EP3047925B1 - Surface treatment method for powdered metal material - Google Patents

Surface treatment method for powdered metal material Download PDF

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Publication number
EP3047925B1
EP3047925B1 EP14845712.0A EP14845712A EP3047925B1 EP 3047925 B1 EP3047925 B1 EP 3047925B1 EP 14845712 A EP14845712 A EP 14845712A EP 3047925 B1 EP3047925 B1 EP 3047925B1
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EP
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Prior art keywords
metal material
powdery metal
powdery
powder
ejection
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EP14845712.0A
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German (de)
English (en)
French (fr)
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EP3047925A4 (en
EP3047925A1 (en
Inventor
Yoshio Miyasaka
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Fuji Kihan Co Ltd
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Fuji Kihan Co Ltd
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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
    • 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
    • B22F1/14—Treatment of metallic powder
    • 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
    • B22F1/14—Treatment of metallic powder
    • B22F1/142—Thermal or thermo-mechanical treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00—Other disintegrating devices or methods
    • B02C19/06—Jet mills
    • 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
    • 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
    • B22F2009/045—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by other means than ball or jet milling
    • 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
    • B22F2207/00—Aspects of the compositions, gradients
    • B22F2207/11—Gradients other than composition gradients, e.g. size gradients
    • B22F2207/13—Size gradients
    • 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
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/05—Light metals
    • B22F2301/052—Aluminium
    • 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
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/10—Copper
    • 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
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/35—Iron
    • 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
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24C—ABRASIVE OR RELATED BLASTING WITH PARTICULATE MATERIAL
    • B24C1/00—Methods for use of abrasive blasting for producing particular effects; Use of auxiliary equipment in connection with such methods
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0205—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips of ferrous alloys

Definitions

  • the present invention relates to a method for surface treatment of a powdery metal material used as a material in manufacture of a metal product or in formation of coating using metal powder such as powder metallurgy such as sintering or thermal spraying.
  • the "sintering”, i.e., obtaining sintered metal by heating and solidifying an aggregate of a powdery metal material at a temperature lower than a melting point is widely used as a type of powder metallurgy for manufacturing various mechanical components such as gears, and particularly recently, use of the powdery metal material as a shaping material in a 3D printer is proposed.
  • Non-Patent Document 1 molding of a desired three-dimensional cubic model directly by the metal material from shape data such as CAD by irradiating a laser beam or an electron beam to a powdery metal material in a predetermined pattern and then sintering it (Non-Patent Document 1), and in the three-dimensional cubic model manufactured by sintering of the powdery metal material as above, unlike a resin model which has been manufactured by a prior-art 3D printer, application not only as a model or a sample but also a direct use as components to be incorporated in a machine or the like are expected.
  • sintered metal obtained by sintering the powdery metal material can easily have a density and strength lower than a case of melt molding due to occurrence of residual pores and the like, and it cannot be used in practice as a mechanical component as it is in many cases.
  • Non-Patent Documents 2 and 3 Non-Patent Documents 2 and 3
  • the mechanical milling treatment by a ball mill is performed to the powdery metal material having a predetermined crystalline structure as illustrated in Fig. 6A so as to apply severe plastic deformation to the powdery metal material in a concentrated manner, a region called a shell formed by refining crystal grains (hereinafter this region shall be referred to as a "fine grain region” ) is generated in the vicinity of a surface of the powdery metal material as illustrated in Fig. 6B , and as a result, a powdery metal material can be obtained provided with a region at a center part called a core maintaining an original crystal grain diameter (hereinafter this region shall be referred to as a "coarse grain region”) and the aforementioned fine grain region covering this coarse grain region.
  • the obtained sintered metal is metal having a structure called "harmonic structure” in which a network-state structure formed of the fine grain regions of the powdery metal materials connected to each other and the coarse grain regions arranged harmonically in the fine grain regions as illustrated in Fig. 6C (in the present invention, such metal is called “harmonic structure metal”) is obtained, and it has been reported that in such harmonic structure metal, strength can be drastically improved while ductility equal to that of sintered metal having uniform equiaxed grain structure obtained by using a normal powdery metal material to which the mechanical milling treatment is not applied is maintained (Non-Patent Document 2).
  • the formed metal coating can also be made the “harmonic structure metal” even if the metal coating is formed on the surface of a base material by "thermal spraying".
  • Non-Patent Documents 2 and 3 when sintering is to be performed by using the powdery metal material subjected to stirring by a ball mill in advance, the sintered metal obtained by the sintering has the "harmonic structure" so that metal having excellent characteristics of both high ductility and high strength is obtained.
  • Non-Patent Documents 2 and 3 when the powdery metal material is treated by the ball mill, treatment efficiency is extremely poor, and treatment time is 100 hours in Non-Patent Document 2 and 32 hours in Non-Patent Document 3 as examples.
  • the treatment of the powdery metal material by the ball mill has a risk of powder dust explosion and is an extremely dangerous work.
  • the powdery metal material used for sintering and the like has a fine grain diameter at approximately 100 ⁇ m in general, if the powdery metal material is contained in the ball mill, stirred under presence of air and subject to a friction force or an impact force, discharge of static electricity generated by friction in stirring can cause powder dust explosion.
  • the powder dust explosion here occurs when the following three elements: presence of oxygen; generation of dusts at explosion lower limit density or more; and presence of ignition source are all satisfied and thus, if occurrence of the powder dust explosion is to be prevented, one or more of these conditions need to be eliminated.
  • the work should be performed in a state in which oxygen is eliminated by filling an inside of the ball mill with an inactive gas or the like, or an input amount of the powdery metal material should be adjusted so as to be less than the explosion lower limit density, or the both should be done.
  • the powdery metal material used for sintering or thermal spraying is manufactured by an atomizing method in general, but since in this atomizing method, the powdery metal material is manufactured by spraying/scattering molten metal for refining and by instantaneously rapid cooling/solidifying it, the oxidized scale adheres to the surface of the powdery metal material.
  • an oxidized film which is a surface oxide is also formed more or less by contact with oxygen in the air.
  • the exfoliated oxides are continuously stirred together with the powdery metal material in the ball mill, a part of the exfoliated oxides is pressed onto the surface of the powdery metal material by friction or impact caused by stirring and adheres thereto again by being embedded or the like.
  • the powdery metal material treated by the ball mill is taken out as it is and used for sintering, improvement of strength is suppressed by presence of the oxides mixed in the powdery metal material.
  • the powdery metal material after the treatment by the ball mill can be subjected to wind-power sorting or the like, for example, but with this method, another process for further eliminating the oxides needs to be provided in addition to the treatment by the ball mill, whereby productivity is further lowered.
  • the oxides mixed in the powdery metal material can be removed to some degree, the oxides re-adhering to the surface of the powdery metal material cannot be separated/removed.
  • the present invention was made in order to overcome the disadvantages in the aforementioned prior-art techniques and has an object to provide a method defined by the appended claim 1 without a concern of powder dust explosion and can perform exfoliation of oxides from the surface and removal of the oxides after the exfoliation easily and reliably and also efficiently in a relatively short time.
  • a method for surface treatment of a powdery metal material for manufacture of harmonic structure metal in which a fine grain region and a coarse grain region are harmonically is defined by the appended claim 1.
  • the collected powder dusts are stored with nonflammable powder, such as calcium carbonate or the like.
  • the ejection powder and the object to be collided may be exchanged each other, i.e., the blasting may be performed by using the powdery metal material as the ejection powder and the medium substance as the object to be collided; and the blasting may be performed by using the medium substance with a powdery shape as the ejection powder and the powdery metal material as the object to be collided.
  • the medium substance may be made a powdery metal material of the same material and the same average grain diameter as the powdery metal material, and the ejection powder and the object to be collided may be both made into the powdery metal material.
  • a material of the medium substance may be metal having hardness equal to or higher than hardness of the powdery metal material or ceramic having hardness equal to or higher than hardness of the powdery metal material after the surface treatment.
  • the means provided with a cyclone for classifying the powder dusts from the ejected powder is to be used as dust collecting means for the blasting, even if the powdery metal powder and the exfoliated surface oxides are collected in the mixed state, the surface oxides can be classified with the powder dusts from the ejected powder and collected so that the powdery metal material from which the surface oxides are removed with higher accuracy could be obtained.
  • This blasting may be so configured that the powdery metal material as the ejection powder is ejected to the medium substance and made to collide against said medium substance, or that the medium substance as the ejection powder is ejected to the powdery metal material and is made to collide against said powdery metal material, but when it is so configured that both the ejection powder and an object to be collided are made to be a powdery metal material having the same average grain diameter and formed of the same material and the powdery metal material is ejected to and is made to collide against the powdery metal material, the surface treatment is applied to both the powdery metal powder as the ejection powder and the powdery metal powder as the object to be collided, and a throughput could be doubled.
  • the present invention is to remove surface oxides such as an oxidized scale prohibiting improvement of strength in sintering or thermal spraying from a surface of a powdery metal material and to form a fine grain region having a crystal grain diameter smaller than the crystal grain diameter at a center part in the vicinity of the surface of the powdery metal material by performing blasting of repeatedly causing the powdery metal material which is a treatment target and a medium substance which collides against the powdery metal material to collide against each other at a predetermined ejection speed by means of a known blasting machine.
  • a metal product obtained by a method of powder metallurgy such as sintering or metal coating manufactured by thermal spraying by using a powdery metal material in which a coarse grain region having a relatively large crystal grain diameter is formed at the center part and a fine grain region with a smaller crystal grain diameter than that of the coarse grain region is formed in the vicinity of the surface become harmonic structure metal having a crystalline structure [see Fig. 6C ] in which the coarse grain regions are harmonically arranged in a network of a fine grain structure formed by binding the fine grain regions and exhibiting an excellent characteristic that both high ductility and high strength are realized.
  • the powdery metal material which is a treatment target in the present invention is powdery metal having an average grain diameter of 10 to 200 ⁇ m to be used as a material in powder metallurgy as sintering or thermal spraying, and various materials can be used as long as it is applicable to powder metallurgy or thermal spraying.
  • the material may be constituted by either one of pure metal and an alloy.
  • metal used for powder metallurgy in general includes iron-, copper-, stainless-, titanium-, and tungsten-based metal and metal used for thermal spraying in general includes zinc, aluminum, copper and the like. They can be all included in the material of the powdery metal material in the present invention.
  • the powdery metal material to be used can be manufactured by various methods, e.g. spraying methods represented by an atomizing method which is a manufacturing method of the powdery metal material used in general in the powder metallurgy and thermal spraying, and various known methods such as mechanical crushing, electrolytic deposition and the like.
  • spraying methods represented by an atomizing method which is a manufacturing method of the powdery metal material used in general in the powder metallurgy and thermal spraying
  • various known methods such as mechanical crushing, electrolytic deposition and the like.
  • a shape of the powder may be spherical but this is not limiting and those with various shapes can be used.
  • the crystal grain diameter of the powdery metal material before treatment is a crystal grain diameter of the aforementioned coarse grain region as it is, and if the crystal grain diameter of the coarse grain region is set within a predetermined range, a powdery metal material with a corresponding crystal grain diameter is selected. Though not particularly limiting, the average crystal grain diameter of the coarse grain region is several to several tens ⁇ m as an example.
  • various substances can be used as long as it has hardness equal to or higher than that of the powdery metal material, and not only those made of metal but those made of ceramic can be used.
  • the medium substance made of ceramic not subjected to work hardening is to be used, it is preferable that ceramic having hardness equal to or higher than that of the powdery metal material after the surface treatment of the present invention is used so that the powdery metal material can maintain the same or improved hardness after the work hardening.
  • the aforementioned fine grain region may be formed in the both of the powdery metal material as the treatment target and the powdery metal material as the medium substance by collision between the powdery metal materials.
  • a shape of the medium substance needs to be constituted as powder when the medium substance is to be used as the ejection powder, but when the treatment is to be performed by using the aforementioned powdery metal material as the ejection powder, the medium substance does not have to be powder but may be constituted in a form of a plate body or the like.
  • the collision between the powdery metal material and the medium substance described above is made by blasting means of the blasting machine.
  • the powdery metal material is ejected as the ejection powder to the medium substance and made to collide against said medium substance, or to the contrary, a powdery medium substance may be prepared as the ejection powder and ejected to the powdery metal material so as to cause a collision against said powdery metal material.
  • the ejection powder and the object to be collided are both constituted by the powdery metal material having the same average grain diameter and made of the same material, and the powdery metal materials are made to collide against each other.
  • blasting machine 1 those with various known constitution can be used as long as it is a blasting machine having a cabinet 21 as a processing chamber and a dust collection function of suctioning an inside of the cabinet 21 for dust collection, and the blasting machine of either one of a direct pressure type and a gravity type may be used.
  • FIG. 1A and Fig. 1B A constitution example of the gravity type blasting machine 1 and a constitution example of the direct pressure type to be used for the surface treatment of the present invention are illustrated in Fig. 1A and Fig. 1B , respectively.
  • the blasting machine 1 used in the method for surface treatment of the present invention is not limited to illustrated constitution.
  • the blasting machine 1 illustrated in Figs. 1A and 1B comprises: the cabinet 21 which becomes a processing chamber for accommodating an ejection nozzle 22 and a workpiece and performing blasting; and a dust collecting machine 38 for suctioning an inside of this cabinet 21.
  • the blasting machine 1 is provided with a cyclone type collection tank 23 between this dust collecting machine 38 and the cabinet 21 for collecting into the collection tank 23 the powdery metal material collected by suctioning of the inside of the cabinet 21 in a state mixed with powder dusts and can collect into the dust collecting machine 38 the powder dusts separated from the powdery metal material in the cyclone type collection tank 23.
  • a barrel basket 24 which is a container rotating during ejection of the ejection powder and opened upward is provided, and the powdery metal material which is the object to be collided can be input therein.
  • this barrel basket 24 is depicted as a mesh with a large number of small pores formed, but the illustrated example is not limiting, and the barrel basket may be constituted without such small pores.
  • the powdery metal material Prior to the treatment by means of the blasting machine 1 constituted as above, the powdery metal material is contained in the collection tank 23 and the powdery metal material is also contained in the barrel basket 24 provided in the processing chamber, and while the barrel basket 24 is rotated in this state, ejection of the powdery metal material from the ejection nozzle 22 is started at the ejection speed of 100 to 300 m/sec and then, the powdery metal material ejected from the ejection nozzle 22 collides against the powdery metal material in the rotating barrel basket 24.
  • An ejection pressure may be 100 m/sec or more in the treatment of a non-iron based powdery metal material, but 150 m/sec or more is preferable for the treatment of an iron-based powdery metal material.
  • the powdery metal material in the barrel basket 24 and the powdery metal material ejected from the ejection nozzle 22 mutually receive energy at the collision so that surface oxides such as oxidized scale formed on the surface of the powdery metal materials are exfoliated. Also, the temperature of the surface in the collision portion is rapidly raised and also cooled so that the crystal grains on the surface of the collision portion are refined, and a fine grain region is formed in which a crystal grain with a diameter smaller than that of the crystal grain on a center portion of the powdery metal material is formed in the vicinity of the surface of the powdery metal material.
  • the fine grain region of the powdery metal material is formed on the surface of the powdery metal material to a depth of approximately 20% at the maximum with respect to the grain diameter if the powdery metal material as the treatment target is less than 100 ⁇ m and formed to a depth of approximately 10% at the maximum with respect to the grain diameter if the powdery metal material as the treatment target is 100 ⁇ m or more, and thus, in the method for surface treatment of the present invention with the powdery metal material having an average grain diameter of 10 to 200 ⁇ m as the treatment target, the aforementioned fine grain region is formed within a range of 2 to 20 ⁇ m from the surface at the maximum depending on the grain diameter of the powdery metal material as the treatment target.
  • the powdery metal material ejected from the ejection nozzle 22 collides against the powdery metal material in the barrel basket 24 and then, accumulates in the barrel basket 24 except those forced out to outside the barrel basket 24 and is stirred with rotation of the barrel basket 24 with the powdery metal material having been originally present in the barrel basket 24.
  • the powdery metal material in the barrel basket 24 increases and overflows from the barrel basket 24 and drops to a bottom part of the cabinet 21.
  • the bottom part of the cabinet 21 is formed as a hopper having an inverted trapezoidal shape, and a lower end of the hopper communicates with the dust collecting machine 38 through an exhaust air passage 33 and the collection tank 23 and thus, when the inside of the cabinet 21 is suctioned by a ventilator 39 provided in the dust collecting machine 38, the dropped powdery metal material and powder dusts are suctioned with the air in the cabinet 21 and supplied into the cyclone type collection tank 23, the powder dusts and the powdery metal material are classified in this collection tank 23 and the powdery metal material is collected downward in the collection tank 23.
  • the surface oxides such as oxidized scale generated on the surface of the powdery metal material are harder and more fragile as compared with the powdery metal material. Therefore, the surface oxides are finely crushed when they are exfoliated by an impact caused by a collision between the powdery metal materials. Thus, the surface oxides are not collected in the collection tank 23 but sent to the dust collecting machine 38 as powder dusts through a pipe 32 connected to an upper part of the collection tank 23 and collected downward in the dust collecting machine 38, and clean air is discharged to the outside air by the ventilator 39.
  • the inside of the processing chamber formed in the cabinet 21 is suctioned at all times, and the powder dusts and the powdery metal material floating in the air are removed and kept to the explosion lower limit density or less.
  • the powder dust explosion in the cabinet even by heat generation by ejection, collision and friction of the ejection powder which is the powdery metal material or generation of static electricity in this embodiment.
  • the powder dusts classified in the cyclone type collection tank 23 and collected in the dust collecting machine 38 are accommodated in the dust collecting machine 38 with an nonflammable powder such as powder of calcium carbonate, for example, so that a density of flammable powder dusts in the air in the dust collecting machine 38 becomes the explosion lower limit density or less, whereby a risk of powder dust explosion in the dust collecting machine 38 is also avoided.
  • an nonflammable powder such as powder of calcium carbonate
  • the powdery metal material collected in the collection tank 23 is ejected again by the ejection nozzle 22 toward the powdery metal material in the barrel basket 24, and the aforementioned process is repeated so that the surface oxides such as oxidized scale are removed from the surfaces of any powdery metal materials, and the fine grain region is formed so as to cover the entirety in the vicinity of the surface.
  • harmonic structure metal in which the coarse grain region is harmonically arranged in the network of the fine grain structures formed by mutually connecting parts of the fine grain regions is obtained.
  • harmonic structure metal excellent characteristics of realization of both the high ductility and high strength are obtained.
  • the surface oxides such as oxidized scale causing lowered strength in sintering or deposition can be favorably removed and thus, strength of the obtained sintered metal or metal coating can be further improved.
  • the constitution is described in which the ejection powder and the object to be collided are both the powdery metal materials and the ejection powder and the object to be collided are made to collide against each other in the barrel basket 24 provided in the cabinet 21, but a plate body formed of a material having hardness equal to or higher than that of the ejection powder is accommodated as the medium substance in the cabinet 21 instead of the aforementioned barrel basket 24, and the surface treatment of the present invention may be configured to be performed by ejecting the powdery metal material as the ejection powder to this plate body and making to collide against the same.
  • the aforementioned blasting machine 1 provided with the barrel basket 24 is used, a powdery medium substance is used as the ejection powder, and the medium substance as the ejection powder is ejected to the powdery metal material contained in the barrel basket 24, and in this case, the powdery metal material and the medium substance are classified after the treatment and collected, respectively.
  • the stainless powder in 10 kg was contained in the barrel basket provided in the processing chamber of the blasting machine and 20 kg into the collection tank, and the treatment of ejecting the stainless powder in the collection tank by the ejection nozzle into the barrel basket was performed continuously for 3 hours under the condition shown in the aforementioned Table 1.
  • Refining of the crystal grain diameter can be evaluated from an increase of a line width of an X-ray analysis peak using the Scherrer (Sherrer, 1918) formula.
  • the line width of the peak drastically increased with respect to the X-ray analysis result (see Fig. 2 ) of the untreated stainless powder.
  • the method for surface treatment of the present invention was performed to a powder high-speed tool steel (SKH equivalent: #150) as the powdery metal material.
  • the treatment conditions are shown in Table 2 below: TABLE 2 Treatment conditions for Example 2 (Powder high-speed tool steel: SKH equivalent) Blasting machine Type Gravity type ("SGK-4LD" by Fuji Manufacturing Co., Ltd.) Barrel basket made of SUS304, no pores, 4 rotations per minute Nozzle Nozzle diameter: ⁇ 9 mm Oscillation: 100 mm in width, 60 times per minute Powdery metal material Material Powder high-speed tool steel ("SPM30" by Sanyo Special Steel Co., Ltd.) (1.3%C 4.0%Cr 5%Mo 6%W 3%V 8%Co) Grain diameter #150 (44 to 125 ⁇ m / 85 ⁇ m on average) Medium substance Same as powdery metal material Blasting conditions Ejection pressure 0.6 MPa Ejection speed 150m/sec or more Ejection distance 200 mm Ejection rate 5 kg/min Ejection time 5 hours Throughput
  • the powdery high-speed tool steel in 10 kg was contained in the barrel basket provided in the processing chamber of the blasting machine and 10 kg into the collection tank, and the treatment of ejecting the powdery high-speed tool steel in the collection tank by the ejection nozzle into the barrel basket was performed continuously for 5 hours under the conditions shown in the aforementioned Table 2.
  • the oxidized scale was removed and the surface was cleaned, and from the X-ray diffraction result, the line width of the X-ray analysis peak increased (see Fig. 5 ) as compared with the untreated one (see Fig. 4 ), and the refining of the surface structure by the treatment according to the method of the present invention was confirmed (see Figs. 4 and 5 ).
  • the method for surface treatment of the present invention was performed to powder of an alloy steel for mechanical structure (SCM equivalent: #150) as the powdery metal material.
  • the treatment conditions are shown in Table 3 below: TABLE 3
  • Example 3 Treatment conditions for powder of alloy steel for mechanical structure (SCM equivalent) Blasting machine Type Gravity type ("SGK-4LD" by Fuji Manufacturing Co., Ltd.) Barrel basket made of SUS304, no pores, 4 rotations per minute Nozzle Nozzle diameter: ⁇ 9 mm Oscillation: 100 mm in width, 60 times per minute Powdery metal material Material Alloy steel for mechanical structure (SCM equivalent) (0.23%C 0.2%Mo 1.5%Cr) Grain diameter #150(44 to 125 ⁇ m / 85 ⁇ m on average) Medium substance Same as powdery metal material Blasting conditions Ejection pressure 0.6 MPa Ejection speed 150 m/sec or more Ejection distance 200 mm Ejection rate 5 kg/min Ejection time 5 hours Throughput 20 kg
  • the power of alloy steel for mechanical structure in 10 kg was contained in the barrel basket provided in the processing chamber of the blasting machine and 10 kg into the collection tank, and the treatment of ejecting the powder of the alloy steel for mechanical structure in the collection tank by the ejection nozzle into the barrel basket was performed continuously for 5 hours under the conditions shown in the aforementioned Table 3.
  • the oxidized scale was removed and the surface was cleaned, and it is considered from the aforementioned rise of hardness that the refined structure is formed on the surface.
  • the method for surface treatment of the present invention was performed to powder of the copper alloy (#150) as the powdery metal material.
  • the copper alloy powder in 20 kg was contained in the collection tank, and the treatment of ejecting the copper alloy powder in the collection tank by the ejection nozzle toward a position where a core was shifted by 100 mm from a center of a plate ( ⁇ 400 mm, thickness 20 mm) made of SKD11 arranged in the processing chamber was performed for 7 hours continuously.
  • the oxidized scale was removed and the surface was cleaned, and it is considered from the aforementioned rise of hardness that the refined structure is formed on the surface.
  • the method for surface treatment of the present invention was performed to powder of aluminum alloy (AC8A: #80) as the powdery metal material.
  • the treatment conditions are shown in Table 5 below: TABLE 5 Treatment conditions for Example 5: Aluminum alloy (AC8A) Blasting machine Type Gravity type ("SGK-4LD" by Fuji Manufacturing Co., Ltd.) Barrel basket made of SUS304, with ( ⁇ 1 mm pores, 4 rotations per minute Nozzle Nozzle diameter: ⁇ 9 mm Oscillation: 100 mm in width, 60 times per minute Powdery metal material Material
  • Grain diameter #80 (105 to 250 ⁇ m / 177 ⁇ m on average)
  • Medium substance Shot made of a high speed steel (#400, 45 ⁇ m on average) Blasting conditions Ejection pressure 0.4 MPa Ejection speed 100 m/sec or more Ejection distance 200 mm Ejection rate 4 kg/min Ejection time 7 hours
  • a barrel basket in which a large number of holes, each having a diameter of 1 mm, are formed was provided in the processing chamber, and the powder of the aluminum alloy (AC8A) was input in 10 kg into this barrel basket, and a treatment of ejecting a shot made of a high speed steel collected in the collection tank into the barrel basket was performed for 7 hours continuously.
  • AC8A aluminum alloy
  • the oxidized scale was removed and the surface was cleaned, and from the aforementioned rise of hardness, it is considered that a component of the high speed steel which is the medium substance is diffused and penetrated into the surface of the powder of the aluminum alloy and the refined structure was formed on the surface.
  • discharge plasma sintering was performed by using the powdery metal material treated by the method for surface treatment of the present invention described as above as Examples 1 to 5.
  • the method for surface treatment of the present invention is a method for surface treatment which can treat the powdery metal material used for manufacture of the harmonic structure metal simply, in a large quantity and moreover, safely.
EP14845712.0A 2013-09-18 2014-09-17 Surface treatment method for powdered metal material Active EP3047925B1 (en)

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JP2013193254A JP5723942B2 (ja) 2013-09-18 2013-09-18 粉末状金属材料の表面処理方法
PCT/JP2014/074518 WO2015041236A1 (ja) 2013-09-18 2014-09-17 粉末状金属材料の表面処理方法

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11845128B2 (en) 2018-06-08 2023-12-19 Hewlett-Packard Development Company, L.P. Powder bed materials

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160236422A1 (en) * 2015-02-13 2016-08-18 Ricoh Company, Ltd. Device and method for removing powder and apparatus for fabricating three-dimensional object
US10913206B2 (en) * 2015-08-03 2021-02-09 Delavan, Inc Systems and methods for post additive manufacturing processing
JP6848521B2 (ja) 2017-02-24 2021-03-24 セイコーエプソン株式会社 金属粉末射出成形用コンパウンド、焼結体の製造方法および焼結体
JP6969113B2 (ja) 2017-03-06 2021-11-24 セイコーエプソン株式会社 金属粉末射出成形用コンパウンド、金属粉末成形体、焼結体の製造方法および焼結体
JP6961972B2 (ja) * 2017-03-24 2021-11-05 富士フイルムビジネスイノベーション株式会社 立体形状成形装置、情報処理装置及びプログラム
TWI638480B (zh) * 2017-10-25 2018-10-11 國立虎尾科技大學 Electrode electrode chip process
CN116571762A (zh) 2018-05-30 2023-08-11 株式会社东芝 3d打印机用金属粉、造型物及造型物的制造方法
JP7164163B2 (ja) * 2018-08-24 2022-11-01 学校法人立命館 炭素含有鉄合金材の製造方法及び炭素含有鉄合金材
WO2020059059A1 (ja) * 2018-09-19 2020-03-26 技術研究組合次世代３Ｄ積層造形技術総合開発機構 金属積層造形用粉末およびその製造方法と、積層造形装置およびその制御プログラム
CN110284105B (zh) * 2019-06-25 2024-02-09 郑州航空工业管理学院 一种粉体表面金属化方法及其装置
JP7470963B2 (ja) * 2020-01-27 2024-04-19 株式会社不二機販 焼結体のバインダ金属相強化方法
CN114535568A (zh) * 2022-02-25 2022-05-27 安徽工业大学 一种对还原铁粉进行高效循环表面纳米化的设备及方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02243701A (ja) * 1989-03-17 1990-09-27 Daido Steel Co Ltd 金属粉末の処理方法

Family Cites Families (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63293105A (ja) * 1987-05-27 1988-11-30 Nkk Corp 金属粉末の製造方法
JPH0822506B2 (ja) * 1987-06-10 1996-03-06 日鉱金属株式会社 亜鉛ブラストショットの製造方法
JPH0822504B2 (ja) * 1987-06-10 1996-03-06 日鉱金属株式会社 アルミダイカスト製品のシヨツトブラスト方法
JPH0761612B2 (ja) * 1988-11-22 1995-07-05 株式会社不二機販 沸騰水型原子力発電設備の発電用タービンの洗浄方法
JP3049165B2 (ja) * 1993-02-15 2000-06-05 株式会社不二製作所 粉末合金の表面層の処理法
JP3379824B2 (ja) * 1994-06-14 2003-02-24 株式会社不二機販 表面硬化金属ショットの製造方法
JP2978137B2 (ja) * 1997-09-01 1999-11-15 プラストロン株式会社 金属表面処理方法およびその処理を施した金属材
JP3730015B2 (ja) * 1998-06-02 2005-12-21 株式会社不二機販 金属成品の表面処理方法
JP2001225270A (ja) * 2000-02-10 2001-08-21 Fuji Seisakusho:Kk サンドブラスト装置及びサンドブラスト装置における研掃材の分級方法及び該方法におけるダスト捕集方法
JP2007297651A (ja) * 2006-04-27 2007-11-15 Fuji Wpc:Kk 硬質金属表面における結晶粒微細化方法
US20080176487A1 (en) * 2007-01-19 2008-07-24 Armstrong Jay T Portable cleaning and blasting system for multiple media types, including dry ice and grit
JP4719249B2 (ja) * 2008-06-11 2011-07-06 株式会社不二機販 表面酸化耐摩耗潤滑被膜及びその形成方法
JP5381045B2 (ja) * 2008-11-26 2014-01-08 新東工業株式会社 ショットピーニング用投射材の製造方法
US8893538B2 (en) * 2010-12-08 2014-11-25 Fuji Kihan Co., Ltd. Instantaneous heat treatment method for metal product

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02243701A (ja) * 1989-03-17 1990-09-27 Daido Steel Co Ltd 金属粉末の処理方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11845128B2 (en) 2018-06-08 2023-12-19 Hewlett-Packard Development Company, L.P. Powder bed materials

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EP3047925A4 (en) 2017-06-07
CN105339112B (zh) 2017-04-19
US20160193658A1 (en) 2016-07-07
EP3047925A1 (en) 2016-07-27
WO2015041236A1 (ja) 2015-03-26

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