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CN110484758B - Preparation method of high-strength T9S titanium alloy plate - Google Patents

Preparation method of high-strength T9S titanium alloy plate Download PDF

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CN110484758B
CN110484758B CN201910700427.5A CN201910700427A CN110484758B CN 110484758 B CN110484758 B CN 110484758B CN 201910700427 A CN201910700427 A CN 201910700427A CN 110484758 B CN110484758 B CN 110484758B
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CN110484758A (en
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张强
李洋
郝晓博
邱稚淳
毛人杰
聂胜东
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Luoyang Sunrui Titanium Precision Casting Co Ltd
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Luoyang Sunrui Titanium Precision Casting Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B1/00Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/38Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
    • CCHEMISTRY; METALLURGY
    • 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
    • C22CALLOYS
    • C22C14/00Alloys based on titanium
    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B1/00Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/38Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
    • B21B2001/386Plates

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Abstract

A preparation method of a high-strength T9S titanium alloy plate comprises the following specific preparation steps: step one, selecting zero-order sponge titanium, aluminum-vanadium alloy, aluminum-silicon alloy, aluminum beans and titanium dioxide for batching and pressing electrodes, adopting an argon arc welding machine for electrode assembly welding, and using a vacuum consumable arc furnace for smelting; forging the cast ingot by using a quick forging machine or an oil press, and milling the surface of the forged blank to obtain a plate blank for rolling of 80-150 mm; step three, welding and coating a layer of pure titanium sheet with the thickness of 0.6-1.5 mm on the upper surface and the lower surface of the plate blank in the step two; step four, rolling and forming the titanium alloy plate by three or four times; step five, annealing the finished blank in the step four; and sixthly, removing the surface oxide skin of the finished blank in the fifth step by adopting sand blasting and acid washing or alkaline acid washing. In conclusion, the process is simple, mass and stable production can be realized, and the prepared T9S board has good comprehensive performance and small difference of transverse and longitudinal performance.

Description

Preparation method of high-strength T9S titanium alloy plate
Technical Field
The invention belongs to the technical field of titanium alloy plate preparation, and particularly relates to a preparation method of a high-strength T9S titanium alloy plate.
Background
The titanium alloy has the advantages of small density, high specific strength, high temperature resistance, corrosion resistance and the like, and is widely applied to the fields of aviation, aerospace, ships, chemical engineering, medical treatment, sports and the like. However, the high cost of titanium alloy limits its application range in weapon, automobile, sports and other fields. Therefore, the research and development of novel low-cost titanium alloy is always a research hotspot in the field of titanium alloy at home and abroad, and the adoption of cheap elements such as Fe, Si, Mo and the like to replace expensive elements such as V and the like is an effective way for reducing the cost of the titanium alloy.
Golf is a high-grade sport, mainly concentrated in developed countries such as the united states, japan, europe, etc., and the demand for golf game equipment is high. In the early days of golf clubs, stainless steel was mainly used, and in japan in the 20 th century 90 years, titanium golf clubs were introduced, which are now in wide use in the market, and titanium has a density smaller than that of stainless steel, a strength comparable to that of stainless steel, a better elastic deformability, and a longer hitting distance. The requirements of the golf head striking panel on the performance of the titanium alloy plate are that the striking distance is long, the accuracy is high, the gravity center is low, the striking sound is pleasant, the design change of performance, function and appearance is pursued, the average production life of a golf tool is 1-1.5 years, and the golf head striking panel needs to be continuously updated and upgraded, and the strength and the elasticity of the plate are continuously improved.
The prior art discloses a striking panel of a golf club head, which has the material density of 4.33g/cm3, and the manufactured striking panel of the golf club head is made of a T9S plate, wherein the tensile strength of the T9S plate is 895-1102 MPa, the yield strength of the T9 plate is 826-1033 MPa, the elastic modulus of the T9 plate is 100-140 GPa, the elongation of the T9 plate is larger than 10 percent, and the hardness of the T9 plate is 30-40 HRC, but the strength of the T9 plate is still lower than the current. In order to meet the requirements of customers on high-strength titanium alloy plates, obtain longer hitting distance and better hitting effect, optimization of the plate production process is necessary to improve the strength of the T9S titanium alloy plates.
Disclosure of Invention
In order to solve the problem that the strength of a T9S titanium alloy plate is low in the prior art, the invention aims to provide the preparation method of the high-strength T9S titanium alloy plate, the plate strength is greatly improved under the condition that the plasticity meets the use requirement through optimization of plate components, optimization of rolling deformation rate and optimization of a heat treatment process, and the requirement of a customer on the high-strength titanium alloy plate is met.
The technical scheme of the invention is as follows: a preparation method of a high-strength T9S titanium alloy plate comprises the following specific preparation steps:
step one, selecting zero-order sponge titanium, aluminum-vanadium alloy, aluminum-silicon alloy, aluminum beans and titanium dioxide for batching and pressing electrodes, carrying out electrode assembly welding by adopting an argon arc welding machine, smelting by using a vacuum consumable electrode electric arc furnace for at least 2 times, cutting off a casting riser after smelting, peeling the surface of a cast ingot by using a lathe, respectively sampling at the head, the middle and the tail of the cast ingot, and detecting chemical components;
step two, forging the ingot by adopting a quick forging machine or an oil press, performing at least three times of upsetting, and measuring the beta transition temperature T of the ingot by a metallographic methodβAfter the blank is forged and the surface of the blank is milled, obtaining a plate blank for rolling of 80-150 mm, wherein the ultrasonic flaw detection of the plate blank is not lower than GB/T5193-2007 standard A level;
step three, welding and coating a layer of pure titanium thin plate with the thickness of 0.6-1.5 mm on the upper surface and the lower surface of the plate blank in the step two, wherein the length and the width of the pure titanium thin plate are the same as those of the plate blank;
rolling and forming the titanium alloy plate by three or four times of fire, wherein the titanium alloy plate is polished after being rolled by one time of fire, the polished semi-finished product is subjected to aging strengthening heat treatment at 500-700 ℃ after being rolled by two times of fire, the surface of the heat treated product is subjected to sand blasting acid cleaning or alkali acid cleaning and secondary polishing, then the titanium alloy plate is rolled by three times of fire into a finished plate, the surface of the finished product is subjected to sand blasting acid cleaning or alkali acid cleaning again, the finished product is cut into two plates with the same length and width specification in a fixed length and a fixed length, the two plates are overlapped, the edges are welded together by an argon arc welding machine to prepare an overlapped blank, and the overlapped blank is rolled into the finished plate by;
step five, carrying out atmospheric annealing treatment on the finished blank in the step four, wherein the annealing temperature is 700-800 ℃, the heat preservation time is 30-60 min, and discharging and air cooling after heat preservation;
and sixthly, removing the surface oxide skin of the finished blank in the fifth step by adopting sand blasting and acid washing or alkaline acid washing, grinding and removing the defects of cracks and pits, and then sizing to obtain the high-strength T9S plates with different specifications.
Further optimizing, the mass fraction of oxygen in the chemical components of the ingot in the first step is controlled to be 0.07-0.14%, the mass fraction of iron is controlled to be 0.15-0.35%, and the mass fraction of hydrogen is controlled to be less than 0.02%.
Further optimizing, the specific method and forging conditions of the three-fire forging in the second step are as follows: one-fire forging blankThe heating temperature of the material is Tβ+ (100-200) DEG C, the upsetting times are not less than 2, and the deformation rate of each upsetting or drawing is not less than 37%; heating temperature T of two-fire forging blankβ- (0-60) DEG C, the number of times of upsetting is not less than 1, and the deformation rate of each upsetting or drawing is not less than 37%; heating temperature T of three-fire forging blankβ- (20-80) DEG C, controlling the total heat deformation rate at 100-180%, and then shaping the blank, wherein the heating temperature of the shaped and forged blank is Tβ- (20-80) DEG C, wherein after each time of forging, the blank is polished and then forged for the next time.
Further optimizing, the specific method and rolling conditions of one-heating rolling in the fourth step are as follows: the heating temperature of the one-fire blank is TβAnd (3) DEG C, the heat preservation time is calculated according to 1.5 +/-0.2 min/mm, the one-pass heat deformation rate is 5-25%, the one-pass heat deformation rate is 70-90%, the roller temperature is 60-150 ℃, hot rollers are required to be heated in advance, and the roller is rolled to the one-pass target thickness by 8-14 passes.
Further optimizing, the specific method and rolling conditions of the second heating rolling in the fourth step are as follows: the heating temperature of the two-fire blank is TβThe temperature is (40-80) DEG C, the heat preservation time is calculated according to 1.3 +/-0.2 min/mm, the secondary-flame deformation rate is 5-20%, the secondary-flame deformation rate is 45-65%, the roller temperature is 50-110 ℃, hot rollers are required to be heated in advance, the rolling direction is parallel to the primary-flame rolling direction, and the target thickness is obtained through 5-9 times of rolling.
Further optimizing, the specific method and rolling conditions of the rolling of three times of heating in the fourth step are as follows: the heating temperature of the three-fire blank is TβThe temperature is (60-100) DEG C, the heat preservation time is calculated according to 1.2 +/-0.2 min/mm, the secondary deformation rate of a third fire path is 4-19%, the secondary deformation rate of the fire path is 30-50%, the temperature of a roller is 50-110 ℃, hot rollers are needed to be heated in advance, the rolling direction is parallel to the rolling direction of a second fire, the target thickness is obtained through 3-6 passes of rolling, and for plates with the thickness being more than or equal to 4mm, the thickness of a finished product can be directly rolled by the third fire.
Further optimizing, the specific method and rolling conditions of four times of heating rolling in the fourth step are as follows: the heating temperature of the four-fire pack-rolled blank is Tβ- (60-100) DEG C, the heat preservation time is calculated according to 1.2 +/-0.2 min/mm, the rate of secondary deformation of four flame paths is 4-15%, the rate of secondary deformation of flame is 20-40%, the temperature of a roller is 50-110 ℃, a hot roller needs to be heated in advance, the rolling direction is parallel to the rolling direction of three flame paths, and the rolling is carried out for 3-6 pathsAnd (4) rolling to the target thickness, and rolling to the finished product thickness specification by four times for providing a plate of a blank for a thin plate with the thickness of 2.5-4 mm and a cold-rolled thin plate with the required thickness of less than or equal to 4.0 mm.
Further optimizing, the aging strengthening heat treatment in the fourth step adopts a trolley furnace or a pit furnace to carry out stacking annealing, the total thickness of the stacked plates is not more than 180mm, the plates are charged at room temperature, the heat is preserved for 4-12 h, the furnace door is opened for 50-200 mm after the plates are charged, the plates are cooled to 300-450 ℃ and discharged, and the cooling time is 10-14 h.
Further optimizing, in the fourth step, the welding current of argon arc welding is 150-250A, the length of a welding seam is 200-400 mm, the interval between adjacent welding seams is 50-100 mm, argon is used for protection during welding, and the weld penetration is 4-8 mm.
The invention has the beneficial effects that:
optimizing chemical components of the cast ingot, and improving the strength of the T9S titanium alloy plate;
secondly, performing aging strengthening heat treatment on the semi-finished product of the second fire to obtain a structure with a uniform structure, wherein the phase change is generated after aging, so that the strength of the plate is improved;
thirdly, the rolling heat deformation rate is optimized, so that the structure is fully crushed and refined, and the strength of the plate is further improved;
fourthly, annealing the finished product at a low temperature of 700-800 ℃, so that the strength of the plate is improved;
in conclusion, the process is simple, mass and stable production can be realized, the prepared T9S board has good comprehensive performance, small difference of transverse and longitudinal performances and 1100 tensile strength
The material has the following characteristics of yield strength of 1000-1250 MPa, yield strength of 1150MPa, elongation of 10-22%, elastic modulus of 100-150 GPa and hardness of 36-42 HRC.
Drawings
FIG. 1 is a microstructure of a 4mm T9S titanium alloy plate prepared in example 1
FIG. 2 is a microstructure of a 4.8mm T9S titanium alloy plate prepared in example 2
FIG. 3 is a microstructure of a 3mm T9S titanium alloy plate prepared in example 3
FIG. 4 is a microstructure of a 4mm T9S titanium alloy sheet prepared in comparative example 1.
Detailed Description
The present invention is described in detail with reference to the following embodiments, which should be pointed out herein for the purpose of further explanation only and are not to be construed as limiting the scope of the present invention, and those skilled in the art can make insubstantial modifications and adaptations in light of the above disclosure.
The specific implementation mode of the invention is as follows:
example 1
Step one, selecting zero-order sponge titanium, aluminum-vanadium alloy, aluminum-silicon alloy, aluminum beans and titanium dioxide for batching and electrode pressing, performing electrode assembly welding by using an argon arc welding machine, smelting for 2 times by using a vacuum consumable electrode furnace, cutting off a dead head of an ingot after secondary smelting, peeling the surface of the ingot by using a lathe, respectively sampling the head, the middle and the tail of the ingot, wherein the mass fraction of oxygen of the ingot is 0.11-0.13%, the mass fraction of iron is 0.18-0.21%, the mass fraction of hydrogen is 0.001%, and the phase transition point of the ingot is 1060 ℃ measured by a metallographic method;
forging the ingot by using a quick forging machine, wherein the heating temperature of the first-heat forging blank is 1200 ℃, the deformation rate of each upsetting or drawing is 40% after twice upsetting and drawing, the surface cracks and the air suction layer are removed after grinding after forging, the heating temperature of the second-heat forging blank is 1080 ℃, and the deformation rate of each upsetting or drawing is 40% after once upsetting and drawing; the heating temperature of the three-fire forged blank is 1040 ℃, the total deformation rate of the fire times is 140%, a blank for rolling with the thickness of 140mm is obtained after the blank is shaped and milled, and the ultrasonic flaw detection of the blank meets the A level of GB/T5193-2007 standard;
thirdly, welding and coating a layer of pure titanium sheet with the thickness of 1.0mm on the upper surface and the lower surface of the plate blank, wherein the length and the width of the pure titanium sheet are the same as those of the plate blank, so that surface cracks during one-shot rolling are reduced;
step four, rolling and forming the titanium alloy plate by three times of fire:
the first-pass rolling is carried out, wherein the heating temperature of a first-pass blank is 1080 ℃, the heat preservation time is 200min, the first-pass rolling is carried out for 12 passes to 17mm, the deformation rate of each pass is 5%, 13%, 16%, 22%, 23%, 21%, 19%, 16%, 15%, 14%, 10% in sequence, the deformation rate of the first-pass rolling is 88%, the temperature of a roller is 100 ℃, a rolled hot plate is scalped and polished by using a grinding wheel and a thousand-blade wheel, the defects of surface oxide skin, an air suction layer, a coating layer, cracks, pressing and the like are removed, and the coping direction is parallel to the first-pass rolling direction;
performing secondary hot rolling, wherein the heating temperature of a secondary hot blank is 1020 ℃, the heat preservation time is 22min, the secondary hot blank is rolled to 7mm by 8 times, the deformation rate of each time is 18%, 15%, 12%, 9%, 8%, 6%, 5%, the deformation rate of the secondary hot blank is 59%, the temperature of a roller is 80 ℃, the rolling direction is parallel to the rolling direction of the primary hot blank, the aging strengthening heat treatment is performed on the secondary hot semi-finished product, the annealing temperature is 650 ℃, the heat preservation time is 12h, a trolley furnace performs stacking annealing, 20 sheets are stacked, the furnace is charged at room temperature, after the heat preservation is finished, a furnace door is opened for 200mm, the temperature is cooled to 300 ℃, the furnace is taken out, the cooling time is 15h, the alkali pickling is performed on the polished surface;
rolling with three fire, wherein the heating temperature of the blank with three fire is 980 ℃, the heat preservation time is 9min, the blank is rolled to 4mm with 4 passes, the deformation rate of each pass is 17%, 14%, 12% and 9%, the deformation rate of the fire is 43%, the temperature of the roller is 70 ℃, and the rolling direction is parallel to the rolling direction with two fire;
step five, annealing in the atmosphere of a roller hearth furnace at the annealing temperature of 750 ℃ for 45min, and discharging and air cooling after heat preservation;
and sixthly, removing surface oxide scales by adopting alkali spraying and acid washing, grinding and removing cracks and pit defects, and then sizing to obtain the high-strength T9S plate with the specification of 4mm, wherein the finished product microstructure of the plate is shown in figure 1, and the mechanical properties are shown in table 1.
According to the thickness of the plate, the heat preservation time of the first-fire rolling is calculated according to 1.5 +/-0.2 min/mm, the heat preservation time of the second-fire rolling is calculated according to 1.3 +/-0.2 min/mm, and the heat preservation time of the third-fire rolling is calculated according to 1.2 +/-0.2 min/mm.
Example 2
Step one, selecting zero-order sponge titanium, aluminum-vanadium alloy, aluminum-silicon alloy, aluminum beans and titanium dioxide for proportioning and electrode pressing, performing electrode assembly welding by using an argon arc welding machine, smelting for 2 times by using a vacuum consumable electrode furnace, cutting off a dead head of an ingot after secondary smelting, peeling the surface of the ingot by using a lathe, respectively sampling the head, the middle and the tail of the ingot, wherein the mass fraction of oxygen of the ingot is 0.08-0.10%, the mass fraction of iron is 0.19-0.22%, the mass fraction of hydrogen is 0.001%, and the phase transition point of the ingot is 1050 ℃ measured by a metallographic method;
secondly, forging the cast ingot by adopting a quick forging machine, wherein the heating temperature of the first-heat forging blank is 1160 ℃, the upsetting and drawing are carried out twice, the deformation rate of each upsetting or drawing is 40%, the grinding is finished to remove surface cracks and a gas suction layer, the heating temperature of the second-heat forging blank is 1060 ℃, the upsetting and drawing are carried out once, and the deformation rate of each upsetting or drawing is 40%; the heating temperature of the three-fire forged blank is 1020 ℃, the total deformation rate of the fire is 160%, a 120mm rolling plate blank is obtained after the blank is shaped and milled, and the ultrasonic flaw detection of the plate blank meets the A level of GB/T5193-2007 standard;
thirdly, welding and coating a layer of pure titanium sheet with the thickness of 1.2mm on the upper surface and the lower surface of the plate blank, wherein the length and the width of the pure titanium sheet are the same as those of the plate blank, so that surface cracks during one-shot rolling are reduced;
step four, rolling and forming the titanium alloy plate by three times of fire:
the first-pass rolling is carried out, wherein the heating temperature of a first-pass blank is 1060 ℃, the heat preservation time is 160min, the first-pass rolling is carried out to 18mm in 10 passes, the deformation rate of each pass is 6%, 17%, 21%, 23%, 21%, 14%, 13% and 10% in sequence, the deformation rate of the first-pass rolling is 85%, the temperature of a roller is 90 ℃, a rolled hot plate is scalped and polished by using a grinding wheel and a thousand-blade wheel, the defects of surface oxide skin, an air suction layer, a coating layer, cracks, pressing and the like are removed, and the coping direction is parallel to the first-pass rolling;
performing secondary hot rolling, wherein the heating temperature of a secondary hot blank is 990 ℃, the heat preservation time is 24min, the secondary hot blank is rolled to 8mm by 6 times, the deformation rate of each time is 17%, 13%, 11%, 10%, 8%, the deformation rate of the secondary hot blank is 56%, the temperature of a roller is 70 ℃, the rolling direction is parallel to the direction of primary hot rolling, the aging strengthening heat treatment is performed on the secondary hot semi-finished product, the annealing temperature is 700 ℃, the heat preservation time is 8h, the trolley furnace is used for stacking annealing, 22 sheets are stacked, the furnace is charged at room temperature, the furnace door is opened for 200mm after the heat preservation is finished, the furnace is cooled to 400 ℃ and taken out, the cooling time is 12h, the surface is subjected to alkali pickling after the heat treatment;
rolling with three fire, wherein the heating temperature of the blank with three fire is 970 ℃, the heat preservation time is 10min, the blank is rolled to 4.8mm by 4 passes, the deformation rate of each pass is 15%, 13%, 12% and 8%, the deformation rate of the fire is 40%, the temperature of the roller is 80 ℃, and the rolling direction is parallel to the rolling direction with two fire;
step five, annealing in the atmosphere of a roller hearth furnace at the annealing temperature of 780 ℃ for 55min, and discharging and air cooling after heat preservation;
removing surface oxide skin by adopting alkali spraying and acid washing, grinding and removing cracks and pit defects, and then sizing to obtain a high-strength T9S plate with the specification of 4.8 mm; the microstructure of the finished product is shown in FIG. 2, and the mechanical properties are shown in Table 1.
According to the thickness of the plate, the heat preservation time of the first-fire rolling is calculated according to 1.5 +/-0.2 min/mm, the heat preservation time of the second-fire rolling is calculated according to 1.3 +/-0.2 min/mm, and the heat preservation time of the third-fire rolling is calculated according to 1.2 +/-0.2 min/mm.
Example 3
Step one, selecting zero-order titanium sponge, aluminum-vanadium alloy, aluminum-silicon alloy, aluminum beans and titanium dioxide for batching and electrode pressing, performing electrode assembly welding by using an argon arc welding machine, smelting for 2 times by using a vacuum consumable electrode furnace, cutting off a dead head of an ingot after secondary smelting, peeling the surface of the ingot by using a lathe, respectively sampling the head, the middle and the tail of the ingot, wherein the mass fraction of oxygen of the ingot is 0.08-0.10%, the mass fraction of iron is 0.23-0.26%, the mass fraction of hydrogen is 0.003%, and the phase transition point of the ingot is 1040 ℃ measured by a metallographic method;
forging the ingot by using a quick forging machine, wherein the heating temperature of the first-heat forging blank is 1180 ℃, the upsetting and drawing are performed twice, the deformation rate of each upsetting or drawing is 40%, the grinding is completed after the forging to remove surface cracks and an air suction layer, the heating temperature of the second-heat forging blank is 1100 ℃, the upsetting and drawing are performed twice, and the deformation rate of each upsetting or drawing is 40%; the heating temperature of a three-fire forged blank is 1010 ℃, the total deformation rate of fire times is 180%, a plate blank for rolling of 100mm is obtained after the blank is shaped and milled, and the ultrasonic flaw detection of the plate blank meets the A-grade of GB/T5193-2007 standard;
thirdly, welding and coating a layer of pure titanium sheet with the thickness of 0.8mm on the upper surface and the lower surface of the plate blank, wherein the length and the width of the pure titanium sheet are the same as those of the plate blank, so that surface cracks during one-shot rolling are reduced;
step four, rolling and forming the titanium alloy plate by four times of heating:
first-time rolling, wherein the heating temperature of a first-time blank is 1040 ℃, the heat preservation time is 140min, the first-time blank is rolled to 16mm in 8 times, the deformation rate of each time is 8%, 17%, 22%, 24%, 25%, 23%, 20% in sequence, the deformation rate of the first-time blank is 84%, the temperature of a roller is 110 ℃, a rolled hot plate is scalped and polished by using a grinding wheel and a millennium wheel, the defects of a surface oxide skin, an air suction layer, a coating layer, cracks, pressing and the like are removed, and the coping direction is parallel to the first-time rolling direction;
carrying out secondary rolling on the blank with the secondary heating temperature of 980 ℃ for 20min, rolling the blank with 6 passes to 6.5mm, sequentially setting the deformation rate of each pass to 19%, 15%, 14%, 13%, 12%, 10%, 60% of secondary deformation rate, and 60% of roller temperature, wherein the rolling direction is parallel to the primary rolling direction, carrying out aging strengthening heat treatment on the semi-finished product with the secondary heating, annealing the semi-finished product with 620 ℃ and heat preservation time of 10h, carrying out stacking annealing on a trolley furnace, stacking 25 sheets of plates, charging the semi-finished product with room temperature, opening a furnace door to 200mm after heat preservation, cooling the semi-finished product to 350 ℃, discharging the semi-finished product, cooling the semi-finished product for 14h, carrying out alkaline pickling and coping on the surface after heat treatment, and;
carrying out three-pass rolling, wherein the heating temperature of a blank with three passes is 960 ℃, the heat preservation time is 8min, the blank is rolled to 4.2mm through 3 passes, the deformation rate of each pass is 18%, 14%, 12% and 35% in sequence, the heat deformation rate of the blank with three passes is 60 ℃, the rolling direction is parallel to the rolling direction with two passes, after the rolling, the surface of a semi-finished product with 4.2mm is subjected to sand blasting and acid washing, the surface defects are removed by grinding, the semi-finished product is cut into two plates with the same length and width specifications by a fixed length, the two plates are overlapped, the edges are aligned, the edges are welded together by using an argon arc welding machine, the welding parameters and the current are 200A, the length of a welding seam is 300mm, the interval between adjacent welding seams is 80mm, four corners;
rolling by four times, wherein the heating temperature of a four-heat pack-rolled blank is 960 ℃, the heat preservation time is 5min, a pack-rolled pack is 8.4mm, the pack-rolled pack is rolled to 6mm by 4 times, the deformation rate of each time is 11%, 9%, 7% and 4% in sequence, the heat deformation is 29%, the temperature of a roller is 70 ℃, and the rolling direction is parallel to the three-heat rolling direction;
step five, annealing in the atmosphere of a roller hearth furnace at the annealing temperature of 720 ℃ for 30min, and discharging and air cooling after heat preservation;
removing surface oxide skin by adopting alkali spraying and acid washing, grinding and removing cracks and pit defects, and then sizing to obtain a high-strength T9S plate with the specification of 3 mm; the microstructure of the finished product is shown in FIG. 3, and the mechanical properties are shown in Table 1.
According to the thickness of the plate, the heat preservation time of the first-fire rolling is calculated according to 1.5 +/-0.2 min/mm, the heat preservation time of the second-fire rolling is calculated according to 1.3 +/-0.2 min/mm, the heat preservation time of the third-fire rolling is calculated according to 1.2 +/-0.2 min/mm, and the heat preservation time of the fourth-fire rolling is calculated according to 1.2 +/-0.2 min/mm.
Comparative example 1
The slab with the thickness of 140mm is used, the phase change point of an ingot is measured to be 1060 ℃, the thickness of the finished product in the comparative example 1 is the same as that in the example 1, the slab is rolled to the target thickness by four times, the rest technological parameters are the same as those in the example, the thicknesses of the four times of rolling are respectively 17mm, 8mm, 5.4 mm and 4mm, the microstructure of the finished product plate prepared in the comparative example 1 is shown in figure 4, and the mechanical properties are shown in table 1.
Comparative example 2
A120 mm thick plate blank is used, the phase change point of an ingot is actually measured to be 1050 ℃, the chemical components of the plate blank in the comparative example 2 are the same as those in the example 2, the semi-finished product of the second fire is not subjected to aging strengthening heat treatment, the thickness of the finished product is 4.5mm, the rest process parameters are the same as those in the example, and the mechanical properties of the finished plate prepared in the comparative example 2 are shown in table 1.
TABLE 1 comparison of mechanical properties at room temperature of the examples with those of comparative example T9S
Figure 13668DEST_PATH_IMAGE001
Compared with the comparative example 1, the heat deformation rate is larger, the structure breaking is more sufficient, and it can be seen from fig. 1 and fig. 4 that the plate prepared in the example 1 recovers after the annealing at the same temperature, the plate prepared in the example 1 recovers and incompletely recrystallizes, and the strength of the plate can be greatly improved by increasing the heat deformation rate.
Example 2 in comparison with comparative example 2, the finished product of comparative example 2 has a higher hot set deformation ratio than example 2, and the strength of the plate is inferior to that of example 2 because the semi-finished product is not subjected to the age-strengthening heat treatment.
The foregoing illustrates and describes the principal features, utilities, and principles of the invention, as well as advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made in the invention without departing from the spirit and scope of the invention. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (5)

1. A preparation method of a high-strength T9S titanium alloy plate is characterized by comprising the following specific preparation steps:
step one, selecting zero-order sponge titanium, aluminum-vanadium alloy, aluminum-silicon alloy, aluminum beans and titanium dioxide for batching and pressing electrodes, carrying out electrode assembly welding by adopting an argon arc welding machine, smelting by using a vacuum consumable electrode furnace for at least 2 times, cutting off a casting riser after smelting, peeling the surface of a cast ingot by using a lathe, respectively sampling at the head, the middle and the tail of the cast ingot, and detecting chemical components;
step two, forging the ingot by adopting a quick forging machine or an oil press, upsetting and drawing the ingot for at least three times, and measuring the beta transition temperature T of the ingot by a metallographic methodβAfter the blank is forged and the surface of the blank is milled, obtaining a plate blank for rolling of 80-150 mm, wherein the ultrasonic flaw detection of the plate blank is not lower than GB/T5193-2007 standard A level;
step three, welding and coating a layer of pure titanium thin plate with the thickness of 0.6-1.5 mm on the upper surface and the lower surface of the plate blank in the step two, wherein the length and the width of the pure titanium thin plate are the same as those of the plate blank;
and step four, rolling and forming the titanium alloy plate by three or four times of fire, wherein the titanium alloy plate is polished after being rolled by one time of fire, the polished semi-finished product is subjected to aging strengthening heat treatment at 500-700 ℃ after being rolled by two times of fire, the surface of the polished semi-finished product is subjected to sand blasting acid cleaning or alkali acid cleaning and secondary polishing after the heat treatment, then rolling by three times of fire into a finished plate, the surface of the finished product is subjected to sand blasting acid cleaning or alkali acid cleaning again, cutting into two plates with the same length and width specification in a fixed length, overlapping the two plates, welding the edges together by using an argon arc welding machine to prepare a rolled blank, and rolling the rolled blank into the finished plate by four times of fire, wherein the specific method for rolling by four times of fire is as:
the specific method and rolling conditions of the first hot rolling are as follows: the heating temperature of the one-fire blank is TβThe temperature is +/-0-40 ℃, the heat preservation time is calculated according to 1.5 +/-0.2 min/mm, the first-pass secondary deformation rate is 5-25%, the second-pass deformation rate is 70-90%, the temperature of a roller is 60-150 ℃, hot rolling is carried out in advance, and the roller is rolled to the first-pass target thickness by 8-14 passes; the specific method and rolling conditions of the secondary fire rolling are as follows: the heating temperature of the two-fire blank is TβThe temperature is controlled to be (40-80 ℃), the heat preservation time is calculated according to 1.3 +/-0.2 min/mm, the secondary-flame-path secondary deformation rate is 5-20%, the secondary-flame-path deformation rate is 45-65%, the roller temperature is 50-110 ℃, hot rollers are required to be heated in advance, the rolling direction is parallel to the primary-flame rolling direction, and the target thickness is obtained through 5-9 times of rolling; the specific method and rolling conditions of the three-fire rolling are as follows: the heating temperature of the three-fire blank is TβThe temperature is (60-100) DEG C, the heat preservation time is calculated according to 1.2 +/-0.2 min/mm, the secondary deformation rate of a third fire path is 4-19 percent, the secondary deformation rate of the fire path is 30-50 percent, the temperature of a roller is 50-110 ℃, hot rollers are needed to be heated in advance, the rolling direction is parallel to the rolling direction of a second fire, the target thickness is obtained through 3-6 passes of rolling, and for a plate with the thickness being more than or equal to 4mm, the thickness of a finished product can be directly rolled by the third fire; the specific method and rolling conditions of four-fire rolling are as follows: the heating temperature of the four-fire pack-rolled blank is TβThe temperature is (60-100) DEG C, the heat preservation time is calculated according to 1.2 +/-0.2 min/mm, the secondary deformation rate of four flame paths is 4-15%, the secondary deformation rate of fire is 20-40%, the temperature of a roller is 50-110 ℃, hot rollers are needed to be heated in advance, the rolling direction is parallel to the rolling direction of three flame paths, the sheet is rolled to the target thickness by 3-6 times, a blank sheet is provided for a sheet with the thickness of 2.5-4 mm and a cold-rolled sheet with the thickness of less than or equal to 4.0mm, and the sheet can be rolled to the finished product thickness by four flame;
step five, carrying out atmospheric annealing treatment on the finished plate in the step four, wherein the annealing temperature is 700-800 ℃, the heat preservation time is 30-60 min, and discharging and air cooling after heat preservation;
and sixthly, removing the surface oxide skin of the finished blank in the fifth step by adopting sand blasting and acid washing or alkaline acid washing, grinding and removing the defects of cracks and pits, and then sizing to obtain the high-strength T9S plates with different specifications.
2. The method for preparing the high-strength T9S titanium alloy plate according to claim 1, wherein the ingot in the first step is controlled to have the chemical components of 0.07-0.14% of oxygen, 0.15-0.35% of iron and less than 0.02% of hydrogen.
3. The method for preparing the high-strength T9S titanium alloy plate according to claim 1, wherein the specific forging method and forging conditions of the three-fire forging in the second step are as follows: the heating temperature of the one-fire forging blank is Tβ+ (100-200) DEG C, the upsetting and drawing times are not less than 2, and the deformation rate of each upsetting or drawing is not less than 37%; heating temperature T of two-fire forging blankβ0-60 ℃, the upsetting and drawing times are not less than 1, and the deformation rate of each upsetting or drawing is not less than 37 percent; heating temperature T of three-fire forging blankβ- (20-80) DEG C, controlling the total heat deformation rate at 100-180%, and then shaping the blank, wherein the heating temperature of the shaped and forged blank is Tβ- (20-80) DEG C, wherein after each time of forging, the blank is polished and then forged for the next time.
4. The preparation method of the high-strength T9S titanium alloy plate according to claim 1, wherein the aging strengthening heat treatment in the fourth step is performed by stacking and annealing in a trolley furnace or a pit furnace, the total thickness of the stacked plates is not more than 180mm, the plates are charged at room temperature, the temperature is kept for 4-12 h, the furnace door is opened for 50-200 mm, the plates are cooled to 300-450 ℃, and the plates are discharged for 10-14 h.
5. The method for preparing the high-strength T9S titanium alloy plate according to claim 1, wherein in the fourth step, the welding current of argon arc welding is 150-250A, the length of the welding seam is 200-400 mm, the interval between adjacent welding seams is 50-100 mm, argon is used for protection during welding, and the penetration of the welding seam is 4-8 mm.
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