CN109097713B - A kind of Ultra-fine Grained Ta material and preparation method thereof - Google Patents

A kind of Ultra-fine Grained Ta material and preparation method thereof Download PDF

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Publication number
CN109097713B
CN109097713B CN201811144716.3A CN201811144716A CN109097713B CN 109097713 B CN109097713 B CN 109097713B CN 201811144716 A CN201811144716 A CN 201811144716A CN 109097713 B CN109097713 B CN 109097713B
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ultra
fine grained
equal
tantalum
rolling
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CN109097713A (en
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李周
蒋任翔
肖柱
彭智
龚深
张立强
邱文婷
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CHANGSHA NANFANG TANTALUM NIOBIUM Co Ltd
Central South University
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CHANGSHA NANFANG TANTALUM NIOBIUM Co Ltd
Central South University
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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
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making alloys
    • C22C1/02Making alloys by melting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C27/00Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/02Alloys based on vanadium, niobium, or tantalum

Abstract

The present invention relates to a kind of Ultra-fine Grained Ta materials and preparation method thereof.The crystallite dimension of the Ultra-fine Grained Ta material is less than or equal to 3 μm;Its ultimate strength is more than or equal to 410MPa, and yield strength is more than or equal to 300MPa.Preparation method are as follows: electron-beam smelting is carried out to tantalum source, after ingot casting, ingot casting is subjected to jacket under protective atmosphere;Carry out three-dimensional hot forging, cogging total deformation 65-75%, 1150-1250 DEG C of cogging temperature;After cogging, removes jacket and carry out low-high temperature and intersect alternately rolling;Obtain Ultra-fine Grained Ta material.Present invention process is simple, and the Ta band crystal grain of preparation is uniform and very tiny, makes it have advantageous intensity and plasticity and toughness.Designed by of the invention and Ultra-fine Grained Ta band is prepared for high-technology fields such as standby electronics, metallurgy, steel, chemical industry, hard alloy, atomic energy, superconductor technology, automotive electronics, aerospace, health care and scientific researches.

Description

A kind of Ultra-fine Grained Ta material and preparation method thereof
Technical field
The present invention relates to a kind of Ultra-fine Grained Ta materials and preparation method thereof, belong to special material design preparation technical field.
Background technique
Tantalum density is 16.68g/cm3, fusing point is 2980 DEG C, with fusing point is high, steam forces down, cold-forming property is good, chemical A series of excellent properties such as stability is high, anti-liquid metal corrosion ability is strong, surface film oxide dielectric constant is big, in electronics, smelting Gold, steel, chemical industry, hard alloy, atomic energy, superconductor technology, automotive electronics, aerospace, health care and scientific research etc. High-technology field has important application.
With the continuous development of generation information technology industrial technology, in order to meet the needs of deep processing, the crystal grain ruler of tantalum More stringent requirements are proposed for very little and anisotropy, it is desirable that crystal grain is more tiny, and anisotropy is the smaller the better.Depth is plastically deformed skill Art is to prepare the main technique of ultra-fine crystallization metal, is specifically included: Equal Channel Angular Pressing, high-pressure rotary, pack rolling method, wrinkle-straightening Method and sandglass extrusion method etc., principle are plastically deformed by passage, and mutually compressing and cut repeatedly occurs for the crystal grain of material internal Shear strain, crystal grain is chopped under this compression and shear action repeatedly, is gradually refined, in conjunction with heat treatment process appropriate Metal recrystallization temperature and speed are controlled, the crystal grain of Ultra-fine Grained or nano-scale is finally obtained.It is to various depth plasticity below The simple introduction of deformation technology:
A kind of Equal Channel Angular Pressing: metal forming technology for realizing block materials large plastometric set in a manner of pure shear.Sample It vertically is put into mold cavity, is then squeezed out from horizontal type chamber, to complete the extrusion process of a passage, Equal Channel Angular Pressing exists Under conditions of not changing material cross-section product and cross-sectional shape, only by deforming generated shear strain amount for several times with regard to suitable Lower 100:1 even the accumulation strain amount of 1000:1 reduction ratio completed is acted in direct stress.
High-pressure rotary: its working principle is that rub relay and shearing force that sample is generated in high pressure, formed punch high speed rotation Under collective effect, Ultra-fine Grained is made.
Sandglass extrusion method: being repeated extrusion process to block materials in an isometrical mold, obtains material very big Cumulative deformation, while crystal grain gradually refines, to obtain super fine crystal material.
One straightening method of wrinkle: its process principle is press-bending, the straightening between flat anvil in a mold repeatedly, per pass by low-temperature sample Straight sample of secondary bending is turn 90 degrees, and calculates the dependent variable of sample by being bent straight road number.Workpiece is by gear-like Roll rolls torsional deformation, and without drafts, workpiece goes out after roll after obtaining first time deformation into two plain-barreled rolls, by distortion Workpiece carries out straightening in elastic range, and at this moment workpiece obtains second of deformation processing, and it is straight then to carry out second order buckling again, work Part crystal grain under processing repeatedly gradually refines.
Pack rolling method: first, plate, which is superimposed face, will carry out ungrease treatment and the polishing of line brush, be then fed into roll rolling.It rolls When processed not with lubricator, reduction ratio 50%, the plate after rolling overlap again after air-cooled, carry out last process repeatedly, make Very big tired deformation can be obtained by obtaining plate, in conjunction with annealing, obtain Ultra-fine Grained crystal grain.
Process above technology can make metal material obtain Ultra-fine Grained by depth theory of plastic strain in matrix, however therein Equal Channel Angular Pressing, high-pressure rotary, sandglass extrusion method and wrinkle straightening method are generally only applicable to the material processing of small dimension size, And process is very many and diverse, is not suitable for the industrialized production of the Ultrafine High Purity tantalum band of big specification.Although pack rolling method is suitable for big The metal material Ultra-fine Grained of specification is processed, however the metal that tantalum easily reacts with O, H, C as one kind, using pack rolling method It is easy to introduce impurity during pack rolling and seriously affect Ta material performance.Against the above deficiency, present invention employs aximal deformation values Three-dimensional hot forging+ultralow temperature and high temperature aximal deformation value tandem rolling technique prepare Ultra-fine Grained Ta material.Wherein aximal deformation value three Dimension hot forging can make Ta material obtain tiny and homogenization grain structure, and ultralow temperature and high temperature aximal deformation value tandem rolling can To control Ta material texture direction in deformation process, further refinement and homogenization tissue, finally prepare Ultra-fine Grained, ultralow each The Ta material of anisotropy.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of Ultra-fine Grained Ta materials;It has also been put forward for the first time and has been become using big simultaneously Shape amount three-dimensional hot forging+ultralow temperature and high temperature aximal deformation value tandem rolling technique prepare Ultra-fine Grained Ta material.
A kind of Ultra-fine Grained Ta material of the present invention;Its crystallite dimension is less than or equal to 3 μm.
A kind of Ultra-fine Grained Ta material of the present invention;The ultimate strength of the Ultra-fine Grained tantalum material is more than or equal to 410MPa, yield strength More than or equal to 300MPa.
A kind of Ultra-fine Grained Ta material of the present invention;The elongation percentage of the Ultra-fine Grained tantalum material is more than or equal to 50%.
A kind of Ultra-fine Grained Ta material of the present invention;In the Ultra-fine Grained tantalum material, | longitudinal strength-transverse strength |/longitudinal strength * 100% less than or equal to 3%, and | longitudinal strength-transverse strength |/transverse strength * 100% is less than or equal to 3%.
A kind of Ultra-fine Grained Ta material of the present invention;In the Ultra-fine Grained tantalum material, | longitudinal elongation percentage-is laterally extended rate | prolongs/longitudinal direction Rate * 100% is stretched less than or equal to 3%, and | longitudinal elongation percentage-is laterally extended rate |/rate * 100% is laterally extended less than or equal to 3%.
A kind of Ultra-fine Grained Ta material of the present invention, in the Ultra-fine Grained Ta material, the mass percentage of Ta is more than or equal to 99.995%.
A kind of preparation method of Ultra-fine Grained Ta material of the present invention, include the following steps: for tantalum billet to be greater than in condition of high vacuum degree etc. In 10-3It carries out electron-beam smelting under conditions of Pa, after ingot casting, ingot casting is subjected to jacket under protective atmosphere;Carry out three-dimensional hot forging Cogging, cogging total deformation 65-75%, 1150-1250 DEG C of cogging temperature;After cogging, removes jacket and rolled;Surpassed Fine grain Ta material;The rolling includes the following steps:
Step A
Blank is cooling under liquid nitrogen, all after cooling thoroughly, carry out ultralow temperature rolling, the pass deformation of ultralow temperature rolling 45-55%;
Step B
By the tantalum material of ultralow temperature cold rolling, it is heated to 1100-1120 DEG C, with ultralow temperature cold rolling rolling direction at vertical direction Carrying out hot rolling, the pass deformation of hot rolling is 45-55%, preferably 50%.
Step C
It is repeated in step A, B at least 5 times and obtains the tantalum material that crystallite dimension is less than or equal to 3 μm.
A kind of preparation method of Ultra-fine Grained Ta material of the present invention, the temperature of electron-beam smelting are more than or equal to 1300 DEG C, are preferably 1300-1350 DEG C, further preferably 1300-1320 DEG C.
A kind of preparation method of Ultra-fine Grained Ta material of the present invention, the jacket are irony jacket;In the irony jacket, Fe's Content is more than or equal to 99.99wt.%.
A kind of preparation method of Ultra-fine Grained Ta material of the present invention, carries out jacket for ingot casting under protective atmosphere;The protection gas Atmosphere is selected from one of argon gas, nitrogen.
A kind of preparation method of Ultra-fine Grained Ta material of the present invention, is repeated in step A, B at least 5 times and obtains crystallite dimension and be less than Ta material equal to 3 μm.
The temperature of a kind of preparation method of Ultra-fine Grained Ta material of the present invention, the ultralow temperature rolling is -30~-196 DEG C, preferably It is -50~-196 DEG C, further preferably -80~-196 DEG C.
A kind of preparation method of Ultra-fine Grained Ta material of the present invention, the temperature of the hot rolling are 1050-1150 DEG C, are preferably 1100-1150 DEG C, further preferably 1100-1120 DEG C.Heating before hot rolling and in course of hot rolling is under protective atmosphere It carries out.
A kind of preparation method of Ultra-fine Grained Ta material of the present invention, prepared Ta material are Ta band.
The present invention improves the purity and consistency of Ta billet, then in argon gas room to billet by billet high vacuum melting High purity iron jacket, aximal deformation value three-dimensional hot forging refine and homogenize grain structure, pass through ultralow temperature and high temperature large deformation Tandem rolling is measured, further refinement and homogenization tissue, finally prepare Ultra-fine Grained, ultralow anisotropic Ta material.The present invention Tantalum material fine microstructures are uniform, the final target for realizing Ta material high-ductility and less anisotropy.
Designed by of the invention and Ultra-fine Grained Ta band is prepared for standby electronics, metallurgy, steel, chemical industry, hard alloy, atom The high-technology fields such as energy, superconductor technology, automotive electronics, aerospace, health care and scientific research.
The invention has the advantages that: gas can sufficiently be excluded due to 1300 DEG C of smelting temperature or more using vacuum arc melting Body and eutectic refine impurity, purify billet tissue.(including argon gas room) carries out high purity iron jacket under protective atmosphere, prevents jacket Tantalum in the process is oxidized, and in process, jacket also acts as solid lubrication effect, prevents strain cracking.Pass through 3 D stereo Big pass deformation forging, keeps billet Tissue distribution uniform.Although tantalum is bcc metals, but its crisp transition temperature of modeling is low In liquid nitrogen temperature, therefore tantalum can be deformed under this ultralow temperature of liquid nitrogen, and plastic deformation, dislocation are carried out under condition of ultralow temperature Sliding is suppressed, and for deformation mechanism based on shear-deformable, shear deformation is the basis for realizing Ultra-fine Grained, passes through ultralow temperature passage Aximal deformation value cold rolling refines grain structure, is then heated to 1100-1120 DEG C, the perpendicular side with ultralow temperature cold rolling rolling direction To hot rolling, rolling reduction 45-55% is carried out again, this temperature is the temperature of the cold working tissue Recrystallization nucleation of tantalum, due to The deformation for carrying out 50% or so simultaneously, can make what is recrystallized to organize further to refine, and since deflection is big, and tissue is more It is uniform.It is repeated in step A, step B at least 5 times, the tissue of plate is made to be evenly distributed in all directions, anisotropy drop It is low, the tantalum plate that crystallite dimension is not more than 3 μm is obtained, and vertical transverse strength and elongation ratio are no more than 3%.
In conclusion a kind of preparation method of the pure tantalum of Ultra-fine Grained of the present invention, can effectively control tantalum material crystallite dimension and It is uniformly distributed, anisotropy is small, and intensity and plasticity are high.
Detailed description of the invention
Attached drawing 1 is the micro-organization chart of 1 gained tantalum plate of embodiment;
Attached drawing 2 is the micro-organization chart of 2 gained tantalum plate of embodiment;
Attached drawing 3 is the micro-organization chart of 1 gained tantalum plate of comparative example.
Specific embodiment
Embodiment 1:
By tantalum billet (purity 99.996%) in vacuum degree 10-4Electron-beam smelting is carried out under conditions of Pa, and (smelting temperature is 1310 DEG C), after ingot casting, ingot casting is subjected to high purity iron jacket in argon gas room;Carry out three-dimensional hot forging, cogging total deformation 75%, 1200 DEG C of cogging temperature.Tantalum ingot after cogging is removed into surface high purity iron jacket, by the billet of hammer cogging under liquid nitrogen It is cooling, all after cooling thoroughly, carry out ultralow temperature rolling (temperature of low temperature cold rolling is -80~-100 DEG C), pass deformation 50%. By the tantalum plate of ultralow temperature cold rolling 50%, 1100 DEG C are heated to, the direction vertical with ultralow temperature cold rolling rolling direction carries out heat herein Roll (temperature of hot rolling is 1100-1120 DEG C), rolling reduction 50%.It is repeated in step A, step B to 7;Obtain tantalum plate Microstructure as shown in Figure 1,2.1 μm of average grain size, performance: ultimate strength 425MPa, yield strength 338MPa prolong Rate 53% is stretched, the intensity of vertical and horizontal and the ratio of elongation are respectively 2.3% and 2.8%.
Embodiment 2:
By tantalum billet (purity 99.997%) in vacuum degree 10-4Electron-beam smelting is carried out under conditions of Pa, and (smelting temperature is 1305 DEG C), after ingot casting, ingot casting is subjected to high purity iron jacket in argon gas room;Carry out three-dimensional hot forging, cogging total deformation 70%, 1100 DEG C of cogging temperature.Tantalum ingot after cogging is removed into surface high purity iron jacket, by the billet of hammer cogging under liquid nitrogen It is cooling, all after cooling thoroughly, carry out ultralow temperature rolling (temperature of low temperature cold rolling is -100~-136 DEG C), pass deformation 50%.By the tantalum plate of ultralow temperature cold rolling 50%, be heated to 1100 DEG C, the direction vertical with ultralow temperature cold rolling rolling direction herein into Row hot rolling (temperature of hot rolling is 1100-1120 DEG C), rolling reduction 50%.It is repeated in step A, B6 times, obtains tantalum plate Microstructure is as shown in Fig. 2, 2.29 μm of its average grain size, performance: ultimate strength 406MPa, yield strength 313MPa, Elongation percentage 50%, the intensity of vertical and horizontal and the ratio of elongation are respectively 2.6% and 2.9%.Typical microstructure is such as Fig. 2.
Comparative example 1
By tantalum billet (purity 99.995%) in vacuum degree 10-4Electron-beam smelting is carried out under conditions of Pa, and (smelting temperature is 1310 DEG C), after ingot casting, ingot casting is subjected to high purity iron jacket in argon gas room;Carry out three-dimensional hot forging, cogging total deformation 70%, 1100 DEG C of cogging temperature.Tantalum ingot after cogging is removed into surface high purity iron jacket, the billet of hammer cogging is subjected to room temperature Rolling, pass deformation 50%.By the tantalum plate of cold rolling 50%, 1100 DEG C are heated to, the direction vertical with room temperature rolling direction is again Secondary progress hot rolling (temperature of hot rolling is 1100-1120 DEG C), rolling reduction 50%.It is repeated in above-mentioned hot-rolled and cold-rolled 6 times, obtains To tantalum plate microstructure as shown in figure 3,5.02 μm of average time size, performance: ultimate strength 395MPa, yield strength 291MPa, elongation percentage 46%, the intensity of the vertical and horizontal of the intensity and elongation of vertical and horizontal and the ratio point of elongation It Wei 2.8% and 2.9%.

Claims (9)

1. a kind of Ultra-fine Grained Ta material;It is characterized by: the crystallite dimension of the Ultra-fine Grained Ta material is less than or equal to 3 μm;It is described ultra-fine Brilliant Ta material is prepared by following step:
Tantalum billet is more than or equal to 10 in condition of high vacuum degree-3Electron-beam smelting is carried out under conditions of Pa, after ingot casting, under protective atmosphere Ingot casting is subjected to jacket;Carry out three-dimensional hot forging, cogging total deformation 65-75%, 1150-1250 DEG C of cogging temperature;Cogging Afterwards, it removes jacket and is rolled;Obtain Ultra-fine Grained Ta material;The rolling includes the following steps:
Step A
Blank is cooling under liquid nitrogen, all after cooling thoroughly, carry out ultralow temperature rolling, the pass deformation 40- of ultralow temperature rolling 60%;
Step B
By the tantalum material of ultralow temperature cold rolling, it is heated to 1100-1120 DEG C, is carried out with ultralow temperature cold rolling rolling direction at vertical direction Hot rolling, the pass deformation of hot rolling are 40-60%;
Step C
Step A, B is repeated until obtaining the tantalum material that crystallite dimension is less than or equal to 3 μm.
2. a kind of Ultra-fine Grained Ta material according to claim 1;It is characterized by: the ultimate strength of the Ultra-fine Grained tantalum material is big In being equal to 410MPa, yield strength is more than or equal to 300MPa.
3. a kind of Ultra-fine Grained Ta material according to claim 1;It is characterized by: the elongation percentage of the Ultra-fine Grained tantalum material is greater than Equal to 50%.
4. a kind of Ultra-fine Grained Ta material according to claim 1;It is characterized by: in the Ultra-fine Grained tantalum material, | it is longitudinal strong Degree-transverse strength |/longitudinal strength * 100% be less than or equal to 3%, and | longitudinal strength-transverse strength |/transverse strength * 100% is small In equal to 3%.
5. a kind of Ultra-fine Grained Ta material according to claim 1;It is characterized by: in the Ultra-fine Grained tantalum material, | it is longitudinal to extend Rate-is laterally extended rate | and/longitudinal elongation percentage * 100% is less than or equal to 3%, and | longitudinal elongation percentage-is laterally extended rate |/be laterally extended Rate * 100% is less than or equal to 3%.
6. a kind of Ultra-fine Grained Ta material according to claim 1;It is characterized by: in the Ultra-fine Grained Ta material, the quality of Ta Percentage composition is more than or equal to 99.995%.
7. a kind of Ultra-fine Grained Ta material according to claim 1, it is characterised in that: the temperature of electron-beam smelting is more than or equal to 1300℃。
8. a kind of Ultra-fine Grained Ta material according to claim 1, it is characterised in that: wrap ingot casting under protective atmosphere Set;The jacket is irony jacket;In the irony jacket, the content of Fe is more than or equal to 99.99wt%;The protective atmosphere choosing From one of argon gas, nitrogen.
9. a kind of Ultra-fine Grained Ta material according to claim 1, it is characterised in that: be repeated in step A, B at least 5 times and obtain Crystallite dimension is less than or equal to 3 μm of tantalum material.
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CN110735068B (en) * 2019-11-21 2020-08-11 中南大学 Preparation method and application of cobalt-tantalum-zirconium alloy target
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US6348113B1 (en) * 1998-11-25 2002-02-19 Cabot Corporation High purity tantalum, products containing the same, and methods of making the same
CN104451567B (en) * 2014-12-29 2017-11-10 宁夏东方钽业股份有限公司 A kind of tantalum target and preparation method thereof
US10655214B2 (en) * 2015-04-10 2020-05-19 Tosoh Smd, Inc. Method of making a tantalum sputter target and sputter targets made thereby
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