CN115679153B - High-strength and high-toughness short-time high-temperature titanium alloy plate and preparation method and application thereof - Google Patents
High-strength and high-toughness short-time high-temperature titanium alloy plate and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a high-strength and high-toughness short-time high-temperature titanium alloy plate and a preparation method and application thereof, and relates to the technical field of titanium alloy materials. The element composition comprises, by mass, 7% -8% of Al, 3% -4% of Sn, 10% -12% of Zr, 2% -3% of Mo, 2% -3% of Nb, 1% -2% of W, 0.5% -0.7% of Si, the balance of Ti and trace unavoidable impurity elements. The invention adopts a thermal mechanical treatment process of solution quenching, forging cogging, double lining plate rolling and aging annealing to obtain the large-size titanium alloy plate which has fine grains, second phase nano dispersion distribution, no edge crack, excellent room temperature process plasticity and high temperature instantaneous strength, and meets the requirements of aerospace and military equipment industry on the comprehensive performance of alloy materials.
Description
Technical Field
The invention relates to the technical field of titanium alloy materials, in particular to a high-strength and high-toughness short-time high-temperature titanium alloy plate and a preparation method and application thereof.
Background
High temperature titanium alloys such as IMI834, ti1100, BT36, ti60, ti600, etc. which are widely used at present have excellent high temperature strength and structural stability at 600 c, and high oxidation resistance and creep resistance, and can stably operate for a long period at 600 c. However, when the temperature is exceeded, the mechanical properties and oxidation resistance of the traditional high-temperature titanium alloys are drastically reduced, and the service requirements cannot be met, so that the development of the high-temperature titanium alloys at 650-700 ℃ which can meet the requirements of rapid development in the fields of aerospace, military industry and the like at present becomes a key problem to be solved. And for materials with special working conditions such as a spacecraft body, a gas compressor disc, military weapon parts and the like, the performances such as high-temperature creep, fatigue and the like of the alloy can be ignored to a certain extent due to short service time, and the room-temperature process plasticity and the instantaneous high-temperature strength are focused, so that a wider thought is provided for developing a novel short-time high-temperature titanium alloy with higher temperature resistance. At present, some researches are carried out on short-time high-temperature titanium alloy at 650-700 ℃, such as Ti65, ti650, BTi-6431S, BTi-62421S and the like, but the research and development stages are not carried out, and large-scale engineering application reports are not seen, particularly, the room-temperature plasticity and the high-temperature mechanical property of the titanium alloy plate with large size (the plate with the width of more than or equal to 400mm, the length of more than or equal to 1000mm and the thickness of 0.2-4 mm) are still required to be further improved when the titanium alloy plate is used as a sheet metal member blank and a high-temperature bearing element. A large number of researches show that the thermal deformation is an important means for refining a coarse initial structure of the high-temperature titanium alloy, regulating and controlling precipitation and distribution of a second phase and effectively improving the comprehensive mechanical property of the high-temperature titanium alloy. However, conventional hot working methods such as extrusion, rolling and forging have difficulty in eliminating inherent defects and realizing precise regulation of microstructure due to large deformation resistance of the titanium alloy and tissue evolution sensitivity to hot process parameters. Therefore, how to prepare a large-size short-time high-temperature titanium alloy plate at 650-700 ℃ is a technical problem to be solved in the prior art.
Disclosure of Invention
Based on the above, the invention provides a high-strength and high-toughness short-time high-temperature titanium alloy plate and a preparation method and application thereof, and adopts a thermomechanical treatment process of solution quenching, forging cogging, double lining plate rolling and aging annealing to prepare a large-size titanium alloy plate with fine grains, second phase nano dispersion distribution, no edge crack and excellent room temperature process plasticity and high-temperature instantaneous strength, thereby overcoming the problems of insufficient room temperature plasticity and high-temperature strength and serious edge crack of the novel 650-700 ℃ short-time high-temperature titanium alloy plate in the prior art.
In order to achieve the above object, the present invention provides the following solutions:
according to one of the technical schemes, the high-strength and high-toughness short-time high-temperature titanium alloy plate comprises, by mass, 7% -8% of Al, 3% -4% of Sn, 10% -12% of Zr, 2% -3% of Mo, 2% -3% of Nb, 1% -2% of W, 0.5% -0.7% of Si, the balance of Ti and trace unavoidable impurity elements.
The second technical scheme of the invention is that the preparation method of the high-strength and high-toughness short-time high-temperature titanium alloy plate comprises the following steps:
melting, mixing and casting the raw materials of each alloy element according to the mass percentage ratio to obtain an alloy cast ingot;
sequentially carrying out solution quenching, forging cogging, double-lining-plate rolling and aging treatment on the alloy cast ingot to obtain the high-strength and high-toughness short-time high-temperature titanium alloy plate;
the solution hardening specifically comprises the following steps: placing the alloy ingot into a silicide to be subjected to solution treatment at a temperature above the silicide dissolution temperature, and then quenching the alloy ingot by using a NaCl aqueous solution;
the forging cogging specifically comprises: forging upsetting for one pass is carried out along the height direction of an alloy sample, the deformation temperature is lower than the alpha+beta/beta phase transition temperature of the alloy cast ingot, the heat preservation is carried out before forging, the process deformation is 60-80%, and the strain rate is 0.05s -1 ～0.1s -1 Air cooling after forging;
the rolling of the double lining plates is specifically as follows: respectively paving a hard alloy lining plate on the upper surface and the lower surface of a sample to be rolled, preserving heat under the temperature condition of being lower than the alpha+beta/beta phase transition temperature of the alloy ingot, synchronously feeding the alloy ingot into a roller for 4-6 times of rolling, and carrying out furnace return heat preservation between the passes of rolling;
the aging treatment specifically comprises the following steps: and (3) performing aging annealing treatment in a vacuum environment at 650-750 ℃ and then performing air cooling.
Further, the alloy ingot is a widmannstatten structure, comprising an initial beta grain, and a lamellar alpha beam domain inside the beta grain.
Further, the solution hardening specifically includes: and (3) placing the alloy ingot into solid solution for 2-4 hours at a temperature of 5-20 ℃ above the silicide dissolution temperature, and then quenching with 5-15 wt.% NaCl aqueous solution.
Further, in the forging and cogging process, the deformation temperature is 80-100 ℃ below the alpha+beta/beta transformation temperature of the alloy ingot, and the temperature is kept for 20-30 min before forging.
Further, the double-lining plate rolling specifically comprises: and respectively paving a hard alloy lining plate on the upper surface and the lower surface of a sample to be rolled, preserving heat for 20-40 min at the temperature of 20-50 ℃ below the alpha+beta/beta transformation temperature of the alloy ingot, synchronously feeding the alloy ingot into a roller for 4-6 times of rolling, wherein the rolling reduction of each time is 15%, the total rolling reduction is 60-90%, and carrying out furnace return heat preservation between the times of the rolling, wherein the temperature and the time of the furnace return heat preservation of each time are the same.
Further, the aging treatment specifically comprises: aging annealing treatment is carried out for 4 to 8 hours in a vacuum environment with the temperature of 650 to 750 ℃ and the vacuum degree of 10 -1 ～10 -2 Pa, followed by air cooling.
The third technical scheme of the invention is the application of the high-strength and high-toughness short-time high-temperature titanium alloy plate in the preparation of aerospace craft bodies, air compressor discs and military weapon parts.
The technical conception of the invention is as follows:
(1) Selecting alloy components: the design principle of critical Al equivalent and critical valence electron concentration is broken through in the component design. Based on the existing Ti-Al-Sn-Zr-Mo-Nb-W-Si short-time high-temperature titanium alloy component, 1) the Al equivalent is improved, and the subsequent aging treatment regulates and controls the brittleness alpha 2 The phase is precipitated in nano size, plays the role of dispersion strengthening, and reasonably utilizes alpha 2 High temperature strengthening effect of the phase; 2) The content of beta-stable element (Mo, nb, W, si) is increasedThe seed element can effectively strengthen beta phase, improve the heat intensity of the alloy, obtain more beta phase in the alloy structure and improve the manufacturability. The addition of too much beta stabilising element will deteriorate the thermal stability of the alloy, but for short-time high temperature titanium alloys the requirements for thermal stability of the alloy are lower due to the short service time. In addition, si exceeding the solid solution limit will precipitate in the form of silicide, which has a strong pinning effect on dislocation and can effectively strengthen grain boundaries and phase boundaries.
(2) Alloy ingot casting: the as-cast alloy is a widmannstatten structure comprising an initial beta grain, and lamellar alpha domains within the beta grain.
(3) Solution hardening: because the content of Zr in the alloy is high (10-12 wt.%), the solid solubility of Si in the matrix is obviously reduced, that is, the dissolution temperature of silicide is greatly raised, and according to the simulation result of phase diagram, the silicide dissolution temperature of the series of alloy is higher than alpha+beta/beta phase transition temperature by 150 ℃, so that coarse silicide precipitated along the initial beta grain boundary in the solidification process possibly exists in the structure of the cast alloy, and the large-size silicide precipitated along the grain boundary obviously has adverse effect on the alloy performance, so that the invention designs the cast alloy to be fully dissolved at 5-20 ℃ above the silicide dissolution temperature (Ts) so as to redissolve the precipitated silicide into the matrix. In order to retain a high-temperature morphology and obtain a fine martensitic structure, post-solutionizing quench treatment. The quenching medium is NaCl water solution, so that the alloy can be cooled at a high cooling speed and uniformly, and oxides on the surface of the alloy can be cracked and peeled off.
(4) Forging and cogging: the martensite phase alpha' obtained after quenching is a supersaturated solid solution of alpha-Ti, and decomposition occurs when heated or deformed at high temperature. Therefore, when the forging deformation is performed at a temperature higher than the recrystallization temperature, the needle-like α' -martensite is crushed and recrystallized to form a locally equiaxed fine grain structure. Notably, a number of defects exist within the α' martensite sheet layer that are capable of providing energy upon recrystallization and serve as nucleation sites, effectively promoting refinement of the matrix grains. The equiaxed fine grain structure has small deformation resistance and provides a good structure foundation for subsequent rolling deformation.
(5) Rolling the double lining plates: compared with the common rolling, the double-lining plate rolling can effectively reduce or even eliminate the edge crack phenomenon of the rolled plate, which is verified in the test, and almost no edge crack is generated around the rolled plate. The rolling temperature is selected to be 20-50 ℃ below the alpha+beta/beta phase transition temperature and is positioned at the upper end of the alpha+beta two-phase region, and a double-state structure with fine grains is obtained under the condition of large deformation. In addition, under the rolling deformation condition, silicide is precipitated again in a micro-nano size, and the silicide has good dislocation strengthening effect when the alloy is deformed under stress.
(6) Aging annealing: to give full play to alpha 2 Phase dispersion strengthening, aging rolled plate to regulate alpha 2 And the phase nano-dispersion is separated out. Furthermore, in order to avoid oxidation of the sheet, the entire ageing process is carried out in a vacuum environment. The sheet obtained in example 1 has a tensile strength at room temperature of 1370MPa and an elongation of 14.2%; the tensile strength at 700 ℃ is 642MPa, the elongation is 22.4%, and the comprehensive performance is obviously better than that of Ti65 and BTi-6431S alloy.
The invention discloses the following technical effects:
(1) The invention adopts a thermal mechanical treatment process of solution quenching, forging cogging, double lining plate rolling and aging annealing to obtain the large-size titanium alloy plate which has fine grains, second phase nano dispersion distribution, no edge crack, excellent room temperature process plasticity and high temperature instantaneous strength, and meets the requirements of aerospace and military equipment industry on the comprehensive performance of alloy materials.
(2) The method has simple process steps and is suitable for mass industrialized production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a macroscopic view, a microscopic SEM image and a spot sweep of the titanium alloy sheet prepared in example 1; wherein, (a) macroscopic view, (b) microscopic SEM view, (c) spot scanning result of precipitated phase.
FIG. 2 is an as-cast OM map, an as-cast SEM map and an as-cast quenched OM map of the step 2 alloy ingot of example 1 and an OM map after forging cogging of step 4; wherein, (a) an as-cast OM map; (b) as-cast SEM images; (c) as-cast quenched OM plot; (d) OM plot after cogging forging.
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 invention provides a high-strength and high-toughness short-time high-temperature titanium alloy plate, which comprises, by mass, 7% -8% of Al, 3% -4% of Sn, 10% -12% of Zr, 2% -3% of Mo, 2% -3% of Nb, 1% -2% of W, 0.5% -0.7% of Si, the balance of Ti and trace unavoidable impurity elements.
The invention also provides a preparation method of the high-strength and high-toughness short-time high-temperature titanium alloy plate, which comprises the following steps:
step 1, weighing raw materials: and calculating and weighing titanium sponge, high-purity aluminum, pure tin particles, zirconium sponge, crystalline silicon, al-Mo, al-Nb and Al-W intermediate alloy as raw materials. Wherein the mass percentages of the components are 7-8% of Al, 3-4% of Sn, 10-12% of Zr, 2-3% of Mo, 2-3% of Nb, 1-2% of W, 0.5-0.7% of Si, the balance of Ti and trace unavoidable impurity elements respectively;
step 2, smelting cast ingots: and (3) sequentially adding the titanium sponge, high-purity aluminum, pure tin particles, zirconium sponge, crystalline silicon, al-Mo, al-Nb and Al-W intermediate alloy weighed in the step (1) into a vacuum consumable furnace for smelting. Firstly, the smelting furnace is vacuumized to 10 -2 ～10 -3 Pa, then raising the power of the power supply to 30-35 KW, wherein the power raising speed is not more than 0.02KW/s, reducing the power to 10-15 KW after the alloy raw materials are completely melted, preserving heat for 15-20 min, and finally pouring into a metal casting mould preheated to 500-600 ℃ to obtain an alloy cast ingot; the alloy cast ingot is a Wittig structure and comprises an initial beta grain and a lamellar alpha beam domain in the beta grain; determining the alpha+beta/beta phase transition temperature of the alloy by adopting a Differential Scanning Calorimetry (DSC);
the widmannstatten structure of the alloy ingot is obtained based on two conditions of element content limitation and preparation method. The alloy composition ratio provided by the invention belongs to near alpha high temperature titanium alloy, and the as-cast structure of the titanium alloy obtained by vacuum induction smelting is Wittig structure. However, if the alloy of this composition is made by other means, such as additive manufacturing, the initial structure obtained may not be a widmannstatten structure.
The alloy cast structures with different element composition ratios in the range are Wittig structures, and the difference is that the size of the initial beta grains and the thickness of the alpha sheet layers are different.
Step 3, solution hardening: the alloy ingot is subjected to solid solution for 2 to 4 hours at a temperature of 5 to 20 ℃ above silicide dissolution temperature (Ts), and then is subjected to quenching treatment by 5 to 15wt.% NaCl aqueous solution;
step 4, forging cogging: forging and upsetting the quenching sample obtained in the step 3 in one pass along the height direction; the alloy sample is coated with a layer of titanium alloy forging protective lubricant (Ti-1200) in advance, the deformation temperature is 80-100 ℃ below the alpha+beta/beta phase transition temperature, the heat preservation is carried out for 20-30 min before forging, the technological deformation is 60-80%, and the strain rate is selected to be 0.05s -1 ～0.1s -1 Air cooling after forging;
step 5, rolling the double lining plates: cutting the sample obtained in the step 4 into a cuboid thick plate, and then rolling by using a hot rolling mill; before rolling, paving a hard alloy (301 stainless steel or other types of stainless steel) lining plate on the upper and lower surfaces of the thick plate respectively, wherein the thickness of the lining plate is 1-2 mm, and synchronously deforming the lining plate and a sample under stress during rolling; the method comprises the following steps: firstly, uniformly coating a high-temperature lubricant on the upper surface and the lower surface of a lining plate and an alloy sample, then putting the lining plate and the alloy sample into a heat treatment furnace for heating, setting the furnace temperature to be 20-50 ℃ below the alpha+beta/beta phase transition temperature, keeping the temperature for 20-40 min, and then synchronously feeding the materials into a roller for 4-6 times of rolling, wherein the rolling amount of each time is 15%, and the total rolling amount is 60-90%; the furnace returning and heat preservation are carried out between the passes, and the parameters are the same as the above;
step 6, aging treatment: aging annealing treatment is carried out on the plate after the rolling of the lining plate for 4 to 8 hours in a vacuum environment with the temperature of 650 to 750 ℃ and the vacuum degree of 10 -1 ～10 -2 Pa, and then air-cooling to room temperature.
The invention also provides application of the high-strength and high-toughness short-time high-temperature titanium alloy plate in preparation of aerospace craft bodies, air compressor discs and military weapon parts.
As used herein, the term "room temperature" means 15 to 30℃unless otherwise specified.
Example 1
The preparation method of the short-time high-temperature titanium alloy plate Ti-7.5Al-3Sn-10Zr-2Mo-2Nb-1W-0.5Si comprises the following steps:
step 1, weighing raw materials: sequentially weighing 50kg of titanium sponge, high-purity aluminum, pure tin particles, zirconium sponge, crystalline silicon, al-Mo, al-Nb and Al-W intermediate alloy serving as raw materials according to the weight percentage of each component.
Step 2, smelting cast ingots: and (3) placing the titanium sponge, high-purity aluminum, pure tin particles, zirconium sponge, crystalline silicon, al-Mo, al-Nb and Al-W intermediate alloy weighed in the step (1) into a vacuum consumable furnace for smelting. Firstly, the smelting furnace is vacuumized to 10 -2 Pa, then raising the power of a power supply to 35KW, wherein the power raising speed is 0.02KW/s, reducing the power to 15KW after the alloy raw materials are completely melted, preserving heat for 20min, and finally pouring into a metal casting mould which is preheated to 600 ℃ to obtain an alloy cast ingot, wherein the alpha+beta/beta phase transition temperature is 1004 ℃ through DSC.
Step 3, solution hardening: as-cast samples of 10 mm. Times.10 mm. Times.6 mm were solution quenched at various temperatures (1120. Times.1140, 1160. Times.1180, 1200 ℃ C.) for 0.5h, and the silicide dissolution temperature was determined to be approximately 1190 ℃ by observing the structure. Thus, the alloy ingot prepared in step 2 was solid-solutionized at 1200 ℃ for 4 hours, followed by quenching with 15wt.% aqueous NaCl.
Step 4, forging cogging: forging and upsetting the quenching sample obtained in the step 3 in one pass along the height direction, wherein the forging and upsetting comprises the following steps of: the quenching sample is coated with a layer of titanium alloy forging protective lubricant (Ti-1200) in advance, the deformation temperature is 920 ℃, the heat preservation is carried out for 30min before forging, the process deformation is 60%, and the strain rate is 0.05s -1 Air cooling after forging.
Step 5, rolling the double lining plates: the specimen obtained in step 4 was cut into thick plates of 320 mm. Times.150 mm. Times.20 mm, followed by rolling using a hot rolling mill. Before rolling, hard alloy (301 stainless steel) lining plates are respectively paved on the upper surface and the lower surface of the thick plate, the thickness of the lining plates is 2mm, and the lining plates and the test sample are synchronously stressed to deform during rolling. The method comprises the following steps: the high-temperature lubricant is firstly uniformly coated on the upper surface and the lower surface of a lining plate and an alloy sample, then the lining plate and the upper surface and the lower surface of the alloy sample are put into a heat treatment furnace together for heating, the furnace temperature is set to 980 ℃, and after the temperature is kept for 40min, the high-temperature lubricant is synchronously sent into a roller for 6-pass rolling, the rolling amount of each pass is 15%, and the total rolling amount is 90%. And carrying out furnace return heat preservation between the passes, wherein parameters are the same as the above. After rolling, a 1500mm by 400mm by 2mm high temperature titanium alloy sheet was obtained.
Step 6, aging treatment: the plate after rolling the double lining plates is heated to 700 ℃ and 10 DEG C -1 And (3) performing aging annealing treatment for 8 hours in a vacuum environment of Pa, and then air-cooling to room temperature to obtain the short-time high-temperature titanium alloy plate Ti-7.5Al-3Sn-10Zr-2Mo-2Nb-1W-0.5Si.
The short-time high-temperature titanium alloy plate prepared by the embodiment has the dimensions of 1500mm multiplied by 400mm multiplied by 2mm, no edge crack, room-temperature tensile strength of 1370MPa and elongation of 14.2%; the tensile strength at 700℃was 642MPa and the elongation was 22.4%.
FIG. 1 is a macroscopic view, a microscopic SEM image and a spot sweep of the titanium alloy sheet prepared in example 1; wherein, (a) is a macroscopic view, (b) is a microscopic SEM view, and (c) is a point scan of the precipitated phase. The drawing (a) shows that the alloy sheet obtained in example 1 has a macroscopic size of 1500mm×400mm×2mm and no edge crack around. From the graph (b), it can be seen that the sheet microstructure is a bimodal structure, including equiaxed alpha grains and beta transformed structures. In addition, it was found that the white granular precipitate was uniformly distributed in the matrix structure and the size was about 60 to 500nm, and EDS results (in the figure (c)) showed that the precipitate phase was silicide.
FIG. 2 is an as-cast OM map, an as-cast SEM map and an as-cast quenched OM map of the step 2 alloy ingot of example 1 and an OM map after forging cogging of step 4; wherein, (a) is an as-cast OM pattern; (b) is an as-cast SEM image; (c) an as-cast quenched OM view; (d) is OM diagram after cogging forging. Fig. 2 shows the alloy structure corresponding to the different steps of example 1. The alloy is in an as-cast condition and is of a Wittig structure, and the three-fork grain boundary of the initial beta grains is clearly visible (a and b) in the figure. After solution hardening at 1200 c, the alloy is transformed into a fine needle-like α' martensitic structure (fig. (c)). This alpha' martensite breaks and recrystallises after forging deformation to form a partially equiaxed fine-grained and refined alpha lamellar structure (figure (d)).
Example 2
The preparation method of the short-time high-temperature titanium alloy plate Ti-8Al-3Sn-12Zr-2Mo-2Nb-1W-0.7Si comprises the following steps:
step 1, weighing raw materials: according to the weight percentage of each component, sequentially weighing 10kg of titanium sponge, high-purity aluminum, pure tin particles, zirconium sponge, crystalline silicon, al-Mo, al-Nb and Al-W intermediate alloy as raw materials.
Step 2, smelting cast ingots: and (3) placing the titanium sponge, high-purity aluminum, pure tin particles, zirconium sponge, crystalline silicon, al-Mo, al-Nb and Al-W intermediate alloy weighed in the step (1) into a vacuum consumable furnace for smelting. Firstly, the smelting furnace is vacuumized to 10 -3 Pa, then raising the power of a power supply to 30KW, wherein the power raising speed is 0.015KW/s, reducing the power to 10KW after the alloy raw materials are completely melted, preserving heat for 15min, and finally pouring into a metal casting mould preheated to 500 ℃ to obtain an alloy cast ingot, wherein the alpha+beta/beta phase transition temperature is 982 ℃ measured by DSC.
Step 3, solution hardening: as-cast samples of 10 mm. Times.10 mm. Times.6 mm were solution quenched at various temperatures (1200 ℃ C., 1220 ℃ C., 1240 ℃ C., 1260 ℃ C., 1280 ℃ C.) for 0.5 hours, and the silicide dissolution temperature was determined to be approximately 1270 ℃ by observing the structure. Thus, the alloy ingot prepared in step 2 was solutionized at 1290 ℃ for 2 hours, followed by quenching with 5wt.% aqueous NaCl solution.
Step 4, forging cogging: forging and upsetting the quenching sample obtained in the step 3 in one pass along the height direction, wherein the forging and upsetting comprises the following steps of: the quenching sample is coated with a layer of titanium alloy forging protective lubricant (Ti-1200) in advance, the deformation temperature is 900 ℃, the heat preservation is carried out for 20 minutes before forging, the process deformation is 80%, and the strain rate is 0.1s -1 Air cooling after forging.
Step 5, rolling the double lining plates: the specimen obtained in step 4 was cut into a thick plate of 100 mm. Times.60 mm. Times.20 mm, followed by rolling using a hot rolling mill. Before rolling, hard alloy (301 stainless steel) lining plates are respectively paved on the upper surface and the lower surface of the thick plate, the thickness of the lining plates is 2mm, and the lining plates and the test sample are synchronously stressed to deform during rolling. The method comprises the following steps: the high-temperature lubricant is firstly uniformly coated on the upper surface and the lower surface of a lining plate and an alloy sample, then the lining plate and the upper surface and the lower surface of the alloy sample are put into a heat treatment furnace together for heating, the furnace temperature is set to 962 ℃, and after 20 minutes of temperature preservation, the high-temperature lubricant is synchronously sent into a roller for 6 times of rolling, the rolling amount of each time is 15%, and the total rolling amount is 90%. And carrying out furnace return heat preservation between the passes, wherein parameters are the same as the above. After rolling, a 510mm by 150mm by 2mm high temperature titanium alloy sheet without edge cracking was obtained.
Step 6, aging treatment: the plate after rolling the double lining plates is heated to 650 ℃ and 10 DEG C -2 And (3) carrying out aging annealing treatment for 4 hours in a vacuum environment of Pa, and then cooling to room temperature by air to obtain the short-time high-temperature titanium alloy plate Ti-8Al-3Sn-12Zr-2Mo-2Nb-1W-0.7Si.
The short-time high-temperature titanium alloy plate prepared by the embodiment has the dimensions of 510mm multiplied by 150mm multiplied by 2mm, no edge crack, the room-temperature tensile strength of 1427MPa and the elongation of 9.8%; the tensile strength at 700℃was 655MPa and the elongation was 17.3%.
Example 3
The preparation method of the short-time high-temperature titanium alloy plate Ti-7Al-3Sn-10Zr-3Mo-3Nb-2W-0.5Si comprises the following steps:
step 1, weighing raw materials: according to the weight percentage of each component, sequentially weighing 10kg of titanium sponge, high-purity aluminum, pure tin particles, zirconium sponge, crystalline silicon, al-Mo, al-Nb and Al-W intermediate alloy as raw materials.
Step 2, smelting cast ingots: and (3) placing the titanium sponge, high-purity aluminum, pure tin particles, zirconium sponge, crystalline silicon, al-Mo, al-Nb and Al-W intermediate alloy weighed in the step (1) into a vacuum consumable furnace for smelting. Firstly, the smelting furnace is vacuumized to 10 -3 Pa, then raising the power of a power supply to 30KW, wherein the power raising speed is 0.015KW/s, reducing the power to 10KW after the alloy raw materials are completely melted, preserving heat for 15min, and finally pouring into a metal casting mould which is preheated to 500 ℃ to obtain an alloy cast ingot, wherein the alpha+beta/beta phase transition temperature is 942 ℃ measured by DSC.
Step 3, solution hardening: as-cast samples of 10 mm. Times.10 mm. Times.6 mm were solution quenched at various temperatures (1140 ℃, 1160 ℃, 1180 ℃, 1200 ℃, 1220 ℃) for 0.5h, and the silicide dissolution temperature was determined to be approximately 1220 ℃ by observing the structure. Thus, the alloy ingot prepared in step 2 was solutionized at 1225 ℃ for 2 hours, followed by quenching with 10wt.% aqueous NaCl.
Step 4, forging cogging: forging and upsetting the quenching sample obtained in the step 3 in one pass along the height direction, wherein the forging and upsetting comprises the following steps of: the quenching sample is coated with a layer of titanium alloy forging protective lubricant (Ti-1200) in advance, the deformation temperature is 862 ℃, the heat preservation is carried out for 20min before forging, the process deformation is 80%, and the strain rate is 0.1s -1 Air cooling after forging.
Step 5, rolling the double lining plates: the specimen obtained in step 4 was cut into a thick plate of 100 mm. Times.60 mm. Times.20 mm, followed by rolling using a hot rolling mill. Before rolling, hard alloy (301 stainless steel) lining plates are respectively paved on the upper surface and the lower surface of the thick plate, the thickness of the lining plates is 2mm, and the lining plates and the test sample are synchronously stressed to deform during rolling. The method comprises the following steps: the high-temperature lubricant is firstly uniformly coated on the upper surface and the lower surface of a lining plate and an alloy sample, then the lining plate and the upper surface and the lower surface of the alloy sample are put into a heat treatment furnace together for heating, the furnace temperature is 922 ℃, the high-temperature lubricant is kept for 20min, and then the high-temperature lubricant is synchronously sent into a roller for 6-pass rolling, the rolling amount of each pass is 15%, and the total rolling amount is 90%. And carrying out furnace return heat preservation between the passes, wherein parameters are the same as the above. After rolling, a 510mm by 150mm by 2mm high temperature titanium alloy sheet without edge cracking was obtained.
Step 6, aging treatment: the plate after rolling the double lining plates is heated to 650 ℃ and 10 DEG C -2 And (3) carrying out aging annealing treatment for 4 hours in a vacuum environment of Pa, and then cooling to room temperature by air to obtain the short-time high-temperature titanium alloy plate Ti-7Al-3Sn-10Zr-3Mo-3Nb-2W-0.5Si.
The short-time high-temperature titanium alloy plate prepared by the embodiment has the dimensions of 510mm multiplied by 150mm multiplied by 2mm, no edge crack, the room-temperature tensile strength of 1223MPa and the elongation of 13.4%; the tensile strength at 700℃was 567MPa and the elongation was 25.6%.
Example 4
The preparation method of the short-time high-temperature titanium alloy plate Ti-7Al-3.5Sn-11Zr-2Mo-3Nb-1W-0.6Si comprises the following steps:
step 1, weighing raw materials: according to the weight percentage of each component, sequentially weighing 20kg of titanium sponge, high-purity aluminum, pure tin particles, zirconium sponge, crystalline silicon, al-Mo, al-Nb and Al-W intermediate alloy as raw materials.
Step 2, smelting cast ingots: and (3) placing the titanium sponge, high-purity aluminum, pure tin particles, zirconium sponge, crystalline silicon, al-Mo, al-Nb and Al-W intermediate alloy weighed in the step (1) into a vacuum consumable furnace for smelting. Firstly, the smelting furnace is vacuumized to 10 -2 Pa, then the power of the power supply is increased to 32KW, the power increasing speed is 0.015KW/s, the power of the alloy raw material is reduced to 12KW after the alloy raw material is completely melted, the alloy raw material is kept for 18min, and finally the alloy raw material is poured into a metal casting mold which is preheated to 550 ℃ to obtain an alloy cast ingot, and the alpha+beta/beta phase transition temperature of the alloy cast ingot is 954 ℃ measured by DSC.
Step 3, solution hardening: as-cast samples of 10 mm. Times.10 mm. Times.6 mm were solution quenched at various temperatures (1200 ℃ C., 1220 ℃ C., 1240 ℃ C., 1260 ℃ C., 1280 ℃ C.) for 0.5 hours, and the silicide dissolution temperature was determined to be approximately 1270 ℃ by observing the structure. Thus, the alloy ingot prepared in step 2 was solid-solutionized at 1280 ℃ for 3 hours, followed by quenching with 10wt.% aqueous NaCl.
Step 4, forging cogging: forging and upsetting the quenching sample obtained in the step 3 in one pass along the height direction, wherein the forging and upsetting comprises the following steps of: the quenching sample is coated with a layer of titanium alloy forging protective lubricant (Ti-1200) in advance, the deformation temperature is 865 ℃, the heat preservation is carried out for 25 minutes before forging, the process deformation is 70%, and the strain rate is 0.05s -1 Air cooling after forging.
Step 5, rolling the double lining plates: the sample obtained in step 4 was cut into a thick plate of 200mm X100 mm X10 mm, followed by rolling using a hot rolling mill. Before rolling, hard alloy (301 stainless steel) lining plates are respectively paved on the upper surface and the lower surface of the thick plate, the thickness of the lining plates is 1mm, and the lining plates and the test sample are synchronously stressed and deformed during rolling. The method comprises the following steps: the high-temperature lubricant is firstly uniformly coated on the upper surface and the lower surface of a lining plate and an alloy sample, then the lining plate and the upper surface and the lower surface of the alloy sample are put into a heat treatment furnace together for heating, the furnace temperature is set to 920 ℃, the materials are synchronously sent into a roller for 4-pass rolling after the temperature is kept for 25min, the rolling amount of each pass is 15%, and the total rolling amount is 60%. And carrying out furnace return heat preservation between the passes, wherein parameters are the same as the above. After rolling, a high temperature titanium alloy sheet with 350mm×180mm×4mm without edge crack was obtained.
Step 6, agingAnd (3) treatment: the plate after rolling the double lining plates is heated to 750 ℃ and 10 DEG C -2 And (3) carrying out aging annealing treatment for 5 hours in a vacuum environment of Pa, and then cooling to room temperature by air to obtain the short-time high-temperature titanium alloy plate Ti-7Al-3.5Sn-11Zr-2Mo-3Nb-1W-0.6Si.
The short-time high-temperature titanium alloy plate prepared by the embodiment has the dimensions of 350mm multiplied by 180mm multiplied by 4mm, no edge crack, the room-temperature tensile strength of 1156MPa and the elongation of 12.9%; the tensile strength at 700℃was 589MPa and the elongation was 21.4%.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (8)
1. The high-strength and high-toughness short-time high-temperature titanium alloy plate is characterized by comprising, by mass, 7% -8% of Al, 3% -4% of Sn, 10% -12% of Zr, 2% -3% of Mo, 2% -3% of Nb, 1% -2% of W, 0.5% -0.7% of Si, the balance of Ti and trace unavoidable impurity elements.
2. A method for preparing the high-strength and high-toughness short-time high-temperature titanium alloy plate as claimed in claim 1, which is characterized by comprising the following steps:
melting, mixing and casting the raw materials of each alloy element according to the mass percentage ratio to obtain an alloy cast ingot;
sequentially carrying out solution quenching, forging cogging, double-lining-plate rolling and aging treatment on the alloy cast ingot to obtain the high-strength and high-toughness short-time high-temperature titanium alloy plate;
the solution hardening specifically comprises the following steps: placing the alloy ingot into a silicide to be subjected to solution treatment at a temperature above the silicide dissolution temperature, and then quenching the alloy ingot by using a NaCl aqueous solution;
the forging cogging specifically comprises: forging upsetting for one pass along the height direction of the alloy sample, wherein the deformation temperature is lower than that of the alloy sampleThe alpha+beta/beta phase transition temperature of the alloy ingot is kept at the temperature before forging, the technological deformation is 60-80%, and the strain rate is 0.05s -1 ～0.1s -1 Air cooling after forging;
the rolling of the double lining plates is specifically as follows: paving a hard alloy lining plate on the upper surface and the lower surface of a sample to be rolled respectively, carrying out 4-6 times of rolling after heat preservation under the temperature condition of being lower than the alpha+beta/beta phase transition temperature of the alloy ingot, and carrying out furnace return heat preservation between the passes of rolling;
the aging treatment specifically comprises the following steps: and (3) performing aging annealing treatment in a vacuum environment at 650-750 ℃ and then performing air cooling.
3. The method for producing a high strength and toughness short-term high temperature titanium alloy sheet according to claim 2, wherein the alloy ingot is a widmannstatten structure comprising an initial beta grain and a lamellar alpha bundle domain inside the beta grain.
4. The method for producing a high-strength and high-toughness short-time high-temperature titanium alloy sheet according to claim 2, wherein the solution hardening is specifically: and (3) placing the alloy ingot into solid solution for 2-4 hours at a temperature of 5-20 ℃ above the silicide dissolution temperature, and then quenching with 5-15 wt.% NaCl aqueous solution.
5. The method for preparing a high-strength and high-toughness short-time high-temperature titanium alloy plate according to claim 2, wherein the deformation temperature is 80-100 ℃ below the alpha+beta/beta transformation temperature of the alloy ingot during forging and cogging, and the temperature is kept for 20-30 min before forging.
6. The method for preparing the high-strength and high-toughness short-time high-temperature titanium alloy plate according to claim 2, wherein the double-lining plate rolling is specifically as follows: and respectively paving a hard alloy lining plate on the upper surface and the lower surface of a sample to be rolled, preserving heat for 20-40 min at the temperature of 20-50 ℃ below the alpha+beta/beta transformation temperature of the alloy ingot, synchronously feeding the alloy ingot into a roller for 4-6 times of rolling, wherein the rolling reduction of each time is 15%, the total rolling reduction is 60-90%, and carrying out furnace return heat preservation between the times of the rolling, wherein the temperature and the time of the furnace return heat preservation of each time are the same.
7. The method for preparing the high-strength and high-toughness short-time high-temperature titanium alloy plate according to claim 2, wherein the aging treatment is specifically: aging annealing treatment is carried out for 4 to 8 hours in a vacuum environment with the temperature of 650 to 750 ℃ and the vacuum degree of 10 -1 ～10 -2 Pa, followed by air cooling.
8. The use of the high strength and toughness short-term high temperature titanium alloy sheet material as claimed in claim 1 for the manufacture of aerospace vehicle bodies, compressor discs and military weapon parts.
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| ZA2023/03062A ZA202303062B (en) | 2022-08-25 | 2023-02-28 | The preparation method and application of a short-time high-temperature titanium alloy sheet with high-strength and high-toughness |
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| CA882041A (en) * | 1971-09-28 | Reactive Metals | Balanced titanium alloy | |
| US4229216A (en) * | 1979-02-22 | 1980-10-21 | Rockwell International Corporation | Titanium base alloy |
| CN105925844A (en) * | 2016-06-08 | 2016-09-07 | 太原理工大学 | Micro and nano double-scale particle reinforced titanium-based composite material and preparation method thereof |
| CN108165820A (en) * | 2016-12-08 | 2018-06-15 | 北京有色金属研究总院 | A kind of strong heat-resistant titanium alloy of superelevation and sheet alloy and preparation method in short-term |
| CN109811193A (en) * | 2019-03-13 | 2019-05-28 | 北京工业大学 | A kind of excellent boron micro-alloyed high-temperature titanium alloy and preparation method thereof of high-temperature behavior |
| CN111188001A (en) * | 2020-03-17 | 2020-05-22 | 山东理工大学 | Method for controlling silicide characteristics of high-temperature titanium-based composite material |
| CN114836651A (en) * | 2022-05-17 | 2022-08-02 | 太原理工大学 | Ultrahigh-strength and toughness beta titanium alloy and preparation method thereof |
| JP7180782B2 (en) * | 2019-07-30 | 2022-11-30 | 日本製鉄株式会社 | Titanium alloy plate and automobile exhaust system parts |
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2022
- 2022-08-25 CN CN202211029554.5A patent/CN115679153B/en active Active
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- 2023-02-28 ZA ZA2023/03062A patent/ZA202303062B/en unknown
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA882041A (en) * | 1971-09-28 | Reactive Metals | Balanced titanium alloy | |
| US4229216A (en) * | 1979-02-22 | 1980-10-21 | Rockwell International Corporation | Titanium base alloy |
| CN105925844A (en) * | 2016-06-08 | 2016-09-07 | 太原理工大学 | Micro and nano double-scale particle reinforced titanium-based composite material and preparation method thereof |
| CN108165820A (en) * | 2016-12-08 | 2018-06-15 | 北京有色金属研究总院 | A kind of strong heat-resistant titanium alloy of superelevation and sheet alloy and preparation method in short-term |
| CN109811193A (en) * | 2019-03-13 | 2019-05-28 | 北京工业大学 | A kind of excellent boron micro-alloyed high-temperature titanium alloy and preparation method thereof of high-temperature behavior |
| JP7180782B2 (en) * | 2019-07-30 | 2022-11-30 | 日本製鉄株式会社 | Titanium alloy plate and automobile exhaust system parts |
| CN111188001A (en) * | 2020-03-17 | 2020-05-22 | 山东理工大学 | Method for controlling silicide characteristics of high-temperature titanium-based composite material |
| CN114836651A (en) * | 2022-05-17 | 2022-08-02 | 太原理工大学 | Ultrahigh-strength and toughness beta titanium alloy and preparation method thereof |
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