CN115807199A - Method for simultaneously improving yield strength and plasticity of bulk amorphous alloy composite material - Google Patents
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- 229910000808 amorphous metal alloy Inorganic materials 0.000 title claims abstract description 90
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Abstract
The invention relates to the technical field of amorphous alloy composite materials, and provides a method for simultaneously improving yield strength and plasticity of a block amorphous alloy composite material. The method comprises the following steps of carrying out cold-hot circulation treatment on a block amorphous alloy composite material containing an amorphous phase and a metastable B2 phase, wherein the cold-hot circulation treatment comprises circularly carrying out heat treatment and cold treatment; the temperature of the heat treatment is T of the bulk amorphous composite material g 40% -62% of the cold treatment temperature is 77.15K; the cycle times of the cold-hot cycle treatment are more than or equal to 10 times. The method provided by the invention can convert part of metastable B2 phase in the alloy into stable martensite phase to improve the yield strength of the alloy, can increase the disorder degree of atomic structures in an amorphous matrix, obtains the amorphous phase in a spring-back state, and promotes shearing in the sample deformation processNucleation, proliferation and interaction of the cut strips, so that the plasticity of the composite material is improved, and the yield strength and the plastic deformation capacity are synchronously improved.
Description
Technical Field
The invention relates to the technical field of amorphous alloy composite materials, in particular to a method for simultaneously improving yield strength and plasticity of a block amorphous alloy composite material.
Background
Compared with the traditional crystalline alloy, the amorphous alloy has the advantages that the internal atomic arrangement mode of the amorphous alloy is short-range ordered and long-range disordered, and crystal defects such as crystal grains, crystal boundaries, dislocation, stacking faults and the like do not exist. However, due to the lack of the plastic deformation carrier inside, the alloy often shows sudden fracture without signs under the action of external force, and the engineering application of the amorphous alloy is severely limited.
In order to improve the plasticity of the amorphous alloy, the prior art is improved from the aspects of alloy components, energy states and the like. The preparation of the bulk amorphous composite material containing the metastable B2 phase is a typical method capable of effectively improving the plastic deformation of the amorphous alloy. The block amorphous composite material can generate martensite transformation from a cubic B2 phase to a monoclinic B19' phase in the deformation process induced by external force, thereby obviously improving the plastic deformation capability of the block amorphous composite material and showing excellent deformation hardening characteristics. However, the yield strength of the bulk amorphous composite material is obviously reduced while good plasticity is obtained, and the application of the bulk amorphous composite material is seriously influenced.
Disclosure of Invention
In view of the above, the present invention provides a method for simultaneously improving yield strength and plasticity of a bulk amorphous alloy composite material. The method provided by the invention can realize the simultaneous improvement of yield strength and plasticity of the bulk amorphous alloy composite material containing the metastable B2 phase.
In order to achieve the above object, the present invention provides the following technical solutions:
a method for simultaneously improving yield strength and plasticity of a bulk amorphous alloy composite material comprises the following steps:
carrying out cold-hot circulation treatment on the block amorphous alloy composite material;
the internal phase structure of the bulk amorphous alloy composite material comprises an amorphous phase and a metastable B2 phase;
the cold and hot circulating treatment comprises circulating heat treatment and cold treatment; the temperature of the heat treatment is T of the bulk amorphous composite material g 40% -62% of the cold treatment temperature is 77.15K; the cycle times of the cold-hot cycle treatment are more than or equal to 10 times.
Preferably, the number of cycles of the cooling-heating cycle treatment is 10 to 20.
Preferably, the heat preservation time of a single heat treatment is 1-5 min.
Preferably, the heat preservation time of the single cold treatment is 1-5 min.
Preferably, the bulk amorphous alloy composite material comprises a Cu-Zr-Al series bulk amorphous alloy composite material.
Preferably, the Cu-Zr-Al series bulk amorphous alloy composite material is Cu 48 Zr 48 Al 4 The temperature of the heat treatment of the block amorphous alloy composite material is 360-420K.
Preferably, the bulk amorphous composite material is in the shape of a cylinder or a cube.
Preferably, the diameter of the bottom surface of the cylinder is 3-5 mm, and the side length of the bottom surface of the cube is independently 3-5 mm.
The invention also provides an amorphous alloy composite material which is obtained by the treatment of the method in the technical scheme, and the internal phase structure of the amorphous alloy composite material comprises a spring-back amorphous phase, a metastable B2 phase and a stable martensite phase.
The invention provides a method for simultaneously improving yield strength and plasticity of a block amorphous alloy composite material, which comprises the following steps: carrying out cold-hot circulation treatment on the block amorphous alloy composite material; the internal phase structure of the bulk amorphous composite material comprises an amorphous phase and a metastable B2 phase; the cold and hot circulating treatment comprises circulating heat treatment and cold treatment; the temperature of the heat treatment is T of the bulk amorphous composite material g 40% to 62% of saidThe temperature of cold treatment is 77.15K; the cycle times of the cold-hot cycle treatment are more than or equal to 10 times. The method provided by the invention can convert part of metastable B2 phase in the alloy into stable martensite phase to improve the overall yield strength of the alloy, and can increase the disorder degree of atomic structures in an amorphous matrix to obtain the amorphous phase in a spring-back state, thereby promoting the nucleation, proliferation and interaction of shear bands in the product structure, so as to improve the plasticity of the composite material and finally realize the synchronous improvement of the yield strength and plastic deformation capacity of the bulk amorphous composite material.
The invention also provides an amorphous alloy composite material which is obtained by the treatment of the method in the technical scheme, and the internal phase structure of the amorphous alloy composite material comprises a rejuvenation state amorphous phase, a metastable B2 phase and a stable martensite phase. The three-phase materials are coupled with each other in a coordinated manner, so that the alloy material shows synchronous improvement of yield strength and plastic deformation capacity relative to an untreated material containing the metastable B2 phase.
Drawings
FIG. 1 is a differential scanning calorimetry trace of the treated amorphous alloy composites prepared in examples 1-3 and a comparative example;
FIG. 2 is an X-ray diffraction pattern of the treated amorphous alloy composite prepared in examples 1-3 and a comparative example;
FIG. 3 is a graph of compressive stress versus strain for the treated amorphous alloy composites prepared in examples 1-3 and a comparative example.
Detailed Description
The invention provides a method for simultaneously improving yield strength and plasticity of a block amorphous alloy composite material, which comprises the following steps:
carrying out cold-hot circulation treatment on the block amorphous alloy composite material;
the internal phase structure of the bulk amorphous composite material comprises an amorphous phase and a metastable B2 phase;
the cold and hot circulating treatment comprises circulating heat treatment and cold treatment; the temperature of the heat treatment is T of the bulk amorphous composite material g 40% to 62% of, thereforeThe temperature of the cold treatment is 77.15K; the cycle times of the cold-hot cycle treatment are more than or equal to 10 times.
Unless otherwise specified, the starting materials for the preparation used in the present invention are commercially available.
The invention carries out cold and hot circulation treatment on the block amorphous alloy composite material to obtain the treated amorphous alloy composite material. In the present invention, the internal phase structure of the bulk amorphous alloy composite material includes an amorphous phase and a metastable B2 phase. In the present invention, the bulk amorphous alloy composite material preferably includes a Cu — Zr — Al series bulk amorphous alloy composite material.
In the present invention, the bulk amorphous alloy composite material is preferably in the shape of a cylinder or a cube, and more preferably a cylinder. In the present invention, the diameter of the bottom surface of the cylinder is preferably 3 to 5mm, more preferably 3 to 4mm, and still more preferably 3mm, and the side length of the bottom surface of the cube is independently 3 to 5mm, more preferably 3 to 4mm, and still more preferably 3mm.
In the invention, the Cu-Zr-Al series block amorphous alloy composite material is preferably prepared by a water-cooling copper mold suction casting method. In the invention, the Cu-Zr-Al series bulk amorphous alloy composite material is preferably Cu 48 Zr 48 Al 4 A bulk amorphous alloy composite material.
In the present invention, the Cu 48 Zr 48 Al 4 The preparation method of the bulk amorphous alloy composite material preferably comprises the following steps: according to the Cu 48 Zr 48 Al 4 Weighing Cu, zr and Al block raw materials with the purity of more than or equal to 99.99 percent respectively according to the atomic ratio of each element in the block amorphous alloy composite material; smelting the Cu, zr and Al block raw materials to obtain a smelting solution, sucking the smelting solution into a water-cooling copper mold for cooling to obtain the Cu 48 Zr 48 Al 4 A bulk amorphous alloy composite material.
In the invention, the smelting mode is preferably arc smelting, the smelting is preferably carried out under a protective atmosphere, and the protective atmosphere preferably comprises argon; the Cu 48 Zr 48 Al 4 Shape optimization of bulk amorphous alloy compositeIs a cylinder, and the diameter of the bottom surface of the cylinder is preferably 3mm. The method for water-cooling copper mold suction casting is preferably selected, so that the internal phase structure of the prepared bulk amorphous alloy composite material can be ensured to comprise an amorphous phase and a metastable B2 phase.
In the present invention, the cold-hot cycle treatment includes performing heat treatment and cold treatment in cycles. In the invention, the temperature of the heat treatment is T of the bulk amorphous alloy composite material g From 40% to 62%, preferably from 51% to 61%, more preferably from 53% to 57%. In the invention, the Cu-Zr-Al series bulk amorphous alloy composite material is preferably Cu 48 Zr 48 Al 4 The temperature of the heat treatment of the bulk amorphous alloy composite material is preferably 360K-420K, and more preferably 370K-400K. In a specific embodiment of the present invention, the Cu 48 Zr 48 Al 4 T of block amorphous alloy composite material g 698K, the temperature of the heat treatment is preferably 360K, 390K or 420K, respectively, of the Cu 48 Zr 48 Al 4 T of block amorphous alloy composite material g 51.6%,55.9% or 60.2%. In the invention, T of the bulk amorphous alloy composite material g Preferably by differential scanning calorimetry, which in a particular embodiment of the invention is preferably of the netzsschdsc 404F1 type.
In the present invention, the temperature of the cold treatment is 77.15K, and the temperature of the cold treatment is preferably obtained by liquid nitrogen refrigeration.
In the present invention, the cold-hot cycle treatment is preferably performed in a liquid nitrogen refrigerated high-low temperature cabinet, the heat treatment is preferably performed in a high-temperature cabinet of the liquid nitrogen refrigerated high-low temperature cabinet, the heat treatment is preferably performed at the same position in the high-temperature cabinet, and the cold treatment is preferably performed in a liquid nitrogen tank of the liquid nitrogen refrigerated high-low temperature cabinet. In the specific embodiment of the invention, the model of the liquid nitrogen refrigeration high-low temperature box is preferably EMC003A-2.
In the present invention, the number of cycles of the cooling-heating cycle treatment is not less than 10, preferably 10 to 20, more preferably 13 to 17, and still more preferably 15. In the present invention, the heat-retaining time for one heat treatment is preferably 1 to 5min, more preferably 1 to 3min, and still more preferably 1min. In the present invention, the heat-retaining time for the single cold treatment is preferably 1 to 5min, more preferably 1 to 2min, and still more preferably 1min.
The invention also provides an amorphous alloy composite material which is obtained by the treatment of the method in the technical scheme, and the internal phase structure of the amorphous alloy composite material comprises a spring-back amorphous phase, a metastable B2 phase and a stable martensite phase. In the invention, the internal phase structure of the amorphous alloy composite material comprises a rejuvenation state amorphous phase, a metastable B2 phase and a stable martensite phase composite material which are coupled with each other, so that the yield strength and the plastic deformation capacity of the processed amorphous alloy composite material are synchronously improved compared with the unprocessed metastable B2 phase-containing material.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
Example 1
1. Preparation of Cu 48 Zr 48 Al 4 The block amorphous alloy composite material comprises the following steps:
1. according to Cu 48 Zr 48 Al 4 Weighing Cu, zr and Al block raw materials with the purity of more than or equal to 99.99 percent respectively according to the atomic ratio of each element in the block amorphous alloy composite material;
2. putting Cu, zr and Al block raw materials into an arc melting chamber, and vacuumizing to 4 multiplied by 10 -3 Below Pa, filling argon into the smelting cavity to enable the air pressure in the cavity to reach-0.05 Pa, striking an arc and striking fire under the argon protective atmosphere, smelting a titanium ingot for 20s, enabling the titanium ingot to absorb redundant oxygen in the cavity, smelting the Cu, zr and Al block raw materials, and smelting for 10s after the block raw materials are completely molten to obtain a smelting liquid of the raw materials, wherein a crucible for smelting the titanium ingot and a crucible for smelting the Cu, zr and Al block raw materials are independent from each other and do not influence each other;
3. and pressing a suction casting valve, sucking the smelting liquid of the raw materials into the water-cooled copper mold, closing the suction casting valve after the smelting liquid is completely sucked into the water-cooled copper mold, and stopping heating to quickly cool the smelting liquid in the water-cooled copper mold to prepare the amorphous alloy composite material cylinder with the bottom surface diameter of 3mm and the length of 70 mm.
2. Performing cold and hot circulation treatment
Ultrasonically cleaning the prepared amorphous alloy composite material cylinder to ensure the surface to be clean, and determining the glass transition temperature T of a sample by using a differential scanning calorimeter with the model of NETZSCHDSC404F1 g 698K; cutting the cylinder of the amorphous alloy composite material into samples with the height-diameter ratio of 2:1, and grinding and polishing two end faces to a mirror surface while ensuring that the cut end faces of the two samples are parallel to each other.
And performing cold-hot circulating treatment on the sample by using an EMC003A-2 liquid nitrogen refrigeration high-low temperature box and liquid nitrogen. The method comprises the following specific steps: and (3) preserving the heat of the sample in a high-temperature box for a period of time for heat treatment, taking out the sample after the heat treatment, placing the sample after the heat treatment in a liquid nitrogen tank for heat preservation for a period of time for cold treatment, taking out the sample after the cold treatment, completing one cold and hot cycle treatment, and then placing the sample after the cold treatment in the high-temperature box for the next cold and hot cycle treatment. The heat treatment ensures that each heating is in the same position in the hot box.
The specific conditions of the cold-hot circulation treatment are as follows: the temperature of the heat treatment was 360K, which is T of the sample g 51.6 percent of the total amorphous alloy composite material, wherein the heat preservation time of the single heat treatment is 1min, the cold treatment is carried out in a liquid nitrogen tank, the temperature of the cold treatment is 77.15K, the heat preservation time of the single cold treatment is 1min, and the total cycle is 15 times, so that the treated amorphous alloy composite material is finally obtained.
Example 2
The temperature of the heat treatment was adjusted to 390K, which is T of the sample g 55.9% of (D), and the remaining treatment conditions were the same as in example 1.
Example 3
The temperature of the heat treatment was adjusted to 420K, which is T of the sample g 60.2% of (A), and the remaining processing conditions were the same as in example 1.
The as-cast test piece prepared in example 1 without the cooling-heating cycle treatment was used as a comparative example.
Using differential scanning calorimetryThe treated amorphous alloy composite materials prepared in examples 1 to 3 and the comparative example were analyzed by an analyzer, and the analysis results are shown in fig. 1. FIG. 1 is a Differential Scanning Calorimetry (DSC) curve of the treated amorphous alloy composites prepared in examples 1-3 and a comparative example. As can be seen from FIG. 1, the glass transition temperatures (T) of the treated amorphous alloy composites prepared in the comparative example and examples 1 to 3 g ) Are very close. It can also be observed at T g The processed amorphous alloy composite materials prepared in the comparative example and the examples 1 to 3 have an unobvious exothermic peak, and the exothermic peak corresponds to the structural relaxation formed by annihilation of free volume in an amorphous structure in the process of continuously heating an amorphous matrix. The free volume content in amorphous structures can be indirectly characterized by the enthalpy of structural relaxation. The higher the content of free volume in the amorphous structure, the higher the corresponding value of the enthalpy of structural relaxation. As can be seen from fig. 1, in the four samples, the content of free volume in the amorphous structure of the comparative example (as-cast state) was the lowest, and the corresponding values of enthalpy of structural relaxation were the lowest, and the enthalpies of structural relaxation of examples 1 to 3 were all higher than that of the as-cast state, indicating that the free volume content of the sample after the cold-heat cycle treatment was increased to different degrees relative to that of the as-cast state sample, indicating that the amorphous phase in the spring-back state was generated. In examples 1 to 3, the larger the temperature difference between the cold and hot treatment temperatures as the heat treatment temperature increases, the better the structural rejuvenation effect of the amorphous matrix, but when the heat treatment temperature increases to a certain extent, the more the structural relaxation of the amorphous matrix is annihilated, the lower the free volume content is, and the relative deterioration of the rejuvenation effect is observed. Therefore, the value of the structural relaxation enthalpy of the amorphous alloy composite material obtained by the treatment at the heat treatment temperature of 390K is the highest in the three embodiments, which shows that the content of the free volume in the amorphous structure is the highest, and the structural rejuvenation effect of the amorphous matrix is the best. After the glass transition temperature, the curves corresponding to the four samples all have a distinct exothermic peak, the peak temperature is about 755K, and the exothermic peak is the exothermic peak when the amorphous phase is transformed into the crystalline phase, further indicating that the amorphous alloy composite materials treated in examples 1-3 have an amorphous structure.
The treated amorphous alloy composite materials prepared in examples 1 to 3 and the comparative example were analyzed by an X-ray diffractometer, and the analysis results are shown in fig. 2. FIG. 2 is an X-ray diffraction pattern of the treated amorphous alloy composite materials prepared in examples 1 to 3 and a comparative example. In FIG. 2, a is the X-ray diffraction pattern of the comparative example, and b to d correspond to the X-ray diffraction patterns of the treated amorphous alloy composites prepared in examples 1 to 3, respectively. From a, the crystal diffraction peaks marked on the X-ray diffraction spectrogram of the comparative example can be marked as a cubic B2-CuZr phase, from B to d, the X-ray diffraction spectrogram of the sample after cold-hot cycle treatment has new crystal diffraction peaks except the original B2-CuZr phase crystal diffraction peaks, and the diffraction peaks can be marked as a monoclinic B19' -CuZr phase which is a monoclinic martensite phase. FIG. 2 shows that Cu 48 Zr 48 Al 4 After the block amorphous alloy composite material is subjected to cold and hot circulation treatment, a part of crystal second phase in the material can be transformed from a cubic phase to a martensite phase under the thermal induction, and the improvement of the overall yield strength of the alloy is facilitated.
The processed amorphous alloy composite materials prepared in the examples 1 to 3 and the comparative example were subjected to quasi-static uniaxial compressive property detection by using an ETM105D universal tester, and the initial strain rate was 2.0
10 -4 s -1 The ambient temperature is room temperature, and the results are shown in fig. 3. FIG. 3 is a graph of compressive stress versus strain for the treated amorphous alloy composites prepared in examples 1-3 and a comparative example. As can be seen from FIG. 3, the treated amorphous alloy composites prepared in comparative examples and examples 1-3 have different degrees of "work hardening" effect in the plastic deformation stage after the yield point is reached. For the comparative example, the crystal phase in the comparative example is only the B2-CuZr phase, and when the sample of the comparative example is loaded by external stress, the change of the mechanical property is mainly influenced by the content of the B2-CuZr phase and the phase change behavior. In a performance test, when the alloy is induced by stress, the B2-CuZr phase with a cubic structure is subjected to phase transition to be converted into a B19'-CuZr phase with a monoclinic structure, and the hardness of the B19' -CuZr phase is far higher than that of the B2-CuZr phase, so that the alloy is suitable for being used as a material for a high-temperature heat-resistant alloyThe overall hardness level of the material is made higher than before the stress loading, so there is a significant "work hardening" effect. In the amorphous alloy composite materials prepared in examples 1 to 3, two crystal phases exist in the amorphous alloy composite materials, one is a B2-CuZr phase which is possessed by the amorphous alloy composite materials, and the other is a B19' -CuZr phase which is obtained by the phase transformation of part of the B2-CuZr phase in the cold and hot circulation treatment process. Therefore, the mechanical behavior of the amorphous alloy composite materials prepared in examples 1 to 3 is mainly influenced by the B2-CuZr phase and the B19'-CuZr phase, on one hand, the "work hardening" effect similar to that of the comparative example is generated, on the other hand, the material hardness is increased due to the generation of the B19' -CuZr phase with higher hardness, so that the yield strength of the material is increased, the cold and hot cycle treatment can generate the amorphous phase in the spring state, and the plastic deformation capability of the treated amorphous alloy composite material is improved. The yield strength and plastic strain of the treated amorphous alloy composite materials prepared in the embodiments 1 to 3 are better than those of the comparative examples on the whole, and the yield strength and the plasticity are improved at the same time. Wherein, the yield strength of the embodiment 2 is improved to 1830MPa from 1680MPa of the comparative example, the plastic strain is improved to 8.9 percent from 5.8 percent of the comparative example, and the simultaneous improvement effect of the yield strength and the plasticity is optimal.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A method for simultaneously improving yield strength and plasticity of a bulk amorphous alloy composite material is characterized by comprising the following steps:
carrying out cold-hot circulation treatment on the block amorphous alloy composite material;
the internal phase structure of the bulk amorphous alloy composite material comprises an amorphous phase and a metastable B2 phase;
the cold and hot circulating treatment comprises circulating heat treatment and cold treatment; the temperature of the heat treatment is that of the bulk amorphous composite materialT g 40% -62% of the cold treatment temperature is 77.15K; the cycle times of the cold-hot cycle treatment are more than or equal to 10 times.
2. The method according to claim 1, wherein the number of cycles of the cold-hot cycle treatment is 10 to 20.
3. The method according to claim 1 or 2, wherein the holding time for a single heat treatment is 1-5 min.
4. The method according to claim 1 or 2, wherein the incubation time for a single cold treatment is 1 to 5min.
5. The method of claim 1, wherein the bulk amorphous alloy composite material comprises a Cu-Zr-Al series bulk amorphous alloy composite material.
6. The method according to claim 5, wherein the Cu-Zr-Al series bulk amorphous alloy composite material is Cu 48 Zr 48 Al 4 The temperature of the heat treatment is 360-420K.
7. The method of claim 1 or 5, wherein the bulk amorphous composite material is in the shape of a cylinder or a cube.
8. The method of claim 7, wherein the diameter of the bottom surface of the cylinder is 3 to 5mm and the side length of the bottom surface of the cube is independently 3 to 5mm.
9. An amorphous alloy composite material obtained by the method of any one of claims 1 to 8, wherein the internal phase structure of the amorphous alloy composite material comprises a springback amorphous phase, a metastable B2 phase and a stable martensite phase.
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| US4878954A (en) * | 1987-06-24 | 1989-11-07 | Compagnie Europeenne Du Zirconium Cezus | Process for improving the ductility of a product of alloy involving martensitic transformation and use thereof |
| US20210102280A1 (en) * | 2017-05-18 | 2021-04-08 | Institute Of Metal Research, Chinese Academy Of Sciences | Zr-based amorphous alloy and manufacturing method thereof |
| CN109972065A (en) * | 2019-03-28 | 2019-07-05 | 西安交通大学 | A method of amorphous alloy plasticity is improved using low temperature thermal cycle |
| CN112391587A (en) * | 2020-10-09 | 2021-02-23 | 太原理工大学 | Preparation method and application of amorphous alloy material toughened in cryogenic cycle combined pre-deformation mode |
| CN115198210A (en) * | 2021-04-08 | 2022-10-18 | 中国科学院金属研究所 | Method for driving massive amorphous alloy to quickly recover spring without damage and application thereof |
| CN114480994A (en) * | 2022-01-27 | 2022-05-13 | 沈阳工业大学 | Device and process for improving deep cooling circulation induced rejuvenation capability of Zr-based amorphous alloy |
Cited By (2)
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| CN116497300A (en) * | 2023-05-09 | 2023-07-28 | 上海大学 | Method for regulating and controlling residual stress and rejuvenation behavior of amorphous alloy by adopting low-temperature thermal cycle treatment |
| CN116497300B (en) * | 2023-05-09 | 2023-10-27 | 上海大学 | Method for regulating and controlling residual stress and rejuvenation behavior of amorphous alloy by adopting low-temperature thermal cycle treatment |
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