WO2008016150A1 - Alliage de magnésium et son procédé de fabrication - Google Patents

Alliage de magnésium et son procédé de fabrication Download PDF

Info

Publication number
WO2008016150A1
WO2008016150A1 PCT/JP2007/065298 JP2007065298W WO2008016150A1 WO 2008016150 A1 WO2008016150 A1 WO 2008016150A1 JP 2007065298 W JP2007065298 W JP 2007065298W WO 2008016150 A1 WO2008016150 A1 WO 2008016150A1
Authority
WO
WIPO (PCT)
Prior art keywords
magnesium
phase
magnesium alloy
alloy
average
Prior art date
Application number
PCT/JP2007/065298
Other languages
English (en)
Japanese (ja)
Inventor
Hidetoshi Somekawa
Alok Singh
Yoshiaki Osawa
Toshiji Mukai
Original Assignee
National Institute For Materials Science
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 National Institute For Materials Science filed Critical National Institute For Materials Science
Priority to JP2008527811A priority Critical patent/JP5429702B2/ja
Publication of WO2008016150A1 publication Critical patent/WO2008016150A1/fr

Links

Classifications

    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00—Extruding metal; Impact extrusion
    • B21C23/002—Extruding materials of special alloys so far as the composition of the alloy requires or permits special extruding methods of sequences

Definitions

  • the present invention relates to a new magnesium alloy having good strength and toughness and a method for producing the same.
  • Magnesium alloys are expected to be applied to various structural members because they are lightweight! And the improvement of the characteristic for practical use is also advanced. In particular, in order to put magnesium alloy into practical use as a mechanical structure material, it is a challenge to have high strength and toughness as well as the feature of being lightweight.
  • a powdered foil strip or the like is mainly used to produce a solidified molded body, and then a warm strain is produced. It is generally attempted to introduce processing.
  • the feature of this method is that the second-phase particles such as intermetallic compounds are uniformly and finely dispersed in the magnesium matrix simultaneously with the refinement of the crystal grain structure.
  • Patent Document 1 Japanese Patent Application Laid-Open No. 2006-2184
  • a powder solidified alloy of Mg — ;! ⁇ 8RE (RE: rare earth element) 1-6Ca is prepared, and then warm extrusion is performed. Force to be used When creating a powder solidified body, it is difficult to improve fracture toughness due to oxide incorporation at the interface between the parent phase and the parent phase.
  • Patent Document 2 Japanese Patent Application Laid-Open No.
  • 2004-149862 relates to a high-strength, high-toughness magnesium alloy using an Mg—Zn—RE alloy.
  • the molten metal added with a high concentration of different elements is used as a rapidly solidified powder and solidified and formed to uniformly disperse the precipitates with a high volume fraction, which depends on the dispersion strengthening of the intermetallic compound. Therefore, there is a problem that the fracture easily progresses at the interface between the high volume fraction dispersion and the matrix phase, and the toughness and the high ductility cannot be achieved.
  • rare earth metals are used, the price of the substrate becomes expensive, but it is difficult to expect significant improvements in properties and functions to meet such an increased burden.
  • Patent Document 3 Japanese Patent Laid-Open No. 5-70880
  • Patent Document 4 Japanese Patent Laid-Open No. 7-3375
  • Patent Document 5 Japanese Patent Laid-Open No. 5-306424 relates to a method for producing a high hardness / strength / toughness magnesium alloy using an Mg—RE alloy.
  • Patent Document 6 Japanese Unexamined Patent Application Publication No. 2003-277899 relates to a manufacturing method in which a pre-strain of 0.4 or less is applied to a forged magnesium alloy and then warm strain processing is performed.
  • pre-strain is applied before warm working to introduce uniform precipitation nucleation sites.
  • Patent Document 6 Although the method of Patent Document 6 is more practically rational in that it uses a forged magnesium alloy that is not a solidified molded body such as a powdery foil body, the method is practically practical. It is not always easy to control and reproduce. For this reason, there is a great difficulty in improving the strength-toughness due to the structure of fine particle dispersion in the magnesium matrix.
  • Non-Patent Document 1 (Materials Transactions, 47 (2006), 1066-1077), manufacturing a high toughness alloy using Mg-RE-Zn-Zr alloy Is disclosed.
  • the forged material is expanded by warm strain processing and then heated.
  • a treatment is applied to disperse precipitates such as second phase particles in the parent phase.
  • the applicant of the present invention also uses high-strength and good ductility as in the case of using the rare earth element of viewpoint 4), as in Patent Document 7 (Japanese Patent Laid-Open No. 2005-113235).
  • Patent Document 7 Japanese Patent Laid-Open No. 2005-113235.
  • This wrought magnesium alloy has a composition represented by the composition formula Mg Zn Y (where a and b are atomic%, and a / 12 ⁇ b ⁇ a / 3, 1.5 ⁇ a ⁇ 10). And a quasicrystal represented by the composition formula Mg Zn Y crystallizes at the grain boundary of the magnesium parent phase (a-Mg), and a quasicrystal having a particle diameter of 100 nm or less and its approximate crystal are the magnesium parent phase. It has a uniformly dispersed structure in the crystal grains! Quasicrystals and approximate crystals are stable without causing phase transformation at temperatures below 250 ° C, and the strength is remarkably increased by strong interaction with dislocations. Slip is suppressed, and these effects synergistically improve the high-temperature strength.
  • the above-mentioned magnesium alloy wrought material has strength and ductility during tensile deformation and high strength. It was developed with an emphasis on improving the temperature and other characteristics are not clear. Considering application to structural members for moving bodies such as vehicles, it is necessary to ensure safety and reliability against contact, collision, etc. For that purpose, it must have high compressive deformability and excellent fracture toughness performance. Is very important.
  • the magnesium alloy is subjected to strain processing such as rolling and extrusion due to the crystal structure peculiar to magnesium, so that the texture oriented in the bottom surface formed during strain processing remains in the material as it is.
  • strain processing such as rolling and extrusion due to the crystal structure peculiar to magnesium
  • commercially available wrought magnesium alloy materials so far show high tensile strength at room temperature, while compressive strength remains at about 50% to 80% of tensile strength. Therefore, when a general magnesium alloy wrought material is applied to a structural member for a moving body, it is difficult to maintain a shape with low strength at a location where compressive strain occurs.
  • the quasicrystals and approximate crystals may be the starting point of fracture, which may reduce fracture toughness.
  • the magnesium alloy wrought material is subjected to hot working of a magnesium alloy forged material at 230 ° C to 420 ° C with a working rate of 50% or more in order to form the above structure. Hold at 370 ° C to 420 ° C for 10 minutes to 10 hours, then cool to room temperature at a cooling rate of 20 ° C / sec or more, then 150 ° C to 250 ° C for 1 hour It is produced by applying a heat treatment consisting of a second stage of cooling to room temperature after holding for ⁇ 15 hours. Thus, it is undeniable that the process is complicated to perform the heat treatment consisting of two stages after the hot working. Simplification of the process is desired for practical technology!
  • the present invention solves the problems of the prior art from the background as described above,
  • the magnesium alloy of the present invention is characterized by the following in order to solve the above problems.
  • a magnesium alloy containing magnesium and zinc, or a non-rare earth element in the alloy composition wherein a second phase particle containing at least zinc is included in a magnesium matrix.
  • the biphasic particles are spherical and the average particle size is nano-sized.
  • Alloy composition is the following formula:
  • the ratio K between the average particle size of the second phase particles represented by the following formula and the average crystal particle size of the magnesium matrix is 0.005 or more and 0.2 or less.
  • K average particle diameter of second phase particles / magnesium parent phase
  • Zinc content is in the range of 1.6 ⁇ a ⁇ 3.5.
  • a magnesium alloy that contains magnesium and zinc, and further contains a non-rare earth element in the alloy composition, and the quasicrystalline particle phase is folded only in the magnesium matrix crystals, and the quasicrystalline particle phase is It is spherical and its average particle size is nano-sized.
  • the alloy composition is:
  • RE represents one or more of rare earth elements
  • y and x represent atomic%, 0.2 ⁇ x ⁇ l .5, 5 Indicates x ⁇ y ⁇ 7x.
  • the ratio K between the average particle size of the quasicrystalline particle phase represented by the following formula and the average crystal particle size of the magnesium parent phase is 0.01 or more and 0.2 or less.
  • K average particle diameter of quasicrystalline particle phase / magnesium matrix phase
  • the average grain size of the magnesium parent phase is 511 m or less, and the average grain size of the quasicrystalline grain phase is 0.2 m or less.
  • Tenth The magnesium alloy according to any one of the above, wherein the rare earth element is at least one of Y, Gd, Tb, Dy, Ho, and Er.
  • the present invention provides a method for producing a magnesium alloy according to the first to tenth inventions described above.
  • the present invention provides a method for producing a magnesium alloy in which the ninth or tenth quasicrystalline particle phase is precipitated, and a homogenization treatment is performed at 460 ° C or lower for 4 hours or longer after melting. It is also characterized by strain processing with a processing ratio of 8: 1 or more in the warm temperature range. The invention's effect
  • the second phase particles containing zinc are precipitated in the magnesium matrix without using rare earth elements as additive elements, and the second phase particles are spherical. It has a nano-sized average particle size! /, And the composition and the composition of the structure make it possible to significantly improve strength and toughness as an alloy based on completely different knowledge.
  • the precipitated particles of the second phase act as dispersion-strengthened particles, and it is possible to further increase the strength simply by improving the strength due to the refinement of the crystal grains of the magnesium matrix.
  • the spherical second-phase precipitated particles can fix more dislocation movements that occur during deformation, and can achieve high strength and high toughness.
  • the refinement of the crystal grains of the magnesium matrix can suppress the generation of deformation twins that are the starting points of fracture, and as a result, high ductility and high fracture toughness can also be obtained.
  • the magnesium alloys of the sixth to tenth inventions are used when a rare earth element is used.
  • the alloy is based on the composition and the structure of the structure that the quasicrystalline phase is precipitated only in the crystal grains of the magnesium matrix and is spherical and the average grain size is nano-sized. As a result, the strength and toughness can be remarkably improved.
  • a magnesium matrix with an average grain size of 5 m or less is represented by the composition formula Mg Zn RE.
  • the quasicrystalline particle phase with an average particle size of 0.2 ⁇ or less within the matrix crystal grains has a uniform interface with a consistent interface, and has a tensile strength at room temperature.
  • the room temperature compressive strength can be significantly increased.
  • non-bottom dislocations can be activated in the deformation process, and the generation of deformation twins that can be the starting point of fracture can be suppressed.
  • High ductility and high fracture toughness can be obtained.
  • the quasicrystalline particle phase has an interface that is consistent with the magnesium matrix phase, it is possible to maintain good deformation continuity, relax stress concentration at the interface, and achieve high ductility and high fracture toughness. It becomes possible. Therefore, the application of the magnesium alloy wrought material to the structural member for a moving body becomes more realistic.
  • the magnesium alloy of the present invention as described above is manufactured by a simple and practically reasonable method. That is, strain processing is introduced in the warm temperature range after homogenizing the forged magnesium alloy to refine the crystal grains of the magnesium matrix, and at the same time, fine precipitate particles of the second phase having a nano-sized spherical shape are formed. This can be achieved by uniformly dispersing in the magnesium matrix or by dispersing the quasicrystalline grain phase in the crystal grains of the magnesium matrix.
  • FIG. 1 is a TEM observation image of the spherical precipitated particle structure of ZK60 in Experiment No. 1.
  • FIG. 3 is a structure observation photograph of an extruded completion part of a Mg—Zn binary magnesium alloy.
  • FIG. 4 is a structure observation photograph of the part during extrusion deformation compared with FIG.
  • FIG. 7 This is a TEM microstructure observation photograph of ZK60 alloy extruded material extruded at 220 ° C in Experiment No. 12.
  • FIG. 9 is a transmission electron microscope (TEM) photograph showing the structure of a Mg-6at.% Zn-lat.% Ho alloy wrought material extruded at 230 ° C (503K).
  • FIG. 10 (a) and (b) are the structure of Mg— 2 ⁇ 7 at.% Zn 0.4 at.% Ho alloy wrought material extruded at 210 ° C (483K) and the quasicrystalline particle phase, respectively.
  • 2 is an enlarged transmission electron microscope (TEM) photograph.
  • (C) is a high-resolution TEM photograph showing the interface between the magnesium matrix and the quasicrystalline particle phase of the wrought alloy.
  • the magnesium alloy containing no rare earth element of the present invention is specified as a composition comprising magnesium and zinc, or magnesium and zinc, and further a non-rare earth element.
  • this magnesium alloy as described above, second-phase particles containing at least zinc are precipitated in the magnesium matrix, the second-phase particles are spherical, and the average particle system is nano-sized.
  • the second phase particles are considered as being in an intermetallic compound of an alloy constituent element, or in an alloy or mixed phase.
  • at least one elemental species constituting the second phase particle is zinc.
  • such second phase particles are “spherical”.
  • the aspect ratio force between the major axis and the minor axis of a crystal particle that is not only a true sphere is the major axis length: the minor axis length. Defined as being in the range of 10: 1 or less.
  • the average particle size force S “nanosize” is defined as being less than ⁇ , more specifically 500 nm or less.
  • Precipitated particles existing on the grain boundaries can be expected to increase in strength, which makes it difficult to maintain continuity of deformation, but it is difficult to achieve high toughness and high ductility as their presence increases. It is desirable that the number of precipitated particles existing on the grain boundary is as small as possible.
  • the aspect ratio is more preferably 5: 1 or less, and the nano-sized average particle diameter is preferably lOOnm or less.
  • the volume fraction related to the density of precipitation of the second phase particles is generally 10% or less as the maximum volume fraction, and the center-to-center spacing of the particles is generally in the range of 100 to 300 nm. It is preferably taken into account.
  • the magnesium matrix may be a solid solution of force or other alloying elements that are mainly composed of magnesium.
  • Such a magnesium matrix preferably has a fine crystal grain size. Normally, the average grain size is 15 m or less, and more preferably 5 ⁇ or less in view of alloy characteristics. Is done. An increase in tensile strength can be expected due to the refinement of crystal grains. In addition, non-bottom dislocations and grain boundary sliding can be performed in the deformation process, which leads to the suppression of the generation of deformation twins, which are the starting points of fracture, and dramatically improves tensile ductility.
  • the ratio between the average particle size of the second phase particles and the average particle size of the magnesium matrix is preferably in the range of 0.005 to 0.2 as a mean value in the above formula.
  • the alloy composition is represented by the following formula:
  • a non-rare earth atom other than zinc is added, it is selected from elements that can be dissolved in magnesium as a parent phase.
  • the range can be one or more of alkaline earth metals and transition metals.
  • examples of such non-rare earth elements include Zr, Ca, Sr, Ba, and Al.
  • the quasicrystalline phase is precipitated and dispersed only in the crystal grains of the magnesium matrix.
  • the quasicrystalline particle phase is spherical and the average particle size is nano-sized.
  • the definition of the magnesium matrix, “spherical”, and “nanosize” in the present invention is the same as in the case of the magnesium alloy of the non-rare earth element.
  • the “quasicrystalline particle phase” is a force S whose composition is already known as Mg Zn RE, the present invention.
  • an approximate stable phase may be included.
  • the quasicrystalline particle phase in the present invention exists substantially only in the crystal grains of the magnesium matrix, and does not exist in the grain boundary. This is the largest and extremely important feature of the present invention and is an essential component of the invention.
  • the magnesium alloy wrought material of the present invention containing a rare earth element has the composition formula Mg Zn RE (wherein RE is any one of Y, Gd, Tb, Dy, Ho, Er) Rare earth
  • X, y are atomic% each, and have a composition represented by 0.2 ⁇ x ⁇ l.5, 5x ⁇ y ⁇ 7x), and an average crystal grain size of 5 m or less In the composition formula Mg Zn RE
  • the magnesium alloy of the present invention in this case has a ternary alloy composition of Mg-Zn-RE, and RE includes rare earths including Y, Gd, Tb, Dy, Ho, and Er. Any one of the elements Is preferably selected.
  • the atom 0 / ox of RE is common to Y, Gd, Tb, Dy, Ho, and Er, and preferably 0 ⁇ 2 ⁇ ⁇ 1.5.
  • the RE atomic degree / is less than 0.2 atomic%, the crystallization of the quasicrystalline particle phase is so small that it is difficult to achieve high strength and high toughness. 1. If it exceeds 5 atomic%, the crystallization of the quasicrystalline particle phase becomes excessive, and the quasicrystalline particle phase becomes the starting point of fracture, and the ductility and fracture toughness tend to decrease.
  • the atomic% of ⁇ is determined based on the atomic degree / of RE, and preferably 5x ⁇ y ⁇ 7 ⁇ . ⁇ If the atomic% of ⁇ is less than 5 ⁇ , it is difficult to form a quasicrystalline particle phase composed of Mg Zn RE. If it exceeds 7 ⁇ , a large number of quasicrystalline particle phases and other intermetallic compounds (for example, MgZn) crystallize, and they become the starting point of the deformation process, which is easy to cause characteristic deterioration.
  • intermetallic compounds for example, MgZn
  • the structure of the magnesium alloy of the present invention has a composition represented by the composition formula Mg Zn RE in the magnesium matrix having an average crystal grain size of 5 m or less, and the average grain size is 0 in the matrix crystal grains.
  • ( ⁇ ) can be 80% or more of the tensile yield strength ( ⁇ ) ( ⁇ ⁇ 0.8 ⁇ ). Also
  • the activity of non-bottom dislocations becomes possible, and the generation of deformation twins, which are the starting points of fracture, can be suppressed.
  • high ductility and high fracture toughness can be obtained.
  • the quasicrystalline particle phase has an interface that is consistent with the magnesium matrix phase, the continuity of deformation can be maintained well, stress concentration at the interface is relaxed, and high ductility and toughness can be achieved. Become.
  • the quasicrystalline particle phase having an average particle diameter of 0.2 ⁇ m or less and uniformly dispersed in the magnesium matrix acts as a dispersion strengthened particle, and further enhances the strength of the magnesium alloy wrought material. .
  • the average particle diameter of the quasicrystalline particle phase exceeds 0.2 ⁇ m, the quasicrystalline particle phase is easily cracked during the deformation process and tends to be a starting point of fracture.
  • the ratio of the average particle size of the fine particle phase to the average crystal particle size of the magnesium mother phase ie, the straight K force determined by the above formula.
  • ⁇ average particle size of quasicrystalline particle phase / average crystal particle size of magnesium matrix phase 0
  • the force S can sufficiently suppress cracks in the deformation process.
  • volume ratio of the quasicrystalline particle phase and the center-to-center spacing can be considered in the same manner as in the case of the non-rare earth element alloy.
  • the quasicrystalline particle phase of the present invention has an interface consistent with the magnesium matrix phase.
  • the quasicrystalline particle phase of the present invention has an interface consistent with the magnesium matrix phase.
  • it is possible to maintain good deformation continuity, and to relieve stress concentration on the interface. This contributes to high ductility and high fracture toughness.
  • a high plane strain fracture toughness value of 25 MPa 'm 172 or higher is obtained. If the interface between the quasicrystalline particle phase and the magnesium matrix phase is inconsistent, deformation is easily cut off at the interface between the magnesium matrix phase and the quasicrystalline phase, and continuity cannot be maintained. Stress concentration occurs and becomes the starting point of fracture. Ductility and fracture toughness are reduced.
  • the magnesium alloy of the present invention in both the non-rare earth system and the rare earth system, the magnesium alloy having the above composition is dissolved and solidified. After homogenization, it is manufactured by straining in the warm temperature range.
  • a homogenization treatment for the base material after melting (forging) is essential for the method of the present invention.
  • the purpose of this homogenization treatment is to prevent the solidified structure after melting (forging) from remaining in the subsequent warm strain processing, and to form second-phase particles or quasicrystalline particle phases.
  • This homogenization treatment is performed by heating the base material, and the heating temperature at this time is usually lower than the recrystallization temperature of the base material, and the second phase particles or quasicrystalline particles are not heated.
  • the heating temperature and the heating time for the homogenization treatment are the force S that can be determined in consideration of the alloy composition, and the predetermined structure and characteristic level, and a general guideline is 200 ° C to 500 ° C. In the temperature range of ° C, it ranges from 2 to 50 hours.
  • the second-phase particles and the quasicrystalline particle phase are mixed with spherical or nano-sized particles that are needle-like or plate-like particles. Is difficult to achieve.
  • strain processing in the warm temperature region after the homogenization treatment is indispensable.
  • the crystal grain size of the magnesium matrix is within the required range, and strain processing is performed to make the second phase particles with a sphere-like average particle size of sphere size or the quasicrystalline particle phase into the required range.
  • strain processing it is desirable to perform strain processing after holding (heat treatment) for a required time at a temperature equivalent to the processing temperature in advance.
  • the holding time here is considered as the time required for the processing temperature to reach the entire base material.
  • the force that varies depending on the composition and size of the base material is generally 10 minutes to 2 hours.
  • the degree of processing at the time of strain processing is considered as a range for obtaining a predetermined alloy structure. Generally, it is 5: 1 or more. For example, 5:;! ⁇ 30: 1 is considered as a guide.
  • a billet for strain processing is formed by machining.
  • a rare earth element-containing alloy more preferably, after melting, homogenization treatment is performed under conditions of 460 ° C or less and 4 hours or more, and after strain processing, magnesium is applied. Hold the time required for the entire base metal to reach the temperature at a temperature at which the size of the parent matrix reaches 5 m or less, and then perform strain processing at a processing ratio of 8: 1 or more above the warm temperature.
  • Production of the base material is not particularly limited.
  • the base material is first subjected to a homogenization treatment under conditions of 460 ° C or lower and 4 hours or longer.
  • a homogenization treatment By this homogenization treatment, a dendrite structure formed at the time of fabrication is reduced! /, A magnesium phase and a quasicrystalline particle phase are formed.
  • the temperature exceeds 460 ° C, the quasicrystalline particle phase dissolves in the magnesium matrix and the desired effect cannot be obtained. If it is less than 4 hours, the homogenization process is insufficient and a forged structure remains.
  • quenching After the homogenization treatment, quenching can be performed.
  • the ability to freeze the tissue once by quenching can stabilize the tissue.
  • the heat treatment temperature is equivalent to the temperature during strain application. If the heat treatment temperature is higher than the strain processing temperature, a fine magnesium matrix with an average crystal grain size of 5 in or less will not be formed. If the heat treatment temperature is lower than the strain processing temperature, cracks will occur during heating, and a healthy extruded material will be Can't get. Even when heat treatment is not performed, cracks and the like occur during strain processing, and a sound extruded material cannot be obtained.
  • the heat treatment time can be set as a rough guide for 15 minutes to 90 minutes.
  • a strain processing of 8: 1 or more is performed at a temperature equal to or higher than the same temperature as the heat treatment.
  • Hi Scumming can be performed by rolling, extruding, forging, or the like. Due to the applied strain, recrystallization occurs and a fine magnesium matrix with an average grain size of 5 m or less is formed, and dislocations are introduced, and the average grain size is 0.2 to 111 or less within the parent phase crystal grains.
  • the quasicrystalline particle phase is formed, and the quasicrystalline particle phase has a consistent interface and is uniformly dispersed in the magnesium matrix.
  • the processing ratio is less than 8: 1, the applied strain is insufficient, a fine magnesium matrix with an average grain size of 5 m or less is not formed, and the quasicrystal with a low density of dislocations to be introduced. A uniform dispersion of the particle phase cannot be obtained.
  • the method for producing a magnesium alloy wrought material according to the present invention includes a simplified process suitable for a practical application technique of homogenization, heat treatment, and strain processing in a warm temperature range. .
  • a magnesium alloy wrought material having high strength and high ductility, as well as high compressive strength and high fracture toughness can be easily produced.
  • the average diameter of the crystal grains and particles of the alloy structure was determined using a commercially available image software (PhotoShop: registered trademark), with a strong contrast! It is regarded as particles, and the average value is obtained by measuring more than 250 crystal grains and particles.
  • the tensile 'compressive strength is obtained from a stress-strain curve. Specifically, the stress value with a strain of 0.2% is measured.
  • ZK60 was kept in a furnace at 500 ° C for 2 hours and homogenized. After removal from the furnace The tissue was frozen by water quenching.
  • an extruded billet was prepared by machining. Next, the billet was heated to 380 ° C. and held for about 0.5 hour, and extrusion was performed at an extrusion ratio of 18: 1 to obtain an extruded material.
  • the average crystal grain size of the magnesium matrix is about 13.5 m, and the second phase has an average particle size of 35-50 nm. It was confirmed to show a structure of spherical precipitated particles.
  • Table 1 shows the measurement results of elongation at break, yield strength, and plane strain fracture toughness for each of the above samples.
  • the plane strain fracture toughness values were obtained from the fracture zone analysis of the fracture toughness specimens collected from each sample. That is, three-point bending fracture toughness specimens having a shape of 5 x 10 x 40 mm in accordance with ASTE-E399 were collected from each extruded material, and plane strain fracture toughness values were obtained by stretch zone fracture surface analysis. .
  • This mother alloy was held in a furnace at 300 ° C or higher for 48 hours, and homogenized. After removal from the furnace, the tissue was frozen by water quenching. Thereafter, an extruded billet was prepared by machining.
  • the billet was heated to about 210 ° C, held for about 0.5 hours, and extruded at an extrusion ratio of about 20: 1 to obtain an extruded material.
  • the average crystal grain size (d) of the magnesium matrix (the dark-contrast part in the figure) is about 1 ⁇ m, and the average grain size of the magnesium matrix is about 0.1 m.
  • the formation of spherical precipitates (indicated by arrows) can be confirmed.
  • spherical precipitate particles are formed by introducing strain processing such as extrusion into the forged magnesium alloy.
  • the master alloy was kept in a furnace at various temperatures (300 ° C, 400 ° C) for 24 48 hours and homogenized. After removal from the furnace, the tissue is frozen by water quenching.
  • an extruded billet was prepared by machining.
  • the billet was heated to various temperatures (200 230 ° C.) and held for about 0.5 hours, and extrusion was performed at an extrusion ratio of 18: 1 to obtain an extruded material.
  • Extrusion was performed at an extrusion ratio of 1 to obtain an extruded material.
  • the average crystal grain size of the parent phase was about 0. ⁇ .
  • Tensile specimens and fracture toughness specimens were sampled from the extruded materials and tested.
  • Fig. 8 shows this magnesium alloy, a general commercial magnesium alloy (Cast Mg, wrough Mg), and an anoremium alloy (J. R. Davis, Aluminum and
  • the magnesium alloy of the present invention has the same strength-toughness characteristics as commercial high-strength aluminum alloys.
  • a master alloy was prepared by dissolving and forging 1.8 atomic% zinc and 0.3 atomic% calcium in commercial pure magnesium (purity 99. 95%).
  • the master alloy was stored in a furnace at 500 ° C. for 2 hours and homogenized. After removal from the furnace, the tissue was frozen by water quenching. Then, the extrusion billet was created by machining. The billet was heated to about 250 ° C., held for about 0.5 hour, and extruded at an extrusion ratio of about 18: 1 to obtain an extruded material.
  • the plane strain fracture toughness value was found to be 28. lMPam 1/2, and high strength was achieved by introducing strain processing to the magnesium alloy forged material in the warm temperature range.
  • Tensile test pieces having a parallel part ⁇ 3 ⁇ 15 mm and compression test pieces having ⁇ 4 ⁇ 8 mm were collected from the extruded material, and subjected to a tensile test and a compression test at room temperature.
  • the tensile test was performed at a strain rate of 10- ⁇ - 1 using a universal testing machine.
  • a universal testing machine was used, and the strain rate was IX lO ⁇ s 1 in the same way.
  • Table 2 shows the results of the tensile test and the compression test. Table 2 also shows the extrusion temperature, the average grain size of the magnesium matrix and the average grain size of the quasicrystalline grain phase.
  • the average crystal grain size of the magnesium matrix is about 3 ⁇ , The average particle size is 0.2 111, which is slightly larger than the sample extruded at 230 ° (5031 (Experiment No. 14).
  • the tensile strength is 265 MPa and the fracture An elongation of 13% and a compressive strength of 248 MPa were confirmed, indicating that it is a wrought magnesium alloy with high strength, high ductility, and high compressive strength, while 230 ° C (503K) (Experiment No. 14 ),
  • the ratio of compressive strength / tensile strength is 0.94, and it can be seen that the compressive strength decreases slightly as the heat treatment temperature and extrusion temperature increase.
  • FIG. 11 shows an image of the fracture surface after the fracture toughness test observed using a scanning electron microscope (SEM).
  • SEM scanning electron microscope
  • the plane strain fracture toughness value was obtained by stretch zone analysis using the fracture surface after fracture toughness.
  • the plane strain fracture toughness value was 32. IMPa 'm 172 , confirming high toughness.
  • the structure was observed using a transmission electron microscope (TEM). It was confirmed that a structure in which quasicrystals with an average particle size of 0.1 am were uniformly dispersed was formed in a magnesium matrix having an average crystal size of about 1111 m.
  • the K value was 0.1.
  • Table 2 shows the results of the tensile test and the compression test.
  • the fracture toughness value was determined. A three-point bending specimen was also taken from the extruded material and a fracture toughness test was conducted. The plane strain fracture toughness value was found to be 32.5 MPa 'm 1/2 , confirming high toughness.
  • Mg—Zn—Dy (Experiment No. 20)
  • Mg—Zn—Gd (Experiment No. 21)
  • Mg— Extruded materials of Zn—Tb (Experiment No. 22)
  • Mg—Zn—Er (Experiment No. 23) were obtained.
  • Table 2 shows the microstructure, observation results, and measurement results of elongation at break, yield strength, and plane strain fracture toughness.

Abstract

L'invention concerne un nouveau matériau expansé en alliage de magnésium, présentant une structure selon laquelle des particules d'une seconde phase, contenant des phases de particules de zinc ou de quasicristal, ayant respectivement une forme sphérique nanométrique avec un diamètre moyen de particule inférieur ou égal à 500 nm, sont déposées dans une matrice de magnésium. Le matériau expansé en alliage de magnésium présente une grande résistance, une grande ductilité, une grande résistance à la compression et une grande ténacité à la rupture.
PCT/JP2007/065298 2006-08-03 2007-08-03 Alliage de magnésium et son procédé de fabrication WO2008016150A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2008527811A JP5429702B2 (ja) 2006-08-03 2007-08-03 マグネシウム合金とその製造方法

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
JP2006211523 2006-08-03
JP2006-211523 2006-08-03
JP2006247824 2006-09-13
JP2006-247824 2006-09-13

Publications (1)

Publication Number Publication Date
WO2008016150A1 true WO2008016150A1 (fr) 2008-02-07

Family

ID=38997322

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2007/065298 WO2008016150A1 (fr) 2006-08-03 2007-08-03 Alliage de magnésium et son procédé de fabrication

Country Status (2)

Country Link
JP (2) JP5429702B2 (fr)
WO (1) WO2008016150A1 (fr)

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008106337A (ja) * 2006-10-27 2008-05-08 Shingijutsu Kenkyusho:Kk マグネシウム合金の圧延材およびその製造方法
JP2010215962A (ja) * 2009-03-17 2010-09-30 National Institute For Materials Science Ｍｇ合金鍛造品とその製造方法
WO2010110272A1 (fr) 2009-03-24 2010-09-30 独立行政法人物質・材料研究機構 ELÉMENT EN ALLIAGE DE MAGNÉSIUM (Mg)
JP2012122102A (ja) * 2010-12-08 2012-06-28 National Institute Of Advanced Industrial Science & Technology 常温成形性と強度を改善したマグネシウム合金板材及びその作製方法
JP2015526591A (ja) * 2012-06-26 2015-09-10 バイオトロニック アクチェンゲゼルシャフト マグネシウム合金、その製造方法およびその使用
JP2015224388A (ja) * 2014-05-30 2015-12-14 不二ライトメタル株式会社 長周期積層構造マグネシウム合金および製造方法
JP2016509875A (ja) * 2013-02-15 2016-04-04 ボストン サイエンティフィック サイムド，インコーポレイテッドＢｏｓｔｏｎ Ｓｃｉｅｎｔｉｆｉｃ Ｓｃｉｍｅｄ，Ｉｎｃ． 内部人工器官用の生体内分解性マグネシウム合金微細構造
WO2018083998A1 (fr) * 2016-11-02 2018-05-11 国立大学法人 熊本大学 Dispositif médical biorésorbable et son procédé de production
US10344365B2 (en) 2012-06-26 2019-07-09 Biotronik Ag Magnesium-zinc-calcium alloy and method for producing implants containing the same
JP2019189941A (ja) * 2018-04-23 2019-10-31 キヤノン株式会社 マグネシウム−リチウム系合金
WO2019208287A1 (fr) * 2018-04-23 2019-10-31 キヤノン株式会社 Alliage à base de magnésium-lithium
JP2019218577A (ja) * 2018-06-15 2019-12-26 株式会社戸畑製作所 マグネシウム合金
US10518001B2 (en) 2013-10-29 2019-12-31 Boston Scientific Scimed, Inc. Bioerodible magnesium alloy microstructures for endoprostheses
US10589005B2 (en) 2015-03-11 2020-03-17 Boston Scientific Scimed, Inc. Bioerodible magnesium alloy microstructures for endoprostheses
US10895000B2 (en) 2012-06-26 2021-01-19 Biotronik Ag Magnesium alloy, method for the production thereof and use thereof
US10995398B2 (en) 2012-06-26 2021-05-04 Biotronik Ag Corrosion resistant stent
WO2021111989A1 (fr) * 2019-12-03 2021-06-10 国立研究開発法人物質・材料研究機構 Matériau de traitement de vieillissement d'alliage de magnésium, procédé pour le produire, dispositif oa l'utilisant, dispositif de transport et composant associé

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104593652B (zh) 2015-02-06 2016-08-24 中北大学 准晶及氧化铝混合颗粒增强镁基复合材料及其制造方法
JP6587174B2 (ja) * 2015-04-28 2019-10-09 国立研究開発法人物質・材料研究機構 高靱性マグネシウム基合金伸展材及びその製造方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0748647A (ja) * 1993-08-04 1995-02-21 Ykk Kk 高力マグネシウム基合金材およびその製造方法
JP2000271693A (ja) * 1999-03-26 2000-10-03 Ykk Corp マグネシウム合金材の製造方法
JP2000271695A (ja) * 1999-03-26 2000-10-03 Ykk Corp 成形品の製造方法
JP2002309332A (ja) * 2001-04-11 2002-10-23 Yonsei Univ 熱間成形性の優れた準結晶相強化マグネシウム系合金
JP2005029871A (ja) * 2003-07-11 2005-02-03 Matsushita Electric Ind Co Ltd マグネシウム合金板材およびその製造法
JP2005113235A (ja) * 2003-10-09 2005-04-28 Toyota Motor Corp 高強度マグネシウム合金およびその製造方法

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004099941A (ja) * 2002-09-05 2004-04-02 Japan Science & Technology Corp マグネシウム基合金及びその製造方法
JP2004099940A (ja) * 2002-09-05 2004-04-02 Japan Science & Technology Corp マグネシウム基合金の製造方法
WO2004085689A1 (fr) * 2003-03-25 2004-10-07 Yoshihito Kawamura Alliage de magnesium de haute resistance et tenacite, et son procede de production
JP2006089772A (ja) * 2004-09-21 2006-04-06 Toyota Motor Corp マグネシウム合金
CN101027420B (zh) * 2004-09-30 2011-08-10 河村能人 高强度高韧性金属及其制造方法
JP4828206B2 (ja) * 2005-10-26 2011-11-30 株式会社神戸製鋼所 高強度マグネシウム合金押出し材
EP1959025B1 (fr) * 2005-11-16 2012-03-21 National Institute for Materials Science Materiau metallique biodegradable a base de magnesium

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0748647A (ja) * 1993-08-04 1995-02-21 Ykk Kk 高力マグネシウム基合金材およびその製造方法
JP2000271693A (ja) * 1999-03-26 2000-10-03 Ykk Corp マグネシウム合金材の製造方法
JP2000271695A (ja) * 1999-03-26 2000-10-03 Ykk Corp 成形品の製造方法
JP2002309332A (ja) * 2001-04-11 2002-10-23 Yonsei Univ 熱間成形性の優れた準結晶相強化マグネシウム系合金
JP2005029871A (ja) * 2003-07-11 2005-02-03 Matsushita Electric Ind Co Ltd マグネシウム合金板材およびその製造法
JP2005113235A (ja) * 2003-10-09 2005-04-28 Toyota Motor Corp 高強度マグネシウム合金およびその製造方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SINGH A. ET AL.: "Quasicrystal strengthened Mg-Zn-Y alloys by extrusion", SCRIPTA MATERIALIA, vol. 49, no. 5, September 2003 (2003-09-01), pages 417 - 422, XP004431948 *

Cited By (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008106337A (ja) * 2006-10-27 2008-05-08 Shingijutsu Kenkyusho:Kk マグネシウム合金の圧延材およびその製造方法
JP2010215962A (ja) * 2009-03-17 2010-09-30 National Institute For Materials Science Ｍｇ合金鍛造品とその製造方法
US8728254B2 (en) 2009-03-24 2014-05-20 National Institute For Materials Science Mg alloy
WO2010110272A1 (fr) 2009-03-24 2010-09-30 独立行政法人物質・材料研究機構 ELÉMENT EN ALLIAGE DE MAGNÉSIUM (Mg)
JP2010222645A (ja) * 2009-03-24 2010-10-07 National Institute For Materials Science Ｍｇ合金部材。
JP2012122102A (ja) * 2010-12-08 2012-06-28 National Institute Of Advanced Industrial Science & Technology 常温成形性と強度を改善したマグネシウム合金板材及びその作製方法
JP2015526591A (ja) * 2012-06-26 2015-09-10 バイオトロニック アクチェンゲゼルシャフト マグネシウム合金、その製造方法およびその使用
US11499214B2 (en) 2012-06-26 2022-11-15 Biotronik Ag Magnesium-zinc-calcium alloy and method for producing implants containing the same
US10344365B2 (en) 2012-06-26 2019-07-09 Biotronik Ag Magnesium-zinc-calcium alloy and method for producing implants containing the same
US10358709B2 (en) 2012-06-26 2019-07-23 Biotronik Ag Magnesium-zinc-calcium alloy, method for production thereof, and use thereof
US10995398B2 (en) 2012-06-26 2021-05-04 Biotronik Ag Corrosion resistant stent
US10895000B2 (en) 2012-06-26 2021-01-19 Biotronik Ag Magnesium alloy, method for the production thereof and use thereof
JP2016509875A (ja) * 2013-02-15 2016-04-04 ボストン サイエンティフィック サイムド，インコーポレイテッドＢｏｓｔｏｎ Ｓｃｉｅｎｔｉｆｉｃ Ｓｃｉｍｅｄ，Ｉｎｃ． 内部人工器官用の生体内分解性マグネシウム合金微細構造
US10518001B2 (en) 2013-10-29 2019-12-31 Boston Scientific Scimed, Inc. Bioerodible magnesium alloy microstructures for endoprostheses
JP2015224388A (ja) * 2014-05-30 2015-12-14 不二ライトメタル株式会社 長周期積層構造マグネシウム合金および製造方法
US10589005B2 (en) 2015-03-11 2020-03-17 Boston Scientific Scimed, Inc. Bioerodible magnesium alloy microstructures for endoprostheses
JPWO2018083998A1 (ja) * 2016-11-02 2019-09-26 国立大学法人 熊本大学 生体吸収性医療機器及びその製造方法
JP7107476B2 (ja) 2016-11-02 2022-07-27 国立大学法人 熊本大学 生体吸収性医療機器及びその製造方法
WO2018083998A1 (fr) * 2016-11-02 2018-05-11 国立大学法人 熊本大学 Dispositif médical biorésorbable et son procédé de production
CN112105753A (zh) * 2018-04-23 2020-12-18 佳能株式会社 镁-锂系合金
WO2019208287A1 (fr) * 2018-04-23 2019-10-31 キヤノン株式会社 Alliage à base de magnésium-lithium
JP2019189941A (ja) * 2018-04-23 2019-10-31 キヤノン株式会社 マグネシウム−リチウム系合金
JP7362267B2 (ja) 2018-04-23 2023-10-17 キヤノン株式会社 マグネシウム－リチウム系合金、光学機器、撮像装置、電子機器、及び移動体
US11840749B2 (en) 2018-04-23 2023-12-12 Canon Kabushiki Kaisha Magnesium-lithium-based alloy
JP2019218577A (ja) * 2018-06-15 2019-12-26 株式会社戸畑製作所 マグネシウム合金
WO2021111989A1 (fr) * 2019-12-03 2021-06-10 国立研究開発法人物質・材料研究機構 Matériau de traitement de vieillissement d'alliage de magnésium, procédé pour le produire, dispositif oa l'utilisant, dispositif de transport et composant associé

Also Published As

Publication number Publication date
JPWO2008016150A1 (ja) 2009-12-24
JP2014040672A (ja) 2014-03-06
JP5804431B2 (ja) 2015-11-04
JP5429702B2 (ja) 2014-02-26

Similar Documents

Publication Publication Date Title
WO2008016150A1 (fr) Alliage de magnésium et son procédé de fabrication
KR100815929B1 (ko) 고강도·고연성 마그네슘 합금 및 그 제조방법
Homma et al. Fabrication of extraordinary high-strength magnesium alloy by hot extrusion
Xu et al. Extruded Mg–Zn–Ca–Mn alloys with low yield anisotropy
CN105154734B (zh) 一种可高速挤压的变形镁合金及其制备方法
JP4415098B2 (ja) 難燃性マグネシウム合金押出材の製造方法及びその押出材
Wang et al. Microstructure evolution and mechanical properties of Mg-Gd-Y-Ag-Zr alloy fabricated by multidirectional forging and ageing treatment
KR100994812B1 (ko) 고강도 고연성 마그네슘 합금 압출재 및 그 제조방법
JPWO2005052204A1 (ja) 高強度高靭性マグネシウム合金及びその製造方法
EP2646585B1 (fr) Alliage d'aluminium résistant à la chaleur et à haute résistance et procédé de production de ce dernier
WO2006036033A1 (fr) Métal de grande dureté et de résistance élevée and procédé de fabrication dudit métal
JP5586027B2 (ja) Ｍｇ基合金
WO2013115490A1 (fr) Alliage de magnésium d'une grande ductilité et d'une grande ténacité et son procédé de préparation
JPH07179974A (ja) アルミニウム合金およびその製造方法
JP2006016658A5 (fr)
JP6860235B2 (ja) マグネシウム基合金展伸材及びその製造方法
WO2008117890A1 (fr) Alliages de magnesium et procede de production associe
JPWO2011114931A1 (ja) マグネシウム合金
JP2005113235A (ja) 高強度マグネシウム合金およびその製造方法
JP2024020484A (ja) マグネシウム合金時効処理材とその製造方法
Zhang et al. Achieving exceptional improvement of yield strength in Mg–Zn–Ca alloy wire by nanoparticles induced by extreme plastic deformation
Li et al. Tension-compression asymmetry in hot-rolled Mg-3wt% Gd alloy under creep loading
KR101700419B1 (ko) 저온 및 저속의 압출공정을 이용한 고강도 마그네슘 합금 압출재 제조방법 및 이에 의해 제조된 마그네슘 합금 압출재
JP5403508B2 (ja) Ｍｇ合金部材。
JP5376488B2 (ja) マグネシウム合金の温間加工方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 07791971

Country of ref document: EP

Kind code of ref document: A1

DPE1 Request for preliminary examination filed after expiration of 19th month from priority date (pct application filed from 20040101)
WWE Wipo information: entry into national phase

Ref document number: 2008527811

Country of ref document: JP

NENP Non-entry into the national phase

Ref country code: DE

NENP Non-entry into the national phase

Ref country code: RU

122 Ep: pct application non-entry in european phase

Ref document number: 07791971

Country of ref document: EP

Kind code of ref document: A1

DPE1 Request for preliminary examination filed after expiration of 19th month from priority date (pct application filed from 20040101)