CN107904440B - High-temperature titanium alloy material and preparation method thereof - Google Patents

High-temperature titanium alloy material and preparation method thereof Download PDF

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CN107904440B
CN107904440B CN201711180652.8A CN201711180652A CN107904440B CN 107904440 B CN107904440 B CN 107904440B CN 201711180652 A CN201711180652 A CN 201711180652A CN 107904440 B CN107904440 B CN 107904440B
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CN107904440A (en
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陈子勇
靳艳芳
柴丽华
金头男
相志磊
唐增辉
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Beijing University of Technology
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/03Making non-ferrous alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • C22F1/183High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon

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Abstract

A high-temperature titanium alloy material and a preparation method thereof, belonging to the technical field of titanium alloy. The alloy consists of Al: 6.5% -7%, Sn: 3% -5%, Zr: 6% -9%, Mo + W + Nb: 1.2-4%, Si: 0.2-0.4%, Re: 0.1-0.3% and the balance Ti. And remelting for 3 times by using a water-cooled copper crucible vacuum induction melting furnace, and then performing multidirectional forging on the alloy at 980 ℃. The high-temperature titanium alloy prepared by the invention has excellent room temperature and high temperature performance, shows excellent service performance and has wide application prospect.

Description

High-temperature titanium alloy material and preparation method thereof
Technical Field
The invention relates to a novel high-temperature titanium alloy material with excellent comprehensive performance and a preparation method thereof, belonging to the technical field of titanium alloys.
Background
The titanium alloy has excellent performances of high melting point, high hardness, small density, high specific strength, corrosion resistance and the like, is widely used for manufacturing parts such as discs, blades, casings and the like of an aero-engine air compressor, replaces steel or other high-temperature alloys, lightens the quality of an engine, improves the thrust-weight ratio of the engine, is developed under the traction of advanced aero-engine requirements, the use temperature is gradually improved, the temperature is improved from 400 ℃ represented by Ti-6Al-4V alloy in the 20 th 50 s to 600 ℃ represented by IMI834 alloy, the titanium alloy used at 600 ℃ is typically 600 ℃ represented by IMI834 alloy, the IMI834 alloy of British empire metal company, the Ti-1100 alloy of American Timet company and the Ti60 of China, the Ti600 alloy system is Ti-Al-Sn-Zr-Mo-Si system, in recent years, the rapid development of the aero industry is carried out, the novel advanced aero-engine provides new requirements for the research on the high-temperature titanium alloy, and the titanium alloy is developed in the world at the temperature of 600 ℃ and above for a long time, and the alloy is rapidly developed and strengthened on the basis of Al- α ℃ of Ti-Sn-2The strengthening with silicide precipitated phase basically reaches the limit, and the most basic requirement on thermal stability is difficult to ensure if the alloying degree is further improved; thus the materialThe effective strengthening and the obdurability matching are the technical problems of developing the high-temperature titanium alloy with the temperature of more than 600 ℃.
Disclosure of Invention
The invention provides a design and forging method of a high-temperature titanium alloy, aiming at the problems that the high-temperature titanium alloy material prepared by the existing method is effectively strengthened and the obdurability cannot be well matched.
In order to achieve the above object, the present invention adopts the following technical solutions.
The high-temperature titanium alloy with excellent comprehensive performance is prepared from the following components in percentage by mass: 6.5% -7%, Sn: 3% -5%, Zr: 6% -9%, Mo + W + Nb: 1.2-4%, Si: 0.2-0.4%, Re: 0.1-0.3% and the balance Ti.
The preparation process of the high-temperature titanium alloy comprises the following steps:
(1) the alloy consists of the following components in percentage by mass: 6.5% -7%, Sn: 3% -5%, Zr: 6% -9%, Mo + W + Nb: 1.2-4%, Si: 0.2-0.4%, Re: 0.1-0.3% of Ti, and the balance of Ti, respectively weighing the raw materials of high-purity aluminum, TiSn, sponge zirconium, Al-Mo, Al-W, Al-Nb, high-purity silicon, sponge titanium and Ti-Re; respectively putting high-purity aluminum, TiSn, sponge zirconium, Al-Mo, Al-W, Al-Nb, high-purity silicon and sponge titanium into corresponding crucibles, then putting the crucibles into a resistance furnace, heating the crucibles to 120 ℃, and removing moisture from the blank;
(2) uniformly mixing the moisture-removed blank and Ti-Re, gradually and uniformly putting the mixture into a die, and pressing the die into a cylindrical blank on a hydraulic press;
(3) putting the cylindrical blank into a clean vacuum induction smelting furnace, and vacuumizing the furnace; then, under the protection of argon, drying the material for 2-5 min under the power of 40-60 KW, and then smelting under the power of 160-180 KW to enable the melt suspension time to be 45-90 s; in order to make the components uniform, the ingot is smelted for 3 times, and the ingot is placed into a preheated mold for casting after the last time to obtain an alloy ingot;
(4) cutting off a riser of the alloy ingot obtained in the step (3), and performing isothermal multidirectional forging, wherein the specific steps are that the ingot is preheated for 1-3 min before ① forging, and then oxygen prevention is sprayedCoating, smearing graphite for lubrication and binding high-temperature cotton, ② placing the ingot obtained in step ① into a resistance furnace heated to 950-1000 ℃ for heat preservation for 30-50 min, ③ transferring the ingot heat-preserved in step ② to forging equipment for first-step forging with the deformation rate of 0.01S-1④, returning the forging stock obtained in the step ③ to a furnace at ② 950-1000 ℃, preserving heat for 10-15 min, then performing forging method like the step ③, and then cooling in air to room temperature.
Preferably:
in the step (3), the relatively low vacuum is firstly extracted, and then the high vacuum is extracted to 10-2-10-1Filling argon for smelting after Pa;
in the step (3), the material is firstly dried for 3min under the protection of argon and under the power of 50 KW.
Preheating the spindle at 980 ℃ for 1min before forging in the step (4) ①, spraying an anti-oxidation coating, smearing graphite on the upper end and the lower end of the cast ingot, and binding high-temperature cotton.
In ② of step (4), the resistance furnace is raised to 980 ℃, and the ingot is kept at the temperature for 40min.
In ③ of the step (4), the upsetting deformation is 40%, and the elongation deformation is 30%.
And (4) returning the forged blank in ④ in the step (4) to the furnace, and keeping the temperature for 10 min.
Mo + W + Nb: 1.2-4% means that the total amount of the three elements is 1.2-4%, and each element is not 0.
The invention prepares a novel high-temperature titanium alloy material with excellent comprehensive performance, solves the problem that the obdurability of the high-temperature titanium alloy at the temperature of more than 600 ℃ cannot be well matched, and has the room-temperature tensile strength of 1118.37MPa, the yield strength of 1026.18MPa and the elongation of 11.88 percent; the tensile strength of 650 ℃ is up to 704.75MPa, the yield strength is up to 592.7MPa, and the elongation is up to 15.06%.
Drawings
FIG. 1 is a stress-strain curve after forging at 980 ℃ after tensile stress-strain curves at room temperature and elevated temperature (650 ℃)
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
The preparation of the novel high-temperature titanium alloy material with excellent comprehensive performance is carried out according to the following steps:
firstly, Al is composed of the following components in percentage by mass: 6.5%, Sn: 2.5%, Zr: 9%, Mo: 0.5%, W: 1%, Nb: 1%, Si: 0.25%, Re: 0.1%, Ti: 79.15%, and weighing the raw materials respectively. Respectively putting weighed high-purity aluminum, TiSn, sponge zirconium, Al-Mo, Al-W, Al-Nb, high-purity silicon and sponge titanium (except Ti-Re) into corresponding crucibles, then putting the crucibles into a resistance furnace, heating to 120 ℃, and removing moisture from the blank.
And secondly, uniformly mixing the moisture-removed blank with the Ti-Re, gradually and uniformly putting the mixture into a corresponding mould, and pressing the mixture into a cylindrical blank on a hydraulic press.
And thirdly, putting the blank into a cleaned vacuum induction melting furnace, vacuumizing the vacuum induction melting furnace, drying the blank for 3min under the protection of argon after the vacuum degree is reached, then melting the blank under the power of 170KW to ensure that the melt is suspended for 60s so as to ensure that the components are uniform, melting the ingot for 3 times, and finally putting the ingot into a preheated die for casting to obtain the alloy ingot with the diameter of 60 × 150 mm.
Fourthly, cutting off a riser of the alloy ingot obtained in the third step, and then carrying out isothermal multidirectional forging, specifically comprising the steps of preheating the ingot for 1min before ① forging, spraying an anti-oxidation coating, then coating graphite for lubrication and binding high-temperature cotton, ② placing the ingot obtained in ① into a resistance furnace heated to 980 ℃ for heat preservation for 40min, ③ transferring the ingot subjected to ② heat preservation to forging equipment for carrying out first-step forging, wherein the deformation rate is 0.01S-1The ingot was subjected to upsetting once and drawing once, with the upset deformation of 40% and the drawing deformation of 30%. ④ the resulting forged billet of ③ was then returned to the furnace, held for 10min, subjected to a forging method such as ③, and then air-cooled to room temperature.
Mechanical property tests are carried out on the high-temperature titanium alloy obtained in example 1, the mechanical property data are shown in table one, and the stress-strain curve is shown in figure 1, so that the comprehensive performance of the high-temperature titanium alloy is excellent.
Tensile properties measured in example 1 are shown in table one:
TABLE 1980 ℃ mechanical Properties after forging at Room temperature and high temperature (650 ℃) stretching
Figure BDA0001479116500000031

Claims (8)

1. The high-temperature titanium alloy material is characterized by comprising the following components in percentage by mass: 6.5% -7%, Sn: 3% -5%, Zr: 6% -9%, Mo + W + Nb: 1.2-4%, Si: 0.2-0.4%, Re: 0.1-0.3% and the balance Ti; the preparation method comprises the following steps:
(1) the alloy consists of the following components in percentage by mass: 6.5% -7%, Sn: 3% -5%, Zr: 6% -9%, Mo + W + Nb: 1.2-4%, Si: 0.2-0.4%, Re: 0.1-0.3% of Ti, and the balance of Ti, respectively weighing the raw materials of high-purity aluminum, TiSn, sponge zirconium, Al-Mo, Al-W, Al-Nb, high-purity silicon, sponge titanium and Ti-Re; respectively putting high-purity aluminum, TiSn, sponge zirconium, Al-Mo, Al-W, Al-Nb, high-purity silicon and sponge titanium into corresponding crucibles, then putting the crucibles into a resistance furnace, heating the crucibles to 120 ℃, and removing moisture from the blank;
(2) uniformly mixing the moisture-removed blank and Ti-Re, gradually and uniformly putting the mixture into a die, and pressing the die into a cylindrical blank on a hydraulic press;
(3) the method comprises the steps of putting a cylindrical blank into a clean vacuum induction melting furnace, vacuumizing the vacuum induction melting furnace, drying the cylindrical blank for 2-5 min under the protection of argon under the power of 40-60 KW, then melting under the power of 160-180 KW to enable the melt to suspend for 45-90 s, melting 3 times, and casting in a preheated mold after the last time to obtain an alloy ingot with the diameter of 60 mm and 60 × 150 mm;
(4) cutting off a riser of the alloy ingot obtained in the step (3), and performing isothermal multidirectional forging, wherein the specific steps are that the ingot is preheated for 1-3 min before ① forging, and then an anti-oxidation coating is sprayedCoating graphite for lubrication and binding high-temperature cotton, ② placing the ingot obtained in step ① into a resistance furnace heated to 950-1000 ℃ for heat preservation for 30-50 min, ③ transferring the ingot heat-preserved in step ② to forging equipment for first-step forging with the deformation rate of 0.01S-1④, returning the forging stock obtained in the step ③ to a furnace at ② 950-1000 ℃, preserving heat for 10-15 min, then performing forging method like the step ③, and then cooling in air to room temperature.
2. A method for preparing a high temperature titanium alloy material according to claim 1, comprising the steps of:
(1) the alloy consists of the following components in percentage by mass: 6.5% -7%, Sn: 3% -5%, Zr: 6% -9%, Mo + W + Nb: 1.2-4%, Si: 0.2-0.4%, Re: 0.1-0.3% of Ti, and the balance of Ti, respectively weighing the raw materials of high-purity aluminum, TiSn, sponge zirconium, Al-Mo, Al-W, Al-Nb, high-purity silicon, sponge titanium and Ti-Re; respectively putting high-purity aluminum, TiSn, sponge zirconium, Al-Mo, Al-W, Al-Nb, high-purity silicon and sponge titanium into corresponding crucibles, then putting the crucibles into a resistance furnace, heating the crucibles to 120 ℃, and removing moisture from the blank;
(2) uniformly mixing the moisture-removed blank and Ti-Re, gradually and uniformly putting the mixture into a die, and pressing the die into a cylindrical blank on a hydraulic press;
(3) the method comprises the steps of putting a cylindrical blank into a clean vacuum induction melting furnace, vacuumizing the vacuum induction melting furnace, drying the cylindrical blank for 2-5 min under the protection of argon under the power of 40-60 KW, then melting under the power of 160-180 KW to enable the melt to suspend for 45-90 s, melting 3 times, and casting in a preheated mold after the last time to obtain an alloy ingot with the diameter of 60 mm and 60 × 150 mm;
(4) cutting off a riser of the alloy ingot obtained in the step (3), and then carrying out isothermal multidirectional forging, specifically comprising the steps of preheating the ingot for 1-3 min before ① forging, spraying an anti-oxidation coating, then coating graphite for lubrication and binding high-temperature cotton, ②, and carrying out ① on the ingot obtained in the stepThe ingot is put into a resistance furnace which is heated to 950 ℃ to 1000 ℃ for heat preservation for 30 min to 50min, ③ the ingot which is well preserved in the step ② is transferred to forging equipment for the first step of forging, the deformation rate is 0.01S-1④, returning the forging stock obtained in the step ③ to a furnace at ② 950-1000 ℃, preserving heat for 10-15 min, then performing forging method like the step ③, and then cooling in air to room temperature.
3. The method of claim 2, wherein step (3) is performed by drawing a relatively low vacuum and then drawing a high vacuum to 10 degrees f-2-10-1And introducing argon for smelting after Pa.
4. The method according to claim 2, wherein in step (3) the material is baked for 3min at 50KW under argon.
5. The method of claim 2, wherein the ingot is preheated at 980 ℃ for 1min before forging in step (4) ①, and then sprayed with the anti-oxidation coating, and the upper and lower ends of the ingot are coated with graphite and then bound with high temperature cotton.
6. The method of claim 2, wherein the resistance furnace is raised to 980 ℃ in ② of step (4) and the ingot is held at that temperature for 40min.
7. The method of claim 2 wherein the upset deformation of step (4) at ③ is 40% and the draw deformation is 30%.
8. The method of claim 2, wherein the billet is annealed at ④ in step (4) and held for 10 min.
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CN108774702A (en) * 2018-06-22 2018-11-09 广西趣创想创客空间管理有限责任公司 A kind of high temperature oxidation resisting titanium alloy and preparation method thereof
CN109536777B (en) * 2019-01-04 2020-01-07 青海聚能钛业股份有限公司 High-temperature titanium alloy and preparation method thereof
CN110484774B (en) * 2019-09-24 2020-12-01 西北有色金属研究院 650 ℃ high-temperature resistant titanium alloy
CN111020289A (en) * 2019-12-18 2020-04-17 佛山科学技术学院 Heat-resistant titanium alloy
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
CN111906610B (en) * 2020-08-14 2021-10-29 丽水学院 Titanium alloy plate preparation process and processing equipment thereof
CN113878037B (en) * 2021-10-11 2023-11-03 飞亚达精密科技股份有限公司 Titanium alloy and manufacturing method of titanium alloy watch appearance piece

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CN104018027B (en) * 2014-05-09 2016-10-05 中国科学院金属研究所 A kind of heat-resistant titanium alloy and machining manufacture thereof and application
CN106555076A (en) * 2017-01-09 2017-04-05 北京工业大学 A kind of resistance to 650 DEG C of high-temperature titanium alloy materials and preparation method thereof

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