WO2012091112A1 - Matériau en alliage de magnésium - Google Patents

Matériau en alliage de magnésium Download PDF

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Publication number
WO2012091112A1
WO2012091112A1 PCT/JP2011/080455 JP2011080455W WO2012091112A1 WO 2012091112 A1 WO2012091112 A1 WO 2012091112A1 JP 2011080455 W JP2011080455 W JP 2011080455W WO 2012091112 A1 WO2012091112 A1 WO 2012091112A1
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Prior art keywords
mass
magnesium alloy
area
region
concentration
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PCT/JP2011/080455
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English (en)
Japanese (ja)
Inventor
山川　真弘
正禎 沼野
崇康 杉原
優吾 久保
光治 井口
水野　修
Original Assignee
住友電気工業株式会社
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Priority claimed from JP2010292518A external-priority patent/JP2012140656A/ja
Priority claimed from JP2010292519A external-priority patent/JP2012140657A/ja
Priority claimed from JP2010292517A external-priority patent/JP2012140655A/ja
Application filed by 住友電気工業株式会社 filed Critical 住友電気工業株式会社
Priority to KR1020157030551A priority Critical patent/KR20150125729A/ko
Priority to US13/977,034 priority patent/US20140308157A1/en
Priority to EP11853525.1A priority patent/EP2660343B1/fr
Priority to KR1020137015544A priority patent/KR20130089664A/ko
Priority to CN201180063110.7A priority patent/CN103282526B/zh
Priority to CA2823292A priority patent/CA2823292C/fr
Publication of WO2012091112A1 publication Critical patent/WO2012091112A1/fr

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    • 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
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • 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
    • C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
    • 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
    • C22C23/06—Alloys based on magnesium with a rare earth metal 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

Definitions

  • the present invention relates to various members such as casings for electric and electronic devices, automobile parts, and magnesium alloy materials suitable for materials of these members.
  • it relates to a magnesium alloy material having excellent corrosion resistance.
  • Magnesium alloys containing various additive elements in magnesium have been used as constituent materials for various members such as casings of portable electric and electronic devices such as mobile phones and notebook personal computers and automobile parts.
  • Patent Document 1 proposes a magnesium alloy plate made of an alloy equivalent to the AZ91 alloy in the ASTM standard and having excellent press workability.
  • the corrosion resistance such as anodizing treatment and chemical conversion treatment is applied to the surface of the above-mentioned member and the magnesium alloy plate as the material to enhance the corrosion resistance.
  • the magnesium alloys containing Al such as AZ31 alloy and AZ91 alloy described above tend to have better corrosion resistance as the Al content increases.
  • AZ91 alloy is said to be excellent in corrosion resistance among magnesium alloys.
  • the above-described anticorrosion treatment is required even for members made of AZ91 alloy (mainly die-cast material or thixomold material). This is because even when a die-cast material made of AZ91 alloy or the like is not subjected to anticorrosion treatment, local corrosion may occur when a corrosion test is performed as described later. Therefore, further improvement in corrosion resistance is desired for the magnesium alloy material.
  • an object of the present invention is to provide a magnesium alloy material having excellent corrosion resistance.
  • the corrosion resistance can be improved as the Al content increases. Accordingly, the present inventors have studied magnesium alloys containing various forms of magnesium alloys containing 7.3% by mass or more of Al and investigated the corrosion resistance. As a result, even if the Al content of the entire magnesium alloy material was the same, the corrosion resistance was superior or inferior depending on the form. In order to elucidate the cause, first, the structure of each form was examined. In the magnesium alloy material inferior in corrosion resistance, coarse precipitates (based on additive elements in the alloy. Typically, Al and Mg In the case of a magnesium alloy material having at least one intermetallic compound and having excellent corrosion resistance, fine precipitates are present in a uniformly dispersed state, or substantially no precipitates are present.
  • the additive element such as Al in the magnesium alloy mainly exists in at least one state of a precipitate (typically an intermetallic compound), a crystallized product, and a solid solution.
  • a precipitate typically an intermetallic compound
  • a crystallized product typically an intermetallic compound
  • a solid solution typically an intermetallic compound
  • the structure in which the coarse precipitate is present is a region where the Al concentration is higher than the surrounding area and the area of this high Al concentration portion is relatively large (mainly the region formed by the precipitate and the surrounding area). It can be said that this organization exists. In other words, it can be said that the region where the Al concentration is relatively low is a local and abundant tissue. And it is thought that corrosion tends to occur in each of the regions where the Al concentration is low, and local corrosion such as pitting corrosion occurs or proceeds.
  • a structure in which fine precipitates uniformly exist can be said to be a structure in which an Al concentration is higher than that of the surroundings and a minute region consisting of this high Al concentration portion exists uniformly.
  • the structure substantially free of precipitates consists of a matrix in which Al is substantially uniformly dispersed, and can be said to be a structure in which very fine precipitates are present slightly or not at all. Since Al is uniformly dispersed, local corrosion as described above is unlikely to occur and progress, and a magnesium alloy material having such a structure is considered to have excellent corrosion resistance.
  • the magnesium alloy material having excellent corrosion resistance contains Al in the entire alloy material.
  • the amount is x mass%
  • the area of x mass% ⁇ ⁇ occupies half of the area, where there are virtually no locations with very little Al content, and there are also places with very high Al content.
  • the present inventors have obtained the knowledge that it is possible to quantitatively specify that the corrosion resistance is excellent by using a parameter such as the area ratio of the Al concentration. In addition, it is considered that this quantitative regulation can be used regardless of the presence form of Al.
  • the present invention is based on the above knowledge, and a magnesium alloy material having excellent corrosion resistance is defined by the Al concentration and its area ratio.
  • the present invention relates to a magnesium alloy material made of a magnesium alloy containing Al in a range of 7.3 mass% to 16 mass%.
  • This magnesium alloy material satisfies the following (1) to (3) when the Al content of the entire magnesium alloy material is x mass%.
  • (1) The area where the Al content is (x x 0.8) mass% or more and (x x 1.2) mass% or less is 50 area% or more
  • the magnesium alloy material of the present invention there is substantially no region with poor corrosion resistance such as Al content of 4.2% by mass or less, and a region with a high Al concentration (0.8x mass% to 1.2x mass%). In addition, more than half of the region) occupies more than half, and there are few regions with a very high Al concentration (regions of 1.4x mass% or more). That is, the magnesium alloy material of the present invention can effectively prevent local corrosion because the region having a low Al concentration does not substantially exist. Further, the magnesium alloy material of the present invention has few or substantially no regions where the concentration of Al is very high (typically, precipitates containing Al etc. are fine and their total abundance is small (form In other words, Al is sufficiently and widely dispersed in the magnesium alloy matrix itself. Thus, the magnesium alloy material of the present invention is in a state in which the Al concentration is uniformly high over at least the entire surface side region. With this configuration, the magnesium alloy material of the present invention is excellent in corrosion resistance.
  • a region where the Al content is (x ⁇ 0.8) mass% or more and (x ⁇ 1.2) mass% or less is 70 area% or more, and the Al content is (x ⁇ 1.4) mass% or more. In which the region is 5 area% or less.
  • a region with a high Al concentration accounts for 70% or more, and a region with a very high Al concentration (region of 1.4x mass% or more) is 5%.
  • Al is less than 3% or less depending on the form, depending on the form, so Al is present more uniformly and is more excellent in corrosion resistance.
  • a region having an Al content of (x ⁇ 0.9) mass% or more and (x ⁇ 1.2) mass% or less is 50 area% or more.
  • the region with higher Al concentration occupies more than half, and there are many regions that are excellent in corrosion resistance.
  • the total area of the intermetallic compound containing at least one of Al and Mg is 3 area% or less in the cross section of the surface side region of the magnesium alloy material.
  • the above-described form is excellent in corrosion resistance because the intermetallic compound containing Al and Mg is very fine and has a small total abundance or not at least over the entire surface side region.
  • the intermetallic compound containing Al is very little or does not exist at all, the Al concentration of the parent phase is uniformly high and the corrosion resistance is excellent.
  • the magnesium alloy material is a plate material.
  • the above-described embodiment can be suitably used for a material of a plastic work material to be subjected to plastic working such as press working, forging work, and bending work.
  • plastic working such as press working, forging work, and bending work.
  • the obtained plastic working material can also maintain the same Al concentration distribution as the plate material, and is excellent in corrosion resistance.
  • the magnesium alloy material is a coil material obtained by winding a long plate material.
  • the coil material is composed of a plate material having excellent corrosion resistance
  • the coil material can be used as a material for a plastic material that is subjected to plastic processing such as press processing, forging processing, and bending processing. It can contribute to mass production of materials.
  • the obtained plastic working material can also maintain the same Al concentration distribution as the coil material, and is excellent in corrosion resistance.
  • the coil material can be rewound and appropriately punched or cut to produce a plate material having a desired shape, which can contribute to mass production of such a plate material. Since the obtained plate material substantially maintains the Al concentration distribution of the coil material, it is excellent in corrosion resistance.
  • the obtained plate material can be used as it is as well as the material of the plastic working material.
  • the magnesium alloy material may be a plastic working material obtained by subjecting a plate material to plastic working.
  • the magnesium alloy material of the present invention can take various forms as described later.
  • it is a plastic working material (molded product) molded into a desired shape as in the above-described embodiment, it can be suitably used for various structural members, cases, and the like.
  • a solution treatment particularly a final solution treatment
  • any plastic work that can be pressed or forged is applied to such a plate material.
  • it Compared to die-cast material and thixomold material, it has excellent toughness in addition to corrosion resistance.
  • the plate material has been subjected to plastic processing such as rolling (primary processing) or when the primary processing material has been further subjected to final solution treatment, voids ( The internal defects such as nests are reduced or substantially eliminated, and the toughness is improved, and the strength is improved by refining crystal grains by rolling or the like.
  • plastic processing such as rolling (primary processing) or when the primary processing material has been further subjected to final solution treatment
  • voids The internal defects such as nests are reduced or substantially eliminated, and the toughness is improved, and the strength is improved by refining crystal grains by rolling or the like.
  • the form in which such plate material is subjected to press working or forging plastic processing (secondary processing) has mechanical properties such as toughness and strength in addition to corrosion resistance, compared to die-casting materials and thixo-mold materials. Also excellent.
  • the magnesium alloy material of the present invention is excellent in corrosion resistance.
  • FIG. 1 (A) shows sample No. 1: coil material (no final solution)
  • Fig. 1 (B) shows sample No. 2: coil material (magnification mapping image of magnesium alloy material by FE-EPMA.
  • FIG. 1 (C) shows Sample No. 3: sheet material (rapid heating and quenching material), and
  • FIG. 1 (D) shows Sample No. 100: die casting material.
  • 2A is a bar graph showing the relationship between the Al concentration and area ratio (%) of a magnesium alloy material.
  • FIG. 2A shows sample No. 1: coil material (no final solution)
  • FIG. 2B shows the sample.
  • No.2 Coil material (with final solution)
  • FIG. 3 shows sample No.3: Sheet material (rapidly heated and quenched), Fig.2 (D) shows sample No.100: Die-cast material .
  • Fig. 3 (A) shows sample No.1: coil material (no final solution), and
  • Fig. 3 (B) shows sample No. 2: coil material (final).
  • 3 (C) shows sample No. 3: sheet material (rapid heating / cooling material), and
  • FIG. 3 (D) shows sample No. 100: die casting material.
  • the magnesium alloy constituting the magnesium alloy material of the present invention includes those having various compositions containing an additive element in Mg (remainder: Mg and impurities, Mg: 50% by mass or more).
  • a high-concentration alloy containing 7.3% by mass or more of an additive element, particularly an Mg—Al alloy containing at least Al as an additive element is used.
  • the Al content is preferably 12% by mass or less, more preferably in terms of plastic workability, particularly 11% by mass or less, and more preferably 8.3% by mass to 9.5% by mass.
  • Additive elements other than Al were selected from Zn, Mn, Si, Be, Ca, Sr, Y, Cu, Ag, Sn, Li, Zr, Ce, Ni, Au, and rare earth elements (excluding Y and Ce)
  • the content of each element is 0.01% by mass or more and 10% by mass or less, and preferably 0.1% by mass or more and 5% by mass or less.
  • at least one element selected from Si, Ca, Sn, Y, Ce, and rare earth elements (excluding Y and Ce) is 0.001% by mass or more in total, preferably 0.1% by mass in total. When it is contained in an amount of 5% by mass or less, heat resistance and flame retardancy are excellent.
  • the rare earth element is contained, the total content is preferably 0.1% by mass or more, and particularly when Y is contained, the content is preferably 0.5% by mass or more.
  • the impurity include Fe.
  • Mg-Al alloys include, for example, ASTM standard AZ alloys (Mg-Al-Zn alloys, Zn: 0.2 mass% to 1.5 mass%), AM alloys (Mg-Al-Mn) Alloy, Mn: 0.15 mass% to 0.5 mass%), Mg-Al-RE (rare earth element) alloy, AX alloy (Mg-Al-Ca alloy, Ca: 0.2 mass% to 6.0 mass%), AS Alloy (Mg—Al—Si alloy, Si: 0.2 mass% to 6.0 mass%), AJ alloy (Mg—Al—Sr alloy, Sr: 0.2 mass% to 7.0 mass%), and the like.
  • an Mg-Al alloy containing 8.3% to 9.5% by mass of Al and 0.5% to 1.5% by mass of Zn, typically AZ91 alloy is preferable because of its excellent corrosion resistance and mechanical properties.
  • the content of Al in the entire magnesium alloy material (hereinafter referred to as Al total average amount): x mass% is the presence state of Al in the magnesium alloy material (mainly precipitates, crystallized materials, and solid solution). Regardless of (at least one), it means the total amount of Al contained in the magnesium alloy material.
  • x mass% is the presence state of Al in the magnesium alloy material (mainly precipitates, crystallized materials, and solid solution).
  • it means the total amount of Al contained in the magnesium alloy material.
  • ICP emission spectroscopy ICP emission spectroscopy
  • ICP-AES Inductively Coupled Plasma Atomic Emission Spectroscopy
  • Al concentration and area ratio (area ratio) The most characteristic feature of the magnesium alloy material of the present invention is the Al concentration distribution. Specifically, when the Al concentration is analyzed with respect to the surface of the alloy material, (1) the area where the Al content is the Al total average amount (x mass%) ⁇ 20% occupies the majority (however, 7.3 ⁇ x ⁇ 16). The area below 0.8x mass% (minimum 5.84 mass%) is inferior in corrosion resistance, and the area above 1.2x mass% (maximum 19.2 mass%) has high corrosion resistance in this area itself. The presence of the concentrated concentration makes it relatively easy to have a region inferior in corrosion resistance.
  • the region of 0.8xmass% to 1.2xmass% (hereinafter, this region is referred to as the central composition region) has a small difference in Al concentration, and the region where such Al concentration is uniform is 50 areas. % Or more, it is difficult for a location where the difference in Al concentration is large, that is, a region of less than 0.8x mass% and a region of more than 1.2x mass% as described above. Accordingly, the magnesium alloy material of the present invention has few or less regions inferior in corrosion resistance, and at least the surface side region of the alloy material is constituted by a region where the Al concentration is relatively high, thereby locally Corrosion hardly occurs and has excellent corrosion resistance.
  • the area ratio of the central composition region is preferably 55 area% or more, particularly 70 area% or more, more preferably 90 area% or more, and particularly preferably 95 area% or more.
  • the Al concentration is higher, specifically, the area of 0.9x mass% to 1.2x mass% is 30 area% or more, more preferably 50 area% or more, the Al concentration is high and this high concentration The presence of a uniform region is superior in corrosion resistance. Details of the Al concentration measurement method and the area ratio measurement method will be described later.
  • the measurement of the Al concentration takes an arbitrary cross section of the magnesium alloy material and can be performed at an arbitrary position of the cross section, but the region most involved in corrosion is the surface of the alloy material. Accordingly, at least the surface of the magnesium alloy material of the present invention satisfies the Al concentration distribution defined above.
  • the internal Al concentration The distribution allows a different form from the surface Al concentration distribution.
  • the magnesium alloy material of the present invention has (2) a region where the Al content is Al total average amount (x mass%) ⁇ 140% or more (however, 7.3 ⁇ x ⁇ 16). In the region of 1.4x mass% (maximum 22.4 mass%) or more, although this region itself has high corrosion resistance, there is a region where Al concentration is relatively low and the corrosion resistance is inferior due to the concentration of Al in this region. It becomes easy to do. On the other hand, in the magnesium alloy material of the present invention, since the region of 1.4x mass% or more (hereinafter, this region is referred to as an ultra-high concentration region) is as small as 17.5 area% or less, there is hardly a region inferior in corrosion resistance. Excellent corrosion resistance.
  • the area ratio of the ultra-high concentration region is 15 area% or less, more preferably 14 area% or less, particularly 5 area% or less, especially 3 area% or less, and further preferably 1 area% or less. More preferably, the ultra-high concentration region is 0.15 area% or less and ideally does not exist.
  • a region having an Al content of 4.2% by mass or less (hereinafter, this region is referred to as a low concentration region), that is, a region inferior in corrosion resistance as described above. not exist.
  • this region is referred to as a low concentration region
  • the magnesium alloy material of the present invention is excellent in corrosion resistance because there are substantially no locations where such an Al concentration is extremely low, that is, locations where corrosion is likely to occur or where corrosion is likely to proceed. “Substantially absent” means that no point of 4.2 mass% or less is observed by EPMA measurement.
  • each intermetallic compound is small (average particle size: 3.0 ⁇ m or less, preferably 0.5 ⁇ m or less) and uniformly dispersed (total area ratio: 11% The following is preferable: Al concentration tends to be uniform.
  • Al-rich precipitates such as the above intermetallic compounds are present uniformly, a function as a barrier against corrosion can be expected.
  • an intermetallic compound containing Mg such as Mg 2 Si, Mg 2 Ca, Mg 2 Sn, Mg 17 Sr 2 can be formed in addition to the Al-rich intermetallic compound described above.
  • the intermetallic compound containing Mg or Al as described above is preferably 3 area% or less because of excellent corrosion resistance. Therefore, in the present invention, there is no particular lower limit for the intermetallic compound.
  • the surface side region in which the area ratio of the intermetallic compound is measured is a region extending from the surface of the magnesium alloy material to 100 ⁇ m in the thickness direction. When the thickness of the magnesium alloy material is less than 100 ⁇ m, the area is from the surface to 1/4 of the thickness in the thickness direction. A method for measuring the area ratio of the intermetallic compound will be described later.
  • Form As a form of the magnesium alloy material of the present invention, when distinguished from the manufacturing process, a wrought material subjected to a stretching process such as a rolled material and an extruded material (however, there is a solution treatment in the middle of manufacturing), the wrought material is subjected to a correction treatment. Straightened material, heat treated material that has been subjected to heat treatment to remove strain, etc., die cast material, thixo mold material, stretched material, straightened material, casting material (for example, by twin roll continuous casting method) The final solution treatment was applied to various forms such as, and the solution treatment was subjected to a stretching process such as rolling / extrusion (after solution treatment), and the solution treatment material was corrected (solution treatment).
  • the rolled material is refined in crystal grains by rolling, for example, an average crystal grain size of 10 ⁇ m or less, further a microstructure of 5 ⁇ m or less, or internal defects such as voids (nests) May be a small, small, or substantially non-existing structure (a structure in which a density actually measured with respect to a theoretical density material calculated from a material composition is 99% or more). Having such a fine structure and a structure having a high density can be an index indicating that the material is a rolled material. As described above, the rolled material has few internal defects, is small, or preferably is substantially non-existent, and has excellent mechanical properties such as tensile strength, elongation, and rigidity. Can be suitably used.
  • leveler roll processing can be used.
  • a straightening material by leveler roll processing may have a structure in which a clear grain boundary is difficult to observe even when microscopic observation is performed by introducing a shear band.
  • the monochromatic X-ray diffraction peak can be obtained, it is a non-amorphous structure, the monochromatic X-ray diffraction peak can be obtained, and it has a structure in which grain boundaries cannot be observed.
  • It can be an index indicating that Correction materials, especially correction materials by leveler roll processing, tend to recrystallize during plastic processing such as press processing, and tend to be excellent in plastic workability.
  • the degree of correction is low, the appearance, structure, and mechanical properties may be similar to the rolled material.
  • additive elements such as Al exist mainly as a solid solution, Al 12 Mg 17 , Al (MnFe), Al 2 Ca, Al 4 Ca, Precipitates such as Al 3 Ni-containing intermetallic compounds are unlikely to exist, and even if present, they are small and few. Therefore, a small proportion of Al-containing intermetallic compounds can be an indicator of a solution material.
  • the ratio of the total area of the intermetallic compound containing at least one of Al and Mg in the cross section of the surface side region of the magnesium alloy material is Those having a content of 3% or less, more preferably 1% or less, can be cited as solution materials.
  • the solution material is subjected to a heat treatment of 400 ° C. ⁇ 30 hours or more, the hardness tends not to decrease after the heat treatment or the elongation does not substantially change (however, the test The piece shall be ground.) Therefore, it is considered that such a degree of change in mechanical properties before and after the heat treatment can be used as an indicator of the solution material.
  • the Al composition has a central composition region of 90 area% or more, an ultrahigh concentration region of 3 area% or less, and further 1 area% or less. Therefore, the solution material is superior in corrosion resistance.
  • the solution material is excellent in plastic workability because there are substantially no defects such as coarse precipitates (typically, intermetallic compounds) that become the starting point of cracking during plastic working. Therefore, this solution material can be suitably used as a material for plastic working material.
  • the abrasive has a smooth surface and excellent surface properties. Therefore, a small surface roughness (for example, a maximum height Rz of 20 ⁇ m or less) or the presence of polishing traces is an indicator of an abrasive.
  • the heat treatment material depends on the heat treatment conditions, for example, (1) no shear band is observed inside the magnesium alloy material, (2) the proportion of particles having a crystal grain size of 0.1 ⁇ m or less in the cross section is 5 area% or less It can be considered that this can be an index indicating that it is a heat treatment material.
  • the plastic processed material also has a central composition region by using a form in which the magnesium alloy material of the present invention is a plate material and performing plastic processing under specific conditions.
  • the machined material described above can substantially maintain the Al concentration distribution of the material.
  • the plate material can be cut and punched to obtain various shapes, for example, a circular shape, an elliptical shape, a polygonal shape, and various forms including a through hole (including a large one such as a window) in a part thereof. Can take the shape of a plane.
  • the plate material includes forms having different thicknesses such as a form having a concave groove in part and a form having a rib (convex part) in part by using a deformed roller as described later.
  • the irregular shape include an arbitrary three-dimensional shape that can be formed by a die casting method or a thixomold method, and a three-dimensional shape that can be formed by plastic working such as press working.
  • the three-dimensional shape body for example, has a protrusion such as a rib or a concave groove integrally on a part of a plate material, a shape partially different in thickness, a cross section used for a housing of various devices, etc.] And a relatively simple shape such as a polygonal columnar body such as a spherical body, an ellipsoidal body, and a triangular columnar body.
  • the irregularly shaped body may have a form including a through hole (including a large one such as a window) in a part thereof.
  • Such a concavo-convex shape or a shape having a through hole can be easily formed by using a die casting method or the like.
  • a material obtained by forming an ingot or the like into a desired shape by cutting or grinding may be used.
  • examples of the irregularly shaped body include a form having a plastic working part in which plastic working such as press working is performed on a part thereof.
  • the magnesium alloy material of the present invention can take various shapes as described above, but if it is a coil material, the magnesium alloy material can be suitably used as a material for a plastic work material subjected to plastic working such as press work. It can contribute to mass production of plastic working materials.
  • the magnesium alloy material of the present invention is a coil material, more specific forms include a solution coil material obtained by subjecting a rolled coil material, a cast coil material, or a rolled coil material to a final solution treatment.
  • These coil materials include, for example, those having a thickness of 10 mm or less, further 5 mm or less, a width of 100 mm or more, further 200 mm or more, particularly 250 mm or more, a length of 30 m or more, further 50 m or more, particularly 100 m or more.
  • a long material and a wide material are suitable for the material of the plastic working material as described above.
  • a rolled material or a material obtained by subjecting the rolled material to a final solution treatment can have a form with a thinner thickness or a longer length as compared with the cast material.
  • a thin material having a thickness of 2 mm or less, particularly 1.5 mm or less, particularly 1 mm or less, or a long material having a length of 50 m or more, further 100 m or more, particularly 200 m or more can be used.
  • Thin-walled materials with a thickness of 2 mm or less can be suitably used as a material for thin and lightweight plastic working materials.
  • the thickness is preferably 0.1 mm or more, and 0.3 mm to 1.2 mm is easy to use.
  • the magnesium alloy material of the present invention is excellent in corrosion resistance, it is expected that it can be used satisfactorily even if it is not subjected to anticorrosion treatment such as chemical conversion treatment or anodizing treatment depending on the corrosive environment. In this case, the anticorrosion process can be reduced, the productivity of the magnesium alloy material can be increased, and waste can be reduced, so that it is expected that the environmental load can be reduced.
  • the magnesium alloy material of the present invention can be in a form in which an anticorrosion treatment such as a chemical conversion treatment or an anodizing treatment is performed, that is, a form having an anticorrosion layer.
  • the Al concentration can be measured by removing the anticorrosion layer by polishing or cutting and exposing the surface of the base material made of a magnesium alloy without performing high-precision cross-sectional observation.
  • the coating layer is provided in addition to the anticorrosion layer, the corrosion resistance can be further improved, and the commercial value can be improved by coloring or applying a pattern. An anticorrosion layer and a coating layer are good to apply to a desired location.
  • the production method of the magnesium alloy material of the present invention includes a form having a rolling process (manufacturing method 1-1 to 1-5) and a form not having a rolling process (manufacturing method 2).
  • a form having a rolling process manufactured by the production method of the magnesium alloy material of the present invention
  • a form not having a rolling process manufactured by the production method described below.
  • at least one step is deleted as long as the magnesium alloy material of the present invention having a specific Al concentration distribution that satisfies the above conditions (1) to (3) is obtained, The order of each process can be changed.
  • the magnesium alloy material of the present invention When the magnesium alloy material of the present invention is used as a rolled material, for example, it can be manufactured by a manufacturing method including the following preparation process, intermediate solution forming process, and rolling process.
  • Preparation step a step of preparing a cast material made of a magnesium alloy containing Al of 7.3 mass% to 16 mass% and manufactured by a continuous casting method.
  • Intermediate solution treatment step A step of producing an intermediate solution material by subjecting the cast material to a solution treatment of holding temperature: not less than the minimum holding temperature below and holding time: not less than 1 hour and not more than 25 hours.
  • Minimum holding temperature Temperature that is 10 ° C lower than the temperature at which Al dissolves in Mg (solidus temperature) in the Mg-Al binary phase diagram (mass%)
  • Rolling process More than 1 pass to the intermediate solution material A process of producing rolled material by performing warm rolling.
  • the total time for maintaining the material to be processed typically rolled material in a temperature range of 150 ° C. or higher and 300 ° C. or lower within 12 hours, and 300
  • the thermal history of the material is controlled so that it is not heated to a temperature higher than ° C.
  • the average cooling rate from the temperature of the material when starting cooling to the temperature of the material becomes 100 ° C or less is 0.8 ° C / min or more
  • a temperature that is 10 ° C. lower than the solidus temperature is typically expressed as follows (also described later in production method 1-2) The same).
  • the solidus temperature is 283 ° C to 437 ° C, and the solidus temperature increases as the Al total average amount increases.
  • the minimum holding temperature is expressed by the following linear expression.
  • the total time for keeping the materials in the temperature range of 150 ° C. to 300 ° C. is shortened to 12 hours or less.
  • the temperature range of 150 ° C. to 300 ° C. is a temperature range in which an Al-rich intermetallic compound such as Al 12 Mg 17 is easily grown.
  • the intermetallic compound Growth can be suppressed, and an increase in the ultra-high concentration region and the low concentration region can be suppressed.
  • Increasing the cooling rate is preferable because the increase in the ultrahigh concentration region and the low concentration region can be suppressed.
  • the growth of the intermetallic compound is also suppressed by preventing the heating above 300 ° C.
  • the magnesium alloy material of the present invention can be manufactured by a manufacturing method including the following preparation process, intermediate solution process, rolling process, and final solution process.
  • Preparation step a step of preparing a cast material made of a magnesium alloy containing Al of 7.3 mass% to 16 mass% and manufactured by a continuous casting method.
  • Intermediate solution treatment step A step of producing an intermediate solution material by subjecting the cast material to a solution treatment of holding temperature: not less than the minimum holding temperature below and holding time: not less than 1 hour and not more than 25 hours.
  • Minimum holding temperature Temperature that is 10 ° C lower than the temperature at which Al dissolves in Mg (solidus temperature) in the Mg-Al binary phase diagram (mass%)
  • Rolling process More than 1 pass to the intermediate solution material
  • Final solution treatment step a step of subjecting the rolled material to a final solution treatment of holding temperature: above the minimum holding temperature and holding time: from 1 hour to 40 hours.
  • the cooling rate in the temperature range of 330 ° C. to 380 ° C. satisfies the following.
  • the surface layer region is cooled at 1 ° C./min or more.
  • the cooling rate after the final warm rolling may be set to a specific range in the same manner as in the manufacturing method 1-1 described above. Also in this production method 1-2, until the final product is obtained after the final solution treatment step, the total time for maintaining the temperature range of 150 ° C. or more and 300 ° C. or less is as short as possible, and more than 300 ° C. It is preferable to control the heat history of the raw material so that it is not heated to a temperature, because the Al concentration distribution of the solution material obtained through the final solution treatment step can be maintained.
  • the rolled material manufactured by the above-described manufacturing method 1-1 can be subjected to a final heat treatment for the purpose of distortion removal. That is, when the magnesium alloy material of the present invention is a heat treatment material that has undergone a rolling process, in addition to the preparation process, intermediate solution forming process, and rolling process of the production method 1-1, a production method that includes a final heat treatment process described later. Can be manufactured.
  • the rolled material or solution material produced by the production methods 1-1 and 1-2 may be subjected to correction (typically warm correction) for the purpose of increasing straightness or the surface properties. Cleaning and polishing can be performed for the purpose of improvement (removal of oxide layer, surface defects, lubricant used in rolling, etc.) and the like.
  • the magnesium alloy material of the present invention when used as an orthodontic material or an abrasive, a preparation process, an intermediate solution forming process, a rolling process (process specified in the manufacturing method 1-1 or 1-2), a final solution forming process (manufacturing method) In addition to the steps defined only for 1-2, it can be produced by a production method comprising at least one of a correction step and a polishing step described later.
  • a manufacturing method comprising the above preparation step, intermediate solution forming step, rolling step, and further comprising at least one step selected from a final solution forming step, a final heat treatment step, a straightening step, a polishing step and a cleaning step.
  • a plate material having a predetermined length a short plate material considered to be difficult to wind (for example, a length of 5 m or less, particularly 1 m or less), hereinafter referred to as a sheet material), or a long plate material is obtained. It is done.
  • the sheet material is obtained, for example, by cutting the cast material into a predetermined length in the preparation step to obtain a cast material (cast plate) having a predetermined length, and using the cast material as a raw material through the subsequent steps.
  • a sheet material can be obtained by winding a long cast material in the preparation step to produce a cast coil material, producing a coil material in each step, and finally cutting it to a predetermined length.
  • magnesium alloy material of the form of a coil material is obtained by winding up this elongate board
  • the magnesium alloy material of the present invention can be produced by using either a sheet material or a coil material as a material for each step.
  • the cast material preferably uses a continuous casting method.
  • the continuous casting method can stably obtain a cast material of uniform quality in the longitudinal direction and can be rapidly solidified, so it can reduce oxides and segregation, and can also be the starting point of cracking during rolling. As a result, it is possible to suppress the formation of coarse crystal precipitates exceeding 10 ⁇ m, which can be obtained, and a cast material excellent in plastic workability such as rolling and extrusion can be obtained.
  • the twin roll continuous casting method is easy to form a plate-shaped cast material with little segregation.
  • the cross-sectional area, thickness, width, and length of the cast material are not particularly limited, but segregation is likely to occur if it is too thick. Therefore, the thickness is preferably 10 mm or less, more preferably 7 mm or less, and particularly preferably 5 mm or less.
  • the long cast material with a length of 30 m or more, 50 m or more, especially 100 m or more, or a wide cast material with a width of 100 mm or more, 250 mm or more, especially 600 mm or more is used as the material of the rolled material, the long Simple rolled plates and wide rolled plates can be produced.
  • the cast material may be a cast coil material wound in a coil shape, or may be a cast sheet material cut into a predetermined length, and may be appropriately selected according to a desired form.
  • the inner diameter of the cast coil material is small when winding it in a coil shape, it can be wound up without cracking when it is heated to 150 ° C or more just before winding the cast material, and the cast coil material can be easily Can be made.
  • ⁇ Intermediate solution process A material that is excellent in plastic workability such as rolling and extrusion by reducing the presence of coarse precipitates by applying an intermediate solution treatment to the above cast material to homogenize the composition and dissolving elements such as Al. It can be.
  • the holding temperature of the intermediate solution treatment is typically 350 ° C. or higher and 450 ° C. or lower, particularly 380 ° C. or higher, and more preferably 390 ° C. or higher and 420 ° C. or lower.
  • the holding time is 1 hour to 25 hours, particularly 10 hours to 25 hours.
  • the holding time is preferably increased as the Al content increases.
  • the cooling rate is increased by using forced cooling such as water cooling or blast as in the final solution treatment described later (preferably 1 ° C./min or more, more preferably 50 ° C./min or more), which is preferable because growth and precipitation of precipitates can be suppressed.
  • forced cooling such as water cooling or blast as in the final solution treatment described later (preferably 1 ° C./min or more, more preferably 50 ° C./min or more)
  • the cast material may be subjected to an intermediate solution treatment as it is, but before the intermediate solution treatment is performed, rolling with a small reduction ratio (a reduction ratio of about 1% / 1 pass to 15% / 1 pass) Alternatively, surface grinding may be performed.
  • the temperature of the material is room temperature, it is difficult to increase the rolling reduction, resulting in a decrease in production efficiency. Therefore, considering productivity, it is preferable to perform at least one pass warm rolling. .
  • Heating the material can improve the plastic workability such as rolling, and the higher the material temperature, the more the plastic workability can be improved.
  • Precipitates such as intermetallic compounds are coarsened, leading to an increase in the ultra-high concentration region and the low concentration region, and a coarse precipitate causes a decrease in plastic workability.
  • the temperature of the material is preferably 300 ° C. or lower, particularly 150 ° C. or higher and 280 ° C. or lower.
  • the material can be heated using a heating means such as an atmospheric heating furnace by providing a preheating step.
  • a heating furnace an appropriate one that can store a material (a sheet material or a coil material) can be used.
  • the holding temperature of the preheating step It is preferable to shorten the holding time.
  • the material is controlled so as to be as short as possible (preferably within 12 hours) when the material is maintained in a specific temperature range: 150 ° C. to 300 ° C. mainly during rolling, precipitates ( In particular, the growth of the Al-rich intermetallic compound) can be effectively suppressed to prevent an increase in the area ratio of the ultrahigh concentration region, the low concentration region, and the intermetallic compound.
  • an in-line heating device typically a heating device using radiant heat, current heating, induction heating, etc.
  • a rolling device typically, a rolling roller
  • the rolled material is immersed in a refrigerant or a lubricant and then rapidly cooled. (Preferably a cooling rate of 1 ° C./sec or more).
  • the time during which the material is maintained at 150 ° C. to 300 ° C. in the rolling process can be effectively shortened.
  • the rapid heating and rapid cooling can be easily performed when the material to be rolled is a short material such as a cast sheet material.
  • the time for heating each material to a uniform temperature is relatively short by providing an appropriate gap between the materials. it can.
  • This technique can also be easily applied when the material to be rolled is a short material such as a cast sheet material.
  • the total holding time in the preheating before rolling is preferably 0.01 hours or more and 8 hours or less, and particularly preferably 0.01 hours or more and 0.3 hours or less.
  • the rolling including the warm rolling may be performed in one pass or multiple passes.
  • a rolled material with a small thickness is obtained, and the average crystal grain size of the structure constituting the rolled material is reduced (for example, 10 ⁇ m or less, preferably 5 ⁇ m or less), or press working. It is possible to improve the plastic workability.
  • the number of passes, the reduction rate of each pass, and the total reduction rate can be appropriately selected so that a rolled material having a desired thickness can be obtained.
  • known rolling conditions for example, appropriate conditions such as heating not only the raw material but also the rolling roll may be used.
  • the final warm rolling was performed.
  • the average cooling rate from the temperature of the material at the start of cooling until the temperature of the material reaches at least 100 ° C. is 0.8 ° C./min or more.
  • the average cooling rate is, for example, the temperature of the raw material when starting cooling after the final warm rolling, and the time t (min) from the obtained measurement temperature: Tmp (° C.) to 100 ° C. Is set to a speed represented by (Tmp-100) / t (° C./min).
  • the cooling state may be adjusted so that (Tmp-100) / t (° C./min) ⁇ 0.8 (° C./min).
  • the material temperature may be measured using either a contact sensor such as a thermocouple or a non-contact sensor such as a thermography. It is recommended to prepare an extremely thin thermocouple and place it on the surface of the material.
  • any cooling means that can achieve the cooling rate can be used.
  • the cooling rate can be increased.
  • forced cooling means such as those that use a gaseous medium such as a fan (air cooling) or blast (jet air cooling), those that use a liquid medium such as water cooling, and those that use a solid medium such as a cooling roll. Can be used.
  • liquid refrigerant that includes a cleaning agent (for example, a surfactant) that can remove the lubricant used in rolling or the like because cooling can be performed together with cooling.
  • the forced cooling means may be arranged off-line, but if arranged in-line, a large contact area between the material surface and the cooling medium can be secured, so that the cooling efficiency can be improved.
  • the cooling may be performed after winding.
  • the cooling may be performed in a wound state, but if it is performed in a rewinded state, the cooling rate can be easily increased. If the cooling rate can be achieved, natural cooling may be performed without using the forced cooling means.
  • intermediate heat treatment can be performed between passes so long as the above-mentioned total time includes the holding time in the temperature range of 150 ° C. to 300 ° C.
  • the holding temperature of the intermediate heat treatment material is also preferably 300 ° C. or lower.
  • the holding temperature is preferably 150 ° C. or higher, particularly 250 ° C. or higher and 280 ° C. or lower.
  • the holding time is, for example, about 0.5 to 3 hours.
  • the thickness, width, and length of the rolled material can be appropriately selected.
  • the frictional resistance at the time of rolling can be reduced, the burning of a raw material etc. is prevented and it is easy to perform rolling.
  • a roll having a groove on the outer periphery of the roll (deformed roller) a rolled material having a rib, and a roller having a convex on the outer periphery of the roll (deformed roller)
  • a rolled material having a groove can be manufactured.
  • the obtained rolled material can be cut or ground to form a desired uneven shape or stepped shape, or a boss or a through hole can be formed.
  • the precipitate By applying a final solution treatment after the rolling, the precipitate can be re-dissolved to sufficiently reduce the ultra-high concentration region and intermetallic compound, and the low concentration region can be substantially absent. .
  • the holding temperature is less than the above-mentioned minimum holding temperature or the holding time is less than 1 hour, a supersaturated solid solution cannot be sufficiently produced, and it is difficult to sufficiently reduce the ultra-high concentration region and the intermetallic compound.
  • the holding temperature is too high (typically over 450 ° C) or the holding time is over 40 hours, it is an energy loss to heat the matrix even after it has been seized or becomes sufficiently solid solution. Since the productivity may be lowered, the holding temperature is preferably set to a low value. For example, 390 ° C. or more and 420 ° C. or less and holding time: 10 hours or more and 25 hours or less can be mentioned.
  • the cooling rate is adjusted so that the cooling rate in the temperature range of 330 ° C. to 380 ° C. is 1 ° C./min or more in the cooling step from the holding temperature.
  • the cooling rate in a magnesium alloy containing a large amount of Al with an Al content of 7.3% by mass or more, precipitates such as Al-rich intermetallic compounds such as Al 12 Mg 17 are likely to occur in the temperature range of 330 ° C. to 380 ° C. It is said. Therefore, it is desirable to pass through this temperature range as quickly as possible. Therefore, in the production of the magnesium alloy material of the present invention having an Al content of 7.3% by mass or more, the cooling rate in the temperature range of 330 ° C. to 380 ° C.
  • the cooling rate is preferably as high as possible, and is preferably 1 ° C./min or more, and more preferably 50 ° C./min or more.
  • the surface layer region of the rolled material to be processed satisfies the above cooling rate.
  • corrosion occurs and proceeds from the surface of the magnesium alloy material.
  • the surface layer region in the magnesium alloy material is excellent in corrosion resistance, that is, it should have a specific Al concentration distribution that satisfies the above conditions (1) to (3), the surface layer region to be processed Is cooled at least at the above cooling rate.
  • forced cooling as described above can be suitably used.
  • air cooling such as blast using a blast means such as a fan or a jet jet mechanism of cold air is used, it is difficult to oxidize and there are few cooling spots. The effect of suppressing the deterioration of the surface properties accompanying the adhesion of is obtained.
  • a cooling method such as mist spraying, spraying water, or immersion in a liquid refrigerant that sprays a liquid refrigerant such as water or a reducing liquid can be used.
  • a lubricant is used as a liquid refrigerant, and cooling is performed by applying the lubricant to the solution material or immersing it in the lubricant. May be.
  • a liquid refrigerant containing a cleaning agent as described above may be used as the forced cooling means.
  • Water cooling using a liquid refrigerant can increase the cooling rate more than air cooling.
  • a coil material it may be cooled as it is, but if it is rewound, it is easy to increase the cooling rate.
  • the cooling rate is about 50 ° C./min, and when performing water cooling, the cooling rate is about 400 ° C./min. be able to. It is good to wind up after cooling to about room temperature.
  • the plate material (including the cast material) that has undergone the final solution treatment process is also excellent in plastic workability, it can be sufficiently wound even at a room temperature of about a winding diameter that is industrially used.
  • the cooling rate is determined by measuring the surface temperature of the material after final solution treatment, setting the time (min) so that the cooling rate in the temperature range of 330 ° C. to 380 ° C. becomes the desired rate, It is good to adjust a cooling state so that it may become.
  • the temperature of the region (surface region) from the surface to the thickness direction of 10 ⁇ m is synonymous with the temperature of the outermost surface. Accordingly, the cooling rate of the surface region can be set by measuring the temperature of the outermost surface of the material and measuring the temperature.
  • any of the above-described contact sensors such as thermocouples and thermography and non-contact sensors can be used.
  • the holding temperature is preferably 300 ° C. or lower. More specific conditions include a holding temperature: 100 ° C. to 300 ° C. and a holding time: 5 minutes to 60 minutes. The time for holding the material (rolled material) in the temperature range of 150 ° C. or higher and 300 ° C. or lower in the final heat treatment step is preferably included in the total time, and the holding time is preferably less than 30 minutes. With such specific conditions, a rolled material having a specific Al concentration distribution that satisfies the above conditions (1) to (3) and reduced or eliminated distortion during rolling can be obtained. can do.
  • the flatness of the plate material can be improved by performing correction after rolling or after the final solution treatment.
  • the correction can be carried out at room temperature or a temperature below room temperature, but if it is carried out warm, the flatness can be further improved.
  • the holding temperature is preferably 300 ° C. or lower. More specific conditions include a holding temperature: 100 ° C. or higher and 300 ° C. or lower, preferably 150 ° C. to 280 ° C. It is preferable that the total time includes the time for holding the material (for example, rolled material) in the temperature range of 150 ° C. or more and 300 ° C. or less in the straightening process.
  • Warm correction is, for example, a heating furnace capable of heating a material, and a roll unit in which a plurality of rolls are arranged in a staggered manner so as to bend (strain) the heated material continuously.
  • a roll leveler device comprising: When a roll leveler is used, even a long material can be continuously corrected.
  • a warm press device can be used for warm correction. Even after warm straightening, if the average cooling rate from the temperature of the material at the start of cooling to the temperature of the material reaches 100 ° C or less is 0.8 ° C / min or more, it is extremely high due to the growth of precipitates.
  • the forced cooling means may be appropriately used as described above, or natural cooling may be used.
  • the cooling rate when performing warm correction continuously from rolling, if the cooling rate is controlled as described above, the Al concentration distribution can be made to be in a specific state, and even when wound in a coil shape, curling is not possible.
  • a plate material that is difficult to stick and is excellent in flatness is preferable.
  • the plastic workability can be improved by heating the material such as the sheet material or the coil material.
  • the temperature of the material is preferably 350 ° C. or lower, more preferably 300 ° C. or lower, and particularly preferably 280 ° C. or lower.
  • 150 ° C. or higher and 280 ° C. or lower, and more preferably 150 ° C. or higher and 220 ° C. or lower are preferable.
  • the retention time is set to 8 hours or less as described above, thereby suppressing the growth of precipitates, increasing the ultra-high concentration region and low concentration region, and the area ratio of intermetallic compounds.
  • the holding time is preferably as short as possible, 0.5 hours or less (30 minutes or less), and more preferably 0.3 hours or less.
  • the coil material may require a longer time for making the entire temperature uniform than that of the sheet material.
  • An apparatus can be used, or a fan or a wind guide plate can be appropriately disposed in the heating furnace.
  • the time during plastic working such as press working itself depends on the shape, it is as short as several seconds to several minutes in press working, and it is considered that defects such as coarsening of precipitates do not substantially occur.
  • the heat treatment conditions include a holding temperature: 100 ° C. to 300 ° C. and a holding time: about 5 minutes to 60 minutes. However, also in this heat treatment, it is preferable that the holding time in the temperature range of 150 ° C. to 300 ° C. is included in the total time.
  • the material is 150 ° C. to 300 ° C. It is preferable to control the total time kept in the temperature range of ° C to a relatively short time of 12 hours or less. In the case of performing the final solution treatment, it is preferable that the total time for keeping the material in the temperature range of 150 ° C. to 300 ° C. is 12 hours or less in the process from the final solution treatment to the final product.
  • the total time of maintaining the temperature range of 150 ° C. to 300 ° C. is preferably 0.01 hours or more. More preferably, the temperature range: 150 ° C. or more and 280 ° C. or less, more preferably 150 ° C. or more and 220 ° C. or less, the total time: 8 hours or less, particularly 0.3 hours or less, the processing degree of each pass in the rolling process Control manufacturing conditions such as total processing degree, preheating conditions (such as preheating means and time), cooling process conditions (such as cooling means and time), and line speed. Moreover, since the Al-rich intermetallic compound described above tends to precipitate as the Al content increases, the total time is preferably adjusted according to the Al content.
  • ⁇ intermediate solution preferably, cooling rate is controlled in the cooling process
  • ⁇ rolling ⁇ intermediate heat treatment cooling depending on the holding temperature
  • the cooling rate is controlled by the process
  • ⁇ rolling ⁇ correction / polishing / cleaning by performing an intermediate solution treatment before rolling, precipitates can be made fine and minimal, and subsequent rolling can refine the structure and improve mechanical properties.
  • the magnesium alloy material of the present invention is a form formed by a manufacturing method that does not include a rolling process, typically a molded body (including irregularly shaped bodies) formed by die casting or the like, for example, the following preparation It can be produced by a production method comprising a process and a final solution treatment process.
  • Preparation step A step of preparing one material selected from a die-cast material made of a magnesium alloy containing Al in a range of 7.3 mass% to 16 mass%, a thixo mold material, and an extruded material.
  • Final solution treatment step Holding temperature in the above material: Mg-Al binary phase diagram (mass%) 10 ° C lower than the temperature at which Al dissolves in Mg (minimum holding temperature), holding time: 1 hour
  • the cooling rate in the temperature range of 330 ° C. to 380 ° C. satisfies the following.
  • the surface layer region is cooled at 1 ° C./min or more.
  • a specific Al concentration distribution that satisfies the above-mentioned conditions (1) to (3) is obtained by subjecting the material prepared in the preparation step to a final solution treatment similar to the production method 1-2 described above. It can be set as the solution material which has this.
  • the production method 2 can be suitably used for producing a magnesium alloy material having a complicated three-dimensional shape as described above.
  • the extruded material can be manufactured, for example, by preparing an ingot made of a magnesium alloy containing the specific amount of Al and extruding it under known conditions.
  • An abrasive having a specific Al concentration distribution that satisfies the above condition (one form of the magnesium alloy material of the present invention) is obtained.
  • the above-described (1) to (3) are further provided by providing a process for performing an anticorrosion process such as a chemical conversion process or an anodizing process or a process for forming a coating layer.
  • the magnesium alloy material of the present invention comprising a base material having a specific Al concentration distribution that satisfies the conditions (2) and an anticorrosion layer or coating layer formed on the base material is obtained.
  • Known materials and conditions can be used for the material and forming conditions of the anticorrosion layer and the coating layer.
  • pretreatment such as degreasing, acid etching, desmutting, and surface adjustment is preferably performed.
  • plastic working if the anticorrosion layer and the coating layer are formed after the plastic working, damage to the anticorrosion layer and the coating layer during the plastic working can be prevented.
  • a magnesium alloy material of Sample Nos. 1 to 5 prepared as follows and a commercially available die-cast material (AZ91 alloy, 3 mm thick, 75 mm wide, 150 mm long plate material) were prepared for comparison.
  • This die cast material was subjected to wet belt polishing under the same conditions as the polishing treatment applied to Samples Nos. 1 to 5 described later to produce a polishing plate.
  • This polishing plate was designated as Sample No. 100.
  • Sample No.1 Coil material (No final solution after rolling) Casting ⁇ Intermediate solution ⁇ Rolling ⁇ Straightening ⁇ Polishing
  • Sample No.2 Solution coil material (with final solution after rolling) Casting-> Intermediate solution->Rolling-> Final solution->Correction-> Polishing
  • Sample No.3 Sheet material (rapid heating and quenching material) * No intermediate winding Casting (cutting after casting)-> Intermediate solution->Rolling->Correction-> Polishing sample No.4: Solution material (die casting) Preparation of die-cast material ⁇ final solution sample No. 5: solution material (extrusion) Preparation of extruded material ⁇ final solution
  • Example No. 1 Long cast plate (thickness 4mm, width 300mm) made of a magnesium alloy with a composition equivalent to AZ91 alloy (Mg-8.75% Al-0.65% Zn (all mass%)) and obtained by twin-roll continuous casting method was wound up once to produce a cast coil material.
  • the obtained intermediate solution coil material was rewound and rolled by multiple passes under the following conditions to produce a rolled coil material having a thickness of 0.6 mm, a width of 250 mm, and a length of 800 m.
  • Rolling rate 5% / pass to 40% / pass Material temperature: 200 ° C to 280 ° C
  • Roll temperature 100 °C ⁇ 250 °C
  • the unwound material is passed between a feeding drum housed in a heating furnace and a take-up drum housed in another heating furnace, and the materials run between both drums by the rotation of both drums. I did it. Further, a rolling roll is disposed between these two drums so that the material to be rolled is rolled.
  • the feeding drum and the winding drum are rotated counterclockwise for each pass, and the feeding and winding are reversed to perform a plurality of passes of rolling continuously. And the raw material wound up by the heating furnace for every pass was heated so that it might become the said temperature, and the raw material of a heating state was made to drive between drums.
  • the final warm rolling pass After the final warm rolling pass is applied to the material, it is wound up as it is, and after adjusting the temperature of the material in the heating furnace, it is cooled by blowing wind adjusted to a certain temperature on the rewinded material. The speed was adjusted.
  • the average cooling rate until the material temperature (200 ° C to 280 ° C) reaches 100 ° C is as follows: Sample No.1: 2.0 ° C / min, Sample No.2: 1.7 ° C / min, 100 ° C to room temperature ( The temperature of the wind was adjusted and cooled so that the average cooling rate until it reached about 20 ° C. was Sample No. 1: 1.0 ° C./min and Sample No. 2: 0.9 ° C./min. And the rolled coil material was produced by winding up the rolled sheet returned to room temperature.
  • the rolled coil material is rewound and warmed by a roll leveler device to produce a straightened coil material (material temperature: 250 ° C.).
  • the straightened coil material is rewound and a # 600 polishing belt is used. Then, wet belt polishing was performed, and the obtained polishing plate was wound up to produce a polishing coil material.
  • This polishing coil material is designated as sample No. 1.
  • sample No. 1 in the manufacturing process from the above intermediate solution treatment until the final polished coil material is obtained, the total time for holding the material in the temperature range of 150 ° C to 300 ° C is within 12 hours, No heating above 300 ° C was performed.
  • the average cooling rate of the surface layer region (region from the surface to 10 ⁇ m in the thickness direction) of the plate material constituting the coil material is 3 ° C / min ( ⁇ 1 ° C / min)
  • the temperature, air volume, and wind speed of the cold air were adjusted so that
  • a thermocouple was attached to an appropriate position of the coil material, and the above adjustment was performed so that the cooling rate at the slowest cooling point was 3 ° C./min.
  • the obtained solution coil material was rewound and subjected to warm correction and wet belt polishing under the same conditions as in Sample No. 1.
  • the obtained polishing coil material is designated as sample No. 2.
  • sample No. 2 the total time for holding the material in the temperature range of 150 ° C to 300 ° C is less than 12 hours in the manufacturing process after the final solution treatment until the final polished coil material is obtained. And heating above 300 ° C. was not performed.
  • the process in which the material is held in the temperature range of 150 ° C. to 300 ° C. after the final solution treatment is substantially only warm correction.
  • the holding time in the temperature range can be set to about several minutes.
  • Example No. 3 A plurality of cast plates (a cast sheet material having a thickness of 5 mm, a width of 300 mm, and a length of 500 mm) made of a magnesium alloy having the same composition as Sample Nos. 1 and 2 and obtained by a twin roll continuous casting method were prepared. Each of the obtained cast plates was subjected to a solution treatment (intermediate solution treatment) at 400 ° C. for 24 hours, and then subjected to the same conditions as sample Nos. 1 and 2 while cutting to adjust the length. Then, a plurality of passes were rolled to produce a rolled plate (sheet material) having a thickness of 0.6 mm, a width of 300 mm, and a length of 2000 mm.
  • a solution treatment intermediate solution treatment
  • Preheating was performed by a heating means capable of rapid heating before each rolling pass, and the material was heated to a predetermined temperature.
  • the total holding time in the preheating is 3 hours.
  • the material was placed on a cooling steel plate (which can be controlled by circulating the heat medium) to adjust the cooling rate.
  • the average cooling rate until the temperature of the material (200 ° C to 280 ° C) reaches 100 ° C is 60 ° C / min
  • the average cooling rate until it reaches room temperature (about 20 ° C) is 40 ° C / min.
  • the steel sheet for cooling was cooled by adjusting the temperature and mounting time.
  • sample No. 3 is the total time for holding the material in the temperature range of 150 ° C to 300 ° C in the manufacturing process after the intermediate solution treatment until the final polishing plate is obtained. Was within 12 hours, and heating above 300 ° C. was not performed.
  • Example No. 5 After remelting and casting a commercially available die-cast material similar to sample No. 100, an extruded material (AZ91 alloy, thickness 3 mm, width 50 mm, length 150 mm) was prepared, and this extruded material was 380 ° C ⁇ After the final solution treatment for 20 hours, it was cooled by forced cooling to room temperature (about 20 ° C.) using a jet ejection mechanism in the same manner as in Sample No. 4. After this forced cooling, correction and wet polishing by warm pressing is performed under the same conditions as in Sample No. 4, and the resulting polishing plate is referred to as Sample No. 5. For sample No. 5, the temperature, air volume, and wind speed of the cold air were adjusted so that the cooling rate of the surface layer in the temperature range of 380 ° C. to 330 ° C. was 50 ° C./min ( ⁇ 1 ° C./min).
  • the adjustment of the cooling rate in the cooling step after the final warm rolling and the cooling rate in the final solution treatment step can be easily performed by preparing the following correlation data in advance and referring to the correlation data.
  • the parameters of forced cooling means such as cold air temperature, air volume, and wind speed are appropriately changed, the temperature of the material at the start of cooling in the cooling process is changed to 100 ° C.
  • the cooling rate is obtained by measuring the time to reach or the time from 380 ° C to 330 ° C, and the correlation data between each parameter and the cooling rate is created.
  • a temperature sensor may be arranged at an appropriate position of the coil material, and correlation data relating to the cooling rate of the slowest cooling portion may be created in advance.
  • the Al content (mass%) in the elemental analysis was determined by preparing the following calibration curve and converting the X-ray intensity of EPMA into the Al content (mass%) using this calibration curve.
  • FIG. 1 is a mapping image (observation field of view: 24 ⁇ m ⁇ 18 ⁇ m) regarding the Al content obtained by analyzing the surface of each sample by FE-EPMA.
  • Fig. 1 (A) is the coil material of sample No. 1
  • Fig. 1 (B) is the solution coil material of sample No. 2
  • Fig. 1 (C) is the sheet material of sample No. 3 (rapid quenching material)
  • FIG. 1 (D) shows the die-cast material of sample No.100. Although shown in gray scale in FIG.
  • FIGS. 1 (A), 1 (B), and 1 (C) and the white variant in FIG. 1 (D) are Al-rich intermetallic compounds.
  • the die-cast material of sample No. 100 has many regions with a very high Al concentration. It can also be seen that there is a region where the Al concentration is very low.
  • the coil material of sample No. 1 the solution coil material of sample No. 2, the sheet material of sample No. 3 (rapid heating and quenching) It can be seen that the material) does not have a large area where the Al concentration is very high.
  • the solution coil material of sample No. 2 has a small and very small region where the Al concentration is very high.
  • the coil material, the solution coil material, and the sheet material are substantially free of a region having a very low Al concentration.
  • FIG. 3 is a scanning electron microscope (SEM) micrograph of each sample No. 1 to 3,100 (5000 times).
  • the light gray granule in FIGS. 3 (A) to 3 (C) and the light gray variant in FIG. 3 (D) show precipitates.
  • FIG. 3 (D) it can be seen that the die-cast material of sample No. 100 has large precipitates and an irregular shape. This is consistent with the fact that in the mapping image, the ultra-high concentration region having a very high Al concentration is large and has an irregular shape.
  • the average particle size ( ⁇ m) and the ratio of the total area (area%) of the intermetallic compounds of each sample No. 1 to 5,100 were measured. The results are also shown in Table 1.
  • the average particle diameter and area ratio can be easily calculated by image processing the above micrograph using a commercially available image processing apparatus.
  • the average particle size of the intermetallic compound was measured as follows. For each sample, five cross sections are taken in the thickness direction, and three fields of view (here, one field of view: 22.7 ⁇ m ⁇ 17 ⁇ m region) are arbitrarily taken from the observation image of each section. Here, the field of view was selected from the surface side region up to 100 ⁇ m in the thickness direction from the surface of each sample. For each observation field, the equivalent circle diameter of each intermetallic compound existing in one observation field (the diameter of the equivalent area circle of the area of each intermetallic compound) is obtained, and the sum of the equivalent circle diameters is obtained as one observation field.
  • a value obtained by dividing by the number of intermetallic compounds present therein: (total of equivalent circle diameter) / (total number) is defined as the average particle diameter of the observation visual field.
  • Table 1 shows the average of the average particle diameters of 15 observation fields for each sample.
  • the ratio of the total area of the intermetallic compound was measured as follows. As described above, the observation field is taken from the surface side region, and for each observation field, the total area is calculated by examining the areas of all intermetallic compounds existing in one observation field, and this total area is calculated by one observation. The value divided by the area of the visual field (here 385.9 ⁇ m 2 ): (total area) / (area of the observation visual field) is the area ratio of the observation visual field. Table 1 shows the average of the area ratios of the 15 observation fields for each sample.
  • Corrosion weight loss was measured as follows by performing a salt spray test in accordance with JIS H 8502 (1999) as a salt water corrosion test. After preparing a test piece for corrosion from sample Nos. 1 to 5,100 and measuring the mass (initial value) of the test piece for corrosion, the test surface of a preset size is exposed on the test piece for corrosion. Mask unnecessary parts of the corrosion test piece. Insert the masked corrosion test piece into the corrosion test equipment and place it leaning at a predetermined angle with respect to the equipment bottom (here, the angle between the equipment bottom and the test piece: 70 ° ⁇ 80 °).
  • the test solution (5 mass% NaCl aqueous solution, temperature: 35 ⁇ 2 ° C.) is sprayed on the corrosion test piece for a predetermined time (here 96 hours). After a predetermined time has elapsed, the corrosion test piece was taken out of the corrosion test apparatus, masking was removed, and the corrosion test piece was generated in accordance with the method described in Reference Table 1 of JIS Z 2371 (2000). Corrosion products are removed by chromic acid dissolution. The mass of the test piece for corrosion after removing the corrosion product is measured, and the value obtained by dividing the difference between the mass and the initial value by the area of the test surface of the test piece for corrosion is weight loss ( ⁇ g / cm 2 ). And
  • the amount of Mg elution was measured as follows by performing a salt water immersion test as a salt water corrosion test under the following conditions.
  • a corrosion test piece is prepared from Sample Nos. 1 to 5,100, and unnecessary portions of the corrosion test piece are masked so that a test surface having a predetermined size is exposed in the corrosion test piece.
  • Make the masked corrosion test piece into the test solution (5 mass% NaCl aqueous solution, liquid amount: (A) x 2 ml when the test piece area (exposed area) is (A) cm 2 ) Hold for a predetermined time in a completely immersed state (here, hold for 96 hours at room temperature (25 ⁇ 2 ° C.) under air conditioning).
  • the test solution is collected, the amount of Mg ions in the test solution is quantified with ICP-AES, and the value obtained by dividing the Mg ion amount by the area of the test surface of the corrosion test piece is the Mg elution amount ( ⁇ g / cm 2 ).
  • Sample Nos. 1 to 3 all have a distribution of Al concentration with a total Al content of each sample: 8.75% by mass and a peak in the vicinity thereof. In addition, it can be seen that Sample Nos. 1 to 3 do not have a location where the Al concentration is extremely low. Samples No. 4 and 5 also showed the same Al concentration distribution as Sample No. 2. As shown in Table 1, Sample Nos. 1 to 5 having a small variation in Al concentration have low corrosion weight loss and Mg elution amount, and are excellent in corrosion resistance.
  • the solution coil material of sample No. 2, the sheet material of sample No. 3, and the solution material of sample Nos. 4 and 5 have a central composition region in which the Al concentration is 0.8x mass% to 1.2x mass%.
  • an ultra-high concentration region with an Al concentration of 1.4x mass% or more is very small at 5% or less, and a sample with a central composition region of 90% or more or an ultra-high concentration region. It can be seen that there are samples with 3 area% or less. That is, it can be seen that Sample Nos. 2 to 5 have Al present more uniformly.
  • Sample No. 2 has a very small ultra-high concentration region and a small difference between the maximum value and the minimum value of Al concentration, indicating that Al is present more uniformly. It can be seen that Samples Nos. 2 to 5 having such a uniform composition are superior in corrosion resistance.
  • solution solution coil material of sample No. 2 and the solution solution materials of sample Nos. 4 and 5 that have undergone the final solution treatment have a low intermetallic compound of 3 area% or less and the maximum value of the Al concentration. It can be seen that it is relatively low. From this, it is considered that Samples Nos. 2, 4, and 5 are excellent in corrosion resistance. In particular, since sample No. 2 is a long material, it can contribute to mass production of a plastic processed material having excellent corrosion resistance, and is expected to have high industrial significance.
  • the die-cast material of sample No. 100 has a low concentration region in which the Al concentration is 0.8x mass% to 1.2x mass% and the central composition region is small, and the Al concentration is 4.2 mass% or less.
  • the minimum value of Al is equivalent to AZ31 alloy.
  • Sample No. 100 has a large area ratio of the intermetallic compound. From this, it can be considered that the sample No. 100 has a relatively inferior corrosion resistance, resulting in inferior corrosion resistance.
  • Test Example 2 After pressing the plate materials of Sample Nos. 1 to 5 prepared in Test Example 1, the Al concentration was measured in the same manner. Both the sample No. 1 coil material and the sample No. 2 solution coil material were unwound and cut to a predetermined length to produce a rectangular plate. Each of the prepared plate materials was preheated to 250 ° C. and subjected to press working in this heated state. The preheating holding time and the total time during pressing are 2 minutes (0.1 hour or less).
  • the present invention is not limited to the above-described embodiment, and can be modified as appropriate without departing from the gist of the present invention.
  • the composition of the magnesium alloy (particularly the Al content), the shape of the magnesium alloy material, the specifications (thickness, width, length), production conditions, etc. can be changed as appropriate.
  • the magnesium alloy material of the present invention is a component member of various electric / electronic devices, particularly a portable or small-sized electric / electronic device casing, members of various fields where high strength is desired, for example, It can be suitably used for components of transportation equipment such as automobile parts and aircraft, skeleton members, bags, and the like. Or this invention magnesium alloy material can be utilized suitably for the raw material of the said member.

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Abstract

La présente invention concerne un matériau en alliage de magnésium présentant une excellente résistance à la corrosion. Le matériau en alliage de magnésium comprend un alliage de magnésium contenant de 7,3 % à 16 % en masse d'Al. Lorsque la teneur en Al de l'ensemble du matériau en alliage de magnésium est de x % en masse, la zone présentant une teneur en Al de 0,8x % à 1,2x % en masse est de 50 % par zone ou plus, la zone présentant une teneur en Al de 1,4x % en masse min. est de 17,5 % par zone max. et il n'y a quasiment pas de zone avec une teneur en Al de 4,2 % en masse max. Ce matériau en alliage de magnésium peut éviter efficacement la survenue d'une corrosion localisée et sa progression, grâce à une faible variation de la concentration en Al et à l'absence de zones présentant une teneur en Al extrêmement faible. En conséquence, le matériau en alliage de magnésium présente une excellente résistance à la corrosion par rapport à un matériau coulé sous pression ayant la même teneur générale en Al. Le matériau en alliage de magnésium peut être utilisé comme matériau de placage, matériau de bobinage comprenant un matériau de longue plaque roulée et comme articles formés.
PCT/JP2011/080455 2010-12-28 2011-12-28 Matériau en alliage de magnésium WO2012091112A1 (fr)

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KR1020157030551A KR20150125729A (ko) 2010-12-28 2011-12-28 마그네슘 합금재
US13/977,034 US20140308157A1 (en) 2010-12-28 2011-12-28 Magnesium alloy material
EP11853525.1A EP2660343B1 (fr) 2010-12-28 2011-12-28 Procédé de fabrication d'une feuille d'alliage de magnésium
KR1020137015544A KR20130089664A (ko) 2010-12-28 2011-12-28 마그네슘 합금재
CN201180063110.7A CN103282526B (zh) 2010-12-28 2011-12-28 镁合金材料
CA2823292A CA2823292C (fr) 2010-12-28 2011-12-28 Materiau en alliage de magnesium

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JP2010-292517 2010-12-28
JP2010-292519 2010-12-28
JP2010292517A JP2012140655A (ja) 2010-12-28 2010-12-28 マグネシウム合金板材
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CN103658173B (zh) * 2013-12-13 2016-01-06 内蒙古科技大学 一种基于管坯轧制不同性能镁合金板材的方法
US11198926B2 (en) * 2013-12-17 2021-12-14 Northwestern University Alloys and methods of forming same
GB2527486A (en) 2014-03-14 2015-12-30 Imp Innovations Ltd A method of forming complex parts from sheet metal alloy
CN105401031A (zh) * 2015-11-13 2016-03-16 太仓旺美模具有限公司 一种镁合金金属材料的配方
CN105779837A (zh) * 2016-05-25 2016-07-20 河南科技大学 一种含Gd牺牲阳极镁合金
CN106868366A (zh) * 2017-02-14 2017-06-20 山东银光钰源轻金属精密成型有限公司 一种汽车用镁合金变速箱结构支架的生产工艺
AT521500B1 (de) * 2018-12-18 2020-02-15 Lkr Leichtmetallkompetenzzentrum Ranshofen Gmbh Verfahren zur Erhöhung einer Korrosionsbeständigkeit eines mit einer Magnesiumbasislegierung gebildeten Bauteiles gegen galvanische Korrosion sowie damit erhältliches korrosionsbeständiges Bauteil

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KR20150125729A (ko) 2015-11-09
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CN103282526A (zh) 2013-09-04
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CA2823292C (fr) 2016-06-14

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