EP1826284A1 - Gehäuse aus magnesiumlegierung - Google Patents

Gehäuse aus magnesiumlegierung Download PDF

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Publication number
EP1826284A1
EP1826284A1 EP05709520A EP05709520A EP1826284A1 EP 1826284 A1 EP1826284 A1 EP 1826284A1 EP 05709520 A EP05709520 A EP 05709520A EP 05709520 A EP05709520 A EP 05709520A EP 1826284 A1 EP1826284 A1 EP 1826284A1
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EP
European Patent Office
Prior art keywords
magnesium alloy
mass
forming
sheet material
case
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.)
Withdrawn
Application number
EP05709520A
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English (en)
French (fr)
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EP1826284A4 (de
Inventor
Y. Chubu Cter Nat.Inst. Adv. Ind.Science & Chino
M. Chubu Ctr Inst. Adv. Ind. Science & Mabuchi
Kazuo; Araki
Hiroyuki; Fujii
Shunji; Sakurai
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.)
AJC Co Ltd
National Institute of Advanced Industrial Science and Technology AIST
Original Assignee
AJC Co Ltd
National Institute of Advanced Industrial Science and Technology AIST
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by AJC Co Ltd, National Institute of Advanced Industrial Science and Technology AIST filed Critical AJC Co Ltd
Priority claimed from PCT/JP2005/001363 external-priority patent/WO2006046320A1/ja
Publication of EP1826284A1 publication Critical patent/EP1826284A1/de
Publication of EP1826284A4 publication Critical patent/EP1826284A4/de
Withdrawn legal-status Critical Current

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    • 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
    • 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
    • C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent

Definitions

  • the present invention relates to a magnesium alloy case comprising a superplastically formed body of a magnesium alloy sheet or plate material, and more particularly to a high-quality magnesium alloy case having a complex shape, which comprises a superplastically formed body and in which the formation of cavities during the superplastic forming is inhibited by highly accurately controlling the material composition and oxygen concentration in the magnesium alloy sheet material, and also to a technology for manufacturing the magnesium alloy case.
  • the present invention provides a novel magnesium alloy case which has such properties as high resistance to fracture and a high strength and which can be used in a wide variety of fields including aerospace material, materials for electronic devices, automobile parts and the like.
  • most magnesium products in Japan are fabricated by a casting process such as die casting and thixocasting.
  • the possibility of forming thin products by such methods is the main reason for successful industrial utilization of magnesium alloy materials.
  • cast magnesium alloy materials have been used for cases, for example, cases of personal computers, cellular phones, and digital cameras.
  • the problems associated with the industrial manufacture of magnesium alloy materials by the existing casting methods include the necessity of conducting the after-treatment to repair the casting defects, a low yield, and problematic strength and rigidity of the products.
  • Plastic processing can be considered as an effective method and the demand therefor is growing because it has a high yield and provides for increased strength and toughness simultaneously with forming.
  • the possibility of fabricating formed bodies from magnesium alloy sheet materials by a deep drawing, stretch forming, and blow forming would enable the manufacture of thin-wall and high-strength formed bodies by an inexpensive process, and strong demand, e.g., for cases of household electronic products manufactured by such a process can be expected.
  • magnesium alloy members fabricated by plastic processing there are only very few examples of magnesium alloy members fabricated by plastic processing.
  • a critical decomposition shear stress of non-base sliding of a magnesium alloy is much larger than that of other sliding systems at normal temperature, and the formability of the magnesium alloy at normal temperature is low. Furthermore, a specific feature of rolled magnesium alloy materials is that a texture in which a ⁇ 0001 ⁇ plane is oriented parallel to the sheet surface is formed therein and strains in the sheet thickness direction during plastic deformation cannot be expected, this being a factor inhibiting formability of the magnesium alloy at normal temperature. Because of the above-described problems, it is essentially difficult to implement cold press forming, which is a major reason why magnesium alloy members cannot be fabricated by plastic processing.
  • a forming method that uses superplastic deformation has attracted attention as a method for forming magnesium alloys, which have poor cold formability, by plastic processing.
  • a superplastic phenomenon is developed in metal materials when crystal grains are refined.
  • superplastic deformation is understood as "a phenomenon in which a deformation stress demonstrates strong dependence on a strain rate in tensile deformation of a polycrystalline material, and a gigantic elongation in excess of several hundreds of percents is demonstrated without causing local shrinkage".
  • the shape of the crystal itself is basically not changed and deformation is attained by sliding at the crystallite interfaces. This phenomenon is called as grain boundary sliding.
  • Superplastic deformation generally occurs when crystal grain diameter of a material is decreased and a sample is heated to a temperature of about 50% the liquidus temperature or to a higher temperature.
  • Examples relating to methods for forming magnesium alloy sheet materials by using superplastic forming include: (1) a magnesium alloy part and a method for manufacture thereof ( Japanese Patent Application Laid-open No. 2004-149841 ), (2) a magnesium alloy part and a method for manufacture thereof ( Japanese Patent Application Laid-open No. 2003-311360 ), (3) a method for spindle processing of a magnesium material and an apparatus therefor ( Japanese Patent Application Laid-open No. 2000-126827 ), and (4) a method for deep drawing of a magnesium alloy sheet material and a formed body obtained ( Japanese Patent Application Laid-open No. 2004-58111 ).
  • An important feature of these methods is that a complex structural member can be fabricated by superplastic forming by performing boss formation, spindle processing, and deep drawing with respect to a sheet material.
  • Grain boundary sliding is the main superplastic deformation mechanism of magnesium alloys.
  • a principle diagram of grain boundary sliding is shown in FIG. 1.
  • Grain boundary sliding indicates a mechanism by which deformation is attained by crystals moving along grain boundaries, without intragranular deformation. When ideal grain boundary sliding occurs between crystals, the crystals move along grain boundaries, without intragranular deformation. Therefore, a cavity unavoidably appears in the vicinity of a triple point of the grain boundary.
  • FIG. 2 shows a temperature dependence of grain boundary diffusion coefficients of various alloys ( M. Mabuchi et al.: “Tensile Properties at Room Temperature to 823 K of Mg-4Y-3RE Alloy", Mater. Trans. 43 (2002), pp. 2063-2068 ).
  • M. Mabuchi et al. “Tensile Properties at Room Temperature to 823 K of Mg-4Y-3RE Alloy", Mater. Trans. 43 (2002), pp. 2063-2068 ).
  • a dimensionless temperature normalized by melting point is plotted against the abscissa.
  • a dimensionless grain boundary diffusion coefficient is plotted against the ordinate.
  • a grain boundary diffusion coefficient of magnesium can be confirmed to be much higher than that of aluminum and iron over the entire temperature range. Even if a cavity appears in the vicinity of a triple point of grain boundaries during superplastic deformation in magnesium, which has a high grain boundary diffusion coefficient, the formation of cavities apparently can be moderated by diffusion. This is why superplastic forming can be actively used as a method for forming magnesium alloys.
  • FIG. 3 shows the pattern of internal cavities occurring when a rolled material of an AZ31 magnesium alloy (Mg - 3 mass% Al - 1 mass% Zn - 0.5 mass% Mn) is subjected to tensile deformation at a temperature of 623 K and a strain rate of 1 x 10 -3 sec -1 to a true strain of 0.9. Further, in this case, the initial grain diameter was 10 ⁇ m. According to FIG.
  • the present invention has been created with the foregoing in view based on the discovery made by the inventors that a process of fabricating and providing a magnetism alloy case which is ensuring formability as a superplastically formed body and having a complex shape can be realized by specifying the composition of the magnesium alloy sheet material and reducing the amount of internal impurities to an appropriate value or below. It is an object of the present invention to provide a high-quality magnesium alloy case that has a complex shape and ensures formability as a superplastically formed body.
  • the present invention that resolves the above-described problems and provides a magnesium alloy case comprising a superplastically formed body of a magnesium alloy sheet material that comprises 1.0 to 10.0 mass% of aluminum, 0.5 to 3.0 mass% of zinc, and 0.1 to 0.8 mass% of manganese as a part of added alloying elements and has an oxygen concentration of 300 mass ppm or less, this superplastically formed body having a structure in which the formation of cavities during the superplastic forming is inhibited.
  • the case comprises a superplastically formed body of a magnesium alloy sheet material with an oxygen concentration of 100 mass ppm or less, (2) some zones of the magnesium alloy sheet material are formed by the superplastic forming, (3) the superplastic forming is a deep drawing, (4) the superplastic forming is a stretch forming, (5) the superplastic forming is a blow forming, and (6) crystal grains in part of the magnesium alloy case have a size of 20 ⁇ m or less.
  • the present invention also relates to a structural lightweight member comprising the magnesium alloy case.
  • the inventors have focused their attention on oxides present inside a magnesium alloy sheet material as means for ensuring formability as a superplastically formed body and making it possible to provide a high-quality magnesium alloy case having a complex shape.
  • magnesium has the highest affinity to oxygen and it has been used as a deoxidizing agent in iron and steel refining and the like.
  • the operations are performed under a cover gas such as a gas mixture of SF 6 and CO 2 so that molten magnesium does not come into contact with the air, but due to process restrictions it is difficult to avoid oxidation of molten magnesium occurring before the solidification stage.
  • Oxides (MgO or Al 2 O 3 ) that are nonmetallic inclusions are presently separated by aggregation, flotation and precipitation induced by blowing argon into magnesium in a molten state.
  • the cavity formation starts from the oxides.
  • a mechanism of cavity formation is shown in FIG. 4. Because stress concentration occurs close to the oxides during superplastic forming and also because dislocations are accumulated around the oxides, cavity formation that starts from oxides is initiated. When cavity formation shown in FIG. 4 occurs frequently in a material, the cavities are associated together, thereby causing fracture.
  • a magnesium alloy can be provided with a complex shape by using superplastic forming by controlling the concentration of oxygen in a magnesium alloy sheet material to 300 mass ppm or less, preferably 100 mass ppm or less.
  • concentration of oxygen in a magnesium alloy sheet material to 300 mass ppm or less, preferably 100 mass ppm or less.
  • the oxides should be prevented as thoroughly as possible from being incorporated into the magnesium alloy sheet material.
  • the inventors have confirmed that a phenomenon according to which the oxides enhance the formation of cavities can be inhibited by suppressing the concentration of oxygen to 300 ppm or less, preferably to 100 ppm. If the concentration of oxygen in the magnesium alloy sheet material exceeds 300 ppm, the aforementioned cavity formation and expansion of cavities cannot be inhibited.
  • the superplastically formed body be manufactured by using a magnesium alloy sheet material in which the concentration of oxygen is highly accurately controlled to a predetermined range so that the concentration of oxygen does not exceed 300 mass ppm.
  • a magnesium alloy has fine crystal grains of 20 ⁇ m or less, preferably fine crystal grains of 15 ⁇ m or less
  • the superplastic phenomenon can be easily demonstrated in a temperature range of 473 K or higher to 723 K or lower and strain rate region of 1 x 10 -5 1/sec or more to 1 x 10 -1 1/sec or less.
  • a process in which a strain in part of a magnesium alloy sheet material is 1.0 or more or part of the sheet material is deformed by grain boundary sliding is defined as superplastic deformation.
  • crystal grains of the sheet material do not grow during forming or the crystal grains are refined following the dynamic recrystallization.
  • the crystal grains in the zone of the formed body where the largest deformation has occurred are 20 ⁇ m or less, preferably 15 ⁇ m, it can serve as evidence of superplastic forming.
  • the crystal grain diameter of a magnesium alloy sheet material supplied to superplastic forming be decreased to 20 ⁇ m or less.
  • a magnesium alloy sheet material having comparatively coarse grains with a diameter of about 40 ⁇ m also can be supplied to superplastic forming. Even when a magnesium alloy sheet material having coarse grains of about 40 ⁇ m in diameter is supplied to superplastic forming, the crystal grains of the sheet material can be refined and effective superplastic forming can be provided to the magnesium alloy sheet material by using dynamic recrystallization that accompanies the processing.
  • the alloy comprise 1.0 to 10.0 mass% of aluminum, 0.5 to 3.0 mass% of zinc, and 0.1 to 0.8 mass% of manganese as a part of added alloy elements.
  • 1.0 to 10.0 mass% or aluminum be added as an additional alloying element.
  • 1 mass% or more of aluminum solid solution strengthening of the magnesium alloy can be expected. If 6 mass% or more of aluminum is added, then a network-like ⁇ phase (Mg 17 Al 12 ) can precipitate on grain boundaries, thereby further increasing the strength of the material.
  • a network-like ⁇ phase Mg 17 Al 12
  • ductility of the magnesium alloy after forming might be greatly degraded. Therefore, it is preferred that the amount of aluminum added to the alloy is 1.0 mass% or more to 10 mass% or less.
  • the addition of zinc is necessary to maintain the strength of recycled material.
  • the addition of 3.0 mass% or more of zinc sometimes causes undesirable degradation of corrosion characteristic.
  • Manganese can moderate the influence of iron that is an impurity element degrading corrosion resistance, and this effect is demonstrated most effectively when manganese is added within the above-described range.
  • the addition of manganese is indispensable for controlling the crystal grain size of the magnesium alloy sheet material.
  • crystal grains inside the material grow during superplastic forming and fine crystal grains that can initiate grain boundary sliding are difficult to maintain unless an appropriate amount of manganese is added.
  • 0.8 mass% or more of manganese is added, then coarse intermetallic compounds of manganese and aluminum are formed inside the material and an adverse effect is produced on ductility and strength of the material. Accordingly, the addition of 0.8 mass% or more of manganese is undesirable.
  • the magnesium alloy case in accordance with the present invention that is obtained by subjecting the magnesium alloy sheet material to a superplastic forming does not depend on the type of the superplastic forming.
  • processes suitable for forming the magnesium alloy sheet material by the superplastic forming include a deep drawing, stretch forming, and blow forming.
  • formability as a superplastically formed body can be ensured and a high-quality case having a complex shape can be manufactured essentially by highly accurately controlling the material quality of the magnesium alloy sheet material, and a magnesium alloy case manufactured by using any method can be the object of the present invention.
  • the formation of cavities in superplastic forming was difficult to prevent and the crystal grains were difficult to refine to a size of 20 ⁇ m or less, but in the magnesium alloy case manufactured in accordance with the present invention, the formation of cavities caused by superplastic forming is inhibited to a degree larger than that in the case manufactured through other processes, the crystal grains are refined to a size of 20 ⁇ m or less, and a product with high fracture resistance and high strength is therefore obtained. By analyzing these properties, the two products can be clearly distinguished (identified).
  • a magnesium alloy case having a complex shape can be manufactured by a superplastic forming by controlling the material composition and oxygen concentration of a magnesium alloy sheet material;
  • a magnesium alloy case comprising a superplastically formed body having a high fracture resistance and a high strength and having a structure in which the cavities to be formed during the superplastic forming is inhibited can thereby be provided;
  • an ultra-lightweight magnesium alloy case that is expected to serve as a next-generation structural lightweight material can be provided.
  • the AZ31 magnesium alloy has a composition of Mg - 3 mass% Al - 1 mass% Zn - 0.5 mass% Mn and is a typical magnesium alloy to be used for wrought material.
  • AZ31 magnesium alloy sheet materials with a width of 50 mm and a thickness of 5 mm that had different internal oxygen concentrations were prepared. These magnesium alloy sheet materials were subjected to hot rolling at a sample temperature of 673 K to manufacture rolled materials of magnesium alloys with a thickness of 1 mm. No roll heating was performed during hot rolling, and the draft ratio per 1 pass was 12%.
  • the concentration of oxygen in the samples obtained and the average crystal grain size of the samples are presented together in Table 1.
  • a rectangular magnesium alloy sheet material with a length of 70 mm, a width of 70 mm, and a thickness of 1 mm was cut out from the rolled material and subjected to superplastic blow forming.
  • a pressure die and a forming die shown in FIG. 5 were used.
  • the magnesium alloy sheet material was fixed between two dies, the dies and the sample piece were heated to 673 K, and blow forming was implemented by blowing N 2 gas under a pressure of 0.2 MPa or 0.5 MPa on the magnesium alloy sheet material from the pressure die.
  • the strain rate of the material under an applied pressure of 0.2 MPa is equivalent to about 1 x 10 -5 sec -1
  • the strain rate of the material under an applied pressure of 0.5 MPa is equivalent to about 1 x 10 -4 sec -1 .
  • the results obtained in blow forming the AZ31 magnesium alloy sheet materials of various types are shown in Table 2.
  • a typical outer shape of the sheet material after blow forming is shown in FIG. 6.
  • Observations of the outer shapes obtained in Embodiment (Example) 1 and Embodiment 7 shown in FIG. 6 confirm that a perfect cup shape could be formed in Embodiment 1.
  • Embodiment 7 although the cup shape could not be formed, a dome-like shape could be formed.
  • the results obtained in Embodiment 1 and Embodiment 7 relate to a sheet material with the lowest internal oxygen concentration (14 mass ppm). According to the embodiments, the formability tended to degraded with the increase in oxygen concentration.
  • Table 2 also shows the crystal grain size of samples after blow forming.
  • the measurement location was a central portion of the sheet material that is the portion with the highest level of deformation of the sheet material.
  • the table demonstrates that a state with fine crystal grains (20 ⁇ m or less) was maintained in all the samples and the samples were deformed by superplastic forming.
  • FIG. 7 shows the results obtained in observing cross sections of the samples subjected to blow forming in Embodiment 3 and Embodiment 11 and measuring the sheet thickness strains in various zones.
  • the X axis shows the measurement zones of strains and shows a sheet thickness strain distribution on concentric circles, wherein the central portion of the sheet material is assumed to be at 0 mm.
  • the Y axis shows the sheet thickness strain distribution in various measurement points. According to FIG. 7, a sheet thickness strain of 1.0 or more was confirmed in some measurement locations at any strain rate, thereby indicating that superplastic forming has been reached. Thus, it was confirmed that superplastic forming was developed in samples with highly accurately controlled oxygen concentration.
  • the present invention relates to a magnesium alloy case, and the invention can provide a magnesium alloy case having a complex shape, high fracture resistance and a high strength, and a structure in which cavity formation is inhibited even in superplastic forming by accurately specifying the composition and impurities of the magnesium alloy sheet material.
  • the present invention is useful because it enables mass production and practical use of ultra-lightweight magnesium alloy cases that can be actively applied to cases of household electronic products, for example, digital cameras, notebook personal computers, and PDA.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Shaping Metal By Deep-Drawing, Or The Like (AREA)
  • Fuel Cell (AREA)
EP05709520A 2004-10-29 2005-01-31 Gehäuse aus magnesiumlegierung Withdrawn EP1826284A4 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2004316333A JP2006127973A (ja) 2004-10-29 2004-10-29 燃料電池セル
PCT/JP2005/001363 WO2006046320A1 (ja) 2004-10-29 2005-01-31 マグネシウム合金製筐体

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EP1826284A1 true EP1826284A1 (de) 2007-08-29
EP1826284A4 EP1826284A4 (de) 2008-01-02

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EP05709520A Withdrawn EP1826284A4 (de) 2004-10-29 2005-01-31 Gehäuse aus magnesiumlegierung

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Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5192702B2 (ja) * 2007-01-31 2013-05-08 京セラ株式会社 横縞型燃料電池セルおよびセルスタック並びに燃料電池
JP5377222B2 (ja) * 2009-10-28 2013-12-25 京セラ株式会社 燃料電池セル、セルスタック装置および燃料電池モジュールならびに燃料電池装置
JP4901997B2 (ja) * 2010-03-26 2012-03-21 日本碍子株式会社 燃料電池セル
JP2012054015A (ja) * 2010-08-31 2012-03-15 Kyocera Corp 固体酸化物形燃料電池セルおよび燃料電池
US8574790B2 (en) * 2010-10-04 2013-11-05 GM Global Technology Operations LLC Fuel cell electrodes with graded properties and method of making
JP2012094427A (ja) * 2010-10-28 2012-05-17 Kyocera Corp 固体酸化物形燃料電池セルおよび燃料電池
KR101812533B1 (ko) 2013-03-28 2017-12-27 쿄세라 코포레이션 고체 산화물형 셀, 셀 스택 장치와 모듈 및 모듈 수납 장치
EP3685462A4 (de) 2017-09-19 2021-06-02 Phillips 66 Company Festoxidbrennstoffzellen mit elektrolyten mit abgestufter dicke

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
LEE C J; HUANG J C: "Cavitation characteristics in AZ31 Mg alloys during LTSP or HSRSP" ACTA MATERIALIA, vol. 52, no. 10, 7 June 2004 (2004-06-07), pages 3111-3122, XP002458956 *
See also references of WO2006046320A1 *

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JP2006127973A (ja) 2006-05-18
EP1826284A4 (de) 2008-01-02

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