in a discharge surface treatment apparatus
- FIG. 3B is a diagram showing a voltage waveform applied between a discharge surface treatment electrode and a workpiece at the time of discharge
- FIG. 3B is a diagram showing a current waveform of a current flowing through the discharge surface treatment device at the time of discharge.
- Fig. 5 is a flowchart showing an example of a manufacturing process of an electrode for electric discharge surface treatment:
- Fig. 5 is a cross-sectional view schematically showing a state of a molding machine when molding powder, and
- Fig. 6 is FIG.
- FIG. 7 is a diagram showing an outline of a test for hardness variation
- FIG. 7 is a diagram showing a particle size distribution of stellite powder after 50 hours of pulverization
- FIG. 8 is a scale having an average particle size of 1.8 m.
- FIG. 9 is a scanning electron microscope (EM) photograph
- FIG. 9 is a SEM photograph showing the inside of a densetsu manufactured as a comparative example using a spherical stellite powder having an average particle diameter of 6 ⁇ .
- Fig. 0 is a photograph showing the state of accumulation when processed under these conditions.
- Fig. 11 is a diagram schematically showing the principle of pulverization of the bead mill, and Fig.
- FIG. 12 is pulverization for 6 hours.
- FIG. 13 is a diagram showing the particle size distribution of the stellite powder after that, FIG. 13 is a diagram schematically showing the configuration of the electrode material of the eighth embodiment, and FIG. FIG. 14B is a SEM photograph showing the appearance of the coating when the discharge surface treatment is performed with a small discharge energy using an electrode having a ratio of 10%, and FIG. 14B shows that the ratio of the large-diameter powder is 50%.
- FIG. 9 is a SEM photograph showing a state of a film when a discharge surface treatment is performed with a small discharge energy using the electrode of FIG. Fig. 14C shows that the surface of the electrode is treated with a large discharge energy using an electrode with a large powder ratio of 50%.
- FIG. 13 is a diagram showing the particle size distribution of the stellite powder after that
- FIG. 13 is a diagram schematically showing the configuration of the electrode material of the eighth embodiment
- FIG. 14B is a SEM photograph showing the appearance of the coating
- FIG. 14D is a SEM photograph showing the state of the coating when the discharge surface treatment was performed with a small discharge energy using an electrode having a large powder ratio of 80%.
- Fig. 14E is a SEM photograph showing the state of the film.
- Fig. 14E shows the state of the film when the discharge surface treatment was performed with a large discharge energy using an electrode with a large powder ratio of 80%.
- FIG. 15 is a graph showing the relationship between the ratio of the large-diameter powder and the denseness of the film.
- FIG. 16 is a graph showing the relationship between the ratio of the large-diameter powder and the moldability of the electrode.
- FIG. 17 is a graph showing the relationship, and FIG.
- FIG. 17 shows a discharge surface treatment using an electrode manufactured from a powder obtained by mixing a 4: 1 mixture of a Co-based metal powder having a particle size of 6 ⁇ and 1 tm.
- FIG. 18 is a SEM photograph showing a cross-sectional view of the coating thus formed.
- FIG. 18 shows the relationship between the particle size of the powder constituting the electrode and the porosity of the coating.
- FIG. 19 is an S-photograph showing a cross-sectional view of a film formed by discharge surface treatment using an electrode manufactured from a Co-based alloy powder having a particle size of 0.7 ⁇ . It is. BEST MODE FOR CARRYING OUT THE INVENTION
- FIG. 2 is a view schematically showing a discharge surface treatment in a discharge surface treatment apparatus.
- the discharge surface treatment apparatus 1 includes a workpiece (hereinafter, referred to as a workpiece) 11 on which a coating 4 is to be formed, an electrode for discharge surface treatment 12 for forming a coating 14 on the surface of the workpiece 11, and a workpiece. And a discharge surface treatment power supply 13 that is electrically connected to the discharge surface treatment electrode 11 and supplies a voltage to both electrodes to generate an arc discharge between them.
- the work tank 16 When the discharge surface treatment is performed in a liquid, the work tank 16 should be filled so that the part of the work 11 and the electrode for discharge surface treatment 12 facing the work 11 is filled with a working liquid 15 such as oil. Is further installed. Also, when performing the discharge surface treatment in the air First, the workpiece 11 and the discharge surface treatment electrode 12 are placed in a treatment atmosphere. FIG. 2 and the following description exemplify a case where the discharge surface treatment is performed in the machining fluid 15.
- the electrode for discharge surface treatment may be simply referred to as an electrode. Further, hereinafter, the distance between the facing surface of the discharge surface treatment electrode 12 and the workpiece 11 is referred to as the distance between the electrodes.
- the discharge surface treatment is, for example, a discharge surface in which a workpiece 11 on which a film 14 is to be formed is used as an anode, and a powder having a mean particle diameter of 10 nm to several ⁇ m of metal / ceramic as a supply source of the film 14 is formed
- the processing electrode 12 is used as a cathode, and a discharge is generated between the electrodes while controlling the distance between the electrodes by a control mechanism (not shown) so that the electrodes do not contact each other in the machining fluid 15.
- FIG. 3A and FIG. 3B are diagrams showing an example of a discharge pulse condition during discharge surface treatment.
- FIG. 3A and FIG. 3B are diagrams showing an example of a discharge pulse condition during discharge surface treatment.
- FIG. 3A is a diagram showing a voltage waveform applied between a discharge surface treatment electrode and a workpiece during discharge.
- FIG. 3B shows a current waveform of a current flowing through the discharge surface treatment apparatus at the time of discharge.
- the voltage in FIG. 3A is a positive side of the voltage waveform graph when the polarity of the electrode 12 is negative when viewed from the peak 11 side.
- a view has a direction positive side to flow to the work 1 1 in Figure 2
- Time t as The force at which no-load voltage ui is applied between the electrodes at the time t after the discharge delay time td elapses, a current starts to flow between the electrodes and discharge starts.
- the voltage at this time is the discharge voltage ue
- the current flowing at this time is the peak current value ie.
- cell 2 - 1 1 is referred to as pulse width seven 'e.
- This time t A voltage waveform in ⁇ t 2, and repeat at the pause time to be applied between the two electrodes.
- the work 11 and a part of the electrode 12 are melted by the heat of the discharge.
- the electrode 12 melted by the blast due to the discharge or the electrostatic force Part (hereinafter referred to as electrode particles) 21 is separated from the electrode 12 and moves toward the surface of the work 11. Then, when the electrode particles 21 reach the surface of the work 11, they are re-solidified to form a film 14.
- a part of the separated electrode particles 21 reacting with the component 22 in the working fluid 15 or the air, 23 also forms a coating 14 on the surface of the workpiece 11. In this way, a film 14 is formed on the surface of the work 11.
- the electrodes 12 cannot be peeled off by blast or electrostatic force due to discharge, and the electrode material cannot be supplied to the workpiece 11.
- whether or not a thick coating can be formed by the discharge surface treatment depends on how the material is supplied from the electrode 12 side, how the supplied material is melted on the surface of the work 11 and how the material is bonded to the work 11 material. Affected.
- the hardness of the electrode 12 affects the supply of the electrode material.
- FIG. 4 is a flow chart showing an example of a process for producing a discharge surface treatment electrode.
- a powder of a metal, a metal compound, or a ceramic having the components of the coating 14 to be formed on the workpiece 11 is ground (step S 1).
- the powder of each component is mixed and ground so as to have a desired ratio.
- a metal-ceramic spherical powder having an average particle size of several tens of ⁇ m, which is distributed on the market is pulverized by a pulverizer such as a pole mill to an average particle size of 3 ⁇ m or less.
- the pulverization may be performed in a liquid, but in this case, the liquid is evaporated to dry the powder (step S2).
- Step S 3 The powder after drying is agglomerated with the powder to form a large lump, so that the large lump is disintegrated and a sieve is used to sufficiently mix the wax and the powder used in the next step.
- a sieve is used to sufficiently mix the wax and the powder used in the next step.
- Step S 3 For example, a ceramic or metal sphere is placed on a sieve net where the agglomerated powder remains. When vibrated, the agglomerates formed by agglomeration fall apart due to collision with the sphere of energy and pass through the mesh. Only the powder that has passed through this mesh is used in the following steps.
- a voltage applied between the discharge surface treatment electrode 12 and the workpiece 11 to generate a discharge is usually in a range of 8 OV to 30 OV.
- the distance between the electrode 12 and the work 11 during the discharge surface treatment is about 0.3 mm.
- the agglomerated mass constituting the electrode 12 is separated from the electrode 12 as it is by the arc discharge generated between the electrodes.
- the size of the lump is less than the distance between the poles (less than 0.3 mm)
- the next discharge can be generated even if there is a lump between the poles.
- discharge occurs at a short distance, discharge occurs where there is a lump, and the lump can be finely broken by the heat energy of the discharge and the explosive power.
- the lump When the size of the lump constituting the electrode 12 is greater than the distance between the electrodes (0.3 mm or more), the lump detaches from the electrode 12 as it is due to the discharge, and the work 11 It accumulates on the top and drifts between the electrodes 12 and the workpiece 11 between the electrodes filled with the working fluid 15.
- the discharge occurs near the distance between the electrode 12 and the work 11, so the discharge concentrates in that part (the large lump) and in other places Discharge cannot be generated, and the coating 14 cannot be deposited uniformly. Also, this large lump cannot be completely melted by the heat of discharge. Therefore, the coating 14 is very brittle and can be cut by hand.
- a step of sieving the aggregated powder in step S3 is required.
- sieving it is necessary to use a mesh with a size smaller than the distance between the poles.
- a powder such as paraffin is mixed into the powder at a weight ratio of about 1% to 10% (step S4).
- step S4 a powder such as paraffin is mixed into the powder at a weight ratio of about 1% to 10%.
- FIG. 5 is a cross-sectional view schematically showing a state of a molding machine when molding powder. Insert the lower punch 104 into the space formed by the lower punch 104 and the mold (die) 105 from the bottom of the hole formed in the mold (die) and 105. Fill the powder sieved in step S5 (or a mixture of powders if they consist of multiple components) 101. Thereafter, the upper punch 103 is inserted from above the hole formed in the mold (die) 105. Then, the powder 101 is compression-molded by applying pressure from both sides of the upper punch 103 and the lower punch 104 filled with the powder 101 using a pressurizer or the like.
- the compression molded powder # 01 is referred to as a green compact.
- the electrode 12 becomes hard, and if the press pressure is decreased, the electrode 12 becomes soft.
- the particle diameter of the electrode material powder 101 is small, the electrode 12 becomes hard, and if the particle diameter of the powder 101 is large, the electrode 12 becomes soft.
- the green compact is taken out of the molding machine and heated in a vacuum furnace or a furnace in a nitrogen atmosphere so as to have a hardness of about black ink (step S7).
- the electrode 12 becomes harder when the heating temperature is increased, and the electrode 12 becomes softer when the heating temperature is reduced. Further, by heating, the electric resistance of the electrode 12 can be reduced. for that reason, Heating is meaningful even when compression molding is performed without mixing in plastics. As a result, the bonding between the powders in the green compact proceeds, and the green compact has conductivity.
- the discharge surface treatment electrode 12 is manufactured.
- the functions 5 required for forming a thick film by the discharge surface treatment in the following Embodiments 1 and 2 include abrasion resistance and lubricity in a high-temperature environment, and components used in a high-temperature environment. It is intended for technologies that can be used for other purposes.
- a powder mainly composed of a metal component is compression-molded, and thereafter, it is often used. Therefore, an electrode subjected to heat treatment is used.
- a large amount of electrode material is supplied to the workpiece 11 by a discharge pulse, so that the hardness of the electrode 12 is reduced to some extent. It is necessary for the electrode 12 to have predetermined characteristics such as hardness and hardness.
- step S6 in the production of the electrode, the powder on the outer periphery is strongly crushed by contact with the mold, but pressure is not sufficiently transmitted to the inside.
- the hardness of the electrode the difference in hardness between the outer peripheral portion of the electrode and the inner portion
- the outer peripheral portion of the electrode 5-became hard and the inner portion became 'soft'. Therefore, in the first embodiment, focusing on this point, a method for obtaining an electrode for discharge surface treatment having no variation in the hardness of the electrode will be described.
- the present inventors have conducted production tests on electrodes for discharge surface treatment using various materials.0 In order to realize electrodes with approximately uniform hardness, pay attention to homogenization during compression molding of electrode material powder. As a result, it was found that the particle size of the electrode material powder had the greatest effect on the hardness of the electrode.
- Table 1 shows the relationship among the electrode material, the particle size of the electrode material powder, the hardness of the electrode material powder, and the variation in electrode hardness. '
- Electrode material which is the material of various electrodes
- particle size m which is the average particle size of the powder of the electrode material
- the average particle size if the average particle size is 3 ⁇ m or less, it is defined as ⁇ small '', 4 to 5 / Xm is defined as ⁇ medium '', and if it is 6 HI or more, ⁇ large ''. .
- binder hardness generally, a material having a Vickers hardness of 500 or less is regarded as “soft”, and a material having a Vickers hardness of about 500 to 1000 is regarded as “medium”. A material having a Vickers hardness of 100 or more is defined as “hard”.
- “hardness variation” indicates a difference in the hardness of the electrode at a plurality of positions on the electrode.
- the hardness of the electrode has a strong relationship with the degree of bonding of the powder, irrespective of the hardness of the powder constituting the electrode. For example, even if the electrode is made of a powder of a hard material, the degree of bonding of the powder is weak. In this case, the electrode becomes soft and easily collapses.
- the degree of bonding of the powder is weak. In this case, the electrode becomes soft and easily collapses.
- JISK 5600—5—4 Stipulated in JISK 5600—5—4 as an index of variation in electrode hardness
- the paint film pencil test is used. If the difference between the evaluation values at multiple locations in the same test is within 3 levels (for example, B and 4B), there is no variation in hardness. If the difference is within 5 levels (() For example, in the case of B and 6B), “ ⁇ ” with little variation in hardness is used, and “X” with more variation is used as “X”. Of course, other equivalent test results may be used as indicators.
- FIG. 6 is a diagram showing an outline of a hardness variation test. This figure shows a case where the discharge surface treatment electrode 12 has a cylindrical shape.
- This bottom surface 12 A is a surface that is disposed so as to face the workpiece during the discharge surface treatment, and is a surface where discharge occurs.
- the hardness variation calculated from the hardness of the electrode at a plurality of locations (for example, points A and B) within the bottom surface 12A, and the electrodes at a few locations on the side surface 12B (for example, points C and D)
- the hardness variation in the entire electrode 12 is evaluated.
- the electrode material No. 1 “CBN (Ti coating)” indicates an electrode manufactured from a powder of cubic boron nitride (Cubic Boron Nitride) coated with Ti.
- the electrode material No. 2 “Stellite 2” is made from powder of Stellite 2 which is an alloy containing Co as a main component and other components such as 0r, Ni, and Mo mixed. Indicates the manufactured electrode, and the electrode material No. 3 ⁇ Stellite 3 '' is made from powder of Stellite 3 material, which is an alloy containing Co as a main component and other components such as Cr, W, and Ni mixed. 2 shows a manufactured electrode.
- the particle size of the powder of the electrode material affects the variation in electrode hardness that occurs during compression molding, as described above. Furthermore, when examining the experimental results, there is no variation in the electrode hardness when a material with a small particle size is used, regardless of the hardness of the material powder. Specifically, in order to produce a homogeneous molded product during compression molding, the average particle size of the powder of the electrode material should be about 3 / zm or less. It is more preferable that the average particle diameter of the powder of the electrode material be about 1 ⁇ m or less. By doing so, it is possible to eliminate variations in the hardness of the electrodes. These considerations include, for example, the comparison of the number 2 electrode with the number 4 electrode, the comparison of the number 5 electrode with the number 6 electrode, or the comparison of the number 7 electrode with the number 8 electrode and the number 9 electrode. It is clear from the comparison.
- the first method is thought to be able to make the hardness of the electrode uniform by increasing the flowability inside the mold during compression molding. Is a method of mixing a large amount of wax.
- the results could improve the electrode uniformity to some extent, but did not completely eliminate the variation.
- No. 3 only 7% by weight of wax was mixed in, and it is possible to further improve by increasing the amount of wax, but if the amount of wax is too large, the fineness of the materials will be combined. This is not a very effective method because some problems such as difficulties are assumed. Therefore, even if a large amount of wax is mixed with the powder of the electrode material, it is difficult to eliminate variations in the hardness of the formed electrode.
- the second method is a method in which the material powder is put into a mold and compressed at a relatively low press pressure by applying vibration to the mold when compressing.
- this method variations in hardness occurred at the final pressing stage, and did not completely eliminate the variations.
- the average value of the particle diameter of the electrode component powder is set to 3 ⁇ m or less, it is possible to manufacture an electrode having no variation and exhibit lubricity in a high-temperature environment.
- a uniform thick film such as a coating can be formed.
- Table 2 shows the electrode material, the particle size of the electrode material, the hardness of the powder of the electrode material, and the hardness of the electrode.
- C is a table showing the relationship of fluctuation
- Electrode material in Table 2, the material used in manufacturing the electrode is described.
- TiC + Ti of No. 1 means that an electrode was manufactured by mixing TiC powder and Ti (titanium) powder at a weight ratio of 1: 1.
- the electrode material “Stellite 2 + Co (2: 1)” refers to a mixture of powder of stellite 2 and powder of Co (conoreto) in a 2: 1 weight ratio to form an electrode. It means that it was manufactured.
- “Stellite 1” of Nos. 3 and 4 is a material called Stellite 1, which is an alloy in which Co is the main component and other components such as Cr, W (tungsten), and Ni (nickel) are mixed. An electrode made from powder is shown.
- particle size ( ⁇ ⁇ .) J shows the average particle diameter of each powder of the electrode material shows a particle size corresponding to a combination of the electrode material.
- the number 7 large (6 ) + Small (1) J, is the electrode material “Stellite 2 + Co J” where the particle size of Stellite 2 powder is large (particle size 6 m) and the particle size of Co powder is small (particle size 1
- the definition of “large”, “medium”, and “small” shown in the particle size is the same as that in Table 1 of Embodiment 1, and therefore the description is omitted. I do.
- “powder hardness” indicates the hardness of each powder of the electrode material, and indicates the particle size corresponding to the combination of the electrode materials.
- “medium + soft” of No. 7 means that the hardness of the Stellite 2 powder among the electrode materials “Stellite 2 + Co” is medium, and the hardness of the Co powder is soft.
- the definitions of “hard”, “medium”, and “soft” indicated in the powder hardness are the same as those in Table 1 of the first embodiment, and thus the description thereof is omitted. Also, the content of “hardness variation” is the same as that described in Table 1 of the first embodiment, and a description thereof will not be repeated.
- the size of the particle size of the powder of the electrode material affects the variation in electrode hardness that occurs during compression molding. Understand. In other words, if the electrodes are formed by mixing powders of different material with a large particle diameter (particle diameter of about 6 im), the hardness of the electrodes will not be uniform during compression molding. By mixing a small (particle size of about 1 ⁇ m) powder, the uniformity of electrode hardness can be increased. Specifically, when manufacturing electrodes by mixing powders of different materials, the average particle size of powder of one material should be 3 ⁇ or less, and the average particle size of powder of another material should be 3 ⁇ m.
- the stellite powder having a relatively large particle size has a small particle size (3 ⁇ or less).
- An example was given in which two (plural) components with different average particle diameters were mixed so as to mix the Co powder.
- a relatively large particle size for example, about 6 m
- stellite powder is used. It is advisable to mix powders of the same component but different particle sizes, such as mixing small .. (for example, about 1 ⁇ ) stellite powder, and then mix different components together.
- a film is formed from an electrode material.
- the electrode material to be a film includes a portion that is melted by the energy of discharge and a portion that is not melted.
- the performance required for a coating is such that the ratio of a portion that melts and a portion that does not melt is a predetermined ratio.
- This ratio can be controlled by controlling the particle size of the electrode powder. Specifically, the ability of powder with a small particle size and the powder to reach the work in a state of being melted by the heat of electric discharge has the property that a large percentage of the powder arrives at the work without being completely melted. It is used to form a film in a desired state.
- an electrode having no variation in hardness can be manufactured, so that a uniform thick film such as a film exhibiting lubricity in a high temperature environment can be formed.
- an electrode having no variation in hardness can be formed, so that the manufacturing cost of the electrode can be reduced.
- the technology for uniformly manufacturing the hardness of the discharge surface treatment electrode has been described.
- variations in electrode hardness still remain.
- a form often seen as a variation in the hardness of the electrode is that the outer peripheral portion of the electrode becomes hard as described above.
- the powder constituting the electrode has a predetermined particle size.
- manufacture an electrode with powder having a particle size of 3 // m or less in order to manufacture an electrode with uniform hardness It is necessary to.
- powder with a particle size of 3 ⁇ or less is distributed only in a limited number of materials at the factory, and the particle size of the coating material formed on the work surface is 3 ⁇ m or less. Is not available on the market.
- WC powder with an average particle size of about 1 m is widely distributed in the factory and is easily and inexpensively available, but other materials are difficult to obtain. For this reason, it is not possible to manufacture electrodes for discharge surface treatment of various materials only with powder having a particle size of 3 m or less that is distributed in the factory. Therefore, in the following Embodiments 3 to 7, a description will be given of a manufacturing method capable of manufacturing electrodes ′ for discharge surface treatment of various materials.
- Embodiments 3 to 7 below mainly relate to the powder crushing step of step S1 in the above-described flowchart of the manufacturing process of the electrode for surface treatment of discharge in FIG.
- the relationship between the particle size of the powder of the electrode material and the hardness of the electrode will be described.
- the electrode becomes hard, and when the particle size of the powder is large, the electrode becomes soft.
- the electrode is manufactured using the powder having an average particle size of several tens of ⁇ without crushing in step S1 in FIG. 4, the electrode has a high surface hardness, Have a hardness variation that is low. ⁇
- the manufactured electrode has a hard surface and a soft inside.
- the electrode material is not supplied to the work side because of its high hardness, and it is a removal process that cuts the work surface like a die sinking electric discharge machining.
- the electrode material is easily supplied to the work side because of its brittle hardness, and is consumed immediately after the processing is started.
- the electrode surface after the discharge surface treatment has a shape in which the outer peripheral portion protrudes and the central portion is depressed.
- discharge occurs only at the outer peripheral part because discharge occurs at a place where the distance to the workpiece is short, and the processing is removal of the workpiece surface. I will. That is, it becomes impossible to perform the deposition processing on the work surface. Therefore, it is necessary to suppress variations in electrode hardness by manufacturing electrodes using powder having a small particle size.
- the electrode powder of the material used for forming the film is crushed by a pulverizing apparatus such as a ball mill, and the powder is finely divided and divided. It is characterized by.
- the powder has an average particle size of 3 / zm or less.
- the powder pulverized by the ball mill is finely crushed while being crushed, its shape becomes a scale-like shape having a flat surface, and its surface area is larger than that of a sphere.
- the powder particles are compression-molded, the particles come into surface contact with each other, so that an electrode having appropriate strength can be manufactured.
- the ground scale-like powder has the property that its planes face each other, so that the space formed between the powders can be made very small. Therefore, at the time of press molding, the pressure of the press can be propagated to the inside of the electrode. Further, the denseness of a film formed using such an electrode is also improved.
- an electrode is manufactured using a powder crushed to an average particle diameter of 3 m or less by a pole mill apparatus and a discharge surface treatment is performed with the electrode.
- an electrode manufactured from stellite powder ground to an average particle size of 1 will be described as an example.
- the stellite powder is an alloy consisting of Cr 25 wt%, Nil 0 tw%, W 7 wt%, C (carbon) 0.5 wt%, and the balance Co.
- an alloy consisting of Mo 2 8 wt%, Cr 17 wt%, Si (silicon) 3 wt%, and the balance Co, and Cr 28 wt% , Ni 5 wt%, W 19 wt%, and the balance may be stellite powder such as an alloy of Co.
- the electrode is manufactured from stellite powder according to the flowchart shown in FIG. 4, a detailed description thereof will be omitted, and only a part related to the third embodiment will be described.
- a stellite powder having an average particle size of about 5 Q ⁇ which is commercially available, was used as a raw material. Some of the stellite powders were large and had a particle size of 0.1 mm or more.
- stellite having an average particle size of about 50 ⁇ m was fed by a vibrating ball mill.
- the material of the container and (pot) balls of a vibration ball mill device used was a Z R_ ⁇ 2 (Jirukonia).
- a predetermined amount of stellite as an electrode powder was put in a container (pot), and a ball was put in the container. Further, the inside of the container was filled with acetone as a solvent, and stearic acid was added as a dispersant. Then, this container (pot) was vibrated and crushed for about 50 hours.
- stearic acid is a surfactant that plays a role in suppressing the aggregation of the finely divided particles. As long as it has such a role, it is not limited to stearic acid, and other nonionic sparse 70 (trade name) sorbitan monooleate may be used. As a solvent, ethanol, methanol, or the like can be used in addition to acetone.
- FIG. 7 is a view showing the particle size distribution of stellite powder after pulverization for 50 hours.
- the horizontal axis shows the particle size (Aim) of the powder in logarithmic memory
- the vertical axis shows the horizontal axis.
- the ratio of powder (right axis) and the cumulative ratio (left axis) present in the section where the particle size to be obtained is classified according to a predetermined standard are shown.
- the bar graph shows the proportion of powder present in each section provided on the horizontal axis
- curve L shows the cumulative proportion of powder present in each section from the smaller particle size side. It shows the cumulative percentage that was calculated.
- the average particle size of the stellite powder could be reduced to 1.8 ⁇ by grinding for 50 hours.
- the particle size distribution of the particles was measured by a laser diffraction 'scattering method.
- This measurement method utilizes the fact that the particles are irradiated with laser light, and that the amount of scattered light and the scattered pattern differ depending on the particle size. Since particles moving in a liquid are irradiated with laser light tens of thousands of times in 30 seconds, the results are counted, and the distribution is obtained, so that averaged data can be obtained. Measuring scaly particles gives an intermediate value between the widest surface (scale surface) and the narrowest surface (scale surface). In general, the particle size distribution of the flaky particles is broader than when the spherical particles are measured. Using the particle size distribution obtained from this measurement method, the results of the particle size distribution are accumulated from the smaller particle size, and the particle size at which the accumulated value becomes 50% is defined as the average particle size (median diameter). .
- FIG. 8 is a SEM (Scanning Electron Microscope) photograph showing the inside of an electrode made of scale-shaped stellar 1 and powder having an average particle size of 1.8 ⁇ m.
- FIG. 9 is a SEM photograph showing the inside of an electrode manufactured as a comparative example using spherical stellite powder having an average particle diameter of 6 ⁇ m.
- the space between the powder particles is small, and the small particles are in a very dense state. I have.
- the shape of the powder particles is substantially spherical, and the space between the powder particles is large. It also has many spaces.
- FIG. 10 is a photograph showing the state of deposition when processed under these conditions.
- the area indicated by the circle on the left indicates the state of the film formed by processing for 5 minutes
- the area indicated by the circle on the right indicates the state of the film formed by processing for 3 minutes. Is shown.
- the surface of the film was homogeneous, and no discharge concentration or short-circuiting was observed. It is considered that stable discharge occurred.
- a film of about l mm could be formed in 5 minutes.
- the amount of electrode powder supplied from the electrode becomes an optimal amount.
- the temperature of the arc column does not decrease, and the upper surface of the work can be melted by the arc.
- the electrode powder is deposited on the molten work, it forms a film having a strong bonding force.
- the electrode material is also sufficiently melted during the transfer to the work, and is deposited on the work in that state, so that the discharge trace formed on the work surface is almost flat. The coating formed by stacking the flat discharge marks becomes dense.
- the third embodiment by using a ball mill device, powder having a desired particle size for producing an electrode having a uniform hardness can be obtained at low cost.
- the electrode powder is crushed and broken by the pole, so that a non-spherical scale-like powder is obtained. As shown in FIG. 8, this scaly powder tends to have the same powder direction, and the space formed in the electrode is reduced. Therefore, the pressure of the press is transmitted to the inside of the electrode at the time of forming the electrode, and a dense electrode having uniform hardness can be manufactured. Further, since the electrodes are dense, there is an effect that the formed film can be dense.
- Japanese Patent Application Laid-Open No. 5-11632 discloses a method for producing a graphite electrode for electric discharge machining, in which a mixture of a binder and a carbonaceous material is pulverized in order to obtain a desired particle size.
- the use of a jet mill device is described. In this milling, when the binder is mixed with the carbon raw material, large lumps are created just like flour mixed with water. 2004/000742
- this pulverization is not to pulverize the powder, but to break up large lumps. Therefore, this is different from the third embodiment in which the shape of the powder is changed and the powder itself is finely divided.
- Japanese Patent Application Laid-Open No. Hei 5-11632 relates to a discharge pump for the purpose of suppressing the consumption of the electrode and removing the work, and using the electrode manufactured by the above method. In the case where the work is performed, the work is removed, and a film cannot be formed as shown in the third embodiment.
- a powder of a desired component is pulverized into a non-spherical powder of 3 ⁇ m or less by a planetary ball mill.
- step S1 in the flowchart shown in FIG. 4 sterite powder having an average particle diameter of 6 ⁇ is ground for 3 hours by a planetary ball mill, and the powder is finely divided into powder having an average particle diameter of 3 m. It has become.
- the Jirukonia container made of a volume 5 0 0 c c, using Jirukoyua made grinding balls of phi 2 mm. Further, the same stellite powder as used in the third embodiment was used.
- the planetary pole mill device is a device that rotates a container containing the electrode powder, balls and solvent, and also pulverizes while rotating the table on which the container is placed. 5 or more of the pole mill: L 0 times. However, it is not suitable for processing large amounts of powder and is suitable for processing small amounts.
- the shape of the powder pulverized by using the planetary pole mill has a flaky shape like the powder obtained by the vibrating ball mill of the third embodiment.
- the inside of the electrode manufactured using the flaky powder having an average particle size of 3 was the same as that in FIG. 8 of the third embodiment described above. That is, even with this powder, an electrode having no variation in hardness could be manufactured as in the third embodiment.
- a discharge surface treatment was performed for 3 minutes under the same processing conditions as in the third embodiment, a stable discharge could be obtained, and a thick film of about 0.1 mm could be deposited.
- powder having a desired particle size for manufacturing an electrode having uniform hardness can be obtained.
- an electrode made of this powder has a small space formed inside, and the pressure of the press is transmitted to the inside of the electrode during electrode molding, so that a dense electrode having uniform hardness can be manufactured. Further, since the electrodes are dense, there is an effect that the formed film can be dense. ⁇ Embodiment 5.
- FIG. 11 is a diagram schematically showing a pulverizing principle of a bead mill device.
- the grinding receptacle 2 0 1 and Z r monument ball 2 made of diameter phi 1 mm (beads) 2 1 0 between the rotor 2 0 2 add about 1. 7 kg.
- a stirring pin 203 is attached to the rotor 202, and when rotated, the pole 210 is stirred.
- the electrode powder is charged into the grinding container 201.
- the electrode powder is mixed with acetone or ethanol, and is put into a grinding container 201 as a slurry. If the powder agglomerates during pulverization, it is advisable to add a dispersant in an amount of 1 to 5% by weight.
- region pole 2 1 0 is agitated when passing through the 2 0 4 '(hereinafter referred to as grinding region), the electrode powder between poles 2 1 0 and the pole 2 1 0 is fine crushed You.
- the slurry passes through the crushing area 204, it passes through the screen 205 acting as a filter paper, flows out of the crushing vessel 201, and is circulated back into the re-milling vessel 201.
- the shape of the powder pulverized using the bead mill 200 has the same flaky shape as the powder obtained by the vibrating ball mill of the third embodiment or the planetary ball mill of the fourth embodiment.
- the same stellite powder as in Embodiment 3 was pulverized using such a bead mill.
- FIG. 12 is a view showing the particle size distribution of stellite powder after pulverization for 6 hours.
- the horizontal axis shows the particle size ( ⁇ m) of the powder in logarithmic memory
- the vertical axis shows the particle size shown on the horizontal axis.
- the ratio of powder (right axis) and the cumulative ratio (left axis) present in the section divided according to the predetermined standard are shown.
- the bar graph shows the proportion of powder present in each section provided on the horizontal axis
- the curve L shows the proportion of powder present in each section in order from the smaller particle size. This shows the cumulative ratio that has been accumulated.
- the average particle size of the stellite powder could be reduced to 1 ⁇ by grinding for 6 hours.
- the bead mill crushes small balls by colliding them at high speed, the grinding power is more than 10 times that of the vibratory pole mill. Therefore, as can be seen from comparison with FIG. 7, the particle size distribution is sharper and narrower than in the case of the vibratory pole mill. Also, when powder having such a sharp particle size distribution is used for manufacturing an electrode, all powders are melted under the same discharge conditions, so that the denseness of the coating is further improved.
- the fifth embodiment by using a bead mill, it is possible to obtain a powder having a desired particle size for manufacturing an electrode having a uniform hardness. Further, in the electrode manufactured by using the powder, the space formed inside becomes small, and the pressure of the press is transmitted to the inside of the electrode when the electrode is formed, so that a dense electrode having uniform hardness can be manufactured. Further, since the particle size distribution of the powder is sharp, the electrode becomes dense, and the formed film can be made more dense.
- the fine with a mean particle size 6.7 1 !! 7 ⁇ 11 2 (titanium hydride) jet mill the powder into average particle size below 3 mu m as an example.
- a jet mill particles are jetted from an opposing nozzle at a supersonic speed or a speed close thereto, and the particles are made to collide with each other to make the powder finer.
- the shape of the pulverized powder is not flattened and is a polyhedral shape with a number of corners, unlike the ball mill and vibratory pole mill.
- Table 3 is a table showing pulverization conditions by a jet mill device. JP2004 / 000742
- a powder frame of TiH 2 powder was formed in nitrogen, and the nozzle pressure was set to 5 MPa. Milling was repeated under the same conditions until the desired average particle size was reached.
- the average particle size of the powder before grinding was 6.7 ⁇ m, but after 15 hours of grinding, the average particle size was 1.2 ⁇ .
- the sixth embodiment by using a jet mill device, it is possible to obtain powder having a desired particle size for manufacturing an electrode having uniform hardness.
- a dense electrode having a uniform hardness can be manufactured as compared with the case where spherical powder is used.
- the situation in which the material of the container of the mill device and the material of the ball are mixed with the material to be ground in the course of the grinding by the mill device is examined.
- the material of the container and the ball of the ball mill was A 1 2 0 3 (alumina)
- the material of the container or pole may be mixed into the powder during the grinding.
- Quantitative analysis of the content of A1 and Zr in the pulverized powder using an EPMA (Electron Probe Micro Analyzer) shows that when alumina is used as the material for the mill equipment, the A1 content is 16 wt%. Used zirconium for the material of the mill equipment In that case, Zr was about 2 wt% and contained no power. This is because the wear resistance of zirconia at room temperature is about 10 times higher than that of alumina.
- the pole material can be mixed into the electrode powder by using a material having low wear resistance at room temperature as the ball material.
- the container and ball of the pole mill device with the material to be ground (that is, the same material as the powder) ', or What is necessary is just to coat the same material as the material to be ground.
- the coating method include thick welding, plating, and thermal spraying.
- the material of the container or the pole of the mill device is appropriately selected, thereby mixing the ball material of the mill device with the electrode material. Can be controlled. Therefore, mixing although been made difficult to mix uniformly the different Do that the material of the powder of the prior few ⁇ ⁇ , (if example embodiment, A l 2 0 3 Z r 0 2) material of the pole or container little by little during grinding the Because it can be mixed with the material to be crushed uniformly.
- the functions required for the thick film formed by the discharge surface treatment of the eighth embodiment include abrasion resistance and lubricity in a high-temperature environment.
- Oxides of Cr and Mo are known as materials having such a function.
- a powder mainly composed of a metal component is compression-molded. Then, if necessary, an electrode manufactured by performing a heat treatment is used.
- a large amount of electrode material is produced by a discharge pulse.
- it is necessary to make the electrode have certain characteristics regarding the material and hardness of the electrode for example, the hardness of the electrode is low to some extent and the hardness does not vary.
- the variation in electrode hardness here means (1) In the manufacturing process of the electrode, the powder at the outer periphery is strongly crushed by contact with the mold during pressing, but the pressure is not sufficiently transmitted to the inside Variations in electrode hardness (difference in hardness between the electrode outer part and the inner part) where the outer peripheral part of the electrode becomes hard and the inner part becomes softer, and (2) When the direction of the press becomes longer This means that there is a large variation in the hardness in the pressing direction caused by the absence of the press pressure transmitted inside. Therefore, in an eighth embodiment, an electrode for discharge surface treatment that can eliminate the variation in electrode hardness that occurs in the electrode manufacturing process and can manufacture a dense coating at low cost will be described.
- the inventors' experiments have clarified the following facts regarding electrode molding when the particle diameter of the material powder of the electrode for discharge surface treatment is increased or decreased.
- the particle size is larger than about 3 / Zm, especially larger than about 6m, the powder on the outer periphery is strongly crushed by contact with the mold when molding the powder by pressing. Pressure is not sufficiently transmitted to the electrode, and the outer periphery of the electrode becomes hard and the inside becomes soft.
- the particle size is smaller than about 3 ⁇ , the phenomenon that the outer peripheral portion of the electrode hardens as described in the above (1).
- a coating film when the powder particle size of the material for the electrode for discharge surface treatment is increased or decreased.
- a film is formed using an electrode formed of a powder having a small particle diameter, a dense film can be formed by a discharge pulse having a small energy. (Conversely, an electrode formed of a powder having a small particle diameter is used. If a film is formed with a discharge pulse of high energy when forming a film, problems such as an increase in space in the film and cracks in the film occur).
- a coating film can be formed with a discharge pulse having a large energy, but there is also a problem that the particle size is large and the energy of the discharge pulse is large, so that the space in the coating is increased and a crack is formed in the coating.
- spherical powders are generally produced by a method such as the atomization method.
- powders of several 10 ⁇ are often produced, and powders of 10 ⁇ m or less are required.
- the powder produced by the atomization method is often obtained by classification.
- powders of the order of several 10 ⁇ m are considered in terms of cost, except for materials with high demand such as Co. It is realistic to obtain by grinding.
- the small-diameter powder produced by pulverization has a flat shape instead of a spherical shape, and the phenomenon that the green compact, which is a compact, expands when the pressure of the press is released is further increased. Have a point. This is because powder flows better during compression molding and is easier to compress. In addition, since it is difficult to control the amount of expansion of the green compact formed from the powder, an electrode having different properties is formed each time the powder is molded, which is a major problem in quality control.
- the force to equalize the amount of expansion of the electrode The force to eliminate the expansion of the electrode, or reduce the amount of expansion of the electrode to a manageable range
- FIG. 13 is a diagram schematically showing the configuration of the electrode material according to the eighth embodiment.
- a state in which powder is placed in a molding machine and compressed is schematically shown. Have been.
- the same components as those in FIG. 5 are denoted by the same reference numerals, and description thereof is omitted.
- a small-diameter powder 112 having a small particle size distribution and a small-diameter powder 112 having a small average particle size distribution are used as the powder of the electrode material.
- a mixture of powder with a large diameter of at least twice as large as 1 1 1 or a powder with a small diameter of 1 ⁇ m or less with an average particle diameter of 3 ⁇ m or less and a powder with a large diameter of 1 ⁇ m with an average particle diameter of 5 ⁇ m or more 1 1 It is characterized by using a mixture of 1 and 2.
- a case where a mixture of a large-diameter powder 1 11 having a particle size of about 6 ⁇ m and a small-diameter powder 1 12 having a particle size of about 1 ⁇ m is used will be described as an example. .
- the small-diameter powder 1 1 2 is the main component of the electrode that contributes to film formation
- the large-diameter powder 1 1 1 is the powder. It is a powder that is added supplementarily to improve the compressibility of the electrode and to perform stable electrode molding, but this also gives an S odor.
- both the large-diameter powder 111 and the small-diameter powder 112 serving as electrode materials are Co-based alloys containing Cr, Ni, W, and the like.
- a Co alloy, a Ni alloy, a Fe alloy, or the like can be used for forming a thick film.
- the large-diameter powder 111 and the small-diameter powder 112 may be the same material or different materials.However, in order to form a coating based on a predetermined alloy material, the same alloy material is used. It is more desirable.
- the large-diameter powder 1 1 1 was selected from powders produced by the atomization method and selected to have a particle size of about 6 It is a powder and has a substantially spherical shape.
- the small-diameter powder 112 a powder having the same composition as that of the large-diameter powder 111 produced by the atomization method and having a mean particle size of about 1 to 2 ⁇ m is used. did. 0742
- the method for manufacturing an electrode using these powders is the same as the method described in the flowchart of FIG. 4 of Embodiment 1, and therefore the description thereof is omitted.
- the small-diameter powder 1 1 and 2 alone, when the pressure was released after pressing, the green compact, which was a compact, was expanded.However, the small-diameter powder 1 '1 2 was spherical. By mixing the large-diameter powder, the flow of the powder was improved, the pressure of the press was evenly transmitted to the electrode (compact), and the expansion of the electrode after the pressure was released almost disappeared.
- the ratio of the large-diameter powder 11 is preferably about 5% to 60% by volume. More desirably, the range of about 5% to 20% seemed to be good from the viewpoint of the denseness of the coating. If the proportion of the large-diameter powder 111 is too small, the electrode does not swell, but if the large-diameter powder 111 is mixed with about 5% or more, the electrode no longer swells. When the amount of the large-diameter powder 11 increases, it becomes difficult to form a film under the condition of a discharge pulse having a small energy, and a problem arises that the surface roughness of the film becomes rough with a discharge pulse having a large energy. Therefore, it is desirable to reduce the proportion of the large-diameter powder 111 as much as possible.
- discharge pulse width te is 10 s
- peak current value i is about 10 A
- discharge pulse width te is 70 ⁇ s or less
- peak current value is 30 If it is A or less, a dense film can be formed.
- the powder material includes a material that easily forms carbide
- the electrolysis material is supplied to the work side in a completely melted state by electric discharge, it becomes carbide and it is difficult to form a thick film.
- M o is because a material easily forming carbide
- Fig. 148 to Fig. 14 ⁇ show the ratio of large-diameter powder in the electrode and the energy of the discharge pulse. It is a SEM photograph which shows the state of the section of the coat according to the difference of the size of a key.
- a discharge surface treatment was performed, and
- the magnification in FIG. 14A is 100 ⁇
- the magnification in FIGS. 144 to 14E is 500 ⁇ .
- the thicknesses of the coatings are different from each other because the processing time is different, and it is irrelevant to the state of the coating itself, and a thin one can be made thicker by increasing the processing time.
- the film thickness may be controlled by the processing time or by the number of discharge pulses. Since the volume of a film that can be formed by a discharge pulse is almost the same for a discharge pulse having the same current waveform, that is, the same pulse width te and the same peak current value ie, the film thickness is controlled by the number of discharge pulses. Is valid. Controlling the coating by the number of discharge pulses makes it extremely easy to manage. For example, it is possible to send information to a discharge surface treatment device over a network for remote management.
- Fig. 14A to Fig. 14E if the ratio of the large-diameter powder is small, a dense film can be formed under the condition of low discharge pulse energy (Fig. 14A, Fig. 14A). (Fig. B), it can be seen that the space in the coating increases as the proportion of large-diameter powder increases (Fig. 14D). Also, even when the ratio of large-diameter powder is large, increasing the energy of the discharge pulse melts the electrode material transferred to the workpiece, but one discharge It can be seen that a large amount of electrode material is melted by the pulse, resulting in a large space and a film (Fig. 14E). In this regard, a similar phenomenon is observed even when the proportion of large-diameter powder is small (Fig.
- FIG. 15 is a graph showing the relationship between the ratio of the large-diameter powder and the denseness of the coating film.
- the horizontal axis shows the volume percentage of the large-diameter powder in the electrode volume
- the vertical axis shows the percentage of the space in the film formed when the electrode shown on the horizontal axis is subjected to discharge surface treatment. Is shown.
- Curve E is the evaluation when the pulse condition is large
- curve F is the parallax when the pulse condition is small.
- the denseness of the coating increases.
- the content of the large-diameter powder exceeds about 60%, the denseness deteriorates and the coating has a large space.
- the coating has more space.
- the treatment is performed under a pulse condition of low energy, if the proportion of the large-diameter powder is less than about 60%, the space of the coating film is reduced, and a dense film can be formed.
- the proportion of large-diameter powder is less than 20%, the space in the coating is very small.
- FIG. 16 is a graph showing the relationship between the ratio of the large-diameter powder and the moldability of the electrode.
- the horizontal axis shows the volume percentage of the large-diameter powder in the electrode volume
- the vertical axis shows the quality of the electrode formability. The higher the vertical axis, the better the electrode formability. Is shown.
- the amount of large-diameter powder exceeds about 80%, it is difficult to press-mold the electrode to make it uniform, and the outside of the electrode tends to be hard and the inside soft. Become. Conversely, if the amount of large-diameter powder becomes too small (about 2004/000742
- the ratio of the large-diameter powder is 5% to 60%, more preferably about 5% to 20%.
- this ratio also depends on the shape of the small-diameter powder that is the main component. In other words, if the small-diameter powder has a shape close to a spherical shape, the ratio of the required large-diameter powder may be small.
- such a result is obtained by mixing a small-sized powder having a particle size distribution with a large-sized powder having an average particle size more than twice as large as a small-sized powder.
- Japanese Patent Application Laid-Open Nos. 5-148686 / 1993 and 8-320207 / 1996 are known. is there.
- these inventions aim at forming a ceramic-based coating, and use ceramics as a main component of the coating as small-diameter powder and metal powder used as a binder as large-diameter powder. This is due to the fact that it is generally difficult to obtain small-diameter powder from metal powder, which is different from the present invention.
- the inventions disclosed in JP-A-5-148681 and JP-A-8-300227 disclose that the required particle size is controlled by controlling the particle size. It means that there is no point of view.
- Japanese Patent Publication No. 7-46696 also states that powders having different particle diameters are mixed to form a shape. Force is then applied to the surface for electric discharge machining (for engraving a workpiece into a predetermined shape). According to the eighth embodiment, a large-diameter powder having a volume ratio of 5% to 60% is added to a small-diameter powder according to the eighth embodiment. Since the electrode for discharge surface treatment is manufactured by mixing, the powder does not expand after the powder is pressed to release the pressure, and an electrode having a uniform hardness can be obtained. As a result, it has the effect of facilitating electrode management. 2004/000742
- the method of separately preparing and mixing powders having different particle diameters has been described. However, depending on the method of pulverizing a powder having a large particle diameter (for example, a powder having a particle diameter of 6 ⁇ ), the method may be omitted. , 'There is a case where powders having different particle sizes are mixed. For example, when crushing powder with a ball mill using zirconia balls, crushing 6 ⁇ m powder with a ⁇ 15 mm pole makes 2 ⁇ m the center of distribution. Powder and powder having 6 ⁇ as the center of distribution were mixed.
- the particle size of powder used as an electrode component is set to 3 ⁇ m or less, or What is necessary is just to mix a predetermined amount of powder having a particle size of 3 ⁇ m or less into the powder used as the electrode component. This is because when the powder is formed into a green compact by pressing, if the particle size is large, for example, about 6 ⁇ , the outer periphery of the green compact is strongly pressed or rubbed from the mold. This is because such a phenomenon does not occur when the # vertical diameter of the powder becomes smaller.
- a force to reduce the particle size of the powder used as the electrode component to 3 ⁇ or less, or a predetermined amount of powder having a particle size of 3 m or less mixed with the powder used as the electrode component There is a problem in that a force coating that suppresses variations in the hardness of the electrodes and furthermore, the variations in the formed coating has many voids.
- Fig. 17 shows the cross section of the coating formed by the discharge surface treatment using an electrode made from a 4 : 1 mixed powder of a Co-based metal powder with a particle size of 6 ⁇ 111 and lm.
- the lower side of the photograph is the work which is the base material, and the film is formed on the upper side.
- the space is large and the ratio is about 10%. Therefore, it cannot be said that a sufficiently dense thick film can still be formed with the electrode as described above. It should be noted that no matter how the processing conditions were changed, it was found by experiments of the inventors that when the particle size was large, the particles did not become dense to some extent.
- the main purpose is to form a film or a thick film mainly composed of a metal or an alloy
- the electrode is also made of a material mainly composed of a metal or an alloy. It is mainly assumed to be used.
- the material of the electrode not necessarily the metal itself, but for example, it is a metal compound such as a metal hydride, but heat is applied to the material.
- a metal compound that is in a state equivalent to a metal may be used.
- Embodiment 9 a case will be described in which the average particle diameter of the powder is 1 ⁇ m or less to manufacture an electrode for discharge surface treatment.
- C with an average particle size of 1 m or less.
- an electrode for discharge surface treatment was manufactured according to the flow chart shown in FIG. 4 of the first embodiment.
- an electrode formed of a powder having a small particle diameter is used, and the film is formed by a discharge pulse of relatively small energy. It is desirable to carry out.
- the discharge pulse applied between the electrode and the workpiece is as shown in FIGS. 3A and 3B.
- FIGS. 3A and 3B schematically show the case where the current pulse is a rectangular wave, it goes without saying that the same can be said for other waveforms.
- the energy of the discharge pulse can be roughly compared by the product of the discharge pulse width t e and the peak current value i e.
- FIG. 18 is a graph showing the relationship between the particle size of the powder constituting the electrode and the porosity of the coating.
- the horizontal axis indicates the particle size (Mm) of the powder constituting the electrode
- the vertical axis indicates the porosity in the coating formed by the electrode having the particle size on the horizontal axis.
- the discharge conditions that allow the formation of the finest film differ depending on the factors that make up the electrode, such as the particle size of the powder and the material of the powder.However, as schematically shown in Fig. 18, the particle size of the electrode and the porosity of the film The relationship is that the porosity decreases as the particle size decreases.
- the density of the coating increased from around 1 or less, and it became possible to form a coating that hardly existed in the space. This is because when the particle size becomes smaller, the material can be sufficiently melted by a discharge pulse with a small energy, and the electrode material arrives at the work as small molten metal particles, so it is possible to deposit and reduce the gap. It can be considered that it is.
- FIG. 19 is an SEM photograph showing a cross section of a film formed by discharge surface treatment using an electrode manufactured from a Co-based alloy powder having a particle diameter of 7 im.
- This Co-based alloy is a Co-based alloy containing Cr, Ni, W and the like.
- the condition of the discharge pulse at this time is such that the discharge pulse width t e is 8 s and the peak current value ⁇ e is 10 A, and the energy is relatively small.
- the coating formed on the workpiece has almost no space. In FIG. 19, the coating was formed by using a Co alloy electrode, but the same result could be obtained with an electrode made of Co powder.
- the same electrode is used to perform a discharge surface treatment with a pulse having a large energy, for example, a discharge pulse width te of about 60 ⁇ s, the discharge energy will increase (approximately 7.5 times). However, the porosity increases. Therefore, it was confirmed that the porosity differs depending on the discharge pulse conditions even for the same electrode.
- the discharge pulse conditions are as follows: discharge pulse width te 20 ⁇ s or less, peak current value ie 30 A or less, more preferably Is the discharge pulse width te about 10 s, the peak current value ie 1 It was confirmed that OA was better. If the discharge pulse condition is larger than such a condition, the space in the coating increases or cracks increase, which is not desirable.
- the proportion of the large-diameter powder to be mixed is about 20% by volume. That is, powder of 1 m or less needs to be about 80% or more.
- the discharge surface treatment is performed by using a compact formed of a metal or alloy powder having an average particle size of 1 ⁇ m or less as an electrode, thereby forming a thick film to be formed.
- This has the effect of increasing the density and forming a layer coating in which almost no space exists. And the coating thus formed becomes extremely strong.
- a thick film is formed by pulse discharge using an electrode manufactured from a material containing a metal component as a main component.
- oil when oil is used as a working fluid, if a material that easily forms carbides is contained in a large amount in the electrode, it reacts with carbon in the oil to form carbides. It has been found that it is difficult to form a thick film. Therefore, when a film is formed by an electrode manufactured using a powder of about several ⁇ m, a material such as Co, Ni, and Fe, which hardly forms a carbide, is included in the electrode to achieve a high density. However, when the particle size of the powder used for the electrode is reduced to about 1 m or less, 4 000742
- a thick film can be formed even by using an electrode composed of only a metal that easily forms carbide, for example, a powder of Mo.
- the pulse condition at this time was such that the discharge pulse ⁇ ⁇ te was 8 s and the peak current value ie was 10 A, and the energy / regulation was relatively small.
- the coating formed using an electrode made of Mo powder with a large particle size of about 4 tm which was tested as a comparative example, contained mostly molybdenum carbide and almost all metallic molybdenum.
- the film formed using the electrode made of Mo powder (0.7 ⁇ ) with a small particle size contained a large amount of molybdenum in a metallic state.
- the film in order to form a thick film, it is necessary for the film to contain a component in the form of a metal that has not been converted into a carbide or the like. From experiments, it has been confirmed that even a metal which is easily formed can be formed into a coating film without being deflected. The cause of this has not been clarified in many places, but by reducing the particle size, the energy of the discharge pulse for forming a dense film is reduced, and the small energy causes carbonization of the electrode material. Therefore, it is considered that the electrode material may form a coating without carbonization.
- the tenth embodiment even if the metal is easily carbonized, by performing a surface discharge treatment under a predetermined machining condition with a particle diameter of less than or equal to a predetermined value, the ratio of carbonization of the electrode material is reduced, and This has the effect that a very thick film can be formed. For this reason, the range of materials that can be formed into a thick film can be expanded, and a dense thick film can be formed without being limited to metals based on Co, Ni, and Fe. ' As described above, according to the present invention, an electrode was manufactured using powder having an average particle diameter of 3 ⁇ m or less, so that there was no variation in hardness and the electrode could be manufactured.
- a uniform thick film such as a film exhibiting lubricity in a high temperature environment can be formed.
- an electrode having no variation in hardness can be formed, so that the electrode cost can be reduced.
- an electrode powder suitable for discharge surface treatment using various materials it is possible to produce an electrode powder suitable for discharge surface treatment using various materials, and to obtain a stable discharge with an electrode produced from the electrode. Also, by performing discharge surface treatment using this electrode, films of various materials can be produced. Further, according to the present invention, it is possible to form a uniform film while having a uniform composition. 'Furthermore, by performing discharge surface treatment using an electrode for discharge surface treatment manufactured using powder with an average particle diameter of 1 ⁇ m, a uniform and dense thick film can be formed. Industrial applicability
- the present invention is suitable for a discharge surface treatment apparatus capable of automating a process of forming a thick film on a work surface.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
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Abstract
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
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CN2004800148728A CN1798870B (zh) | 2003-05-29 | 2004-01-28 | 放电表面处理用电极、放电表面处理用电极的制造方法、放电表面处理装置和放电表面处理方法 |
US10/558,384 US20070068793A1 (en) | 2003-05-29 | 2004-01-28 | Electrode for discharge surface treatment, manufacturing method for electrode for discharge surface treatment, discharge surface treatment apparatus, and discharge surface treatment method |
EP04705940.7A EP1643007B1 (en) | 2003-05-29 | 2004-01-28 | Discharge surface treatment electrode and process for its manufacture |
JP2005506446A JP4523545B2 (ja) | 2003-05-29 | 2004-01-28 | 放電表面処理用電極、放電表面処理装置および放電表面処理方法 |
TW093104213A TWI265062B (en) | 2003-05-29 | 2004-02-20 | Electrode for discharge surface treatment, method for making an electrode for discharge surface treatment, discharge surface treatment apparatus and method |
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JP2003152578 | 2003-05-29 | ||
JP2003-152578 | 2003-05-29 | ||
JP2003-160506 | 2003-06-05 | ||
JP2003160506 | 2003-06-05 | ||
JP2003166015 | 2003-06-11 | ||
JP2003166013 | 2003-06-11 | ||
JP2003-166015 | 2003-06-11 | ||
JP2003-166013 | 2003-06-11 |
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WO2004106587A1 true WO2004106587A1 (ja) | 2004-12-09 |
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PCT/JP2004/000742 WO2004106587A1 (ja) | 2003-05-29 | 2004-01-28 | 放電表面処理用電極、放電表面処理用電極の製造方法、放電表面処理装置および放電表面処理方法 |
Country Status (6)
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US (1) | US20070068793A1 (ja) |
EP (1) | EP1643007B1 (ja) |
JP (1) | JP4523545B2 (ja) |
CN (1) | CN1798870B (ja) |
TW (1) | TWI265062B (ja) |
WO (1) | WO2004106587A1 (ja) |
Cited By (3)
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WO2010119865A1 (ja) * | 2009-04-14 | 2010-10-21 | 株式会社Ihi | 放電表面処理用電極及びその製造方法 |
WO2011027825A1 (ja) * | 2009-09-03 | 2011-03-10 | 株式会社Ihi | 放電表面処理 |
JP2015140461A (ja) * | 2014-01-29 | 2015-08-03 | 株式会社Ihi | 放電表面処理用の電極及びその製造方法 |
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EP1544321B1 (en) * | 2002-09-24 | 2016-08-10 | IHI Corporation | Method for coating sliding surface of high temperature member |
US9284647B2 (en) * | 2002-09-24 | 2016-03-15 | Mitsubishi Denki Kabushiki Kaisha | Method for coating sliding surface of high-temperature member, high-temperature member and electrode for electro-discharge surface treatment |
CA2483528C (en) * | 2002-10-09 | 2015-07-21 | Ishikawajima-Harima Heavy Industries Co., Ltd. | Rotating member and method for coating the same |
KR100753273B1 (ko) * | 2003-06-10 | 2007-08-29 | 미쓰비시덴키 가부시키가이샤 | 방전 표면 처리용 전극과 그 평가 방법, 및 방전 표면 처리방법 |
RU2365677C2 (ru) * | 2005-03-09 | 2009-08-27 | АйЭйчАй КОРПОРЕЙШН | Способ обработки поверхности и способ ремонта |
KR101108818B1 (ko) * | 2006-09-11 | 2012-01-31 | 가부시키가이샤 아이에이치아이 | 방전표면처리용 전극의 제조방법 및 방전표면처리용 전극 |
WO2010095590A1 (ja) * | 2009-02-18 | 2010-08-26 | 株式会社Ihi | 電極の製造方法及びこれを利用した放電表面処理 |
US20130292612A1 (en) * | 2011-11-22 | 2013-11-07 | Mitsubishi Electric Corporation | Electrode for electric-discharge surface treatment and method for forming electrode for electric-discharge surface treatment |
US9573192B2 (en) * | 2013-09-25 | 2017-02-21 | Honeywell International Inc. | Powder mixtures containing uniform dispersions of ceramic particles in superalloy particles and related methods |
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CN108927595B (zh) * | 2017-05-24 | 2020-09-25 | 宝山钢铁股份有限公司 | 一种用于线切削电极轮的修磨和电灼加工系统 |
CN111394722B (zh) * | 2020-03-25 | 2022-03-25 | 广东工业大学 | 一种多尺度碳化钛颗粒增强铜基复合涂层及其制备方法和应用 |
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JP2015140461A (ja) * | 2014-01-29 | 2015-08-03 | 株式会社Ihi | 放電表面処理用の電極及びその製造方法 |
Also Published As
Publication number | Publication date |
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EP1643007A4 (en) | 2009-07-29 |
EP1643007A1 (en) | 2006-04-05 |
TWI265062B (en) | 2006-11-01 |
JP4523545B2 (ja) | 2010-08-11 |
CN1798870A (zh) | 2006-07-05 |
EP1643007B1 (en) | 2014-01-15 |
CN1798870B (zh) | 2011-10-05 |
JPWO2004106587A1 (ja) | 2006-07-20 |
TW200425985A (en) | 2004-12-01 |
US20070068793A1 (en) | 2007-03-29 |
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