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WO2006134980A1 - Matière pulvérulente en alliage de magnésium brut, alliage de magnésium présentant des limites d’élasticité élevées, procédé de production de matières pulvérulentes en alliage de magnésium brut, et procédé d - Google Patents

Matière pulvérulente en alliage de magnésium brut, alliage de magnésium présentant des limites d’élasticité élevées, procédé de production de matières pulvérulentes en alliage de magnésium brut, et procédé d Download PDF

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Publication number
WO2006134980A1
WO2006134980A1 PCT/JP2006/311952 JP2006311952W WO2006134980A1 WO 2006134980 A1 WO2006134980 A1 WO 2006134980A1 JP 2006311952 W JP2006311952 W JP 2006311952W WO 2006134980 A1 WO2006134980 A1 WO 2006134980A1
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WIPO (PCT)
Prior art keywords
magnesium alloy
magnesium
powder
alloy powder
raw material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
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PCT/JP2006/311952
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English (en)
Japanese (ja)
Inventor
Katsuyoshi Kondoh
Mitsuhiro Goto
Hideaki Fukui
Kantaro Kaneko
Shuji Shiozaki
Katsuhito Itakura
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kurimoto Ltd
Gohsyu Co Ltd
Original Assignee
Kurimoto Ltd
Gohsyu Co Ltd
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Application filed by Kurimoto Ltd, Gohsyu Co Ltd filed Critical Kurimoto Ltd
Priority to US11/922,226 priority Critical patent/US20090263268A1/en
Priority to CN2006800203616A priority patent/CN101193715B/zh
Priority to EP06766721A priority patent/EP1897638A4/fr
Publication of WO2006134980A1 publication Critical patent/WO2006134980A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES, PROFILES OR LIKE SEMI-MANUFACTURED PRODUCTS OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00—Extruding metal; Impact extrusion
    • B21C23/01—Extruding metal; Impact extrusion starting from material of particular form or shape, e.g. mechanically pre-treated
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES, PROFILES OR LIKE SEMI-MANUFACTURED PRODUCTS OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00—Extruding metal; Impact extrusion
    • B21C23/002—Extruding materials of special alloys so far as the composition of the alloy requires or permits special extruding methods of sequences
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • 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
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • 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
    • 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
    • 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
    • C22C1/0408—Light metal alloys
    • 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
    • C22C1/047—Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • B22F2003/208—Warm or hot extruding
    • 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
    • B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, 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
    • B22F2009/046—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 by cutting
    • 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

Definitions

  • the present invention relates to a magnesium alloy powder raw material, a magnesium alloy produced using the powder raw material, and a production method thereof, and particularly relates to a magnesium alloy that achieves both high yield strength and elongation and a production method thereof. is there.
  • Mg alloy Magnesium (hereinafter referred to as Mg) alloy, which is the lightest of industrial metal materials, uses its light weight effect to produce sports equipment, home appliances, aerospace equipment, and other machinery. Widely used for parts.
  • Mg alloys in order to apply Mg alloys to products and parts that require high reliability such as automobile parts, further increase in strength is required.
  • elongation in particular, there is a strong demand for improved proof stress in component design, and at the same time, it is necessary to achieve high elongation (toughness). In other words, by realizing high yield strength and high elongation, it is possible to replace the current lightweight aluminum alloy.
  • JP-A-2-182806 describes a method of extruding after solidifying the Mg alloy powder by hot pressing
  • JP-A-5-320715 discloses forming and extruding the Mg alloy powder. How to do is described.
  • the effect of the extrusion process is to refine the crystal grains constituting the base of the extruded Mg alloy.
  • Al 7.8 to 9.2 wt%
  • manganese (Mn) 0.12 to 0.35 wt%
  • zinc (Zn) 0.2 to 0 ⁇ 8% by weight
  • Mg remainder
  • AZ80 Magnesium alloy with the following composition: T6 heat-treated with cutting powder made by molding ⁇ Extrusion Mg alloy obtained at room temperature
  • Tensile strength is 3 82MPa and elongation is 27%.
  • T6 heat treatment is not applied, tensile strength is reported to be 330 MPa and elongation is 15%. .
  • the proof stress of the extruded material is 196 MPa when T6 heat treatment is performed.
  • the cause is considered as follows.
  • the Mg alloy crystal grains (50-700 ⁇ m) produced by the conventional melting * forging method recrystallization occurs and the crystal grains are refined by the extrusion process. Considering the data disclosed so far, it is about 10 to 20 xm. In order to improve the tensile strength, it is necessary to further refine the crystal grains.
  • miniaturization to 1 to 5 ⁇ m or less is effective in improving the resistance to light.
  • An Mg alloy having such a fine crystal grain size cannot be realized only by a manufacturing method in which a T6 heat-treated cutting powder is compacted and extruded.
  • the intermetallic compound Mg A1 which was precipitated and dispersed in the substrate by T6 heat treatment, was extruded.
  • An object of the present invention is to provide a magnesium alloy that achieves both high yield strength and elongation, and a method for producing the same.
  • Another object of the present invention is to provide a magnesium alloy powder raw material used for producing the magnesium alloy and a method for producing the same.
  • the magnesium alloy powder raw material according to the present invention is obtained by subjecting a starting raw material powder having a relatively large crystal grain size to plastic deformation by compressing or shearing it through a pair of rolls. It has a relatively small crystal grain size and is characterized by the following. That is, the starting material powder is a magnesium alloy powder in which fine intermetallic compounds are precipitated and dispersed in the substrate by heat treatment. In the magnesium alloy powder after plastic working, there is a working strain around the precipitated intermetallic compound. The maximum size of the magnesium alloy powder after plastic working is 10 mm or less, and the minimum size is 0.1 mm or more. The maximum crystal grain size of the magnesium particles constituting the base of the magnesium alloy powder after plastic molding is 20 ⁇ m or less.
  • the intermetallic compound is Mg Al, Al Ca, Mg Si, MgZn, Al Re (Re: 3 ⁇ 4r
  • the maximum particle size of the intermetallic compound is 5 x m or less, more preferably 2 x m or less.
  • the maximum crystal grain size of magnesium particles constituting the base of the magnesium alloy powder is 10 x m or less.
  • a high-magnesium-resistant magnesium alloy according to the present invention is obtained by compacting a magnesium alloy powder raw material having the above-described characteristics and then extruding it, and has the following characteristics. Yes. That is, the maximum grain size of the magnesium particles constituting the alloy substrate is 10 ⁇ m or less, and the tensile strength at room temperature is 250 MPa or more. [0017] Preferably, the maximum crystal grain size force of the magnesium particles constituting the base of the magnesium alloy is 3 ⁇ 4 ⁇ ⁇ or less, and the tensile strength at room temperature is 350 MPa or more.
  • Mg Al, Al Ca, Mg Si, MgZn, A in the base of the magnesium alloy is Mg Al, Al Ca, Mg Si, MgZn, A in the base of the magnesium alloy
  • Two intermetallic compounds are deposited and dispersed.
  • the magnesium alloy contains strontium (eg, zirconium), an active metal element selected from the group consisting of scandium (Sc) and titanium (Ti) in an amount of 0.5% to 4% on a weight basis. Contains the following.
  • the crystal grain size of the magnesium particles constituting the substrate of the starting raw material powder is reduced by subjecting the starting raw material powder to a plastic case.
  • This is a method of miniaturization and has the following characteristics. That is, a magnesium alloy powder in which fine intermetallic compounds are precipitated and dispersed in the substrate by heat treatment is prepared as a starting material powder.
  • the plastic working is a plastic working in which the starting raw material powder is passed through a pair of rolls and subjected to compression deformation or shear deformation to impart processing strain around the intermetallic compound. The plastic working is repeated until the maximum size of the powder is 10 mm or less, the minimum size is 0.1 mm or more, and the maximum crystal grain size of the magnesium particles constituting the powder substrate is 20 ⁇ m or less.
  • the step of preparing a magnesium alloy powder as a starting raw material powder includes preparing a magnesium alloy ingot by a forging method, solution treating the magnesium alloy ingot, and subsequently aging heat treatment.
  • preparing a magnesium alloy ingot by a forging method To deposit and disperse fine intermetallic compounds in the base of the ingot, and to remove the magnesium alloy powder from the ingot by machining.
  • the temperature of the starting raw material powder to be introduced and the surface temperature of the roll in contact with the starting raw material powder are set to be equal to or lower than the temperature of the aging heat treatment.
  • a method for producing a high-magnesium-resistant magnesium alloy according to the present invention includes a step of obtaining a compacted body by pressing a magnesium alloy powder raw material having the above-described characteristics in a state where the mold is filled, and magnesium The process of heating the compacted compact of the alloy at a temperature of 150 ° C or higher and 450 ° C or lower, and immediately after the heating, the compacted compact of the magnesium alloy is extruded to form the magnesium composite.
  • a process for producing gold includes a step of obtaining a compacted body by pressing a magnesium alloy powder raw material having the above-described characteristics in a state where the mold is filled, and magnesium The process of heating the compacted compact of the alloy at a temperature of 150 ° C or higher and 450 ° C or lower, and immediately after the heating, the compacted compact of the magnesium alloy is extruded to form the magnesium composite.
  • the maximum grain size of magnesium particles constituting the base of the magnesium alloy is not more than SlOm, and the tensile resistance at room temperature is not less than 50MPa. More preferably, the magnesium alloy powder compact is heated at a temperature of 200 ° C to 350 ° C.
  • FIG. 1 is an illustrative view showing a roller compactor device.
  • FIG. 2 is an illustrative view showing a state in which processing strain exists around an intermetallic compound.
  • FIG. 3 Structure photograph of AZ91D ingot, (a) Structure photograph after fabrication, (b) Structure photograph after solution heat treatment, (c) Structure after T6 heat treatment (solution + aging heat treatment) The photo is shown.
  • FIG. 4 is an enlarged structural photograph of the structure after T6 heat treatment.
  • FIG. 5 Structure photograph of AZ91D powder that has been subjected to plastic caulking with a roll.
  • A shows the structure after T6 treatment
  • (b) shows the structure after solution treatment. .
  • FIG. 6 A diagram showing test results of micro hardness (micro Vickers hardness) of powder.
  • FIG. 8 A structural photograph in the extrusion direction of an Mg alloy obtained by extruding and solidifying a powder that has been plasticized with a roll 3, 10, 20, 30 times.
  • the present invention has been made to solve the above-described conventional problems, and a magnesium alloy powder in which fine intermetallic compounds are precipitated and dispersed in a substrate by heat treatment is used as a starting material powder. By passing this between a pair of rolls and applying plastic working to compress and / or shear deform, a coarse Mg alloy powder with a fine structure is produced, and this is compacted and extruded. It is intended to provide a Mg alloy having a high tensile strength exceeding 250 to 350 MPa and a method for producing the same. [0027] (1) Starting material powder and production method thereof
  • Mg as the main component, and other elements that form intermetallic compounds such as Al, Mn, Zn, Re (rare earth elements), Ca, Si, strontium (Sr), zirconium (Zr), scandium (Sc) and
  • An Mg alloy ingot to which an active metal element selected from the group consisting of titanium (Ti) is added is produced by a forging method.
  • T6 heat treatment solution heat treatment + aging heat treatment
  • fine intermetallic compounds produced by each additive element are precipitated and dispersed in the substrate.
  • Precipitation ⁇ Dispersing intermetallic compound is, for example, Mg
  • Al Al, Al Ca, Mg Si, MgZn, Al Re (Re: rare earth elements), Al Re, Al Mn, etc.
  • intermetallic compounds are evenly dispersed in the base material of the Mg alloy after extrusion, it contributes to the improvement of the proof stress.
  • Active metal elements such as strontium (Sr), zirconium (Zr), scandium (Sc) and titanium (Ti) are 0.5 on a weight basis. / 0 or more 4. By containing less than / 0, the strength can be further increased.
  • the heat treatment conditions vary depending on the type of element to be added and the amount of the element to be added. Therefore, it is necessary to set appropriate conditions by observing the structure or measuring the hardness (age hardening curve).
  • a powder having a size of about 0.1 to 10 mm is collected from an Mg alloy ingot by mechanical cutting such as milling, and this is used as the starting material powder of the present invention.
  • the particle size of the powder is less than 0.1 mm, it tends to ignite, so from the viewpoint of safety, use a cutting powder of 0.1 mm or more, more preferably 0.5 mm or more.
  • the Mg alloy powder that has been subjected to the above T6 heat treatment is used as the starting raw material powder, and this is put into the single compactor device shown in Fig. 1.
  • a roller compactor device shown in FIG. 1 includes a case 11, a multistage roll rotating body 12 disposed in the case 11, a crushing device 13, a powder temperature / supply amount control system 14, and a cradle 15 and.
  • the multi-stage roll rotating body 12 constitutes a plastic working part that performs plastic working on the starting raw material powder, and has three pairs of rolls 12a, 12b, and 12c that perform rolling.
  • the starting material powder undergoes compression deformation and / or shear deformation when passing between the pair of rolls.
  • the starting raw material powder has a predetermined temperature and a predetermined The amount is adjusted and put into Case 11.
  • the predetermined temperature is equal to or lower than the temperature of the aging heat treatment described later.
  • the inside of the case 11 is kept in an inert gas atmosphere, a non-oxidizing gas atmosphere, or a vacuum atmosphere from the viewpoint of preventing oxidation of the powder surface.
  • the surface temperature of the multistage roll rotating body 12 and the atmospheric temperature in the case 11 are equal to or lower than the temperature of aging heat treatment described later.
  • the powder delivered from the roll pair 12c is subsequently crushed by the crushing device 13 into a granular powder.
  • the granular powder may be returned to the powder temperature / supply amount control system 14 again, and the plastic check by the multistage roll rotating body 12 may be repeated.
  • the processed granular powder is stored in the cradle 15.
  • the following structure control is performed by applying a plastic calorie in which the powder is passed between a pair of rolls to compress and / or shear.
  • the maximum size of the powder after plastic processing is 10 mm or less, and the minimum size of the powder is 0.1 mm or more.
  • the starting material powder is relatively smaller than the crystal grain size of magnesium.
  • the maximum crystal grain size of the magnesium particles constituting the powder base is 20 ⁇ m or less.
  • the Mg alloy powder raw material that has been subjected to the plastic casing by the roll is subjected to crushing-pulverization 'sizing treatment, and then plastic processing by the roll is performed again under the same conditions.
  • an Mg alloy powder raw material having the microstructure defined by the present invention is created.
  • JP-A-5-306404 a method of producing a Mg alloy member by extruding the compact after compacting the Mg alloy powder collected by cutting from an A1-containing Mg alloy member that has undergone T6 treatment with a hot press has proposed.
  • the strong plastic case as proposed in the present invention is forcibly applied to the cutting Mg alloy powder treated with T6.
  • fine crystal grains that cannot form the nucleation sites for dynamic recrystallization as described above cannot be obtained.
  • the tensile strength of the Mg alloy when using the AZ80 alloy cutting powder subjected to T6 heat treatment is as low as about 200 MPa.
  • the tensile strength of the extruded material when using AZ80 powder not subjected to T6 heat treatment is 200 MPa, which is not much different from that during T6 heat treatment. This is fundamentally different from the manufacturing method in which processing strain is preferentially accumulated around dispersed particles and used as a nucleation site for dynamic recrystallization.
  • processing strain is imparted in a random (disordered) direction by repeatedly performing a plastic cage with a pair of rolls on the powder.
  • the crystal orientation is disordered in the Mg alloy after extrusion and the elongation is improved.
  • the force S that reduces the elongation when the (0001) bottom surface, which is the sliding surface of Mg, is arranged along the extrusion direction, and the plastic working by the pair of rolls of the present invention.
  • non-bottom surfaces such as (10-10) column surfaces and (10-11) conical surfaces are arranged along the extrusion direction.
  • the size of the intermetallic compound particles has a strong correlation with the amount of processing strain accumulated around the particles.
  • the smaller the particle size of the intermetallic compound the more processing strain can be accumulated, and as a result, an Mg alloy having high resistance to mosquitoes can be obtained.
  • an Mg alloy having high resistance exceeding 250 MPa can be obtained. If the maximum particle size of the intermetallic compound is 2 ⁇ m or less, more processing strain can be accumulated with less plastic cage. As a result, a high yield strength can be obtained, and an Mg alloy having fine crystal grains and high strength resistance can be produced under a condition in which the number of plastic rolls in a pair of rolls is reduced. The economic effect is also obtained.
  • the maximum size of the Mg alloy powder after plastic processing with a pair of rolls is set to 10 mm or less, and the minimum size of the powder is set to 0.1 mm or more. If the maximum size of the powder exceeds 10 mm, the bonding between the powders will be reduced during the compacting of the powder, which is the next process, or the corners of the mold will be filled when placed in the mold. As a result, there is a problem in that a chipping occurs at the end of the green compact after molding. On the other hand, when the minimum size of the Mg alloy powder is less than 0.1 mm, it tends to ignite, which causes a safety problem in handling.
  • Mg having a relatively small size and crystal grains relative to the crystal grain diameter of magnesium of the starting raw material powder make alloy powder.
  • the maximum crystal grain size of the magnesium particles constituting the substrate is set to 20 xm or less.
  • the magnesium particles of the powder after plastic casting with a roll When the crystal grain size exceeds 20 ⁇ m, it is difficult to obtain high resistance exceeding 250 MPa with Mg alloy prepared using such Mg alloy powder.
  • the base crystal grain size of the Mg alloy powder after plastic casting with a pair of rolls should be 10 ⁇ m or less. There is a need to.
  • the temperature of the starting raw material powder to be charged and the surface temperature of the roll in contact with the powder must be equal to or lower than the aging heat treatment temperature in the subsequent step.
  • the amount of working strain accumulated around the intermetallic compound particles decreases due to the overaging phenomenon, and the dynamic recrystallization during the extrusion process effectively proceeds. As a result, it is difficult to obtain a high strength Mg alloy having fine crystal grains.
  • the magnesium alloy powder raw material subjected to the above-described plastic molding by the roll is compacted and warm-extruded to obtain a high strength Mg alloy having the following characteristics.
  • the maximum crystal grain size of magnesium particles constituting the base of the obtained Mg alloy is 10 ⁇ m or less C.
  • the alloy has a tensile strength at room temperature of S250 MPa or more.
  • the inventors of the present application in particular, in the case of using a raw material having a magnesium alloy crystal grain size of 10 / m or less in the base of the Mg alloy powder, It was found that the maximum crystal grain size constituting the substrate was 5 / m or less, and the tensile strength of the alloy at room temperature was 350 MPa or more.
  • the above-mentioned magnesium alloy powder raw material that has been subjected to plastic covering with a roll is pressed in a state of being filled in a mold to produce a green compact.
  • the compact is heated in the temperature range of 150 ° C to 450 ° C, and then immediately solidified by extrusion to produce a magnesium alloy material. If the heating temperature is less than 150 ° C, dynamic recrystallization does not proceed and fine magnesium crystal grains cannot be obtained. On the other hand, if the heating temperature exceeds 450 ° C, it will be fine. There is a problem that the recrystallization structure grows and becomes coarse.
  • the molded body temperature is preferably 200 ° C to 350 ° C. From the viewpoint of densification, the extrusion ratio is 10 or more, more preferably 30 or more.
  • Each AZ91D powder was used as a starting material, and was subjected to plastic caloe using a roller compactor device.
  • the roll diameter was 100 mm
  • the peripheral speed of the roll was 100 mm / second
  • the clearance between the rolls was 0.1 mm
  • the surface temperature of the roll and the raw material powder temperature were both normal temperatures.
  • Predetermined magnesium alloy powder (one-pass product) was prepared by pulverizing the plate-like connected powders, which were plastic-carried by rolls, to a length of about 5 mm to 5 mm using a cutter mill device. By repeating this process, the crystal grains were refined.
  • Fig. 3 is a structure photograph of AZ91D ingot, (a) is a structure photograph after fabrication, (b) is a structure photograph after solution treatment, (c) is after T6 heat treatment (solution + aging heat treatment) Show your organization picture.
  • the solution treatment causes the coarse Mg A1 compound that has precipitated after forging to form a solid solution in the magnesium substrate.
  • Fig. 4 shows an enlarged structure photograph of AZ91D after T6 heat treatment in Fig. 3 (c). 500-800 nanometers (nm) of fine granular compounds are uniformly dispersed, and T6 heat treatment As a result, the predetermined tissue structure that is the object of the present invention is formed in the starting material.
  • FIG. 5 shows an organizational photograph of the AZ91D powder that has been subjected to plastic covering by a roll.
  • (A) shows the structure after T6 treatment according to the present invention
  • (b) shows the structure in the case of only the solution treatment of the comparative example.
  • the magnesium substrate shows a homogeneous structure with 20 and 40 plastic rolls, and the grain size is 2-5 microns. It is recognized that it is miniaturized to the extent.
  • the substrate is heterogeneous even after 40 plastic cycles (white and black areas are mixed in the photo).
  • the magnesium substrate is composed of coarse grain strength exceeding 20 microns.
  • Fig. 6 shows the microhardness (micro Vickers hardness) test results of each powder.
  • the hardness increases with an increase in the number of plastic cages by the roll, but the hardness of the AZ91D powder subjected to T6 heat treatment shows a higher value.
  • the difference in hardness between the two increases as the number of machining operations increases.
  • the AZ91D powder that has undergone T6 heat treatment accumulates more effectively in the substrate than the processing strain force caused by the plastic cage using the direction roll.
  • the tensile strength and 0.2% resistance of the extruded material that passed through plastic working by Ronole both increased remarkably.
  • the tensile strength was high, exceeding 250 to 300 MPa.
  • the elongation at break remains high at around 18%.
  • the tensile strength and tensile strength increase as the number of rolls of plastic by roll increases.
  • those values are low, and in particular, the tensile strength reaches 250 MPa.
  • Fig. 7 shows the results of tissue observation of the extruded material when the roll was plastic-cured 40 times using an optical microscope.
  • the crystal grain size distribution of the magnesium substrate was measured by image analysis.
  • the maximum crystal grain size was 4.2 ⁇
  • the average crystal The particle size was 1.5 ⁇
  • a fine texture was formed by dynamic recrystallization during the extrusion process.
  • the solution-treated AZ91D powder which is a comparative example of (b)
  • the maximum crystal grain size of the extruded material was 21 ⁇
  • the average crystal grain size was 9.6 ⁇ .
  • the structure is extremely coarse.
  • T6 heat-treated Mg alloy powder of the present invention is subjected to plastic working with a roll, more applied strain is generated around fine intermetallic compound precipitates deposited and dispersed on the substrate. As a result, dynamic recrystallization promoted more effectively and formed fine crystal grains.
  • Example 3 [0065] ZAXE1713 ingot produced by forging method (composition— ⁇ 1: 7 ⁇ 1, Zn: 0.95, Ca: 0.
  • Example 1 the roll diameter was 100 mm, the roll peripheral speed was 100 mm / second, the clearance between the rolls was 0.1 mm, and the roll surface temperature and raw material powder temperature were both normal. did.
  • Predetermined magnesium alloy powder one-pass product was prepared by crushing the plate-like connected powder that had been subjected to plastic casing by a roll to a length of about 5 mm to 5 mm with a cutter mill device. By repeating this, the crystal grains were refined.
  • Each ZAXE1713 powder was die-molded at room temperature using a hydraulic press to produce a cylindrical extrusion billet.
  • Tensile specimen from each magnesium alloy extruded material (the parallel portion 20 mm) were collected and subjected to tensile test at room temperature Nitehi Zumi rate per 5 X 10- 4.
  • Table 2 shows the measurement results of tensile strength (0.2% strain), tensile strength, and elongation at break.
  • AZ80A ingot (composition _A1: 8.2, Zn: 0.51%, Mn: 0.18 wt%, Mg: balance) prepared by the forging method was subjected to solution heat treatment (410 ° CX after heating for 6 hours) After air cooling, aging heat treatment (175 ° C ⁇ 26 hours after heating and cooling in a nitrogen gas furnace) was performed. Powder was prepared from this ingot by pulverization (T6 heat treatment AZ80A powder). On the other hand, as a comparison, a powder was produced by pulverization under the same conditions without heat treatment of the fabricated ingot (AZ80A powder without heat treatment). All powders had a particle size in the range of 0.6 to 4 mm.
  • Each AZ80A powder was used as a starting material, and was subjected to plastic caloe using a roller compactor device.
  • the roll diameter was 100 mm
  • the roll peripheral speed was 100 mm / sec
  • the clearance between rolls was 0.1 mm
  • the roll surface temperature and raw material powder temperature were both room temperature.
  • Each AZ80A powder was molded at room temperature using a hydraulic press to produce a cylindrical extrusion billet.
  • Tensile from each Ma Guneshiumu alloy extruded material specimen (parallel part 20 mm) were collected and subjected to tensile test at a rate per second 5 X 10- 4 strain at room temperature.
  • Table 3 shows the measurement results of tensile strength (0.2% strain), tensile strength, and elongation at break.
  • the tensile strength is 262 to 317 MPa, which is high at 17 ⁇ 9-18.9% Has breaking elongation.
  • the tensile strength was as low as 208 MPa unless plastic processing was performed by rolls.
  • the tensile strength is 218 MPa even when plastic processing with a roll is performed 20 times, which is significantly lower than the example of the present invention.
  • the tensile strength is a high value exceeding 300 MPa.
  • the billet temperature which is a comparative example, is 130 ° C
  • recrystallization during the extrusion process does not proceed sufficiently, so a high bow [cannot obtain tension resistance].
  • the billet temperature is 480 ° C, which is a comparative example, a fine recrystallization structure grows and coarsens during the extrusion process, so high tensile strength cannot be obtained.
  • the obtained Mg composite when the temperature of the roll surface and the powder is normal temperature, the obtained Mg composite
  • the tensile strength and tensile strength of the extruded gold material were V and the deviation was high.
  • the temperature of the roll surface and powder which is a comparative example, is higher than the aging treatment temperature (175 ° C) and 200 ° C, the tensile strength and tensile strength are both This was significantly lower than that of the inventive example.
  • the resistance was almost constant despite the increase in the number of machining operations. This is because when Mg alloy powder is heated to a temperature higher than the aging treatment temperature and rolls are subjected to plastic caching, the work strain does not accumulate sufficiently around the precipitates due to the overaging phenomenon. This is because it is difficult to form a fine structure due to dynamic recrystallization in the processing process, resulting in a decrease in yield strength.
  • the Mg alloy material obtained by extruding the T6 heat treated Mg alloy powder after applying the plastic casing using the roll specified by the present invention to the dynamic recycle is shown in FIG.
  • the fracture elongation (toughness) is improved due to disorder of the texture.
  • a forged magnesium ingot having the composition shown in Table 6 was subjected to a solution heat treatment (420 ° CX, air-cooled after holding for 16 hours), followed by an aging heat treatment (180 ° CX, 36 hours after holding for 36 hours). Cooling in a furnace in a gas atmosphere.
  • a magnesium alloy powder was produced from each ingot by pulverization. All powders had a particle size in the range of 0.6 to 4 mm. Each powder was used as a starting material, and a plastic cage was applied using a roller compactor. Here, as in Example 1, the roll diameter was 100 mm, the roll peripheral speed was lOO mmZ seconds, the clearance between the rolls was 0.1 mm, the roll surface temperature and the raw material powder temperature were low, and the deviation was normal temperature.
  • each processed powder was molded at room temperature using a hydraulic press to produce a cylindrical extrusion billet.
  • Tensile specimen from each magnesium alloy extruded material (the parallel portion 20 mm) were collected and subjected to tensile test at room temperature Nitehizu seen rate per 5 X 10- 4.
  • Table 7 shows the measurement results of tensile strength (0.2% strain), tensile strength, and elongation at break.
  • Sample Nos .:! To 9 are examples of the present invention, and Samples Nos. 2 to 9 are forged magnesium alloys in which an active metal element such as Zr, Sr, Sc, and Ti is added to Sample No. 1 in an appropriate range. It is an extruded material obtained using powder collected from an ingot. Compared to the characteristics of sample No. 1, the addition of active metal elements such as Zr, Sr, Sc, Ti improves the tensile strength and tensile strength without significantly reducing elongation (toughness). be able to.
  • an active metal element such as Zr, Sr, Sc, and Ti
  • the present invention can be advantageously used to obtain a magnesium alloy that achieves both high yield strength and elongation.

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Abstract

L’invention concerne une matière pulvérulente en alliage de magnésium brut obtenue en soumettant une poudre de départ, possédant un diamètre de grain cristallin relativement large, à un travail plastique dans lequel la poudre est passée à travers une paire de rouleaux afin de la soumettre à une déformation par compression ou une déformation par cisaillement, et réduire ainsi le diamètre du grain cristallin. La poudre de départ est une poudre en alliage de magnésium dans laquelle un fin composé intermétallique (21) a été précipité/dispersé dans une base (20) grâce à un traitement thermique. Dans la poudre en alliage de magnésium qui a subi un travail plastique, il y a des contraintes (22) qui s’exercent autour du composé intermétallique (21) précipité. La poudre en alliage de magnésium qui a subi un travail plastique a une taille maximale inférieure ou égale à 10 mm et une taille minimale égale ou supérieure à 0,1 mm, et les particules de magnésium composant la base (20) ont un diamètre de grain cristallin maximal inférieur ou égal à 20 µm.
PCT/JP2006/311952 2005-06-16 2006-06-14 Matière pulvérulente en alliage de magnésium brut, alliage de magnésium présentant des limites d’élasticité élevées, procédé de production de matières pulvérulentes en alliage de magnésium brut, et procédé d Ceased WO2006134980A1 (fr)

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US11/922,226 US20090263268A1 (en) 2005-06-16 2006-06-14 Raw Magnesium Alloy Powder Material, Magnesium Alloy with High Proof Stress, Manufacturing Method of Raw Magnesium Alloy Powder Material and Manufacturing Method of Magnesium Alloy with High Proof Stress
CN2006800203616A CN101193715B (zh) 2005-06-16 2006-06-14 镁合金粉体原料、高屈服强度镁合金、镁合金粉体原料的制造方法以及高屈服强度镁合金的制造方法
EP06766721A EP1897638A4 (fr) 2005-06-16 2006-06-14 Matière pulvérulente en alliage de magnésium brut, alliage de magnésium présentant des limites d'élasticité élevées, procédé de production de matières pulvérulentes en alliage de magnésium brut, et procédé de production d'un alliage de magnesium a grande elasticité

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JP2005-176410 2005-06-16
JP2005176410A JP2006348349A (ja) 2005-06-16 2005-06-16 マグネシウム合金粉体原料、高耐力マグネシウム合金、マグネシウム合金粉体原料の製造方法および高耐力マグネシウム合金の製造方法

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JP2007051305A (ja) * 2005-08-12 2007-03-01 Topy Ind Ltd マグネシウム基複合材料
JP4185549B1 (ja) * 2007-07-31 2008-11-26 株式会社栗本鐵工所 押出用ビレットの製造方法およびマグネシウム合金素材の製造方法
JP4372827B1 (ja) * 2008-06-20 2009-11-25 株式会社栗本鐵工所 マグネシウム合金素材の製造方法
RU2011120482A (ru) * 2008-10-22 2012-11-27 Сумитомо Электрик Индастриз, Лтд. Формованное изделие из магниевого сплава и лист из магниевого сплава
WO2012022038A1 (fr) * 2010-08-18 2012-02-23 Hu Xinyu Dispositif et procédé permettant de refaçonner des particules de poudre
KR20130089664A (ko) * 2010-12-28 2013-08-12 스미토모덴키고교가부시키가이샤 마그네슘 합금재
JP6048217B2 (ja) * 2013-02-28 2016-12-21 セイコーエプソン株式会社 マグネシウム基合金粉末およびマグネシウム基合金成形体
JP6048216B2 (ja) * 2013-02-28 2016-12-21 セイコーエプソン株式会社 マグネシウム基合金粉末およびマグネシウム基合金成形体
JP2016017183A (ja) * 2014-07-04 2016-02-01 国立研究開発法人物質・材料研究機構 マグネシウム基合金展伸材及びその製造方法
JP6376209B2 (ja) * 2016-11-21 2018-08-22 セイコーエプソン株式会社 マグネシウム基合金粉末およびマグネシウム基合金成形体
CN109084008A (zh) * 2018-08-27 2018-12-25 重庆元和利泰镁合金制造有限公司 镁合金变速箱壳体及其制备方法
CN110681869B (zh) * 2019-10-15 2021-08-03 上海交通大学 选区激光熔化增材制造技术制备高强韧镁稀土合金的方法
US20210115566A1 (en) * 2019-10-18 2021-04-22 Rolls-Royce Corporation Multi-component deposits
CN111283212B (zh) * 2020-03-27 2022-05-17 陕西理工大学 一种剥层自锐结构钨合金材料及其制备方法和应用

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KR20080028362A (ko) 2008-03-31
US20090263268A1 (en) 2009-10-22
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CN101193715B (zh) 2010-12-08
JP2006348349A (ja) 2006-12-28
EP1897638A1 (fr) 2008-03-12

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