CN114657415B - 750 ℃ high-temperature titanium alloy bar and forging method thereof - Google Patents

750 ℃ high-temperature titanium alloy bar and forging method thereof Download PDF

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CN114657415B
CN114657415B CN202210318504.2A CN202210318504A CN114657415B CN 114657415 B CN114657415 B CN 114657415B CN 202210318504 A CN202210318504 A CN 202210318504A CN 114657415 B CN114657415 B CN 114657415B
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forging
temperature
heating
titanium alloy
upsetting
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CN114657415A (en
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安震
张海鸿
齐铭
丁旭
张阔
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Xian Aeronautical University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21JFORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J5/00Methods for forging, hammering, or pressing; Special equipment or accessories therefor
    • B21J5/002Hybrid process, e.g. forging following casting
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/06Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires
    • 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
    • C22F1/002Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
    • 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

The invention discloses a large-size bar of 750 ℃ high-temperature titanium alloy and a forging method thereof, wherein the bar comprises the components of Al, sn, zr, ni, cr, mo, nb, W, si, fe, ta and Y, and the balance of Ti; the forging method comprises preheating treatment, cogging forging, forging at the temperature of 20-50 ℃ below the phase transformation point, forging at the temperature of 150-350 ℃ above the phase transformation point, forging at the temperature of 20-50 ℃ below the phase transformation point, forging at the temperature of 120-300 ℃ above the phase transformation point, forging below the phase transformation point and heat treatment after forging. Compared with the internationally advanced Ti600 and Ti60 alloys, the 750 ℃ high-temperature titanium alloy large-size bar has international advancement; can be used for preparing titanium alloy bars with uniform tissues and high performance and can meet the AMS-STD-2154A-level requirement for flaw detection; the method can be used for manufacturing parts such as compressor disk blades and casings of aero-engines, and the urgent need of the aero-manufacturing industry is met.

Description

750 ℃ high-temperature titanium alloy bar and forging method thereof
Technical Field
The invention belongs to the technical field of nonferrous metal processing, relates to an alpha-type titanium alloy, a titanium alloy bar and a forging method thereof, and particularly relates to a large-size 750-DEG C high-temperature titanium alloy bar for a heat-resistant part of an aircraft engine and a forging method thereof.
Background
In recent years, the country has started projects such as large airplanes, and according to the design principle that novel large airplane parts are structured and integrated and have weight-reducing benefits, high-temperature titanium alloy can partially replace heat-resistant steel and high-temperature alloy, reduce part of weight, and serve as an important material in the field of aircrafts. In particular, the high-temperature titanium alloy belongs to a key material of an aeroengine, and is suitable for parts such as a compressor disk blade, a casing and the like of the aeroengine.
At present, the high-temperature titanium alloy applied to the aviation field mainly comprises Ti60 and Ti600 alloys, the heat-resistant temperature of the high-temperature titanium alloy reaches about 550 ℃, and under the condition that the dual requirements on the heat-resistant temperature and the weight reduction effect of an aviation structural component are continuously increased, the requirement on the heat-resistant temperature of the high-temperature titanium alloy is also continuously increased.
The alpha-type titanium alloy is sensitive to parameters of a hot working process, the structure and the performance after thermal deformation are difficult to control, and in addition, the titanium alloy has high processing temperature and large ingot blank cogging forging difficulty, so that large-scale forging equipment and a reasonable forging process are required to be adopted, and various defects in the forging process are avoided. Most of the existing forging processes of the alpha-type titanium alloy firstly adopt forging for a plurality of times above a phase transformation point and then forging for a plurality of times below the phase transformation point, and the forging processes easily cause the defects of uneven tissues, incomplete recrystallization phenomenon, production of processing streamline and the like of each part of a titanium alloy product.
In view of the above, a high temperature titanium alloy with higher use temperature than the conventional aviation titanium alloy is needed, and a forging method for solving the defects of the conventional titanium alloy is provided.
Disclosure of Invention
The embodiment of the invention aims to provide a 750 ℃ high-temperature titanium alloy bar and a forging method thereof, the obtained titanium alloy has good comprehensive mechanical property at 750 ℃ and can be used for a long time at 750 ℃, the bar with the diameter phi of 200-400 mm is produced by the forging method, the structure is uniform, the mechanical property is high, the stability is strong, the flaw detection meets the AMS-STD-2154A-grade requirement, and the forging method is suitable for industrial production.
The technical scheme adopted by the invention is that a 750 ℃ grade high-temperature titanium alloy bar comprises the following components in percentage by mass: 5.0 to 6.0 percent of Al, 3.0 to 6.0 percent of Sn, 2.0 to 3.0 percent of Zr, 0.5 to 1.5 percent of Ni, 1.5 to 2.5 percent of Cr, 0.5 to 2.0 percent of Mo, 0.8 to 1.5 percent of Nb, 1.0 to 3.0 percent of W, 0.3 to 0.8 percent of Si, 0.5 to 1.5 percent of Fe, 0.3 to 1.5 percent of Ta, 0.5 to 1.5 percent of Y and the balance of Ti.
Another object of the present invention is to provide a method for forging the 750 ℃ high temperature titanium alloy bar, comprising the following steps:
step 1, preheating treatment;
step 2, cogging and forging;
step 3, forging at 20-50 ℃ below the phase transformation point;
step 4, forging at 150-350 ℃ above the phase transformation point;
step 5, forging at the temperature of 20-50 ℃ below the phase transformation point;
step 6, forging at 120-300 ℃ above the phase transformation point;
step 7, forging below the phase transformation point;
step 8, adopting a heat treatment mode after forging to perform T treatment on the forged blank obtained in the step 7 β -50 ℃ and T β Carrying out graded heat treatment at the temperature of minus 300 ℃, and carrying out furnace cooling in the middle to obtain a high-temperature titanium alloy bar at the temperature of 750 ℃;
wherein, in the step 1, the preheating treatment specifically comprises the following steps: transferring a large industrial titanium alloy ingot containing components of a 750 ℃ grade high-temperature titanium alloy bar and mass percent of the large industrial titanium alloy ingot to a heating furnace, setting the heating temperature in the furnace to be 350-500 ℃ above a beta transformation point, and preserving heat for 20-40 h to obtain a titanium alloy ingot subjected to preheating treatment;
in the step 2, the cogging forging specifically comprises the following steps: cogging and forging the titanium alloy ingot subjected to preheating treatment, wherein the cogging heating temperature is 200-300 ℃ above the phase transition point, the heating and heat preservation time is 300-450 min, and 1 firing is carried out; then, upsetting and drawing the titanium alloy ingot for 3 to 6 times, gradually reducing the forging temperature of 85 to 120 ℃ each time, controlling the forging ratio of 1.5 to 2.0 each time, uniformly pressing by hammers, and performing air cooling or water quenching after forging; upsetting forging, namely two upsetting and two drawing, one upsetting and two drawing or two drawing and one upsetting are adopted.
Further, in the step 3, the forging at the temperature of 20-50 ℃ below the transformation point is specifically as follows: performing 1-time upsetting-drawing forging on the forging stock obtained in the step 2, wherein the material heating temperature is 20-50 ℃ below the phase change point, and the heating and heat preservation time is 300-450 min; the forging ratio is controlled to be 1.3-1.8, the forging is carried out under the condition of uniform speed pressing by hammers, and air cooling or water quenching is adopted after the forging.
Further, in the step 4, the forging at 150-350 ℃ above the transformation point specifically comprises: and (3) carrying out upsetting-drawing forging on the forging stock obtained in the step (3) for 1 to 2 times, wherein the material heating temperature is 150 to 350 ℃ above the phase transition point, the heating and heat preservation time is 300 to 450min, the forging temperature is decreased by 60 to 80 ℃ each time, the forging ratio is controlled to be 1.5 to 2.0, the forging is carried out under constant-speed pressing by a hammer, and air cooling or water quenching is adopted after forging.
Further, in the step 5, the forging at the temperature of 20-50 ℃ below the transformation point is specifically as follows: carrying out 3-time upsetting-drawing forging on the forging stock obtained in the step 4, and heating the material to T β -20 ℃ reversing upsetting and drawing, T β -25 ℃ diagonal elongation plus upsetting and T β Two upsetting and two drawing at minus 30 ℃, wherein the heating and heat preservation time of each heating time is 250-450 min; air cooling or water quenching is adopted after forging.
Further, in step 6, the forging at 120-300 ℃ above the transformation point specifically comprises: upsetting and drawing the forging stock obtained in the step 5 for 1 to 2 times, wherein the material heating temperature is 120 to 300 ℃ above the phase transformation point, and the heating and heat preservation time is 300 to 450min; the forging temperature is decreased by 30-50 ℃ every time, the forging ratio is controlled between 1.5-2.0, the forging is carried out at a constant speed by hammer, and air cooling or water quenching is adopted after forging to obtain the equiaxial beta crystal grain intermediate blank.
Further, in step 7, the forging with the transformation point as follows is specifically: carrying out 2-time upsetting-drawing forging on the forging stock obtained in the step 6, and heating the material to the temperature T below the phase change point β -30 ℃ reversing upsetting and T β Upsetting is added to the diagonal elongation at minus 35 ℃, and the heating and heat preservation time of each heating is 250-450 min; air cooling or water quenching is adopted after forging; then carrying out T β Chamfering at-40 ℃ and drawing out, T β The steel wire is rolled and drawn at minus 45 ℃, the forging ratio is controlled to be 1.2 to 1.9, and the heating and heat preservation time of each heating time is 250 to 450min; air cooling or water quenching is adopted after forging.
Furthermore, in the step 8, the time of each stage of heat treatment is 20-40 h.
Further, in the steps 1-7, before each heating, the method also comprises the step of brushing an anti-oxidation coating on the surface of the forging stock.
Further, TLC1350-1, TB1200-15, TB1200-16 or TB1260-18 is adopted for the oxidation resistant coating.
The invention has the beneficial effects that:
(1) Firstly, the titanium alloy is subjected to pre-forging component homogenization heat treatment, so that heavy metal elements in the titanium alloy are more uniformly distributed, and the component segregation is prevented. Secondly, two-pass 'high-low-high' process reduces the difference of the finish forging temperature of the edge part and the core part of the material, so that the structure and the components are more uniform, firstly, forging and crushing cast crystal grains above a phase change point, secondly, forging for 1 fire time below the phase change point, enabling the primary alpha phase of the titanium alloy to be equiaxial, thirdly, forging for 1-2 fire times above the phase change point, repeating the 'high-low-high process' for two times, re-crystallizing beta crystal grains, refining the crystal grains in a multi-recrystallization mode, finally obtaining fine and uniform beta crystal grains, and finally, forging for a plurality of fire times below the phase change point to obtain the finished bar. And finally, graded heat treatment is adopted, and a gradual cooling mode is adopted in the middle, so that the structure of the alloy is more uniform and meets the product requirements.
(2) The nominal composition of the heat-resistant (750 ℃ grade) titanium alloy is as follows:
ti-6Al-5Sn-3Zr-2Cr-1Ni-1Mo-1Nb-2W-0.5Si-1Fe-1Ta-1Y, which belongs to alpha type titanium alloy. Compared with the international advanced Ti600 and Ti60 alloy, the alloy has slightly excellent performance level and international advancement. Can be used for preparing titanium alloy bars with uniform tissues and high performance and can meet the AMS-STD-2154A-level requirements for flaw detection. The rod material specification phi is 200 mm-400 mm, and can be used for manufacturing parts such as a compressor disk blade, a casing and the like of an aeroengine, thereby solving the urgent requirement of the aeronautical manufacturing industry.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a macroscopic view of a 750 ℃ grade high-temperature titanium alloy bar material annealed in example 1 of the present invention.
Fig. 2a is a microstructure of the edge of a bar according to an embodiment of the invention.
FIG. 2b shows the microstructure of the core of the rod according to the embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
A750 ℃ high-temperature titanium alloy bar comprises the following components in percentage by mass:
5.0 to 6.0 percent of Al, 3.0 to 6.0 percent of Sn, 2.0 to 3.0 percent of Zr, 0.5 to 1.5 percent of Ni, 1.5 to 2.5 percent of Cr, 0.5 to 2.0 percent of Mo, 0.8 to 1.5 percent of Nb, 1.0 to 3.0 percent of W, 0.3 to 0.8 percent of Si, 0.5 to 1.5 percent of Fe, 0.3 to 1.5 percent of Ta, 0.5 to 1.5 percent of Y and the balance of Ti.
Wherein Si, fe, ta and Y are added by adopting intermediate alloy. In some preferred embodiments, the Si master alloy is silicon dioxide, the Fe master alloy is an Fe-Al alloy, the Ta master alloy is an Al-Ta alloy, and the Y master alloy is an Al-Ti-B-Y alloy.
In the components of the 750 ℃ high-temperature titanium alloy bar, the alloy is an alpha alloy by adding heat-resistant alloy elements of Ni, cr, mo and Nb and adding Al, so that the primary alpha phase content is increased, and the service temperature of the 750 ℃ high-temperature titanium alloy bar is increased.
The 750 ℃ high-temperature titanium alloy ingot is obtained by three times of vacuum consumable arc melting. The third vacuum consumable electric arc means that the materials are continuously melted for three times in a vacuum consumable electric arc melting furnace.
The forging method of the 750 ℃ grade high-temperature titanium alloy bar is characterized in that the raw material is a phi 720mm large-scale industrial titanium alloy ingot, the components and the mass percent of the components are shown as above, and the forging process route of the 750 ℃ grade high-temperature titanium alloy bar is as follows: preheating treatment → cogging forging → forging below the phase change point → forging above the phase change point → forging below the phase change point → graded heat treatment, which comprises the following steps:
step 1, preheating treatment:
selecting a large industrial titanium alloy ingot with the raw material phi of 720mm, putting the large industrial titanium alloy ingot into a heating furnace with the components and the mass percentages thereof as shown in the above, setting the heating temperature in the furnace to be 350-500 ℃ above the beta transformation point, and preserving the heat for 20-40 h to obtain the titanium alloy ingot subjected to preheating treatment.
Because the alloy raw material elements of the 750 ℃ high-temperature titanium alloy bar are more in variety, the phenomenon of component segregation is difficult to avoid, and the preheating treatment is carried out on the titanium alloy ingot in the step, so that the thermal motion of atoms in the ingot is intensified, and the component uniformity is increased.
Step 2, cogging and forging:
cogging and forging the titanium alloy ingot subjected to preheating treatment, wherein the cogging heating temperature is 200-300 ℃ above the phase transition point, the heating and heat preservation time is 300-450 min, and 1 firing is carried out; and then carrying out upsetting-drawing forging on the titanium alloy ingot for 3 to 6 times, wherein the forging temperature is decreased by 85 to 120 ℃ each time, the forging ratio is controlled to be 1.5 to 2.0 each time, the forging is carried out at a constant speed by hammers, and air cooling or water quenching is adopted after forging. The upsetting forging of the invention adopts two upsetting and two drawing or one upsetting and two drawing or two upsetting and one upsetting as required.
Step 3, forging at the temperature of 20-50 ℃ below the phase transformation point:
performing 1-time upsetting-drawing forging on the forging stock obtained in the step 2, wherein the material heating temperature is 20-50 ℃ below the phase change point, and the heating and heat preservation time is 300-450 min; the forging ratio is controlled to be 1.3-1.8, the forging is carried out under the condition of uniform speed pressing by hammers, and air cooling or water quenching is adopted after the forging.
Step 4, forging at 150-350 ℃ above the phase transformation point:
and (3) carrying out upsetting-drawing forging on the forging stock obtained in the step (3) for 1 to 2 times, wherein the material heating temperature is 150 to 350 ℃ above the phase transition point, the heating and heat preservation time is 300 to 450min, the forging temperature is decreased by 60 to 80 ℃ each time, the forging ratio is controlled to be 1.5 to 2.0, the forging is carried out at a constant speed by a hammer, and air cooling or water quenching is adopted after forging.
Step 5, forging at the temperature of 20-50 ℃ below the phase transformation point:
carrying out 3-time upsetting-drawing forging on the forging stock obtained in the step 4, and heating the material to T β -20 ℃ reversing upsetting and drawing, T β -25 ℃ diagonal elongation plus upset, T β Two upsetting and two drawing at minus 30 ℃, wherein the heating and heat preservation time of each heating time is 250-450 min; air cooling or water quenching is adopted after forging.
Step 6, forging at 120-300 ℃ above the transformation point:
upsetting and drawing the forging stock obtained in the step 5 for 1 to 2 times, wherein the material heating temperature is 120 to 300 ℃ above the phase transformation point, and the heating and heat preservation time is 300 to 450min; the forging temperature is decreased by 30-50 ℃ every time, the forging ratio is controlled between 1.5-2.0, the forging is carried out at a constant speed by hammer, and air cooling or water quenching is adopted after forging to obtain the equiaxial beta crystal grain intermediate blank with the crystal grain size of 1-4 mm.
And 7, forging the following phase transformation points:
carrying out 2-time upsetting-drawing forging on the forging stock obtained in the step 6, and heating the material to the temperature T below the phase change point β -30 ℃ reversing upsetting and drawing, T β Upsetting is added to the diagonal elongation at minus 35 ℃, and the heating and heat preservation time of each heating is 250-450 min; air cooling or water quenching is adopted after forging; then carrying out T β Chamfering at-40 ℃ and drawing out, T β The round is dropped and drawn out at minus 45 ℃, the forging ratio is controlled between 1.2 and 1.9, and the heating and heat preservation time of each heating time is 250 to 450 minutes; air cooling or water quenching is adopted after forging.
Step 8, adopting a heat treatment mode after forging to perform T treatment on the forged blank obtained in the step 7 β -50 ℃ and T β And carrying out graded heat treatment at the temperature of minus 300 ℃, and carrying out furnace cooling in the middle for 20-40 h per grade to obtain the 750 ℃ high-temperature titanium alloy bar. The step of graded heat treatment is used for adjusting the form of a precipitated phase (secondary alpha phase) in the material.
Before each firing in the steps 1-7, an anti-oxidation coating can be brushed on the surface of the forging stock, the anti-oxidation coating is a commercial product of Tianli Chuang company, the type number of the anti-oxidation coating is TLC1350-1, TB1200-15, TB1200-16 or TB1260-18, the anti-oxidation coating is used for preventing oxygen in the air from reacting with titanium alloy at high temperature, and meanwhile, the difference of finish forging temperature of the edge part and the center part of the material in the forging process is further reduced, so that the metal elements of the forging stock are distributed more uniformly, and the composition segregation is prevented.
Example 1
The 750 ℃ high-temperature titanium alloy bar comprises the following components in percentage by mass:
5.0 percent of Al, 3.0 percent of Sn, 2.0 percent of Zr, 0.5 percent of Ni, 1.5 percent of Cr, 0.5 percent of Mo, 0.8 percent of Nb, 1.0 percent of W, 0.3 percent of Si, 0.5 percent of Fe, 0.3 percent of Ta, 0.5 percent of Y and the balance of Ti.
The forging method of the 750 ℃ high-temperature titanium alloy bar comprises the following steps (the upsetting-drawing forging adopts two upsetting-two drawing):
(1) Preheating treatment: the raw material is a large industrial titanium alloy ingot with the diameter of 720mm, the components and the mass percentage of the large industrial titanium alloy ingot are as shown above, the large industrial titanium alloy ingot is put into a heating furnace, the heating temperature in the furnace is set to be more than 350 ℃ of beta transformation point (the transformation point is determined by adopting a metallographic method in the example, the temperature of the transformation point is about 1050-1055 ℃), and the temperature is kept for 20h, so that the titanium alloy ingot subjected to preheating treatment is obtained.
(2) Cogging and forging: cogging and forging the titanium alloy ingot subjected to preheating treatment, wherein the cogging heating temperature is 200 ℃ above the phase transition point, the heating and heat preservation time is 300min, and 1 firing is carried out; and then carrying out upsetting-drawing forging on the titanium alloy ingot for 3 times, brushing an anti-oxidation coating TLC1350-1 before each firing except for 1 firing, gradually reducing the forging temperature by 85 ℃ every firing, controlling the forging ratio at 1.5 every firing, pressing at a constant speed by a hammer, and cooling by air after forging.
(3) Forging at 20 ℃ below the transformation point: carrying out upsetting forging on the forging stock obtained in the step (2) for 1 heating time, brushing an oxidation resistant coating TLC1350-1 on the surface of the forging stock before upsetting forging, heating the material at the temperature of 20 ℃ below the phase transition point, and heating and preserving heat for 300min; controlling the forging ratio at 1.3, pressing down at constant speed by a hammer, and cooling by air after forging.
(4) Forging at 150 ℃ above the transformation point: and (3) carrying out upsetting forging on the forging stock obtained in the step (3) for 1 time, wherein the material heating temperature is 150 ℃ above the phase transition point, the heating and heat preservation time is 300min, before each time of heating, brushing an anti-oxidation coating TLC1350-1 on the surface of the forging stock, reducing the forging temperature by 60 ℃ every time of heating, controlling the forging ratio to be 1.5, pressing by a hammer at a constant speed, and cooling by air after forging.
(5) Forging at 20 ℃ below the transformation point: carrying out upsetting-drawing forging on the forging stock obtained in the step (4) for 3 times, brushing an oxidation resistant coating TLC1350-1 on the surface of the forging stock before each heating time, and heating the material to T β -20 ℃ reversing upsetting and drawing, T β -25 ℃ diagonal elongation plus upsetting and T β Carrying out two upsetting and two drawing at the temperature of minus 30 ℃, wherein the heating and heat preservation time of each heating time is 250min; air cooling is adopted after forging.
(6) Forging at 120 ℃ above the transformation point: performing 1-time upsetting-drawing forging on the forging stock obtained in the step (5), brushing an antioxidant coating TLC1350-1 on the surface of the forging stock before each heating time, heating the material at the temperature of 120 ℃ above the phase transition point, and keeping the heating temperature for 300min; the forging temperature is decreased by 30 ℃ every time, the forging ratio is controlled at 1.5, the forging is carried out at a constant speed by a hammer, and the equiaxial beta-crystal grain intermediate blank is obtained by air cooling after forging.
(7) Forging with the following transformation points: upsetting and forging the forging stock obtained in the step (6) for 2 times, brushing an oxidation resistant coating TLC1350-1 on the surface of the forging stock before each time of upsetting, and heating the material to below the phase transition point T β -30 ℃ reversing upsetting and drawing, T β Upsetting at the diagonal draw length of-35 ℃, wherein the heating and heat preservation time of each heating time is 250min; air cooling is adopted after forging; then, T is performed β Chamfering at-40 ℃ and drawing out, T β Rounding at-45 deg.C and drawing out, controlling forging ratio at 1.2, and heating and holding time of each fire for 250min; air cooling is adopted after forging.
(8) Performing post-forging heat treatment on the forged blank obtained in the step (7) at T β -50 ℃ and T β And (3) carrying out graded heat treatment at the temperature of minus 300 ℃, and carrying out furnace cooling in the middle for 20 hours per grade to obtain the 750-grade high-temperature titanium alloy bar with the phi 350mm specification.
The room-temperature tensile strength of the 750 ℃ high-temperature titanium alloy bar prepared by the embodiment is not less than 1200MPa, the elongation is not less than 8%, the 700 ℃ tensile strength is not less than 650MPa, the elongation is not less than 13.5%, the 750 ℃ tensile strength is not less than 550MPa, and the elongation is not less than 13.5%. The macroscopic structure diagram of the 750 ℃ high-temperature titanium alloy bar obtained in the embodiment after annealing is uniform and compact in macroscopic structure, low in segregation degree and high in product qualification rate, as shown in fig. 1. The microstructure is a two-state structure corresponding to the microstructures of the edge and the core of the bar, wherein figure 2a is the edge, figure 2b is the core, the grain size of the primary alpha phase is about 15 mu m, and the content of the primary alpha phase reaches about 75%.
Example 2
750 ℃ high-temperature titanium alloy bar:
the procedure of example 1 was repeated except that the surface of the ingot or the forged billet was not coated with an antioxidant coating in steps (1) to (8).
Example 3
The 750 ℃ high-temperature titanium alloy bar comprises the following components in percentage by mass:
6.0 percent of Al, 6.0 percent of Sn, 3.0 percent of Zr, 1.5 percent of Ni, 2.5 percent of Cr, 2.0 percent of Mo, 1.5 percent of Nb, 3.0 percent of W, 0.8 percent of Si, 1.5 percent of Fe, 1.5 percent of Ta, 1.5 percent of Y and the balance of Ti.
The forging method of the 750 ℃ high-temperature titanium alloy bar comprises the following steps (the upsetting-drawing forging adopts one upsetting-two drawing):
(1) Preheating treatment: the raw material is a large industrial titanium alloy ingot with the diameter of 720mm, the components and the mass percentage of the large industrial titanium alloy ingot are as shown above, the large industrial titanium alloy ingot is put into a heating furnace, the heating temperature in the furnace is set to be more than 500 ℃ of beta transformation point (the transformation point is determined by adopting a metallographic method in the example, the temperature of the transformation point is about 1050 ℃ -1055 ℃), and the temperature is kept for 40h, so that the titanium alloy ingot subjected to preheating treatment is obtained.
(2) Cogging and forging: cogging and forging the titanium alloy ingot subjected to preheating treatment, wherein the cogging heating temperature is 300 ℃ above the phase transition point, the heating and heat preservation time is 450min, and 1 firing is carried out; and then carrying out upset drawing forging on the titanium alloy ingot for 6 times, except 1 time of heating, decreasing the forging temperature by 120 ℃ every time, controlling the forging ratio every time to be 2.0, pressing down at constant speed by a hammer, and carrying out water quenching after forging.
(3) Forging at 50 ℃ below the transformation point: performing upsetting forging on the forging stock obtained in the step (2) for 1 time, brushing an antioxidant coating TB1260-18 on the surface of the forging stock before upsetting forging, heating the material at the temperature of 50 ℃ below a phase change point, and heating and preserving heat for 450min; controlling the forging ratio at 1.8, pressing at constant speed by hammers, and quenching with water after forging.
(4) Forging at 350 ℃ above the transformation point: and (4) carrying out upsetting-drawing forging on the forging stock obtained in the step (3) for 2 times, wherein the material heating temperature is 350 ℃ above the phase change point, the heating and heat preservation time is 450min, the forging temperature is decreased by 80 ℃ each time, the forging ratio is controlled to be 2.0, the forging is carried out at a constant speed by hammers, and water quenching is adopted after forging.
(5) Forging at 50 ℃ below the transformation point: upsetting and drawing the forging stock obtained in the step (4) for 3 times, brushing an antioxidant coating TB1260-18 on the surface of the forging stock before each heating time, and heating the materials to T β -20 ℃ reversing upsetting and drawing, T β -25 ℃ diagonal elongation plus upsetting and T β Carrying out two heading and two drawing at the temperature of minus 30 ℃, wherein the heating and heat preservation time of each heating time is 450min; water quenching is adopted after forging.
(6) Forging at 300 ℃ above the transformation point: carrying out upsetting-drawing forging on the forging stock obtained in the step (5) for 2 times, wherein the material heating temperature is 300 ℃ above the phase transformation point, and the heating and heat preservation time is 450min; the forging temperature is decreased by 50 ℃ every time, the forging ratio is controlled to be 2.0, the forging is carried out at a constant speed by hammers, and air cooling or water quenching is adopted after forging to obtain the equiaxed beta crystal grain intermediate blank.
(7) Forging with the following transformation points: upsetting and drawing the forging stock obtained in the step (6) for 2 times, brushing an oxidation resistant coating TB1260-18 on the surface of the forging stock before each time of heating, and heating the materials to a temperature T below a phase change point β -30 ℃ reversing upsetting and drawing, T β Upsetting at the diagonal draw length of-35 ℃, wherein the heating and heat preservation time of each heating time is 450min; air cooling or water quenching is adopted after forging; then carrying out T β Chamfering at-40 ℃ and drawing out, T β Rounding at-45 ℃ and drawing out, controlling the forging ratio to be 1.9, and keeping the heating and heat preservation time of each heating time to be 450 minutes; water quenching is adopted after forging.
(8) Performing post-forging heat treatment on the forged blank obtained in the step (7) at T β -50 ℃ and T β And carrying out graded heat treatment at the temperature of-300 ℃, and carrying out furnace cooling in the middle for 40h per grade of heat treatment time to obtain the 750 ℃ grade high-temperature titanium alloy bar.
Example 4
The 750 ℃ high-temperature titanium alloy bar comprises the following components in percentage by mass:
5.5 percent of Al, 4.5 percent of Sn, 2.5 percent of Zr, 1 percent of Ni, 2 percent of Cr, 1.2 percent of Mo, 1.1 percent of Nb, 2 percent of W, 0.55 percent of Si, 1 percent of Fe, 0.9 percent of Ta, 1 percent of Y and the balance of Ti.
The forging method of the 750 ℃ grade high-temperature titanium alloy bar comprises the following steps (the upsetting-drawing forging adopts two upsetting-one drawing):
(1) Preheating treatment: the raw material is a large industrial titanium alloy ingot with the diameter of 720mm, the components and the mass percentage of the large industrial titanium alloy ingot are as shown above, the large industrial titanium alloy ingot is placed into a heating furnace, the heating temperature in the furnace is set to be beta phase transformation point (in the example, the phase transformation point is measured by adopting a metallographic method, the temperature of the phase transformation point is about 1050 ℃ -1055 ℃) to be more than 425 ℃, and the temperature is kept for 30 hours, so that the titanium alloy ingot subjected to preheating treatment is obtained.
(2) Cogging and forging: cogging and forging the titanium alloy ingot subjected to preheating treatment, wherein the cogging heating temperature is 250 ℃ above the phase transition point, the heating and heat preservation time is 375min, and 1 firing is carried out; and then carrying out upsetting and drawing forging on the titanium alloy ingot for 4 times, wherein the forging temperature decreases by 100 ℃ every time, the forging ratio is controlled at 1.8 every time, the forging is carried out at a constant speed by hammer division, and air cooling is adopted after forging.
(3) Forging at 35 ℃ below the transformation point: carrying out upsetting-drawing forging on the forging stock obtained in the step (2) for 1 heating time, brushing an antioxidant coating TB1200-16 on the surface of the forging stock before upsetting-drawing forging, heating the material at the temperature of 35 ℃ below the phase transition point, and heating and preserving heat for 375min; controlling the forging ratio at 1.5, pressing at constant speed by a hammer, and quenching with water after forging.
(4) Forging at 250 ℃ above the transformation point: and (3) upsetting and drawing the forging stock obtained in the step (3) for 2 times, wherein the material heating temperature is 250 ℃ above the phase transition point, the heating and heat preservation time is 375min, the forging temperature is decreased by 70 ℃ each time, the forging ratio is controlled to be 1.7, the forging is carried out at a constant speed by a hammer, and air cooling is adopted after forging.
(5) Forging at 35 ℃ below the transformation point: upsetting and forging the forging stock obtained in the step (4) for 3 times, brushing an antioxidant coating TB1200-16 on the surface of the forging stock before each heating time, and heating the materials to T β -20 ℃ reversing upsetting and drawing, T β -25 ℃ diagonal elongation plus upsetting and T β Carrying out two heading and two drawing at the temperature of minus 30 ℃, wherein the heating and heat preservation time of each heating time is 350min; water quenching is adopted after forging.
(6) Forging at 210 ℃ above the transformation point: carrying out upsetting-drawing forging on the forging stock obtained in the step (5) for 1 time, wherein the material heating temperature is 210 ℃ above the phase transformation point, and the heating and heat preservation time is 375min; the forging temperature is decreased by 40 ℃ every time, the forging ratio is controlled at 1.7, the forging is carried out at a constant speed by a hammer, and water quenching is adopted after forging to obtain the equiaxed beta crystal grain intermediate blank.
(7) Forging with the following transformation points: upsetting and drawing the forging stock obtained in the step (6) for 2 times, brushing an antioxidant coating TB1200-16 on the surface of the forging stock before each time of heating, and heating the material to a temperature T below a phase transition point β -30 ℃ reversing upsetting and drawing, T β Upsetting at the diagonal draw length of-35 ℃, wherein the heating and heat preservation time of each heating time is 350min; air cooling or water quenching is adopted after forging; then, T is performed β Chamfering at-40 ℃ and drawing out, T β Rounding and drawing at-45 ℃, controlling the forging ratio at 1.5, and keeping the heating and heat preservation time of each heating time at 350 minutes; air cooling or water quenching is adopted after forging.
(8) Performing post-forging heat treatment on the forged blank obtained in the step (7) at T β -50 ℃ and T β And (3) carrying out graded heat treatment at the temperature of-300 ℃, and carrying out furnace cooling in the middle for 30 hours per grade to obtain the 750 ℃ grade high-temperature titanium alloy bar.
Example 5
The high-temperature titanium alloy bar except for the 750 ℃ grade consists of the following components in percentage by mass:
5.2 percent of Al, 5.8 percent of Sn, 2.2 percent of Zr, 1.3 percent of Ni, 2.3 percent of Cr, 0.6 percent of Mo, 0.9 percent of Nb, 1.5 percent of W, 0.4 percent of Si, 0.6 percent of Fe, 0.5 percent of Ta, 0.7 percent of Y and the balance of Ti.
The rest is the same as in example 1.
Example 6
The titanium alloy bar material except the 750 ℃ high temperature comprises the following components in percentage by mass:
5.6 percent of Al, 4.2 percent of Sn, 2.8 percent of Zr, 0.8 percent of Ni, 1.8 percent of Cr, 1.6 percent of Mo, 01.3 percent of Nb, 2.8 percent of W, 0.6 percent of Si, 1.4 percent of Fe, 1.2 percent of Ta, 1.2 percent of Y and the balance of Ti.
The rest is the same as in example 1.
Example 7
The forging method of the 750 ℃ high-temperature titanium alloy bar comprises the following steps:
removing (1) preheating treatment: the raw material is a large industrial titanium alloy ingot with the diameter of 720mm, the components and the mass percentage of the large industrial titanium alloy ingot are as shown above, the large industrial titanium alloy ingot is put into a heating furnace, the heating temperature in the furnace is set to be more than 450 ℃ and the temperature is kept for 25 hours, wherein the phase transformation point is determined by a metallographic method (the temperature of the phase transformation point is about 1050-1055 ℃) and is higher than the beta phase transformation point, and the preheated titanium alloy ingot is obtained.
(2) Cogging and forging: cogging and forging the titanium alloy ingot subjected to preheating treatment, wherein the cogging heating temperature is 220 ℃ above the phase transition point, the heating and heat preservation time is 450min, and 1 firing is carried out; and then carrying out upsetting-drawing forging on the titanium alloy ingot for 5 times, wherein the forging temperature decreases by 110 ℃ every time, the forging ratio every time is controlled at 1.9, the forging is carried out at a constant speed by hammer division, and water quenching is adopted after forging.
(3) Forging at the temperature of 45 ℃ below the phase transition point: carrying out upsetting-drawing forging on the forging stock obtained in the step (2) for 1 heating time, brushing an oxidation resistant coating TB1200-15 on the surface of the forging stock before upsetting-drawing forging, heating the material at 45 ℃ below the phase transition point, and heating and preserving heat for 330min; controlling the forging ratio at 1.4, pressing at constant speed by a hammer, and quenching with water after forging.
(4) Forging at 170 ℃ above the transformation point: and (4) carrying out upsetting-drawing forging on the forging stock obtained in the step (3) for 1 time, wherein the material heating temperature is 170 ℃ above the phase transformation point, the heating and heat preservation time is 320min, the forging temperature is decreased by 75 ℃ each time, the forging ratio is controlled to be 1.8, the forging is carried out at a constant speed by a hammer, and air cooling is adopted after forging.
(5) Forging at 25 ℃ below the transformation point: forging the forging stock obtained in the step (4) by upsetting and drawing for 3 times, brushing an antioxidant coating TB1200-15 on the surface of the forging stock before each heating time, and heating the material to T β -20 ℃ reversing upsetting and T β -25 ℃ diagonal elongation plus upsetting and T β Heating at-30 deg.C for 4250min for each heating time; air cooling is adopted after forging.
(6) Forging at 280 ℃ above the transformation point: carrying out upsetting-drawing forging on the forging stock obtained in the step (5) for 2 times, wherein the material heating temperature is 280 ℃ above the transformation point, and the heating and heat preservation time is 320min; the forging temperature decreases 45 ℃ every time, the forging ratio is controlled at 1.8, the forging is carried out at a constant speed by a hammer, and air cooling is adopted after forging to obtain the equiaxed beta crystal grain intermediate blank.
(7) Forging with the following transformation points: upsetting and drawing the forging stock obtained in the step (6) for 2 times, brushing an oxidation resistant coating TB1200-15 on the surface of the forging stock before each time of upsetting, and heating the materials to a temperature T below the phase transition point β -30 ℃ reversing upsetting and drawing, T β Upsetting at the diagonal draw length of-35 ℃, wherein the heating and heat preservation time of each heating time is 260min; water quenching is adopted after forging; then, T is performed β Chamfering and drawing at-40 ℃ and T β Round-drawing at-45 ℃, controlling the forging ratio to be 1.3, and heating and heat-preserving time of each heating time to be 420 minutes; water quenching is adopted after forging.
(8) Performing post-forging heat treatment on the forged blank obtained in the step (7) at T β -50 ℃ and T β And (3) carrying out graded heat treatment at the temperature of-300 ℃, and carrying out furnace cooling in the middle for 28 hours per grade of heat treatment time to obtain the 750 ℃ grade high-temperature titanium alloy bar.
The rest of the process was the same as in example 1.
Comparative example 1
The forging method of the titanium alloy bar comprises the following steps:
the procedure was as in example 1 except that the steps (5) to (8) were not carried out.
Comparative example 2
The titanium-removing alloy bar comprises the following components in percentage by mass:
3 percent of Al, 2 percent of Sn, 1.5 percent of Zr, 2 percent of Ni, 3 percent of Cr, 0.2 percent of Mo, 2 percent of Nb and the balance of Ti.
The rest is the same as comparative example 2.
Comparative example 3
The forging method of the titanium alloy bar comprises the following steps:
the procedure was as in example 1 except that step (8) was not carried out.
Examples of the experiments
The mechanical strength of the 750 ℃ high-temperature titanium alloy bar prepared by the specific embodiment of the invention is tested, and the test results are shown in table 1.
TABLE 1 mechanical Strength test results of 750 ℃ high temperature titanium alloy bars prepared in accordance with examples of the present invention
Figure BDA0003569648540000121
As can be seen from Table 1, the 750 ℃ grade high-temperature titanium alloy bar prepared by the embodiment of the invention has good mechanical strength at the use temperature of 700-750 ℃. The mechanical properties of the titanium alloy bar prepared by only one round of high-low-high process, other alloy components and methods such as heat treatment after forging and the like are reduced to a certain degree.
All the embodiments in the present specification are described in a related manner, and the same and similar parts among the embodiments may be referred to each other, and each embodiment focuses on differences from other embodiments. In particular, as for the system embodiment, since it is substantially similar to the method embodiment, the description is relatively simple, and reference may be made to the partial description of the method embodiment for relevant points.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.

Claims (7)

1. The forging method of the 750 ℃ high-temperature titanium alloy bar is characterized by comprising the following components in percentage by mass: 5.0 to 6.0 percent of Al, 3.0 to 6.0 percent of Sn, 2.0 to 3.0 percent of Zr, 0.5 to 1.5 percent of Ni, 1.5 to 2.5 percent of Cr, 0.5 to 2.0 percent of Mo, 0.8 to 1.5 percent of Nb, 1.0 to 3.0 percent of W, 0.3 to 0.8 percent of Si, 0.5 to 1.5 percent of Fe, 0.3 to 1.5 percent of Ta, 0.5 to 1.5 percent of Y, and the balance of Ti; the method comprises the following steps:
step 1, preheating treatment;
step 2, cogging and forging;
step 3, forging at the temperature of 20-50 ℃ below the phase transformation point;
step 4, forging at 150-350 ℃ above the phase transformation point;
step 5, forging at the temperature of 20-50 ℃ below the phase transformation point;
step 6, forging at 120-300 ℃ above the phase transformation point;
step 7, forging below the phase transformation point;
step 8, adopting a heat treatment mode after forging to perform T treatment on the forged blank obtained in the step 7 β -50 ℃ and T β Carrying out graded heat treatment at the temperature of-300 ℃, and carrying out furnace cooling in the middle to obtain the 750 ℃ high-temperature titanium alloy bar;
in the step 1, the preheating treatment specifically comprises the following steps: transferring a large industrial titanium alloy ingot containing the components of the 750 ℃ grade high-temperature titanium alloy bar and the mass percent of the large industrial titanium alloy ingot to a heating furnace, setting the heating temperature in the furnace to be 350-500 ℃ above the beta transformation point, and preserving the heat for 20-40 h to obtain a titanium alloy ingot subjected to preheating treatment;
in step 2, the cogging forging specifically comprises the following steps: cogging and forging the titanium alloy ingot subjected to preheating treatment, wherein the cogging heating temperature is 200-300 ℃ above the phase transition point, the heating and heat preservation time is 300-450 min, and 1 heating is carried out; then, upsetting and drawing the titanium alloy ingot for 3 to 6 times, gradually reducing the forging temperature of 85 to 120 ℃ each time, controlling the forging ratio of 1.5 to 2.0 each time, uniformly pressing by hammers, and performing air cooling or water quenching after forging; the upsetting forging adopts two upsetting and two drawing, one upsetting and two drawing or two upsetting and one upsetting;
in the step 8, the heat treatment time of each stage is 20-40 h;
in the steps 1-7, before each firing, brushing an anti-oxidation coating on the surface of the forging stock;
the Si, fe, ta and Y elements are added by adopting an intermediate alloy, the Si intermediate alloy is silicon dioxide, the Fe intermediate alloy is Fe-Al alloy, the Ta intermediate alloy is Al-Ta alloy, and the Y intermediate alloy is Al-Ti-B-Y alloy.
2. The forging method of the 750 ℃ high-temperature titanium alloy bar according to claim 1, wherein in the step 3, the forging at the temperature of 20-50 ℃ below the transformation point is specifically as follows: carrying out upsetting-drawing forging on the forging stock obtained in the step 2 for 1 time, wherein the material heating temperature is 20-50 ℃ below the phase transformation point, and the heating and heat preservation time is 300-450 min; the forging ratio is controlled between 1.3 and 1.8, the forging is carried out by hammering at a constant speed and pressing down, and air cooling or water quenching is adopted after forging.
3. The forging method of the 750 ℃ high-temperature titanium alloy bar according to claim 1, wherein in the step 4, the forging at 150-350 ℃ above the transformation point specifically comprises: and (3) carrying out upsetting-drawing forging on the forging stock obtained in the step (3) for 1 to 2 times, wherein the material heating temperature is 150 to 350 ℃ above the phase transition point, the heating and heat preservation time is 300 to 450min, the forging temperature is decreased by 60 to 80 ℃ each time, the forging ratio is controlled to be 1.5 to 2.0, the forging is carried out under constant-speed pressing by a hammer, and air cooling or water quenching is adopted after forging.
4. The forging method of the 750 ℃ high-temperature titanium alloy bar according to claim 1, wherein in the step 5, the forging at the temperature of 20-50 ℃ below the transformation point is specifically as follows: carrying out 3-time upsetting-drawing forging on the forging stock obtained in the step 4, and heating the material to T β -20 ℃ reversing upsetting and T β -25 ℃ diagonal elongation plus upsetting and T β Two upsetting and two drawing at minus 30 ℃, wherein the heating and heat preservation time of each heating time is 250-450 min; air cooling or water quenching is adopted after forging.
5. The forging method of the 750 ℃ high-temperature titanium alloy bar according to claim 1, wherein in the step 6, the forging at 120-300 ℃ above the transformation point specifically comprises the following steps: upsetting and drawing the forging stock obtained in the step 5 for 1 to 2 times, wherein the material heating temperature is 120 to 300 ℃ above the phase transformation point, and the heating and heat preservation time is 300 to 450min; the forging temperature is decreased by 30-50 ℃ every time, the forging ratio is controlled between 1.5-2.0, the forging is carried out at a constant speed by hammer, and air cooling or water quenching is adopted after forging to obtain the equiaxial beta crystal grain intermediate blank.
6. The forging method of the 750 ℃ high-temperature titanium alloy bar according to claim 1, wherein in the step 7, the forging with the transformation point as follows is specifically: carrying out 2 times of upsetting-drawing forging on the forging stock obtained in the step 6, and heating the material to T below the phase change point β -30 ℃ reversing upsetting and drawing, T β Upsetting at the diagonal drawing at the temperature of minus 35 ℃, wherein the heating and heat preservation time of each heating time is 250-450 min; air cooling or water quenching is adopted after forging; then carrying out T β Chamfering at-40 ℃ and drawing out, T β The steel wire is rolled and drawn at minus 45 ℃, the forging ratio is controlled to be 1.2 to 1.9, and the heating and heat preservation time of each heating time is 250 to 450min; air cooling or water quenching is adopted after forging.
7. The forging method of the 750 ℃ grade high-temperature titanium alloy bar according to claim 1, wherein the anti-oxidation coating adopts TLC1350-1, TB1200-15, TB1200-16 or TB1260-18.
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