CN112962014B - Method for improving strength and plasticity of multi-component alloy based on annealing hardening - Google Patents
Method for improving strength and plasticity of multi-component alloy based on annealing hardening Download PDFInfo
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
Abstract
The invention discloses a method for improving the strength and the plasticity of a multi-component alloy based on annealing hardening, which comprises the following steps: s1: mixing three elements of transition metal cobalt, chromium and nickel according to equal atomic ratio or approximate equal atomic ratio, preparing CoCrNi multi-component alloy by adopting a vacuum induction melting method, and then carrying out high-temperature homogenization treatment; s2: different deformation amounts are introduced into the CoCrNi multi-component alloy by the deformation mode of cold rolling. Compared with other modes of introducing defects by cold deformation (rolling, equal-channel extrusion, high-pressure torsion and the like), the method has the advantages of uniform defect introducing structure, simplicity in operation, cost saving and the like, and the yield strength, the tensile strength and the plasticity of the CoCrNi multi-component alloy are respectively improved from 692.2MPa, 772.3MPa and 28.7 percent to 773.6MPa, 897.7MPa and 34.6 percent after the total predeformation is 40 percent; respectively increased by 11.7%, 16.2% and 20.8%.
Description
Technical Field
The invention relates to a method for improving the strong plasticity of a multi-component alloy, in particular to a method for improving the strong plasticity of the multi-component alloy based on annealing hardening, and belongs to the technical field of metal plasticity.
Background
The single-phase face-centered cubic multicomponent alloy has attracted people's attention due to its excellent low-temperature mechanical properties. Among the many equal atomic ratio multicomponent alloys are: CoCrNi, CoCrFeNi, CoCrFeMnNi, etc., CoCrNi shows better yield strength, tensile strength and plasticity. (Z.Wu, H.Bei, G.M.Pharr, et al.temperature dependency of the mechanical properties of electronic devices with surface-centered cubic crystal structures [ J ]. Acta material 81(2014) 428-. In order to achieve the requirement that the commercial alloy has tensile strength in the range of 900-2400 MPa and yield strength in the range of 500-2200 MPa, researchers have proposed a plurality of methods to improve the strength of CoCrNi and maintain good plasticity. Such as: wang et al used a spark plasma sintering method to add 5 wt.% of Mo element to a CoCrNi matrix, and the mu phase precipitated from the CoCrNi matrix increased the yield strength from 352MPa to 815MPa and still maintained near 25% plasticity. Lu et Al introduced 0-30 at.% Al atoms into the CoCrNi matrix, and since Al has a larger atomic radius and electronegativity than the matrix elements, the alloy changes from single-phase FCC to FCC plus BCC to dual-phase BCC as the Al elements increase, the solid solution strengthening effect of the Al atoms and the increase of the BCC phase increase the compressive strength of the original CoCrNi from 204MPa to 1792 MPa. (Jianying Wang, Hailin Yang, Hua Huang et Al. in-situ modified CoCrNi media entry alloy [ J ]. Journal of Alloys and Compounds 798(2019)576E586.Wenjie Lu, Xian Luo, Yanqing Yang, et Al. effects of Al addition on structural evaluation and mechanical properties of the CrCoNi media entry alloy [ J ]. Materials Chemistry and Physics 238 (2019)) for centuries, the development of metallic structural Materials has still relied primarily on alloying techniques, i.e. combining metals and other elements to achieve the desired properties, the purpose of which is to alter the electronic and lattice properties of the substrate, or to have alternative phase properties to those of the substrate. The mechanical properties of the CoCrNi alloy can be effectively adjusted by adjusting the composition of the CoCrNi alloy and adding other metal elements. However, alloying makes material development more resource-dependent, exposing it to the risk of gradual depletion of resources and unavailability of key elements. Also the recovery of complex composition alloy materials becomes more difficult and, in addition, the overall production costs of the alloys are increasing, especially those containing precious metal alloying elements.
Li and Lu propose that the introduction of defect structures (vacancies, dislocations, grain boundaries or phase boundaries) into metal materials can efficiently and sustainably improve the properties of the metal materials, and the defects can replace alloying elements to adjust the properties of the materials without changing chemical compositions. (Xiuyan Li, K.Lu. Playing with defects in metals [ J ] Nature Materials 16(2017) 700. 701.) Deng et al introduced dislocations, faults, twins in the CoCrNi multicomponent alloy by equal channel extrusion, and adjusted the mechanical properties by adjusting the defect structure and density in the CoCrNi by different passes of equal channel extrusion, and the yield strength of the CoCrNi increased from 200MPa to 829MPa, 1068MPa and 1191MPa respectively after 1 pass, 2 passes and 3 passes of equal channel extrusion, and still maintained 9% plasticity after 3 passes. The method is characterized in that after CoCrNi is subjected to 3-pass equal-channel extrusion and annealed for 1 hour at 300-1000 ℃, Vickers hardness and yield strength of the CoCrNi show a trend of increasing firstly and then decreasing, the strength reaches a peak value when the CoCrNi is annealed for 1 hour at 500 ℃, the yield strength reaches 1298MPa, the plasticity is 4%, and the authors believe that the CoCrNi generates a nano twin crystal and HCP phase composite structure at low temperature annealing to promote the strength of the CoCrNi. (H.W.Deng, Z.M.Xie, B.L.Zhao et al.Tailliming mechanical properties of a CoCrNi media-even by controlling nano-steel-HCP lamellae and connecting wires [ J ] Materials Science & Engineering A744 (2019) 241-246.) it can be seen that low temperature annealing after cold deformation or cold deformation is an effective method for improving the strength of a metal material.
There are many phenomena like the increase in strength caused by low temperature annealing (below recrystallization temperature) after large deformation, such as: cu alloy, Mg alloy, CoCrFeMnNi and other multicomponent alloys, but the hardening increment is not very large (< 15%), and the annealing hardening effect needs to be improved while other alloying elements are not introduced. And the large-deformation metal has high strength, but has large plastic sacrifice, uneven defect structure and instability, is not beneficial to the practical application of engineering structure, improves the strength of the large-deformation metal after low-temperature annealing, but the plasticity can be further reduced, Gu et al also observe a hardening phenomenon after the high-pressure twisted CoCrFeMnNi multi-component alloy is annealed at low temperature, the strength is increased to 1300MPa from 1150MPa, and the plasticity is almost reduced to zero, (Ji Gu, Min Song.Annealing-induced plasticity alloying in a cold rolled CrMnFeCoNi high even alloy [ J ]. Scripta Materialia 162(2019) 345. 349.), therefore, the method of combining repeated predeformation and post low-temperature annealing (500 ℃) is adopted, the strength and the plasticity are simultaneously improved, the yield strength is improved by 11.7 percent, the tensile strength is improved by 16.2 percent, the plasticity is improved by 20.8 percent, and the high-pressure twisted CoCrFeMnNi multi-component alloy has wide application prospect in engineering structural materials.
Disclosure of Invention
The invention aims to introduce a defect structure into a metal material to replace alloying elements to regulate and control the performance of the material, and develops a method for low-temperature annealing after repeated predeformation of a CoCrNi multi-component alloy on the problems of small low-temperature annealing hardening effect, rapid reduction of plasticity and the like of the traditional metal material after cold deformation. Provides a way for reducing the use of alloying elements, saving resources and reducing cost, and provides wide application prospect for manufacturing key parts in the fields of national defense, military industry and the like.
In order to achieve the purpose, the invention provides the following technical scheme: the method comprises the following steps:
s1: mixing three elements of transition metal cobalt, chromium and nickel according to equal atomic ratio or approximate equal atomic ratio, preparing CoCrNi multi-component alloy by adopting a vacuum induction melting method, and then carrying out high-temperature homogenization treatment;
s2: introducing different deformation quantities into the CoCrNi multi-component alloy in a cold rolling deformation mode, annealing samples of each deformation quantity at 100-800 ℃ for 1h at intervals of 100 ℃, cooling along with a furnace, and observing the micro Vickers hardness of the samples of each deformation quantity at different temperatures;
s3: introducing a certain deformation amount to the multicomponent alloy by a deformation mode of room-temperature uniaxial stretching, wherein pre-deformed stretching samples are divided into two groups, one group is not subjected to annealing treatment after pre-deformation, and the other group is subjected to low-temperature annealing treatment after pre-deformation;
s4: the two groups of CoCrNi multi-component alloys are subjected to independent pre-deformation and low-temperature annealing treatment respectively, and then subjected to uniaxial tensile test.
As a preferred technical solution of the present invention, the size of the cobalt, chromium, and nickel metal particles used in step S1 is about 3 to 10 mm; the temperature of vacuum induction melting is more than 2000 ℃, and the technological parameters are as follows: the current is 400-450A, the water-cooled copper mold is cooled, and the smelting times are 3-5 times; the high temperature homogenization condition is that annealing is carried out for 4 hours at 1200 ℃, and then water quenching is carried out.
In a preferred embodiment of the present invention, the multicomponent alloy in step S1 has a single-phase face-centered cubic crystal structure as a main matrix phase; is a substitutional solid solution alloy; no obvious oxide inclusion or casting defect (such as segregation, shrinkage cavity and the like).
In a preferred embodiment of the present invention, the deformation amount introduced to the CoCrNi multi-component alloy by the cold rolling deformation manner in step S2 is 20%, 40%, 60%, 80%, 90%, and the micro vickers hardness of the same deformation sample shows a tendency of increasing first and then decreasing with increasing temperature, and the peak temperature is 500 ℃.
In a preferred embodiment of the present invention, the pre-deformation amount in step S3 is 5%, and the heat treatment after pre-deformation is performed under the conditions of 500 ℃ annealing for 1 hour and water quenching.
In a preferred embodiment of the present invention, the number of times of repeating the pre-deformation and the low temperature annealing in step S4 is 5, and the 5 times of pre-deformation are gradually accumulated, and the number of times of pre-deformation is as follows: 5 percent, 10 percent, 20 percent, 30 percent, 40 percent and 5 times of heat treatment are annealed for 1 hour at 500 ℃ and then water quenched.
As a preferred technical scheme of the invention, after the repeated predeformation and low-temperature annealing are carried out for 5 times in the step S4, and the total predeformation is 40%, compared with the CoCrNi multi-component alloy which is repeatedly predeformed and is not annealed at low temperature, the yield strength of the water-quenched CoCrNi multi-component alloy is improved by 11.7%, the tensile strength is improved by 16.2%, and the plasticity is improved by 20.8% after annealing for 1h at 500 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. compared with other modes of introducing defects by cold deformation (rolling, equal-channel extrusion, high-pressure torsion and the like), the method for improving the strong plasticity of the multicomponent alloy based on annealing hardening has the advantages of uniform defect introducing structure, simplicity in operation, cost saving and the like.
2. According to the method for improving the strength and plasticity of the multi-component alloy based on annealing hardening, the yield strength, the tensile strength and the plasticity of the CoCrNi multi-component alloy are respectively improved from 692.2MPa, 772.3MPa and 28.7% to 773.6MPa, 897.7MPa and 34.6% after the total pre-deformation is 40%; respectively increased by 11.7%, 16.2% and 20.8%.
Drawings
FIG. 1 shows the micro-hardness curves of CoCrNi at different rolling amounts at 100-800 ℃;
FIG. 2 shows engineering stress-strain plots for two sets of alloys that were not and not low temperature annealed after pre-deformation;
FIG. 3 shows a graph comparing the yield strength of two sets of alloys that were not and not low temperature annealed after different prestrains.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-3, the present invention provides a method for improving the strength and plasticity of a multi-component alloy based on annealing hardening, which comprises the following steps:
example 1
Pre-deforming the CoCrNi multicomponent alloy by 10% and then annealing at low temperature. The method comprises the following specific steps:
(1) preparing a CoCrNi multi-component alloy: the method comprises the steps of smelting Co, Cr and Ni particles with equal atomic ratio weighed in advance into ingots with the size of 80mm multiplied by 55mm multiplied by 15mm by adopting an induction smelting method, wherein the purity of the Co, Cr and Ni particles is more than 99.5%, the size of the Co, Cr and Ni particles is 3-10 mm, the induced current is 450A, and the smelting temperature is about 2000 ℃. Annealing the smelted cast ingot at 1200 ℃ for 4h to homogenize;
(2) making CoCrNi multi-component alloy with different deformation: then cutting out 5 samples with the height of 10mm by using a wire-cut electric discharge machine, polishing the surfaces of the samples by using 2000-mesh abrasive paper, and then carrying out cold rolling, wherein the cold rolling accounts for 20%, 40%, 60%, 80% and 90% respectively;
(3) the annealing hardening peak temperature is explored: annealing the CoCrNi multi-component alloy with different deformation amounts at 100-800 ℃ for 1h at intervals of 100 ℃, cooling the alloy along with a furnace, grinding and polishing the annealed sample, and observing the micro Vickers hardness;
(4) pre-deformation of 5% and low-temperature annealing: preparing a plate-shaped tensile sample with the gauge length of 17mm multiplied by 5mm multiplied by 2mm by using wire-cut electric discharge machining equipment, firstly pre-deforming the tensile sample by 5 percent, dividing the tensile sample into two groups, wherein one group does not carry out annealing treatment, and the other group carries out annealing treatment at 500 ℃ for 1 h;
(5) 5% of secondary deformation and low-temperature annealing: and (3) performing secondary pre-deformation for 5% on the tensile sample which is subjected to the pre-deformation of 5% and the annealing treatment at 500 ℃ for 1h, and also performing annealing treatment at 500 ℃ for 1h on the sample subjected to the annealing treatment in the step (4). Thus, a sample was obtained which had been pre-deformed by 10% and annealed at 500 ℃ for 1 hour.
As can be seen from FIG. 1, the Vickers hardness values of CoCrNi multi-component alloys with different deformation amounts show a trend of decreasing after increasing with the temperature, and the peak temperature is 500 ℃, so the low-temperature annealing temperature after pre-deformation is 500 ℃; as can be seen from the engineering stress-strain curve of FIG. 2 and the yield strength plot of FIG. 3, the yield strength of the annealed samples increased from 369.5MPa to 394.8MPa when annealed at 500 deg.C for 1h after 10% pre-strain.
Example 2
Pre-deforming the CoCrNi multicomponent alloy by 20% and then annealing at low temperature. The method comprises the following specific steps:
(1) preparing a CoCrNi multi-component alloy: the method comprises the steps of smelting Co, Cr and Ni particles with equal atomic ratio weighed in advance into an ingot with the size of 80mm multiplied by 55mm multiplied by 15mm by adopting an induction smelting method, wherein the purity of the Co, Cr and Ni particles is more than 99.5%, the size of the Co, Cr and Ni particles is 3-10 mm, the induced current is 450A, and the smelting temperature is about 2000 ℃. Annealing the smelted cast ingot at 1200 ℃ for 4h to homogenize;
(2) making CoCrNi multi-component alloy with different deformation: then cutting out 5 samples with the height of 10mm by using a wire-cut electric discharge machine, polishing the surfaces of the samples by using 2000-mesh abrasive paper, and then carrying out cold rolling, wherein the cold rolling accounts for 20%, 40%, 60%, 80% and 90% respectively;
(3) the annealing hardening peak temperature is explored: annealing the CoCrNi multi-component alloy with different deformation amounts at 100-800 ℃ for 1h at intervals of 100 ℃, cooling the alloy along with a furnace, grinding and polishing the annealed sample, and observing the micro Vickers hardness;
(4) pre-deformation of 5% and low-temperature annealing: preparing a plate-shaped tensile sample with the gauge length of 17mm multiplied by 5mm multiplied by 2mm by using wire-cut electric discharge machining equipment, firstly pre-deforming the tensile sample by 5 percent, dividing the tensile sample into two groups, wherein one group does not carry out annealing treatment, and the other group carries out annealing treatment at 500 ℃ for 1 h;
(5) 5% of secondary deformation and low-temperature annealing: and (3) performing secondary pre-deformation for 5% on the tensile sample which is subjected to the pre-deformation of 5% and the annealing treatment at 500 ℃ for 1h, and also performing annealing treatment at 500 ℃ for 1h on the sample subjected to the annealing treatment in the step (4). Thus obtaining a sample which is pre-deformed by 10 percent and annealed for 1h at 500 ℃;
(6) re-deformation by 10% and low-temperature annealing: the above two groups of stretched samples which were 5% re-deformed and not annealed at 500 ℃ for 1 hour were re-deformed by 10%, and similarly, the samples annealed at step (5) were also annealed at 500 ℃ for 1 hour. Thus, a sample with 20% pre-deformation and 1h annealing at 500 ℃ can be obtained.
From the engineering stress-strain curve of fig. 2 and the yield strength plot of fig. 3, it can be seen that the yield strength of the annealed samples increased from 476.6MPa to 509.6MPa when pre-strained at 20% and annealed at 500 ℃ for 1 h.
Example 3
Pre-deforming the CoCrNi multicomponent alloy by 40% and then annealing at low temperature. The method comprises the following specific steps:
(1) preparing a CoCrNi multi-component alloy: the method comprises the steps of smelting Co, Cr and Ni particles with equal atomic ratio weighed in advance into ingots with the size of 80mm multiplied by 55mm multiplied by 15mm by adopting an induction smelting method, wherein the purity of the Co, Cr and Ni particles is more than 99.5%, the size of the Co, Cr and Ni particles is 3-10 mm, the induced current is 450A, and the smelting temperature is about 2000 ℃. Annealing the smelted cast ingot at 1200 ℃ for 4h to homogenize;
(2) making CoCrNi multi-component alloy with different deformation: then cutting out 5 samples with the height of 10mm by using a wire cut electric discharge machine, polishing the surfaces of the samples by using 2000-mesh sand paper, and then performing cold rolling, wherein the cold rolling accounts for 20%, 40%, 60%, 80% and 90% respectively;
(3) the annealing hardening peak temperature is explored: annealing the CoCrNi multi-component alloy with different deformation amounts at 100-800 ℃ for 1h at intervals of 100 ℃, cooling the alloy along with a furnace, grinding and polishing the annealed sample, and observing the micro Vickers hardness;
(4) pre-deformation of 5% and low-temperature annealing: preparing a plate-shaped tensile sample with the gauge length of 17mm multiplied by 5mm multiplied by 2mm by using wire-cut electric discharge machining equipment, firstly pre-deforming the tensile sample by 5 percent, dividing the tensile sample into two groups, wherein one group does not carry out annealing treatment, and the other group carries out annealing treatment at 500 ℃ for 1 h;
(5) 5% of secondary deformation and low-temperature annealing: and (3) performing secondary pre-deformation for 5% on the tensile sample which is subjected to the pre-deformation of 5% and the annealing treatment at 500 ℃ for 1h, and also performing annealing treatment at 500 ℃ for 1h on the sample subjected to the annealing treatment in the step (4). Thus obtaining a sample which is pre-deformed by 10 percent and annealed for 1h at 500 ℃;
(6) re-deformation by 10% and low-temperature annealing: the above two groups of stretched samples which were 5% re-deformed and not annealed at 500 ℃ for 1 hour were re-deformed by 10%, and similarly, the samples annealed at step (5) were also annealed at 500 ℃ for 1 hour. Thus obtaining a sample which is pre-deformed by 20 percent and is annealed for 1h at 500 ℃;
(7) re-deformation by 10% and low-temperature annealing: the above two groups of stretched samples which were 5% re-deformed and 1h annealed at 500 ℃ were re-deformed by 10%, and similarly, the samples annealed in step (6) were also annealed at 500 ℃ for 1 h. Thus obtaining a sample which is pre-deformed by 30 percent and annealed for 1h at 500 ℃;
(8) re-deformation by 10% and low-temperature annealing: the above two groups of stretched samples which were 5% re-deformed and 1h annealed at 500 ℃ were re-deformed by 10%, and similarly, the samples annealed in step (7) were also annealed at 500 ℃ for 1 h. Thus, a sample was obtained which had been pre-deformed by 40% and annealed at 500 ℃ for 1 hour.
As can be seen from the engineering stress-strain curve of FIG. 2 and the yield strength plot of FIG. 3, when the pre-strain is 40% and annealed at 500 ℃ for 1h, the yield strength, tensile strength and plasticity of the annealed samples are respectively increased from 692.2MPa, 772.3MPa, 28.7% to 773.6MPa, 897.7MPa and 34.6% as compared to the unannealed samples; respectively increased by 11.7%, 16.2% and 20.8%.
In the description of the present invention, it is to be understood that the ease of description and simplicity of description are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and is not to be considered limiting.
In the present invention, unless otherwise explicitly specified or limited, for example, it may be fixedly attached, detachably attached, or integrated; can be mechanically or electrically connected; the terms may be directly connected or indirectly connected through an intermediate, and may be communication between two elements or interaction relationship between two elements, unless otherwise specifically limited, and the specific meaning of the terms in the present invention will be understood by those skilled in the art according to specific situations.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. A method for improving the strength and the plasticity of a multi-component alloy based on annealing hardening is characterized by comprising the following steps:
s1: mixing three elements of transition metal cobalt, chromium and nickel according to equal atomic ratio, preparing CoCrNi multi-component alloy by adopting a vacuum induction melting method, then carrying out high-temperature homogenization treatment, annealing at 1200 ℃ for 4h under the high-temperature homogenization condition, and then carrying out water quenching;
s2: introducing different deformation quantities into the CoCrNi multi-component alloy in a cold rolling deformation mode, annealing samples of each deformation quantity at 100-800 ℃ for 1h at intervals of 100 ℃, cooling along with a furnace, and observing the micro Vickers hardness of the samples of each deformation quantity at different temperatures;
s3: introducing a certain deformation amount to the multicomponent alloy by a deformation mode of room-temperature uniaxial stretching, wherein pre-deformed stretching samples are divided into two groups, one group is not subjected to annealing treatment after pre-deformation, and the other group is subjected to low-temperature annealing treatment after pre-deformation; wherein the pre-deformation amount is 5%, the low-temperature annealing condition after pre-deformation is that annealing is carried out for 1h at 500 ℃, and then water quenching is carried out;
s4: the two groups of CoCrNi multi-component alloys are subjected to independent repeated predeformation and low-temperature annealing treatment respectively and then subjected to uniaxial tensile test; the times of repeated predeformation and low-temperature annealing are 5 times, and the 5 times of predeformation are gradually accumulated and respectively: 5%, 10%, 20%, 30%, 40%, 5 times of low temperature annealing conditions are all 500 ℃ annealing for 1h, and then water quenching is carried out; after 5 times of repeated predeformation and low-temperature annealing, the total predeformation amount is 40%, compared with the CoCrNi multi-component alloy which is repeatedly predeformed and is not annealed at low temperature, the yield strength of the water-quenched CoCrNi multi-component alloy is improved by 11.7% after annealing for 1h at 500 ℃, the tensile strength is improved by 16.2%, and the plasticity is improved by 20.8%.
2. The method for improving the strength and the plasticity of the multi-component alloy based on annealing hardening as claimed in claim 1, wherein the annealing hardening is performed by the following steps: the sizes of the cobalt, chromium and nickel metal particles used in the step S1 are 3-10 mm; the temperature of vacuum induction melting is more than 2000 ℃, and the technological parameters are as follows: the current is 400-450A, and the water-cooled copper mold is cooled for 3-5 times.
3. The method for improving the strength and the plasticity of the multi-component alloy based on annealing hardening as claimed in claim 1, wherein the annealing hardening is performed by the following steps: the multicomponent alloy of step S1 having a single-phase face-centered cubic crystal structure as the main matrix phase; is a substitutional solid solution alloy; no obvious oxidation inclusion or casting defect.
4. The method for improving the strength and the plasticity of the multi-component alloy based on annealing hardening as claimed in claim 1, wherein the annealing hardening is performed by the following steps: in the step S2, the deformation amount introduced to the CoCrNi multi-component alloy by the cold rolling deformation mode is 20%, 40%, 60%, 80% and 90%, the micro Vickers hardness of the same deformation sample shows a trend of increasing firstly and then decreasing with the increase of the temperature, and the peak temperature is 500 ℃.
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