Preparation method of high-temperature titanium alloy plate
By employing β-single-phase region rolling, β+α two-phase region high-strain rate rolling, and low-temperature air cooling processes, combined with Zr and Sn elements, high-temperature titanium alloy plates with fine lamellar structures were prepared. This solved the problem of brittle compound precipitation during the rolling process of high-temperature titanium alloys and improved both high-temperature strength and room-temperature plasticity.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-02-27
- Publication Date
- 2026-04-03
AI Technical Summary
Brittle Ti3Sn compounds are easily formed during the rolling process of existing high-temperature titanium alloys, which leads to deterioration of room temperature plasticity and makes it difficult to maintain a balance between high strength and plasticity at high temperatures.
By employing a process of β single-phase region billet rolling, β+α two-phase region high strain rate rolling and low temperature air cooling, combined with the effects of Zr and Sn elements, a fine lamellar structure is formed, which inhibits the precipitation of Ti3Sn compounds.
It significantly improves the room temperature plasticity and high temperature strength of high-temperature titanium alloys, solving the dilemma of the contradiction between strength and plasticity in traditional methods, and is suitable for applications at higher temperatures and for complex parts.
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Figure CN121780935A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of high-temperature titanium alloy rolling technology, and more particularly to a method for preparing high-temperature titanium alloy plates. Background Technology
[0002] High-temperature titanium alloys are lightweight, high-temperature structural materials used in the aerospace field, finding wide application in hot-section components of high-end equipment such as aero-engines and hypersonic vehicles. Generally, high-temperature titanium alloys are near-alpha alloys, with aluminum (Al), tin (Sn), zirconium (Zr), and silicon (Si) being key strengthening elements. Sn, as an effective alpha phase stabilizer and solid solution strengthener, significantly improves the room-temperature and high-temperature strength of the alloy, while also enhancing its room-temperature plasticity. However, current processing techniques lead to the formation of brittle Ti3Sn compounds during rolling, deteriorating room-temperature plasticity. Therefore, the addition of Sn should be limited, generally not exceeding 4 wt%.
[0003] High-temperature titanium alloys face a dilemma regarding high-temperature strength and room-temperature plasticity: as service temperatures increase, the requirements for high-temperature strength of high-temperature titanium alloys become increasingly stringent. However, traditional methods for improving the high-temperature strength of titanium alloys inevitably lead to a decrease in room-temperature plasticity, which is extremely detrimental to the formability of high-temperature titanium alloys and hinders their application in higher-temperature and more complex components.
[0004] However, to improve the high-temperature strength of titanium alloys, precipitated phase strengthening is necessary. Unlike Ti3Al and Ti3Sn phases, silicide phases do not suppress the α phase.<a+c> Slip facilitates dislocation activation without reducing room temperature plasticity. Furthermore, recent studies have shown that Sn can substitute for Si in silicides, forming Sn-containing complex silicides, which also helps reduce the formation of brittle Ti3Sn compounds.
[0005] Therefore, developing a rolling scheme for high-temperature titanium alloy plates that can suppress the precipitation of Ti3Sn compounds and significantly improve strength and high plasticity will become a key technical issue that needs to be addressed in this field. Summary of the Invention
[0006] To address the aforementioned problems, the present invention aims to provide a method for preparing high-temperature titanium alloy plates. By performing β single-phase region billet rolling, β+α two-phase region high strain rate rolling, and low-temperature air cooling, a special fine-grained structure is obtained, thereby effectively improving the room temperature plasticity and high-temperature strength of the Ti-8Zr-6Al-0.3Si-9Sn-1Nb-1W-1Ta alloy.
[0007] The technical solution adopted in this invention is as follows:
[0008] The present invention provides a method for preparing a high-temperature titanium alloy plate, the method comprising the following steps: Step 1: Place high-purity raw materials Ti, Zr, Al, Sn, Si, Ti-Nb, Ti-W and Ti-Ta alloys into a vacuum non-consumable arc melting furnace, evacuate the furnace and then fill it with inert gas, using metallic Ti or Zr as the gas-absorbing material, and melt the above raw materials into alloy ingots. Step 2: The alloy ingot is then homogenized and annealed in a vacuum heat treatment furnace, held at the temperature for a period of time, and then cooled in the furnace. Step 3: Heat the cooled alloy ingot to the β single-phase region in a muffle furnace, hold it at that temperature for a period of time, and then hot roll it using a hydraulic two-roll mill. Finally, use water cooling to cool it quickly and suppress the precipitation of brittle phases. Step 4: The alloy material after billet preparation is heated to the β+α two-phase region in a muffle furnace, and then subjected to rapid rolling with high rolling speed and small deformation to promote grain and silicide refinement. Step 5: The total rolling deformation is 75-85%, and low-temperature rapid cooling is used after rolling to promote the formation of fine lamellar layers.
[0009] Furthermore, in step 1, the vacuum degree of the vacuum non-consumable arc melting furnace is 6~8×10⁻⁶. -4 Pa.
[0010] Furthermore, in step 2, the homogenization annealing temperature is 1150-1250℃, and the holding time is 110-130min.
[0011] Furthermore, in step 3, the hot rolling process involves two passes, the feed rate of the hydraulic two-roll mill is 30-40 mm / s, the deformation per pass is 20-25%, and the hot rolling is followed by furnace holding for 8-12 minutes.
[0012] Furthermore, in step 3, after the alloy ingot is heated to the β single-phase region, it is held at that temperature for 35-45 minutes.
[0013] Furthermore, in step 4, the roll speed is adjusted to 100-120 mm / s, and the deformation per pass is adjusted to 4-8%. After each hot rolling pass, the rolls are returned to the furnace for heat preservation for 3-5 minutes.
[0014] Furthermore, in step 5, the rapid cooling temperature is 8-12℃.
[0015] Compared with the prior art, the present invention has the following beneficial effects: 1. This invention utilizes a rolling process that combines high deformation speed and small deformation in the two-phase region, which can significantly refine the grain size and form a fine lamellar structure under the action of low temperature and rapid cooling, which is beneficial to improving plasticity and strength.
[0016] 2. This invention utilizes the properties of Zr to promote silicide precipitation and Sn to replace Si in silicides. Under the combined action of 9wt% Zr, a composite silicide containing Sn is formed, which can effectively suppress the formation of brittle Ti3Sn phase and further improve the high-temperature strength and room-temperature plasticity of high-temperature titanium alloys. Attached Figure Description
[0017] Figure 1 This is a schematic diagram of the microstructure of the fine grains and lamellar structure of the high-temperature titanium alloy sheet prepared in Example 1 of the present invention; Figure 2 This is a schematic diagram of the microstructure of the fine grains and lamellar structure of the high-temperature titanium alloy sheet prepared in Example 2 of the present invention; Figure 3 This is a schematic diagram of the microstructure of the fine grains and lamellar structure of the high-temperature titanium alloy sheet prepared for comparison. Detailed Implementation
[0018] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0019] It should be noted that in the description of this invention, the terms "upper", "lower", "top", "bottom", "one side", "the other side", "left", "right", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this invention and simplifying the description, and do not mean that the device or element must have a specific orientation, or be constructed and operated in a specific orientation.
[0020] The present invention provides a method for preparing a high-temperature titanium alloy plate, comprising the following steps: The chemical composition of the high-temperature titanium alloy, by weight percentage, consists of the following components: Zr 8%, Al 6%, Sn 9%, Nb 1%, W 1%, Ta 1%, Si 0.3%, with the balance being Ti.
[0021] Step 1: Place high-purity raw materials Ti (99.99wt%), Zr (99.95wt%), Al (99.99wt%), Sn (99.99wt%), Si (99.99wt%), Ti-Nb, Ti-W, and Ti-Ta alloys into a vacuum non-consumable arc melting furnace according to the corresponding measurements, and evacuate to 6~8×10⁻⁶. -4Pa, then inert gas is introduced, and titanium or zirconium is used as the gas absorber material to melt it into an alloy ingot.
[0022] Step 2: Then, use a vacuum heat treatment furnace to perform homogenization annealing on the alloy ingot at 1150-1250℃, hold for 110-130 minutes, and then cool with the furnace.
[0023] Step 3: After annealing and cooling, the alloy ingot is heated to the β single-phase region in a muffle furnace and held for 35-45 minutes. Then, it is hot rolled into a billet using a hydraulic two-roll mill with a roll feed rate of 30-40 mm / s and a deformation of 20-25% per pass. After each hot rolling pass, it is returned to the furnace for holding for 8-12 minutes. The billet rolling passes are 2. After billet rolling, it is rapidly cooled by water to suppress the precipitation of brittle phases.
[0024] Step 4: Heat the alloy material after billet preparation to the β+α two-phase region in a muffle furnace, adjust the roll speed to 100-120 mm / s, and adjust the deformation per pass to 4-8% to carry out rapid rolling with high rolling speed and small deformation to promote grain and silicide refinement; after each hot rolling pass, return to the furnace for 3-5 minutes for heat treatment.
[0025] Step 5: The total rolling deformation is 75-85%, and rapid cooling at a low temperature of 8-12℃ is used after rolling to promote the formation of fine lamellar layers.
[0026] The purpose of rolling the β single-phase region is to accumulate a large amount of strain, promote the refinement of the β phase, and provide a fine-grained structure for subsequent two-phase deformation. Water cooling is to suppress the precipitation of silicides when the cooling rate is slow. High rolling speed rolling in the α+β two-phase region is to further refine the structure while reducing rolling time and suppressing silicide precipitation. Low-temperature rapid cooling at 8-12℃ is to form a fine lamellar structure and prevent furnace cooling or slow cooling from causing the lamellars to become coarse.
[0027] The present invention will be further illustrated below through specific embodiments and comparative examples: Example 1 Using a non-consumable vacuum arc furnace method, each metal component was weighed to a total of 100g. The mixture was then melted using an electric arc in a high-purity argon atmosphere, with titanium as the getter material, and the vacuum was evacuated to 6×10⁻⁶. -4 Pa, melted 8 times and magnetic stirring was used to ensure that its composition was uniform; The ingots were homogenized and annealed at 1200℃ for 120 minutes in a vacuum heat treatment furnace, and then cooled in the furnace. The billet is heated to the β single-phase region in a muffle furnace and held for 40 minutes. It is then hot-rolled using a hydraulic two-roll mill with a feed rate of 30 mm / s and a deformation of 25% per pass. After each hot rolling pass, the billet is returned to the furnace for 10 minutes of holding. The billet is rolled twice and then rapidly cooled by water to suppress the precipitation of brittle phases.
[0028] The rolls are heated to the β+α two-phase region in a muffle furnace, the roll speed is adjusted to 100 mm / s, and the deformation per pass is adjusted to 8% to perform rapid rolling with high rolling speed and small deformation, which promotes grain and silicide refinement; after each hot rolling pass, the rolls are returned to the furnace for 5 minutes to hold. The total rolling deformation is 80%, and rapid cooling at a low temperature of 10℃ is used after rolling to promote the formation of fine lamellar layers.
[0029] The titanium alloy material prepared in this embodiment exhibits fine grain and lamellar structure as follows: Figure 1 As shown.
[0030] Example 2 Using a non-consumable vacuum arc furnace method, each metal component was weighed to a total of 100g. The mixture was then melted using an electric arc in a high-purity argon atmosphere, with titanium as the getter material, and the vacuum was evacuated to 6×10⁻⁶. -4 Pa, melted 8 times and magnetic stirring was used to ensure that its composition was uniform; The ingots were homogenized and annealed at 1200℃ for 120 minutes in a vacuum heat treatment furnace, and then cooled in the furnace. The billet is heated to the β single-phase region in a muffle furnace and held for 40 minutes. It is then hot-rolled using a hydraulic two-roll mill with a feed rate of 40 mm / s and a deformation of 20% per pass. After each hot rolling pass, the billet is returned to the furnace for 10 minutes of holding. The billet is rolled twice and then rapidly cooled by water to suppress the precipitation of brittle phases. The rolls are heated to the β+α two-phase region in a muffle furnace, with the roll speed adjusted to 120 mm / s and the pass deformation adjusted to 4%. This high-speed, low-deformation rapid rolling process promotes grain and silicide refinement. Each hot-rolled pass is then held in the furnace for 5 minutes.
[0031] The total rolling deformation is 80%, and rapid cooling at a low temperature of 10℃ is used after rolling to promote the formation of fine lamellar layers.
[0032] The titanium alloy material prepared in this embodiment exhibits fine grain and lamellar structure as follows: Figure 2 As shown.
[0033] Comparative Example Using a non-consumable vacuum arc furnace method, each metal component was weighed to a total of 100g. The mixture was then melted using an electric arc in a high-purity argon atmosphere, with titanium as the getter material, and the vacuum was evacuated to 6×10⁻⁶. -4Pa, melted 8 times and magnetic stirring was used to ensure that its composition was uniform; The ingots were homogenized and annealed at 1200℃ for 120 minutes in a vacuum heat treatment furnace, and then cooled in the furnace.
[0034] The billet is heated to the β single-phase region in a muffle furnace and held for 40 minutes. It is then hot-rolled using a hydraulic two-roll mill with a feed rate of 40 mm / s and a deformation of 10% per pass. After each hot rolling pass, the billet is returned to the furnace for 10 minutes. The billet is rolled in 4 passes and then rapidly cooled by water to suppress the precipitation of brittle phases. The rolls are heated to the β+α two-phase region in a muffle furnace, with the roll speed adjusted to 40 mm / s and the pass deformation adjusted to 10%. This high-speed, low-deformation rapid rolling process promotes grain and silicide refinement. After each hot rolling pass, the rolls are returned to the furnace for 5 minutes of heat treatment.
[0035] The total rolling deformation is 80%, and air cooling is used after rolling.
[0036] The titanium alloy material prepared in this comparative example exhibits fine grain and lamellar structure, such as... Figure 3 As shown.
[0037] The properties of the titanium alloy materials prepared in Examples 1, 2, and the comparative examples are shown in the table below:
[0038] Compared with the comparative example, the titanium alloy material prepared by the present invention has an excellent high-temperature strength of more than 730 MPa at 650℃ due to its fine lamellar structure, and still has a tensile strength of more than 600 MPa at 700℃.
[0039] Matters not covered in this invention are common knowledge.
[0040] The embodiments described above are merely preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Various modifications and improvements made by those skilled in the art to the technical solutions of the present invention without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims
1. A method for preparing a high-temperature titanium alloy sheet, characterized in that, The method includes the following steps: Step 1: Place high-purity raw materials Ti, Zr, Al, Sn, Si, Ti-Nb, Ti-W and Ti-Ta alloys into a vacuum non-consumable arc melting furnace, evacuate the furnace and then fill it with inert gas, using metallic Ti or Zr as the gas-absorbing material, and melt the above raw materials into alloy ingots. Step 2: The alloy ingot is then homogenized and annealed in a vacuum heat treatment furnace, held at the temperature for a period of time, and then cooled in the furnace. Step 3: Heat the cooled alloy ingot to the β single-phase region in a muffle furnace, hold it at that temperature for a period of time, and then hot roll it using a hydraulic two-roll mill. Finally, use water cooling to cool it quickly and suppress the precipitation of brittle phases. Step 4: The alloy material after billet preparation is heated to the β+α two-phase region in a muffle furnace, and then subjected to rapid rolling with high rolling speed and small deformation to promote grain and silicide refinement. Step 5: The total rolling deformation is 75-85%, and low-temperature rapid cooling is used after rolling to promote the formation of fine lamellar layers.
2. The method for preparing a high-temperature titanium alloy plate according to claim 1, characterized in that: In step 1, the vacuum degree of the vacuum non-consumable arc melting furnace is 6~8×10⁻⁶. -4 Pa.
3. The method for preparing a high-temperature titanium alloy plate according to claim 1, characterized in that: In step 2, the homogenization annealing temperature is 1150-1250℃, and the holding time is 110-130min.
4. The method for preparing a high-temperature titanium alloy plate according to claim 1, characterized in that: In step 3, the hot rolling process involves two passes, the feed rate of the hydraulic two-roll mill is 30-40 mm / s, the deformation per pass is 20-25%, and the hot rolling is followed by furnace holding for 8-12 minutes.
5. The method for preparing a high-temperature titanium alloy plate according to claim 1, characterized in that: In step 3, after the alloy ingot is heated to the β single-phase region, it is held at that temperature for 35-45 minutes.
6. The method for preparing a high-temperature titanium alloy plate according to claim 1, characterized in that: In step 4, the roll speed is adjusted to 100-120 mm / s, and the deformation per pass is adjusted to 4-8%. After each hot rolling pass, the rolls are returned to the furnace for heat preservation for 3-5 minutes.
7. The method for preparing a high-temperature titanium alloy plate according to claim 1, characterized in that: In step 5, the rapid cooling temperature is 8-12℃.