EP1347074B1 - Method of manufacturing magnesium alloy products - Google Patents

Method of manufacturing magnesium alloy products Download PDF

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Publication number
EP1347074B1
EP1347074B1 EP03002095A EP03002095A EP1347074B1 EP 1347074 B1 EP1347074 B1 EP 1347074B1 EP 03002095 A EP03002095 A EP 03002095A EP 03002095 A EP03002095 A EP 03002095A EP 1347074 B1 EP1347074 B1 EP 1347074B1
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EP
European Patent Office
Prior art keywords
forging
temperature
magnesium alloy
crystal grain
cast
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Expired - Fee Related
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EP03002095A
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German (de)
English (en)
French (fr)
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EP1347074A1 (en
Inventor
Kinji c/o Takata Corporation Hirai
Kenji Higashi
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ADVANCED TECHNOLOGIES, INC.
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Takata Corp
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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 figure.
  • magnesium alloys are extremely lightweight.
  • magnesium alloys have higher specific modulus than the that of aluminum alloys and are excel 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 figures. 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 so that 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 ratio. Further, because puttying should be required for such defects, the manufacturing cost should 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 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 structrure to be miniaturized 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 figure can be obtained. Further, in Japanese Unexamined Patent Publication Nos.
  • the dynamic recrystallization process is initiated by hot forging the material.
  • the starting materials of this process are generally extruded materials.
  • the initial material may further be annealed.
  • the hot forging process is characterized by the Zener-Hollomon parameter.
  • magnesium alloy is easily solidified as mentioned above, however, flow lines may be easily created when molded by die casting. In addition, in some figures, it is difficult to fill the magnesium alloy in every corner. Accordingly, there are limitations on size and thickness. As the injection speed is increased, air or gas may be easily entrapped in liquid alloy, thereby creating porosities and thus reducing the reliability of properties.
  • magnesium alloy has low ductility and poor formability, magnesium alloy is hardly formed into a complex figure, 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 contracting 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.
  • preferably employed as the material to be pressed and forged are A231 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 the 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 figure and exhibit high reliability of properties and enough corrosion resistance, at sufficiently high yield.
  • a method of manufacturing magnesium alloy products according to the invention comprises steps of: casting of series AZ21, AZ31, AZ41, AZ51, and AZ61 using a die casting or a thixo molding method a magnesium alloy 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 under conditions of a strain rate and temperature which are set to have a value of the Zener-Hollomon parameter Z in the range from 10 9 to 10 13 , 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 figure.
  • the crystal grains are enlarged, but second-phase grains which are formed during the casting and are large and fragile disappear, thereby increasing the elongation and thus improving the plastic formability.
  • the cast semifinished product having the improved plastic formability attained by the solution treatment is forged.
  • the dynamic recrystallization according to this forging miniaturizes 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 figure.
  • the solution treatment is preferably conducted at a temperature between 380 and 440 °C for 1 to 24 hours and and the shaping forging is 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 .
  • a magnesium alloy of series AZ21, AZ31, AZ41, AZ51, and AZ61 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 should be 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 as the following step and it is impossible to obtain products after solution treatment having excellent forgeability. Therefore, the aluminum content of the magnesium alloy is from 2 to 10 mass %, preferably, from 2.5 to 6 mass %.
  • a die casting method or a thixo molding method is employed because their cooling/solidification speed is relatively high and the crystal grains can be miniaturized.
  • the obtained cast product has generally large thickness so that the solidification of melt magnesium alloy is slow. Therefore, crystals should grow during the cooling/solidification so as to have large crystal grain size to the extent of 200 ⁇ m.
  • the cooling/solidification speed is fast so that crystal grains are miniaturized to have crystal grain size not greater than 30 ⁇ m.
  • 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 thus obtained cast product having crystal grain size not greater than 30 ⁇ m is then subjected to solution treatment.
  • 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 the 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, huge 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 miniaturizing crystal grains will be sometimes referred to as "grain-miniaturizing forging”).
  • the forged semifinished product is further forged for shaping the semifinished product into a desired figure, thereby obtaining a product (hereinafter, the forging for shaping a semifinished product into a desired figure will be sometimes referred to as "shaping forging").
  • the grain-miniaturizing forging is conducted for miniaturizing crystal grains of cast semifinished product by dynamic recrystallization.
  • the grain-miniaturizing forging and the shaping forging should be conducted under conditions allowing forging process depending on the composition of magnesium alloy.
  • the conditions of the grain-miniaturizing forging depend on the composition of magnesium alloy. However, the conditions of strain rate and temperature for the grain-miniaturizing forging are set to have a Z value in a range from 10 9 to 10 13 , 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-miniaturizing 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 miniaturized to have crystal grain size not greater than 10 ⁇ m by grain-miniaturizing 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-miniaturizing forging is from 1 to 10 ⁇ m.
  • a magnesium alloy of series AZ21, AZ31, AZ41, AZ51 and AZ61 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 %.
  • the crystal grain size of the cast semifinished product is preferably smaller and may be 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 method of claim 1, 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 figure.
  • the forging should be conducted under conditions allowing forging process depending on the composition of magnesium alloy similarly to the forging processes of the method of claim 1.
  • 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 chaps, 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 I 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-allowing condition by controlling the temperature of a barrel and a nozzle of the molding machine because each ingot has each melting point.
  • Table 2 shows the temperatures of the barrel tips during casting process of the respective alloys.
  • the limit of AZ alloys allowing the casting by the thixo molding machine is 2.5% aluminum content.
  • 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 as 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 equal to or more than 25 mass % in view of castability and equal to or less than 6 mass % in view of plastic formability.
  • the forging conditions for miniaturizing 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 .
  • Samples in which crystal grain miniaturization by the aforementioned forging was sufficient and samples in which crystal grain miniaturization was insufficient were selected.
  • Plate-like specimens of 20 mm ⁇ 20 mm ⁇ 1.5 mm thickness were cut and taken from these selected samples. Each specimen was inserted into a cavity of 20 mm ⁇ 20 mm as a drag of a casting mold.
  • Each specimen was forged under conditions shown in Table 5 until the true strain reaches -1.1 by using a cope having a cylindrical concave of 3 mm diameter and 10 mm height and was formed into a boss shape. The respective forgeabilities during the forging process were evaluated. The evaluation results are shown in Table 5.
  • 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 figure is a Z value of 10 13 or less, preferably in a range from 10 8 to 10 13 .
  • Casting tests were conducting in the die casting method instead of thixo molding of Example 1. Die having the same shape as that for the thixo molding was used. Used alloys were ingots of the same batch as those used for the thixo molding machine, but not processed to be chips. By using a cold chamber die casting machine DC650tCLS available from Toshiba Machine Co., Ltd., articles were sequentially formed by casting under conditions that the temperature of liquid alloy was 700 °C, the injection speed was set at 5.0 m/sec at the highest, and the die temperature was set at 250 °C. The cast articles had the same size and shape as those of Example 1.
  • 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-miniaturizing 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.
  • Example 7 Since the obtained cast articles already had fine crystal grains, casting was conducted under the same conditions as those for grain-miniaturizing forging which had been conducted for the thixo molding articles in Example 1. For giving indication of forgeability of the respective cast articles, it was checked whether cracks were formed or not. As for the samples before the solution treatment, preliminary forging tests were conducted with the result that cracks were easily formed. This may be because the ⁇ -phase was thick so that the grain boundary sliding was hardly occurred. This tendency was enhanced as the aluminum content increased. Therefore, only for the samples after solution treatment, tests were conducted. The results are shown in Table 7. The tests were conducted with plate-like specimens of 20 mm ⁇ 20 mm ⁇ 1.5 mm thickness which were cut and taken from these samples. Each specimen was forged at a constant strain rate. The true strain for the forging was -1.1.
  • AZ91 through AZ71 created serious cracks during forging even when the processing temperature was raised to 350 °C.
  • 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 % corresponding to magnesium alloy of series AZ21, AZ31, AZ41, AZ51 and AZ61 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 figure and exhibit high reliability of properties and enough corrosion resistance, at sufficiently high yield ratio.
EP03002095A 2002-03-12 2003-01-30 Method of manufacturing magnesium alloy products Expired - Fee Related EP1347074B1 (en)

Applications Claiming Priority (2)

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JP2002067184 2002-03-12
JP2002067184A JP3861720B2 (ja) 2002-03-12 2002-03-12 マグネシウム合金の成形方法

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EP1347074B1 true EP1347074B1 (en) 2006-05-03

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US (1) US20030173005A1 (ko)
EP (1) EP1347074B1 (ko)
JP (1) JP3861720B2 (ko)
KR (1) KR20030074385A (ko)
CN (1) CN1283822C (ko)
DE (1) DE60304920T8 (ko)
TW (1) TWI263681B (ko)

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CN103447433A (zh) * 2013-09-04 2013-12-18 中南大学 一种大尺寸镁合金锻饼的制备方法
DE102016223089A1 (de) 2016-11-23 2018-05-24 Schaeffler Technologies AG & Co. KG Verfahren zur Herstellung einer Wälzlagerkomponente aus einer Nickel-Titan-Legierung

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Publication number Priority date Publication date Assignee Title
CN103447433A (zh) * 2013-09-04 2013-12-18 中南大学 一种大尺寸镁合金锻饼的制备方法
DE102016223089A1 (de) 2016-11-23 2018-05-24 Schaeffler Technologies AG & Co. KG Verfahren zur Herstellung einer Wälzlagerkomponente aus einer Nickel-Titan-Legierung

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JP2003268513A (ja) 2003-09-25
JP3861720B2 (ja) 2006-12-20
US20030173005A1 (en) 2003-09-18
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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