CN114855028A - Obtaining micro-nano dual-scale Ti 2 Preparation method of AlNb alloy - Google Patents
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 115
- 239000000956 alloy Substances 0.000 title claims abstract description 115
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000005242 forging Methods 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 10
- 238000004590 computer program Methods 0.000 claims abstract description 8
- 230000007246 mechanism Effects 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims description 23
- 238000001816 cooling Methods 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 17
- 230000035882 stress Effects 0.000 claims description 13
- 239000006104 solid solution Substances 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 11
- 238000000137 annealing Methods 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 9
- 238000005482 strain hardening Methods 0.000 claims description 7
- 238000010275 isothermal forging Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 4
- 238000010304 firing Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000001953 recrystallisation Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 238000003723 Smelting Methods 0.000 abstract description 4
- 238000005266 casting Methods 0.000 abstract description 4
- 238000007670 refining Methods 0.000 abstract description 2
- 230000003631 expected effect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
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Abstract
The invention discloses a method for obtaining micro-nano dual-scale Ti 2 The preparation method of the AlNb alloy comprises the following steps of S1: cogging and forging stage: s11: and connecting a power supply of the forging mechanism with an external power supply, setting various cogging forging values through a computer program, and controlling and starting the forging mechanism through the computer program after the setting is finished. The obtained micro-nano dual-scale Ti 2 Method for preparing AlNb alloy and improved Ti 2 The preparation method of the AlNb alloy adopts a plastic deformation method to introduce larger deformation amount in the deformation process, thereby being capable of treating Ti 2 Refining the coarse grains of the AlNb-based alloy blank to obtain a rod-shaped sample with a certain specification, and then adopting a proper heat treatment process to further accurately regulate and control the microstructure of the alloy so as to prepare the micro-nano dual-scale alloyTi 2 The AlNb alloy solves the problems of coarse grains in the smelting and casting process and the control problem of the grain size, so that the alloy has higher strength and plasticity, and the prepared double-scale Ti with more excellent performance 2 An AlNb alloy.
Description
Technical Field
The invention relates to Ti 2 The technical field of AlNb alloy preparation, in particular to a method for obtaining micro-nano dual-scale Ti 2 A preparation method of AlNb alloy.
Background
Intermetallic compound Ti based on ordered orthorhombic O-phase 2 The AlNb-based alloy is one of the first-selected novel light high-temperature structural materials of the aircraft engine due to the excellent comprehensive performance. With the rapid development of the aerospace industry, the Ti alloy 2 The service performance of the AlNb-based alloy puts higher demands. Ti 2 The AlNb-based alloy is a multi-phase structure, the phase transformation process is very complicated, and Ti is optimized by effective improvement 2 The preparation process of the AlNb-based alloy realizes the precise control of the microstructure (phase composition, dimension, morphology and distribution thereof) of the AlNb-based alloy, and is always regarded as an effective way for improving the toughness of the alloy by most scientific researchers.
The micro-nano double-scale alloy is characterized in that the microstructure of the alloy comprises double-size crystal grains of nano crystals with the size of less than 100nm and micro crystals with the size of more than 1 mu m. The nanocrystalline is utilized to ensure the high strength of the alloy, and the microcrystalline keeps higher plasticity, so that the strength and toughness of the alloy can be better considered at the same time by the micro-nano double-scale crystal grains, and the service performance of the alloy is improved.
Traditionally, smelting and casting are mostly adopted to prepare Ti 2 However, the AlNb-based alloy contains Ti, which is a highly active element, and Al, which is a volatile element, and therefore macro-micro segregation of different components occurs during melting and solidification, and the obtained as-cast structure has coarse grains and poor mechanical properties. The most common preparation method at present is Ti prepared by adopting a laser additive manufacturing process 2 The method of the AlNb-based alloy solves the defects of the traditional process, can obtain a fine structure, but cannot accurately control the phase composition, the grain size and the like of the alloy in the preparation process.
Disclosure of Invention
The invention aims to provide a method for obtaining micro-nano dual-scale Ti 2 The preparation method of the AlNb alloy aims to solve the problems of coarse grains and grain size control in the smelting and casting process in the background technology, so that the alloy has higher strength and plasticity, and the prepared double-scale Ti with more excellent performance 2 Problems with AlNb alloys.
In order to achieve the purpose, the invention provides the following technical scheme: obtaining micro-nano dual-scale Ti 2 The preparation method of the AlNb alloy comprises the following steps,
s1: a raw material selection stage:
s11: determination of Ti 2 The nominal component of the AlNb-based alloy is Ti-22Al-24Nb, and the chemical components by mass percent are as follows: 10.6% of Al, 41.2% of Nb, 0.88% of Mo, 0.047% of Fe, 0.07% of Si, Cu:<0.01％，Ni:<0.01, and the balance being Ti;
s12: according to determined Ti 2 The components of the AlNb-based alloy are proportioned, and Ti meeting the standard is selected 2 AlNb-based alloy is reserved;
s2: cogging and forging stage:
s21: connecting a power supply of the forging mechanism with an external power supply, setting various cogging forging values through a computer program, and controlling and starting the forging mechanism through the computer program after the setting is finished;
s22: will be as-cast Ti 2 AlNb base alloy is respectively in beta single phase region and (alpha 2 +)B2) Cogging and forging the two-phase region, wherein the forging is completed by 3-5 heating times, and each heating time is about 25% of the total deformation until the Ti is in an as-cast state 2 The deformation of the AlNb-based alloy reaches 40-60 percent;
s23: and the blank is sheathed, so that the temperature loss of the blank in the forging and transferring processes is reduced.
S3: and (3) stress relief annealing treatment stage:
s31: after cogging and forging are finished, stress relief annealing is respectively carried out in a beta single-phase region and an (alpha 2+ B2) two-phase region, and the heat preservation time of the beta single-phase region and the (alpha 2+ B2) two-phase region is 30 min;
s32: cooling the beta single-phase region and the (alpha 2+ B2) two-phase region in air to room temperature to finally obtain Ti with the phi 110mm coarse crystal further refined 2 An AlNb alloy bar;
s4: a sample selecting stage:
s41: isothermal forging of Ti using a wire cutter 2 Cutting the AlNb alloy bar to obtain Ti with the dimension specification of 8mm in diameter and 12mm in height 2 An AlNb alloy sample;
s5: a solution treatment stage:
s51: mixing Ti 2 Heating an AlNb alloy sample in a (O + B2) phase region to a high temperature, keeping the temperature constant, fully dissolving an excess phase into a solid solution, and then rapidly cooling to obtain a supersaturated solid solution;
s52: after solution treatment, the average size of O-phase crystal grains in the alloy is about 2.7 mu m;
s6: and (3) aging treatment stage:
s61: subjecting the solution treated Ti 2 Aging the AlNb alloy sample in the (O + B2) phase region to enhance the strength and hardness of the sample;
s62: after aging treatment, the O phase size of the long lath in the alloy is about 200nm, and the O phase size of the fine lath is about 40 nm.
Preferably, the cogging forging in S2 is to cast Ti 2 The production process of forging and pressing AlNb-based alloy into blank with certain specification and performance.
Preferably, the cogging of S22The heat preservation time is 0.1-0.2mm/min, and the strain rate is 0.01S -1 。
Preferably, the stress relief annealing in S3 is Ti after cold deformation 2 Heat treatment of the AlNb-based alloy to remove internal stresses but still retain the cold work hardening effect by heating below the recrystallization temperature.
Preferably, Ti in S32 2 The alpha 2 phase of the AlNb alloy bar material accounts for about 6 percent of the total volume fraction, the B2 phase accounts for about 73 percent of the total volume fraction, the O phase accounts for 21 percent of the total volume fraction, and the Ti obtained at the moment is calculated 2 The average size of the AlNb alloy crystal grains is about 92 mu m.
Preferably, the solution treatment in the S51 is performed at 950 ℃, the solution heat preservation time is 2 hours, and the cooling mode is water cooling.
Preferably, the aging treatment in S61 is Ti 2 After AlNb alloy sample is treated by solution treatment, quenched at high temperature or deformed by cold working to a certain extent, the sample is placed at higher temperature or room temperature to keep the shape and size of the sample, so that Ti is formed 2 The properties of the AlNb alloy specimens change over time.
Preferably, the temperature selected in the aging treatment in S61 is 720 ℃, the aging time is 10h, and the cooling mode is selected to be air cooling.
Compared with the prior art, the invention provides the method for obtaining the micro-nano dual-scale Ti 2 The preparation method of the AlNb alloy has the following advantages:
the invention is through the reaction of Ti 2 The AlNb alloy is subjected to isothermal forging to generate severe deformation, so that crystal grains are effectively refined, solid solution and aging are carried out by adjusting proper process parameters, the strengthening effect of the O phase is higher than that of the alpha 2 phase, the alloy with the lath O phase distributed on the B2 matrix has the best comprehensive performance, the solid solution and aging are carried out in the (O + B2) phase region, and finally the micro-nano dual-scale Ti is obtained 2 AlNb alloy, modified Ti 2 The preparation method of the AlNb alloy adopts a plastic deformation method to introduce larger deformation amount in the deformation process, thereby being capable of carrying out Ti 2 Refining coarse grains of the AlNb-based alloy blank to obtain a rod-shaped sample with a certain specificationThen adopting a proper heat treatment process to further accurately regulate and control the microstructure of the alloy so as to prepare and obtain the micro-nano dual-scale Ti 2 The AlNb alloy solves the problems of coarse grains in the smelting and casting process and the control problem of the grain size, so that the alloy has higher strength and plasticity, and the prepared double-scale Ti with more excellent performance 2 An AlNb alloy.
Drawings
FIG. 1 shows that Ti is obtained after S2 isothermal forging stress-relief annealing of the invention 2 OM diagram of AlNb alloy;
FIG. 2 shows Ti after S4 solution treatment according to the present invention 2 SEM image of AlNb alloy;
FIG. 3 shows micro-nano dual-scale Ti obtained after the aging treatment of S5 2 TEM image of AlNb alloy.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-3, the present invention provides a technical solution: obtaining micro-nano dual-scale Ti 2 The preparation method of the AlNb alloy comprises the following steps,
s1: a raw material selection stage:
s11: determination of Ti 2 The nominal component of the AlNb-based alloy is Ti-22Al-24Nb, and the chemical components by mass percent are as follows: 10.6% of Al, 41.2% of Nb, 0.88% of Mo, 0.047% of Fe, 0.07% of Si, Cu:<0.01％，Ni:<0.01, and the balance being Ti;
s12: according to determined Ti 2 The components of the AlNb-based alloy are proportioned, and Ti meeting the standard is selected 2 AlNb-based alloy is reserved;
s2: cogging and forging stage:
s21: connecting a power supply of the forging mechanism with an external power supply, setting various cogging forging values through a computer program, and controlling and starting the forging mechanism through the computer program after the setting is finished;
s22: will be as-cast Ti 2 The AlNb-based alloy is subjected to cogging forging in a beta single-phase region and an (alpha 2+ B2) two-phase region respectively, the forging is completed by 3-5 firing times, each firing time is about 25% of the total deformation amount until as-cast Ti 2 The deformation of the AlNb-based alloy reaches 40-60 percent;
s23: and the blank is sheathed, so that the temperature loss of the blank in the forging and transferring processes is reduced.
S3: and (3) stress relief annealing treatment stage:
s31: after cogging and forging are finished, stress relief annealing is respectively carried out in a beta single-phase region and an (alpha 2+ B2) two-phase region, and the heat preservation time of the beta single-phase region and the (alpha 2+ B2) two-phase region is 30 min;
s32: cooling the beta single-phase region and the (alpha 2+ B2) two-phase region in air to room temperature to finally obtain Ti with the phi 110mm coarse crystal further refined 2 An AlNb alloy bar;
s4: a sample selecting stage:
s41: isothermal forging of Ti using a wire cutter 2 Cutting the AlNb alloy bar to obtain Ti with the dimension specification of 8mm in diameter and 12mm in height 2 An AlNb alloy sample;
s5: a solution treatment stage:
s51: mixing Ti 2 Heating an AlNb alloy sample in a (O + B2) phase region to a high temperature, keeping the temperature constant, fully dissolving an excess phase into a solid solution, and then rapidly cooling to obtain a supersaturated solid solution;
s52: after solution treatment, the average size of O-phase crystal grains in the alloy is about 2.7 mu m;
s6: and (3) aging treatment stage:
s61: subjecting the solution treated Ti 2 Aging the AlNb alloy sample in the (O + B2) phase region to enhance the strength and hardness of the sample;
s62: after aging treatment, the O phase size of the long lath in the alloy is about 200nm, the O phase size of the fine lath is about 40nm, and the Ti phase size is about 2 The state of the AlNb alloy is shown in fig. 3.
The cogging forging in S2 is to cast Ti 2 The production process of forging and pressing AlNb-based alloy into a blank with certain specification and performance;
the heat preservation time of the cogging forging in the S22 is 0.1-0.2mm/min, and the strain rate is 0.01S -1， The alloy treatment can be facilitated to achieve the expected effect by strictly controlling the working conditions of cogging and forging;
the stress relief annealing in S3 means Ti after cold deformation 2 Heat treatment of AlNb-based alloys to remove internal stresses but retain the cold work hardening effect by heating below recrystallization temperature without altering Ti 2 The structural state of the AlNb-based alloy is kept, and the alloy is heated at a lower temperature under the conditions of cold working, hot working or surface hardening so as to remove internal stress and reduce the possibility of deformation and cracking tendency of the alloy;
ti in S32 2 The alpha 2 phase of the AlNb alloy bar material accounts for about 6 percent of the total volume fraction, the B2 phase accounts for about 73 percent of the total volume fraction, the O phase accounts for 21 percent of the total volume fraction, and the Ti obtained at the moment is calculated 2 The average size of the AlNb alloy grains is about 92 mu m;
the temperature selected in the solid solution treatment in the S51 is 950 ℃, the solid solution heat preservation time is 2h, the cooling mode is water cooling, and the alloy treatment can achieve the expected effect by strictly controlling the temperature, time and cooling mode of the solid solution treatment;
the aging treatment in S61 means Ti 2 After AlNb alloy sample is treated by solution treatment, quenched at high temperature or deformed by cold working to a certain extent, the sample is placed at higher temperature or room temperature to keep the shape and size of the sample, so that Ti is formed 2 The performance of the AlNb alloy sample changes 0 along with time, and the strength and hardness of the alloy can be effectively improved and the performance of the alloy can be strengthened through aging treatment;
the temperature selected in the aging treatment in the S61 is 720 ℃, the aging time is 10h, the cooling mode is selected to be air cooling, and the alloy treatment can achieve the expected effect by strictly controlling the temperature, the time and the cooling mode of the aging treatment.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. Obtaining micro-nano dual-scale Ti 2 The preparation method of the AlNb alloy comprises the following steps, and is characterized in that:
s1: a raw material selection stage:
s11: determination of Ti 2 The nominal component of the AlNb-based alloy is Ti-22Al-24Nb, and the chemical components by mass percent are as follows: 10.6% of Al, 41.2% of Nb, 0.88% of Mo, 0.047% of Fe, 0.07% of Si, Cu:<0.01％，Ni:<0.01, and the balance being Ti;
s12: according to determined Ti 2 The components of the AlNb-based alloy are proportioned, and Ti meeting the standard is selected 2 AlNb-based alloy is reserved;
s2: cogging and forging stage:
s21: connecting a power supply of the forging mechanism with an external power supply, setting various cogging forging values through a computer program, and controlling and starting the forging mechanism through the computer program after the setting is finished;
s22: will be as-cast Ti 2 The AlNb-based alloy is subjected to cogging forging in a beta single-phase region and an (alpha 2+ B2) two-phase region respectively, the forging is completed by 3-5 firing times, each firing time is about 25% of the total deformation amount until as-cast Ti 2 The deformation of the AlNb-based alloy reaches 40-60 percent;
s23: and the blank is sheathed, so that the temperature loss of the blank in the forging and transferring processes is reduced.
S3: and (3) stress relief annealing treatment stage:
s31: after cogging and forging are finished, stress relief annealing is respectively carried out in a beta single-phase region and an (alpha 2+ B2) two-phase region, and the heat preservation time of the beta single-phase region and the (alpha 2+ B2) two-phase region is 30 min;
s32: air-cooling the beta single-phase region and the (alpha 2+ B2) two-phase region to room temperature to finally obtain Ti with the coarse crystal of phi 110mm and further refined 2 An AlNb alloy bar;
s4: a sample selecting stage:
s41: isothermal forging of Ti using a wire cutter 2 Cutting the AlNb alloy bar to obtain Ti with the dimension specification of 8mm in diameter and 12mm in height 2 An AlNb alloy sample;
s5: a solution treatment stage:
s51: mixing Ti 2 Heating an AlNb alloy sample in a (O + B2) phase region to a high temperature, keeping the temperature constant, fully dissolving an excess phase into a solid solution, and then rapidly cooling to obtain a supersaturated solid solution;
s52: after solution treatment, the average size of O-phase crystal grains in the alloy is about 2.7 mu m;
s6: and (3) aging treatment stage:
s61: subjecting the solution treated Ti 2 Aging the AlNb alloy sample in the (O + B2) phase region to enhance the strength and hardness of the sample;
s62: after aging treatment, the O phase size of the long lath in the alloy is about 200nm, and the O phase size of the fine lath is about 40 nm.
2. The method for obtaining micro-nano dual-scale Ti according to claim 1 2 The preparation method of the AlNb alloy is characterized by comprising the following steps: the cogging forging in S2 is to cast Ti 2 The production process of forging and pressing AlNb-based alloy into blank with certain specification and performance.
3. Obtaining micro-nano dual-scale Ti according to claim 1 2 The preparation method of the AlNb alloy is characterized by comprising the following steps: the heat preservation time of the cogging forging in the S22 is 0.1-0.2mm/min, and the strain rate is 0.01S -1 。
4. Obtaining micro-nano dual-scale Ti according to claim 1 2 The preparation method of the AlNb alloy is characterized by comprising the following steps: the stress relief annealing in S3 refers to Ti after cold deformation 2 Heat treatment of the AlNb-based alloy to remove internal stresses but still retain the cold work hardening effect by heating below the recrystallization temperature.
5. Obtaining micro-nano dual-scale Ti according to claim 1 2 The preparation method of the AlNb alloy is characterized by comprising the following steps: ti in said S32 2 The alpha 2 phase of the AlNb alloy bar material accounts for about 6 percent of the total volume fraction, the B2 phase accounts for about 73 percent of the total volume fraction, the O phase accounts for 21 percent of the total volume fraction, and the Ti obtained at the moment is calculated 2 The average size of the AlNb alloy crystal grains is about 92 mu m.
6. Obtaining micro-nano dual-scale Ti according to claim 1 2 The preparation method of the AlNb alloy is characterized by comprising the following steps: the temperature selected in the S51 is 950 ℃, the solid solution heat preservation time is 2h, and the cooling mode is water cooling.
7. Obtaining micro-nano dual-scale Ti according to claim 1 2 The preparation method of the AlNb alloy is characterized by comprising the following steps: the aging treatment in S61 is Ti 2 After AlNb alloy sample is treated by solution treatment, quenched at high temperature or deformed by cold working to a certain extent, the sample is placed at higher temperature or room temperature to keep the shape and size of the sample, so that Ti is formed 2 The properties of the AlNb alloy specimens change over time.
8. Obtaining micro-nano dual-scale Ti according to claim 1 2 The preparation method of the AlNb alloy is characterized by comprising the following steps: the temperature selected in the aging treatment in the S61 is 720 ℃, the aging time is 10h, and the cooling mode is selected to be air cooling.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116987991A (en) * | 2023-09-26 | 2023-11-03 | 成都先进金属材料产业技术研究院股份有限公司 | Regulating Ti 2 Method for preparing AlNb-based alloy with yield ratio |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116987991A (en) * | 2023-09-26 | 2023-11-03 | 成都先进金属材料产业技术研究院股份有限公司 | Regulating Ti 2 Method for preparing AlNb-based alloy with yield ratio |
| CN116987991B (en) * | 2023-09-26 | 2024-01-23 | 成都先进金属材料产业技术研究院股份有限公司 | Regulating Ti 2 Method for preparing AlNb-based alloy with yield ratio |
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