CN117230394A - High-strength beta titanium alloy heat treatment method based on stress induced martensite reverse phase transformation - Google Patents
High-strength beta titanium alloy heat treatment method based on stress induced martensite reverse phase transformation Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 119
- 239000000956 alloy Substances 0.000 title claims abstract description 119
- 229910001040 Beta-titanium Inorganic materials 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 46
- 230000009466 transformation Effects 0.000 title claims abstract description 39
- 238000010438 heat treatment Methods 0.000 title claims abstract description 38
- 229910000734 martensite Inorganic materials 0.000 title claims abstract description 28
- 238000005096 rolling process Methods 0.000 claims abstract description 71
- 238000000137 annealing Methods 0.000 claims abstract description 18
- 238000005242 forging Methods 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 27
- 230000035882 stress Effects 0.000 claims description 24
- 238000003723 Smelting Methods 0.000 claims description 23
- 239000011651 chromium Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 15
- 229910052782 aluminium Inorganic materials 0.000 claims description 13
- 229910052804 chromium Inorganic materials 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 13
- 229910052726 zirconium Inorganic materials 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 10
- 239000010936 titanium Substances 0.000 claims description 10
- 238000005266 casting Methods 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 9
- 238000010274 multidirectional forging Methods 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 7
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 6
- 229910001182 Mo alloy Inorganic materials 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 229910000756 V alloy Inorganic materials 0.000 claims description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- UNQHSZOIUSRWHT-UHFFFAOYSA-N aluminum molybdenum Chemical compound [Al].[Mo] UNQHSZOIUSRWHT-UHFFFAOYSA-N 0.000 claims description 6
- HIMLGVIQSDVUJQ-UHFFFAOYSA-N aluminum vanadium Chemical compound [Al].[V] HIMLGVIQSDVUJQ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
- 230000007704 transition Effects 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 239000006104 solid solution Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000000265 homogenisation Methods 0.000 claims description 3
- 229910000851 Alloy steel Inorganic materials 0.000 claims description 2
- 229910001069 Ti alloy Inorganic materials 0.000 abstract description 9
- 238000005336 cracking Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 15
- 230000009467 reduction Effects 0.000 description 11
- 238000013461 design Methods 0.000 description 10
- 229910052750 molybdenum Inorganic materials 0.000 description 7
- 229910052720 vanadium Inorganic materials 0.000 description 7
- 229910000831 Steel Inorganic materials 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005098 hot rolling Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 229910021332 silicide Inorganic materials 0.000 description 3
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000002431 foraging effect Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 238000005097 cold rolling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
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- 238000012545 processing Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a heat treatment method of high-strength beta titanium alloy based on stress induced martensite reverse phase transformation, which belongs to the technical field of titanium alloy. The alloy is deformed to induce martensitic transformation due to large room temperature deformation in the rolling process, deformation induced plasticity is generated, and cold deformation capacity is improved. Asynchronous rolling effectively avoids the problem of cracking of the plate in the rolling process while improving the deformation. And carrying out short-time annealing treatment and solution treatment on the alloy in a single-phase region and performing time-efficient treatment to obtain fine equiaxed beta grains, separating out a micron primary alpha phase and a nanometer secondary alpha phase, constructing a multi-scale microstructure, and effectively improving the alloy performance, thereby obtaining the high-strength near-beta titanium alloy sheet with excellent performance. The tensile strength of the plate obtained by the regulation and control of the method can reach 1600MPa; the elongation rate can reach 9 percent.
Description
Technical Field
The invention belongs to the technical field of titanium alloy, and particularly relates to a high-strength beta titanium alloy heat treatment method based on stress induced martensitic reverse transformation.
Background
As a "third alloy", titanium alloys have been widely used in the leading fields of aerospace, biomedical and the like with their excellent specific strength, lower density, higher hardness. As the market demands on titanium alloy properties become higher, the disadvantage of mismatch between high strength and plasticity is also continuously amplified. How to obtain better performance of the titanium alloy through a forming method and heat treatment regulation and control is always the focus of titanium alloy research.
Disclosure of Invention
In order to solve the problem that the high strength and the low plasticity of the beta titanium alloy plate are not matched, the mechanical property of the plate is improved, and the high-strength beta titanium alloy with high strength hardness and excellent plasticity is obtained.
In order to achieve the above purpose, the invention provides a high-strength beta titanium alloy heat treatment method based on stress induced martensitic reverse transformation, which comprises the following steps:
casting a beta titanium alloy cast ingot with the following mass composition: 2-5% of Al,6-9% of Mo,2-4% of V,1-4% of Cr,1-3% of Zr, and the balance of Ti and unavoidable impurity elements;
homogenizing the beta alloy cast ingot, cogging and forging, then cooling, freely and multidirectional forging, wherein the final forging temperature is 30-70 ℃ below the beta transition temperature, and a forging piece is obtained; after homogenization treatment and cogging forging, the cast ingot has more uniform structure components, eliminates casting defects, and breaks the as-cast coarse grains. After cogging forging, cooling and free multidirectional forging are carried out, so that grains are further refined, a structure is homogenized, and the density of the product is improved;
carrying out solution treatment on the forging at 20-50 ℃ above the beta transformation temperature; the solution treatment can eliminate the internal stress of forging deformation;
carrying out room-temperature asynchronous rolling on the forging subjected to solution treatment; compared with the traditional rolling, the room-temperature asynchronous rolling can reduce the rolling force, improve the deformation condition, improve the deformation capacity, and combine the deformation induced plasticity, so that the single-pass deformation is increased, the number of passes is less, and the sheet forming is excellent. Stress-induced martensite is generated in the rolling process, conditions are provided for constructing the beta titanium alloy multi-scale microstructure by subsequent heat treatment, the grain refinement effect is more obvious, and the alloy shaping is effectively promoted;
the product after asynchronous rolling is subjected to heat treatment, and the martensite is induced by the asynchronous rolling deformation so that the energy generated in the titanium alloy drives the annealing treatment of the single-phase region to recover and recrystallize, the temperature at which the recrystallization occurs can be reduced, and the single-phase region is dissolved into the parent phase after annealing. Needle-like martensite enables recrystallization to be more fully completed, and uniform and fine equiaxed beta grains are obtained after annealing; and carrying out solution treatment in a two-phase region to obtain a micron-sized primary alpha phase, and carrying out long-time aging treatment to obtain a very fine nano-sized secondary alpha phase which is dispersed and distributed in a beta phase. The multi-scale microstructure is constructed, the fine grain strengthening of beta phase and the dispersion strengthening of alpha phase lead the alloy strength to be improved, and finally the beta titanium alloy with high strength and excellent plasticity is obtained.
Further, according to Mo equivalent and d electron theory B o 、M d Designing beta titanium alloy components according to a value design principle; according to the invention, by designing the titanium alloy components, the Mo equivalent of the alloy is in the range of 9% -11%, the Bo value is in the range of 2.77-2.79, the Md value is in the range of 2.35-2.39, the alloy is near beta titanium alloy at this time, and the cold deformation mechanism is stress induced martensitic transformation, so that the plastic deformation capability of the plate in the rolling deformation process is improved;
the process of casting the beta titanium alloy ingot is as follows: the method comprises the steps of taking titanium sponge, pure aluminum, pure chromium, pure zirconium, aluminum-molybdenum alloy (Mo content is 75.15%) and aluminum-vanadium alloy (V content is 85.22%) as raw materials, weighing the raw materials according to the weight percentage of each component, mixing, and then smelting and casting ingots to obtain alloy cast ingots.
Further, according to Mo equivalent and d electron theory B o 、M d The process of designing the beta titanium alloy composition according to the value design principle is as follows:
mo equivalent:
[Mo] eq ＝1.0Mo+0.67V+0.44W+0.28Nb+0.22Ta+1.6Cr+2.9Fe+1.54Mn+1.25Ni-1.0Al
d electron theory B o 、M d Value design principle:
B o ＝ΣX i (B o ) i
M d ＝ΣX i (M d ) i
wherein X is i Is the atomic fraction of alloy element i, (B) o ) i Sum (M) d ) i B of alloy element i respectively o And M d Values.
The invention designs (Mo) a high-strength beta titanium alloy for inducing martensitic transformation based on a deformation mechanism eq ＝9-11，B o ＝2.77-2.79，M d ＝2.35-2.39。
Further, the smelting adopts a vacuum consumable arc furnace (VAR) smelting method, and ingot casting is carried out after smelting for 4 times.
Further, the homogenization treatment is carried out at 1000 ℃ for 1-2 hours;
in the cooling free multidirectional forging process, the temperature is reduced by 30-50 ℃ each time, and the deformation amount is 50% each time.
Further, the solution treatment time is 0.2-0.5h.
Further, in the asynchronous rolling process: the differential speed ratio is 1.1-1.5, the rolling is carried out in 2-4 times, and the total deformation is 90%.
Further, the asynchronous rolling specifically comprises:
cutting the forging subjected to solution treatment into a plate blank with the specification of 80X 30X 2mm, using hard alloy steel as a lining plate, rolling by using an asynchronous rolling mill, setting the speed ratio of the asynchronous rolling mill to be 1.1-1.5, then placing the plate blank into the asynchronous rolling mill for rolling, placing the lining plate on the plate blank, and rolling for 2-4 times, thereby finally obtaining the beta titanium alloy sheet with the thickness of 0.05-0.2mm, wherein the total deformation is 90%.
Further, the heat treatment is an annealing treatment, a solution treatment and a time-efficient treatment.
Further, the annealing treatment is a single-phase zone short-time annealing treatment, specifically: heating the asynchronously rolled product to a temperature which is 10-50 ℃ above the beta transformation temperature, and annealing for 0-0.5h to obtain equiaxed fine beta grains, wherein the annealing time is not 0;
the solid solution treatment is as follows: cooling the annealed product to a temperature which is 10-60 ℃ below the beta transformation temperature along with a furnace, and carrying out solution treatment for 0-0.5h to obtain a micron-sized primary alpha phase, wherein the solution treatment time is not 0;
the aging treatment is as follows: aging the product after solution treatment for 1-24h at the temperature of 200-500 ℃ below the beta transformation temperature to obtain the nanoscale secondary alpha phase.
According to the invention, by designing specific titanium alloy components and adopting room-temperature asynchronous rolling and combining a heat treatment process, the high-strength beta titanium alloy with a multi-scale microstructure is regulated and controlled. The alloy is deformed to induce martensitic transformation due to large room temperature deformation in the rolling process, deformation induced plasticity is generated, and cold deformation capacity is improved. The application of asynchronous rolling effectively avoids the problem of cracking of the plate in the rolling process while improving the deformation. And carrying out short-time annealing treatment and solution treatment on the alloy in a single-phase region and performing time-efficient treatment to obtain fine equiaxed beta grains, separating out a micron primary alpha phase and a nanometer secondary alpha phase, constructing a multi-scale microstructure, and effectively improving the alloy performance, thereby obtaining the high-strength beta titanium alloy sheet with excellent performance. The tensile strength of the plate obtained by the regulation and control of the method can reach 1600MPa; the elongation rate can reach 9 percent.
The high-strength beta titanium alloy based on stress induced martensite reverse phase transformation is obtained by processing according to the method, wherein the phase composition of the high-strength beta titanium alloy comprises equiaxed beta grains, micron-sized primary alpha phases and nano-sized secondary alpha phases which are dispersed and distributed in the beta phases, the average size of the equiaxed beta grains is 11-26 mu m, the average size of the micron-sized primary alpha phases is 1.1-2.0 mu m, and the average size of the nano-sized secondary alpha phases is 30-45nm; the tensile strength of the beta titanium alloy is 1300-1600MPa, the elongation is 6-11%, and the area shrinkage is 20-30%.
Compared with the prior art, the invention has the following advantages and technical effects:
(1) Through alloy composition design, cold deformation induced martensite deformation mechanism is combined with room temperature asynchronous rolling deformation process, room temperature deformation capacity of the beta titanium alloy plate is improved, deformation amount is improved, grain size is effectively refined, and plasticity is improved.
(2) The multi-scale microstructure is constructed in the heat treatment process, so that the excellent plasticity of the beta titanium alloy plate is ensured, meanwhile, the strength and the hardness are effectively improved, and the performance is good.
(3) The process is simple, the operation is easy, and the effective control of the process parameters can be realized.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. In the drawings:
FIG. 1 is a flow chart of a heat treatment process for a high strength beta titanium alloy based on stress induced martensitic reverse transformation;
FIG. 2 is a TEM image of an alloy after asynchronous lining at room temperature of example 1, the insert being the stress-induced martensitic structure after asynchronous lining;
fig. 3 is an SEM image (left image) of the alloy after the heat treatment of example 1 and a TEM image (right image) of the alloy after the heat treatment of example 1.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples of the present invention are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
The room temperature in the examples of the present invention is 25.+ -. 2 ℃ unless otherwise indicated.
Sponge titanium, high-purity aluminum (Al content is more than 99.999%), pure chromium, pure zirconium, aluminum-molybdenum alloy (Mo content is 75.15%) and aluminum-vanadium alloy (V content is 85.22%) in the embodiment of the invention are all purchased from Liaoyuan nonferrous alloy limited company.
The invention discloses a high-strength beta titanium alloy heat treatment process flow chart based on stress induced martensite reverse phase transformation, which is shown in figure 1.
Example 1
Step one, designing the components of beta titanium alloy:
according to Mo equivalent and d electron theory B o 、M d The alloy composition designed in this example is as follows: 3% Al,8% Mo,3% V,2% Cr,2% Zr, the balance being Ti and unavoidable impurity elements. Design [ Mo]eq＝8+1.6*2+0.67*3-0.5*2-3＝9.21，B o ＝2.426*0.055+3.063*0.041+2.805*0.029+2.779*0.019+3.086*0.011+2.790*0.845＝2.778，M d =2.200×0.055+1.961×0.041+1.872×0.029+1.478×0.019+2.934×0.011+2.447×0.845 = 2.379. The alloy designed according to the Mo equivalent value belongs to high-strength beta titanium alloy, and according to B o 、M d The values indicate that the deformation induced martensitic transformation occurs under the condition of large deformation at room temperature.
Step two, alloy smelting and forging:
(1) The method comprises the steps of taking titanium sponge, high-purity aluminum, pure chromium, pure zirconium, aluminum-molybdenum alloy (Mo content is 75.15%) and aluminum-vanadium alloy (V content is 85.22%) as raw materials, weighing the raw materials according to the weight percentage of each component, mixing, smelting, and smelting the alloy by adopting a vacuum consumable electrode arc furnace smelting method to obtain cast ingots after smelting for 4 times.
(2) Homogenizing the cast ingot at 1000 ℃ for 2 hours, then cogging and forging, then cooling, freely and multidirectional forging, wherein the temperature is reduced by 50 ℃ each time, the deformation amount is 50% each time, and the final forging temperature is 50 ℃ below the beta transition temperature, so as to obtain the forged piece.
Step three, room temperature asynchronous rolling
Solution treatment is carried out for 0.5h at 30 ℃ above the beta transus temperature to eliminate internal stress of forging deformation. The forgings were cut into slabs of 80X 30X 2mm by wire cutting machine using cemented carbide steel as a backing plate. The rolling is carried out by using an asynchronous rolling mill, the speed ratio of the asynchronous rolling mill is set to be 1.2, and then a plate blank (a lining plate is placed up and down) is stably placed into the asynchronous rolling mill for rolling. And 3 times of rolling are carried out, so that a high-strength beta titanium alloy sheet with the thickness of 0.1mm is finally obtained, the total deformation is 95%, and a TEM image of the alloy after room-temperature asynchronous lining rolling in the embodiment is shown in figure 2.
Step four, heat treatment
Annealing the rolled beta titanium alloy sheet for 0.1h at the temperature of 30 ℃ above the beta transformation temperature to obtain equiaxed fine beta grains; cooling the annealed sheet to 40 ℃ below the beta transformation temperature in a furnace for solution treatment for 0.2h to obtain a micron-sized primary alpha phase; and heating the sheet after solid solution to the temperature below the beta transformation temperature for aging treatment for 8 hours at 350 ℃ to obtain the nanoscale secondary alpha phase.
The SEM image of the alloy after heat treatment in this example is shown in the left image in fig. 3, the TEM image of the alloy after heat treatment is shown in the right image in fig. 3, and the phase composition of the beta titanium alloy sheet prepared in this example is equiaxed beta grains, micron-sized primary alpha phase and nano-sized secondary alpha phase dispersed in the beta phase, the average size of the beta grains is 12 μm, the average size of the primary alpha phase is 1.1 μm, and the average size of the secondary alpha phase is 30nm. The tensile strength of the beta titanium alloy sheet alloy is 1600MPa, the elongation is 9%, and the area reduction is 26%.
Example 2
The difference from example 1 is only that the rolled beta titanium alloy sheet is annealed for 0.2h at 30 ℃ above the beta transus temperature in step four (i.e. example 2 differs from example 1 only by the variation of the annealing time, the rest of the process is unchanged, and the subsequent solution treatment and aging treatment are unchanged).
The beta titanium alloy sheet prepared in this example comprises equiaxed beta grains, a micron-sized primary alpha phase and a nanometer-sized secondary alpha phase dispersed in the beta phase, wherein the average size of the beta grains is 26 mu m, the average size of the primary alpha phase is 1.2 mu m, and the average size of the secondary alpha phase is 35nm. The tensile strength of the alloy is 1300MPa, the elongation is 6%, and the area reduction is 25%.
Example 3
The difference from example 1 is only that the beta titanium alloy composition, in mass fraction, is: 2% Al,9% Mo,2% V,1% Cr,3% Zr, the balance being Ti and unavoidable impurity elements. Design [ Mo ] eq=9+1.6+0.67×2-0.5×3-2=8.44, bo= 2.426 x 0.037+3.063 x 0.047+2.805 x 0.020+2.779 x 0.010+3.086 x 0.017+2.790 x 0.870 =2.797, md= 2.200×0.037+1.961×0.047+1.872×0.020+1.478×0.010+2.934×0.017+2.447×0.870 = 2.404.
The beta titanium alloy sheet prepared in this example comprises equiaxed beta grains, a micron-sized primary alpha phase and a nanometer-sized secondary alpha phase dispersed in the beta phase, wherein the average size of the beta grains is 20 mu m, the average size of the primary alpha phase is 1.1 mu m, and the average size of the secondary alpha phase is 25nm. The tensile strength of the alloy is 1600MPa, the elongation is 6%, and the area reduction is 20%.
Example 4
The difference from example 1 is only that the beta titanium alloy composition, in mass fraction, is: 5% Al,6% Mo,4% V,4% Cr,1% Zr, the balance being Ti and unavoidable impurity elements. Design [ Mo ] eq=6+1.6×4+0.67×4-0.5-5=9.58, bo= 2.426 x 0.089+3.063 x 0.030+2.805 x 0.038+2.779 x 0.037+3.086 x 0.005+2.790 x 0.801 =2.767, md= 2.200×0.089+1.961×0.030+1.872×0.038+1.478×0.037+2.934×0.005+2.447×0.801 =2.355.
The beta titanium alloy sheet prepared in this example comprises unstable beta grains, a micron-sized primary alpha phase and a nanometer-sized secondary alpha phase dispersed in the beta phase, wherein the average size of the beta grains is 15 μm, the average size of the primary alpha phase is 2.0 μm, and the average size of the secondary alpha phase is 45nm. The tensile strength of the alloy is 1300MPa, the elongation is 11%, and the area reduction is 30%.
Example 5
Step one, designing the components of beta titanium alloy:
the beta titanium alloy comprises the following components in percentage by mass: 3% Al,7% Mo,2% V,2% Cr,2% Zr, the balance being Ti and unavoidable impurity elements. Design [ Mo ] eq=7+1.6×2+0.67×2-0.5×2-3=7.54, bo= 2.426 x 0.055+3.063 x 0.036+2.805 x 0.019+2.779 x 0.019+3.086 x 0.011+2.790 x 0.861 =2.786, md= 2.200×0.055+1.961×0.036+1.872×0.019+1.478×0.019+2.934×0.011+2.447×0.861 =2.394.
Step two, alloy smelting and forging:
(1) The method comprises the steps of taking titanium sponge, high-purity aluminum, pure chromium, pure zirconium, aluminum-molybdenum alloy (Mo content is 75.15%) and aluminum-vanadium alloy (V content is 85.22%) as raw materials, weighing the raw materials according to the weight percentage of each component, mixing, smelting, and smelting the alloy by adopting a vacuum consumable electrode arc furnace smelting method to obtain cast ingots after smelting for 4 times.
(2) Homogenizing the cast ingot at 1000 ℃ for 2 hours, then cogging and forging, then cooling, freely and multidirectional forging, wherein the temperature is reduced by 30 ℃ each time, the deformation amount is 50% each time, and the final forging temperature is 30 ℃ below the beta transition temperature, so that the forged piece is obtained.
Step three, room temperature asynchronous rolling
Solution treatment is carried out for 0.2h at 50 ℃ above the beta transus temperature to eliminate internal stress of forging deformation. The forgings were cut into slabs of 80X 30X 2mm by wire cutting machine using cemented carbide steel as a backing plate. The rolling is carried out by using an asynchronous rolling mill, the speed ratio of the asynchronous rolling mill is set to be 1.5, and then a plate blank (a lining plate is placed up and down) is stably placed into the asynchronous rolling mill for rolling. And rolling for 2 times to finally obtain the high-strength beta titanium alloy sheet with the thickness of 0.2mm, wherein the total deformation is 90%.
Step four, heat treatment
Annealing the rolled beta titanium alloy sheet for 0.1h at the temperature of 30 ℃ above the beta transformation temperature to obtain equiaxed fine beta grains; cooling the annealed sheet to 40 ℃ below the beta transformation temperature in a furnace for solution treatment for 0.2h to obtain a micron-sized primary alpha phase; and heating the sheet after solid solution to the temperature below the beta transformation temperature for aging treatment for 8 hours at 350 ℃ to obtain the nanoscale secondary alpha phase.
The beta titanium alloy sheet prepared in this example comprises equiaxed beta grains, a micron-sized primary alpha phase and a nanometer-sized secondary alpha phase dispersed in the beta phase, wherein the average size of the beta grains is 20 mu m, the average size of the primary alpha phase is 1.3 mu m, and the average size of the secondary alpha phase is 31nm. The tensile strength of the alloy is 1500MPa, the elongation is 6%, and the area reduction is 23%.
Example 6
Step one, designing the components of beta titanium alloy:
the beta titanium alloy comprises the following components in percentage by mass: 3% Al,8% Mo,3% V,2% Cr,2% Zr, the balance being Ti and unavoidable impurity elements. Design [ Mo]eq＝8+1.6*2+0.67*3-0.5*2-3＝9.21，B o ＝2.426*0.055+3.063*0.041+2.805*0.029+2.779*0.019+3.086*0.011+2.790*0.845＝2.778，M d ＝2.200*0.055+1.961*0.041+1.872*0.029+1.478*0.019+2.934*0.011+2.447*0.845＝2.379。
Step two, alloy smelting and forging:
(1) The method comprises the steps of taking titanium sponge, high-purity aluminum, pure chromium, pure zirconium, aluminum-molybdenum alloy (Mo content is 75.15%) and aluminum-vanadium alloy (V content is 85.22%) as raw materials, weighing the raw materials according to the weight percentage of each component, mixing, smelting, and smelting the alloy by adopting a vacuum consumable electrode arc furnace smelting method to obtain cast ingots after smelting for 4 times.
(2) Homogenizing the cast ingot at 1000 ℃ for 1h, then cogging and forging, then cooling, freely and multidirectional forging, wherein the temperature is reduced by 40 ℃ each time, the deformation amount is 50% each time, and the final forging temperature is 70 ℃ below the beta transition temperature, so that the forged piece is obtained.
Step three, room temperature asynchronous rolling
Solution treatment is carried out for 0.5h at 40 ℃ above the beta transus temperature to eliminate internal stress of forging deformation. The forgings were cut into slabs of 80X 30X 2mm by wire cutting machine using cemented carbide steel as a backing plate. The rolling is carried out by using an asynchronous rolling mill, the speed ratio of the asynchronous rolling mill is set to be 1.1, and then a plate blank (a lining plate is placed up and down) is stably placed into the asynchronous rolling mill for rolling. And 4 times of rolling are carried out, and finally the high-strength beta titanium alloy sheet with the thickness of 0.05mm is obtained, wherein the total deformation is 97.5%.
Step four, heat treatment
Annealing the rolled beta titanium alloy sheet for 0.2h at the temperature of 30 ℃ above the beta transformation temperature to obtain equiaxed fine beta grains; cooling the annealed sheet to 40 ℃ below the beta transformation temperature in a furnace for solution treatment for 0.2h to obtain a micron-sized primary alpha phase; and heating the sheet after solid solution to a temperature below the beta transition temperature for ageing treatment for 8 hours at 400 ℃ to obtain the nanoscale secondary alpha phase.
The beta titanium alloy sheet prepared in this example comprises equiaxed beta grains, a micron-sized primary alpha phase and a nanometer-sized secondary alpha phase dispersed in the beta phase, wherein the average size of the beta grains is 18 mu m, the average size of the primary alpha phase is 1.2 mu m, and the average size of the secondary alpha phase is 35nm. The tensile strength of the alloy is 1650MPa, the elongation is 8%, and the area reduction is 26%.
Comparative example 1
The difference from example 1 is that the beta titanium alloy composition, in mass fraction, is: 6% Al,8% Mo,2% V,2% Cr,2% Zr, the balance being Ti and unavoidable impurity elements.
The beta titanium alloy sheet prepared in this comparative example has a phase composition of a small amount of unstable beta grains, a micron-sized primary alpha phase and a nanometer-sized secondary alpha phase dispersed and distributed in the beta phase, wherein the average size of the beta grains is 15 mu m, the average size of the primary alpha phase is 3.0 mu m, and the average size of the secondary alpha phase is 60nm. The tensile strength of the alloy is 1250MPa, the elongation is 13%, and the area reduction is 35%. From example 1 and the comparative example, it is clear that the alloy strength is greatly reduced and the plasticity is remarkably improved due to the excessively high content of the alpha stabilizing element Al element in the alloy.
Comparative example 2
The difference from example 1 is that the beta titanium alloy composition, in mass fraction, is: 4% Al, 3% Zr, 9% Mo, 2.4% V,2% Cr, 2.5% Nb, 0.5% Si, the balance being Ti and unavoidable impurities.
The phase composition of the beta titanium alloy sheet prepared in the comparative example is equiaxed beta grains, nano-grade silicide dispersed in the beta phase and at the grain boundary, micron-grade primary alpha phase and nano-grade secondary alpha phase dispersed in the beta phase, the average size of the beta grains is 40 mu m, the average size of the primary alpha phase is 1.3 mu m, and the average size of the silicide of the secondary alpha phase is 45nm. The tensile strength of the alloy is 1800MPa, the elongation is 5%, and the area reduction is 20%. From example 1 and the comparative example, it is known that silicide is produced after Si element is added into the alloy, the advantage of multi-scale micro control is lost, the strength is increased, and the plasticity is reduced.
Comparative example 3
The difference from example 1 is that the rolling process in step three is hot rolling: rolling the forging piece for the first time at 750 ℃ until the deformation is 20%, then carrying out furnace return heat preservation for 5min at 750 ℃ and then carrying out second-time rolling until the deformation is 35%, and finally carrying out furnace return heat preservation for 5min at 750 ℃ and then carrying out third-time rolling until the deformation is 45%, thus obtaining a blank after hot rolling; the total deformation was 71.4%.
The beta titanium alloy sheet prepared in the comparative example comprises equiaxed beta grains, a micron-sized primary alpha phase and a nanometer-sized secondary alpha phase which is dispersed and distributed in the beta phase, wherein the average size of the beta grains is 45 mu m, the average size of the primary alpha phase is 2.0 mu m, and the average size of the secondary alpha phase is 40nm. The tensile strength of the alloy is 1400MPa, the elongation is 11%, and the area reduction is 30%. From example 1 and this comparative example, it is known that the refining effect of the cold rolling process on the crystal grains is better than that of the hot rolling process, and the grain size is increased after the hot rolling process is adopted, so that the strength of the alloy is reduced and the plasticity is improved.
Comparative example 4
The difference from example 1 is that the rolling process in step three is room temperature lining plate rolling, and solution treatment is performed for 0.5h at 40 ℃ above the beta transus temperature to eliminate internal stress of forging deformation. The forgings were cut into slabs of 80X 30X 2mm by wire cutting machine using cemented carbide steel as a backing plate. And rolling by using a double rolling mill, smoothly placing a plate blank (with lining plates placed up and down) into the double rolling mill for rolling, and carrying out 3-pass rolling to finally obtain the high-strength beta titanium alloy sheet with the thickness of 0.1mm, wherein the total deformation is 95%. The beta titanium alloy sheet prepared in the comparative example comprises equiaxed beta grains, a micron-sized primary alpha phase and a nanometer-sized secondary alpha phase which is dispersed and distributed in the beta phase, wherein the average size of the beta grains is 30 mu m, the average size of the primary alpha phase is 1.5 mu m, and the average size of the secondary alpha phase is 35nm. The tensile strength of the alloy is 1500MPa, the elongation is 7%, and the area reduction is 25%. From example 1 and this comparative example, it is clear that room temperature asynchronous backing plate rolling makes the deformation of the plate more sufficient, the effect of refining the crystal grains better, and at the same time makes the alloy deformability better and the strength higher than room temperature backing plate rolling.
Comparative example 5
The difference from example 1 is that no heat treatment was performed after asynchronous rolling at room temperature.
The beta titanium alloy sheet prepared in this comparative example had a phase composition of elongated non-uniform beta grains having an average size of 200 μm. The alloy has tensile strength of 1350MPa, elongation of 3% and reduction of area of 19%. From the example 1 and the comparative example, the heat treatment can construct a multi-scale microscopic regulation system, refine grains, and uniform structure, thereby greatly improving the mechanical properties of the alloy.
The present invention is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present invention are intended to be included in the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims (10)
1. The heat treatment method of the high-strength beta titanium alloy based on stress induced martensite reverse phase transformation is characterized by comprising the following steps of:
casting a beta titanium alloy cast ingot with the following mass composition: 2-5% of Al,6-9% of Mo,2-4% of V,1-4% of Cr,1-3% of Zr, and the balance of Ti and unavoidable impurity elements;
homogenizing the beta alloy cast ingot, cogging and forging, then cooling, freely and multidirectional forging, wherein the final forging temperature is 30-70 ℃ below the beta transition temperature, and a forging piece is obtained;
carrying out solution treatment on the forging at 20-50 ℃ above the beta transformation temperature;
asynchronous rolling is carried out on the forging subjected to solution treatment;
and carrying out heat treatment on the asynchronously rolled product.
2. The heat treatment method of high-strength beta titanium alloy based on stress induced martensitic reverse transformation according to claim 1, wherein the process of casting beta titanium alloy cast ingot is as follows: the method comprises the steps of taking titanium sponge, pure aluminum, pure chromium, pure zirconium, aluminum-molybdenum alloy and aluminum-vanadium alloy as raw materials, weighing the raw materials according to the weight percentage of each component, mixing, and then smelting and casting ingots to obtain alloy cast ingots.
3. The heat treatment method of the high-strength beta titanium alloy based on stress induced martensitic reverse transformation according to claim 2, wherein the smelting adopts a vacuum consumable electrode arc furnace smelting method, and ingot casting is carried out after smelting for 4 times.
4. The heat treatment method of the high-strength beta titanium alloy based on stress induced martensitic reverse transformation according to claim 1, wherein the temperature of the homogenization treatment is 1000 ℃ and the time is 1-2h;
in the cooling free multidirectional forging process, the temperature is reduced by 30-50 ℃ each time, and the deformation amount is 50% each time.
5. The method for heat treatment of high-strength beta titanium alloy based on stress induced martensitic reverse transformation according to claim 1, wherein the time of solution treatment is 0.2-0.5h.
6. The method for heat treatment of high-strength beta titanium alloy based on stress induced martensitic reverse transformation according to claim 1, wherein in the asynchronous rolling process: the differential speed ratio is 1.1-1.5, the rolling is carried out in 2-4 times, and the total deformation is 90%.
7. The heat treatment method of high-strength beta titanium alloy based on stress induced martensitic reverse transformation according to claim 6, wherein the asynchronous rolling specifically comprises:
cutting the forging subjected to solution treatment into a plate blank with the specification of 80X 30X 2mm, using hard alloy steel as a lining plate, rolling by using an asynchronous rolling mill, setting the speed ratio of the asynchronous rolling mill to be 1.1-1.5, then placing the plate blank into the asynchronous rolling mill for rolling, placing the lining plate on the plate blank, and rolling for 2-4 times, thereby finally obtaining the beta titanium alloy sheet with the thickness of 0.05-0.2mm, wherein the total deformation is 90%.
8. The heat treatment method of the high-strength beta titanium alloy based on stress induced martensitic reverse transformation according to claim 1, wherein the heat treatment is to sequentially perform annealing treatment, solution treatment and time-efficient treatment on an asynchronously rolled product.
9. The method for heat treatment of high-strength beta titanium alloy based on stress induced martensitic reverse transformation according to claim 8, wherein the annealing treatment is: heating the asynchronously rolled product to a temperature 10-50 ℃ above the beta transformation temperature, and annealing for 0-0.5h, wherein the annealing time is not 0;
the solid solution treatment is as follows: cooling the annealed product to a temperature which is 10-60 ℃ below the beta transformation temperature along with a furnace, and carrying out solution treatment for 0-0.5h, wherein the solution treatment time is not 0;
the aging treatment is as follows: aging the product after solution treatment for 1-24h at 200-500 ℃ below the beta transformation temperature.
10. The high-strength beta titanium alloy based on stress induced martensite reverse phase transformation is characterized in that the high-strength beta titanium alloy is obtained by treatment according to any one of the claims 1-9, and the phase composition comprises equiaxed beta grains, micron-sized primary alpha phases and nanoscale secondary alpha phases which are dispersed and distributed in the beta phases, wherein the average size of the equiaxed beta grains is 11-26 mu m, the average size of the micron-sized primary alpha phases is 1.1-2.0 mu m, and the average size of the nanoscale secondary alpha phases is 30-45nm.
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