WO2004106577A1 - Method for producing high strength ultra plastic material - Google Patents

Method for producing high strength ultra plastic material Download PDF

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Publication number
WO2004106577A1
WO2004106577A1 PCT/JP2004/007370 JP2004007370W WO2004106577A1 WO 2004106577 A1 WO2004106577 A1 WO 2004106577A1 JP 2004007370 W JP2004007370 W JP 2004007370W WO 2004106577 A1 WO2004106577 A1 WO 2004106577A1
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Prior art keywords
metal material
alloy
temperature
strength
ultrasonic
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PCT/JP2004/007370
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French (fr)
Japanese (ja)
Inventor
Kazutomi Yamamoto
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Furukawa Co., Ltd.
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Application filed by Furukawa Co., Ltd. filed Critical Furukawa Co., Ltd.
Priority to DE112004000826T priority Critical patent/DE112004000826T5/en
Priority to JP2005506503A priority patent/JPWO2004106577A1/en
Priority to AU2004243728A priority patent/AU2004243728A1/en
Priority to GB0521161A priority patent/GB2414952B/en
Priority to US10/553,882 priority patent/US20060231174A1/en
Publication of WO2004106577A1 publication Critical patent/WO2004106577A1/en

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F3/00—Changing the physical structure of non-ferrous metals or alloys by special physical methods, e.g. treatment with neutrons

Definitions

  • the present invention relates to the refinement of crystal grains of a metal material using ultrasonic waves, and relates to a method for producing a metal material having high-strength superplastic characteristics.
  • the general definition of superplasticity is a phenomenon in which the tensile stress of a polycrystalline material shows a high strain dependence of the deformation stress and a huge elongation of several hundred percent or more without local shrinkage.
  • a material with equiaxed small crystal grains of 10 ⁇ or less deformed at a temperature of 1/2 or more of the melting point expressed in absolute temperature and a strain rate of ⁇ -4 / s. At times, it is said that a large deformation is developed with a low deformation stress of lOMPa or less.
  • Grain refining methods for iron and steel materials and non-ferrous metal materials include a method of adding an element that suppresses the growth of crystal grains, a method of utilizing transformation, precipitation, and recrystallization due to thermomechanical treatment, and a method of strong shearing. (See, for example, JP-A-2003-041331, JP-A-2002-194472, JP-A-2002-105568, and JP-A-2000-271693).
  • Magnesium which has a structure, has a drawback that high-quality parts and casings cannot be produced unless molded by die casting or thixomolding, which is difficult for secondary calories due to low stretchability at room temperature. This limitation of the manufacturing method is also a reason for narrowing the applications of magnesium alloys.
  • Extrusion and roll-rolling are common methods for metal materials.
  • the ECAP method (Equal Channel Angular Pressing method) has recently been studied.
  • Extrusion is a method in which a billet or slab is literally extruded from a die having a hole of a predetermined shape, and a direct method of extruding through an orifice of the die is generally used.
  • pure magnesium extrudes billets or slabs at a temperature of 350-400 ° C and extrudes it.
  • ⁇ Compared to aluminum, it is difficult to balance the billet temperature and extrusion speed.
  • Roll rolling is a method in which a metal material is fed in one direction while being pressed by upper and lower rolls.
  • the repetitive joining rolling is a method in which a rolled plate is halved in a length direction, subjected to a surface treatment such as degreasing, and then two plates are overlapped and rolled again.
  • This method has the characteristic that it can be strongly sheared without changing the plate thickness, but it has a high manufacturing cost and disadvantages.
  • Cryogenic rolling is a method of rolling at a temperature of liquid nitrogen that does not recover as much as possible the strain introduced by rolling, and then rapidly heating to form fine recrystallized grains. No fruit has been obtained.
  • Different peripheral speed rolling is a method of applying a strong shearing force to the material by changing the peripheral speed of the upper and lower rolls.However, since the rolling is performed without lubrication, the surface condition that is easily subjected to uneven shearing force is roughened. is there.
  • Melt rolling is a method of rapidly cooling, for example, by pouring a molten metal in which an additive element is supersaturated into a water-cooled roll, and has the effect of suppressing the grain growth while promoting the generation of recrystallization nuclei.
  • metal materials that are easily oxidized are not suitable for mass production because sufficient atmosphere adjustment is required.
  • Warm rolling is a method of rolling at a temperature equivalent to the middle point between hot rolling at a temperature higher than the recrystallization temperature and cold rolling at normal temperature.
  • an appropriate amount of Zr is added to an A1-Zn-Mg_Cu alloy The effect of some of the alloys has been confirmed, such as obtaining a fine grain structure.
  • the ECAP method is a method in which a billet or slab is put into a die having a hole with a certain angle, and a high shear force is applied to the billet or slab by pressing and extruding to obtain a fine grain structure.
  • a high shear force is applied to the billet or slab by pressing and extruding to obtain a fine grain structure.
  • billets or slabs that have been subjected to strong shearing force are very tough, so secondary processing such as rolling is difficult to improve workability.
  • hot rolling is performed, crystal grains grow and do not satisfy sufficient strength, toughness and high ductility at practical levels.
  • Either method is a method in which a billet or the like that has been melted is subjected to a strong shearing process, and a very large stress is required for the shearing process, or the initial shape of the metal material cannot be maintained. Disclosure of the invention
  • the present invention solves the above-mentioned problems of the prior art, and has a high strength in which the structure of the metal material is fine crystal grain force. It is intended to provide a method for producing a material.
  • the metal material is heated at a temperature obtained by multiplying its melting point expressed in absolute temperature by 0.35 to 0.6. The above problem is solved by processing.
  • the metal material is attenuated when vibration is applied, and finally the vibration stops.
  • the other is internal friction, a mechanism by which vibration energy is converted into heat or strain inside a metal material. Internal friction is also called damping capacity.
  • the damping ability is classified into the following four types depending on the difference in vibration energy conversion mechanism. (1) By viscous or plastic flow at the interface between the parent phase and the second phase.
  • the dislocation is caused by the detachment from the fixing point by the impurity atom.
  • the force is consumed as heat in any of the conversion mechanisms in the category of 4), or accumulated as strain. Since a large strain equal to or greater than mechanical shearing is introduced into the metal material in which the strain is accumulated, the metal material has a melting point expressed in absolute temperature of 0.35 to 0.35. When heat treatment is carried out at a temperature multiplied by 1.6, it is considered that the lattice defects change to a recrystallized structure consisting of equiaxed fine crystal grains in the process of energy release due to rearrangement or mutual annihilation.
  • a metal material having a large damping capacity generally means a specific damping capacity (specific damping capacity).
  • SDC is 10% or more, and is collectively referred to as high attenuation metal materials.
  • pure gold Mg, Ni, and Fe have a large specific damping capacity, and alloys such as Mg alloy, Mn-Cu alloy, Mn-Cu-A1 alloy, Cu-Zn-A1 alloy, Cu-Al_Ni alloy, Fe_Cr alloy (12Cr steel ), Fe_Cr-A1 alloy, Fe_Cr-Mo alloy, Co_Ni alloy, Fe_Cr-Al_Mn alloy, Ni-Ti alloy, Cu_Zn_Al alloy, Al_Zn alloy, intergranular corrosion treatment 18-8 stainless steel, Fe_C_Si alloy (flake graphite-iron) Or, spheroidal graphite (iron rolled iron) has a large specific damping capacity and is called a high damping alloy, a vibration damping alloy or a vibration damping alloy.
  • the intrinsic damping capacity is represented by a vibration energy loss rate per cycle of a vibrating object as follows.
  • W is the vibrational energy and is the energy lost in one cycle.
  • Mg or Mg alloy force is most suitable for applying this method.
  • Mg has the largest damping ability among all metallic materials and has a specific damping ability of 60% or more.Therefore, it is easy to accumulate vibration energy as strain, and heat treatment at an appropriate temperature makes it possible to regenerate fine crystal grains. It is possible to have a crystal structure. Mg is relatively low in strength and corrosion resistance.This problem has been solved.A Mg alloy added with Al, Zn, Zr, etc., has a lower damping capacity than Mg, but some of the ultrasonic vibration energy is lost. It accumulates as strain and becomes a recrystallized structure composed of fine crystal grains by the heat treatment due to the synergistic effect with the effect of the added element, and it is possible to achieve both higher strength and superplasticity.
  • Mg alloy includes Mg-A1 alloy, Mg-A1-Zn alloy, Mg-Zr alloy, Mg-Zn-Zr alloy, Mg_Mg2 Ni alloy, Mg— RE— Zn alloy (RE is rare earth), Mg— Ag-RE alloys (RE is rare earth), Mg_Y_RE alloys (RE is rare earth), etc. are known as practical alloys.
  • Mg-A1 alloy and Mg-A1-Zn Among alloys, Mg_10% Al alloy (A1100), Mg_9% Al_l% Zn alloy (AZ91), Mg_6% ⁇ 1_3. / 0
  • the specific damping capacity of ⁇ alloy (AZ63) is 10. less than / o.
  • the ultrasonic vibration energy applied to Mg or the Mg alloy is, as described in the above-mentioned vibration energy conversion mechanism (3), the dislocation is detached from the anchoring point by the impurity atom. It is believed that it is consumed or consumed to form deformation twins.
  • the metal material to which ultrasonic waves are applied undergoes recrystallization by heat treatment at a temperature obtained by multiplying the melting point expressed in absolute temperature by 0.35 to 0.6. If the temperature is higher than 0.6 multiplied by the melting point expressed in absolute temperature, which is difficult to control because there is energy loss to suppress the growth of recrystallized grains, and if the temperature is lower than 0.35 multiplied by metal, Only the recovery, which is a phenomenon in which the strain inside the material partially disappears, is performed, and no recrystallized grains are generated.
  • the recrystallization temperature is a temperature at which the metal structure subjected to cold working is practically completely changed to a structure having new recrystallized grains by a heat treatment for 1 hour in practice. It is a specific value that changes depending on the purity, the degree of internal strain, etc., but tends to converge to a certain temperature as the internal strain increases. That is, in a metal material that has undergone a large internal strain, it is considered that grain growth is suppressed by setting the above temperature range as one guide, and a desired high-strength superplastic material can be easily obtained.
  • the shape of the metal material There is no particular limitation on the shape of the metal material.
  • a plate material, a rod material, a pipe which is a powder solidified molded product or a molten material, or a molded product which is press-molded into a target shape can be used.
  • the powder solidified compact is a powder sintered compact or a solid compact formed by compressive shearing of a powder
  • the ingot material is a molded product or a metal material that has been melted and solidified after being pressed or extruded into a desired shape.
  • stuffed food Such as stuffed food.
  • a method of applying ultrasonic waves to the metal material for example, a method in which a horn connected to an ultrasonic vibrator is brought into close contact with the metal material and ultrasonic waves are applied for a certain period of time is used.
  • Grease or the like can be inserted between the horn and the metal material to efficiently transmit vibration from the horn to the metal material.
  • grease is difficult to be deteriorated or ignited by vibrations, and safe grease must be used.
  • silicone grease can be used.
  • the ultrasonic frequency, output and application time must be determined by taking into account the melting point, intrinsic damping capacity, size, etc. of metallic materials, and optimal values must be determined.
  • a 200W ultrasonic wave with a frequency of 19KHz is output using a 22mm diameter titanium alloy horn for 5-60 seconds. It is good to apply.
  • the metal material to which the ultrasonic wave is applied is heated at the recrystallization temperature for one hour.
  • AZ31 is expected to have a recrystallization temperature of 180 230 ° C, and is heated at 230 ° C in vacuum for lh. If it is other than vacuum, it is preferable to heat under an argon atmosphere. When heated in nitrogen, hydrogen or oxygen, it forms compounds with these and deteriorates surface and mechanical properties. It should be noted that any oxidation-resistant metal material may be heated in the air.
  • the recrystallized metal material maintains its initial shape, and its crystal grain size becomes 1 / 10-1 / 150 of that before ultrasonic waves were applied.
  • the size of the material does not change, and the crystal structure with a crystal grain size of 150-200 / im is an equiaxed crystal structure of 11/15 / m.
  • a pure A1 wrought material for industrial use CFIS alloy number 1100
  • a test piece of 20 mm X 50 mm X 1.25 mm was cut out with a peripheral blade cutter, and the surface was quickly washed with ethanol.
  • an ultrasonic homogenizer as an ultrasonic application means, an appropriate amount of silicone grease was applied to the end face of a horn made of titanium alloy and having a diameter of 22mm, and the above-mentioned industrial pure A1 wrought material test piece was jacked there.
  • the operation of applying ultrasonic vibration of 300 W at 19 KHz for 60 seconds was performed three times while pressing.
  • the commercial pure Al wrought specimen to which ultrasonic waves were applied was inserted into a vacuum heating furnace and subjected to lh heat treatment at a degree of vacuum of 5 Pa and a heating temperature of 468 K, ie, a heating temperature / melting point of 0.50.
  • the tensile strength of the heat-treated industrial pure A1 wrought material was 180 MPa, the elongation at break was 473 K, and the strain rate was 10_4Zs. The tensile strength was 150%, indicating that the superplastic phenomenon had occurred. all right.
  • a lOmm X IOmm XI .25mm microstructure observation test piece was cut out, etched with 0.5% aqua regia, and then subjected to simple polarization observation with an optical microscope.
  • the crystal grain size was found to be about 15 ⁇ m.
  • the crystal grain size before application of ultrasonic waves was 1/10 of 150 xm.
  • test piece of 20 mm ⁇ 50 mm ⁇ I.25 mm was cut out from a cold rolled material of industrial pure iron with an outer peripheral cutter, and the surface was quickly washed with ethanol.
  • an ultrasonic homogenizer as an ultrasonic application means, an appropriate amount of silicone grease was applied to the end face of a horn made of a titanium alloy and having a diameter of 22 mm, and the above-mentioned industrial pure iron cold-rolled material test piece was jacked there. Ultrasonic vibration of 300 K at 19 KHz was applied for 60 seconds while pressing with.
  • test piece of cold rolled industrial pure iron to which ultrasonic waves were applied was inserted into a vacuum heating furnace and subjected to lh heat treatment at a vacuum of 5 Pa and a heating temperature of 923 K, that is, a heating temperature / melting point of 0.51.
  • the tensile strength of the heat-treated industrial pure iron cold-rolled material was 700 MPa, and the elongation at break was 923 K and the strain rate was 10_3Zs. all right.
  • a 20 mm X 50 mm X 1.25 mm test piece was cut out from AZ31 wrought material with an outer edge cutter, and the surface was quickly washed with ethanol.
  • an ultrasonic homogenizer as an ultrasonic application means, an appropriate amount of silicone grease was applied to the end surface of a horn made of a titanium alloy and having a diameter of 22mm, and the above-mentioned AZ31 expanded specimen was pressed with a jack. While applying 200W ultrasonic vibration at 19KHz for 15 seconds
  • the AZ31 wrought specimen to which the ultrasonic wave was applied was introduced into a vacuum heating furnace, and subjected to lh heat treatment at a degree of vacuum of 5 Pa and a heating temperature of 503 K, that is, a heating temperature / melting point of 0.54.
  • the tensile strength of the heat-treated AZ31 wrought material was 300 MPa, the elongation at break was 503K, and the strain rate was ⁇ -2 / s. The strain rate was 100%, indicating that the superplastic phenomenon occurred.
  • the strain rate was 100%, indicating that the superplastic phenomenon occurred.
  • the AZ31 wrought specimen with the ultrasonic wave applied was inserted into a vacuum heating furnace and subjected to lh heat treatment at a degree of vacuum of 5 Pa and a heating temperature of 463 K, that is, a heating temperature / melting point of 0.50. A similar operation was performed.
  • the tensile strength of the heat-treated AZ31 wrought material was 310 MPa, and the elongation at break was measured at 503 K and the strain rate was ⁇ -2 / s. I understand.
  • a lOmm X IOmm XI .25 mm microstructure observation test piece was cut out, etched with a 1% ethanol nitrate solution, and subjected to simple polarization observation with an optical microscope.
  • the crystal grain size was about 3 ⁇ m, It was 1/50 of the crystal grain size of 150 ⁇ m before the application of sound waves.
  • the tensile strength of the heat-treated AZ31 wrought material was 300 MPa, the elongation at break was 503K, and the strain rate was ⁇ -2 / s. The strain rate was 100%, indicating that the superplastic phenomenon occurred.
  • the strain rate was 100%, indicating that the superplastic phenomenon occurred.
  • a lOmmXIOmmXI. 25mm microstructure observation test piece was cut out, etched with a 1% ethanol nitrate solution, and then subjected to simple polarization observation with an optical microscope.
  • the crystal grain size was found to be about 5 ⁇ m. It was 1/30 of the crystal grain size of 150 ⁇ m before sound wave application.
  • test piece of 20 mm ⁇ 50 mm ⁇ 1.25 mm was cut out from AZ31 wrought material with an outer cutter, and the surface was quickly washed with ethanol.
  • An ultrasonic homogenizer was used as an ultrasonic application means, and a horn end face made of a titanium alloy and having a diameter of 22mm was installed at a distance of 2cm from an AZ31 wrought material test piece submerged in pure water. Then, ultrasonic vibration of 240 W at 19 KHz was applied for 300 seconds.
  • test piece of AZ31 material to which the ultrasonic wave was applied was inserted into a vacuum heating furnace and subjected to lh heat treatment at a vacuum degree of 5 Pa and a heating temperature of 453 K, ie, a heating temperature / melting point of 0.49.
  • the tensile strength of the heat-treated AZ31 wrought material was 375MPa, and the elongation at break was 233K when examined at 503K and the strain rate ⁇ ⁇ -2 / s, indicating that the superplastic phenomenon occurred.
  • a lOmmXIOmmXI 25mm tissue observation specimen was cut out, etched with a 1% ethanol nitrate solution, and then subjected to simple polarization observation with an optical microscope. As a result, the crystal grain size was about lxm. The crystal grain size before application was 1/150 of 150 zm.
  • An ultrasonic homogenizer was used as a means for applying ultrasonic waves, and the horn end face made of a titanium alloy and having a diameter of 22mm was set at a distance of 2cm from an AZ31 wrought material specimen submerged in pure water. Then, ultrasonic vibration of 240 W at 19 KHz was applied for 300 seconds.
  • test piece of AZ31 material to which ultrasonic waves were applied was introduced into a vacuum heating furnace, and subjected to lh heat treatment at a vacuum degree of 5 Pa and a heating temperature of 303 K, that is, a heating temperature / melting point of 0.33.
  • the tensile strength of the heat-treated AZ31 wrought material was 260 MPa, the elongation at break was 503K, and the strain rate was ⁇ -2 / s.When measured at 50%, it was confirmed that the superplastic phenomenon did not occur. Was done.
  • a lOmm X IOmm XI .25mm microstructure observation test piece was cut out, etched with a 1% ethanol nitrate solution, and then subjected to simple polarization observation with an optical microscope.
  • the crystal grain size was found to be about 150 ⁇ . There was no change with respect to the crystal grain size of 150 / im before the application of ultrasonic waves.
  • the tensile strength of the heat-treated AZ31 wrought material was 280 MPa, the elongation at break was measured at 503 K and the strain rate was ⁇ -2 / s, indicating 80%, confirming that no superplastic phenomenon had occurred.
  • the tensile strength of the heat-treated AZ31 wrought material was 280 MPa, the elongation at break was measured at 503 K and the strain rate was ⁇ -2 / s, indicating 80%, confirming that no superplastic phenomenon had occurred.
  • a lOmm X IOmm XI. 25mm microstructure observation specimen was cut out, etched with a 1% ethanol nitrate solution, and then subjected to simple polarization observation with an optical microscope.
  • the crystal grain size was found to be about 30 ⁇ m. And 15 with a crystal grain size of 150 ⁇ m before the application of ultrasonic waves.
  • a large internal strain can be given to a metal material, and a high-strength superplastic material in which the structure of the metal material is composed of fine crystal grains can be easily obtained. Obtainable.

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Abstract

A method for producing a high strength ultra plastic material which comprises applying an ultrasonic wave to a metal material and subjecting the resultant material to a heating treatment at a temperature obtained by multiplying the melting point of the material represented by an absolute temperature by 0.35 to 0.6. The metal material is preferably a high damping metal material having a specific damping capacity of 10 % or more, and in particular, Mg or an Mg alloy is most suitable for the metal material. The above method allows the production of a high strength ultra plastic metal material, which has a metal structure comprising fine crystal grains, with simplicity and ease.

Description

明 細 書  Specification
高強度'超塑性材料の製造方法  Method of manufacturing high strength 'superplastic material'
技術分野  Technical field
[0001] 本発明は、超音波を利用した金属材料の結晶粒微細化に係るものであり、高強度' 超塑性特性を有する金属材料の製造方法に関する。  The present invention relates to the refinement of crystal grains of a metal material using ultrasonic waves, and relates to a method for producing a metal material having high-strength superplastic characteristics.
背景技術  Background art
[0002] 金属材料は、結晶粒が小さくなるほど強度、靱性および耐食性が大きくなることが 知られている。その結晶粒を数/ m以下にすると超塑性現象が発現し、常温では極 めて高強度でありながら特定の加熱条件下で加工性が飛躍的に向上する。  [0002] It is known that the strength, toughness, and corrosion resistance of a metal material become larger as the crystal grain becomes smaller. When the crystal grains are reduced to a few g / m or less, a superplastic phenomenon occurs, and the workability is drastically improved under specific heating conditions while having extremely high strength at room temperature.
一般的な超塑性の定義は、多結晶材料の引張変形において、変形応力が高い歪 み依存性を示し、局部収縮を生じることなく数百％以上の巨大な伸びを示す現象とさ れており、具体的には、等軸状で 10 μ ΐη以下の小さな結晶粒を有する材料は、絶対 温度で表された融点の 1/2以上の温度で、歪み速度 ΙΟ-4/s程度で変形したとき 、 lOMPa以下の低い変形応力で巨大な伸びを発現すると言われている。  The general definition of superplasticity is a phenomenon in which the tensile stress of a polycrystalline material shows a high strain dependence of the deformation stress and a huge elongation of several hundred percent or more without local shrinkage. Specifically, a material with equiaxed small crystal grains of 10 μΐη or less deformed at a temperature of 1/2 or more of the melting point expressed in absolute temperature and a strain rate of ΙΟ-4 / s. At times, it is said that a large deformation is developed with a low deformation stress of lOMPa or less.
[0003] 鉄鋼材料および非鉄金属材料の結晶粒微細化方法としては、結晶粒の成長抑制 元素を添加する方法、加工熱処理による変態、析出、再結晶を利用する方法、強せ ん断カ卩ェを加える方法などが知られている（例えば、特開 2003—041331号公報、 特開 2002— 194472号公報、特開 2002— 105568号公報、特開 2000— 271693号 公報参照）。  [0003] Grain refining methods for iron and steel materials and non-ferrous metal materials include a method of adding an element that suppresses the growth of crystal grains, a method of utilizing transformation, precipitation, and recrystallization due to thermomechanical treatment, and a method of strong shearing. (See, for example, JP-A-2003-041331, JP-A-2002-194472, JP-A-2002-105568, and JP-A-2000-271693).
[0004] 鉄鋼材料は、加工熱処理による変態、析出、再結晶を利用する方法が有効で、実 験室規模で 1 μ m未満の微細結晶粒組織が得られている力 S、大量生産に対応する ため如何に工程を簡素化できるかが課題である。  [0004] For iron and steel materials, it is effective to use transformation, precipitation, and recrystallization by thermomechanical treatment, and it is suitable for mass production in the laboratory scale, where the fine grain structure of less than 1 μm is obtained. The challenge is how to simplify the process.
一方の非鉄金属材料、特にアルミニウムについては、従来 10 x m以下の微細結晶 粒組織を均一に作ることが難しぐ 日本にぉレ、ては 3 μ m以下の微細結晶粒組織創 製のため新エネルギー ·産業技術総合開発機構 (NEDO)によるプロジェクトとして平 成 9年から 5年計画で技術開発が行われた力 S、その基本となる技術は材料に強せん 断加工をカ卩える方法である。 [0005] また、最近では、軽量かつ強靱で高レ、振動吸収性を有するマグネシウム合金がノ ート型パーソナルコンピュータ、携帯電話の筐体に使用されているが、結晶構造が六 方最密充填構造であるマグネシウムは室温で低延伸性のためプレス等の二次カロェ が難しぐダイキャストやチクソモールディングで成形しなければ良質の部品や筐体 ができない欠点がある。このような製造方法の制限は、マグネシウム合金の用途を狭 めている原因でもある。 On the other hand, for non-ferrous metal materials, especially aluminum, it has been difficult to uniformly produce a fine grain structure of less than 10 xm in the past. In Japan, new energy is required to create a fine grain structure of less than 3 μm. · Technology development was carried out as a project by the National Institute of Advanced Industrial Science and Technology (NEDO) in 1997 to 5 years, and the basic technology is a method of cutting strong shearing into materials. [0005] Recently, lightweight, tough, high-performance, vibration-absorbing magnesium alloys have been used for the housings of notebook personal computers and mobile phones, but the crystal structure is hexagonal close-packed. Magnesium, which has a structure, has a drawback that high-quality parts and casings cannot be produced unless molded by die casting or thixomolding, which is difficult for secondary calories due to low stretchability at room temperature. This limitation of the manufacturing method is also a reason for narrowing the applications of magnesium alloys.
[0006] さらに、マグネシウム合金の強度の不足は、 自動車や航空機といった輸送機器へ の適用が進まない一因ともなつている。  [0006] Furthermore, the lack of strength of magnesium alloys also contributes to the lack of application to transportation equipment such as automobiles and aircraft.
この課題を解決するため、 1 β m以下の微細結晶粒を得る技術開発が検討されて いる。その一つはアルミニウムと同様に強せん断カ卩ェをカ卩える方法である。  To solve this problem, technology development to obtain fine crystal grains of 1 βm or less is being studied. One of them is a method of kneading strongly sheared kamen like aluminum.
強せん断カ卩ェをカ卩える方法は、金属材料では、押出し、ロール圧延が一般的であ る力 最近では ECAP法（Equal Channel Angular Pressing法）などが研究されている  Extrusion and roll-rolling are common methods for metal materials. The ECAP method (Equal Channel Angular Pressing method) has recently been studied.
[0007] 押出しは、文字通りビレットまたはスラブを所定の形状の穴を有するダイスから押出 す方法で、一般的にはダイスのオリフィスを通して押出す直接法が用いられる。例え ば、純マグネシウムは 350— 400°Cにビレットまたはスラブを加熱し押出す力 \アルミ 二ゥムに較べるとビレット温度と押出し速度のバランスが難しぐ温度が少しでも低い と押出されず、温度を上げると酸化してしまう欠点があり、 Mg— A1— Zn合金 (AZ合金 ) [0007] Extrusion is a method in which a billet or slab is literally extruded from a die having a hole of a predetermined shape, and a direct method of extruding through an orifice of the die is generally used. For example, pure magnesium extrudes billets or slabs at a temperature of 350-400 ° C and extrudes it. \ Compared to aluminum, it is difficult to balance the billet temperature and extrusion speed. Mg-A1-Zn alloy (AZ alloy)
などはさらに精密な制御が必要である。  For example, more precise control is required.
[0008] ロール圧延は、金属材料を上下のロールで加圧しながら一方向に送り出す方法で[0008] Roll rolling is a method in which a metal material is fed in one direction while being pressed by upper and lower rolls.
、繰り返し接合圧延（Accumulative Roll Bonding),極低温圧延、異周速圧延、溶湯圧 延、温間圧延などが研究されている。 Accumulative Roll Bonding, cryogenic rolling, different peripheral speed rolling, melt rolling, warm rolling, etc. are being studied.
繰り返し接合圧延は、圧延された板を長さの方向に半割りし、脱脂等の表面処理を 施した後、二枚の板を重ね合わせて再度圧延する方法である。この方法は板厚を変 化させずに強せん断カ卩ェできる特徴が有るが、製造コストが高レ、欠点がある。  The repetitive joining rolling is a method in which a rolled plate is halved in a length direction, subjected to a surface treatment such as degreasing, and then two plates are overlapped and rolled again. This method has the characteristic that it can be strongly sheared without changing the plate thickness, but it has a high manufacturing cost and disadvantages.
[0009] 極低温圧延は、圧延で導入した歪みを可能な限り回復させない液体窒素温度で圧 延し、その後急速加熱で微細な再結晶粒の形成をねらった方法であるが、十分な効 果は得られていない。 [0009] Cryogenic rolling is a method of rolling at a temperature of liquid nitrogen that does not recover as much as possible the strain introduced by rolling, and then rapidly heating to form fine recrystallized grains. No fruit has been obtained.
異周速圧延は、上下のロールの周速を変えて材料に強せん断力卩ェを加える方法 であるが、無潤滑で圧延するため不均一なせん断力を受け易ぐ表面状態が荒れる 欠点がある。  Different peripheral speed rolling is a method of applying a strong shearing force to the material by changing the peripheral speed of the upper and lower rolls.However, since the rolling is performed without lubrication, the surface condition that is easily subjected to uneven shearing force is roughened. is there.
[0010] 溶湯圧延は、添加元素を過飽和に固溶させた溶湯を水冷したロールに流し込むな どで急速冷却する方法で、添加元素が再結晶核発生を促すと同時に粒成長を抑制 させる効果があるが、酸化されやすい金属材料は、十分な雰囲気調整が必要で大量 生産に向かない。  [0010] Melt rolling is a method of rapidly cooling, for example, by pouring a molten metal in which an additive element is supersaturated into a water-cooled roll, and has the effect of suppressing the grain growth while promoting the generation of recrystallization nuclei. However, metal materials that are easily oxidized are not suitable for mass production because sufficient atmosphere adjustment is required.
温間圧延は、再結晶温度以上で圧延する熱間圧延と常温で圧延する冷間圧延の 中間に相当する温度で圧延する方法で、例えば A1— Zn— Mg_Cu合金に適当量の Z rを添加した合金では、微細結晶粒組織が得られるなど一部の合金で効果が確認さ れている。しかし、中間温度の制御は非常に難しぐ他の金属材料に対して効果が得 られるか不明な点が多い。  Warm rolling is a method of rolling at a temperature equivalent to the middle point between hot rolling at a temperature higher than the recrystallization temperature and cold rolling at normal temperature.For example, an appropriate amount of Zr is added to an A1-Zn-Mg_Cu alloy The effect of some of the alloys has been confirmed, such as obtaining a fine grain structure. However, it is not clear whether controlling the intermediate temperature is effective for other metal materials that are very difficult.
[0011] ECAP法は、ある角度を持った穴を有するダイスの中にビレットまたはスラブを入れ 、加圧、押出すことでビレットまたはスラブに強せん断力を加える方法で、微細結晶 粒組織を得る方法として非常に効果的であり注目を集めているが、強せん断カを受 けたビレットまたはスラブは非常に強靱であるため、例えば圧延などの二次加工が難 しぐ加工性を良くするために熱間圧延を行うと結晶粒が成長し実用レベルで十分な 強度、靱性および高延性を満たしていないのが実状である。  [0011] The ECAP method is a method in which a billet or slab is put into a die having a hole with a certain angle, and a high shear force is applied to the billet or slab by pressing and extruding to obtain a fine grain structure. Although it is very effective as a method and attracts attention, billets or slabs that have been subjected to strong shearing force are very tough, so secondary processing such as rolling is difficult to improve workability. When hot rolling is performed, crystal grains grow and do not satisfy sufficient strength, toughness and high ductility at practical levels.
[0012] なお、 ECAP法の欠点を補う方法として、 ECAP法を連続化した連続せん断変形 加工法（Conshearing法）も提案されている（Saitou外 2名、「PROPOSAL OF NOVEL CONTINUOUS HIGH STRATING PROCESS-DEVELOPMENT OF  [0012] As a method of compensating for the shortcomings of the ECAP method, a continuous shear deformation processing method (Conshearing method), which is a continuous version of the ECAP method, has also been proposed (Saitou et al., "PROPOSAL OF NOVEL CONTINUOUS HIGH STRATING PROCESS-DEVELOPMENT"). OF
CONSHEARING PROCESS」、 Advanced Technology of Plasticity、 Vol.III、  CONSHEARING PROCESS, Advanced Technology of Plasticity, Vol.III,
Proceedings of the 6th International Conference on Technology of Plasticity、 Sept, 19一 24， 1999、 p.2459 2464参照）。  Proceedings of the 6th International Conference on Technology of Plasticity, Sept, 19-24, 1999, p.2459 2464).
[0013] 何れの方法も溶製したビレット等を強せん断加工する方法であり、せん断加工に非 常に大きな応力を必要とするか、または金属材料の初期形状を維持することができな レ、。 発明の開示 [0013] Either method is a method in which a billet or the like that has been melted is subjected to a strong shearing process, and a very large stress is required for the shearing process, or the initial shape of the metal material cannot be maintained. Disclosure of the invention
[0014] 本発明は、上記従来技術の問題点を解決するものであって、金属材料の組織が微 細結晶粒力 なる高強度 ·超塑性材料を簡便に得ることのできる高強度 ·超塑性材料 の製造方法を提供することを目的とする。  [0014] The present invention solves the above-mentioned problems of the prior art, and has a high strength in which the structure of the metal material is fine crystal grain force. It is intended to provide a method for producing a material.
本発明の高強度'超塑性材料の製造方法では、金属材料に超音波を印加した後、 この金属材料を絶対温度で表されたその融点に 0. 35乃至 0. 6を乗じた温度で加熱 処理することで上記課題を解決してレ、る。  In the method for producing a high-strength 'superplastic material of the present invention, after applying ultrasonic waves to a metal material, the metal material is heated at a temperature obtained by multiplying its melting point expressed in absolute temperature by 0.35 to 0.6. The above problem is solved by processing.
[0015] 金属材料は、多くの場合、振動が与えられるとやがて減衰し、最後に振動は停止す る。振動が減衰する機構は二つあり、一つは外部摩擦（external friction)と呼ばれ、 振動し [0015] In many cases, the metal material is attenuated when vibration is applied, and finally the vibration stops. There are two mechanisms for damping vibration, one of which is called external friction.
ている金属材料から外部へ空気等を介して振動エネルギーが放出される機構である 。他の一つは内部摩擦 (internal friction)で、金属材料内部で振動エネルギーが熱 あるいは歪み等に変換される機構である。内部摩擦は減衰能 (damping capacity)とも 呼ばれる。  This is a mechanism in which vibration energy is released from the metal material to the outside via air or the like. The other is internal friction, a mechanism by which vibration energy is converted into heat or strain inside a metal material. Internal friction is also called damping capacity.
[0016] 減衰能は、振動エネルギーの変換機構の違いによって次の四つに分類される。 (1 )母相と第 2相との間の界面で粘性流動または塑性流動をおこすことによるもの。  [0016] The damping ability is classified into the following four types depending on the difference in vibration energy conversion mechanism. (1) By viscous or plastic flow at the interface between the parent phase and the second phase.
(2)磁区壁の非可逆移動によるもの。  (2) Due to irreversible movement of the domain wall.
(3)転位が不純物原子による固着点から離脱することによるもの。  (3) The dislocation is caused by the detachment from the fixing point by the impurity atom.
(4)母相とマルテンサイト相との境界などにおける変態双晶境界の移動によるもの。  (4) Due to the movement of the transformation twin boundary at the boundary between the parent phase and the martensite phase.
[0017] 特に減衰能が大きな金属材料においては、振動エネルギーの一部が前記（1)一 ([0017] In particular, in a metal material having a large damping capacity, a part of the vibration energy
4)の分類のいずれかの変換機構で熱として消費される力、、あるいは歪みとして蓄積 される。歪みが蓄積された金属材料には、機械的にせん断をカ卩えるのと同等以上の 大きな歪みが導入されるため、その金属材料を絶対温度で表されたその融点に 0. 3 5乃至 0. 6を乗じた温度で加熱処理すると、格子欠陥が再配列または相互に合体消 滅することによるエネルギー開放の過程で等軸状の微細結晶粒からなる再結晶組織 に変化すると考えられる。 The force is consumed as heat in any of the conversion mechanisms in the category of 4), or accumulated as strain. Since a large strain equal to or greater than mechanical shearing is introduced into the metal material in which the strain is accumulated, the metal material has a melting point expressed in absolute temperature of 0.35 to 0.35. When heat treatment is carried out at a temperature multiplied by 1.6, it is considered that the lattice defects change to a recrystallized structure consisting of equiaxed fine crystal grains in the process of energy release due to rearrangement or mutual annihilation.
[0018] 減衰能が大きな金属材料とは、一般的に固有減衰能（specific damping [0018] A metal material having a large damping capacity generally means a specific damping capacity (specific damping capacity).
capacity:S.D.C)が 10%以上のものを指し、高減衰金属材料などと総称される。純金 属では Mg、 Ni、 Feが大きな固有減衰能を有し、合金では Mg合金、 Mn— Cu合金、 Mn - Cu - A1合金、 Cu - Zn - A1合金、 Cu - Al_Ni合金、 Fe_Cr合金（12Cr鋼）、 Fe _Cr一 A1合金、 Fe_Cr - Mo合金、 Co_Ni合金、 Fe_Cr - Al_Mn合金、 Ni - Ti合金 、 Cu_Zn_Al合金、 Al_Zn合金、粒界腐食処理 18—8ステンレス鋼、 Fe_C_Si合金 (片状黒鉛铸鉄または球状黒鉛铸鉄を圧延した圧延錡鉄)などが大きな固有減衰能 を有し、高減衰合金、制振合金または防振合金などと呼ばれる。 capacity: SDC) is 10% or more, and is collectively referred to as high attenuation metal materials. pure gold Mg, Ni, and Fe have a large specific damping capacity, and alloys such as Mg alloy, Mn-Cu alloy, Mn-Cu-A1 alloy, Cu-Zn-A1 alloy, Cu-Al_Ni alloy, Fe_Cr alloy (12Cr steel ), Fe_Cr-A1 alloy, Fe_Cr-Mo alloy, Co_Ni alloy, Fe_Cr-Al_Mn alloy, Ni-Ti alloy, Cu_Zn_Al alloy, Al_Zn alloy, intergranular corrosion treatment 18-8 stainless steel, Fe_C_Si alloy (flake graphite-iron) Or, spheroidal graphite (iron rolled iron) has a large specific damping capacity and is called a high damping alloy, a vibration damping alloy or a vibration damping alloy.
[0019] 固有減衰能は、次式の通り、振動する物体の 1サイクルあたりの振動エネルギー損 失率で表される。 [0019] The intrinsic damping capacity is represented by a vibration energy loss rate per cycle of a vibrating object as follows.
S.D.C(%) = ( AW/W) X 100  S.D.C (%) = (AW / W) X 100
ここで Wは振動エネルギー、 は 1サイクルに失われるエネルギーである。  Where W is the vibrational energy and is the energy lost in one cycle.
固有減衰能が 10%以上の高減衰金属材料の中でも Mgまたは Mg合金力 本方法 を適用するのに最適である。 Mgはすべての金属材料の中で最も減衰能が大きく固 有減衰能が 60%以上を示すため、振動エネルギーを歪みとして蓄積し易く適切な温 度で加熱処理することで微細結晶粒からなる再結晶組織にすることが可能である。 M gは強度および耐食性が比較的小さぐこの課題が改善された Al、 Zn、 Zrなどを添 カロした Mg合金は、 Mgと比較すると減衰能が低下するが、超音波振動エネルギーの 一部を歪みとして蓄積し、添加元素の効果との相乗効果で加熱処理によって微細結 晶粒からなる再結晶組織となり、より一層の高強度と超塑性を両立することが可能で める。  Even among high damping metallic materials with an intrinsic damping capacity of 10% or more, Mg or Mg alloy force is most suitable for applying this method. Mg has the largest damping ability among all metallic materials and has a specific damping ability of 60% or more.Therefore, it is easy to accumulate vibration energy as strain, and heat treatment at an appropriate temperature makes it possible to regenerate fine crystal grains. It is possible to have a crystal structure. Mg is relatively low in strength and corrosion resistance.This problem has been solved.A Mg alloy added with Al, Zn, Zr, etc., has a lower damping capacity than Mg, but some of the ultrasonic vibration energy is lost. It accumulates as strain and becomes a recrystallized structure composed of fine crystal grains by the heat treatment due to the synergistic effect with the effect of the added element, and it is possible to achieve both higher strength and superplasticity.
[0020] Mg合金は、 Mg - A1合金、 Mg - A1 - Zn合金、 Mg - Zr合金、 Mg - Zn - Zr合金、 M g_Mg2 Ni合金、 Mg— RE— Zn合金（REはレアアース）、 Mg— Ag— RE合金（REはレ ァアース）、 Mg_Y_RE合金（REはレアアース）などが実用合金として知られている 力 A1添加量が増加すると減衰能が低下するので Mg— A1合金および Mg— A1— Zn 合金の中でも Mg_10%Al合金（A1100)、 Mg_9%Al_l %Zn合金（AZ91)、 Mg_ 6%Α1_3。/0Ζη合金 (AZ63)などの固有減衰能は 10。/o未満である。 [0020] Mg alloy includes Mg-A1 alloy, Mg-A1-Zn alloy, Mg-Zr alloy, Mg-Zn-Zr alloy, Mg_Mg2 Ni alloy, Mg— RE— Zn alloy (RE is rare earth), Mg— Ag-RE alloys (RE is rare earth), Mg_Y_RE alloys (RE is rare earth), etc. are known as practical alloys. As the amount of A1 added increases, the damping capacity decreases, so Mg-A1 alloy and Mg-A1-Zn Among alloys, Mg_10% Al alloy (A1100), Mg_9% Al_l% Zn alloy (AZ91), Mg_6% Α1_3. / 0 The specific damping capacity of Ζη alloy (AZ63) is 10. less than / o.
[0021] Mgまたは Mg合金に印加された超音波振動エネルギーは、前記振動エネルギー の変換機構（3)に記述したように、転位が不純物原子による固着点から離脱すること によって 消費されるか、または変形双晶の生成に消費されると考えられる。 [0021] The ultrasonic vibration energy applied to Mg or the Mg alloy is, as described in the above-mentioned vibration energy conversion mechanism (3), the dislocation is detached from the anchoring point by the impurity atom. It is believed that it is consumed or consumed to form deformation twins.
超音波を印加した金属材料は、絶対温度で表された融点に 0. 35乃至 0. 6を乗じ た温度で加熱処理することで再結晶化が行われるが、絶対温度で表された融点に 0 . 6を乗じた温度より高温では、再結晶粒の成長を抑制するためのエネルギーロスが あり制御が難しぐ絶対温度で表された融点に 0. 35を乗じた温度より低温では、金 属材料内部の歪みが一部消失する現象である回復が行われるだけで再結晶粒は発 生しない。  The metal material to which ultrasonic waves are applied undergoes recrystallization by heat treatment at a temperature obtained by multiplying the melting point expressed in absolute temperature by 0.35 to 0.6. If the temperature is higher than 0.6 multiplied by the melting point expressed in absolute temperature, which is difficult to control because there is energy loss to suppress the growth of recrystallized grains, and if the temperature is lower than 0.35 multiplied by metal, Only the recovery, which is a phenomenon in which the strain inside the material partially disappears, is performed, and no recrystallized grains are generated.
[0022] 再結晶温度は、実用上、冷間加工を受けた金属組織が、 1時間の熱処理によって 新たな再結晶粒を有する組織に完全に変化する温度であり、本来、金属材料の種類 、純度、内部歪みの程度などによって変化する特有の値であるが、内部歪みが増加 するにしたがって一定の温度に収束する傾向がある。すなわち、大きな内部歪みを 受けた金属材料では、上記の温度範囲を一つの目安とすることで粒成長が抑制され 、 目的とする高強度 ·超塑性材料が得られ易いと考えられる。  [0022] The recrystallization temperature is a temperature at which the metal structure subjected to cold working is practically completely changed to a structure having new recrystallized grains by a heat treatment for 1 hour in practice. It is a specific value that changes depending on the purity, the degree of internal strain, etc., but tends to converge to a certain temperature as the internal strain increases. That is, in a metal material that has undergone a large internal strain, it is considered that grain growth is suppressed by setting the above temperature range as one guide, and a desired high-strength superplastic material can be easily obtained.
発明を実施するための最良の形態  BEST MODE FOR CARRYING OUT THE INVENTION
[0023] 金属材料の形状に特別な制限を設けない。例えば、粉末固化成形体または溶製 材である板材、棒材、パイプあるいは目的形状にプレス成形した成形体等を用いるこ とができる。粉末固化成形体とは、粉末焼結体あるいは粉末の圧縮せん断によって 作製した固化成形体などであり、溶製材とは、錡造物あるいは溶融後固化した金属 材料を目的の形状にプレス加工または押出しカ卩ェした物などである。  There is no particular limitation on the shape of the metal material. For example, a plate material, a rod material, a pipe which is a powder solidified molded product or a molten material, or a molded product which is press-molded into a target shape can be used. The powder solidified compact is a powder sintered compact or a solid compact formed by compressive shearing of a powder, and the ingot material is a molded product or a metal material that has been melted and solidified after being pressed or extruded into a desired shape. Such as stuffed food.
[0024] 金属材料へ超音波を印加する方法としては、例えば、超音波振動子に接続された ホーンを金属材料に密着させ、一定時間超音波を印加する方法が用いられる。ホー ンから金属材料へ振動を効率よく伝達するためにホーンと金属材料との間にグリース 等を入れることも可能である。ただし、グリースは、振動によって劣化あるいは発火な どし難レ、安全なものを使用しなければならなレ、。例えばシリコ一ングリースなどは使用 可能である。  As a method of applying ultrasonic waves to the metal material, for example, a method in which a horn connected to an ultrasonic vibrator is brought into close contact with the metal material and ultrasonic waves are applied for a certain period of time is used. Grease or the like can be inserted between the horn and the metal material to efficiently transmit vibration from the horn to the metal material. However, grease is difficult to be deteriorated or ignited by vibrations, and safe grease must be used. For example, silicone grease can be used.
[0025] その他、水中または有機溶媒中に金属材料を入れ、ホーンから発せられる振動を、 水または有機溶媒を介して金属材料に伝達させるなど中間媒体を介して振動を伝達 させることも可能であり、効率よく安全に振動を伝達できる方法であれば、上記以外 の方法を用いても差し支えない。 [0025] In addition, it is also possible to put the metal material in water or an organic solvent and transmit the vibration through an intermediate medium such as transmitting the vibration generated from the horn to the metal material through the water or the organic solvent. Any other method that can transmit vibration efficiently and safely The method of the above may be used.
超音波の振動数と出力および印加時間は、金属材料の融点、固有減衰能、大きさ などを十分考慮に入れ最適値を決定しなければならなレ、が、例えば高減衰合金の M g合金である Mg_3%Al_l %Zn合金（AZ31)展伸材（20mm X 50mm X 1. 25m m)では、周波数 19KHzで出力 200Wの超音波を直径 22mmのチタン合金製のホ ーンで 5— 60秒間印加するとよい。  The ultrasonic frequency, output and application time must be determined by taking into account the melting point, intrinsic damping capacity, size, etc. of metallic materials, and optimal values must be determined. In the wrought Mg_3% Al_l% Zn alloy (AZ31) (20mm x 50mm x 1.25mm), a 200W ultrasonic wave with a frequency of 19KHz is output using a 22mm diameter titanium alloy horn for 5-60 seconds. It is good to apply.
[0026] 超音波を印加した金属材料は、再結晶温度で 1時間加熱する。例えば AZ31は、 再結晶温度が 180 230°Cと予想され、 230°C、 lh真空中で加熱する。真空以外で あればアルゴン雰囲気下で加熱することが好ましい。窒素、水素または酸素中で加 熱すると、これらとの化合物を形成し、表面性状や機械的性質を悪化させる。なお、 耐酸化性の金属材料であれば大気中加熱でも構わなレ、。  [0026] The metal material to which the ultrasonic wave is applied is heated at the recrystallization temperature for one hour. For example, AZ31 is expected to have a recrystallization temperature of 180 230 ° C, and is heated at 230 ° C in vacuum for lh. If it is other than vacuum, it is preferable to heat under an argon atmosphere. When heated in nitrogen, hydrogen or oxygen, it forms compounds with these and deteriorates surface and mechanical properties. It should be noted that any oxidation-resistant metal material may be heated in the air.
[0027] 超音波を印加した後、再結晶化した金属材料は、初期形状を維持したまま、その結 晶粒径は、超音波を印加する前の 1/10— 1/150となる。例えば AZ31展伸材（2 Omm X 50mm X I . 25mm)は、材料の大きさは変化せず、結晶粒径 150— 200 /i mあった結晶組織が等軸状の 1一 15 / mの結晶組織となり、高強度で超塑性を発現 する AZ31材へ改良することが可能である。  [0027] After the application of ultrasonic waves, the recrystallized metal material maintains its initial shape, and its crystal grain size becomes 1 / 10-1 / 150 of that before ultrasonic waves were applied. For example, in the case of AZ31 wrought material (2 Omm X 50mm XI.25mm), the size of the material does not change, and the crystal structure with a crystal grain size of 150-200 / im is an equiaxed crystal structure of 11/15 / m. Thus, it is possible to improve to AZ31 material which exhibits high strength and superplasticity.
[0028] 以上に示すような本発明の高強度'超塑性材料の製造方法によれば、金属材料の 形状を  [0028] According to the method for producing a high-strength 'superplastic material of the present invention as described above, the shape of the metal material is reduced.
変化させることなしに、内部組織が均一な微細結晶粒組織からなる高強度 ·超塑性 材料を得ること力 Sできる。  It is possible to obtain a high-strength superplastic material with a uniform internal structure consisting of fine-grained grains without any change.
〔実施例 1〕  (Example 1)
金属材料として、工業用純 A1展伸材 CFIS合金番号 1100)力 20mm X 50mm X 1. 25mmの試験片を外周刃カッターで切り出し、エタノールで速やかに表面を洗浄 した。  As a metal material, a pure A1 wrought material for industrial use, CFIS alloy number 1100) A test piece of 20 mm X 50 mm X 1.25 mm was cut out with a peripheral blade cutter, and the surface was quickly washed with ethanol.
[0029] 超音波の印加手段として、超音波ホモジナイザーを使用し、チタン合金で作製され た直径 22mmのホーン端面にシリコーングリースを適量塗り、そこに上記工業用純 A1 展伸材試験片をジャッキで押し当てたまま、 19KHzで 300Wの超音波振動を 60秒 間印加する操作を 3回行った。 超音波を印加した工業用純 Al展伸材試験片は、真空加熱炉に挿入し、真空度 5P a、加熱温度 468Kすなわち加熱温度/融点 =0. 50で、 lh加熱処理を行った。 [0029] Using an ultrasonic homogenizer as an ultrasonic application means, an appropriate amount of silicone grease was applied to the end face of a horn made of titanium alloy and having a diameter of 22mm, and the above-mentioned industrial pure A1 wrought material test piece was jacked there. The operation of applying ultrasonic vibration of 300 W at 19 KHz for 60 seconds was performed three times while pressing. The commercial pure Al wrought specimen to which ultrasonic waves were applied was inserted into a vacuum heating furnace and subjected to lh heat treatment at a degree of vacuum of 5 Pa and a heating temperature of 468 K, ie, a heating temperature / melting point of 0.50.
[0030] 以上の処理による工業用純 A1展伸材試験片の変形および寸法の変化はほとんど 認められなかった。  [0030] Deformation and dimensional change of the pure A1 wrought specimen for industrial use by the above treatment were hardly recognized.
加熱処理を行った工業用純 A1展伸材の引張強さは 180MPaであり、破断伸びを 4 73K、歪み速度 10_4Zsで調べたところ 150%を示し、超塑性現象が発現しているこ とがわかった。  The tensile strength of the heat-treated industrial pure A1 wrought material was 180 MPa, the elongation at break was 473 K, and the strain rate was 10_4Zs.The tensile strength was 150%, indicating that the superplastic phenomenon had occurred. all right.
[0031] さらに lOmm X IOmm X I . 25mmの組織観察試験片を切り出し、 0. 5%王水で エッチングした後、光学顕微鏡で簡易偏光観察を行ったところ、結晶粒径は約 15 μ mであり、超音波印加前の結晶粒径 150 x mの 1/10であった。  [0031] Further, a lOmm X IOmm XI .25mm microstructure observation test piece was cut out, etched with 0.5% aqua regia, and then subjected to simple polarization observation with an optical microscope. The crystal grain size was found to be about 15 µm. The crystal grain size before application of ultrasonic waves was 1/10 of 150 xm.
〔実施例 2〕  (Example 2)
金属材料として、工業用純鉄冷間圧延材から 20mm X 50mm X I . 25mmの試験 片を外周刃カッターで切り出し、エタノールで速やかに表面を洗浄した。  As a metal material, a test piece of 20 mm × 50 mm × I.25 mm was cut out from a cold rolled material of industrial pure iron with an outer peripheral cutter, and the surface was quickly washed with ethanol.
[0032] 超音波の印加手段として、超音波ホモジナイザーを使用し、チタン合金で作製され た直径 22mmのホーン端面にシリコーングリースを適量塗り、そこに上記工業用純鉄 冷間圧延材試験片をジャッキで押し当てたまま、 19KHzで 300Wの超音波振動を 6 0秒間印加した。  [0032] Using an ultrasonic homogenizer as an ultrasonic application means, an appropriate amount of silicone grease was applied to the end face of a horn made of a titanium alloy and having a diameter of 22 mm, and the above-mentioned industrial pure iron cold-rolled material test piece was jacked there. Ultrasonic vibration of 300 K at 19 KHz was applied for 60 seconds while pressing with.
超音波を印加した工業用純鉄冷間圧延材試験片は、真空加熱炉に挿入し、真空 度 5Pa、加熱温度 923Kすなわち加熱温度/融点 =0. 51で、 lh加熱処理を行った  The test piece of cold rolled industrial pure iron to which ultrasonic waves were applied was inserted into a vacuum heating furnace and subjected to lh heat treatment at a vacuum of 5 Pa and a heating temperature of 923 K, that is, a heating temperature / melting point of 0.51.
[0033] 以上の処理による工業用純鉄冷間圧延材試験片の変形および寸法の変化はほと んど認められなかった。 [0033] Deformation and dimensional change of the test piece of industrial pure iron cold-rolled material by the above treatment were hardly observed.
加熱処理を行った工業用純鉄冷間圧延材の引張強さは 700MPaであり、破断伸 びを 923K、歪み速度 10_3Zsで調べたところ 200%を示し、超塑性現象が発現して いることがわかった。  The tensile strength of the heat-treated industrial pure iron cold-rolled material was 700 MPa, and the elongation at break was 923 K and the strain rate was 10_3Zs. all right.
[0034] さらに lOmm X IOmm X I . 25mmの組織観察試験片を切り出し、 1%硝酸エタノ ール溶液でエッチングした後、光学顕微鏡で簡易偏光観察を行ったところ、結晶粒 径は約 10 μ mであり、超音波印加前の結晶粒径 150 μ mの lZl5であった 〔実施例 3〕 [0034] Further, a lOmm X IOmm XI .25mm microstructure observation test piece was cut out, etched with a 1% ethanol nitrate solution, and then subjected to simple polarization observation with an optical microscope to find that the crystal grain size was about 10 µm. Yes, lZl5 with a crystal grain size of 150 μm before ultrasonic application (Example 3)
金属材料として、 AZ31展伸材から 20mm X 50mm X 1. 25mmの試験片を外周 刃カッターで切り出し、エタノールで速やかに表面を洗浄した。  As a metal material, a 20 mm X 50 mm X 1.25 mm test piece was cut out from AZ31 wrought material with an outer edge cutter, and the surface was quickly washed with ethanol.
[0035] 超音波の印加手段として、超音波ホモジナイザーを使用し、チタン合金で作製され た直径 22mmのホーン端面にシリコーングリースを適量塗り、そこに上記 AZ31展伸 材試験片をジャッキで押し当てたまま、 19KHzで 200Wの超音波振動を 15秒間印 加し [0035] Using an ultrasonic homogenizer as an ultrasonic application means, an appropriate amount of silicone grease was applied to the end surface of a horn made of a titanium alloy and having a diameter of 22mm, and the above-mentioned AZ31 expanded specimen was pressed with a jack. While applying 200W ultrasonic vibration at 19KHz for 15 seconds
た。  Was.
超音波を印加した AZ31展伸材試験片は、真空加熱炉に揷入し、真空度 5Pa、加 熱温度 503Kすなわち加熱温度/融点 =0. 54で、 lh加熱処理を行った。  The AZ31 wrought specimen to which the ultrasonic wave was applied was introduced into a vacuum heating furnace, and subjected to lh heat treatment at a degree of vacuum of 5 Pa and a heating temperature of 503 K, that is, a heating temperature / melting point of 0.54.
[0036] 以上の処理による AZ31展伸材試験片の変形および寸法の変化はほとんど認めら れなかった。 [0036] Deformation and dimensional change of the AZ31 wrought specimen by the above treatment were hardly observed.
加熱処理を行った AZ31展伸材の引張強さは 300MPaであり、破断伸びを 503K 、歪み速度 ΙΟ-2/sで調べたところ 100%を示し、超塑性現象が発現していることが わかった。  The tensile strength of the heat-treated AZ31 wrought material was 300 MPa, the elongation at break was 503K, and the strain rate was ΙΟ-2 / s.The strain rate was 100%, indicating that the superplastic phenomenon occurred. Was.
[0037] さらに lOmm X IOmm X I . 25mmの組織観察試験片を切り出し、 1%硝酸エタノ ール溶液でエッチングした後、光学顕微鏡で簡易偏光観察を行ったところ、結晶粒 径は約 5 β mであり、超音波印加前の結晶粒径 150 μ mの 1/30であった。 [0037] Further cut out lOmm X IOmm XI. 25mm tissue observation specimen, after etching in 1% nitric acid ethanol solution was subjected to a simple polarization observation with an optical microscope, the crystal grain size is about 5 beta m Yes, 1/30 of the crystal grain size of 150 μm before ultrasonic application.
〔実施例 4〕  (Example 4)
超音波を印加した AZ31展伸材試験片を、真空加熱炉に挿入し、真空度 5Pa、加 熱温度 463Kすなわち加熱温度/融点 =0. 50で、 lh加熱処理を行う以外は実施 例 3と同様の操作を行った。  The AZ31 wrought specimen with the ultrasonic wave applied was inserted into a vacuum heating furnace and subjected to lh heat treatment at a degree of vacuum of 5 Pa and a heating temperature of 463 K, that is, a heating temperature / melting point of 0.50. A similar operation was performed.
[0038] 加熱処理を行った AZ31展伸材の引張強さは 310MPaであり、破断伸びを 503K 、歪み速度 ΙΟ-2/sで調べたところ 130%を示し、超塑性現象が発現していることが わかった。 [0038] The tensile strength of the heat-treated AZ31 wrought material was 310 MPa, and the elongation at break was measured at 503 K and the strain rate was ΙΟ-2 / s. I understand.
さらに lOmm X IOmm X I . 25mmの組織観察試験片を切り出し、 1%硝酸エタノ ール溶液でエッチングした後、光学顕微鏡で簡易偏光観察を行ったところ、結晶粒 径は約 3 μ mであり、超音波印加前の結晶粒径 150 μ mの 1/50であった。 [0039] 〔実施例 5〕 Further, a lOmm X IOmm XI .25 mm microstructure observation test piece was cut out, etched with a 1% ethanol nitrate solution, and subjected to simple polarization observation with an optical microscope.The crystal grain size was about 3 μm, It was 1/50 of the crystal grain size of 150 μm before the application of sound waves. [Example 5]
超音波を印加した AZ31展伸材試験片を、真空加熱炉に挿入し、真空度 5Pa、カロ 熱温度 523Kすなわち加熱温度/融点 =0. 57で、 0. 5h加熱処理を行う以外は実 施例 3と同様の操作を行つた。  Insert the AZ31 wrought specimen to which the ultrasonic wave was applied into the vacuum heating furnace, and perform the heat treatment at a vacuum of 5 Pa and a calo heating temperature of 523 K, that is, heating temperature / melting point = 0.57 for 0.5 h. The same operation as in Example 3 was performed.
加熱処理を行った AZ31展伸材の引張強さは 300MPaであり、破断伸びを 503K 、歪み速度 ΙΟ-2/sで調べたところ 100%を示し、超塑性現象が発現していることが わかった。  The tensile strength of the heat-treated AZ31 wrought material was 300 MPa, the elongation at break was 503K, and the strain rate was ΙΟ-2 / s.The strain rate was 100%, indicating that the superplastic phenomenon occurred. Was.
[0040] さらに lOmmXIOmmXI. 25mmの組織観察試験片を切り出し、 1%硝酸エタノ ール溶液でエッチングした後、光学顕微鏡で簡易偏光観察を行ったところ、結晶粒 径は約 5 μ mであり、超音波印加前の結晶粒径 150 μ mの 1/30であった。  [0040] Further, a lOmmXIOmmXI. 25mm microstructure observation test piece was cut out, etched with a 1% ethanol nitrate solution, and then subjected to simple polarization observation with an optical microscope. The crystal grain size was found to be about 5 μm. It was 1/30 of the crystal grain size of 150 μm before sound wave application.
〔実施例 6〕  (Example 6)
金属材料として、 AZ31展伸材から 20mmX50mmXl.25mmの試験片を外周 刃カッターで切り出し、エタノールで速やかに表面を洗浄した。  As a metal material, a test piece of 20 mm × 50 mm × 1.25 mm was cut out from AZ31 wrought material with an outer cutter, and the surface was quickly washed with ethanol.
[0041] 超音波の印加手段として、超音波ホモジナイザーを使用し、チタン合金で作製され た直径 22mmのホーン端面を純水中に沈めた AZ31展伸材試験片と 2cmの距離に なるように設置し、 19KHzで 240Wの超音波振動を 300秒間印加した。 [0041] An ultrasonic homogenizer was used as an ultrasonic application means, and a horn end face made of a titanium alloy and having a diameter of 22mm was installed at a distance of 2cm from an AZ31 wrought material test piece submerged in pure water. Then, ultrasonic vibration of 240 W at 19 KHz was applied for 300 seconds.
超音波を印加した AZ31材試験片は、真空加熱炉に挿入し、真空度 5Pa、加熱温 度 453Kすなわち加熱温度/融点 =0. 49で、 lh加熱処理を行った。  The test piece of AZ31 material to which the ultrasonic wave was applied was inserted into a vacuum heating furnace and subjected to lh heat treatment at a vacuum degree of 5 Pa and a heating temperature of 453 K, ie, a heating temperature / melting point of 0.49.
[0042] 以上の処理による AZ31展伸材試験片の変形および寸法の変化はほとんど認めら れなかった。 [0042] Deformation and dimensional change of the AZ31 wrought specimen by the above treatment were hardly observed.
加熱処理を行った AZ31展伸材の引張強さは 375MPaであり、破断伸びを 503K 、歪み速度 ΙΟ-2/sで調べたところ 233%を示し、超塑性現象が発現していること がわかった。  The tensile strength of the heat-treated AZ31 wrought material was 375MPa, and the elongation at break was 233K when examined at 503K and the strain rate 調 べ -2 / s, indicating that the superplastic phenomenon occurred. Was.
[0043] さらに lOmmXIOmmXI. 25mmの組織観察試験片を切り出し、 1%硝酸エタノ ール溶液でエッチングした後、光学顕微鏡で簡易偏光観察を行ったところ、結晶粒 径は約 l xmであり、超音波印加前の結晶粒径 150 zmの 1/150であった。  [0043] Further, a lOmmXIOmmXI. 25mm tissue observation specimen was cut out, etched with a 1% ethanol nitrate solution, and then subjected to simple polarization observation with an optical microscope. As a result, the crystal grain size was about lxm. The crystal grain size before application was 1/150 of 150 zm.
〔比較例 1〕  (Comparative Example 1)
金属材料として、 AZ31展伸材から 20mmX50mmXl. 25mmの試験片を外周 刃カッターで切り出し、エタノールで速やかに表面を洗浄した。 20mmX50mmXl.25mm test piece from AZ31 wrought material as metal material It was cut out with a blade cutter and the surface was quickly washed with ethanol.
[0044] 超音波の印加手段として、超音波ホモジナイザーを使用し、チタン合金で作製され た直径 22mmのホーン端面を純水中に沈めた AZ31展伸材試験片と 2cmの距離に なるように設置し、 19KHzで 240Wの超音波振動を 300秒間印加した。  [0044] An ultrasonic homogenizer was used as a means for applying ultrasonic waves, and the horn end face made of a titanium alloy and having a diameter of 22mm was set at a distance of 2cm from an AZ31 wrought material specimen submerged in pure water. Then, ultrasonic vibration of 240 W at 19 KHz was applied for 300 seconds.
超音波を印加した AZ31材試験片は、真空加熱炉に揷入し、真空度 5Pa、加熱温 度 303Kすなわち加熱温度/融点 =0. 33で、 lh加熱処理を行った。  The test piece of AZ31 material to which ultrasonic waves were applied was introduced into a vacuum heating furnace, and subjected to lh heat treatment at a vacuum degree of 5 Pa and a heating temperature of 303 K, that is, a heating temperature / melting point of 0.33.
[0045] 以上の処理による AZ31展伸材試験片の変形および寸法の変化はほとんど認めら れなかった。  [0045] Deformation and dimensional change of the AZ31 wrought specimen by the above treatment were hardly observed.
加熱処理を行った AZ31展伸材の引張強さは 260MPaであり、破断伸びを 503K 、歪み速度 ΙΟ-2/sで調べたところ 50%を示し、超塑性現象は発現していないことが 確認された。  The tensile strength of the heat-treated AZ31 wrought material was 260 MPa, the elongation at break was 503K, and the strain rate was ΙΟ-2 / s.When measured at 50%, it was confirmed that the superplastic phenomenon did not occur. Was done.
[0046] さらに lOmm X IOmm X I . 25mmの組織観察試験片を切り出し、 1%硝酸エタノ ール溶液でエッチングした後、光学顕微鏡で簡易偏光観察を行ったところ、結晶粒 径は約 150 μ ΐηであり、超音波印加前の結晶粒径 150 /i mに対して変化が認められ なかった。  [0046] Further, a lOmm X IOmm XI .25mm microstructure observation test piece was cut out, etched with a 1% ethanol nitrate solution, and then subjected to simple polarization observation with an optical microscope. The crystal grain size was found to be about 150μΐη. There was no change with respect to the crystal grain size of 150 / im before the application of ultrasonic waves.
〔比較例 2〕  (Comparative Example 2)
超音波を印加した AZ31展伸材試験片を、真空加熱炉に挿入し、真空度 5Pa、カロ 熱温度 533Kすなわち加熱温度/融点 =0. 62で、 lh加熱処理を行う以外は比較 例 1と同様の操作を行つた。  Insert the AZ31 wrought specimen to which the ultrasonic wave was applied into a vacuum heating furnace, and apply the same procedure as in Comparative Example 1 except that the vacuum degree was 5 Pa, the caro heating temperature was 533 K, that is, the heating temperature / melting point was 0.62, and the lh heat treatment was performed. A similar operation was performed.
[0047] 以上の処理による AZ31展伸材試験片の変形および寸法の変化はほとんど認めら れなかった。 [0047] Deformation and dimensional change of the AZ31 wrought specimen by the above treatment were hardly observed.
加熱処理を行った AZ31展伸材の引張強さは 280MPaであり、破断伸びを 503K 、歪み速度 ΙΟ-2/sで調べたところ 80%を示し、超塑性現象が発現していないことが 確認された。  The tensile strength of the heat-treated AZ31 wrought material was 280 MPa, the elongation at break was measured at 503 K and the strain rate was ΙΟ-2 / s, indicating 80%, confirming that no superplastic phenomenon had occurred. Was done.
[0048] さらに lOmm X IOmm X I . 25mmの組織観察試験片を切り出し、 1%硝酸エタノ ール溶液でエッチングした後、光学顕微鏡で簡易偏光観察を行ったところ、結晶粒 径は約 30 μ mであり、超音波印加前の結晶粒径 150 μ mの 1 5であった。  [0048] Further, a lOmm X IOmm XI. 25mm microstructure observation specimen was cut out, etched with a 1% ethanol nitrate solution, and then subjected to simple polarization observation with an optical microscope. The crystal grain size was found to be about 30μm. And 15 with a crystal grain size of 150 μm before the application of ultrasonic waves.
産業上の利用の可能性 本発明の高強度'超塑性材料の製造方法によれば、金属材料に大きな内部歪みを 与えることが可能であり、金属材料の組織が微細結晶粒からなる高強度 ·超塑性材 料を簡便に得ることができる。 Industrial potential According to the method for producing a high-strength superplastic material of the present invention, a large internal strain can be given to a metal material, and a high-strength superplastic material in which the structure of the metal material is composed of fine crystal grains can be easily obtained. Obtainable.

Claims

請求の範囲 The scope of the claims
[1] 金属材料に超音波を印加した後、該金属材料を絶対温度で表されたその融点に 0.  [1] After applying ultrasonic waves to a metal material, the metal material is brought to a melting point expressed in absolute temperature of 0.1%.
35乃至 0. 6を乗じた温度で加熱処理することを特徴とする高強度 ·超塑性材料の製 造方法。  A method for producing a high-strength superplastic material, comprising performing heat treatment at a temperature multiplied by 35 to 0.6.
[2] 金属材料が固有減衰能 10%以上の高減衰金属材料であることを特徴とする請求項 [2] The metal material is a high-damping metal material having a specific damping capacity of 10% or more.
1記載の高強度'超塑性材料の製造方法。 1. The method for producing a high-strength superplastic material according to 1.
[3] 固有減衰能 10%以上の高減衰金属材料が、 Mgまたは Mg合金であることを特徴と する請求項 2記載の高強度'超塑性材料の製造方法。 3. The method for producing a high-strength superplastic material according to claim 2, wherein the high-damping metal material having an intrinsic damping capacity of 10% or more is Mg or an Mg alloy.
[4] 絶対温度で表された融点に 0. 35乃至 0. 6を乗じた温度が、その金属材料の再結晶 温度であることを特徴とする請求項 1、 2または 3記載の高強度'超塑性材料の製造 方法。 [4] The high strength according to claim 1, 2, or 3, wherein the temperature obtained by multiplying the melting point expressed in absolute temperature by 0.35 to 0.6 is the recrystallization temperature of the metal material. Manufacturing method of superplastic material.
PCT/JP2004/007370 2003-05-30 2004-05-28 Method for producing high strength ultra plastic material WO2004106577A1 (en)

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AU2004243728A AU2004243728A1 (en) 2003-05-30 2004-05-28 Method for producing high strength ultra plastic material
GB0521161A GB2414952B (en) 2003-05-30 2004-05-28 Method for producing high strength superplastic material
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JP2007169675A (en) * 2005-12-19 2007-07-05 Furukawa Co Ltd Method for producing superplastic magnesium alloy material

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DE102007009996B4 (en) * 2007-03-01 2014-03-27 Minebea Co., Ltd. electric motor
CN102220527B (en) * 2011-05-27 2012-09-12 重庆大学 Method for improving damping performance of extruded Mg-Cu-Mn series alloy
US9458534B2 (en) 2013-10-22 2016-10-04 Mo-How Herman Shen High strain damping method including a face-centered cubic ferromagnetic damping coating, and components having same
US10023951B2 (en) 2013-10-22 2018-07-17 Mo-How Herman Shen Damping method including a face-centered cubic ferromagnetic damping material, and components having same

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