CN114085969A - Preparation process of high-entropy alloy plate with heterogeneous laminated structure - Google Patents
Preparation process of high-entropy alloy plate with heterogeneous laminated structure Download PDFInfo
- Publication number
- CN114085969A CN114085969A CN202111350364.9A CN202111350364A CN114085969A CN 114085969 A CN114085969 A CN 114085969A CN 202111350364 A CN202111350364 A CN 202111350364A CN 114085969 A CN114085969 A CN 114085969A
- Authority
- CN
- China
- Prior art keywords
- entropy alloy
- cold
- temperature
- laminated
- rolling
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000956 alloy Substances 0.000 title claims abstract description 59
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims description 40
- 238000003466 welding Methods 0.000 claims description 28
- 238000000137 annealing Methods 0.000 claims description 24
- 238000005096 rolling process Methods 0.000 claims description 23
- 238000005097 cold rolling Methods 0.000 claims description 14
- 238000001953 recrystallisation Methods 0.000 claims description 14
- 238000005520 cutting process Methods 0.000 claims description 9
- 238000007731 hot pressing Methods 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 9
- 239000000725 suspension Substances 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000009792 diffusion process Methods 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000000265 homogenisation Methods 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 150000002739 metals Chemical class 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000010960 cold rolled steel Substances 0.000 claims description 2
- 241000764238 Isis Species 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 14
- 239000010410 layer Substances 0.000 description 12
- 238000011160 research Methods 0.000 description 10
- 235000012431 wafers Nutrition 0.000 description 10
- 238000003723 Smelting Methods 0.000 description 5
- 238000005728 strengthening Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 238000003475 lamination Methods 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 244000137852 Petrea volubilis Species 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 230000008520 organization Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 238000005482 strain hardening Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010273 cold forging Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000002173 cutting fluid Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
- C21D8/0236—Cold rolling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0247—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/07—Alloys based on nickel or cobalt based on cobalt
-
- 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
-
- 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
-
- 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
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
- B21B2001/386—Plates
Abstract
The invention relates to a preparation process of a heterogeneous laminated structure high-entropy alloy plate, belonging to the technical field of high-entropy alloy composite plate preparation. The heterostructure has nonuniform structures among layers and nonuniform tissue structures in the layers, and is particularly beneficial to the generation and storage of geometrical necessary dislocation due to the interface action among the layers, so that the deformation hardening capacity is improved in the strain process, the strong plasticity matching of the CoCrFeMnNi high-entropy alloy is improved to a certain extent, and the comprehensive mechanical property of the CoCrFeMnNi high-entropy alloy is improved.
Description
Technical Field
The invention belongs to the technical field of high-entropy alloy composite board preparation, and particularly relates to a preparation process of a high-entropy alloy board with a heterogeneous laminated structure.
Background
In view of the inherent properties of high-entropy alloys, the high-entropy alloys have very excellent performance in extreme environments (low-temperature or high-temperature environments), and are favored by those in the field of industrial research. However, the strength of the face-centered cubic high-entropy alloy is low at present, and particularly the yield strength of the single-phase high-entropy alloy is low, so that the wide application of the high-entropy alloy in the field of structural materials is limited.
Wu et al prepared a titanium plate of a heterogeneous stack structure in pure titanium by a simple asynchronous rolling and annealing process, which exhibited surprising mechanical properties, and the toughness and plasticity were greatly improved without a decrease in strength. However, the research is limited by equipment and other conditions, and related research on CoCrFeMnNi high-entropy alloy asynchronous rolling cannot be carried out in the research, but the research is carried out by Hanzhenhua and the like, and the research shows that compared with common rolling, the mechanical property of the asynchronously rolled plate is improved, and the surface layer and the core part of the plate have different grain sizes and are in a gradient structure. Inspired by research of Zhang Link et al, a heterogeneous laminated structure is regulated and controlled in IF steel through hot-press welding lamination, cold forging and annealing heat treatment, the IF steel plate with the structure greatly improves the comprehensive mechanical property of the IF steel, and improves the deformation hardening capacity.
Through analyzing the traditional strengthening mechanism of the high-entropy alloy and combining the excellent performance of the heterostructure material in strong plastic matching in recent years, it is not difficult to find that the organization structure of the general material is uniform, and the traditional strengthening mechanism regulates and controls the grain boundary and the phase in the material by changing the components, the structure and the like of the material with the uniform structure so as to ensure the dislocation plugging, and finally aims to improve the strength and the hardness of the material. However, a number of studies have shown that these ways of strengthening and toughening uniform structural materials consistently present a short slab that does not have the combination of strength and toughness. At present, the preparation mode of the heterostructure material is still not mature, so the preparation process is researched and clarified, the strengthening mechanism is explored, and the heterostructure material has very important significance for disclosing the strengthening and toughening mechanism existing behind the heterostructure material and improving the strong plastic matching relationship of the material.
Disclosure of Invention
The invention aims to overcome the defects in the background technology, and provides a preparation process of a high-entropy alloy plate with a heterogeneous laminated structure, which improves the comprehensive mechanical property of the CoCrFeMnNi high-entropy alloy, further optimizes the strong-toughness-plasticity matching relationship, saves resources and improves economic benefits.
The design concept of the invention is as follows:
research is carried out on the CoCrFeMnNi high-entropy alloy, the heterostructure high-entropy alloy is prepared, the original strong-plastic toughness matching relation and mechanical property of the heterostructure high-entropy alloy are improved on the basis, and the change of the organization structure of the heterostructure high-entropy alloy during plastic deformation is analyzed. The method comprises the steps of laminating cold-rolled and annealed CoCrFeMnNi high-entropy alloy plates, then performing hot-press welding, cold rolling and subsequent annealing heat treatment, and in the final annealing process, controlling the temperature to enable the previous cold-rolled plate to recover so as to keep ultrafine grains, and enabling original annealed coarse grains to grow and coarsen, so that the high-entropy alloy with the heterogeneous laminated structure is finally prepared. The heterostructure has nonuniform structures among layers, the structure in the layers is not uniform due to the effect of a preparation process, and the interface effect among the layers is particularly beneficial to the generation and storage of Geometric Necessary Dislocation (GND), so that the deformation hardening capacity is improved in the strain process, and the strong plasticity matching of the CoCrFeMnNi high-entropy alloy is improved to a certain extent.
The technical scheme adopted by the invention is as follows:
a preparation process of a high-entropy alloy plate with a heterogeneous laminated structure sequentially comprises the following steps:
s1, preparing as-cast CoCrFeMnNi high-entropy alloy cast ingot
Under the protection of a high-purity nitrogen atmosphere, putting a mixture of pure metals of Co, Cr, Fe, Mn and Ni with equal atomic ratio into a magnetic suspension melting furnace and melting, stirring by magnetic suspension during melting, and solidifying to obtain an as-cast CoCrFeMnNi high-entropy alloy ingot;
s2, homogenization treatment: the annealing temperature is 1000 ℃, and the heat preservation time is 8 hours;
s3, rolling at room temperature: cutting the homogenized CoCrFeMnNi high-entropy alloy cast ingot into a plurality of slabs according to the requirement, polishing the surfaces of the slabs, and performing cold rolling at room temperature, wherein the rolling deformation is 80 percent, so as to prepare a plurality of cold-rolled slabs;
s4, cutting off the edge of the cold-rolled plate blank for later use;
s5, recrystallization annealing: vacuumizing a heating furnace in advance by using a vacuum pump, setting the recrystallization annealing temperature to be 1000 ℃, setting the temperature rise rate to be 5 ℃/min, raising the temperature to a target temperature, then, sending the trimmed partial cold-rolled plate blank into the heating furnace for recrystallization annealing, and keeping the temperature for 1 hour;
s6, stacking high-entropy alloy plates: cleaning the surfaces of the cold-rolled plate blank prepared in the step S4 and the cold-rolled plate blank subjected to the recrystallization annealing treatment in the step S5, and then overlapping the cold-rolled plate blank and the cold-rolled plate blank in a staggered manner to prepare a laminated cylinder;
s7, hot-press welding of the laminated cylinders: the hot-press welding temperature is 600 ℃, the heating rate is 5 ℃/min, loads are applied to two ends of the laminated cylinder while the temperature is increased, and the strain rate is 0.01s-1Carrying out thermal insulation diffusion welding connection and hot pressing deformation through constant load force, wherein the hot pressing deformation is 35-40%, and preparing a laminated column blank;
s8, cold rolling of laminated column blanks: rolling the hot-press welded laminated column blank at room temperature, and further cold-rolling and deforming the hot-press welded sample for accumulating larger deformation amount, wherein the accumulated deformation amount is 90 percent, so as to prepare a heterogeneous laminated structure high-entropy alloy plate blank;
s9, heat treatment: and (3) vacuumizing the heating furnace in advance by using a vacuum pump, setting the heating temperature to be 600 ℃, the heating rate to be 5 ℃/min, heating to the target temperature, then keeping the temperature stable, putting the heterogeneous laminated structure high-entropy alloy plate blank prepared in the step S8 into the heating furnace for heating for 4 hours, taking out after the heat preservation is finished, and air-cooling to the room temperature to prepare the heterogeneous laminated structure high-entropy alloy plate.
Further, in the step S6, the rolling directions of the laminated high-entropy alloy sheet materials are consistent.
Further, the thickness of the final cold-rolled steel sheet obtained in step S8 is 1 mm.
Compared with the prior art, the invention has the beneficial effects that:
1. the high-entropy alloy cast ingot obtained by applying the magnetic suspension smelting technology has uniform structural components and basically no segregation phenomenon;
2. the hot-press welding quality of the laminated cylinder (cold-rolled and annealed plates) is closely related to the heat preservation time and the diameter of the cylinder. The temperature gradient exists between the laminated cylindrical core part and the surface layer due to too short heat preservation time, and the problems of cracking and dislocation can occur; too small a diameter may cause the laminated cylinder to distort during the hot press deformation stage, resulting in edge cracking. And the heat preservation time is prolonged to 30min, and when the diameter is increased to 15mm, the laminated cylinder does not generate dislocation during hot-pressing deformation.
3. The heterogeneous laminated structure is novel in that: firstly, the difference of tissues among layers comprises grain size, dislocation density and the like; secondly, the special structure of 'hard phase surrounding soft phase' exists in the inner layer structure, which benefits from the particularity of the preparation process, and in addition, the heterogeneous laminated structure comprises a plurality of interfaces, namely the interfaces between layers. The characteristics are all helpful for generating and storing the dislocation which is necessary for geometry to coordinate plastic deformation, and the deformation hardening capacity of the plastic deformation is improved in the actual mechanical property test.
Drawings
FIG. 1 is a schematic view of a thermal compression bonding process of the present invention. In the drawings, (a) shows the lamination, fig. (b) shows the thermocompression bonding, fig. (c) shows the cold rolling deformation, and fig. (d) shows the heat treatment.
Fig. 2 is a graph of the mechanical properties (engineering stress-strain) of the samples.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. Unless otherwise specified, the examples follow conventional experimental conditions. In addition, it will be apparent to those skilled in the art that various modifications or improvements can be made to the material components and amounts in these embodiments without departing from the spirit and scope of the invention as defined in the appended claims.
A preparation process of a high-entropy alloy plate with a heterogeneous laminated structure comprises the following steps:
s1, preparing an as-cast CoCrFeMnNi high-entropy alloy ingot:
under the protection of a high-purity nitrogen atmosphere, putting a mixture of pure metals (with the purity of more than 99.7 wt.%) of Co, Cr, Fe, Mn and Ni with equal atomic ratio into a magnetic suspension melting furnace and melting, in order to ensure the uniformity of components, adopting magnetic suspension stirring during melting, and obtaining an as-cast CoCrFeMnNi high-entropy alloy ingot after solidification; in this example, the surface of the high-entropy alloy ingot was uneven and was cut by a lathe to obtain an ingot having a diameter of 105mm and a height of 42 mm. The high-entropy alloy smelting does not need to be repeated for many times like an electric arc smelting process, and the ingot with good component uniformity can be obtained only through one-time magnetic suspension smelting, so that the process is simplified, the energy is saved, the generation of waste gas during smelting is reduced, and the serious pollution to the environment is avoided.
S2, homogenization treatment: the annealing temperature is 1000 ℃, and the holding time is 8 hours, so as to ensure that the dendritic crystal segregation is further eliminated.
S3, rolling at room temperature: cutting the homogenized CoCrFeMnNi high-entropy alloy cast ingot into a plurality of slabs according to the requirement, polishing the surfaces of the slabs, and performing cold rolling at room temperature, wherein the rolling deformation is 80 percent, so as to prepare a plurality of cold-rolled slabs; in the embodiment, an electric spark cutting machine is used for cutting the CoCrFeMnNi high-entropy alloy cast ingot into a plate with a certain thickness, and then the thickness of the plate blank after being polished is 5 mm; the rolling mill used in the embodiment is a weighted phi 250X300 two-roll cold rolling mill produced by the mechanical Limited company of vibration far from the City, and the rolling working principle is that when a rolled piece is contacted with symmetrically installed working rolls, a speed reduction motor enables the two working rolls to rotate reversely at the same rotating speed through gear transmission, and the rolled piece is meshed into the rolls by the working rolls under the action of friction force to finish one-pass rolling.
S4, cutting off the edge of the cold-rolled plate blank for later use;
the cold-rolled sheet was cut into round pieces with a diameter of 15mm using a wire electric discharge machine, and it was noted here that for the subsequent division of the Rolling direction, 1mm was cut away from the outermost radius of the round piece in a direction perpendicular to the Rolling-direction (RD). Since the rolled sheet material has grains crushed in the rolling direction and the grain size is between 100nm and 1um, the wafer in the cold rolled state is referred to as UFG (Ultra-fine grain) for the sake of convenience of explanation.
S5, recrystallization annealing: in order to avoid surface oxidation, a vacuum pump is used for vacuumizing a heating furnace in advance, the recrystallization annealing temperature is set to be 1000 ℃, the temperature rise rate is 5 ℃/min, the temperature is stabilized after the temperature is raised to the target temperature, then the trimmed part of the cold-rolled plate blank is sent into a heating furnace for recrystallization annealing, and the heat preservation time is 1 hour;
the heat treatment equipment used in this example was a model SK-G05123K tubular vacuum furnace manufactured by tianjin medium-ring electric furnace company. The crystal grains of the cold-rolled plate after recrystallization annealing treatment are recovered, recrystallized and grown, and the size of the crystal grains is larger than 1um through subsequent statistics, so that the wafer in the recrystallization annealing treatment state is marked as CG (Coarse-grain).
S6, stacking high-entropy alloy plates: cleaning the surfaces of the cold-rolled plate blank prepared in the step S4 and the cold-rolled plate blank subjected to the recrystallization annealing treatment in the step S5, and then overlapping the cold-rolled plate blank and the cold-rolled plate blank in a staggered manner to prepare a laminated cylinder; since the rolling directions are distinguished by the cut-off portions when the small wafers are cut in step S4, the rolling directions of the laminated high-entropy alloy sheets are uniform;
before lamination, the surfaces of UFG and CG wafers often have rolling scratches, residual cutting fluid from spark cutting, or oxide scale formed on the surfaces due to high temperature annealing, and these residues must be cleaned to ensure a tight thermocompression bond and to form a strong bonding interface. Therefore, the wafer is firstly polished by eagle black sand paper, and the mesh number of the sand paper is from coarse to fine: 240#, 400#, 600#, 800#, 1000#, 1500#, 2000#, 2500#, 3000#, until the surface is as bright as a mirror; ultrasonically cleaning the polished wafer for 30min by using acetone and alcohol, wherein the purpose of acetone cleaning is to remove impurities such as grease and the like attached to the surface of the wafer, immediately drying the wafer by using strong cold air after cleaning is finished, and cleanly storing the wafer for lamination;
the number of layers stacked in this example is 9, i.e. each resulting stacked cylinder is made by interleaving 5 UFG and 4 CG wafers.
S7, hot-press welding of the laminated cylinders: the hot-press welding temperature is 600 ℃, the heating rate is 5 ℃/min, loads are applied to two ends of the laminated cylinder while the temperature is increased, in order to ensure that the welding interface deforms uniformly, a lower strain rate is adopted, and the strain rate is 0.01s-1Carrying out thermal insulation diffusion welding connection and hot pressing deformation through constant load force, wherein the hot pressing deformation is 35-40%, and preparing a laminated column blank;
and (3) carrying out hot-press welding on the laminated cylinders by using a Gleeble3800 thermal simulation testing machine, wherein the maximum compression tonnage of the Gleeble3800 is 20t, and the diameter of the anvil head is 19 mm. And welding a thermocouple before hot-press welding, wherein an R-type thermocouple is selected in consideration of higher temperature and longer test time. And welding the positive and negative thermocouples to the end surfaces of the two sides of the laminated cylinder one by using a thermocouple welding machine in an impact welding mode, wherein the center distance between welding points of the two thermocouples is 4-10 times of the diameter of the thermocouple wire, and the diameter of the R-shaped thermocouple in the embodiment is 0.2 mm. The welding ladle of a good welding spot is not too large, and the thermocouple is optimally welded on the surface of a sample in a vertical mode, the thermocouple looks like a 'seed' on the surface of the sample, no large sparks exist during welding, no substances such as redundant welding ladles exist nearby the welding spot, and the thermocouple is not welded on the surface of the sample;
placing the laminated cylinder welded with the thermocouple into a Gleeble3800 thermal simulator, fixing the laminated cylinder by using an anvil head, fixing a carbon sheet and a tantalum sheet on two sides of the anvil head respectively by using lubricating grease, wherein the tantalum sheet has the function of preventing diffusion connection with the anvil head; after the fixation is finished, vacuumizing to a certain vacuum degree; then, heating is started, and a load is applied to the laminated cylinder while heating is started, namely, the target loading force is also loaded after heating is finished;
the hot-press welding aims at two purposes, one is that the stacked cylinders form diffusion connection, and diffusion welding is carried out between layers to form a connection interface; and secondly, the difference of the structures among the layers is kept as much as possible so as to prepare the final heterogeneous laminated structure. The diameter of the laminated cylindrical blank after hot press deformation cannot exceed the diameter of the anvil head in consideration of the limitations of the maximum compression tonnage and the diameter of the anvil head. In order to obtain the heterostructure plate with the final thickness of 1mm in the embodiment, the deformation amount is as large as possible in the hot pressing deformation stage, the final hot pressing deformation amount is controlled to be 35% -40%, and then other processing technology can be applied to further deform to obtain larger deformation amount.
S8, cold rolling of laminated column blanks:
through subsequent test observation, the interface between layers of the obtained sample after hot-press welding is well combined, and the original tissue morphology of the UFG layer and the CG layer is well kept; in order to further obtain more deformation and obtain excellent matching of strong plasticity mechanical properties, the hot-press welded laminated column blank is rolled at room temperature, the hot-press welded sample is further cold-rolled and deformed, the final thickness after cold rolling is 1mm, the accumulated deformation is 90 percent compared with the laminated column blank, and larger deformation is accumulated to prepare a heterogeneous laminated structure high-entropy alloy plate blank; the thickness of the heterogeneous laminated structure high-entropy alloy slab is 1 mm. The rolling mill used in step S8 is the same model as the rolling mill used in step S3.
S9, heat treatment:
and (3) residual large amount of processing stress in the plate subjected to the final cold rolling deformation, vacuumizing a heating furnace by using a vacuum pump in advance in order to regulate and control the final heterogeneous laminated structure, setting the heating temperature to 600 ℃, the heating rate to 5 ℃/min, heating to a target temperature, and then placing the heterogeneous laminated structure high-entropy alloy plate blank prepared in the step S8 into the heating furnace for heating, keeping the temperature for 1 hour, taking out the plate blank after the heat preservation is finished, and air-cooling the plate blank to room temperature to prepare the heterogeneous laminated structure high-entropy alloy plate. The heating furnace used in step S9 is the same model as the heating furnace used in step S5. Firstly, comparing the performances of the plate in the initial state, the initial cold rolling state (deformation 80%) is directly obtained by cold rolling deformation in the cast state, the yield strength is 1180MPa, and the ductility and toughness are poor due to the work hardening and a large amount of internal residual stress; and the initial annealed sheet is recrystallized and annealed for 1000-1 h, so that the toughness and plasticity are obviously improved, the fracture elongation reaches 44%, the yield strength is about 300MPa, and the ultimate tensile strength is 620 MPa. When the U & C sample is tested later, the situation that the chuck still slips after repeated stretching is found, the U & C sample is limited by stretching experimental equipment, and an accurate stress-strain curve of the U & C sample cannot be obtained through the research. However, the U & C sample is too high in strength reflected from the side surface, the preparation effectively carries out severe plastic deformation, and a large amount of dislocation energy is accumulated and stored, so that the stretching is difficult.
Then, the control group tested was U & C + A600 ℃/650 ℃/700 ℃ -1 h. After the U & C sample is annealed, recovered and recrystallized at 650 ℃/700-1 h, the yield strength is obviously reduced compared with that of a 600-1 h heat treatment, but instead, the fracture elongation of the U & C + A650-1 h sample is increased to 20.2%, and the yield strength is reduced to 906.3 MPa; the fracture elongation of the U & C + A sample is increased to 30.0% within 700-1 h, the yield strength is reduced to 757.2MPa, and compared with other research results for improving CoCrFeMnNi high-entropy alloy, the performance shows the middle gauge; it should be noted that after the U & C sample is annealed at 600 ℃ for 1 hour, the stress-strain curve does not show the work hardening stage, which indicates that the inside of the structure still has high dislocation density and distortion energy, and the annealing temperature or the holding time needs to be further increased.
So the following example designs two groups of U & C + A600-4 h/8h as further study objects. As a result, the performance of the U & C + A for 600-4 h is best, the yield strength reaches 1101.1MPa, the elongation at break is 15.3%, and after the annealing time is doubled, the elongation at break is basically kept unchanged, and the yield strength is reduced to 1017.7 MPa. The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (3)
1. A preparation process of a high-entropy alloy plate with a heterogeneous laminated structure is characterized by sequentially comprising the following steps of:
s1, preparing as-cast CoCrFeMnNi high-entropy alloy cast ingot
Under the protection of a high-purity nitrogen atmosphere, putting a mixture of pure metals of Co, Cr, Fe, Mn and Ni with equal atomic ratio into a magnetic suspension melting furnace and melting, stirring by magnetic suspension during melting, and solidifying to obtain an as-cast CoCrFeMnNi high-entropy alloy ingot;
s2, homogenization treatment: the annealing temperature is 1000 ℃, and the heat preservation time is 8 hours;
s3, rolling at room temperature: cutting the homogenized CoCrFeMnNi high-entropy alloy cast ingot into a plurality of slabs according to the requirement, polishing the surfaces of the slabs, and performing cold rolling at room temperature, wherein the rolling deformation is 80 percent, so as to prepare a plurality of cold-rolled slabs;
s4, cutting off the edge of the cold-rolled plate blank for later use;
s5, recrystallization annealing: vacuumizing a heating furnace in advance by using a vacuum pump, setting the recrystallization annealing temperature to be 1000 ℃, setting the temperature rise rate to be 5 ℃/min, raising the temperature to a target temperature, then, sending the trimmed partial cold-rolled plate blank into the heating furnace for recrystallization annealing, and keeping the temperature for 1 hour;
s6, stacking high-entropy alloy plates: cleaning the surfaces of the cold-rolled plate blank prepared in the step S4 and the cold-rolled plate blank subjected to the recrystallization annealing treatment in the step S5, and then overlapping the cold-rolled plate blank and the cold-rolled plate blank in a staggered manner to prepare a laminated cylinder;
s7, hot-press welding of the laminated cylinders: the hot-press welding temperature is 600 ℃, the heating rate is 5 ℃/min, loads are applied to two ends of the laminated cylinder while the temperature is raised, and the strain rate isIs 0.01s-1Carrying out thermal insulation diffusion welding connection and hot pressing deformation through constant load force, wherein the hot pressing deformation is 35-40%, and preparing a laminated column blank;
s8, cold rolling of laminated column blanks: rolling the hot-press welded laminated column blank at room temperature, wherein the accumulated deformation is 90%, and preparing a heterogeneous laminated structure high-entropy alloy plate blank;
s9, heat treatment: and (3) vacuumizing the heating furnace in advance by using a vacuum pump, setting the heating temperature to be 600 ℃, the heating rate to be 5 ℃/min, heating to the target temperature, then keeping the temperature stable, putting the heterogeneous laminated structure high-entropy alloy plate blank prepared in the step S8 into the heating furnace for heating for 1 hour, taking out after the heat preservation is finished, and air-cooling to the room temperature to prepare the heterogeneous laminated structure high-entropy alloy plate.
2. The preparation process of the heterogeneous laminated structure high-entropy alloy plate according to claim 1, characterized by comprising the following steps: in the step S6, the rolling directions of the laminated high-entropy alloy plates are consistent.
3. The preparation process of the heterogeneous laminated structure high-entropy alloy plate according to claim 1, characterized by comprising the following steps: the thickness of the final cold-rolled steel sheet obtained in step S8 is 1 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111350364.9A CN114085969B (en) | 2021-11-15 | 2021-11-15 | Preparation process of high-entropy alloy plate with heterogeneous laminated structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111350364.9A CN114085969B (en) | 2021-11-15 | 2021-11-15 | Preparation process of high-entropy alloy plate with heterogeneous laminated structure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114085969A true CN114085969A (en) | 2022-02-25 |
| CN114085969B CN114085969B (en) | 2023-03-10 |
Family
ID=80300741
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111350364.9A Active CN114085969B (en) | 2021-11-15 | 2021-11-15 | Preparation process of high-entropy alloy plate with heterogeneous laminated structure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114085969B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114921671A (en) * | 2022-05-11 | 2022-08-19 | 东北大学 | Preparation method of large-size CoCrFeMnNi high-entropy alloy |
| CN115976349A (en) * | 2022-12-13 | 2023-04-18 | 西南交通大学深圳研究院 | Preparation method of high-strength high-plasticity metastable state high-entropy alloy with heterogeneous grain structure |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110621499A (en) * | 2017-05-12 | 2019-12-27 | 株式会社大赛璐 | Sheet, method for manufacturing sheet, and method for attaching sheet |
| CN111360074A (en) * | 2020-02-13 | 2020-07-03 | 中南大学 | Preparation method of heterogeneous lamellar structure medium/high-entropy alloy foil |
| KR102130690B1 (en) * | 2019-03-15 | 2020-07-06 | 포항공과대학교 산학협력단 | Clad using high entropy alloy and manaufacturing method of the same |
| CN112195317A (en) * | 2020-10-15 | 2021-01-08 | 温州大学 | Cold rolling composite laser surface annealing process method for high-entropy alloy with heterogeneous structure |
| CN112547798A (en) * | 2020-10-30 | 2021-03-26 | 南京理工大学 | Method for preparing high-strength heterogeneous high-entropy alloy through accumulative pack rolling |
| CN113122763A (en) * | 2021-04-14 | 2021-07-16 | 中北大学 | Preparation method of high-strength high-toughness high-entropy alloy |
-
2021
- 2021-11-15 CN CN202111350364.9A patent/CN114085969B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110621499A (en) * | 2017-05-12 | 2019-12-27 | 株式会社大赛璐 | Sheet, method for manufacturing sheet, and method for attaching sheet |
| KR102130690B1 (en) * | 2019-03-15 | 2020-07-06 | 포항공과대학교 산학협력단 | Clad using high entropy alloy and manaufacturing method of the same |
| CN111360074A (en) * | 2020-02-13 | 2020-07-03 | 中南大学 | Preparation method of heterogeneous lamellar structure medium/high-entropy alloy foil |
| CN112195317A (en) * | 2020-10-15 | 2021-01-08 | 温州大学 | Cold rolling composite laser surface annealing process method for high-entropy alloy with heterogeneous structure |
| CN112547798A (en) * | 2020-10-30 | 2021-03-26 | 南京理工大学 | Method for preparing high-strength heterogeneous high-entropy alloy through accumulative pack rolling |
| CN113122763A (en) * | 2021-04-14 | 2021-07-16 | 中北大学 | Preparation method of high-strength high-toughness high-entropy alloy |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114921671A (en) * | 2022-05-11 | 2022-08-19 | 东北大学 | Preparation method of large-size CoCrFeMnNi high-entropy alloy |
| CN115976349A (en) * | 2022-12-13 | 2023-04-18 | 西南交通大学深圳研究院 | Preparation method of high-strength high-plasticity metastable state high-entropy alloy with heterogeneous grain structure |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114085969B (en) | 2023-03-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114085969B (en) | Preparation process of high-entropy alloy plate with heterogeneous laminated structure | |
| Wang et al. | Microstructure evolution and tensile properties of as-rolled TiB/TA15 composites with network microstructure | |
| EP3391976B1 (en) | Magnesium alloy sheet rolling and preparation method | |
| CN107847993B (en) | Titanium billet for hot rolling | |
| US10480042B2 (en) | Edge formability in metallic alloys | |
| RU2555267C2 (en) | Method of fabrication of thin sheets from two-phase titanium alloy and product from these sheets | |
| CN112222413B (en) | Cold rolling composite laser additive manufacturing process method of gradient structure high-entropy alloy | |
| CN115198162B (en) | Entropy alloy in high-toughness heterogeneous multi-phase core-shell organization structure and preparation method thereof | |
| KR20190028481A (en) | High yield strength steel plate | |
| CN111842488A (en) | Process method for realizing TiAl alloy uniform fine grain structure based on cross sheath rolling | |
| CN114622120B (en) | TRIP-assisted AlFeMnCoCr three-phase heterogeneous high-entropy alloy and preparation method thereof | |
| CN110306137B (en) | Preparation method of layered copper-chromium-zirconium-pure copper composite plate | |
| Shuai et al. | Effect of annealing temperature on microstructure and mechanical properties of cold-rolled commercially pure titanium sheets | |
| CN109825785B (en) | Preparation method of industrial pure titanium with heterogeneous layered structure | |
| CN109487102B (en) | Preparation method of aluminum-magnesium-scandium alloy plate for superplastic forming | |
| CN105773074B (en) | A kind of preparation method of molybdenum alloy boat | |
| EP2690185A1 (en) | Molybdenum material | |
| CN114622145B (en) | Cobalt-free maraging steel with dual-phase structure and preparation method thereof | |
| CN112251684B (en) | Micro-nanocrystalline maraging steel and preparation method thereof | |
| CN112626431B (en) | Preparation method of prestressed bolt for medical ultrasonic transducer | |
| JP3835707B2 (en) | Method for producing Al-Mg alloy plate for forming | |
| JPH03155427A (en) | Hot forging method for titanium alloy sintered material | |
| JP4402541B2 (en) | Manufacturing method of α + β type titanium alloy | |
| CN115852283B (en) | High-strength plastic nickel-based alloy plate with double-peak structure and preparation method thereof | |
| CN115404371A (en) | Core-shell structure high-entropy alloy and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20231213 Address after: 030000, 29th Floor, 28th Floor, Building 4, Zhonghai Huanyu Tianxia, No. 8, Section 1, Jinci Road, Wanbailin District, Taiyuan City, Shanxi Province (settled at No. 2903-6 Zhongzhou Incubator) Patentee after: Shanxi Hengjia Technology Co.,Ltd. Address before: No. 66, Berlin District, Wan Berlin District, Taiyuan, Shanxi Patentee before: TAIYUAN University OF SCIENCE AND TECHNOLOGY |
|
| TR01 | Transfer of patent right |