CN114164379B - Hot processing method of TiVTaNb high-entropy alloy prepared based on smelting technology - Google Patents
Hot processing method of TiVTaNb high-entropy alloy prepared based on smelting technology Download PDFInfo
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Abstract
The invention relates to a hot working method of TiVTaNb high-entropy alloy prepared based on a smelting technology, and belongs to the technical field of high-entropy alloy processing. The method comprises the steps of placing TiVTaNb high-entropy alloy prepared by adopting a smelting technology in a metal die, sealing, carrying out multi-pass thermal deformation treatment after heat preservation for 0.5-2 h at 1100-1200 ℃, and carrying out air cooling after the thermal deformation treatment is finished to finish the thermal processing treatment of the TiVTaNb high-entropy alloy. The invention adopts a vacuum sheath hot rolling method, avoids the TiVTaNb high-entropy alloy from being oxidized at high temperature by optimizing the hot rolling process parameters, realizes the rapid homogenization of the TiVTaNb high-entropy alloy, eliminates the cast defect and component segregation of the TiVTaNb high-entropy alloy, and refines crystal grains, so that the tensile strength of the TiVTaNb high-entropy alloy after hot processing is obviously improved on the basis of keeping good plasticity. In addition, the method has the advantages of simple process, short treatment period, high production efficiency, suitability for industrial production and good application prospect.
Description
Technical Field
The invention relates to a hot working method of TiVTaNb high-entropy alloy prepared based on a smelting technology, and belongs to the technical field of high-entropy alloy processing.
Background
The TiVTaNb refractory high-entropy alloy shows good strong plasticity matching (tensile yield strength is not less than 853MPa, plasticity is more than 24%) at room Temperature, has good thermal stability under high-Temperature conditions, can keep higher compressive strength (595 MPa at 900 ℃), can be used as a high-Temperature structural material, and has good application prospects in various fields of aerospace, nuclear engineering and the like (Temperature dependency of elastic and plastic deformation behavor of a reactivity high-entry alloy. Science advance. Lee Chanho, kim George, choouyi, music Brianna L, gao Michael C, an Keou Ke, soGigan, ch YiChia, kepps vessel, chen Cheni, liaw K.2020,6 (37)).
The TiVTaNb refractory high-entropy alloy is prepared by a smelting technology, generally has large and thick grains, and is easy to have the problems of casting defects, component segregation and the like, so that the mechanical property of the high-entropy alloy is deteriorated, and the service life of the high-entropy alloy is shortened. Therefore, there is a need to eliminate the casting defects and improve the microstructure of TiVTaNb refractory high-entropy alloys by hot isostatic pressing, or cold deformation combined with annealing. However, the equipment used for hot isostatic pressing is complex and involves many process parameters, including temperature, pressure, dwell time, process sequence, etc., and it is usually necessary to determine suitable process parameters by means of simulation or extensive experiments. The TiVTaNb refractory high-entropy alloy is a novel metal material, and lacks a corresponding empirical model, so that the selection of process parameters is particularly difficult. Although the defects of TiVTaNb refractory high-entropy alloy casting can be eliminated by adopting cold deformation, a deformation zone is introduced at the same time to influence the plasticity of the high-entropy alloy, so that the influence of the deformation zone is eliminated by depending on long-time annealing treatment, the whole process is complex, and the period is long.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a hot working method of TiVTaNb high-entropy alloy prepared based on a smelting technology, which can quickly eliminate the as-cast defects and component segregation of the TiVTaNb high-entropy alloy, can refine crystal grains, can keep good plasticity and obviously improve the strength, and is simple in process, short in treatment period, high in production efficiency and suitable for industrial production.
The purpose of the invention is realized by the following technical scheme.
The hot processing method of the TiVTaNb high-entropy alloy prepared based on the smelting technology comprises the following steps:
placing the TiVTaNb high-entropy alloy prepared by adopting a smelting technology into a metal mold, sealing, vacuumizing a cavity of the metal mold, then placing the metal mold into a heat treatment furnace, heating to 1100-1200 ℃, preserving heat for 0.5-2 h, performing multi-pass thermal deformation treatment after the heat preservation is finished, performing air cooling after the thermal deformation treatment is finished, and finally taking out the TiVTaNb high-entropy alloy after the thermal deformation treatment from the metal mold;
wherein the initial rolling temperature of the thermal deformation treatment is 1100-1200 ℃, the final rolling temperature is 900-1100 ℃, the rolling speed is 0.1-0.25 m/s, the deformation of each pass is 10-25%, and the total deformation is 70-90%.
Further, the material of the metal mold is preferably 304 stainless steel, 1Cr18Ni9Ti stainless steel, or TC4 titanium alloy.
Further, the wall thickness of the metal mold is preferably 4mm to 10mm.
Furthermore, gaps exist among the TiVTaNb high-entropy alloy, the periphery of the metal die and the upper end of the metal die, and the gaps are preferably 1-3 mm.
Further, the degree of vacuum of the metal mold cavity is preferably less than 1 × 10 -2 Pa。
Further, in the multi-pass hot deformation treatment, the rolling rate is preferably 0.1m/s to 0.25m/s.
Furthermore, in the multi-pass thermal deformation treatment process, the temperature of the inter-pass furnace returning is preferably 1020-1220 ℃, and the time of the inter-pass furnace returning and heat preservation is preferably 10-30 min.
Has the advantages that:
the TiVTaNb high-entropy alloy is subjected to vacuum sheath hot rolling, oxidation of the TiVTaNb high-entropy alloy at high temperature is avoided by optimizing hot rolling process parameters, rapid homogenization of the TiVTaNb high-entropy alloy is realized, as-cast defects and component segregation of the TiVTaNb high-entropy alloy are eliminated, crystal grains are refined, and compared with the as-cast TiVTaNb high-entropy alloy, the TiVTaNb high-entropy alloy treated by the method disclosed by the invention has the advantage that the tensile strength of the TiVTaNb high-entropy alloy is improved by about 200MPa on the basis of keeping good plasticity. The hot processing method provided by the invention is simple in process, short in treatment period, high in production efficiency, suitable for industrial production and good in application prospect.
Drawings
FIG. 1 is a schematic structural view of a metal mold used in the examples; the method comprises the following steps of 1-TiVTaNb high-entropy alloy ingot casting, 2-metal mold and 3-vacuum pumping pipeline.
FIG. 2 is a microstructure photograph of a TiVTaNb high-entropy alloy ingot prepared by an arc melting method in example 1.
FIG. 3 is a microstructure photograph of a TiVTaNb high-entropy alloy after hot deformation treatment in example 1.
Fig. 4 is a tensile stress strain curve diagram of the high entropy alloy ingots of TiVTaNb prepared by the arc melting method in example 1.
FIG. 5 is a tensile stress strain plot of the TiVTaNb high-entropy alloy after the hot deformation treatment in example 1.
FIG. 6 is a microstructure photograph of a TiVTaNb high-entropy alloy after hot deformation treatment in example 2.
FIG. 7 is a microstructure photograph of a TiVTaNb high-entropy alloy after hot deformation treatment in example 3.
FIG. 8 is a tensile stress strain plot of a TiVTaNb high-entropy alloy after a hot deformation treatment in comparative example 2.
Detailed Description
The present invention is further illustrated by the following figures and detailed description, wherein the processes are conventional unless otherwise specified, and the starting materials are commercially available from a public source without further specification.
In the following examples:
testing room temperature tensile property: according to the standard GB-T228.1-2010, a CMT4305 type microcomputer electronic universal testing machine is adopted to carry out room-temperature (25 ℃) axial quasi-static tensile test, and the strain rate is selected to be 10 -3 s -1 。
Microstructure observation and elemental composition measurement: the equipment used is a cold field emission scanning electron microscope Regulus 8230.
Example 1
(1) The simple substances of Ti, V, ta and Nb with the purity of more than 99.99at.% are processedMechanically polishing to remove oxide skin on the surface, cleaning with alcohol, respectively weighing 64.26g of Ti, 68.34g of V, 242.76g of Nb and 124.64g of Ta, sequentially putting the weighed metal simple substances into a crucible in a smelting furnace according to the melting point from low to high, and vacuumizing the furnace to 2.5 multiplied by 10 -3 Pa, then flushing argon to 0.5 atmospheric pressure, carrying out alloying smelting on the metal simple substance in the crucible in an arc heating mode, simultaneously applying electromagnetic stirring, cooling to form an alloy ingot after smelting for 10min, turning over the alloy ingot, and repeatedly smelting for four times to obtain a TiVTaNb high-entropy alloy ingot 1;
(2) Cutting the TiVTaNb high-entropy alloy ingot 1 into blocks with the size of 24mm multiplied by 12mm multiplied by 8mm, putting the block TiVTaNb high-entropy alloy ingot 1 into a metal mold 2 with an opening at the top end, then putting a top cover, welding and sealing, connecting a vacuumizing pipeline 3 on the top cover to vacuumize the cavity of the metal mold 2, and ensuring that the vacuum degree of the cavity of the metal mold 2 is less than 5 multiplied by 10 -3 Pa; wherein the material of the metal mold 2 is 304 stainless steel, the wall thickness of the metal mold 2 is 4mm, a 1mm gap exists between the TiVTaNb high-entropy alloy ingot 1 and the periphery of the metal mold 2, and a 2mm gap exists between the TiVTaNb high-entropy alloy ingot 1 and the top cover of the metal mold 2, as shown in FIG. 1;
(3) Placing the vacuumized metal mold 2 into a heat treatment furnace, heating to 1200 ℃, preserving heat for 0.5h, and performing multi-pass thermal deformation treatment after heat preservation;
wherein the initial rolling temperature of the thermal deformation treatment is 1200 ℃, the final rolling temperature is 1050 ℃, the rolling speed is 0.2m/s, the deformation of each pass is about 16%, the total deformation is 80%, the temperature of the inter-pass furnace return is 1200 ℃, and the time of the inter-pass furnace return for heat preservation is 10min;
(4) And after the thermal deformation treatment is finished, air cooling is firstly carried out, then the metal die 2 is removed by a wire cutting machine, the TiVTaNb high-entropy alloy after the thermal deformation treatment is taken out for cleaning and drying, and then the thermal processing treatment of the TiVTaNb high-entropy alloy is finished.
Comparing fig. 2 and fig. 3, it can be seen that the TiVTaNb high-entropy alloy after hot working treatment has no significant casting defects and has significantly refined grains, the average size of the as-cast grains before hot working treatment is about 113.3 μm, and the average size of the grains after hot working treatment is about 21.6 μm.
The detection proves that the TiVTaNb high-entropy alloy ingot has the composition segregation phenomenon, and the composition fluctuation of each element is more than 5 percent; the TiVTaNb high-entropy alloy after the hot working treatment has even component distribution, and the component fluctuation of each element is less than or equal to 2 percent.
The test shows that the tensile yield strength of the TiVTaNb high-entropy alloy ingot is 853MPa, the elongation is 26.3 percent, and the tensile yield strength is shown in FIG. 4; the tensile yield strength of the TiVTaNb high-entropy alloy after the hot working treatment is 930MPa, and the elongation is 24.5%, as shown in FIG. 5.
Example 2
(1) Preparing a TiVTaNb high-entropy alloy ingot 1 according to the method of the step (1) of the embodiment 1;
(2) Cutting the TiVTaNb high-entropy alloy ingot 1 into blocks with the size of 25mm multiplied by 15mm multiplied by 7.5mm, putting the block TiVTaNb high-entropy alloy ingot 1 into a metal mold 2 with an opening at the top end, then putting a top cover on the top cover, welding and sealing the top cover, connecting a vacuumizing pipeline 3 on the top cover to vacuumize the cavity of the metal mold 2, and ensuring that the vacuum degree of the cavity of the metal mold 2 is less than 5 multiplied by 10 -3 Pa; wherein the metal die 2 is made of 304 stainless steel, the wall thickness of the metal die 2 is 4mm, a 1mm gap exists between the TiVTaNb high-entropy alloy ingot 1 and the periphery of the metal die 2, and a 2mm gap exists between the TiVTaNb high-entropy alloy ingot 1 and a top cover of the metal die 2;
(3) Placing the vacuumized metal mold 2 into a heat treatment furnace, heating to 1200 ℃, preserving heat for 0.5h, and performing multi-pass thermal deformation treatment after heat preservation is finished;
wherein the initial rolling temperature of the thermal deformation treatment is 1200 ℃, the final rolling temperature is 1050 ℃, the rolling speed is 0.2m/s, the deformation of each pass is about 15%, the total deformation is 85%, the temperature of the inter-pass furnace return is 1200 ℃, and the time of the inter-pass furnace return for heat preservation is 10min;
(4) And after the thermal deformation treatment is finished, air cooling is carried out, the metal die 2 is removed by a wire cutting machine, the TiVTaNb high-entropy alloy after the thermal deformation treatment is taken out for cleaning and drying, and then the thermal processing treatment of the TiVTaNb high-entropy alloy is completed.
The TiVTaNb high-entropy alloy after the hot working treatment has no obvious casting defects and fine crystal grains, and the average size of the crystal grains is about 16.7 mu m, as shown in figure 6.
The detection proves that the TiVTaNb high-entropy alloy after the hot working treatment has uniform component distribution, and the component fluctuation of each element is less than or equal to 2 percent.
Tests show that the tensile yield strength of the TiVTaNb high-entropy alloy after the hot working treatment is 996MPa, and the elongation is 18.8%.
Example 3
(1) Preparing a TiVTaNb high-entropy alloy ingot 1 according to the method of the step (1) of the embodiment 1;
(2) Cutting the TiVTaNb high-entropy alloy ingot 1 into blocks with the size of 20mm multiplied by 10mm, putting the block TiVTaNb high-entropy alloy ingot 1 into a metal mold 2 with an opening at the top end, then putting a top cover, welding and sealing, connecting a vacuumizing pipeline 3 on the top cover to vacuumize the cavity of the metal mold 2, and ensuring that the vacuum degree of the cavity of the metal mold 2 is less than 5 multiplied by 10 -3 Pa; the material of the metal mold 2 is 304 stainless steel, the wall thickness of the metal mold 2 is 5mm, a 1mm gap exists between the TiVTaNb high-entropy alloy ingot 1 and the periphery of the metal mold 2, and a 2mm gap exists between the TiVTaNb high-entropy alloy ingot 1 and a top cover of the metal mold 2;
(3) Placing the vacuumized metal mold 2 into a heat treatment furnace, heating to 1100 ℃, preserving heat for 1h, and performing multi-pass thermal deformation treatment after heat preservation;
wherein the initial rolling temperature of the thermal deformation treatment is 1100 ℃, the final rolling temperature is 950 ℃, the rolling speed is 0.15m/s, the deformation of each pass is about 10%, the total deformation is 90%, the temperature of the inter-pass furnace return is 1100 ℃, and the time of the inter-pass furnace return is 15min;
(4) And after the thermal deformation treatment is finished, air cooling is carried out, the metal die 2 is removed by a wire cutting machine, the TiVTaNb high-entropy alloy after the thermal deformation treatment is taken out for cleaning and drying, and then the thermal processing treatment of the TiVTaNb high-entropy alloy is completed.
The TiVTaNb high-entropy alloy after the hot working treatment has no obvious casting defects and fine grains, and the average size of the grains is about 12.1 mu m, as shown in figure 7.
The detection proves that the TiVTaNb high-entropy alloy after the hot working treatment has uniform component distribution, and the component fluctuation of each element is less than or equal to 2 percent.
Tests show that the tensile yield strength of the TiVTaNb high-entropy alloy after the hot working treatment is 1080MPa, and the elongation is 12.6%.
Comparative example 1
(1) Preparing a TiVTaNb high-entropy alloy ingot 1 according to the method of the step (1) of the embodiment 1;
(2) Cutting the TiVTaNb high-entropy alloy ingot 1 into blocks with the size of 20mm multiplied by 10mm multiplied by 8mm, putting the block TiVTaNb high-entropy alloy ingot 1 into a metal mold 2 with an opening at the top end, then putting a top cover on the top cover, welding and sealing the top cover, connecting a vacuumizing pipeline 3 on the top cover to vacuumize the cavity of the metal mold 2, and ensuring that the vacuum degree of the cavity of the metal mold 2 is less than 5 multiplied by 10 -3 Pa; wherein the metal die 2 is made of 304 stainless steel, the wall thickness of the metal die 2 is 4mm, a 1mm gap exists between the TiVTaNb high-entropy alloy ingot 1 and the periphery of the metal die 2, and a 2mm gap exists between the TiVTaNb high-entropy alloy ingot 1 and a top cover of the metal die 2;
(3) Placing the vacuumized metal mold 2 into a heat treatment furnace, heating to 900 ℃, preserving heat for 0.5h, and performing multi-pass thermal deformation treatment after heat preservation;
wherein the initial rolling temperature of the thermal deformation treatment is 900 ℃, the final rolling temperature is 750 ℃, the rolling speed is 0.2m/s, the deformation of each pass is about 16%, the total deformation is 80%, the temperature of the inter-pass furnace return is 900 ℃, and the time of the inter-pass furnace return and the heat preservation is 10min;
(4) And after the thermal deformation treatment is finished, air cooling is carried out, the metal die 2 is removed by a wire cutting machine, the TiVTaNb high-entropy alloy after the thermal deformation treatment is taken out for cleaning and drying, and then the thermal processing treatment of the TiVTaNb high-entropy alloy is completed.
The detection shows that the component fluctuation of each element of the TiVTaNb high-entropy alloy after the hot working treatment is more than or equal to 3 percent.
The tensile yield strength of the TiVTaNb high-entropy alloy after heat treatment is 1169MPa, but the elongation is only 2.74 percent.
Comparative example 2
(1) Preparing a TiVTaNb high-entropy alloy ingot 1 according to the method of the step (1) of the embodiment 1;
(2) Cutting the TiVTaNb high-entropy alloy ingot 1 into blocks with the size of 24mm multiplied by 12mm multiplied by 6mm, putting the block TiVTaNb high-entropy alloy ingot 1 into a metal mold 2 with an opening at the top end, then putting a top cover, welding and sealing, connecting a vacuumizing pipeline 3 on the top cover to vacuumize the cavity of the metal mold 2, and ensuring that the vacuum degree of the cavity of the metal mold 2 is less than 5 multiplied by 10 -3 Pa; wherein the metal die 2 is made of 304 stainless steel, the wall thickness of the metal die 2 is 4mm, a 1mm gap exists between the TiVTaNb high-entropy alloy ingot 1 and the periphery of the metal die 2, and a 2mm gap exists between the TiVTaNb high-entropy alloy ingot 1 and a top cover of the metal die 2;
(3) Placing the vacuumized metal mold 2 into a heat treatment furnace, heating to 1200 ℃, preserving heat for 0.5h, and performing multi-pass thermal deformation treatment after heat preservation;
wherein the initial rolling temperature of the thermal deformation treatment is 1200 ℃, the final rolling temperature is 1050 ℃, the rolling speed is 0.2m/s, the deformation of each pass is about 12.5%, the total deformation is 50%, the temperature of the inter-pass furnace return is 1200 ℃, and the heat preservation time of the inter-pass furnace return is 10min;
(4) And after the thermal deformation treatment is finished, air cooling is firstly carried out, then the metal die 2 is removed by a wire cutting machine, the TiVTaNb high-entropy alloy after the thermal deformation treatment is taken out for cleaning and drying, and then the thermal processing treatment of the TiVTaNb high-entropy alloy is finished.
The detection shows that the TiVTaNb high-entropy alloy after heat treatment also has the composition segregation phenomenon, and the composition fluctuation of each element is more than 5 percent.
The tensile yield strength and the elongation of the TiVTaNb high-entropy alloy after heat treatment are 811MPa and 24.0 percent respectively, which are shown in FIG. 8.
In summary, the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. The hot processing method of the TiVTaNb high-entropy alloy prepared based on the smelting technology is characterized by comprising the following steps: the hot processing method comprises the following steps:
placing the TiVTaNb high-entropy alloy prepared by adopting a smelting technology in a metal mold, sealing, vacuumizing a cavity of the metal mold, then placing the metal mold in a heat treatment furnace, heating to 1100-1200 ℃, preserving heat for 0.5-2 h, performing multi-pass thermal deformation treatment after the heat preservation is finished, performing air cooling after the thermal deformation treatment is finished, and finally taking out the TiVTaNb high-entropy alloy after the thermal deformation treatment from the metal mold;
wherein the initial rolling temperature of the thermal deformation treatment is 1100-1200 ℃, the final rolling temperature is 900-1100 ℃, the deformation of each pass is 10-25%, and the total deformation is 70-90%; in the multi-pass thermal deformation treatment process, the inter-pass furnace returning temperature is 1020-1220 ℃, and the inter-pass furnace returning heat preservation time is 10-30 min.
2. The hot working method of the TiVTaNb high-entropy alloy prepared based on the smelting technology as claimed in claim 1, wherein: the metal die is made of 304 stainless steel, 1Cr18Ni9Ti stainless steel or TC4 titanium alloy.
3. The hot working method of the TiVTaNb high-entropy alloy prepared based on the smelting technology as claimed in claim 1 or 2, characterized in that: the wall thickness of the metal mold is 4mm to 10mm.
4. The hot working method of the TiVTaNb high-entropy alloy prepared based on the smelting technology as claimed in claim 1, is characterized in that: gaps are reserved between the TiVTaNb high-entropy alloy and the periphery of the metal die and the upper end of the metal die, and the gaps are 1mm to 3mm.
5. The hot working method of the TiVTaNb high-entropy alloy prepared based on the smelting technology as claimed in claim 1, wherein: the vacuum degree of the metal mold cavity is less than 1 multiplied by 10 -2 Pa。
6. The hot working method of the TiVTaNb high-entropy alloy prepared based on the smelting technology as claimed in claim 1, wherein: in the multi-pass thermal deformation treatment process, the rolling speed is 0.1m/s-0.25m/s.
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