CN112048682B - Processing heat treatment process for medium-entropy alloy plate - Google Patents
Processing heat treatment process for medium-entropy alloy plate Download PDFInfo
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- CN112048682B CN112048682B CN202010892697.3A CN202010892697A CN112048682B CN 112048682 B CN112048682 B CN 112048682B CN 202010892697 A CN202010892697 A CN 202010892697A CN 112048682 B CN112048682 B CN 112048682B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
Abstract
The invention relates to a processing heat treatment process of a medium-entropy alloy plate, which comprises the following steps: s1: preparing a first alloy ingot; s2: carrying out heat treatment on the first alloy ingot to obtain a second alloy ingot; s3: carrying out first cold rolling on the second alloy ingot at room temperature, and controlling the deformation amount of the second alloy ingot to be 50-70% to obtain a third alloy ingot; s4: carrying out heat treatment on the third alloy ingot to obtain a fourth alloy ingot; s5: carrying out secondary cold rolling on the fourth alloy ingot at room temperature, and controlling the deformation amount to be 20-55% to obtain a fifth alloy ingot; then, performing cold rolling for the third time after cooling the fifth alloy ingot at low temperature, and controlling the deformation amount of the fifth alloy ingot to be between 40 and 60 percent so as to obtain a sheet; s6: the sheet is heat treated a third time. The alloy plate prepared by the processing heat treatment process of the medium-entropy alloy plate provided by the invention has the advantages of uniform component distribution, obviously improved strength and excellent mechanical property.
Description
Technical Field
The invention relates to the technical field of alloy plate manufacturing, in particular to a processing heat treatment process of a medium-entropy alloy plate.
Background
The advent of multi-principal alloy provides a new alloy design idea for material researchers, breaking the concept of traditional alloys with one or two elements as principal elements, and multi-principal alloy usually consists of more than 3 principal elements, forming simple single-phase solid solution structure, such as FCC (Face Center Cubic), BCC (Body-centered Cubic), or HCP (Hexagonal close packed) structure solid solution. The multi-principal-element alloy has a series of excellent performances such as high strength, high hardness, high wear resistance, high-temperature oxidation resistance, high corrosion resistance, good thermal stability and the like, and has a very wide application prospect.
CoCrNi multi-principal element alloy, also called mid-entropy alloy, is a single-phase FCC solid solution structure. Different from the characteristic that the strength of a common metal material is increased at low temperature but the ductility and the toughness are reduced, the strength and the plasticity of the CoCrNi intermediate entropy alloy are simultaneously increased at low temperature, the CoCrNi intermediate entropy alloy is a low-temperature structural material with great application potential, and has great application potential in the fields of aviation, aerospace and the like. However, although the CoCrNi alloy has good plasticity, the strength is low, and the application of the CoCrNi alloy as a high-performance structural material is greatly limited.
The deformation strengthening is an effective means for improving the performance of the alloy, such as rolling, die forging, extrusion and the like. The deformation strengthening usually involves complex process parameters, and the deformation, the deformation times, the deformation temperature and the like all have very important influence on the alloy performance. Generally, the deformation strengthening can effectively improve the strength of the alloy, but improper control often leads to great reduction of the plasticity of the alloy. How to control the technological parameters to obtain the alloy plate with high strength and good plasticity is still the technical problem faced at present.
Disclosure of Invention
The invention aims to provide a processing heat treatment process of a medium-entropy alloy plate, so that the prepared medium-entropy alloy plate is high in strength and good in plasticity.
The invention provides a processing heat treatment process of a medium-entropy alloy plate, which comprises the following steps:
s1: preparing a metal raw material into a first alloy ingot;
s2: carrying out primary heat treatment on the first alloy ingot to obtain a second alloy ingot;
s3: carrying out first cold rolling on the second alloy ingot at room temperature, and controlling the deformation of the second alloy ingot to be 50-70% in the rolling process to obtain a third alloy ingot;
s4: carrying out second heat treatment on the third alloy ingot to obtain a fourth alloy ingot;
s5: carrying out second cold rolling on the fourth alloy ingot at room temperature for 2-6 passes, and controlling the deformation of the fourth alloy ingot to be 20-55% to obtain a fifth alloy ingot; then, the fifth alloy ingot is put into a vacuum flask filled with liquid nitrogen or liquid helium to be cooled for 10-80 minutes, then is subjected to cold rolling for 4-10 passes for the third time, and the deformation of the fifth alloy ingot is controlled to be 40-60 percent, so that a sheet is obtained;
s6: and carrying out third heat treatment on the thin plate.
Further, the atomic composition of the medium entropy alloy sheet material is CoxCryNi1-x-yWherein the value ranges of x and y are both 0.3-0.35.
Further, the first heat treatment and the second heat treatment are both performed in an argon or vacuum environment.
Further, the temperature of the first heat treatment is controlled between 1000 ℃ and 1300 ℃, and the time is 10-30 h.
Further, the temperature of the second heat treatment is controlled between 750 ℃ and 950 ℃ for 0.5-3 h.
Further, the third heat treatment is performed in air.
Further, the temperature of the third heat treatment is controlled between 350 ℃ and 800 ℃ and the time is 0.5-2 h.
Further, the first cold rolling, the second cold rolling and the third cold rolling are all completed by adopting symmetrical compression rollers.
Further, the rolling speeds of the first cold rolling, the second cold rolling and the third cold rolling are all 5-10 m/min.
Further, the first cold rolling, the second cold rolling and the third cold rolling are always performed in the same direction.
The processing heat treatment process of the medium-entropy alloy plate provided by the invention has the following beneficial effects:
1. by utilizing the severe plastic deformation at room temperature and ultra-low temperature, the dislocation and twin crystal in the alloy start to deform, and the defect density as large as possible is generated, so that the mechanical property of the medium-entropy alloy plate is improved, the tensile strength can reach 1.6Gpa, the breaking strain can reach 20%, and the strength is obviously improved compared with the plate prepared by other processes.
2. By combining rolling with three times of heat treatment, the problems of component segregation, coarse grains and the like in the material are effectively eliminated, the alloy structure is fine, the components are uniformly distributed, and the mechanical property is very excellent.
3. The method has simple process and strong applicability, and can be popularized in medium-entropy alloys of other components, thereby obtaining the high-performance alloy plate.
Drawings
FIG. 1 is a flow chart of a processing heat treatment process of a medium-entropy alloy plate provided by an embodiment of the invention;
fig. 2 is an XRD spectrum of the medium-entropy alloy sheet in scheme 1, scheme 2 and scheme 3 provided by the embodiment of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
As shown in fig. 1, an embodiment of the present invention provides a processing heat treatment process for a medium-entropy alloy plate, including the following steps:
s1: preparing a metal raw material into a first alloy ingot.
Specifically, according to the components of each metal in the medium-entropy alloy, Co, Cr and Ni metals are prepared into a first alloy ingot by an arc melting method. Putting Co, Cr and Ni metal raw materials into an electric arc melting furnace, vacuumizing the melting furnace, filling high-purity protective gas, adjusting melting current to completely melt the metal raw materials, and turning over for one time to continue melting after the metal raw materials are melted into alloy ingots; in order to make the medium-entropy alloy components uniform, magnetic stirring is started for 10s during each smelting, the alloy is repeatedly turned over and smelted for 4-5 times, and a first alloy ingot is obtained after the alloy is cooled along with the furnace.
The high-purity protective gas can be high-purity argon with the purity of 99.999 percent, and the smelting current can be set between 200 and 350A.
In a possible embodiment, the atomic composition of the medium entropy alloy is CoxCryNi1-x-yWherein the value ranges of x and y are both 0.3-0.35, and the metal raw materials can be weighed according to the proportion when the alloy ingot is prepared.
S2: and carrying out primary heat treatment on the first alloy ingot to obtain a second alloy ingot.
The first heat treatment can be carried out in an argon or vacuum environment, and the temperature is controlled between 1000 ℃ and 1300 ℃ for 10-30 h.
S3: and carrying out first cold rolling on the second alloy ingot at room temperature, wherein the deformation of the second alloy ingot is controlled to be 50-70% in the rolling process, so as to obtain a third alloy ingot.
The rolling can be completed by adopting symmetrical compression rollers, and the rolling speed is 5-10 m/min. During the rolling process, the rolling is always carried out along the same direction.
S4: and carrying out secondary heat treatment on the third alloy ingot to obtain a fourth alloy ingot.
The second heat treatment can be performed in an argon or vacuum environment, and the temperature is controlled at 750 ℃ and 950 ℃ for 0.5-3 h.
S5: performing secondary cold rolling on the fourth alloy ingot at room temperature for 2-6 passes, and controlling the deformation of the fourth alloy ingot to be 20-55% to obtain a fifth alloy ingot; and then, placing the fifth alloy ingot into a vacuum flask filled with liquid nitrogen or liquid helium to be cooled for 10-80 minutes, then carrying out cold rolling for 4-10 times for the third time, and controlling the deformation of the fifth alloy ingot to be between 40% and 60%, thereby obtaining the sheet.
The second cold rolling can be completed by adopting symmetrical compression rollers, and the rolling speed is 5-10 m/min. In the cold rolling, rolling is always performed in the same direction, and the rolling direction is the same as that in step S3.
The third cold rolling can also be completed by adopting symmetrical compression rollers, and the rolling speed is 5-10 m/min. In the cold rolling process, rolling is always carried out along the same direction, and the rolling direction is the same as that of cold rolling, so that uniform deformation can be ensured.
S6: and carrying out third heat treatment on the thin plate.
The third heat treatment can be carried out in air, and the temperature is controlled between 350 ℃ and 800 ℃ for 0.5-2 h.
According to the processing heat treatment process of the medium-entropy alloy plate provided by the embodiment of the invention, the severe plastic deformation at room temperature and ultra-low temperature is utilized, so that the dislocation and twin crystal deformation in the alloy start to generate the defect density as large as possible, the mechanical property of the medium-entropy alloy plate is improved, the tensile strength can reach 1.6Gpa, the breaking strain can reach 20%, and the strength is obviously improved compared with plates prepared by other processes.
According to the processing heat treatment process of the medium-entropy alloy plate, provided by the embodiment of the invention, the problems of component segregation, coarse grains and the like in the material are effectively solved by combining rolling with three heat treatments, and the medium-entropy alloy plate is fine in alloy structure, uniform in component distribution and very excellent in mechanical property. The process is simple and high in applicability, and can be popularized in medium-entropy alloys of other components, so that the high-performance alloy plate is obtained.
The following 3 practical schemes are taken as examples to illustrate the effect of the processing heat treatment process of the medium-entropy alloy plate provided by the embodiment of the invention.
Scheme 1
In the scheme, the component Co is based on the atomic percentage of the alloy35Cr32Ni33Weighing each pure metal raw material, wherein the total mass is 60g, and preparing an alloy ingot by adopting an electric arc melting method. And (3) placing the alloy ingot into a tube furnace for first heat treatment, vacuumizing the tube furnace, and then filling high-purity argon, wherein the set temperature is 1000 ℃, and the heat preservation time is 20 hours. And (3) rolling the alloy ingot after the first annealing at room temperature at the speed of 5m/min, repeatedly rolling in the same direction, and circulating for 5 times, wherein the single-pass rolling reduction is 10%. The alloy cast ingot after rolling is continuously put intoThe second heat treatment is carried out in a tubular furnace, the annealing temperature is 750 ℃, and the heat preservation time is 0.5 h. And after the second annealing, the alloy is cold-rolled for 4 passes at room temperature, and the single-pass deformation is 12%, so that the alloy plate is obtained. And then placing the alloy plate rolled at the room temperature into a vacuum flask filled with liquid nitrogen, cooling for 50 minutes, then rolling, and repeatedly rolling at the low temperature for 6 passes, wherein the single-pass deformation is 10%, so as to obtain the sheet. And finally, placing the cold-rolled and formed plate into a box furnace, and carrying out third heat treatment in air atmosphere, wherein the annealing temperature is 350 ℃ and the time is 0.5 h.
As shown in FIG. 2, the heat-treated Co was treated35Cr32Ni33Phase analysis is carried out on the alloy plate, and the alloy phase is still in an FCC structure after processing and heat treatment, the tensile strength of the alloy phase reaches 1600MPa, and the elongation of the alloy phase is 20%. Compared with the cast CoCrNi medium entropy alloy, the tensile strength is improved by about 290 percent.
Scheme 2
In the scheme, the component Co is based on the atomic percentage of the alloy35Cr32Ni33Weighing each pure metal raw material, wherein the total mass is 60g, and preparing an alloy ingot by adopting an electric arc melting method. And (3) placing the alloy ingot into a tube furnace for first heat treatment, vacuumizing the tube furnace, and then filling high-purity argon, wherein the set temperature is 1100 ℃, and the heat preservation time is 20 hours. And (3) rolling the alloy ingot after the first annealing at room temperature at the speed of 5m/min, repeatedly rolling in the same direction, and circulating for 5 times, wherein the single-pass rolling reduction is 10%. And (3) continuously putting the rolled alloy ingot into a tube furnace for secondary heat treatment, wherein the secondary heat treatment is also carried out in high-purity argon, the annealing temperature is 800 ℃, and the heat preservation time is 1.5 hours. And after the second annealing, the alloy is cold-rolled for 3 passes at room temperature, and the single-pass deformation is 15%, so that the alloy plate is obtained. And then placing the alloy plate rolled at the room temperature into a vacuum flask filled with liquid nitrogen, cooling for 50 minutes, then rolling, and repeatedly rolling at the low temperature for 5 passes, wherein the single-pass deformation is 10%, so as to obtain the sheet. And finally, placing the cold-rolled and formed plate into a box furnace, and carrying out third heat treatment in air atmosphere, wherein the annealing temperature is 600 ℃ and the time is 1 h.
As shown in FIG. 2, the heat-treated Co was treated35Cr32Ni33Phase analysis is carried out on the alloy plate, and the alloy phase is still in an FCC structure after processing and heat treatment, the tensile strength of the alloy plate reaches 1215MPa, and the elongation of the alloy plate is 29%. Compared with the cast CoCrNi medium entropy alloy, the tensile strength is improved by about 220 percent.
Scheme 3
In the scheme, the component Co is based on the atomic percentage of the alloy32Cr35Ni33Weighing each pure metal raw material, wherein the total mass is 60g, and preparing an alloy ingot by adopting an electric arc melting method. And (3) placing the alloy ingot into a tube furnace for first heat treatment, vacuumizing the tube furnace, and then filling high-purity argon, wherein the set temperature is 1200 ℃ and the heat preservation time is 30 hours. And (3) rolling the alloy ingot after the first annealing at room temperature at the speed of 5m/min, repeatedly rolling in the same direction, and circulating for 5 times, wherein the single-pass rolling reduction is 10%. And (3) continuously putting the rolled alloy ingot into a tube furnace for secondary heat treatment, wherein the secondary heat treatment is also carried out in high-purity argon, the annealing temperature is 800 ℃, and the heat preservation time is 1 h. And after the second annealing, the alloy is cold-rolled for 4 passes at room temperature, and the single-pass deformation is 10 percent, so that the alloy plate is obtained. And then placing the alloy plate rolled at the room temperature into a vacuum flask filled with liquid nitrogen, cooling for 50 minutes, then rolling, and repeatedly rolling at the low temperature for 5 passes, wherein the single-pass deformation is 8%, so as to obtain the sheet. And finally, placing the cold-rolled and formed plate into a box furnace, and carrying out third heat treatment in air atmosphere, wherein the annealing temperature is 700 ℃ and the time is 1 h.
As shown in FIG. 2, the heat-treated Co was treated32Cr35Ni33Phase analysis is carried out on the alloy plate, and the alloy phase is still in an FCC structure after processing and heat treatment, the tensile strength of the alloy plate reaches 1028MPa, and the elongation of the alloy plate is 43%. Compared with the cast CoCrNi medium entropy alloy, the tensile strength is improved by about 187 percent.
Therefore, the medium-entropy alloy plate prepared by the processing heat treatment process of the medium-entropy alloy plate provided by the embodiment of the invention has higher strength and better plasticity.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.
Claims (6)
1. The processing heat treatment process of the medium-entropy alloy plate is characterized in that the atomic composition of the medium-entropy alloy plate is CoxCryNi1-x-yWherein the value ranges of x and y are both 0.3-0.35, and the processing heat treatment process comprises the following steps:
s1: preparing a metal raw material into a first alloy ingot;
s2: carrying out primary heat treatment on the first alloy ingot to obtain a second alloy ingot, wherein the temperature of the primary heat treatment is controlled between 1000 ℃ and 1300 ℃ and the time is 10-30 h;
s3: carrying out first cold rolling on the second alloy ingot at room temperature, and controlling the deformation of the second alloy ingot to be 50-70% in the rolling process to obtain a third alloy ingot;
s4: carrying out second heat treatment on the third alloy ingot to obtain a fourth alloy ingot, wherein the temperature of the second heat treatment is controlled to be between 750 ℃ and 950 ℃ and the time is 0.5-3 h;
s5: carrying out second cold rolling on the fourth alloy ingot at room temperature for 2-6 passes, and controlling the deformation of the fourth alloy ingot to be 20-55% to obtain a fifth alloy ingot; then, the fifth alloy ingot is put into a vacuum flask filled with liquid nitrogen or liquid helium to be cooled for 10-80 minutes, then is subjected to cold rolling for 4-10 passes for the third time, and the deformation of the fifth alloy ingot is controlled to be 40-60 percent, so that a sheet is obtained;
s6: and carrying out third heat treatment on the thin plate, wherein the temperature of the third heat treatment is controlled between 350 ℃ and 800 ℃ and the time is 0.5-2 h.
2. The process for carrying out heat treatment on a medium-entropy alloy sheet according to claim 1, wherein the first heat treatment and the second heat treatment are carried out in an argon gas or vacuum environment.
3. The process for carrying out heat treatment on a medium-entropy alloy plate according to claim 1, wherein the third heat treatment is carried out in air.
4. A process for processing and heat treating a medium entropy alloy sheet according to claim 1, wherein the first cold rolling, the second cold rolling and the third cold rolling are all performed by symmetrical pressing rolls.
5. A process heat treatment process for a medium entropy alloy sheet according to claim 4, wherein the rolling speeds of the first cold rolling, the second cold rolling and the third cold rolling are all 5-10 m/min.
6. A process heat treatment process for a medium entropy alloy sheet according to claim 1, wherein the first cold rolling, the second cold rolling and the third cold rolling are performed in the same direction all the time.
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| CN115537687B (en) * | 2022-09-16 | 2023-06-13 | 华东理工大学 | Entropy alloy in multi-level twin crystal-stacking fault structure and preparation method thereof |
| CN115478201B (en) * | 2022-09-16 | 2023-07-28 | 华东理工大学 | CoNiV-based medium entropy alloy containing double ordered phases and preparation method thereof |
| CN115725887B (en) * | 2022-11-21 | 2023-09-19 | 广东省科学院中乌焊接研究所 | Medium-entropy alloy and preparation method and application thereof |
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| CN108906889A (en) * | 2018-05-08 | 2018-11-30 | 中南大学 | A kind of deep cooling asynchronous rolling method preparing high-performance CrCoNi medium entropy alloy foil |
| CN109201740A (en) * | 2018-11-15 | 2019-01-15 | 中南大学 | A kind of multistage deep cooling milling method preparing high density twin medium entropy alloy |
| CN110273095A (en) * | 2019-03-26 | 2019-09-24 | 东北大学 | A kind of preparation method of tensile strength 1.5GPa medium entropy alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108906889A (en) * | 2018-05-08 | 2018-11-30 | 中南大学 | A kind of deep cooling asynchronous rolling method preparing high-performance CrCoNi medium entropy alloy foil |
| CN109201740A (en) * | 2018-11-15 | 2019-01-15 | 中南大学 | A kind of multistage deep cooling milling method preparing high density twin medium entropy alloy |
| CN110273095A (en) * | 2019-03-26 | 2019-09-24 | 东北大学 | A kind of preparation method of tensile strength 1.5GPa medium entropy alloy |
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