EP3363925A1 - Alliage de magnésium ayant un effet super élastique et/ou un effet de mémoire de forme - Google Patents

Alliage de magnésium ayant un effet super élastique et/ou un effet de mémoire de forme Download PDF

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Publication number
EP3363925A1
EP3363925A1 EP16855461.6A EP16855461A EP3363925A1 EP 3363925 A1 EP3363925 A1 EP 3363925A1 EP 16855461 A EP16855461 A EP 16855461A EP 3363925 A1 EP3363925 A1 EP 3363925A1
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Prior art keywords
alloy
superelastic
alloys
effect
less
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German (de)
English (en)
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EP3363925A4 (fr
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Daisuke Ando
Yuji Suto
Yukiko Ogawa
Junichi Koike
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Tohoku University NUC
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Tohoku University NUC
CLINO Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium
    • C22C23/06Alloys based on magnesium with a rare earth metal as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working

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  • the present invention relates to a magnesium alloy (hereinafter, referred to as a Mg alloy) that exhibits superelastic effect and/or shape memory effect.
  • the present invention relates to a Mg alloy containing a certain amount of scandium (Sc).
  • Sc scandium
  • the present application is an application related to Japanese Patent Application No. 2015-201830 , filed at Japanese Patent Office on October 13, 2015, and claims the priority based on the foregoing Japanese Patent Application.
  • the whole of the contents of the following papers of the present inventors are cited: Ando, D., et al., Materials Letters, Vol. 161, p. 5-8 ; Ogawa, Y., et al., Science, 2016, Vol. 353(6297), pp. 368-370 ; Ogawa, Y., et al., Scripta Materialia, doi.org/10.1016/j.scriptamat.2016.09.024 .
  • Mg alloys are the lowest in density and the lightest in weight among the metals used for structural materials. Accordingly, when Mg alloys are used as the structural materials for automobiles, aircraft and the like, the Mg alloys contribute to weight saving and energy saving effect can be expected. Mg alloys are also excellent in recyclability, and have an advantage that Mg alloys can be more easily recycled as compared with plastics. Moreover, Mg alloys are high in specific strength, the resources for Mg alloys are abundant, and thus, a few tens of years have passed since Mg alloys began to be referred to as next-generation structural materials and attract attention. However, widely used Mg alloys have never been developed. As one of the reasons why Mg alloys have not yet been sufficiently practically used although there have been developed Mg alloys light in weight, high in specific rigidity and excellent in shock absorption, insufficient mechanical properties such as poor cold workability, or low strength may be mentioned.
  • Alloys have been developed in which Al is added to Mg in order to increase the strength, but suffer from the drawback that cold workability is poor.
  • examples of typical Mg alloys containing Al as added therein include AZ31 (Al: 3% by mass, Zn: 1% by mass, the balance: Mg), AZ61 (Al: 6% by mass, Zn: 1% by mass, the balance: Mg), AZ91 (Al 9% by mass, Zn 1% by mass, the balance: Mg), AM (Al 6% by mass, Mn: less than 1% by mass, the balance: Mg).
  • AZ31 allows rolled materials highly versatile as structural materials to be easily obtained; however, even rolled materials of AZ31 allow press working only at approximately 250°C, and find difficulty in press working at room temperature. The drawback of being poor in cold workability inhibits the practical use in various applications.
  • Patent Literature 1 Patent Literature 2, Non Patent Literature 3
  • HCP structure HCP structure
  • BCC body-centered cubic
  • Mg-Li alloys are low in hardness and strength, and poor in thermal stability. Therefore, Mg-Li alloys cannot be used as materials requiring strength, such as materials for automobiles or aircraft.
  • Mg-Li alloys are poor in corrosion resistance, and accordingly require surface treatment, and hence the applications of Mg-Li alloys are extremely limited.
  • Mg alloys have no such functionality as the functionality of Ti alloys, and thus the application range of Mg alloys is not widened.
  • Ti alloys have high specific strength, and are excellent in ductility, and in particular, Ti alloys having BCC structure are known to exhibit superelastic effect (Patent Literature 3). It is also known that fundamentally, materials exhibiting superelastic effect due to the martensite transformation caused by loading stress exhibit shape memory effect depending on the transformation temperature in the state free from loading of stress. By utilizing these properties, Ti alloys are increasingly applied to accessories such as frames of spectacles, and to medical fields involving stents, catheters and guide wires.
  • the superelastic effect means a property getting back to the original shape immediately after the removal of stress even when a large deformation strain is applied.
  • the shape memory effect means a property of an object getting back to the original memorized shape when the temperature is equal to or higher than a certain temperature even when the object is deformed by an external force.
  • As a shape memory alloy having superelastic effect there have been developed alloys having various metals as bases such as Ni-Ti, Cu-Al-Ni, Cu-Zn, Cu-Zn-Al, Cu-Al-Mn, Ti-Nb-Al, and Ni-Al.
  • a Mg alloy mainly composed of Mg, containing as an alloy element at least one element selected from Sc, Y, La, Ce, Pr and the like, and having a unidirectional crystal structure has a pseudoelasticity (Patent Literature 4).
  • Patent Literature 4 As a mechanism allowing a Mg alloy to have a pseudoelasticity, there has been disclosed a mechanism in which the addition of Sc, Y, La, Ce, Pr or the like suppresses the bottom plane sliding of the hexagonal crystal of Mg, and promotes the generation of twin crystals.
  • Patent Literature 4 discloses, as an Example, a Mg alloy including 1.0 to 1.7 at% of Y as added therein; the pseudoelasticity in the case of including other elements is not disclosed, but it is recognized that the content of the element component to be added to the matrix phase is assumed to fall within a range of 1.0 to 6.0 at%.
  • the pseudoelasticity originating from the reversible change of the twin crystals a plenty of residual strain is found, and a nearly perfect shape recovery as high as 90% or more cannot be expected.
  • it is necessary to prepare a single crystal and thus, the practical use of such a Mg alloy is limited.
  • the present inventors have made a study while focusing attention on the crystal structure of Mg alloys.
  • the present inventors have considered that Mg alloys are poor in cold workability because of taking HCP structure high in anisotropy, and accordingly have searched Mg alloys having BCC structure.
  • the Mg-Sc alloy including Sc as added therein has been anticipated to have a BCC structure at a high Mg concentration.
  • the present inventors have already produced Mg alloys including Sc as added therein, and have analyzed and reported the possibility of the two-phase microstructure control, the relation with mechanical properties, and moreover, the crystal orientation (Non Patent Literature 4 to Non Patent Literature 8).
  • Non Patent Literature 4 restriction to the two phases, namely, the BCC phase and the HCP phase, allows the achievement of high strength to be performed.
  • the present inventors have found that an aging treatment at a temperature of 175°C to 400°C produces fine HCP structure deposits in the BCC phase, and consequently the Mg alloy is hardened (Non Patent Literature 5, 6).
  • An object of the present invention is to provide a Mg alloy having superelastic effect and/or shape memory effect, and being excellent in cold workability.
  • the present inventors made a diligent study, and consequently have discovered that a Mg-Sc alloy having a BCC structure having a specific composition range exhibits superelastic effect concomitantly with stress-induced transformation. Moreover, the present inventors have discovered that the foregoing Mg-Sc alloy has shape memory effect (Non Patent Literature 9 and Non Patent Literature 10).
  • the present invention relates to the following alloy in which a certain amount of Sc is added to Mg, and a method for producing the same.
  • the Mg alloy of the present invention is excellent in cold workability, and also exhibits a superelastic effect and a shape memory effect. Accordingly, applications in various fields can be expected for the Mg alloy of the present invention.
  • Mg dissolves in living organisms, accordingly when Mg is used for medical materials such as stents to be left in living organisms, such materials are not required to be exenterated from patients, and therefore burdens to patients can be reduced in an extremely useful manner.
  • Mg alloys are light in weight and high in specific strength, Mg alloys are excellent in cold workability, and therefore, Mg alloys can be expected to be applied to various structural materials in the aerospace field, the automobile field and the like.
  • the Mg alloy of the present invention includes Sc within the range of more than 13 at% and 30 at% or less.
  • the addition content of Sc is 13 at% or less, the BCC phase is not obtained, and the superelastic effect and the shape memory effect cannot be obtained.
  • the addition content of Sc is 30 at% or more, the alloy is poor in ductility and undergoes grain boundary fracture.
  • the Mg alloy of the present invention may include, if necessary, at least one or more additive elements selected from the group consisting of Li, Al, Zn, Y, Ag, In, Sn and Bi, in a total content of 0.001 to 9 at% in relation to the amount of the whole alloy defined to be 100 at%.
  • additive elements selected from the group consisting of Li, Al, Zn, Y, Ag, In, Sn and Bi, in a total content of 0.001 to 9 at% in relation to the amount of the whole alloy defined to be 100 at%.
  • the inclusion of these elements allows the further improvement of the superelastic effect and the regulation of the mechanical strength to be expected.
  • the content of the additive element(s) exceeds 9 at%, the alloy is embrittled, and is hence liable to be poor in workability.
  • the content of the additive element(s) is less than 0.001 at%, no effect can be expected.
  • Li is an element stabilizing the BCC structure, and is regarded as effective in the improvement of the workability.
  • At least one or more elements selected from the group consisting of Ca, Mn, Zr, and Ce, refining the crystal microstructure without impairing the superelastic effect may also be added.
  • These elements are known to be able to achieve high strength and high ductility by refining the crystal grains, and accordingly a high strength and a high ductility of the Mg alloy can be expected to be achieved (Non Patent Literature 11).
  • These additive elements can be included in a content of 0.01 to 2 at% in relation to the amount of the whole alloy defined to be 100 at%. When the content of the additive element(s) exceeds 2 at%, embrittlement is liable to occur. When the content of the additive element(s) is less than 0.01 at%, the effects of the high strength and the high ductility cannot be expected.
  • an alloy of the present invention is described.
  • a predetermined amount of each of the foregoing elements is added, and the resulting mixture is melted in an inert gas atmosphere.
  • high frequency heating melting is preferable.
  • the molten alloy is turned into a molten ingot, and the ingot is subjected to hot rolling and cold rolling to be processed into a predetermined shape.
  • a solution treatment is performed in which the Mg alloy processed into a predetermined shape is heated to a solution treatment temperature range, to transform the crystal microstructure into the BCC phase, and then rapidly cooled.
  • the solution treatment is performed at a temperature of 500°C or higher.
  • the solution treatment temperature is varied depending on the composition of the sample; in general, with the increase of the Sc content, the temperature can be decreased. In an alloy having a relatively larger Sc content, a perfect solution treatment is possible at a temperature of approximately 500°C; however, in an alloy having a lower Sc content, the solution treatment is required to be performed at a higher temperature.
  • the treatment temperature is preferably 550°C or higher and 800°C or lower.
  • a temperature of 550°C or lower alloys lower in the Sc content sometimes undergo formation of a large amount of the HCP phase to fail in obtaining the superelastic effect.
  • the material starts to melt.
  • the retention time at the treatment temperature may be 1 minute or more; however, when the retention time exceeds 24 hours, the effect of oxidation cannot be ignored. Accordingly, the retention time at the treatment temperature preferably falls within a range from 1 minute to 24 hours.
  • the cooling rate is preferably 1000°C/min or more.
  • the aging treatment temperature is preferably 100°C or higher and 400°C or lower.
  • Mg alloys were produced by mixing Sc alone in Mg (Examples 1 to 6), and by further mixing Li, Al, Zn, Y, Ag, In, Sn, and Bi (Examples 7 to 16).
  • each of the ingots was hot rolled at a temperature of 600°C to a thickness of approximately 2 mm, and then cold rolled to a thickness of approximately 0.7 mm at a temperature of 600°C, while annealing was being repeated.
  • the obtained sample was subjected to a solution treatment at a temperature of 500°C to 700°C for 30 minutes, and then rapidly cooled at a rate of 1000°C/min or more to prepare a Mg alloy sample.
  • the solution treatment temperature is verified by investigating the temperature allowing the BCC phase to be obtained as a single phase by using an optical microscope.
  • the alloys of Comparative Examples 1 to 4 were prepared as follows. The materials were weighed out according to the compositions shown in Table 1, and were melted by using a high frequency melting furnace in the same manner as in Examples. Next, in each of Comparative Examples 1 and 2, the ingot was hot rolled to a thickness of approximately 2 mm at a temperature of 600°C, and then cold rolled to a thickness of approximately 0.7 mm at a temperature of 600°C, while annealing was being repeated. On the other hand, in each of Comparative Examples 3 and 4, the ingot was hot rolled to a thickness of approximately 2 mm at a temperature of 300°C, and cold rolled to a thickness of approximately 0.7 mm at a temperature of 300°C while annealing was being repeated.
  • the obtained samples were heat treated at a temperature of 300°C for 30 minutes, and then rapidly cooled at a rate of 1000°C/min or more to prepare Mg alloy samples.
  • the hot rolling temperatures and the subsequent heat treatment temperatures of the samples are different from each other because the melting temperatures are different depending on the compositions of the samples.
  • specimens were prepared with the alloys, and measurements were performed to determine whether or not the superelasticity was exhibited.
  • Each of the specimens was subjected to mechanical surface polishing so as to have a final thickness of 0.5 mm.
  • the size of each of the specimens was set to be 3.5 mm in width, 0.5 mm in thickness, and 10 mm in gauge length; a test was performed at a test temperature of -150°C, and at a tensile rate of 0.5 mm/min. After loading a 4% pre-strain, the stress was unloaded, and thus the superelastic shape recovery rate of the given strain was determined.
  • the superelastic shape recovery rate was defined as the shape recovery magnitude due to the superelasticity after the unloading of the load of the 4% tensile strain, and was evaluated on the basis of the following formula:
  • Superelastic shape recovery rate % ⁇ SE / ⁇ t ⁇ 100
  • the stress-strain curve obtained in the sample of Example 1 is shown in Figure 1 .
  • a stress is applied, first an elastic strain proportional to the stress is generated.
  • the yield point around 1% strain in Figure 1
  • subsequently strain is generated without largely increasing the stress.
  • Figure 1 by unloading the stress after loading of the 4% pre-strain, the sample of Example 1 manifested an excellent superelastic effect such that the given strain was restored to a nearly original state.
  • Example 5 in which Sc was added in a content of 26.5 at% is compared with Example 6 in which Sc was added in a content of 29.5 at%, it is found that Example 5 smaller in the Sc content was higher in the superelastic shape recovery rate.
  • Sc is added alone, it is understood that a high superelastic shape recovery rate can be obtained with a peak around the addition amount of Sc of 26.5 at%.
  • Li contributes to the workability improvement
  • Al, Zn, Y, Ag, In and Sn contribute to the strength improvement through solid-solution hardening or precipitation hardening
  • the addition of these additive elements allows the improvement of the mechanical properties other than the improvement of the superelastic effect to be expected. Accordingly, the addition of a plurality of additive elements allows the improvement of different mechanical properties other than the superelastic effect to be expected.
  • At least one or more additive elements selected from the group consisting of Ca, Mn, Zr, and Ce may be added.
  • the addition of Ca, Mn, Zr and Ce refines the crystal microstructure, and accordingly allows the strength improvement and the workability improvement to be expected.
  • Example 1 The Mg alloy sample of Example 1 was subjected to a tensile cycle test, and the obtained maximum superelastic strain magnitude was evaluated.
  • the tensile cycle test gives the results of the superelastic recovery strain magnitude ( ⁇ SE ) measured while the tensile load strain magnitude ( ⁇ t ) is being gradually increased.
  • Figure 2A shows the stress-strain cycle test chart.
  • ⁇ y denotes the yield stress
  • ⁇ t i denotes the tensile load strain magnitude in the cycle i
  • ⁇ e i denotes the pure elastic recovery strain magnitude in the cycle i
  • ⁇ SE i denotes the superelastic recovery strain magnitude in the cycle i
  • ⁇ r i denotes the residual strain magnitude in the cycle i.
  • the alloy sample is loaded with a tensile force up to a strain magnitude of 1%, and then unloaded.
  • the alloy sample is loaded with a tensile force up to a strain magnitude of 2%, and then unloaded. While this operation was repeated to the eighth cycle, the stress was measured.
  • Figure 2B shows the relation between the tensile load strain magnitude and the superelastic recovery strain magnitude, obtained from the measurement results of the tensile cycle test, and the maximum pure elastic recovery strain magnitude of the Mg alloy of Example 1 was 4.4%.
  • the Mg alloys of other Examples also exhibited equivalent maximum pure elastic recover strain magnitudes.
  • the present inventors have already revealed that some Mg-Sc alloys are provided with the BCC structure, and in addition, in order to elucidate the relation between the Mg alloys exhibiting the superelasticity and the BCC structure, an crystal structure analysis was performed on the basis of X-ray diffraction.
  • the specimens of the alloys of Examples 1, 4, 6, and Comparative Example 3 were prepared by performing solution treatment by heat treatment and performing rapid cooling in the same manner as described above. Each of the specimens was set to have a size of 10 mm ⁇ 20 mm ⁇ 0.7 mm, and the surface of the specimen was mirror-finished by physical polishing.
  • the prepared specimens were subjected to X-ray diffraction. An X-ray diffractometer, Ultima, manufactured by Rigaku Corporation was used, the ⁇ /2 ⁇ method was adopted and Cu K- ⁇ was used as an X-ray source. The results thus obtained are shown in Figure 3 . Herein, the ordinate is given in logarithmic scale.
  • Example 1 the peaks (marked with ⁇ in the chart) indicating the BCC phases are large in strength, showing that substantially the BCC phases are present as single phases. It is to be noted that in Example 1, the peaks (marked with ⁇ in the chart) indicating the HCP phase were observed to some extent, but these were produced during rapid cooling after heat treatment, and the fraction of the HCP phase was 10% or less. On the other hand, in Comparative Example 3, strong peaks of the HCP phase were observed, showing that the HCP phase is present as a single phase. From these results, it has been shown that the presence of the BCC phase is important for exhibiting the superelasticity.
  • FIG. 4 shows the results of an X-ray diffraction of the sample of Example 1 performed at -150°C while a stress was being loaded on the sample of Example 1.
  • Example 1 in the state of being free from stress loading at -150°C, the BCC phase is observed as the main phase in the same manner as in the results (measured at room temperature in a state of being free from stress loading) of Example 1 of Figure 3 , and the HCP phase produced during cooling is observed to some extent.
  • Figure 4 in the state of being loaded with a stress at -150°C, additionally phases being probably orthorhombic crystal structures are observed (marked with arrows in the chart). The orthorhombic crystal products disappear after unloading the stress.
  • the superelastic effect is obtained in the Mg-Sc alloy having the BCC phase in connection with the stress-induced transformation, in the same manner as in common shape memory alloys. In this way, in the Mg-Sc alloy, an excellent superelastic shape recovery rate is obtained in connection with the reversible transformation in association with the stress loading-unloading in the BCC phase.
  • the Mg alloy (Mg alloy containing 20.5 at% of Sc) having the same composition as the composition of Example 1 was subjected to the solution treatment, and then Mg alloys were produced by varying the cooling rate so as to be 1000°C/sec, 1000°C/min, 100°C/min, and 20°C/min.
  • the produced Mg alloys were subjected to a tensile test to measure the superelastic shape recovery rate.
  • the produced Mg alloys were also subjected to X-ray diffraction to analyze the phase structure. The results thus obtained are shown in Table 2.
  • Cooling rate Superelastic shape recovery rate Phase structure 1000°C/sec 90% BCC (+HCP) 1000°C/min 70% BCC (+HCP) 100°C/min 0% HCP 20°C/min 0% HCP
  • Figure 5A shows the X-ray diffraction patters at 20°C and -190°C, of a Mg alloy having the BCC phase, and containing Sc in a content of 20.5 at%.
  • the results obtained as follows are shown: first, an X-ray diffraction was performed at 20°C, and then the sample was cooled to -190°C and subjected to an X-ray diffraction.
  • the Mg alloy sample containing Sc in a content of 20.5 at% did not show any change between 20°C to -190°C, and it is shown that martensitic transformation did not occur at this temperature.
  • the Mg alloy sample containing Sc in a content of 19.2 at% underwent a temperature change from 20°C to - 190°C, and back to 20°C, and was subjected to X-ray diffraction at the respective temperatures ( Figure 5B ).
  • the cooling to -190°C caused a martensitic transformation from a body-centered cubic structure to an orthorhombic structure (orthorhombic martensite phase, denoted as ortho-M in the chart).
  • ortho-M orthorhombic martensite phase
  • the martensite phase is reversibly changed into the BCC phase by again increasing the temperature to 20°C. Because the Mg alloy having this composition undergoes temperature-dependent martensitic transformation between 20°C and-190°C, the shape memory property was suggested to be exhibited.
  • the shape memory property was analyzed.
  • a plate-shaped sample having this composition was bend-deformed so as to have a surface distortion of approximately 3% at the liquid nitrogen temperature, and then heated to 50°C or higher, and thus recovered to a nearly straight shape.
  • the shape recovery rate was found to be 95% or more, so as to be in good agreement with the above result obtained by using DSC.
  • This result shows that when Sc is contained in a certain content, even a sample containing elements other than Sc has the shape memory property.
  • this alloy composition allows the shape recovery at room temperature or higher to be achieved, and allows the alloy having this alloy composition to be used at an environmental temperature in the vicinity of room temperature. By regulating the composition in the manner as in present Example, an alloy that exhibits the shape memory effect at an environmental temperature in the vicinity of room temperature is obtained, and thus, the application range of such an alloy can be widened.
  • the Mg alloy containing Sc in a content of 20.5 at% was investigated with respect to the yield stress ⁇ y , the pure elastic recovery strain magnitude, and the relation of the relative crystal grain diameter to the plate thickness of the sample (crystal grain diameter d/sample plate thickness t).
  • the Mg alloy of the present invention is excellent in cold workability, and also exhibits superelastic property and shape memory property.
  • the Mg alloy of the present invention having superelastic property and shape memory property can be utilized in the aerospace field, the automobile field and the like, because of the feature of being "light" in weight.
  • Mg has biodegradability, when the Mg alloy having superelastic effect is used in medical tools such as stents, such medical tools are expected to be dissolved after being left in living bodies for certain periods, and thus the Mg alloy provides significant benefits to patients.

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EP16855461.6A 2015-10-13 2016-10-13 Alliage de magnésium ayant un effet super élastique et/ou un effet de mémoire de forme Withdrawn EP3363925A4 (fr)

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CN110747382B (zh) * 2019-12-11 2021-04-23 浙江工贸职业技术学院 一种超高压力作用下的Mg-Sc-X合金及其制备方法
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