CN114231870A - Rapid fine grain preparation method by rolling deformation composite self-resistance heating annealing of tantalum alloy - Google Patents

Rapid fine grain preparation method by rolling deformation composite self-resistance heating annealing of tantalum alloy Download PDF

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CN114231870A
CN114231870A CN202111554190.8A CN202111554190A CN114231870A CN 114231870 A CN114231870 A CN 114231870A CN 202111554190 A CN202111554190 A CN 202111554190A CN 114231870 A CN114231870 A CN 114231870A
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tantalum alloy
rolling
plate blank
resistance heating
annealing
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肖寒
黄树海
舒大禹
周利
陈强
吴洋
詹红
张菲玥
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Harbin Institute of Technology
No 59 Research Institute of China Ordnance Industry
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Harbin Institute of Technology
No 59 Research Institute of China Ordnance Industry
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    • 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
    • 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
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26Methods of annealing
    • 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
    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/0081Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for slabs; for billets

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  • Organic Chemistry (AREA)
  • Metal Rolling (AREA)

Abstract

The invention relates to the technical field of metal plastic forming, and discloses a rapid fine grain preparation method by rolling deformation and self-resistance heating annealing of tantalum alloy, which comprises the following steps: step 1, obtaining a rectangular coarse-grain tantalum alloy plate; step 2, performing room-temperature asynchronous rolling deformation on the coarse-grain tantalum alloy plate through asynchronous rolling equipment; step 3, performing high-temperature anti-oxidation spraying treatment on the tantalum alloy rolling plate blank; step 4, carrying out self-resistance heating isothermal annealing treatment on the tantalum alloy rolling plate blank subjected to the anti-oxidation treatment by adopting a high-energy pulse direct-current power supply; step 5, judging whether rolling needs to be continued; step 6, carrying out rotation treatment on the tantalum alloy annealed plate blank; and 7, straightening the tantalum alloy plate blank finally obtained in the step 4 to obtain the tantalum alloy plate blank with uniform and fine grain structure. The invention solves the problems of limited refinement degree of the conventional cold deformation and furnace thermal annealing grain structure, long period, high energy consumption and the like.

Description

Rapid fine grain preparation method by rolling deformation composite self-resistance heating annealing of tantalum alloy
Technical Field
The invention relates to the technical field of metal plastic forming, in particular to a rapid grain refining preparation method by rolling deformation and self-resistance heating annealing of tantalum alloy.
Background
The tantalum alloy has a high density (16.67 g/cm)3) The high-ductility explosive-shaped shell has the advantages of high melting point (2996 ℃), high ductility (the elongation at room temperature is more than 40%), excellent penetration performance (more than 30% higher than that of copper), remarkably improved penetration capability and anti-interference capability under high explosive conditions, and is one of ideal materials for explosive-shaped shot (EFP) and rod-type Jet (JPC) explosive-shaped shells. The application of tantalum alloy to the warhead of key models, such as SADARM in the United states, SMART in Germany, BONUS in Sweden, and ACED155 in France, has been successfully realized in the 90 s of the 20 th century in China. The problem of insufficient penetration capability of the tantalum alloy shaped charge liner in China generally exists, and one of the fundamental reasons is that the traditional blank making process has technical bottlenecks of large grains, mixed crystals, low ductility and the like, and the high ductility tantalum alloy material with uniform, fine-grained and weak texture tissues cannot be prepared.
At present, the traditional preparation method of the fine-grain tantalum alloy material is electron beam melting, cold deformation and vacuum furnace thermal annealing, and has the following problems: firstly, the preparation efficiency is low, the annealing temperature of the tantalum alloy is up to more than 1000 ℃, the annealing needs to be carried out in a vacuum furnace for preventing the blank from being oxidized at high temperature, the time consumed by heating and cooling is long, the intermediate annealing times are many, the blank preparation link efficiency is low, and the blank preparation period is up to more than 30 h. Secondly, the tissue optimization potential can not be exerted efficiently, as the temperature rise process of furnace thermal annealing is slow, a great part of deformation energy storage obtained by the tantalum alloy in the cold deformation stage is released in the temperature rise process in a recovery mode, the recrystallization driving force is insufficient, the grain structure refinement degree is limited, the tissue optimization potential can not be exerted efficiently, and the problems of coarse crystals, mixed crystals and the like are easily caused, for example, the fine crystals of 10 microns and the coarse crystals of 120 microns in the grain structure of the tantalum alloy shaped charge cover formed by the traditional process by Penghai Jian and the like of Beijing institute of nonferrous metals and the like; thirdly, the energy consumption in the preparation process is high, only a small part of the energy in the high-temperature annealing process is used for improving the structure of the material, the energy utilization rate is low, and the energy consumption in the preparation process is high. Therefore, a new mechanism based tantalum alloy recrystallization annealing process method is needed to be provided to realize the efficient preparation of the tantalum alloy blank with fine grains, weak texture and high ductility.
Disclosure of Invention
According to the rapid fine grain preparation method through the rolling deformation composite self-resistance heating annealing of the tantalum alloy, provided by the invention, shearing large plastic deformation is introduced through asynchronous rolling, and efficient annealing is carried out by using the Joule heat effect of high-energy pulse current, so that the aim of preparing a uniform fine grain structure tantalum alloy material is fulfilled.
The invention is realized by the following technical scheme:
a rapid fine grain preparation method of tantalum alloy rolling deformation composite self-resistance heating annealing comprises the following steps:
step 1, obtaining a rectangular coarse-grain tantalum alloy plate;
step 2, carrying out room-temperature asynchronous rolling deformation on the coarse-grain tantalum alloy plate through asynchronous rolling equipment to obtain a tantalum alloy rolling plate blank;
step 3, performing high-temperature anti-oxidation spraying treatment on the tantalum alloy rolling plate blank, and drying the tantalum alloy rolling plate blank for later use;
step 4, carrying out self-resistance heating isothermal annealing treatment on the tantalum alloy rolled plate blank subjected to the anti-oxidation treatment by adopting a high-energy pulse direct-current power supply, rapidly cooling the annealed tantalum alloy rolled plate after the heat preservation time reaches a set time length to obtain a tantalum alloy annealed plate blank, and carrying out surface cleaning inspection on the cooled tantalum alloy rolled plate for later use;
step 5, judging whether rolling is needed to be continued, if so, jumping to step 6, otherwise, jumping to step 7; the judgment of whether the rolling needs to be continued can be carried out according to the cycle number of rolling-heating-annealing-cooling, and the cycle number can be 3-8.
Step 6, performing rotation treatment on the tantalum alloy annealed slab to obtain a tantalum alloy slab, performing room-temperature asynchronous rolling deformation on the tantalum alloy slab through asynchronous rolling equipment to obtain a tantalum alloy rolled slab, and returning to the step 3;
and 7, straightening the tantalum alloy plate blank finally obtained in the step 4 to obtain the tantalum alloy plate blank with uniform and fine grain structure.
In the technical scheme, firstly, a tantalum plate is asynchronously rolled at room temperature to obtain a cold deformation rolling plate blank, and then self-resistance heating recrystallization annealing treatment is carried out on the cold deformation rolling plate blank by applying high-energy pulse current; and (3) obtaining the tantalum alloy plate blank with fine and uniform grain structure by repeating cold rolling and self-resistance heating annealing treatment.
As an optimization, in the step 1, the method for obtaining the rectangular coarse-grained tantalum alloy plate comprises the following steps: the coarse-grain tantalum alloy blank is manufactured by adopting a machining mode, and the thickness of the coarse-grain tantalum alloy plate is not more than 20 mm.
As an optimization, in step 2, after the tantalum alloy rolling slab is obtained, the surface of the tantalum alloy rolling slab needs to be cleaned.
As an optimization, in the step 4, the specific steps of performing self-resistance heating isothermal annealing treatment by using a high-energy pulse direct-current power supply are as follows:
step 4.1, clamping two ends of the tantalum alloy rolling plate blank subjected to the anti-oxidation treatment through electrodes respectively, and meanwhile, connecting the two electrodes with the positive electrode and the negative electrode of the high-energy pulse direct-current power supply through leads respectively to form a current heating loop;
the electrode adopts tungsten-copper alloy, the lead in the current loop adopts red copper bar, the section size of the red copper bar is more than or equal to 24mm multiplied by 250 mm; by high energy pulsesThe average current density parameter of the tantalum alloy plate blank self-resistance heating annealing of a direct current power supply is as follows: 18-24A/mm 2, annealing heat preservation temperature of 1000-1300 ℃, and self-resistance heating annealing time of 1-5 min. The current density is equal to the current passing through the metal divided by the cross-sectional area of the metal blank, e.g. 50 x 10-500 mm in cross-sectional area of tantalum alloy sheet2And the current magnitude is 10000A, then the current density is 10000/500 ═ 20A/mm2
And 4.2, setting parameters of the high-energy pulse direct-current power supply, turning on a switch of the high-energy pulse direct-current power supply, and electrifying and heating the tantalum alloy rolling plate blank.
As optimization, the parameters of the high-energy pulse direct-current power supply are as follows: 20000A/12V, the current pulse frequency range is 100-3000 Hz, and the current duty ratio range is 1-100%. The parameters of the high-energy pulse direct-current power supply are fixed parameters of the power supply, and mean that the average current of the power supply can reach 20000A at most and the voltage can reach 12V at most.
As an optimization, in step 4, the specific manner of rapidly cooling the annealed tantalum alloy rolled sheet is as follows: and rapidly cooling the annealed tantalum alloy rolled plate by adopting a liquid nitrogen gas injection mode. Generally, the higher the heating current density and the higher the temperature, the shorter the annealing time should be set to prevent the crystal grains from growing; and after annealing, rapidly cooling by adopting a liquid nitrogen gas injection mode.
Preferably, in step 3, the spraying agent for performing the high-temperature anti-oxidation spraying treatment on the tantalum alloy rolling slab includes, but is not limited to, a high-temperature resistant material such as boron nitride emulsion or a high-temperature resistant water-based ceramic coating.
In the step 2, the asynchronous rolling equipment comprises an upper roller and a lower roller, the linear speed of the upper roller is 1-2 m/s, the linear speed of the lower roller is 1m/s, the rolling speed ratio of 1-2 can be obtained, and the rolling deformation (rolling reduction/pre-rolling thickness) of each pass is 5-50%.
As an optimization, in step 6, the specific rotating direction of the tantalum alloy annealed blank subjected to the rotating treatment is as follows: and rotating by 180 degrees by taking the rolling direction as an axis.
As an optimization, in step 6, the specific rotating direction of the tantalum alloy annealed blank subjected to the rotating treatment is as follows: and rotating 180 degrees by taking the rolling direction as an axis, and rotating 90 degrees by taking an axis perpendicular to the rolling surface direction as an axis.
Compared with the prior art, the invention has the following advantages and beneficial effects:
according to the invention, the shearing deformation characteristic of asynchronous room temperature rolling is utilized to obtain a large-plastic deformation tantalum alloy material, the joule heating effect when high-energy pulse current acts on the metal material is utilized to enable the temperature of the cold deformation tantalum alloy material to rise to over 1000 ℃ in a very short time, and the deformation tantalum alloy is rapidly recrystallized under the action of the current joule heating effect and the electromigration effect, so that the problems of limited grain structure refinement degree, long period, high energy consumption and the like of conventional cold deformation and furnace thermal annealing are solved.
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In order to more clearly illustrate the technical solutions of the exemplary embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and that for those skilled in the art, other related drawings can be obtained from these drawings without inventive effort. In the drawings:
FIG. 1 is a schematic diagram of the asynchronous room temperature rolling and self-resistance heating annealing process in the rapid fine grain preparation method by tantalum alloy rolling deformation composite self-resistance heating annealing according to the present invention;
FIG. 2 is a schematic view of a rotation mode of a tantalum alloy annealed slab before rolling in the tantalum alloy rolling deformation composite self-resistance heating annealing rapid fine grain preparation method of the invention;
fig. 3 is a microstructure of tantalum alloy, a left figure is a microstructure of an original tantalum alloy blank, and a right figure is a microstructure of a tantalum alloy blank prepared by the preparation method of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
The invention discloses a rapid fine grain preparation method by rolling deformation composite self-resistance heating annealing of tantalum alloy, which comprises the following steps:
step 1, obtaining a rectangular coarse-grain tantalum alloy plate;
step 2, carrying out room-temperature asynchronous rolling deformation on the coarse-grain tantalum alloy plate through asynchronous rolling equipment to obtain a tantalum alloy rolling plate blank;
step 3, performing high-temperature anti-oxidation spraying treatment on the tantalum alloy rolling plate blank, and drying the tantalum alloy rolling plate blank for later use;
step 4, carrying out self-resistance heating isothermal annealing treatment on the tantalum alloy rolled plate blank subjected to the anti-oxidation treatment by adopting a high-energy pulse direct-current power supply, rapidly cooling the annealed tantalum alloy rolled plate after the heat preservation time reaches a set time length to obtain a tantalum alloy annealed plate blank, and carrying out surface cleaning inspection on the cooled tantalum alloy rolled plate for later use;
step 5, judging whether rolling is needed to be continued, if so, jumping to step 6, otherwise, jumping to step 7; the judgment of whether the rolling needs to be continued can be carried out according to the cycle number of rolling-heating-annealing-cooling, and the cycle number can be 3-8.
Step 6, performing rotation treatment on the tantalum alloy annealed slab to obtain a tantalum alloy slab, performing room-temperature asynchronous rolling deformation on the tantalum alloy slab through asynchronous rolling equipment to obtain a tantalum alloy rolled slab, and returning to the step 3;
and 7, straightening the tantalum alloy plate blank finally obtained in the step 4 to obtain the tantalum alloy plate blank with uniform and fine grain structure.
In the technical scheme, firstly, a tantalum plate is asynchronously rolled at room temperature to obtain a cold deformation rolling plate blank, and then self-resistance heating recrystallization annealing treatment is carried out on the cold deformation rolling plate blank by applying high-energy pulse current; and (3) obtaining the tantalum alloy plate blank with fine and uniform grain structure by repeating cold rolling and self-resistance heating annealing treatment.
Specifically, example 1 of the present invention is as follows:
fig. 1 is a schematic view showing a flow of asynchronous room temperature rolling and self-resistance heating annealing according to the present invention, and fig. 2 is a schematic view showing a rotation manner of performing rotation processing on the tantalum alloy annealed slab.
The invention discloses a rapid fine grain preparation method by rolling deformation composite self-resistance heating annealing of tantalum alloy, which specifically comprises the following steps:
step (1), machining a coarse-grain tantalum alloy blank (the microstructure is shown in figure 3 (left)) with the brand number of Ta2.5W into a rectangular coarse-grain tantalum alloy plate, wherein the coarse-grain tantalum alloy plate is a rectangular square block with the length, width and height of 100 multiplied by 80 multiplied by 15 mm;
step (2), setting the linear velocity of an upper roller of asynchronous rolling equipment to be 1.5m/s, setting the linear velocity of a lower roller of asynchronous rolling equipment to be 1.0m/s, setting the rolling speed ratio to be 1.5, setting the rolling reduction to be 6mm, setting the corresponding rolling deformation to be 40.0%, thinning the thickness from 15mm to 9mm, carrying out room-temperature asynchronous rolling deformation on the rectangular coarse-grain tantalum alloy plate obtained in the step (1) along the length direction (from left to right or from right to left in figure 1), obtaining a tantalum alloy rolling plate blank, and carrying out surface cleaning inspection for later use;
step (3), carrying out high-temperature anti-oxidation spraying treatment on the tantalum alloy rolling plate blank obtained in the step (2) by using a boron nitride spraying agent, and drying for later use;
step (4), tightly clamping the tantalum alloy plate blank subjected to the anti-oxidation treatment obtained in the step (3) by adopting a tungsten-copper electrode, and then performing current density parameter setting at 24.0A/mm2Annealing at the temperature of 1300 ℃ for 1min under the conditions of 1000Hz and duty ratio of 50%; cooling to room temperature by adopting liquid nitrogen gas injection after annealing to obtain an annealed tantalum alloy plate blank, and carrying out surface cleaning inspection on the annealed tantalum alloy plate blank for later use;
step (5), performing rotation treatment on the annealed tantalum alloy plate blank obtained in the step (4) in a rotation mode of rotating 180 degrees by taking the rolling direction as an axis and rotating 90 degrees by taking the rolling direction as an axis for standby;
step (6), setting the linear velocity of an upper roller of asynchronous rolling equipment to be 1.5m/s, setting the linear velocity of a lower roller of asynchronous rolling equipment to be 1.0m/s, setting the rolling speed ratio to be 1.5, setting the rolling reduction to be 3mm, setting the corresponding rolling deformation to be 33.3%, thinning the thickness from 9mm to 6mm, and carrying out second-pass room-temperature asynchronous rolling on the tantalum alloy plate blank after the rotation of the step (5) to obtain the tantalum alloy rolling plate blank, and carrying out surface cleaning inspection for standby application;
step (7), carrying out high-temperature anti-oxidation spraying treatment on the tantalum alloy rolling plate blank obtained in the step (6) by using a boron nitride spraying agent, and drying for later use;
step (8), tightly clamping the tantalum alloy plate blank subjected to the anti-oxidation treatment and obtained in the step (7) by adopting a tungsten-copper electrode, and then performing current density parameter setting at 22.8A/mm2Annealing at the temperature of 1200 ℃ for 2min under the conditions of 200Hz and 50% duty ratio; cooling to room temperature by adopting liquid nitrogen gas injection after annealing to obtain an annealed tantalum alloy plate blank, and carrying out surface cleaning inspection on the annealed tantalum alloy plate blank for later use;
step (9), performing rotation treatment on the annealed tantalum alloy plate blank obtained in the step (8) in a rotation mode of rotating 180 degrees by taking the rolling direction as an axis for later use;
step (10), setting the linear velocity of an upper roller of asynchronous rolling equipment to be 1.25m/s, setting the linear velocity of a lower roller of asynchronous rolling equipment to be 1.0m/s, setting the rolling speed ratio to be 1.25, setting the rolling reduction to be 2mm, setting the corresponding rolling deformation to be 33.3%, thinning the thickness from 6mm to 4mm, carrying out third-pass room-temperature asynchronous rolling on the tantalum alloy plate blank after the rotation of the step (9) is finished, obtaining the tantalum alloy rolling plate blank, and carrying out surface cleaning inspection for standby application;
step (11), carrying out high-temperature anti-oxidation spraying treatment on the tantalum alloy rolling plate blank obtained in the step (10) by using a boron nitride spraying agent, and drying the tantalum alloy rolling plate blank for later use;
step (12), tightly clamping the tantalum alloy plate blank subjected to the anti-oxidation treatment obtained in the step (11) by adopting a tungsten-copper electrode, and then performing current density parameter setting at 22.8A/mm2Annealing at the temperature of 1200 ℃ for 2min under the conditions of 200Hz and 50% duty ratio; cooling to room temperature by adopting liquid nitrogen gas injection after annealing to obtain an annealed tantalum alloy plate blank, and carrying out annealing on the annealed tantalum alloy plate blankCarrying out surface cleaning inspection for standby;
step (13), performing rotation treatment on the annealed tantalum alloy plate blank obtained in the step (12) in a rotation mode of rotating 180 degrees by taking the rolling direction as an axis for standby;
step (14), setting the linear velocity of an upper roller of asynchronous rolling equipment to be 1.1m/s, setting the linear velocity of a lower roller of asynchronous rolling equipment to be 1.0m/s, setting the rolling speed ratio to be 1.1, setting the rolling reduction to be 1mm, setting the corresponding rolling deformation to be 25.0%, thinning the thickness from 4mm to 3mm, and carrying out fourth-pass room-temperature asynchronous rolling on the tantalum alloy plate blank after the rotation of the step (13) to obtain the tantalum alloy rolling plate blank, and carrying out surface cleaning inspection for standby application;
step (15), carrying out high-temperature anti-oxidation spraying treatment on the tantalum alloy rolling plate blank obtained in the step (14) by using a boron nitride spraying agent, and drying the tantalum alloy rolling plate blank for later use;
step (16), tightly clamping the tantalum alloy plate blank subjected to the anti-oxidation treatment and obtained in the step (15) by adopting a tungsten-copper electrode, and then performing current density parameter setting of 21.8A/mm2Annealing at the temperature of 1100 ℃ for 4min under the conditions of 100Hz and 50% duty ratio; cooling to room temperature by adopting liquid nitrogen gas injection after annealing to obtain an annealed tantalum alloy plate blank, and carrying out surface cleaning inspection on the annealed tantalum alloy plate blank for later use;
and (17) straightening the annealed tantalum alloy plate blank obtained in the step (16) to obtain the tantalum alloy plate blank with uniform and fine grain structure (the microstructure is shown in figure 3 (right)).
Analyzing the metallographic structure and the mechanical property of the tantalum alloy blank obtained in the step (17): the average grain size of the original coarse-grain tantalum billet is refined from 154 mu m to 22 mu m, the structure of the tantalum alloy billet is fine and uniform, and no local coarse-grain structure exists; the yield strength at room temperature is 340 plus or minus 10MPa, the tensile strength is 430 plus or minus 10MPa, and the elongation after fracture is 43 plus or minus 3 percent. The process is summarized as follows: the period of the blank making of the fine-grain tantalum alloy is 1-2 hours, and is shortened by more than 80% compared with the traditional cold deformation and vacuum furnace thermal annealing process.
Embodiment 2, a coarse-grained tantalum alloy plate with different thicknesses is prepared, the preparation process is the same as that in embodiment 1, and the preparation parameters are set according to actual conditions, which are not described herein again.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. A rapid fine grain preparation method of tantalum alloy rolling deformation composite self-resistance heating annealing is characterized by comprising the following steps:
step 1, obtaining a rectangular coarse-grain tantalum alloy plate;
step 2, carrying out room-temperature asynchronous rolling deformation on the coarse-grain tantalum alloy plate through asynchronous rolling equipment to obtain a tantalum alloy rolling plate blank;
step 3, performing high-temperature anti-oxidation spraying treatment on the tantalum alloy rolling plate blank, and drying the tantalum alloy rolling plate blank for later use;
step 4, carrying out self-resistance heating isothermal annealing treatment on the tantalum alloy rolling plate blank subjected to the anti-oxidation treatment by adopting a high-energy pulse direct-current power supply, and quickly cooling the annealed tantalum alloy rolling plate after the heat preservation time reaches a set time length to obtain a tantalum alloy annealing plate blank;
step 5, judging whether rolling is needed to be continued, if so, jumping to step 6, otherwise, jumping to step 7;
step 6, performing rotation treatment on the tantalum alloy annealed slab to obtain a tantalum alloy slab, performing room-temperature asynchronous rolling deformation on the tantalum alloy slab through asynchronous rolling equipment to obtain a tantalum alloy rolled slab, and returning to the step 3;
and 7, straightening the tantalum alloy plate blank finally obtained in the step 5 to obtain the tantalum alloy plate blank with uniform and fine grain structure.
2. The method for preparing the tantalum alloy rolled deformation composite self-resistance heating annealing fast fine crystals according to the claim 1, wherein the method for obtaining the rectangular coarse crystal tantalum alloy plate material in the step 1 comprises the following steps: the coarse-grain tantalum alloy blank is manufactured by adopting a machining mode, and the thickness of the coarse-grain tantalum alloy plate is not more than 20 mm.
3. The method for preparing tantalum alloy rolled deformation composite self-resistance heating annealing rapid fine crystals according to claim 1, wherein in the step 2 and the step 6, after the tantalum alloy rolled slab is obtained, the surface of the tantalum alloy rolled slab needs to be cleaned.
4. The method for preparing the tantalum alloy rolled deformation composite self-resistance heating annealing fast fine grains according to the claim 1, wherein in the step 4, the specific steps of carrying out the self-resistance heating isothermal annealing treatment by adopting the high-energy pulse direct current power supply are as follows:
step 4.1, clamping two ends of the tantalum alloy rolling plate blank subjected to the anti-oxidation treatment through electrodes respectively, and meanwhile, connecting the two electrodes with the positive electrode and the negative electrode of the high-energy pulse direct-current power supply through leads respectively to form a current heating loop;
and 4.2, setting parameters of the high-energy pulse direct-current power supply, turning on a switch of the high-energy pulse direct-current power supply, and electrifying and heating the tantalum alloy rolling plate blank.
5. The method for preparing rapid fine crystals by rolling deformation and self-resistance heating annealing of tantalum alloys according to claim 4, wherein the average current density parameters of self-resistance heating of the high-energy pulse direct-current power supply are as follows: 18 to 24A/mm2The current pulse frequency range is 100-3000 Hz, and the current duty ratio range is 1-100%.
6. The method for preparing rapid fine crystals by rolling deformation and self-resistance heating annealing of tantalum alloy according to claim 1, wherein in the step 4, the specific way for rapidly cooling the annealed tantalum alloy rolled plate is as follows: and rapidly cooling the annealed tantalum alloy rolled plate by adopting a liquid nitrogen gas injection mode.
7. The method for preparing rapid fine crystals by rolling deformation and self-resistance heating annealing of tantalum alloy according to claim 1, wherein in the step 3, the spraying agent for performing the high-temperature anti-oxidation spraying treatment on the rolling plate blank of tantalum alloy comprises but is not limited to boron nitride emulsion or high-temperature resistant water-based ceramic paint.
8. The method for preparing tantalum alloy rolled deformation composite self-resistance heating annealing fast fine crystals according to claim 1, wherein in the step 2 and the step 6, the asynchronous rolling equipment comprises an upper roller and a lower roller, the linear speed of the upper roller is 1 m/s-2 m/s, the linear speed of the lower roller is 1m/s, and the rolling deformation of each pass is 5% -50%.
9. The method for preparing the tantalum alloy rolled deformation composite self-resistance heating annealing rapid fine crystals according to any one of the claims 1, wherein in the step 6, the specific rotating direction for carrying out the rotating treatment on the tantalum alloy annealed plate blank is as follows: rotated 180 degrees with the rolling direction as the axis.
10. The method for preparing rapid fine crystals by rolling deformation and self-resistance heating annealing of tantalum alloy according to claim 1, wherein in the step 6, the specific rotating direction for rotating the tantalum alloy annealed plate blank is as follows: the rolling direction is taken as an axis to rotate 180 degrees, and the axial line perpendicular to the rolling surface direction is taken as an axis to rotate 90 degrees.
CN202111554190.8A 2021-12-17 2021-12-17 Rapid fine grain preparation method by rolling deformation composite self-resistance heating annealing of tantalum alloy Pending CN114231870A (en)

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Cited By (1)

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CN117531833A (en) * 2024-01-10 2024-02-09 太原理工大学 Pulse current assisted rolling compounding method for magnesium/titanium composite plate with large thickness ratio

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Application publication date: 20220325