CN111500959A - Hot processing and heat treatment process for preparing near α type high-temperature titanium alloy layered structure - Google Patents
Hot processing and heat treatment process for preparing near α type high-temperature titanium alloy layered structure Download PDFInfo
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Abstract
A hot working and heat treatment process for preparing a near α type high-temperature titanium alloy lamellar structure belongs to the technical field of titanium alloy preparation, and comprises the steps of firstly, preserving heat for 55-65 min below a β/(β 0+ β) phase transformation point of a high-temperature titanium alloy subjected to two-phase region forging within a range of 30-35 ℃, then air cooling to obtain an equiaxed structure, preserving heat for 55-65 min within a range of 15-20 ℃ below a β/(α + β) phase transformation point of the high-temperature titanium alloy, directly carrying out hot rolling, preserving heat for 10-15 min within a range of 85-90 ℃ below a β/(α + β) phase transformation point of the high-temperature titanium alloy, and directly carrying out hot rolling to obtain a titanium alloy with αp/αsAnd carrying out stabilization and aging heat treatment on the high-temperature titanium alloy plate with the micro-nano layered structure. The invention not only greatly improves the tensile property of the high-temperature titanium alloy, but also ensures the tensile strength (sigma) of the alloyb) And yield strength (σ)0.2) Are improved and the elongation () is slightly increased.
Description
Technical Field
The invention belongs to the technical field of titanium alloy preparation (the field of thermomechanical deformation of deformation and phase change control), and particularly relates to a high-temperature titanium alloy plate with a micro-nano layered structure and a hot processing and heat treatment process thereof.
Background
Along with the increasing requirements of high thrust-weight ratio aircraft engines on novel light high-temperature-resistant structural materials, urgent requirements are put forward on the research and development of novel high-temperature-resistant titanium alloys resistant to higher temperature and the development of advanced forming processes. The service temperature of the high-temperature titanium alloy is increased from 300 ℃ to 650 ℃, the service temperature and the performance of the high-temperature titanium alloy are improved by taking the improvement of the alloying degree as a main means, and the reduction of the structural stability under the service condition is caused. Therefore, further increasing the service temperature of high temperature titanium alloys is mainly limited by the structural stability under service conditions. Under the condition of designing high-temperature titanium alloy by using the principle of ensuring the thermal stability of the alloy, the microstructure regulation becomes the most effective means for improving the service performance of the high-temperature titanium alloy at higher temperature.
The characteristic of the overall α phase morphology and the relation between the characteristic and the property are that the typical structure of the titanium alloy is divided into widmannstatten structure, basket structure, equiaxed structure and two-state structure, wherein widmannstatten structure has higher creep resistance, endurance strength and fracture toughness but poor plasticity, basket structure plasticity, creep resistance and high temperature characteristic and other comprehensive properties but poor fatigue property, equiaxed structure has higher plasticity but lower creep resistance, two-state structure has higher fatigue strength and plasticity but not much improved creep resistance, for the typical 600 ℃ high temperature titanium alloy, the fatigue property of the alloy is optimized, IMI834 is designed and the two-state structure is proposed, and the high temperature creep property of the high temperature titanium alloy is mainly targeted to be enhanced, Ti1100 is designed and the alloy is proposed to adopt lamellar structure, however, the structure mode with room temperature, high temperature, toughness, thermal stability, high temperature creep property and fatigue property is still under study, the invention provides a novel structure of potential high temperature titanium alloy, namely αp/αsThe micro-nano laminated structure is characterized in that the thermal deformation processing and the phase change thermal treatment process are combined to prepare the nano-sized lamellar αsPhase structure and micron-sized lamellar αpPhase structure, and αsAnd αpAlternatingAre arranged in layers.
Disclosure of Invention
The invention aims to provide a hot working and heat treatment process for preparing a layered structure of a nearly α type high-temperature titanium alloy, which comprises the following components, by mass, 6.0-6.2% of Al, 3.0-3.3% of Sn, 2.3-2.5% of Zr, 0.5-0.6% of Hf, 0.5-0.6% of Mo, 0.8-1.0% of Nb, 0.9-1.0% of Ta, 0.4-0.5% of Si, 0.1-0.3% of Er, and the balance of Ti. α prepared by the methodp/αsThe high-temperature titanium alloy plate with the layered micro-nano structure breaks through the traditional microstructure mode of titanium alloy, and has excellent comprehensive mechanical properties, so that the service performance of the high-temperature titanium alloy is improved.
The invention provides a hot processing method for preparing a layered structure of a nearly α type high-temperature titanium alloy, which comprises the following steps:
step one
Obtaining a high-temperature titanium alloy ingot by adopting a conventional casting method, cogging and forging the ingot in a β single-phase region at 140-155 ℃ above the phase transformation point of β/(α + α 1), then forging the ingot in a (α + β) two-phase region at 25-35 ℃ below the phase transformation point of β/(α 0+ β) to obtain a bar, carrying out heat treatment on the bar, keeping the heat treatment temperature within the range of 30-35 ℃ below the phase transformation point of β/(α + β) of the high-temperature titanium alloy, keeping the temperature for 55-65 minutes, and cooling to room temperature in an air cooling mode after the heat preservation is finished to obtain an equiaxed structure.
The step is to perform static spheroidization on the high-temperature titanium alloy subjected to cogging forging in the two-phase region, so as to prevent the genetic influence of the structure and micro-orientation formed in the forging process on the subsequent structure regulation.
Step two
And (3) repeatedly performing heat treatment on the alloy material with the equiaxed structure obtained in the step one, wherein the heat treatment temperature is within 15-20 ℃ below the phase transition point of the high-temperature titanium alloy β/(α + β), the heat preservation time is 55-65 minutes, a double-state structure with the primary α phase content of 10-15% is obtained, and cooling treatment is not performed.
Step three
And (3) carrying out first hot rolling on the alloy material with the duplex structure obtained in the step two within the range of 15-20 ℃ below the phase transformation point of the high-temperature titanium alloy β/(α + β), wherein the hot rolling deformation is 50-60%.
The β phase deformation is mainly regulated and controlled in the step, so that α in fine strip arrangement at room temperature is obtainedsAnd (4) phase(s).
Step four
Keeping the alloy material subjected to the first-pass hot rolling in the third step at the temperature of 85-90 ℃ below the phase transformation point of the high-temperature titanium alloy β/(α + β) for 10-15 minutes to perform second-pass hot rolling, wherein the hot rolling deformation is 20-30%, and the α% of the alloy material is obtainedp/αsA plate with a micro-nano layered structure.
The step is based on the shape/phase change process, and mainly regulates and controls αpPhase deformation to obtain α elongated in rolling directionpAnd (4) phase(s).
The invention relates to a heat treatment process of a layered structure of a nearly α type high-temperature titanium alloy, which specifically comprises the following five steps:
step five
Subjecting the product of step four to reaction with αp/αsAnd (3) carrying out stabilization treatment and aging heat treatment on the plate with the micro-nano laminated structure, wherein the stabilization process is 800 ℃/1h/AC, and the aging process is 700 ℃/3 h/AC. The high-performance micro-nano layered structure high-temperature titanium alloy plate with the yield strength of more than 1000MPa and the elongation of more than 10% is obtained.
The invention has the following beneficial effects:
the invention prepares α with nanometer size by hot processing and heat treatment processsα arranged in long strips of micron sizepα elongated and elongated in the direction of thermal deformationsAnd αpHierarchically arranged tissue features, i.e. αp/αsThe micro-nano layered structure has excellent mechanical properties, the tensile strength of the micro-nano layered structure reaches 1100MP, the yield strength reaches 1030MP, and the elongation rate reaches 12%, so that the micro-nano layered structure is a novel high-temperature titanium alloy organization structure with excellent comprehensive mechanical properties.
Obtained by the invention has αp/αsThe high-temperature titanium alloy with the layered micro-nano structure has a high two-state structure compared with that obtained by solution aging treatmentThe warm titanium alloy greatly improves the comprehensive mechanical property of the alloy, and leads the tensile strength (sigma) of the alloyb) And yield strength (σ)0.2) All increased, with a slight increase in its elongation ().
Drawings
FIG. 1 α obtained by a shape/phase change processp/αsMicro-nano layered structure microstructure morphology.
FIG. 2 α obtained by the shape/phase change processp/αsMicro-nano layered structure transmission microstructure morphology
FIG. 3 α obtained by the shape/phase change processp/αsAnd (3) micro-nano laminar structure EBSD microstructure morphology.
FIG. 4: the microstructure morphology of the micro-nano layered structure after stabilization and aging treatment.
FIG. 5: stabilizing the stress-strain curve of the aged state; wherein: 1-1 is a rolling direction drawing sample, and 2-1 is a transverse direction drawing sample.
The invention is further described with reference to the following figures and detailed description.
Detailed Description
Example 1
The near α type high temperature titanium alloy of this example, which comprises, in mass%, 6.2% of Al, 3.0% of Sn, 2.5% of Zr, 0.5% of Hf, 0.5% of Mo, 1.0% of Nb, 1.0% of Ta, 0.4% of Si, 0.2% of Er, and the balance Ti, is obtained by a conventional casting method, and then a DSC (differential scanning calorimeter) test is used to obtain β/(α + β) of the alloy, a first step of cogging and forging a bar in a single phase region at 1150 ℃ β, and then a second step of heat treating the bar in a two phase region at 980 ℃ (α + β) in a heat treatment furnace, wherein the heat treatment process is 980 ℃/1h/AC to obtain an equiaxial structure, a second step of heat treating the material having an equiaxial structure obtained in the first step, a heat treatment process of 990 ℃/1h is performed without cooling, a third step of performing a second heat treatment of the material having a double heat-rolled structure at a temperature of α.64% and a second step of hot-rolled material obtained by performing a double heat treatment at 990Rolling deformation of 54% in the fourth step, the second hot rolling was carried out at 920 ℃ with a rolling deformation of 22% to obtain a steel sheet having α shown in FIG. 1p/αsAnd in fig. 2 and 3, a microstructure of the laminated micro-nano structure sheet is displayed by utilizing a transmission electron microscope photo and an EBSD (electron back scattering diffraction) grain boundary distribution diagram. And fifthly, stabilizing and aging the plate, wherein the stabilizing process is 800 ℃/1h/AC, the aging process is 700 ℃/3h/AC, and the tissue morphology after stabilizing and aging treatment is shown in figure 4, so that the plate has better tissue stability.
Example 2
The near α type high temperature titanium alloy of this example, which comprises, in mass%, 6.2% of Al, 3.0% of Sn, 2.5% of Zr, 0.5% of Hf, 0.5% of Mo, 1.0% of Nb, 1.0% of Ta, 0.4% of Si, 0.2% of Er, and the balance Ti, was obtained by a conventional casting method as a high temperature titanium alloy ingot, and then obtained by DSC (differential scanning calorimeter) testing that the transformation point of β/(α + β) was 1010 ℃p/αsA layered micro-nano structure plate.
Example 3
The near α type high temperature titanium alloy of this example, which comprises, in mass percent, 6.2% Al, 3.0% Sn, 2.5% Zr, 0.5% Hf, 0.5% Mo, 1.0% Nb, 1.0% Ta, 0.4% Si, 0.2% Er, and the balance Ti, was prepared by a conventional casting method to obtain a high temperature titanium alloy ingot, which was then tested by DSC (differential scanning calorimeter) to obtain the alloy β/(α + β) with a transformation point of 1010. the first step, which was forged in a single phase region of β at 1150 deg.C, followed by forging in a single phase region of β at 1150 deg.C980 ℃ (α + β) two-phase region forged bar is subjected to heat treatment in a heat treatment furnace, the heat treatment process is 980 ℃/1h/AC, and an equiaxial structure is obtained, in the second step, the material with the equiaxial structure obtained in the first step is subjected to second heat treatment, the heat treatment process is 990 ℃/1h, cooling treatment is not needed, in the third step, the alloy material obtained in the second step is subjected to first hot rolling, the hot rolling temperature is 990 ℃, the hot rolling deformation is 55%, in the fourth step, the second hot rolling is carried out, the hot rolling temperature is 920 ℃, the hot rolling deformation is 26%, and α% is obtainedp/αsA layered micro-nano structure plate.
The plates obtained in the 3 examples are stabilized and aged, the stabilizing process is 800 ℃/1h/AC, the aging process is 700 ℃/3h/AC, and the morphology of the structure after the stabilizing and aging treatment is shown in figure 4 (namely, the morphology of the structure after the stabilizing and aging treatment of the examples 2 and 3 is basically similar to that of the structure after the stabilizing and aging treatment of the example 1), so that the plates have better structure stability. The sheet material in the stabilized and aged state of example 1 was processed into tensile test specimens in accordance with GB/T228.1-2010, and the tensile mechanical properties of the alloys in different sampling directions were measured in a tensile tester, as shown in Table 1.
As can be seen from Table 1, the product obtained by the hot working and heat treatment process had a composition of αp/αsCompared with the same high-temperature titanium alloy with a two-state structure, the high-temperature titanium alloy with the layered micro-nano structure improves the tensile strength, obviously increases the yield strength, does not reduce the elongation of the alloy, and maintains a higher level, and the properties of the material have good uniformity by comparing the properties of a rolled sample and a transverse tensile sample, namely αp/αsThe novel tissue mode of the layered micro-nano structure has higher comprehensive mechanical property and better matching of strength and plasticity mainly because of the specific reduction of stress concentration and the change of the stress state of the crack tip.
TABLE 1 EXAMPLE 1 high temperature titanium alloys with different morphology in the stabilized + aged tensile Properties
Table of properties: 1-1 is the rolling direction performance, and 2-1 is the transverse direction performance.
Claims (5)
1. A hot working method for preparing a layered structure of a near α type high-temperature titanium alloy is characterized by comprising the following steps:
the high temperature titanium alloy of approximately α type consists of Al 6.0-6.2 wt%, Sn 3.0-3.3 wt%, Zr 2.3-2.5 wt%, Hf 0.5-0.6 wt%, Mo 0.5-0.6 wt%, Nb 0.8-1.0 wt%, Ta 0.9-1.0 wt%, Si 0.4-0.5 wt%, Er 0.1-0.3 wt%, and Ti for the rest;
obtaining β/(α + α 1) phase transition point temperature through testing, cogging and forging β single-phase region above α 2/(α 0+ β) phase transition point and 140-155 ℃, then forging (α + β) two-phase region below β/(α + β) phase transition point and 25-35 ℃ to form a bar, keeping the temperature of the bar within 30-35 ℃ below β phase transition temperature for 55-65 minutes, and then cooling the bar to room temperature by air;
carrying out secondary repeated heat treatment on the high-temperature titanium alloy bar subjected to the primary heat treatment, wherein the heat treatment temperature is within 15-20 ℃ below the β/(α + β) phase transition point of the high-temperature titanium alloy, the heat preservation time is 55-65 min, and cooling treatment is not carried out;
and (3) carrying out first hot rolling on the high-temperature titanium alloy bar subjected to the second heat treatment within the range of 15-20 ℃ below the β/(α + β) phase transformation point of the high-temperature titanium alloy, wherein the hot rolling deformation is 50-60%, and preparing the high-temperature titanium alloy plate.
And (3) keeping the temperature of the high-temperature titanium alloy plate subjected to the first-pass hot rolling for 10-15 minutes within the range of 85-90 ℃ below the phase transformation point of β/(α + β) of the high-temperature titanium alloy, and performing second-pass hot rolling, wherein the hot rolling deformation is 20-30%.
2. The hot working method according to claim 1, wherein the high temperature titanium alloy bar obtained by the first heat treatment has an equiaxed structure, and the high temperature titanium alloy bar obtained by the second heat treatment hasThe high-temperature titanium alloy plate prepared by the second-pass hot rolling has a primary α degree of duplex structure with 10-15 percent of primary α phase contentpPhase with secondary αsα of compositionp/αsA micro-nano layered structure.
3. The layered structure material of the near α type high-temperature titanium alloy prepared by the hot working method according to claim 1 or 2.
4. The heat treatment process of the high temperature titanium alloy layered structure material near α type prepared by the hot working method according to claim 1 or 2, wherein the obtained material has α typep/αsAnd (3) carrying out stabilization treatment and aging heat treatment on the plate with the micro-nano laminated structure, wherein the stabilization process is 800 ℃/1h/AC, and the aging process is 700 ℃/3 h/AC.
5. The layered structure material of the near α type high temperature titanium alloy obtained by the heat treatment process according to claim 4.
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Cited By (5)
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| CN112251645A (en) * | 2020-09-29 | 2021-01-22 | 中国科学院金属研究所 | High-thermal-stability equiaxial nanocrystalline Ti-Co alloy and preparation method thereof |
| CN112251637A (en) * | 2020-09-29 | 2021-01-22 | 中国科学院金属研究所 | High-thermal-stability equiaxial nanocrystalline Ti-Fe alloy and preparation method thereof |
| CN112760581A (en) * | 2020-12-19 | 2021-05-07 | 北京工业大学 | Forging-rolling composite processing and heat treatment process of near-alpha type high-temperature titanium alloy |
| CN114045453A (en) * | 2021-12-23 | 2022-02-15 | 西安稀有金属材料研究院有限公司 | Method for preparing titanium, zirconium, hafnium and alloy materials thereof in bionic brick-laying layered structure |
| CN114672694A (en) * | 2022-03-30 | 2022-06-28 | 北京工业大学 | Low-temperature rolling and heat treatment process of near-alpha type high-temperature titanium alloy |
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| CN112760581B (en) * | 2020-12-19 | 2022-03-22 | 北京工业大学 | Forging-rolling composite processing and heat treatment process of near-alpha type high-temperature titanium alloy |
| CN114045453A (en) * | 2021-12-23 | 2022-02-15 | 西安稀有金属材料研究院有限公司 | Method for preparing titanium, zirconium, hafnium and alloy materials thereof in bionic brick-laying layered structure |
| CN114672694A (en) * | 2022-03-30 | 2022-06-28 | 北京工业大学 | Low-temperature rolling and heat treatment process of near-alpha type high-temperature titanium alloy |
| CN114672694B (en) * | 2022-03-30 | 2022-08-16 | 北京工业大学 | Preparation method of near-alpha type high-temperature titanium alloy |
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