US20030173005A1 - Method of manufacturing magnesium alloy products - Google Patents

Method of manufacturing magnesium alloy products Download PDF

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Publication number
US20030173005A1
US20030173005A1 US10/385,722 US38572203A US2003173005A1 US 20030173005 A1 US20030173005 A1 US 20030173005A1 US 38572203 A US38572203 A US 38572203A US 2003173005 A1 US2003173005 A1 US 2003173005A1
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magnesium alloy
forging
temperature
crystal grain
semifinished product
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US10/385,722
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Kenji Higashi
Kinji Hirai
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ADVANCED TECHNOLOGIES Inc
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Takata Corp
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Publication of US20030173005A1 publication Critical patent/US20030173005A1/en
Assigned to ADVANCED TECHNOLOGIES, INC. reassignment ADVANCED TECHNOLOGIES, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: TAKATA CORPORATION
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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
    • 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 a method of manufacturing magnesium alloy products comprising casting a magnesium alloy and forging the thus obtained cast semifinished product into a desired shape.
  • magnesium (Mg) has a specific gravity of 1.8 which is smaller than the specific gravity of 2.7 of aluminum (Al) as a typical light metal
  • magnesium alloys are extremely lightweight.
  • magnesium alloys have higher specific modulus than that of aluminum alloys and have excellent in heat conductivity. Accordingly, magnesium alloys are widely used as materials for casings and parts of electric equipments and electronics devices.
  • Magnesium alloys have poor formability and are therefore hardly formed into desired shapes. That is, magnesium alloys have small specific latent heat of solidification and are thus fast in solidification speed. Therefore, it is difficult to cast magnesium alloy because defects such as porosities and flow lines may be easily created in obtained cast products. Especially on appearance-conscious products, the magnesium alloy has low yield. Further, because puttying should be required for such defects, the manufacturing cost increase. Magnesium alloys have hexagonal close-packed crystal structure and have therefore low ductility. Since the work of pressing or forging a plate or rod material should be conducted at a high temperature from 300 to 500° C., there are problems such as low processing speed, the increased number of processes, die's short life, and the like.
  • Japanese Unexamined Patent Publication No. 2001-294966 (incorporated by reference herein). That is, a magnesium alloy is injected by a die-cast or thixo molding machine to mold a plate. After rolling the plate at a normal temperature and giving a distortion to the plate, the plate is heated at a temperature from 350 to 400° C. to recrystallize the crystal structure to be refined into small grains from 0.1 to 30 ⁇ m, thereby improving the ductility. By pressing or forging the obtained magnesium alloy plate having improved ductility, products formed in an arbitrary shape can be obtained. Further, Japanese Unexamined Patent Publication Nos.
  • 2001-170734 and 2001-170736 (both incorporated by reference herein) teach a method of forming a boss part having a thickness of seven times or ten times of that of a main part of a product by forging a magnesium alloy plate and a plurality of rough forging steps and finishing forging steps.
  • magnesium alloy has low ductility and poor formability, magnesium alloy is difficult to form into a complex shape, for example, it is difficult to form a boss as formed by the casting.
  • the casting property and the elongation property of magnesium alloys are in an inverse relationship.
  • the material to be cast are AZ91, AM50, AM60, and the like containing a larger amount of aluminum so as to have low melting temperature.
  • AZ31 preferably employed as the material to be pressed and forged are AZ31 containing a smaller amount of aluminum so as to have high ductility. The larger the aluminum content is, the higher the corrosion resistance is. Accordingly, AZ31 is poor in corrosion resistance as compared to AZ91. The poor corrosion resistance is one of reasons for limited application of AZ31.
  • the present invention was made under the aforementioned conventional circumstances and at least one object of the present invention is to provide a method of manufacturing magnesium alloy products comprising a combination of casting and forging for forming a magnesium alloy of which composition allows casting and which is excellent in forgeability, thereby achieving the manufacture of products, which have complex and accurate shape and exhibit high reliability of properties and enough corrosion resistance, at sufficiently high yield.
  • the present invention includes a method of manufacturing magnesium alloy products comprising: casting a magnesium alloy containing 2-10 mass % aluminum to obtain a cast semifinished product having crystal grain size not greater than 30 ⁇ m, subjecting the cast semifinished product to solution treatment at a temperature between the solid solution temperature and the solidus curve of the composition of the alloy, after that, forging the semifinished product to have a forged semifinished product having crystal grain size not greater than 10 ⁇ m, and further forging the forged semifinished product to have a desired shape.
  • the cast semifinished product which is made to have crystal grain size not greater than 30 ⁇ m by casting is subjected to solution treatment, the crystal grains are enlarged, but second-phase grains which are formed during the casting and are large and fragile are disappeared, thereby increasing the elongation and thus improving the plastic formability.
  • the cast semifinished product having improved plastic formability attained by the solution treatment is forged.
  • the dynamic recrystallization according to this forging refines the crystal grain size to be 10 ⁇ m or less, thereby further improving the forgeability.
  • the cast semifinished product which is made to have crystal grain size not greater than 30 ⁇ m by casting is subjected to solution treatment, after that, is forged to have crystal grain size not greater than 10 ⁇ m, and is further forged into a desired shape.
  • the suitable aluminum content of the magnesium alloy is in a range from 2.5 to 6 mass % and the casting is preferably conducted in the die casting method or the thixo molding method.
  • the solution treatment is preferably conducted at a temperature between 380 and 440° C. for 1 to 24 hours and the forging for refining crystal grains after solution treatment and the shaping forging after that are preferably conducted under conditions of a strain rate and temperature which are set to have a Z value in a range from 10 9 to 10 13 .
  • the present invention also includes a method of manufacturing magnesium alloy products comprising: casting a magnesium alloy containing 2-10 mass % aluminum to obtain a cast semifinished product having crystal grain size not greater than 10 ⁇ m, subjecting the cast semifinished product to solution treatment at a temperature between the solid solution temperature and the solidus curve of the composition of the alloy, and after that, forging the semifinished product to have a desired shape.
  • the cast semifinished product which is made to have crystal grain size not greater than 10 ⁇ m by casting is subjected to solution treatment, the crystal grains are enlarged, but second-phase grains which are formed during the casting and are large and fragile are disappeared, thereby increasing the elongation and thus improving the plastic formability.
  • the product can be formed into a desired shape.
  • the cast semifinished product which is made to have crystal grain size not greater than 10 ⁇ m by casting is subjected to solution treatment, and after that, is further forged into the desired shape.
  • the suitable aluminum content of the magnesium alloy is in a range from 2 to 6 mass % and the casting is preferably conducted in the die casting method.
  • the solution treatment is preferably conducted at a temperature between 380 and 440° C. for 1 to 24 hours and the forging is preferably conducted under conditions of a strain rate and temperature which are set to have a Z value lower than 10 13 .
  • the Z value is a temperature-compensating strain rate indicating the relation between temperature and strain rate and is so-called Zener-Hollomon Parameter defined by the following equation (I) as the relational expression for the dependence of temperature and strain rate on the flow stress:
  • FIG. 1 is a graph showing crystal grain sizes of thixo molding cast articles (after solution treatment) in Example 1.
  • FIG. 3 is a graph showing crystal grain sizes of die cast articles (after solution treatment) in Example 2.
  • a method of manufacturing magnesium alloy products includes the following steps. First, a magnesium alloy containing 2-10 mass % aluminum is cast to obtain a cast semifinished product having crystal grain size not greater than 30 ⁇ m.
  • the aluminum content of the magnesium alloy is less than 2 mass %, the corrosion resistance is generally poor and the melting temperature is high so that it is not suitable for casting. If the aluminum content of the magnesium alloy is more than 10 mass %, it is impossible to obtain enough increase of plastic formability obtained by solution treatment in a subsequent step and it is impossible to obtain products after solution treatment having excellent forgeability. Therefore, the aluminum content of the magnesium alloy is preferably from 2 to 10 mass %, more preferably, from 2.5 to 6 mass %.
  • the obtained cast product has generally large thickness so that the solidification of melt magnesium alloy is slow.
  • crystal grain size of the cast product is better.
  • the crystal grain size not greater than 30 ⁇ m is allowed.
  • the casting is conducted to have crystal grain size from 15 to 30 ⁇ m depending on the employed casting method and the composition of used alloy.
  • the temperature of the solution treatment may be in a range between the solid solution temperature and the solidus curve of the composition of the used alloy and a suitable temperature is from 380 to 430° C.
  • a suitable temperature is from 380 to 430° C.
  • the temperature of the solution treatment is lower than the solid solution temperature or lower than 380° C.
  • large compounds of aluminum and magnesium may be deposited, impairing the plastic formability.
  • the temperature of the solution treatment exceeds the solidus curve or 430° C., liquid phase may be generated, thus impairing the plastic formability.
  • the time period of the solution treatment is suitably from 1 to 24 hours. It is preferable to increase the time period when the temperature is low and to decrease the time period when the temperature is high.
  • the semifinished product is forged to obtain a forged semifinished product having crystal grain size not greater than 10 ⁇ m (hereinafter, the forging for refining crystal grains will be sometimes referred to as “grain-refining forging”).
  • the forged semifinished product is further forged for shaping the semifinished product into a desired shape, thereby obtaining a product (hereinafter, the forging for shaping a semifinished product into a desired shape will be sometimes referred to as “shaping forging”).
  • the grain-refining forging is conducted for refining crystal grains of cast semifinished product by dynamic recrystallization.
  • the grain-refining forging and the shaping forging should be conducted under conditions which are a function of the composition of magnesium alloy.
  • the conditions of the grain-refining forging depend on the composition of magnesium alloy. However, the conditions of strain rate and temperature for the grain-refining forging are preferably set to have a Z value in a range from 10 9 to 10 13 , more preferably, in a range from 10 10 to 10 13 .
  • the conditions of the shaping forging also depend on the composition of magnesium alloy.
  • the conditions of strain rate and temperature for the shaping forging are preferably set to have a Z value of 10 13 or less, preferably in a range from 10 8 to 10 13 , more preferably, in a range from 10 9 to 10 12 .
  • the forging conditions outside of the range of Z value may create defects such as cracks and splits, not allowing the forging.
  • the condition for conducting the grain-refining forging is determined according to the composition of the alloy to have a Z value in the suitable range within a range from 10 ⁇ 3 to 10 ⁇ 1 sec ⁇ 1 of the strain rate and a range from 200 to 500° C. of the temperature.
  • the condition for conducting the shaping forging is determined according to the composition of the alloy to have a Z value in the suitable range within a range from 10 ⁇ 3 to 10 ⁇ 2 sec ⁇ 1 of the strain rate and a range from 200 to 400° C. of the temperature.
  • the crystal grains are refined to have crystal grain size not greater than 10 ⁇ m by grain-refining forging, thereby improving the plastic formability as an effect of the forging, thus allowing the product to be subjected to the shaping forging.
  • the crystal grain size not greater than 10 ⁇ m is allowed.
  • the range of crystal grain sizes to be obtained by the grain-refining forging is from 1 to 10 ⁇ m.
  • a method of manufacturing magnesium alloy products includes the following steps. First, a magnesium alloy containing 2-10 mass % aluminum is cast to obtain a cast semifinished product having crystal grain size not greater than 10 ⁇ m.
  • the aluminum content of the magnesium alloy is less than 2 mass %, the corrosion resistance should be poor. If the aluminum content of the magnesium alloy is more than 10 mass %, it is impossible to obtain enough increase of plastic formability to be attained by solution treatment as the following step and it is impossible to obtain products after solution treatment having excellent forgeability. Therefore, the aluminum content of magnesium alloy is from 2 to 10 mass %, preferably, from 2 to 6 mass %.
  • [0049] Preferably employed are die casting method because its cooling/solidification speed is relatively high and the crystal grains can be significantly refined.
  • the crystal grain size of the cast semifinished product is preferably smaller and maybe 10 ⁇ m or less. Generally, the range of crystal grain size of the semifinished product obtained by the casting is from 5 to 10 ⁇ m.
  • the thus obtained cast semifinished product having crystal grain size not greater than 10 ⁇ m is then subjected to solution treatment at a temperature between the solid solution temperature and the solidus curve of the composition of the used alloy. Because of the same reasons of the solution treatment as the aforementioned method, the suitable temperature is from 380 to 430° C. and the suitable time period of the solution treatment is from 1 to 24 hours. After the solution treatment, the cast semifinished product is forged to obtain a product of a desired shape.
  • the forging should be conducted under conditions allowing forging process depending on the composition of magnesium alloy similarly to the forging processes described above.
  • the conditions of the forging depend on the composition of magnesium alloy. However, the conditions of strain rate and temperature for the forging are preferably set to have a Z value less than 10 13 , more preferably in a range from 10 6 to 10 12 .
  • the Z value of 10 13 or more may create defects such as clacks and splits, not allowing the forging.
  • the conditions for conducting the forging is determined according to the composition of the alloy to have a Z value in the suitable range within a range from 10 ⁇ 3 to 10 ⁇ 1 sec ⁇ 1 of strain rate and a range from 200 to 500° C. of temperature.
  • Mg alloy ingots used for the following examples were prepared by adding magnesium and zinc to the AZ91 alloy ingots and governing the qualities of the ingots. In this manner, Mg alloy ingots having compositions from AZ81 to AZ 21 were prepared. Table 1 shows results of componential analysis of the used AZ 91 alloy ingot and prepared ingots.
  • the ingots from AZ91 to AZ21 were ground to make chips for thixo molding.
  • the chips were used in casting process.
  • the injection speed was set at 4 m/sec that is the maximum under the idling condition and the die temperature was set at 250° C.
  • cast articles of a box shape of 181 mm length ⁇ 255 mm width ⁇ 10 mm height having a bottom and no lid and 1.5 mm thickness were obtained.
  • the casting process was conducted with finding a mold-filling condition by controlling the temperature of a barrel and a nozzle of the molding machine because each ingot has each own melting point.
  • Table 2 shows the temperatures of the barrel tips during casting process of the respective alloys. TABLE 2 TEMPERATURES OF BARREL TIPS DURING THIXO MOLDING CASTING ALLOY TEMPERATURE (° C.) AZ91 620 AZ81 618 AZ71 619 AZ61 624 AZ51 627 AZ41 640 AZ31 638
  • the cast articles were subjected to heat treatment at 430° C. for 1 hour and, after that, the crystal grain size were measured again in the same manner.
  • AZ91 has crystal grain size of 28 ⁇ m, i.e. relatively large grain size, because of small temperature difference
  • AZ51 has crystal grain size of 14 ⁇ m, i.e. relatively small grain size, because of large temperature difference.
  • AZ41, ZA31 have grain size from 18 to 20 ⁇ m because cooling delay effect is attained in high-temperature liquid alloy.
  • AZ91 through AZ71 aluminum-rich alloys have lower elongation from 15 to 24%, while AZ61 through AZ31 have elongation of 40% or more, significantly improving the plastic formability.
  • the aluminum content of cast article to be forged is preferably equal to or more than 25 mass % in view of castability and preferably equal to or less than 6 mass % in view of plastic formability.
  • the forging conditions for refining crystal grain size to be 10 ⁇ m or less allowing superplasticity forging are Z value ranging from 10 9 to 10 13 , preferably from 10 10 to 10 13 .
  • Alloys containing larger amount of aluminum in which ⁇ -phase is easily deposited at grain boundaries so as to easily impair the grain boundary sliding, should require higher processing temperature, that is, higher Z value to form boss. On the other hand, even when the crystal grain size exceeds 10 ⁇ m, some alloys are allowed to form boss by setting the temperature high.
  • the mold temperature of 400° C. or more impairs the durability of mold so that it is not practical. It is possible to improve the heat resistivity of the mold by applying heat resistance material or treating the surface. However, since the cost of the mold is increased, it is not preferable.
  • the forging condition for forming alloy into a desired shape is a Z value of 10 13 or less, preferably in a range from 10 8 to 10 13 .
  • the crystal grain sizes of the die cast articles were smaller than the crystal grain sizes of the thixo molding cast articles. Even before the solution treatment, the crystal grain sizes were below 10 ⁇ m so that the grain-refining forging is not required. This is attributed to the fact that the cooling effect could be attained because the molding machine was so fast in filling speed.
  • composition suitable for forging alloy cast to have crystal grain size not greater than 10 ⁇ m is aluminum content ranging from 2 to 6 mass % and the forging condition is a Z value of 1.0 ⁇ 10 13 or less.
  • a combination of casting and forging is employed for forming magnesium alloy of which composition allows casting and which is excellent in forgeability, thereby achieving the manufacture of products, which have complex and accurate shape and exhibit high reliability of properties and enough corrosion resistance, at sufficiently high yield ratio.
US10/385,722 2002-03-12 2003-03-12 Method of manufacturing magnesium alloy products Abandoned US20030173005A1 (en)

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JP2002067184A JP3861720B2 (ja) 2002-03-12 2002-03-12 マグネシウム合金の成形方法
JP2002-067184 2002-03-12

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EP (1) EP1347074B1 (ko)
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DE (1) DE60304920T8 (ko)
TW (1) TWI263681B (ko)

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US20050150577A1 (en) * 2004-01-09 2005-07-14 Takata Corporation Magnesium alloy and magnesium alloy die casting
CN100424216C (zh) * 2006-10-14 2008-10-08 重庆工学院 一种用于Mg-Al系铸造镁合金热处理强化的固溶处理方法
US20110033332A1 (en) * 2004-06-30 2011-02-10 Sumitomo Electric Industries, Ltd. Producing method for magnesium alloy material
US9903010B2 (en) 2014-04-18 2018-02-27 Terves Inc. Galvanically-active in situ formed particles for controlled rate dissolving tools
US10150713B2 (en) 2014-02-21 2018-12-11 Terves, Inc. Fluid activated disintegrating metal system
US10329643B2 (en) 2014-07-28 2019-06-25 Magnesium Elektron Limited Corrodible downhole article
US10625336B2 (en) 2014-02-21 2020-04-21 Terves, Llc Manufacture of controlled rate dissolving materials
US10689740B2 (en) 2014-04-18 2020-06-23 Terves, LLCq Galvanically-active in situ formed particles for controlled rate dissolving tools
US10870146B2 (en) 2014-02-21 2020-12-22 Terves, Llc Self-actuating device for centralizing an object
US11649526B2 (en) 2017-07-27 2023-05-16 Terves, Llc Degradable metal matrix composite
US11674208B2 (en) 2014-02-21 2023-06-13 Terves, Llc High conductivity magnesium alloy

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JP5050199B2 (ja) * 2006-03-30 2012-10-17 国立大学法人電気通信大学 マグネシウム合金材料製造方法及び装置並びにマグネシウム合金材料
US20080000557A1 (en) * 2006-06-19 2008-01-03 Amit Ghosh Apparatus and method of producing a fine grained metal sheet for forming net-shape components
JP2008229650A (ja) * 2007-03-19 2008-10-02 Mitsui Mining & Smelting Co Ltd マグネシウム合金塑性加工部材及びその製造方法
AU2007202131A1 (en) * 2007-05-14 2008-12-04 Joka Buha Method of heat treating magnesium alloys
JP2009255149A (ja) * 2008-04-18 2009-11-05 Mitsui Mining & Smelting Co Ltd 非鉄金属成形体の製造方法
CN101921940B (zh) * 2009-06-16 2013-03-13 富准精密工业(深圳)有限公司 镁合金及其制备方法
WO2012091112A1 (ja) * 2010-12-28 2012-07-05 住友電気工業株式会社 マグネシウム合金材
JP5700005B2 (ja) * 2012-09-05 2015-04-15 株式会社豊田中央研究所 複合マグネシウム合金部材およびその製造方法
CN103203602B (zh) * 2013-04-15 2015-06-10 中国兵器工业第五二研究所 一种镁合金轮毂的制备方法
CN103447433B (zh) * 2013-09-04 2015-09-09 中南大学 一种大尺寸镁合金锻饼的制备方法
CN103447432B (zh) * 2013-09-04 2015-09-09 中南大学 一种大尺寸镁合金零件的等温模锻工艺
CN105951012B (zh) * 2016-06-27 2017-10-03 长沙新材料产业研究院有限公司 一种低合金化镁合金的变温锻造强化工艺
DE102016223089A1 (de) * 2016-11-23 2018-05-24 Schaeffler Technologies AG & Co. KG Verfahren zur Herstellung einer Wälzlagerkomponente aus einer Nickel-Titan-Legierung
CN107245681B (zh) * 2017-05-31 2018-08-28 江苏金基特钢有限公司 一种高耐蚀性镁合金的优化热处理工艺

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Cited By (21)

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Publication number Priority date Publication date Assignee Title
US20050150577A1 (en) * 2004-01-09 2005-07-14 Takata Corporation Magnesium alloy and magnesium alloy die casting
US9943904B2 (en) * 2004-06-30 2018-04-17 Sumitomo Electric Industries, Ltd. Producing method for magnesium alloy material
US20110033332A1 (en) * 2004-06-30 2011-02-10 Sumitomo Electric Industries, Ltd. Producing method for magnesium alloy material
CN100424216C (zh) * 2006-10-14 2008-10-08 重庆工学院 一种用于Mg-Al系铸造镁合金热处理强化的固溶处理方法
US11365164B2 (en) 2014-02-21 2022-06-21 Terves, Llc Fluid activated disintegrating metal system
US10870146B2 (en) 2014-02-21 2020-12-22 Terves, Llc Self-actuating device for centralizing an object
US11685983B2 (en) 2014-02-21 2023-06-27 Terves, Llc High conductivity magnesium alloy
US11674208B2 (en) 2014-02-21 2023-06-13 Terves, Llc High conductivity magnesium alloy
US11613952B2 (en) 2014-02-21 2023-03-28 Terves, Llc Fluid activated disintegrating metal system
US10625336B2 (en) 2014-02-21 2020-04-21 Terves, Llc Manufacture of controlled rate dissolving materials
US11097338B2 (en) 2014-02-21 2021-08-24 Terves, Llc Self-actuating device for centralizing an object
US10150713B2 (en) 2014-02-21 2018-12-11 Terves, Inc. Fluid activated disintegrating metal system
US10760151B2 (en) 2014-04-18 2020-09-01 Terves, Llc Galvanically-active in situ formed particles for controlled rate dissolving tools
US10724128B2 (en) 2014-04-18 2020-07-28 Terves, Llc Galvanically-active in situ formed particles for controlled rate dissolving tools
US10689740B2 (en) 2014-04-18 2020-06-23 Terves, LLCq Galvanically-active in situ formed particles for controlled rate dissolving tools
US9903010B2 (en) 2014-04-18 2018-02-27 Terves Inc. Galvanically-active in situ formed particles for controlled rate dissolving tools
US10329653B2 (en) 2014-04-18 2019-06-25 Terves Inc. Galvanically-active in situ formed particles for controlled rate dissolving tools
US10337086B2 (en) 2014-07-28 2019-07-02 Magnesium Elektron Limited Corrodible downhole article
US10329643B2 (en) 2014-07-28 2019-06-25 Magnesium Elektron Limited Corrodible downhole article
US11649526B2 (en) 2017-07-27 2023-05-16 Terves, Llc Degradable metal matrix composite
US11898223B2 (en) 2017-07-27 2024-02-13 Terves, Llc Degradable metal matrix composite

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JP3861720B2 (ja) 2006-12-20
EP1347074B1 (en) 2006-05-03
CN1443862A (zh) 2003-09-24
KR20030074385A (ko) 2003-09-19
DE60304920T8 (de) 2007-05-16
TW200304496A (en) 2003-10-01
TWI263681B (en) 2006-10-11
DE60304920D1 (de) 2006-06-08
CN1283822C (zh) 2006-11-08
EP1347074A1 (en) 2003-09-24
DE60304920T2 (de) 2007-01-04

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