CN115807199B - Method for simultaneously improving yield strength and plasticity of bulk amorphous alloy composite material - Google Patents
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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 invention carries out cold and hot circulation treatment on the bulk amorphous alloy composite material containing amorphous phase and metastable state B2 phase, wherein the cold and hot circulation treatment comprises heat treatment and cold treatment in a circulating way; the temperature of the heat treatment is T of the bulk amorphous composite material g The temperature of the cold treatment is 77.15K; the cycle times of the cold and hot cycle treatment are more than or equal to 10 times. The method provided by the invention can convert part of metastable state B2 phase in the alloy into stable state martensitic phase to improve the yield strength of the alloy, and can increase the disorder degree of atomic structure in an amorphous matrix to obtain an amorphous phase in a spring state, promote nucleation, proliferation and interaction of a shear band in the sample deformation process, thereby improving the plasticity of the composite material and realizing synchronous improvement of the yield strength and plastic deformation capacity.
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
The amorphous alloy is different from the traditional crystalline alloy, the internal atomic arrangement mode of the amorphous alloy shows short-range order and long-range disorder, crystal defects such as crystal grains, crystal boundaries, dislocation and stacking faults are avoided, and the unique atomic arrangement mode enables the amorphous alloy to have higher breaking strength and elastic limit compared with the traditional crystalline alloy, and further shows attractive application prospects in the high-tech fields such as national defense, aerospace and the like. However, due to the internal lack of plastic deformation carriers, the alloy often shows sudden fracture without symptoms under the action of external force, and the engineering application of amorphous alloy is severely restricted.
In order to improve the plasticity of amorphous alloys, the prior art has been improved in terms of alloy composition, energy state, and the like. Among them, the preparation of bulk amorphous composites containing metastable B2 phase is a more typical method that can effectively improve the plastic deformation of amorphous alloys. The bulk amorphous composite material can generate martensitic transformation from cubic B2 phase to monoclinic B19' phase in the deformation process induced by external force, thereby obviously improving the plastic deformation capacity of the bulk 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 material is seriously influenced.
Disclosure of Invention
In view of this, the present invention provides a method for simultaneously increasing the yield strength and plasticity of bulk amorphous alloy composites. The method provided by the invention can realize the simultaneous improvement of yield strength and plasticity of the bulk amorphous alloy composite material containing 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, comprising the following steps:
carrying out cold and hot circulation treatment on the bulk 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-hot cycle treatment comprises heat treatment and cold treatment in a circulating way; the temperature of the heat treatment is T of the bulk amorphous composite material g The temperature of the cold treatment is 77.15K; the cycle times of the cold and hot cycle treatment are more than or equal to 10 times.
Preferably, the cycle number of the cold and hot cycle treatment is 10 to 20.
Preferably, the heat preservation time of the 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 block amorphous alloy composite material is Cu 48 Zr 48 Al 4 The temperature of the heat treatment of the bulk amorphous alloy composite material is 360K-420K.
Preferably, the bulk amorphous composite material is cylindrical or cubic in shape.
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 after the treatment by the method in the technical scheme, and the internal phase structure of the amorphous alloy composite material comprises a spring state amorphous phase, a metastable state B2 phase and a steady state martensitic phase.
The invention provides a method for simultaneously improving yield strength and plasticity of a bulk amorphous alloy composite material, which comprises the following steps: carrying out cold and hot circulation treatment on the bulk 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-hot cycle treatment comprises heat treatment and cold treatment in a circulating way; the temperature of the heat treatment is T of the bulk amorphous composite material g The temperature of the cold treatment is 77.15K; the cycle times of the cold and hot cycle treatment are more than or equal to 10 times. The method provided by the invention can convert part of metastable state B2 phase in the alloy into stable state martensitic phase to improve the overall yield strength of the alloy, and can increase the disorder degree of atomic structure in an amorphous matrix to obtain an amorphous phase in a spring state, so as to promote nucleation, proliferation and interaction of a shear band in a product structure, thereby improving the plasticity of the composite material, and finally realizing 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 after the treatment by the method in the technical scheme, and the internal phase structure of the amorphous alloy composite material comprises a spring state amorphous phase, a metastable state B2 phase and a steady state martensitic 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 untreated metastable B2-phase-containing materials.
Drawings
FIG. 1 is a differential scanning calorimeter analysis graph of the treated amorphous alloy composite materials prepared in examples 1-3 and comparative examples;
FIG. 2 is an X-ray diffraction chart of the treated amorphous alloy composite materials prepared in examples 1 to 3 and comparative example;
fig. 3 is a graph showing the compressive stress-strain comparison of the treated amorphous alloy composites prepared in examples 1 to 3 and comparative examples.
Detailed Description
The invention provides a method for simultaneously improving yield strength and plasticity of a bulk amorphous alloy composite material, which comprises the following steps:
carrying out cold and hot circulation treatment on the bulk 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-hot cycle treatment comprises heat treatment and cold treatment in a circulating way; the temperature of the heat treatment is T of the bulk amorphous composite material g The temperature of the cold treatment is 77.15K; the cycle times of the cold and hot cycle treatment are more than or equal to 10 times.
The preparation raw materials used in the invention are all commercially available unless otherwise specified.
The invention carries out cold and hot circulation treatment on the bulk 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 cylindrical or cubic in shape, more preferably cylindrical. In the present invention, the diameter of the bottom surface of the cylinder is preferably 3 to 5mm, more preferably 3 to 4mm, 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, 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 Bulk amorphous alloy composite materials.
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 The atomic ratio of each element in the bulk amorphous alloy composite material is respectively used for weighing Cu, zr and Al bulk raw materials with the purity of more than or equal to 99.99 percent; smelting the Cu, zr and Al block raw materials to obtain smelting liquid, sucking the smelting liquid into a water-cooling copper mold, and cooling to obtain the Cu 48 Zr 48 Al 4 Bulk amorphous alloy composite materials.
In the present invention, the smelting means is preferably arc smelting, the smelting is preferably performed under a protective atmosphere, and the protective atmosphere preferably comprises argon gas; the Cu is 48 Zr 48 Al 4 The bulk amorphous alloy composite material is preferably cylindrical in shape, and the diameter of the bottom surface of the cylinder is preferably 3mm. The method for preferably carrying out suction casting on the water-cooled copper mould can ensure that the internal phase structure of the prepared bulk amorphous alloy composite material comprises an amorphous phase and a metastable state B2 phase.
In the present invention, the cold-hot cycle treatment includes a cycle of heat treatment and cold treatment. 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 is preferably 360K to 420K, more preferably 370K to 400K. In a specific embodiment of the present invention, the Cu 48 Zr 48 Al 4 T of bulk amorphous alloy composite material g 698K, the heat treatmentThe temperature is preferably 360K, 390K or 420K, respectively Cu 48 Zr 48 Al 4 T of bulk amorphous alloy composite material g 51.6%,55.9% or 60.2%. In the invention, the T of the bulk amorphous alloy composite material g Preferably by a differential scanning calorimeter, which in particular embodiments of the invention is preferably of the type NETZSCH DSC404F1.
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 and hot cycle treatment is preferably performed in a liquid nitrogen cooled high and low temperature tank, the heat treatment is preferably performed in a high temperature tank of the liquid nitrogen cooled high and low temperature tank, the heat treatment is preferably performed at the same position in the high temperature tank, and the cold treatment is preferably performed in a liquid nitrogen tank of the liquid nitrogen cooled high and low temperature tank. 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 cycle number of the heat and cold cycle treatment is not less than 10 times, preferably 10 to 20 times, more preferably 13 to 17 times, still more preferably 15 times. In the present invention, the holding time for the heat treatment is preferably 1 to 5 minutes, more preferably 1 to 3 minutes, and still more preferably 1 minute, per one heat treatment. In the present invention, the holding time for the single cold treatment is preferably 1 to 5 minutes, more preferably 1 to 2 minutes, and still more preferably 1 minute.
The invention also provides an amorphous alloy composite material which is obtained after the treatment by the method in the technical scheme, and the internal phase structure of the amorphous alloy composite material comprises a spring state amorphous phase, a metastable state B2 phase and a steady state martensitic phase. In the invention, the internal phase structure of the amorphous alloy composite material comprises a spring state amorphous phase, a metastable state B2 phase and a steady state martensitic phase composite material, and the three phases are mutually coupled, so that the amorphous alloy composite material obtained after treatment shows synchronous improvement of yield strength and plastic deformation capacity relative to an untreated metastable state B2 phase-containing material.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention.
Example 1
1. Preparation of Cu 48 Zr 48 Al 4 The bulk amorphous alloy composite material comprises the following steps:
1. according to Cu 48 Zr 48 Al 4 The atomic ratio of each element in the bulk amorphous alloy composite material is respectively used for weighing Cu, zr and Al bulk raw materials with the purity of more than or equal to 99.99 percent;
2. placing Cu, zr and Al block raw materials into an arc melting cavity, vacuumizing to 4×10 -3 Filling argon into a smelting cavity below Pa, enabling the air pressure in the cavity to reach-0.05 Pa, striking an arc and striking a fire under the protection atmosphere of the argon, smelting a titanium ingot for 20s, enabling the titanium ingot to absorb redundant oxygen in the cavity, smelting Cu, zr and Al block raw materials, and smelting for 10s after the block raw materials are completely melted to obtain 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 mutually independent and are not influenced;
3. and pressing down a suction casting valve, sucking the smelting liquid of the raw materials into a water-cooling copper mold, closing the suction casting valve after the smelting liquid is completely sucked into the water-cooling copper mold, and stopping heating at the same time, so that the smelting liquid is rapidly cooled in the water-cooling copper mold, and obtaining the amorphous alloy composite 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 cylinder to ensure clean surface, and determining the glass transition temperature T of a sample by using a differential scanning calorimeter model NETZSCH DSC404F1 g 698K; cutting the amorphous alloy composite material cylinder into samples with the height-to-diameter ratio of 2:1, and polishing the two end surfaces to mirror surfaces while ensuring that the cut end surfaces of the two samples are parallel to each other.
And (3) cooling the sample by using an EMC003A-2 liquid nitrogen refrigerating high-low temperature box and liquid nitrogen. The method comprises the following specific steps: and (3) carrying out heat treatment on the sample in a high-temperature box for a period of time, taking out the sample after the heat treatment, placing the sample after the heat treatment in a liquid nitrogen tank for heat treatment for a period of time, taking out the sample after the cold treatment, completing one-time cold-hot circulation treatment, and placing the sample after the cold treatment in the high-temperature box for the next cold-hot circulation treatment. The heat treatment ensures that each heating is at the same position in the high temperature box.
The specific conditions of the cold and hot circulation treatment are as follows: the temperature of the heat treatment is 360K, which is T of the sample g The heat preservation time of 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 single cold treatment is 1min, and the total circulation is carried out for 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 The other 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 The other treatment conditions were the same as in example 1.
As a comparative example, an as-cast sample prepared in example 1 was not subjected to heat and cold cycle treatment.
The treated amorphous alloy composite materials and the comparative examples prepared in examples 1 to 3 were analyzed by using a differential scanning calorimeter, and the analysis results are shown in fig. 1. FIG. 1 is a graph showing differential scanning calorimetric analysis of the treated amorphous alloy composite materials prepared in examples 1 to 3 and comparative examples. As can be seen from FIG. 1, the glass transition temperatures (T) of the treated amorphous alloy composite materials prepared in comparative examples and examples 1 to 3 g ) Is very close. It can also be observed at T g Previously, the treated amorphous alloy composite materials prepared in comparative examples and examples 1 to 3 have an unobvious exothermic peak, which corresponds to the structural relaxation of the amorphous matrix due to annihilation of free volume in the amorphous structure during the continuous heating process. The free volume content in amorphous tissue can be indirectly characterized by the structural relaxation enthalpy. The higher the content of free volume in the amorphous tissue, the higher the corresponding value of the structural relaxation enthalpy. As can be seen from fig. 1, among the four typesIn the samples, the amorphous structure of the comparative example (as-cast) has the lowest free volume content, the corresponding structure relaxation enthalpy has the lowest value, and the structure relaxation enthalpies of the examples 1-3 are all higher than those of the as-cast samples, so that the free volume content of the samples subjected to the cold and hot cycle treatment is increased to different degrees relative to that of the as-cast samples, and the generation of the amorphous phase in the spring state is shown. For examples 1 to 3, the greater the difference in the cold and hot treatment temperatures, the better the structure spring effect of the amorphous matrix, but when the heat treatment temperature is raised to a certain extent, the more serious the structure relaxation annihilation of the amorphous matrix, the lower the free volume content, and the spring effect relatively worsened. Therefore, the value of the structural relaxation enthalpy of the amorphous alloy composite material obtained by treatment at the heat treatment temperature of 390K is highest in three embodiments, which shows that the content of free volume in an amorphous structure is highest, and the structure spring effect of an amorphous matrix is best. After the glass transition temperature, the curves corresponding to the four samples all show a remarkable exothermic peak, the peak temperature is about 755K, and the exothermic peak is an exothermic peak when the amorphous phase is converted into the crystalline phase, and further shows that the amorphous alloy composite materials processed in the examples 1-3 have amorphous structures.
The treated amorphous alloy composite materials and comparative examples prepared in examples 1 to 3 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 comparative example. In fig. 2, a is an X-ray diffraction pattern of the comparative example, and b to d correspond to the X-ray diffraction patterns of the treated amorphous alloy composite materials prepared in examples 1 to 3, respectively. As can be seen 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, and from B-d, new crystal diffraction peaks appear in the X-ray diffraction spectrogram of the sample after the cold and hot cycle treatment except for the original B2-CuZr phase crystal diffraction peaks, and the diffraction peaks can be marked as monoclinic B19'-CuZr phases, wherein the monoclinic B19' -CuZr phases are monoclinic martensite phases. 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, the materialThe second phase of the internal part of the crystals can be transformed from the cubic phase to the martensitic phase under the induction of heat, which is beneficial to improving the yield strength of the whole alloy.
The treated amorphous alloy composite materials prepared in examples 1 to 3 and comparative examples were subjected to quasi-static uniaxial compression performance test using an ETM105D universal tester with an initial strain rate of 2.0X10 -4 s -1 The ambient temperature was room temperature and the detection result is shown in fig. 3. Fig. 3 is a graph showing the compressive stress-strain comparison of the treated amorphous alloy composites prepared in examples 1 to 3 and comparative examples. As can be seen from fig. 3, the treated amorphous alloy composites prepared in comparative examples and examples 1 to 3 all have different degrees of "work hardening" effect in the plastic deformation stage after reaching the yield point. For the comparative example, the internal crystal phase only has 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 the performance test, when the cubic structure B2-CuZr phase is subjected to stress induction, the cubic structure B2-CuZr phase is transformed into a monoclinic structure B19'-CuZr phase, and the hardness of the B19' -CuZr phase is far higher than that of the B2-CuZr phase, so that the overall hardness level of the material is higher than that of the material before stress loading, and therefore, a significant 'work hardening' effect exists. In the amorphous alloy composite materials prepared in examples 1 to 3, two crystal phases exist inside, one is a B2-CuZr phase which is self-contained, and the other is a B19' -CuZr phase which is obtained by phase change conversion of part of the B2-CuZr phase in the cold and hot circulation treatment process. Therefore, the mechanical behaviors of the amorphous alloy composite materials prepared in examples 1 to 3 are mainly affected by the B2-CuZr phase and the B19'-CuZr phase, so that a similar work hardening effect as that of the comparative example can be generated, on the one hand, the hardness of the material is increased due to the generation of the B19' -CuZr phase with higher hardness, the yield strength of the material is further increased, a rejuvenation amorphous phase can be generated through cold-hot cycle treatment, and the plastic deformation capability of the treated amorphous alloy composite material is improved. The treated amorphous alloy composite materials prepared in examples 1 to 3 are superior to the comparative examples in both yield strength and plastic strain as a whole,the yield strength and the plasticity are improved simultaneously. Wherein, the yield strength of the example 2 is increased from 1680MPa of the comparative example to 1830MPa, the plastic strain is increased from 5.8% of the comparative example to 8.9%, and the yield strength and the plastic are improved simultaneously with the best effect.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (6)
1. A method for simultaneously improving yield strength and plasticity of a bulk amorphous alloy composite material, which is characterized by comprising the following steps:
carrying out cold and hot circulation treatment on the bulk 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-hot cycle treatment comprises heat treatment and cold treatment in a circulating way; the temperature of the heat treatment is 390K, and the temperature of the cold treatment is 77.15K; the cycle times of the cold and hot cycle treatment are 10-20 times;
the cold-hot circulation treatment is to heat-treat the block amorphous alloy composite material in a high-temperature box, take out a sample after the heat treatment is finished, place the heat-treated sample in a liquid nitrogen tank for heat preservation and cold treatment, take out the sample after the cold treatment is finished, and finish one-time cold-hot circulation treatment;
the block amorphous alloy composite material is Cu 48 Zr 48 Al 4 Bulk amorphous alloy composite materials.
2. The method according to claim 1, wherein the heat treatment is performed for a single time of 1 to 5 minutes.
3. The method according to claim 1, wherein the heat-retaining time of the single cold treatment is 1 to 5 minutes.
4. The method of claim 1, wherein the bulk amorphous alloy composite material is cylindrical or cubic in shape.
5. The method of claim 4, wherein 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 3-5 mm.
6. An amorphous alloy composite material, characterized in that the amorphous alloy composite material is obtained after treatment by the method of any one of claims 1 to 5, and the internal phase structure of the amorphous alloy composite material comprises a spring state amorphous phase, a metastable state B2 phase and a steady state martensitic 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 |
| 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 |
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