EP2995694A1 - MATÉRIAU DE BARRE ET MATÉRIAU DE PLAQUE À BASE DE Cu-Al-Mn PRÉSENTANT UNE SUPERÉLASTICITÉ STABLE, PROCÉDÉ DE FABRICATION DESDITS MATÉRIAU DE BARRE ET MATÉRIAU DE PLAQUE, ÉLÉMENT DE CONTRÔLE SISMIQUE DANS LEQUEL LESDITS MATÉRIAU DE BARRE ET MATÉRIAU DE PLAQUE SONT UTILISÉS, ET STRUCTURE DE CONTRÔLE SISMIQUE DANS LAQUELLE LEDIT ÉLÉMENT DE CONTRÔLE SISMIQUE EST UTILISÉ - Google Patents

MATÉRIAU DE BARRE ET MATÉRIAU DE PLAQUE À BASE DE Cu-Al-Mn PRÉSENTANT UNE SUPERÉLASTICITÉ STABLE, PROCÉDÉ DE FABRICATION DESDITS MATÉRIAU DE BARRE ET MATÉRIAU DE PLAQUE, ÉLÉMENT DE CONTRÔLE SISMIQUE DANS LEQUEL LESDITS MATÉRIAU DE BARRE ET MATÉRIAU DE PLAQUE SONT UTILISÉS, ET STRUCTURE DE CONTRÔLE SISMIQUE DANS LAQUELLE LEDIT ÉLÉMENT DE CONTRÔLE SISMIQUE EST UTILISÉ Download PDF

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Publication number
EP2995694A1
EP2995694A1 EP14794166.0A EP14794166A EP2995694A1 EP 2995694 A1 EP2995694 A1 EP 2995694A1 EP 14794166 A EP14794166 A EP 14794166A EP 2995694 A1 EP2995694 A1 EP 2995694A1
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Prior art keywords
temperature
rod
heating
mass
carried out
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EP14794166.0A
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German (de)
English (en)
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EP2995694A4 (fr
Inventor
Toshihiro Omori
Tomoe Kusama
Ryosuke Kainuma
Kiyohito Ishida
Toyonobu Tanaka
Sumio KISE
Kenji Nakamizo
Koji Ishikawa
Misato FUJII
Satoshi Teshigawara
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Tohoku University NUC
Furukawa Electric Co Ltd
Furukawa Techno Material Co Ltd
Original Assignee
Tohoku University NUC
Furukawa Electric Co Ltd
Furukawa Techno Material Co Ltd
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Publication of EP2995694A1 publication Critical patent/EP2995694A1/fr
Publication of EP2995694A4 publication Critical patent/EP2995694A4/fr
Withdrawn legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/006—Resulting in heat recoverable alloys with a memory effect
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
    • B22D21/02—Casting exceedingly oxidisable non-ferrous metals, e.g. in inert atmosphere
    • B22D21/025—Casting heavy metals with high melting point, i.e. 1000 - 1600 degrees C, e.g. Co 1490 degrees C, Ni 1450 degrees C, Mn 1240 degrees C, Cu 1083 degrees C
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • C22C9/01—Alloys based on copper with aluminium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • C22C9/05—Alloys based on copper with manganese as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • 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
    • C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon

Definitions

  • the present invention relates to a Cu-Al-Mn-based alloy rod and sheet exhibiting excellent stable superelastic characteristics, a method of producing the same, a vibration damping material, and a vibration damping structure constructed by using the vibration damping material.
  • Shape memory alloys/superelastic alloys exhibit a remarkable shape memory effect and superelastic characteristics concomitantly to reverse transformation of the thermoelastic martensite transformation, and have excellent functions near the living environment temperature. Accordingly, these alloys have been put to practical use in various fields.
  • Representative alloys of the shape memory alloys/superelastic alloys include TiNi alloys and Cu-based alloys. Copper-based shape memory alloys/superelastic alloys (hereinafter, those are simply referred to copper-based alloys) have characteristics inferior to those of TiNi alloys in terms of repetition characteristics, corrosion resistance, and the like. On the other hand, since the cost is inexpensive, there has been a movement to extend the application range of copper-based alloys.
  • Cu-Al-Mn-Ni alloys are controlled to be ultrafine crystalline grain microstructure of 10 ⁇ m or less. Further, Cu-Al-Mn-Ni alloys described in Patent Literature 1 contain Ni necessarily, and Ni content up to 10 mass% is allowed to be contained. By including Ni, even though crystals are refined, a vibration damping performance is exhibited. Therefore, the crystalline orientation of a ⁇ single phase (austenitic single phase) is easily controlled. However, a quenching property is reduced.
  • the quenching property indicates the relationship between the cooling speed in the quenching and the stability of microstructure in the quenching just before the quenching.
  • the shape memory characteristics and superelastic characteristics to be manifested by those alloys are less stable, and, from the viewpoint that these characteristics are not stable, the copper-based alloys are at a level having a room for further improvement.
  • Patent Literature 2 in order to improve the shape memory characteristics and superelastic characteristics of the copper-based alloys, there have been proposed that the crystalline orientations of a ⁇ single phase are controlled; in the case of a rod, the average grain size is to be the half of the rod diameter or more or in the case of a sheet, it is to be the sheet thickness or more; and also, the region having the grain diameter is to be 30% or more of the total length of the rod or the total region of the sheet.
  • Patent Literature 3 in order to improve the shape memory characteristics of the copper-based alloys and also to make the copper-based alloys to have a large cross sectional size that can be applied for a structure, there has been proposed a large crystalline microstructure, in which the maximum grain size is larger than 8 mm.
  • the grain size distribution of the grains having a predetermined large grain diameter in the Cu-AI-Mn-based alloys is still controlled insufficiently, and shape memory characteristics and superelastic characteristics are still yet insufficiently stable.
  • the present invention is implemented for providing a Cu-Al-Mn-based alloy rod and sheet which stably exhibits satisfactory superelastic characteristics; for providing a method of producing the same; for providing a vibration damping material using the same; and for providing a vibration damping structure constructed by using the vibration damping material.
  • the inventors of the present invention conducted a thorough investigation in order to solve the problems of the related art as described above. As a result, the inventors found that, in Cu-Al-Mn-based copper alloys having a coarse crystalline grain microstructure that is close to so-called bamboo microstructure (which is a metal microstructure having a crystalline structure, in which a grain boundary is situated like bamboo joints), with most of the regions thereof being configured by large grains in a predetermined size or more, and the area ratio of the large grains in the predetermined size or more and the average grain size of the large grains in the predetermined size or more being controlled in the proper range, respectively, Cu-Al-Mn-based alloys which stably exhibit satisfactory superelastic characteristics can be obtained. The inventors also found that the controlling of the grain size distribution and average grain size could be obtained by performing the memory heat treatment at the memory heating conditions by a specific slow-lowering speed or raising speed in temperature. The present invention was completed based on these findings.
  • the present invention provides the following means:
  • the Cu-Al-Mn-based alloy rod and sheet of the present invention is preferably such that, as the superelastic characteristics, the residual strain after 6% strain loading is 1.0% or less, and the elongation at breakage is 6% or more.
  • the expression 'having a recrystallized microstructure substantially formed from a ⁇ single phase' means that the proportion occupied by the ⁇ phase in the recrystallization structure is generally 90% or more, and preferably 95% or more.
  • the Cu-Al-Mn-based superelastic alloy rod and sheet of the present invention can be used in various applications where superelastic characteristic are required, and applications are expected, for example, in antennas of mobile phones, spectacle frames, as well as orthodontic wires, guide wires, stents, correcting tools for ingrown nails, and orthoses for hallux valgus, as medical products.
  • the Cu-Al-Mn-based superelastic alloy rod and sheet of the present invention is suitable as a vibration damping material, such as a bus bar, due to its excellent superelastic characteristics.
  • a vibration damping structure may be constructed by using such a vibration damping material.
  • the cooling and heating in the memory heat treatment (also called a shape memory heat treatment) before the quenching are carried out at the predetermined slow temperature lowering and slow temperature raising, respectively, and thus, the grains thereof are sufficiently grown to the predetermined large size, and also, the grain size distribution thereof can be properly controlled. As a result, satisfactory superelastic characteristic can be stably exhibited.
  • the rod and sheet of the present invention a small amount of the grains having a small grain size may be present, but the most grains have a large grain size.
  • the region, in which the grain size of the respective grains is the radius of the rod or more, is 90% or more of the longitudinal direction cross section at any locations of the rod, and the average grain size of the grains, in which the grain size is the radius of the rod or more, is 80% or more of the diameter of the rod. It is preferable that the average grain size is the diameter of the rod or more.
  • the region, in which the grain size of the respective grains is the half of the sheet thickness or more, is 90% or more of the cross section of the sheet thickness direction and the longitudinal direction at any locations of the sheet, and the average grain size of the grains, in which the grain size is the half of the sheet thickness or more, is 80% or more of the sheet thickness. It is preferable that the average grain size is the sheet thickness or more.
  • the present ratio of the large grains in the predetermined range is expressed, it is defined as the area ratio, in which the grains in the predetermined size or more occupy the rod or sheet. Further, by defining the average grain size of the grains in the predetermined size or more, the structural characteristics are defined.
  • the shape of the sheet is not a round-shaped cross section, and thus, has a low symmetric property.
  • the standard of the grain size is a sheet thickness, not a sheet width. The reason is based on the fact that, after the grains penetrate through the sheet thickness or sheet width, the driving force of the growth of the grain boundary interface by the grains is lowered, and thus, the grains are increased in their sizes, but it is difficult to penetrate through the sheet width as well as the sheet thickness.
  • the average grain size of the matrix (the base material) is to be the proper size. This is because in the Cu-Al-Mn-based alloys, when the average grain size is too small, the restriction between the grains is generated from the surrounding grains at the time of being deformed, and thus, the resistance to the deformation becomes larger, thereby deteriorating the superelastic characteristics.
  • the upper limit of the average grain size is not particularly limited, and for example, there are particularly no problems as long as the upper limit is practically obtained (for example, about 150 mm).
  • the region, in which the grain size of the respective grains is the radius of the rod or more, is 90% or more of the longitudinal direction cross section at any locations of the rod or "the region, in which the grain size of the respective grains is the half of the sheet thickness or more, is 90% or more of the cross section of the sheet thickness direction and the longitudinal direction at any locations of the sheet”
  • the grain size distribution is defined by the respective area ratio.
  • the rod and sheet are defined as different product inventions.
  • the rod and sheet are different each other in that the grain size is defined to the diameter of the rod or the grain size is defined to the sheet thickness, but the special technical features of both inventions are common, and thus, both the inventions have the common technical significance (features).
  • the inventions of the method of producing a rod and the method of producing a sheet the same can be said to the product inventions. Therefore, it can be interpreted that both the inventions have the common technical significance.
  • the grains in the predetermined grain size distribution and the predetermined size or more have the average grain size in the predetermined size or more. This is because the effect of the grains each having the size that is considered less than the predetermined size may be ignored, since the grain size of the grains each having the size that is the predetermined size or more is defined, the amount of the grains each having the size that is less than the predetermined size is conspicuously low as compared to the grains each having the size that is the predetermined size or more, and the effect to the superelastic characteristics is small.
  • the Cu-Al-Mn-based alloy rod and sheet of the present invention is substantially composed of a ⁇ single phase.
  • the expression 'being substantially composed of a ⁇ single phase' means that the existence ratio of a phase other than the ⁇ phase, for example, an ⁇ phase, is generally 10% or less, and preferably 5% or less.
  • a Cu-8.1 mass% Al-11.1 mass% Mn alloy is a ⁇ (BCC) single phase at 900°C, but is the two phases of an ⁇ (FCC) phase + the ⁇ phase at 700°C or less.
  • a production process such as described below may be mentioned, in connection with the production conditions for obtaining the superelastic alloy rod and sheet which stably exhibit satisfactory superelastic characteristics such as described above. Further, a preferred example of the production process is illustrated in Figs. 2-1 and 2-2 .
  • the treatment temperatures and treatment times (maintaining time periods) in the heat treatments illustrated in the figures, and the working ratio in the cold-working are representatively represented as the values utilized in the Examples, but the present invention is not limited thereto.
  • the grains can be sufficiently grown to the predetermined large sizes, and also, by controlling properly the grain size distribution thereof, a Cu-Al-Mn-based alloy is obtained, which stably exhibits satisfactory superelastic characteristics.
  • the intermediate annealing at 400 to 600°C for 1 to 120 minutes and the cold-working in which the working ratio of the cold-rolling or cold-drawing is in the range of 30% or more, may be repeatedly performed at least each one time after the hot working and before the memory heat treatment.
  • the intermediate annealing is only performed at 400 to 600°C for 1 to 120 minutes, and after the intermediate annealing, the memory heat treatment may be performed without performing the cold working.
  • the heating may be performed to raise the temperature to the temperature range of the transformation temperature or more in the ⁇ phase, in which the ⁇ + ⁇ phase is first changed to the ⁇ phase, and such a heating temperature is maintained for 1 to 120 minutes.
  • the heating to the temperature range of the transformation temperature or more, in which the initial ⁇ + ⁇ phase is changed into the ⁇ phase at the time of memory heat treatment is performed from a room temperature after cooling the temperature to a room temperature in general.
  • the heating may be performed, just after the hot working without cooling the temperate to the room temperate after the hot working, or the heating may be performed, in the cooling process after the hot working.
  • the transformation temperature from the ⁇ + ⁇ phase to the ⁇ phase is the boundary temperature between the ⁇ + ⁇ phase and the ⁇ phase in the phase diagram as illustrated in Fig. 4 .
  • a temperature is determined, for example, by measuring the caloric change at the time of heating the materials from a low temperature to a high temperature by a differential scanning calorimetry (DSC) measuring device, and the like. Then, the heat treatment cycle, in which the temperature is lowered by the cooling to be the temperature range that is less than the transformation temperature, and then, immediately, the temperature is raised by the heating to be the temperature range that is to be the ⁇ phase, is repeated at least one time, such that the ⁇ phase becomes the ⁇ + ⁇ phase.
  • DSC differential scanning calorimetry
  • the heating temperature is preferably higher than the transformation temperature by 50°C or more. Further, in the case where the temperature is lowered by the cooling to be the temperature range that is less than the transformation temperature for the ⁇ + ⁇ phase, the temperature is preferably lower than the transformation temperature by 50°C or less.
  • the temperature lowering speed at the time of cooling to less than the transformation temperature (the cooling of [Step 3-2]), and the temperature raising speed at the time of heating to the transformation temperature or more (the heating of [Step 3-3]) are preferably slow as described below. Then, finally, the solid-solution treatment including the quenching (the quenching of [Step 3-4]) is performed.
  • the temperature lowering speed (the temperature lowering speed at the cooling of [Step 3-2]) and the temperature raising speed (the temperature raising speed at the heating of [Step 3-3]) are both set to be slow (in this specification, called a temperature slow-lowering speed and a temperature slow-raising speed).
  • the temperature lowering speed at the time of the temperature slow-lowering and the temperature raising speed at the time of the temperature slow-raising each are generally 0.1 to 100°C/minutes, preferably 0.1 to 10°C/minutes, more preferably 0.1 to 3°C/minutes, and particularly preferably 0.2 to 1°C/minutes.
  • the quenching is performed.
  • a quenching may be performed by the water-cooling, in which the Cu-Al-Mn-based alloys subjected to the heat treatment are put into the cooling water.
  • the production process such as follows may be mentioned.
  • the memory heat treatment [Step 3] is carried out in this order. Then, after the memory heat treatment [Step 3], aging-heating [Step 4] may be carried out.
  • the melting and casting [Step 1] and the hot working [Step 2] are carried out; then, the intermediate annealing [Step 2-1] and cold-working [Step 2-2] are carried out each at least one time; and then, the memory heat treatment [Step 3] is carried out, in this order.
  • the memory heat treatment [Step 3] the aging-heating [4] may be carried out.
  • the melting and casting [Step 1] and the hot working [Step 2] are carried out; then, the intermediate annealing [Step 2-1] is carried out; and then, the memory heat treatment [Step 3] is carried out, in this order.
  • the memory heat treatment [Step 3] the aging-heating [4] may be carried out.
  • the memory heat treatment [Step 3] contains the steps of: heating by the temperature range to be the ⁇ phase; maintaining such a heating temperature for 1 to 120 minutes; temperature-raising treatment [Step 3-1] for making such a heating temperature to be the ⁇ single phase temperature range, for example, 700 to 950°C (preferably, 800 to 920°C); temperature-lowering treatment [Step 3-2] for cooling the temperature from such a heating temperature to the temperature range to be the ⁇ + ⁇ phase at the temperature-lowering speed, for example, 300 to 700°C (preferably, 400 to 550°C); temperature-raising treatment [Step 3-3] for heating the temperature from such a temperature-lowering temperature to the temperature range to be the ⁇ phase at the temperature-raising speed, and maintaining such a heating temperature for certain time periods (preferably, 1 to 120 minutes); and then quenching [Step 3-4], for example, by cold water.
  • temperature-raising treatment [Step 3-1] for making such a heating temperature to be the ⁇ single phase temperature range, for example, 700 to 950
  • the temperature-raising speed is not particularly limited, but the temperature-raising speed in the temperature-raising treatment [Step 3-3] may be used or a faster speed than the above speed may be used.
  • the heating maintaining time at the ⁇ phase in the temperature-raising treatment [Step 3-1] is less than 1 minute, the heating is insufficient, and when it exceeds 120 minutes, the heating is already sufficient, and even if maintaining over the time, there are no newly improvement and also a waste of thermal energy. Therefore, the heating maintaining time at the ⁇ phase in the temperature-raising treatment [Step 3-1] is set to be 1 to 120 minutes.
  • the heat treatment cycle including the temperature-lowering treatment [Step 3-2] and the temperature-raising treatment [Step 3-3] may be repeatedly carried out each at least one time as described above.
  • the cooling speed at the time of quenching [Step 3-4] is generally 30°C/second or more, preferably 100°C/second or more, and more preferably, 1,000°C/second or more.
  • the intermediate annealing [Step 2-1] and the cold-working [Step 2-2] may be carried out or may not be carried out. Even if any intermediate annealing [Step 2-1] and cold-working [Step 2-2] are to be carried out, they may be carried out each once in this order or may be repeatedly carried out once two times in this order.
  • the cold-working [Step 2-2] may not be carried out, but the intermediate annealing [Step 2-1] may be only carried out.
  • the aging-heating [Step 4] at 80 to 250°C for 5 to 60 minutes may be carried out. Any aging-heating [Step 4] may be preferably carried out.
  • the aging temperature is too low, the ⁇ phase is unstable, and when putting at a room temperature, the martensite transformation temperature may be changed.
  • the aging temperature is too high, the precipitation of ⁇ phase may be carried out, and thus, there may be a trend that the shape memory characteristic and superelastic characteristics are conspicuously lowered.
  • the intermediate annealing [Step 2-1] and cold-rolling or cold-wire-drawing [Step 2-2] may be repeatedly carried out at a plurality of times, and thereby, grain growth may be more stable.
  • the repetition number of intermediate annealings [Step 2-1] and cold-rollings or cold-wire-drawings [Step 2-2] is preferably 2 times or more, and more preferably 3 times or more. This repetition number is not particularly limited in terms of the upper limit, but generally 10 times or less, and preferably 7 times or less.
  • Step 2-1 As the repetition number of intermediate annealings [Step 2-1] and cold-rollings or cold-wire-drawings [Step 2-2] is high, the driving force of the grain growth becomes high, and thus, it is easy to uniformly make the size of the grain coarse.
  • the intermediate annealing [Step 2-1] is preferably carried out at 400 to 600°C for 1 minute to 120 minutes. It is preferable that this intermediate annealing temperature be set to a lower temperature within this range; and the intermediate annealing temperature is more preferably set to 400 to 550°C, further preferably 400 to 500°C, and particularly preferably 400°C to 450°C.
  • the annealing time is more preferably 30 minute to 120 minutes, and even if the influence of the sample size is considered, an annealing time of 60 minutes is sufficient for a round rod with diameter ⁇ 20 mm.
  • Step 2-2 For the cold-rolling or cold-wire-drawing [Step 2-2], it is preferable to carry out the step at a working ratio of 30% or higher, more preferably 40% or higher, further preferably from 45 to 75%, and particularly preferably from 45 to 60%.
  • the Cu-Al-Mn-based alloy rod and sheet of the present invention is formed of a copper alloy which has the ⁇ single phase at a high temperature, and a two-phase microstructure of ⁇ + ⁇ at a low temperature, and is formed of a copper-based alloy containing at least Al and Mn.
  • the Cu-Al-Mn-based alloy that forms the rod and sheet of the present invention has a composition containing 3 to 10 mass% of Al and 5 to 20 mass% of Mn, with the balance being Cu and unavoidable impurities. If the content of elemental Al is too small, the ⁇ single phase cannot be formed, and if the content is too large, the resultant alloy becomes very brittle.
  • the content of elemental Al may vary depending onto the content of elemental Mn, but a preferred content of elemental Al is 6 to 10 mass%.
  • the alloy contains elemental Mn, the range of existence of the ⁇ phase extends to a lower Al-content side, and cold workability is markedly enhanced, for thereby making the form-working readily. If the amount of addition of elemental Mn is too small, satisfactory workability is not obtained, and the region of the ⁇ single phase cannot be formed. Also, if the amount of addition of elemental Mn is too large, sufficient shape recovery characteristics are not obtained.
  • a preferred content of Mn is 8 to 12 mass%.
  • the Cu-Al-Mn alloy having the above-described composition has high hot workability and cold workability, and enables to obtain a working ratio of 20 to 90% or higher in cold working.
  • the alloy can be readily worked by forming into sheets and wires (rods), as well as fine wires, foils, pipes and the like that have been conventionally difficult to produce.
  • the Cu-AI-Mn-based alloy that forms the rod and sheet of the present invention can further contain, as an optionally adding alloying element(s), at least one selected from the group consisting of Co, Fe, Ti, V, Cr, Si, Nb, Mo, W, Sn, Mg, P, Be, Sb, Cd, As, Zr, Zn, and Ag.
  • an optionally adding alloying element(s) at least one selected from the group consisting of Co, Fe, Ti, V, Cr, Si, Nb, Mo, W, Sn, Mg, P, Be, Sb, Cd, As, Zr, Zn, and Ag.
  • These elements enhance the physical strength of the resultant Cu-Al-Mn-based alloy, while maintaining cold workability.
  • the content in total of these elements is preferably 0.001 to 10 mass%, and particularly preferably 0.001 to 5 mass%. If the content of these elements is too large, the martensite transformation temperature is lowered, and the ⁇ single phase microstructure becomes unstable.
  • Co, Fe and Sn are elements that are effective for strengthening of the matrix microstructure. Co makes the grains coarse by forming CoAl; however, Co in an excess amount causes lowering of toughness of the alloy.
  • a preferred content of Co is 0.001 to 2 mass%.
  • a preferred content of Fe is 0.001 to 3 mass%.
  • a preferred content of Sn is 0.001 to 1 mass%.
  • Ti is bonded to N and O, which are inhibitory elements, and forms oxynitride.
  • a preferred content of Ti is 0.001 to 2 mass%.
  • V, Nb, Mo and Zr have an effect of enhancing hardness, and enhance abrasion resistance. Further, since these elements are hardly solid-solubilized into the matrix, the elements precipitate as the ⁇ phase (bcc crystals), for thereby enhancing the physical strength.
  • Preferred contents of V, Nb, Mo and Zr are respectively 0.001 to 1 mass%.
  • Cr is an element effective for retaining abrasion resistance and corrosion resistance.
  • a preferred content of Cr is 0.001 to 2 mass%.
  • Si has an effect of enhancing corrosion resistance.
  • a preferred content of Si is 0.001 to 2 mass%.
  • W is hardly solid-solubilized into the matrix, and thus has an effect of precipitation strengthening.
  • a preferred content of W is 0.001 to 1 mass%.
  • Mg eliminates N and O, which are inhibitory elements, fixes S that is an inhibitory element as sulfide, and has an effect of enhancing hot workability or toughness. Addition of a large amount of Mg brings about grain boundary segregation, and causes embrittlement. A preferred content of Mg is 0.001 to 0.5 mass%.
  • P acts as a de-oxidation agent, and has an effect of enhancing toughness.
  • a preferred content of P is 0.01 to 0.5 mass%.
  • Be, Sb, Cd, and As have an effect of strengthening the matrix microstructure.
  • Preferred contents of Be, Sb, Cd and As are respectively 0.001 to 1 mass%.
  • Zn has an effect of raising the shape memory treatment temperature.
  • a preferred content of Zn is 0.001 to 5 mass%.
  • Ag has an effect of enhancing cold workability.
  • a preferred content of Ag is 0.001 to 2 mass%.
  • the superelastic Cu-Al-Mn-based alloy that forms the rod and sheet of the present invention preferably has a Ni content of 1 mass% or less, and more preferably 0.15 mass% or less, and it is particularly preferable that the alloy does not contain Ni. It is because if the alloy contains Ni in a large amount, but the quench-hardening property previously explained is deteriorated.
  • the superelastic Cu-Al-Mn-based alloy rod and sheet of the present invention has the following physical properties.
  • the residual strain after 6% deformation is generally 1.0% or less, preferably 0.5% or less, and more preferably 0.2% or less.
  • the elongation (elongation at breakage) is generally 6% or more, preferably 8% or more, and more preferably 10% or more.
  • the residual strain as the superelastic characteristics and the elongation have no unevenness in the performance, even if specimens are cut out from at any sites from a same alloy and analyzed.
  • the expression 'having unevenness' means that, in regard to the residual strain and elongation, for example, when three specimens are cut out from a same alloy and analyzed, one or more specimens have a residual strain value of more than 1.0%, or have an elongation value of less than 6%.
  • the diameter thereof is generally 8 mm or more, and for example, 8 mm to 50 mm may also be employed.
  • the diameter of the rod may be the size of 8 mm to 16 mm depending on the use thereof.
  • the sheet may have the thickness of generally 1 mm or more, and for example, 1 mm to 15 mm.
  • the rod of the present invention may have the shape of a tube having a tube wall and a hollow shape.
  • the vibration damping material of the present invention is constituted of the rod or sheet.
  • Examples of the vibration damping material are not particularly limited, but for example, may include brace, fastener, anchor bolt, and the like.
  • the vibration damping structure of the present invention is constructed of the vibration damping material.
  • Examples of the vibration damping structure are not particularly limited, but any kinds of the structures may be used as long as the structures are constructed of using the above-described brace, fastener, anchor bolt, and the like.
  • the copper alloys that give the compositions as indicated in Table 1-1 and Table 1-2, pure copper, pure Mn, pure Al, and materials of other optionally adding alloying elements were subjected respectively to melting in a highfrequency induction furnace.
  • the copper alloys thus melted were cooled, to obtain ingots with diameter of 80 mm ⁇ length of 300 mm.
  • the ingots thus obtained were subjected to hot forging at 800°C, to obtain round rods with diameter 20 mm.
  • the round rods were again subjected to (1) hot forging or (2) cold-wire-drawing, if necessary, to obtain the rods having the diameters as indicated in Table 2-1 and Table 2-2 with the conditions as follows.
  • the rods in Examples and Comparative Examples which have the diameters listed in Table 2-1 and Table 2-2, were prepared by: temperature-raising at the temperature-raising speed of 30°C/minutes to be 900°C (the temperature to the ⁇ single phase); maintaining this temperature for 5 minutes; temperature-lowering at the temperature-lowering speed listed in Table 2-1 and Table 2-2 to be 500°C (the temperature to the ⁇ + ⁇ phase); immediately, temperature-raising at the temperature-raising speed listed in Table 2-1 and Table 2-2 to be 900°C (the temperature to the ⁇ single phase); maintaining this temperature for 1 hour; and finally, quenching from 900°C by cold water cooling.
  • Fig. 2-1 and Fig. 2-2 are charts illustrating the examples of respective process, and the working ratio of cold-working and the numbers of repetition cycles of the cold-workings and intermediate annealings were changed to be as listed in Table 2-1 and Table 2-2, to carry out the respective process.
  • the working ratios in the respective cold workings indicates one time working ratio ⁇ second time working ratio ⁇ third time working ratio ⁇ ... working ratios, in order, from the left side to the right side in the column of "cold-working ratio (%)".
  • the numbers of repetition cycles of the intermediate annealings and cold-workings indicate "the numbers of cycles of cold-workings".
  • the intermediate annealing [Step 2-1] at 500°C for 1 hour was carried out, and then, the respective cold-wire-drawings [Step 2-2] in the numbers of cycles (the numbers of cycles in Tables) of cold-working ratios and cold-workings listed in Table 2-1 and Table 2-2 were carried out. Further, in Fig 2-1 and Fig. 2-2 , the aging-heating [Step 4] was omitted, but was carried out as the following conditions to all Test Examples.
  • Rod specimens thus obtained which were subjected through the working and heat treatment processes, and to final quenching (rapid cooling) by water cooling, thereby for obtaining samples of the ⁇ (BCC) single phase.
  • the respective sample was, then, subjected to age-heating at 200°C for 15 minutes.
  • the rods of Comparative Examples 3 to 8 were obtained in the same manner as in Examples 1 to 23, except for Comparative Examples 4 and 5, in which the productions were stopped due to the forging cracks occurred in the mid way of productions.
  • the rods of Comparative Examples 1 and 2 were obtained in the same manner as in Examples 1 to 23, except that, in the memory heat treatment of Examples 1 to 23, the temperature-lowering step [Step 3-2] ( ⁇ ⁇ ⁇ + ⁇ ) was carried out at the temperature-lowering speed of 150°C/minute of the rapid temperature-lowering (Comparative Example 2) or the temperature-raising step [Step 3-3] ( ⁇ + ⁇ ⁇ ⁇ ) was carried out at the temperature-raising speed of 150°C/minute of the rapid temperature-raising (Comparative Example 1).
  • Comparative Examples 1 and 2 are Test Examples simulating JP-A-2001-20026 (Patent Literature 2) and WO 2011/152009 A1 (Patent Literature 3), respectively.
  • Patent Literature 2 and WO 2011/152009 A1 Patent Literature 3
  • any kinds of reviews are not carried out on the temperature-lowering speed or temperature-raising speed at the time of carrying the memory heat treatment out, and thus, in detail, there are no disclosures in that the tests are carried out using what kinds of the temperature-raising speed or temperature-lowering speed.
  • the tests were carried out at rapid speeds (rapid temperature-raising or rapid temperature-lowering) that is outside of the slow temperature-raising or slow cooling as defined in the present invention.
  • Comparative Examples 7 and 8 were obtained in the same manner as the present invention but using copper alloys containing Ni in the too high contents that were outside of the range defined in the present invention as indicated in Table 1-1. It was confirmed that the Comparative Examples 7 and 8 were poor in quench-hardening sensitivity, and also poor in superelastic characteristics.
  • the stress loading-unloading by a tensile test was carried out, to obtain a stress-strain curve (S-S curve), thereby for obtaining and evaluating a residual deformation and an elongation.
  • S-S curve stress-strain curve
  • the residual strain and elongation were the average value obtained from those three values.
  • the samples were prepared by cutting each of the rods at any locations of longitudinal direction and then cutting the half of the cut rod.
  • the cut length a (mm) was not particularly defined, but was five times or more of the diameter thereof.
  • the cross sections of the samples were polished, and then, etched with aqueous ferric chloride solution, and the microstructures thereof were photographed.
  • the schematic diagram is illustrated in Fig. 1 .
  • S-S curve A stress-strain curve (S-S curve) was determined by performing a tensile test, and the residual strain was determined and evaluated.
  • the cycle of strain loading used herein was as follows: as 0 MPa (strain at zero load) ⁇ 1% ⁇ 0 MPa ⁇ 2% ⁇ 0 MPa ⁇ 3% ⁇ 0 MPa ⁇ 4% ⁇ 0 MPa ⁇ 5% ⁇ 0 MPa ⁇ 6% ⁇ 0 MPa ⁇ 7% ⁇ 0 MPa ⁇ 8% ⁇ 0 MPa, the loading and unloading of the load were repeated by turns alternately, and while the strain at the time of loading was increased from 1% by 1% each, the loading and unloading of eight strain were repeated till adding 8% of the loading strain.
  • a stress-strain curve (S-S curve) was illustrated in Fig. 3a and Fig. 3b .
  • Fig. 3a illustrates the rod of Example (Example 1)
  • Fig. 3b illustrates the rod of Comparative Example (Comparative Example 2), respectively.
  • the elongation at breakage was measured, according to the method defined in JIS H7103.
  • the amount of precipitation of the ⁇ phase obtained when a sample was cooled at a cooling speed of 300°C/sec after heating was evaluated as the volume proportion based on an image analysis of SEM images.
  • Examples 1 to 12 were Test Examples to the alloy compositions, in which essentially adding elements were only contained and their contents (composition ratio) were variously changed.
  • Examples 13 to 15 and 16 to 23 were Test Examples to various alloy compositions, in which optionally adding elements (small amounts of optionally adding elements) were added to the essentially adding elements.
  • Examples 1 to 6 and 24 to 28 were Test Examples, in which the production conditions were variously changed to Examples 7 to 23.
  • the materials (rods), each of which satisfy the grain size distribution of the given large grain size and the average grain size thereof as defined in the present invention can be obtained, by satisfying the given production conditions (for example, the temperature-lowering speed and temperature-raising speed at the time of the memory heat treatment, and the like) as defined in the present invention, and also making the alloy compositions to be in the preferred range of the present invention, regardless of whether the intermediate annealing after hot working or the cold-working thereafter was carried out, or not.
  • the desired excellent superelastic characteristics can be obtained, and also the elongation and quench-hardening sensitivity can become excellent.
  • each of Comparative Examples 3 and 6 satisfied the grain size distribution of the grain of the predetermined large grain size as defined in the present invention and the average grain size thereof, but did not exhibit the desired superelastic characteristics.
  • Comparative Example 4 the content of Al was too large, and for Comparative Example 5, the content of Mn was too small. Thus, with respect to Comparative Examples 4 and 5, the workability was poor, the cracks were occurred in the forging-working, and it was impossible to produce the samples.
  • Ni was contained in the alloy component at a too large content, and thus, they satisfied the grain size distribution of the grain of the predetermined large grain size as defined in the present invention and the average grain size thereof. However, in the microstructures of those materials (rods) of Comparative Examples 7 and 8, it was confirmed that the precipitation of the ⁇ phase was occurred, the quench-hardening sensitivity was poor, and the desired superelastic characteristics was impossible to exhibit.
  • test results were omitted but not shown.
  • the similar results as those Examples can be obtained.
  • Samples (specimens) of sheets were produced under the following conditions.
  • the copper alloys that give the compositions as indicated in Table 1-1 and Table 1-2, pure copper, pure Mn, pure Al, and materials of other optionally adding alloying elements were subjected respectively to melting in a highfrequency induction furnace.
  • the copper alloys thus melted were cooled, to obtain ingots with diameter of 80 mm ⁇ length of 300 mm.
  • the ingots thus obtained were subjected to hot forging at 800°C, to obtain sheets with sheet thickness 15 mm and sheet width 30 mm.
  • the sheets were further subjected to hot rolling, to obtain sheets with sheet thickness of 10 mm, and if necessary, the sheets were subjected to cold rolling, to obtain sheets with the sheet thicknesses as indicated in Table 2-3 and Table 2-4 with the conditions as follows.
  • the sheets in Examples and Comparative Examples which have the sheet thicknesses listed in Table 2-3 and Table 2-4, were prepared by: temperature-raising at the temperature-raising speed of 30°C/minutes to be 900°C (the temperature to the ⁇ single phase); maintaining this temperature for 5 minutes; temperature-lowering at the temperature-lowering speed listed in Table 2-3 and Table 2-4 to be 500°C (the temperature to the ⁇ + ⁇ phase); immediately, temperature-raising at the temperature-raising speed listed in Table 2-3 and Table 2-4 to be 900°C (the temperature to the ⁇ single phase); maintaining this temperature for 1 hour; and finally, quenching from 900°C by cold water cooling.
  • Sheet specimens thus obtained which were subjected through the working and heat treatment processes, and to final quenching (rapid cooling) by water cooling, thereby for obtaining samples of the ⁇ (BCC) single phase.
  • the respective sample was, then, subjected to age-heating at 200°C for 15 minutes.
  • the sheets of Comparative Examples 11 to 16 were obtained in the same manner as in Examples 29 and the like, except for Comparative Examples 12 and 13, in which the productions were stopped due to the forging cracks occurred in the mid way of productions.
  • the sheets of Comparative Examples 9 and 10 were obtained in the same manner as in Examples 29 to 51, except that, in the memory heat treatment of Examples 29 and the like, the temperature-lowering step [Step 3-2] ( ⁇ ⁇ ⁇ + ⁇ ) was carried out at the temperature-lowering speed of 150°C/minute of the rapid temperature-lowering (Comparative Example 10) or the temperature-raising step [Step 3-3] ( ⁇ + ⁇ ⁇ ⁇ ) was carried out at the temperature-raising speed of 150°C/minute of the rapid temperature-raising (Comparative Example 9).
  • Comparative Examples 9 and 10 are Test Examples simulating JP-A-2001-20026 (Patent Literature 2) and WO 2011/152009 A1 (Patent Literature 3), respectively.
  • Patent Literature 2 and WO 2011/152009 A1 Patent Literature 3
  • any kinds of reviews are not carried out on the temperature-lowering speed or temperature-raising speed at the time of carrying the memory heat treatment out, and thus, in detail, there are no disclosures in that the tests are carried out using what kinds of the temperature-raising speed or temperature-lowering speed.
  • the tests were carried out at rapid speeds (rapid temperature-raising or rapid temperature-lowering) that is outside of the slow temperature-raising or slow cooling as defined in the present invention.
  • Comparative Examples 15 and 16 were obtained in the same manner as the present invention but using copper alloys containing Ni in the too high contents that were outside of the range defined in the present invention as indicated in Table 1-1. It was confirmed that the Comparative Examples 15 and 16 were poor in quench-hardening sensitivity, and also poor in superelastic characteristics.
  • the samples were prepared by cutting each of the sheets in the sheet thickness direction at any locations of longitudinal direction and then cutting the half of the cut sheet.
  • the cut length a (mm) was not particularly defined, but five times or more of the sheet width.
  • the cross sections of the samples were polished, and then, etched with aqueous ferric chloride solution, and the microstructures thereof were photographed.
  • the schematic diagram is illustrated in Fig. 1 and the grain size d (mm) is determined in the same manner as in the rod samples.
  • Examples 29 to 40 were Test Examples to the alloy compositions, in which essentially adding elements were only contained and their contents (composition ratio) were variously changed.
  • Examples 41 to 43 and 44 to 51 were Test Examples to various alloy compositions, in which optionally adding elements (small amounts of optionally adding elements) were added to the essentially adding elements.
  • Examples 29 to 34 and 52 to 56 were Test Examples, in which the production conditions were variously changed to Examples 35 to 51.
  • the materials (sheets), each of which satisfy the grain size distribution of the given large grain size and the average grain size thereof as defined in the present invention can be obtained, by satisfying the given production conditions (for example, the temperature-lowering speed and temperature-raising speed at the time of the memory heat treatment, and the like) as defined in the present invention, and also making the alloy compositions to be in the preferred range of the present invention, regardless of whether the intermediate annealing after hot working or the cold-working thereafter was carried out, or not.
  • the desired excellent superelastic characteristics can be obtained, and also the elongation and quench-hardening sensitivity can become excellent.
  • Comparative Examples 9 and 10 since the temperature-raising speed in [Step 3-3] or the temperature-lowering speed in [Step 3-2] in the memory heat treatment was too fast, it was difficult to satisfy the grain size distribution of the grain having the predetermined large grain size as defined in the present invention, and also it was difficult to satisfy the average grain size thereof. Thus, each of Comparative Examples 9 and 10 did not exhibit desired superelastic characteristics, and also, was small in improvement of elongation. For Comparative Example 11, the content of Al was too small, and for Comparative Example 14, the content of Mn was too much.
  • each of Comparative Examples 11 and 14 satisfied the grain size distribution of the grains of the predetermined large grain size as defined in the present invention and the average grain size thereof, but did not exhibit the desired superelastic characteristics.
  • Comparative Example 12 the content of Al was too large, and for Comparative Example 13, the content of Mn was too small. Thus, with respect to Comparative Examples 12 and 13, the workability was poor, the cracks were occurred in the forging-working, and it was impossible to produce the samples.
  • Ni was contained in the alloy component at a too large content, and thus, they satisfied the grain size distribution of the grain of the predetermined large grain size as defined in the present invention and the average grain size thereof. However, in the microstructures of those materials (sheets) of Comparative Examples 15 and 16, it was confirmed that the precipitation of the ⁇ phase was occurred, the quench-hardening sensitivity was poor, and the desired superelastic characteristics was impossible to exhibit.
  • test results were omitted but not shown.
  • the similar results as those Examples can be obtained.

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EP14794166.0A 2013-05-10 2014-04-14 MATÉRIAU DE BARRE ET MATÉRIAU DE PLAQUE À BASE DE Cu-Al-Mn PRÉSENTANT UNE SUPERÉLASTICITÉ STABLE, PROCÉDÉ DE FABRICATION DESDITS MATÉRIAU DE BARRE ET MATÉRIAU DE PLAQUE, ÉLÉMENT DE CONTRÔLE SISMIQUE DANS LEQUEL LESDITS MATÉRIAU DE BARRE ET MATÉRIAU DE PLAQUE SONT UTILISÉS, ET STRUCTURE DE CONTRÔLE SISMIQUE DANS LAQUELLE LEDIT ÉLÉMENT DE CONTRÔLE SISMIQUE EST UTILISÉ Withdrawn EP2995694A4 (fr)

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PCT/JP2014/060586 WO2014181642A1 (fr) 2013-05-10 2014-04-14 MATÉRIAU DE BARRE ET MATÉRIAU DE PLAQUE À BASE DE Cu-Al-Mn PRÉSENTANT UNE SUPERÉLASTICITÉ STABLE, PROCÉDÉ DE FABRICATION DESDITS MATÉRIAU DE BARRE ET MATÉRIAU DE PLAQUE, ÉLÉMENT DE CONTRÔLE SISMIQUE DANS LEQUEL LESDITS MATÉRIAU DE BARRE ET MATÉRIAU DE PLAQUE SONT UTILISÉS, ET STRUCTURE DE CONTRÔLE SISMIQUE DANS LAQUELLE LEDIT ÉLÉMENT DE CONTRÔLE SISMIQUE EST UTILISÉ

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JP5567093B2 (ja) * 2012-09-16 2014-08-06 国立大学法人東北大学 安定した超弾性を示すＣｕ−Ａｌ−Ｍｎ系合金材とその製造方法
CN106460098B (zh) 2014-03-14 2019-01-08 古河电气工业株式会社 Cu-Al-Mn系合金材料及其制造方法、以及使用了该合金材料的棒材或板材
CN105562448B (zh) * 2016-01-11 2019-05-10 中国兵器工业第五九研究所 药型罩细晶材料的低温制备方法
JP6490608B2 (ja) * 2016-02-10 2019-03-27 国立大学法人東北大学 Ｃｕ−Ａｌ−Ｍｎ系合金材の製造方法
CN105690040B (zh) * 2016-04-06 2018-04-03 台州市椒江永固船舶螺旋桨厂 螺旋桨浇注、打磨工艺及其铜合金配方
CN105734337A (zh) * 2016-05-05 2016-07-06 太仓小小精密模具有限公司 一种耐磨型铜合金模具材料
CN106834796A (zh) * 2017-01-25 2017-06-13 广东广信科技有限公司 一种用于配电柜的高强度铜合金材料及其制备方法
CN107123811B (zh) * 2017-04-11 2020-01-10 华南理工大学 双尺度多孔铜铝锰形状记忆合金复合材料及其制备方法与应用
CN108998694A (zh) * 2018-07-06 2018-12-14 武汉理工大学 一种超弹性合金局部增强混凝土抗震柱的制备方法
CN108972862A (zh) * 2018-07-28 2018-12-11 武汉理工大学 一种超弹性合金局部增强抗震自修复混凝土梁的制备方法
JP7103588B2 (ja) * 2019-01-31 2022-07-20 株式会社古河テクノマテリアル ねじ部を有するＣｕ－Ａｌ－Ｍｎ系形状記憶合金成形体及びその製造方法
CN111139373B (zh) * 2020-02-10 2021-11-05 江西理工大学 高强亚稳态弹性铜合金及其制备方法
CN111394611B (zh) * 2020-04-08 2021-07-13 公牛集团股份有限公司 一种耐磨高弹性铜合金插套材料及其制备方法
CN113234957B (zh) * 2021-04-27 2022-04-01 中机智能装备创新研究院(宁波)有限公司 一种铜合金焊丝、制备方法及应用
CN113373342B (zh) * 2021-05-28 2022-07-22 上海理工大学 一种高超弹性CuAlMn形状记忆合金线材的制备方法
CN113846244B (zh) * 2021-09-20 2022-06-21 哈尔滨工程大学 一种CuAlMn形状记忆合金及制备方法
CN113862508B (zh) * 2021-09-29 2022-09-02 哈尔滨工程大学 一种CuAlMnCoNi形状记忆合金及其制备方法
CN114807648B (zh) * 2022-05-27 2023-08-18 天津理工大学 一种高温形状记忆合金及其制备方法

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