CN116497257A - Light high-strength multi-component refractory alloy with ultrahigh room temperature tensile ductility and preparation method thereof - Google Patents
Light high-strength multi-component refractory alloy with ultrahigh room temperature tensile ductility and preparation method thereof Download PDFInfo
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- 229910000753 refractory alloy Inorganic materials 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 150
- 239000000956 alloy Substances 0.000 claims abstract description 150
- 230000001427 coherent effect Effects 0.000 claims abstract description 6
- 238000003723 Smelting Methods 0.000 claims description 38
- 238000000137 annealing Methods 0.000 claims description 29
- 238000005097 cold rolling Methods 0.000 claims description 20
- 238000005096 rolling process Methods 0.000 claims description 20
- 238000002844 melting Methods 0.000 claims description 14
- 230000008018 melting Effects 0.000 claims description 14
- 229910052758 niobium Inorganic materials 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 229910052715 tantalum Inorganic materials 0.000 claims description 10
- 239000011261 inert gas Substances 0.000 claims description 8
- 229910052726 zirconium Inorganic materials 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 2
- 238000010791 quenching Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000007123 defense Effects 0.000 abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 24
- 238000005520 cutting process Methods 0.000 description 13
- 229910052786 argon Inorganic materials 0.000 description 12
- 239000010453 quartz Substances 0.000 description 12
- 239000002994 raw material Substances 0.000 description 12
- 238000007789 sealing Methods 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 239000002245 particle Substances 0.000 description 9
- 210000001519 tissue Anatomy 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 238000013461 design Methods 0.000 description 6
- 238000005498 polishing Methods 0.000 description 6
- 230000001681 protective effect Effects 0.000 description 6
- 238000009864 tensile test Methods 0.000 description 6
- 241001062472 Stokellia anisodon Species 0.000 description 5
- 238000010891 electric arc Methods 0.000 description 5
- 238000005098 hot rolling Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 210000000988 bone and bone Anatomy 0.000 description 4
- 238000005266 casting Methods 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000001739 density measurement Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
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- 239000000126 substance Substances 0.000 description 3
- 229910000601 superalloy Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
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- 238000009792 diffusion process Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
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- 238000001953 recrystallisation Methods 0.000 description 2
- 238000004098 selected area electron diffraction Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 238000002524 electron diffraction data Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
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- 239000007858 starting material Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
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- 229910052720 vanadium Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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Abstract
The invention discloses a light high-strength multi-component refractory alloy with ultra-high room temperature tensile ductility and a preparation method thereof, wherein the alloy comprises, by atomic percentage, 22.0-38.0% of Nb, 26.0-36.0% of Ti, 23.0-32.0% of Zr, 5.0-10.0% of Al and 2.0-3.5% of Ta; the random state of the alloy is a BCC/B2 coherent structure, wherein the size of B2 is 0.5-2.5 nm. Compared with the existing multi-component refractory alloy, the light high-strength multi-component refractory alloy with ultra-high room temperature tensile ductility, which is prepared by the invention, has lower mass density, higher room temperature tensile ductility and excellent high-temperature softening resistance, and has the potential of serving in high-temperature environments such as aerospace, national defense and military industry and the like.
Description
Technical Field
The invention belongs to the technical field of metal material design and processing, and particularly relates to a light high-strength multi-component refractory alloy with ultrahigh room temperature tensile ductility.
Background
The rapid development of high-precision fields such as aerospace, national defense, military industry, nuclear power and the like puts higher requirements on structural materials serving in high-temperature environments, such as aerospace aircrafts which are served in extreme conditions of ultrahigh temperature and high pressure, use temperatures of more than 1000 ℃, working temperatures of supersonic combustion ramjet engines of more than 2000 ℃ and the like. The service temperature of the existing single crystal nickel-based superalloy with the highest service temperature reaches the limit (1150 ℃), so that the service requirement of a higher temperature environment is difficult to meet, and a structural material capable of being used at a higher temperature is needed to be developed.
The new generation of high-performance structural materials are required to be light and have excellent toughness matching, and the traditional structural materials are often mainly made of one or two metals, so that the simultaneous matching of multiple excellent performances is difficult to achieve. As an innovative alloy design concept, the multi-component alloy breaks through the traditional alloy design category, and provides possibility for exploring ideal performance in a wide combination space. The multicomponent alloy tends to form FCC (face centered cubic) and BCC (body centered cubic) structural solid solution phases after component and process adjustment, but the multicomponent alloy of the FCC structure has better ductility and lower yield strength, while the multicomponent alloy of the BCC structure mainly comprises IV, V, IV subgroup elements Ti, cr, nb, mo, zr, hf, V, ta, W and the like has high yield strength at room temperature and high temperature due to the characteristics of the component elements, and has wide application value and research potential.
The multi-component alloy with the BCC structure has relatively fewer internal sliding systems and sliding directions, lower ductile-brittle transition temperature, larger lattice mismatch and higher stress fluctuation, so that the dislocation movement lattice resistance is higher, and the inherent brittleness is caused. Thus, it remains a challenge to design a multi-component refractory alloy that is lightweight, high strength, and ultra-high room temperature tensile ductility.
Disclosure of Invention
This section is intended to outline some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as well as in the description summary and in the title of the application, to avoid obscuring the purpose of this section, the description summary and the title of the invention, which should not be used to limit the scope of the invention.
The present invention has been made in view of the above and/or problems occurring in the prior art.
One of the objects of the present invention is to provide a lightweight high strength multi-component refractory alloy having ultra-high room temperature tensile ductility.
In order to solve the technical problems, the invention provides the following technical scheme: a light high-strength multi-component refractory alloy with ultrahigh room-temperature stretching ductility comprises,
the alloy comprises 22.0 to 38.0 percent of Nb, 26.0 to 36.0 percent of Ti, 23.0 to 32.0 percent of Zr23.0 to 10.0 percent of Al and 2.0 to 3.5 percent of Ta by atomic percentage;
wherein the sum of the atomic percentages of Nb, ti and Zr is less than or equal to 93.0 percent and more than or equal to 87.5 percent; the sum of the atomic percentages of Al and Ta is less than or equal to 12.5 percent and more than or equal to 7.0 percent; the sum of the atomic percentages of the components is 100 percent;
the random state of the alloy is a BCC/B2 coherent structure, wherein the size of B2 is 0.5-2.5 nm.
As a preferable scheme of the light high-strength multi-component refractory alloy, the invention comprises the following steps: the alloy comprises 24.0-36.5% of Nb, 28.0-34.0% of Ti, 25.0-30.0% of Zr, 6.0-9.0% of Al and 2.5-3.0% of Ta by atomic percentage.
As a preferable scheme of the cast light high-strength multi-component refractory alloy, the invention comprises the following steps: the alloy has the following characteristics:
(a) The density of the alloy is 6.00-6.80 g/cm 3 ；
(b) The tensile yield strength of the multi-component refractory alloy at room temperature is 800-1100 MPa;
(c) The elongation percentage of the multi-component refractory alloy at room temperature is 6.5 to 35.0 percent.
Another object of the present invention is to provide a method for preparing a lightweight high strength multi-component refractory alloy having ultra-high room temperature tensile ductility, comprising,
the alloy is prepared by preparing the components according to the atomic percentage of the alloy, and smelting under the vacuum or inert gas protection condition.
As a preferable scheme of the preparation method of the light high-strength multi-component refractory alloy, the invention comprises the following steps: smelting under the vacuum condition, and maintaining the vacuum degree in the furnace at 1-0.0001 Pa; smelting under the protection of inert gas, charging inert gas and maintaining the gas pressure at 0.000001-0.05 MPa.
The invention also aims to provide a preparation method of the light high-strength multi-component refractory alloy with ultrahigh room temperature tensile ductility, which comprises the steps of directly cold-rolling and annealing the as-cast light high-strength multi-component refractory alloy obtained by the preparation method to obtain the homogeneous alloy with compact structure.
As a preferable scheme of the preparation method of the light high-strength multi-component refractory alloy with the ultra-high room temperature tensile ductility, the invention comprises the following steps: the direct cold rolling is carried out, the multi-pass cold rolling is carried out, the single-pass rolling reduction is less than or equal to 25%, and the total rolling reduction is 40-100%.
As a preferable scheme of the preparation method of the light high-strength multi-component refractory alloy with the ultra-high room temperature tensile ductility, the invention comprises the following steps: and the annealing treatment is carried out under vacuum or inert gas atmosphere, the annealing temperature is 800-1200 ℃, the annealing time is 5-30 min, and then quenching is carried out immediately.
It is another object of the present invention to provide a lightweight high strength multi-component refractory alloy with ultra-high room temperature tensile ductility obtained by the above-described preparation method.
As a preferable scheme of the homogeneous light high-strength multi-component refractory alloy with ultra-high room temperature tensile ductility, the invention comprises the following steps: the alloy has the following characteristics:
(a) The density of the alloy is 6.00-6.80 g/cm 3 ；
(b) The tensile yield strength of the multi-component refractory alloy at room temperature is 800-1200 MPa;
(c) The elongation percentage of the multi-component refractory alloy at room temperature is 15.0-50.0%.
Compared with the prior art, the invention has the following beneficial effects:
the light high-strength multi-component refractory alloy with ultra-high room temperature tensile ductility prepared by the invention presents a BCC/B2 coherent structure, has tensile yield strength of 800-1200 MPa, and realizes tensile elongation of up to 6.5-50.0%; the density is 6.00-6.80 g/cm 3 . Compared with the existing multi-component refractory alloy, the light high-strength multi-component refractory alloy has lower mass density and better toughness matching, and meanwhile, the light high-strength multi-component refractory alloy designed by the patent has excellent high-temperature softening resistance, has the potential of serving in high-temperature environments such as aerospace, national defense and military industry, and is simple in process flow and low in energy consumption and cost.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art. Wherein:
FIG. 1 shows as-cast Nb obtained in example 1 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 Scanning electron microscope tissue map of the alloy.
FIG. 2 shows as-cast Nb obtained in example 1 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 XRD pattern of the alloy.
FIG. 3 is an as-cast Nb obtained in example 1 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 And (3) a transmission electron microscope dark field image and a selected area electron diffraction pattern of the alloy.
FIG. 4 shows as-cast Nb obtained in example 1 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 Tensile engineering stress-engineering strain curve of the alloy.
FIG. 5 shows the obtained homogeneous Nb in example 2 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 Scanning electron microscope tissue map of the alloy.
FIG. 6 shows the obtained homogeneous Nb in example 2 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 The transmission electron diffraction image and the homogeneous transmission electron microscope dark field image of the alloy are selected in an embedded mode.
FIG. 7 shows the obtained homogeneous Nb in example 2 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 Tensile engineering stress-engineering strain curve of the alloy.
FIG. 8 shows the homogeneous Nb obtained in example 3 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 Scanning electron microscope tissue map of the alloy.
FIG. 9 shows the homogeneous Nb obtained in example 3 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 Tensile engineering stress-engineering strain curve of the alloy.
FIG. 10 shows the homogeneous Nb obtained in example 4 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 Scanning electron microscope tissue map of the alloy.
FIG. 11 shows the homogeneous Nb obtained in example 4 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 Tensile engineering stress-engineering strain curve of the alloy.
FIG. 12 is a homogeneous Nb in example 5 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 Scanning electron microscope tissue map of the alloy.
FIG. 13 shows a homogeneous Nb in example 5 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 Tensile engineering stress-engineering strain curve of the alloy.
FIG. 14 shows as-cast Nb obtained in example 6 36.5 Zr 25 Ti 30 Al 6 Ta 2.5 XRD pattern of the alloy.
FIG. 15 shows as-cast Nb obtained in example 6 36.5 Zr 25 Ti 30 Al 6 Ta 2.5 Tensile engineering stress-engineering strain curve of the alloy.
FIG. 16 shows the homogeneous Nb obtained in example 7 36.5 Zr 25 Ti 30 Al 6 Ta 2.5 Scanning electron microscope tissue map of the alloy.
FIG. 17 shows the homogeneous Nb obtained in example 7 36.5 Zr 25 Ti 30 Al 6 Ta 2.5 Tensile engineering stress-engineering strain curve of the alloy.
FIG. 18 is an as-cast Nb obtained in example 8 24 Zr 30 Ti 34 Al 9 Ta 3 XRD pattern of the alloy.
FIG. 19 is an as-cast Nb obtained in example 8 24 Zr 30 Ti 34 Al 9 Ta 3 Tensile engineering stress-engineering strain curve of the alloy.
FIG. 20 shows the homogeneous Nb obtained in example 9 24 Zr 30 Ti 34 Al 9 Ta 3 Scanning electron microscope tissue map of the alloy.
FIG. 21 shows the homogeneous Nb obtained in example 9 24 Zr 30 Ti 34 Al 9 Ta 3 Tensile engineering stress-engineering strain curve of the alloy.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Unless otherwise indicated, all starting materials used in the examples were commercially available.
Example 1
This example relates to a multi-component refractory alloy with light weight, high strength and ultra-high room temperature tensile ductility, having the chemical formula Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 (atomic percent) the preparation steps are as follows:
(1) Pretreatment of raw materials: nb, zr and Ta particles with the purity of more than or equal to 99.90 weight percent and Ti and Al particles with the purity of 99.95 weight percent are put into a beaker of absolute ethyl alcohol to be ultrasonically cleaned for 20 minutes at room temperature so as to remove surface dirt and impurities, and finally are put into a drying box to be dried for standby.
(2) The raw materials are as follows: 38.752g, 17.473g, 35.071g, 2.812g and 5.912g of each metal raw material are respectively weighed according to Nb, ti, zr, al and Ta by converting the mole percentage and the mass percentage of the light high-strength multi-component refractory alloy based on 100g of alloy.
(3) Smelting: according to the melting point, the raw materials weighed in the step (2) are sequentially put into a water-cooled copper crucible of a vacuum arc furnace, al particles with low melting point are put at the bottommost part, and the vacuum is pumped to 5 multiplied by 10 -3 Pa, repeating three times; argon is filled to 0.05MPa as a protective atmosphere; melting additional Ti ingots preset in a hearth for 2min before smelting to consume residual oxygen, nitrogen and the like in a smelting furnace, wherein the smelting current is 320A, and the smelting time is 90 seconds; and (3) starting to smelt the alloy ingot, repeatedly smelting for 6 times, controlling the smelting current to be 380A, and keeping the electric arc for 6 minutes each time and assisting an electromagnetic stirring technology, wherein the current frequency is 8Hz, so that the alloy is fully and uniformly mixed.
(4) Casting: placing the alloy which is uniformly smelted into a water-cooled copper mold with the thickness of 80 multiplied by 30 multiplied by 10mm in a vacuum arc furnace for remelting molding, and taking out a sample after the sample is cooled, wherein the specific operation is as follows: vacuumizing to 5×10 -3 Pa, repeating three times; argon is filled to 0.05MPa as a protective atmosphere; melting additional Ti ingots preset in a hearth for 2min before smelting, wherein the smelting current is 320A, and the smelting time is 90 seconds; and starting to smelt the alloy ingot, repeatedly smelting for 4 times, controlling the smelting current to be 380A, and keeping the electric arc for 8 minutes each time. Obtaining the productTo as-cast Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 And (3) alloy.
The obtained as-cast Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 The scanning electron microscope structure diagram of the alloy is shown in fig. 1, and it can be seen that the as-cast alloy is of a typical dendritic morphology.
Fig. 2 is an XRD pattern of the as-cast alloy obtained in example 1, and fig. 3 is a transmission electron microscope dark field image and a selected area electron diffraction pattern of the as-cast alloy obtained in example 1, and it can be seen that the alloy has a BCC/B2 coherent structure, in which B2 is uniformly dispersed in the alloy, and the size of B2 is 1.2±0.36nm.
For the obtained as-cast Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 The tensile properties of the alloy were tested and FIG. 4 is a tensile engineering stress-engineering strain curve for the as-cast alloy of example 1, which can be seen to have a yield strength of 891MPa and a tensile elongation of 6.9% at room temperature.
For the obtained as-cast Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 The alloy is subjected to density measurement, the alloy is measured by an Archimedes drainage method, firstly, a 5 multiplied by 5mm block sample is uniformly cut from the cast alloy sample, ultrasonic cleaning is carried out for 20 minutes at room temperature before measurement to remove surface dirt and impurities, and finally, the alloy is placed in a drying box for drying; weigh each specimen dry weight M 1 Each sample was weighed 3 times to reduce measurement errors; reweighing the mass M of each sample in water 2 Each sample was weighed 3 times; finally, the density calculation is performed according to the following formula:
wherein ρ is 0 At a water temperature of 0.9982g/cm 3 (20℃)；ρ 1 Is air density of 0.0012g/cm 3 . Average value of ρ= 6.498g/cm obtained by three measurements 3 。
Example 2
For the casting obtained in example 1State Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 The alloy is subjected to cold rolling annealing treatment: cutting the cast alloy into a strip-shaped sample with the thickness of 9.5mm, wherein the rolling amount of a single pass is 10 percent, and the total rolling amount is 80 percent; placing the rolled sample into a quartz tube for sealing, and vacuumizing the quartz tube to 2.5X10 -3 Pa, argon is filled again, and the air pressure in the tube is kept to be 0.025MPa. After sealing, the sample is immediately water quenched after heat preservation for 5min at 850 ℃ to obtain homogeneous Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 And (3) alloy.
Cutting the homogeneous alloy into dog bone shaped tensile test pieces of 1.5X7.5X121 mm by wire cutting, polishing on abrasive paper of No. 180, no. 400, no. 800, no. 1200, no. 2000, no. 3000, no. 5000, ultrasonically cleaning the polished test pieces for 15min, drying, and collecting the test pieces at 1X 10 -3 s -1 Is stretched at the strain rate of (c).
Experimental findings, example 1Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 The light high-strength multi-component refractory alloy can be subjected to large deformation structure regulation and control in an as-cast state, cold rolling deformation amount is up to 80% at room temperature, and then uniform structure is obtained after heat preservation for 5min at 850 ℃.
FIG. 5 shows the obtained homogeneous Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 Scanning electron microscope tissue diagram of alloy; it can be seen that after the cold rolling annealing treatment, the alloy structure is compact and the grain size distribution is uniform.
FIG. 6 shows the obtained homogeneous Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 An electron diffraction pattern and a homogeneous state transmission electron microscope dark field image are selected in the transmission electron microscope bright field image of the alloy; the alloy can be seen to be a BCC/B2 coherent structure, wherein B2 is uniformly dispersed and distributed in the alloy.
FIG. 7 shows the obtained homogeneous Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 The tensile engineering stress-engineering strain curve graph of the alloy shows an ultra-high room temperature tensile elongation of 47.4% and a tensile yield strength of 1021MPa after the tensile annealing treatment.
Example 3
For as-cast Nb obtained in example 1 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 The alloy is subjected to cold rolling annealing treatment: cutting the as-cast alloy into a strip-shaped sample with the thickness of 9mm, wherein the rolling amount of a single pass is 8%, and the total rolling amount is 60%; placing the rolled sample into a quartz tube for sealing, and vacuumizing the quartz tube to 2.5X10 -3 Pa, argon is filled again, and the air pressure in the tube is kept to be 0.025MPa. After sealing, the sample is immediately water quenched after heat preservation for 15min at 1000 ℃ to obtain the homogeneous Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 And (3) alloy.
The test pieces were cut into 1.5X7.5X121 mm dog bone tensile test pieces by wire cutting, polished on No. 180, no. 400, no. 800, no. 1200, no. 2000, no. 3000, no. 5000 sandpaper, ultrasonically cleaned for 20min after polishing, and dried at 1X 10 -3 s -1 Is stretched at the strain rate of (c).
FIG. 8 shows the obtained homogeneous Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 The scanning electron microscope structure diagram of the alloy can show that after cold rolling annealing treatment, the alloy has compact structure, relatively large crystal grains and uniform distribution.
FIG. 9 shows the obtained homogeneous Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 The tensile engineering stress-engineering strain curve of the alloy, after the tensile annealing treatment, exhibited a tensile yield strength of 931MPa and a tensile elongation of 25.2%.
Example 4
For as-cast Nb obtained in example 1 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 The alloy is subjected to cold rolling annealing treatment: cutting the as-cast alloy into a strip-shaped sample with the thickness of 10.0mm, wherein the rolling amount of a single pass is 10% and the total rolling amount is 90%; placing the rolled sample into a quartz tube for sealing, and vacuumizing the quartz tube to 2.5X10 -3 Pa, argon is filled again, and the air pressure in the tube is kept to be 0.025MPa. After sealing, the sample is immediately water quenched after being kept at 800 ℃ for 5min to obtain the homogeneous Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 And (3) alloy.
The test pieces were cut into dog bone-shaped tensile test pieces of 1.0X17.5X121 mm by wire cutting, polished on abrasive paper of No. 180, no. 400, no. 800, no. 1200, no. 2000, no. 3000, no. 5000, ultrasonically cleaned in a beaker for 20min after polishing, dried, and then dried in a beaker of 1X 10 -3 s -1 Is stretched at the strain rate of (c).
FIG. 10 shows the obtained homogeneous Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 The scanning electron microscope structure diagram of the alloy can show that after the cold rolling annealing treatment, the alloy has obvious band-shaped structure and is elongated along the rolling direction.
FIG. 11 shows the obtained homogeneous Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 The tensile engineering stress-engineering strain curve graph of the alloy shows a tensile yield strength of 993MPa and a room temperature tensile elongation of 36.3% after the tensile annealing treatment.
Example 5
For as-cast Nb obtained in example 1 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 The alloy is subjected to cold rolling annealing treatment: cutting the as-cast alloy into a lath-shaped sample with the thickness of 11.0mm, wherein the rolling amount of a single pass is 10 percent, and the total rolling amount is 100 percent; placing the rolled sample into a quartz tube for sealing, and vacuumizing the quartz tube to 2.5X10 -3 Pa, argon is filled again, and the air pressure in the tube is kept to be 0.025MPa. After sealing, the sample is immediately water quenched after being kept at 800 ℃ for 5min to obtain the homogeneous Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 And (3) alloy.
The test pieces were cut into 0.8X7.5X121 mm dog bone tensile test pieces by wire cutting, polished on No. 180, no. 400, no. 800, no. 1200, no. 2000, no. 3000, no. 5000 sandpaper, ultrasonically cleaned in a beaker for 20min after polishing, and dried at 1X 10 -3 s -1 Is stretched at the strain rate of (c).
FIG. 12 shows the obtained homogeneous Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 The scanning electron microscope structure diagram of the alloy can be seen at the cold rolling annealing positionAfter that, the alloy had a large-area distinct band structure, elongated in the rolling direction.
FIG. 13 shows the obtained homogeneous Nb 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 The tensile engineering stress-engineering strain curve graph of the alloy shows a tensile yield strength of 1091MPa and a room temperature tensile elongation of 30.6% after the tensile annealing treatment.
Example 6
The embodiment designs a multi-component refractory alloy with light weight, high strength and ultra-high room temperature tensile ductility, and the chemical formula is Nb 36.5 Zr 25 Ti 30 Al 6 Ta 2.5 (atomic percent) the preparation steps are as follows:
(1) Pretreatment of raw materials: nb, zr and Ta particles with the purity of more than or equal to 99.90 weight percent and Ti and Al particles with the purity of 99.95 weight percent are put into a beaker of absolute ethyl alcohol to be ultrasonically cleaned for 15 minutes at room temperature so as to remove surface dirt and impurities, and finally are put into a drying box to be dried for standby.
(2) The raw materials are as follows: 43.911g, 18.599g, 29.528g, 2.097g and 5.863g of each metal raw material are respectively weighed according to Nb, ti, zr, al and Ta by converting the mole percentage and the mass percentage of the light high-strength multi-component refractory alloy based on 100g of alloy.
(3) Smelting: according to the melting point, the raw materials weighed in the step (2) are sequentially put into a water-cooled copper crucible of a vacuum arc furnace, al particles with low melting point are put at the bottommost part, and the vacuum is pumped to 5 multiplied by 10 -3 Pa, repeating three times; argon is filled to 0.05MPa as a protective atmosphere; additional Ti ingots preset in a hearth are melted for 2min before smelting to further consume free oxygen in the furnace, the smelting current is 330A, and the smelting time is 80 seconds; and (3) starting to smelt the alloy ingot, repeatedly smelting for 6 times, controlling the smelting current to be 380A, and keeping the electric arc for 6 minutes each time and assisting an electromagnetic stirring technology, wherein the current frequency is 8Hz, so that the alloy is fully and uniformly mixed.
(4) Casting: placing the alloy which is evenly smelted into a water-cooled copper mold with the thickness of 80 multiplied by 30 multiplied by 10mm in a vacuum arc furnace for remelting molding, taking out a sample after the sample is cooled,the specific operation is as follows: vacuumizing to 5×10 -3 Pa, repeating three times; argon is filled to 0.05MPa as a protective atmosphere; melting additional Ti ingots preset in a hearth for 2min before smelting, wherein the smelting current is 320A, and the smelting time is 80 seconds; and starting to smelt the alloy ingot, repeatedly smelting for 4 times, controlling the smelting current to be 380A, and keeping the electric arc for 8 minutes each time. Obtaining as-cast Nb 36.5 Zr 25 Ti 30 Al 6 Ta 2.5 And (3) alloy.
FIG. 14 shows the as-cast Nb 36.5 Zr 25 Ti 30 Al 6 Ta 2.5 XRD patterns of the alloy indicate that the alloy has a BCC/B2 structure.
FIG. 15 shows the as-cast Nb 36.5 Zr 25 Ti 30 Al 6 Ta 2.5 The tensile engineering stress-engineering strain curve graph of the alloy shows that the as-cast alloy has a tensile yield strength of 891MPa and a room temperature tensile elongation of 28.9%.
The as-cast Nb obtained was obtained in the same manner as in example 1 36.5 Zr 25 Ti 30 Al 6 Ta 2.5 The alloy is subjected to density measurement, and the average value of the measurement is rho= 6.683g/cm 3 。
Example 7
For as-cast Nb obtained in example 6 36.5 Zr 25 Ti 30 Al 6 Ta 2.5 The alloy is subjected to cold rolling annealing treatment: cutting the as-cast alloy into a lath-shaped sample with the thickness of 8mm, wherein the rolling amount of a single pass is 10 percent, and the total rolling amount is 80 percent; placing the rolled sample into a quartz tube for sealing, and vacuumizing the quartz tube to 2.5X10 -3 Pa, argon is filled again, and the air pressure in the tube is kept to be 0.025MPa. After sealing, the sample is immediately water quenched after heat preservation for 10min at 900 ℃ to obtain homogeneous Nb 36.5 Zr 25 Ti 30 Al 6 Ta 2.5 And (3) alloy.
The test pieces were cut into 1.5X7.5X121 mm dog bone tensile test pieces by wire cutting, polished on No. 180, no. 400, no. 800, no. 1200, no. 2000, no. 3000, no. 5000 sandpaper, ultrasonically cleaned for 20min after polishing, and dried at 1X 10 -3 s -1 Is stretched at the strain rate of (c).
FIG. 16 shows the obtained homogeneous Nb 36.5 Zr 25 Ti 30 Al 6 Ta 2.5 The scanning electron microscope structure diagram of the alloy shows that after cold rolling annealing treatment, the alloy structure is compact and the grain size distribution is uniform.
FIG. 17 shows the obtained homogeneous Nb 36.5 Zr 25 Ti 30 Al 6 Ta 2.5 The tensile engineering stress-engineering strain curve of the alloy, after recrystallization annealing treatment, exhibited a room temperature tensile elongation of 31.3% and a tensile yield strength of 1085 MPa.
Example 8
The embodiment designs a multi-component refractory alloy with light weight, high strength and ultra-high room temperature tensile ductility, and the chemical formula is Nb 24 Zr 30 Ti 34 Al 9 Ta 3 (atomic percent) the preparation steps are as follows:
(1) Pretreatment of raw materials: nb, zr and Ta particles with the purity of more than or equal to 99.90 weight percent and Ti and Al particles with the purity of 99.95 weight percent are put into a beaker of absolute ethyl alcohol to be ultrasonically cleaned for 20 to 25 minutes at room temperature so as to remove surface dirt and impurities, and finally are put into a drying box to be dried for standby.
(2) The raw materials are as follows: 30.208g, 22.066g, 37.078g, 3.293g and 7.361g of each metal raw material are respectively weighed according to Nb, ti, zr, al and Ta by converting the mole percentage and the mass percentage of the light high-strength multi-component refractory alloy based on 100g of alloy.
(3) Smelting: according to the melting point, the raw materials weighed in the step (2) are sequentially put into a water-cooled copper crucible of a vacuum arc furnace, al particles with low melting point are put at the bottommost part, and the vacuum is pumped to 5 multiplied by 10 -3 Pa, repeating three times; argon is filled to 0.05MPa as a protective atmosphere; melting additional Ti ingots preset in a hearth for 2min before smelting to consume residual oxygen, nitrogen and the like in a smelting furnace, wherein the smelting current is 320A, and the smelting time is 80 seconds; the alloy ingot is melted, the melting current is controlled at 380A for 6 times, each melting arc lasts for 6min and is assisted by electromagnetic stirring technology, the current frequency is 8Hz, and the alloy is ensured to be sufficientMixing well.
(4) Casting: placing the alloy which is uniformly smelted into a water-cooled copper mold with the thickness of 80 multiplied by 30 multiplied by 10mm in a vacuum arc furnace for remelting molding, and taking out a sample after the sample is cooled, wherein the specific operation is as follows: vacuumizing to 5×10 -3 Pa, repeating three times; argon is filled to 0.05MPa as a protective atmosphere; melting additional Ti ingots preset in a hearth for 2min before smelting, wherein the smelting current is 320A, and the smelting time is 80 seconds; and starting to smelt the alloy ingot, repeatedly smelting for 4 times, controlling the smelting current to be 380A, and keeping the electric arc for 8 minutes each time. Obtaining as-cast Nb 24 Zr 30 Ti 34 Al 9 Ta 3 And (3) alloy.
FIG. 18 shows the as-cast Nb 24 Zr 30 Ti 34 Al 9 Ta 3 XRD patterns of the alloy indicate that the alloy has a BCC/B2 structure.
FIG. 19 shows the as-cast Nb 24 Zr 30 Ti 34 Al 9 Ta 3 The tensile engineering stress-engineering strain curve graph of the alloy, and the as-cast alloy has a tensile yield strength of 1011MPa and a room temperature tensile elongation of 31.3%.
The as-cast Nb obtained was obtained in the same manner as in example 1 24 Zr 30 Ti 34 Al 9 Ta 3 The alloy is subjected to density measurement, and the average value of the measurement is rho= 6.330g/cm 3 。
Example 9
For as-cast Nb obtained in example 8 24 Zr 30 Ti 34 Al 9 Ta 3 The alloy is subjected to cold rolling annealing treatment: cutting the as-cast alloy into a lath-shaped sample with the thickness of 8mm, wherein the rolling amount of a single pass is 10 percent, and the total rolling amount is 80 percent; placing the rolled sample into a quartz tube for sealing, and vacuumizing the quartz tube to 2.5X10 -3 Pa, argon is filled again, and the air pressure in the tube is kept to be 0.025MPa. After sealing, the sample is immediately water quenched after being heat-preserved for 10min at 850 ℃ to obtain the homogeneous Nb 24 Zr 30 Ti 34 Al 9 Ta 3 And (3) alloy.
The test pieces were cut into dog bone-like tensile test pieces of 1.5X7.5X121 mm by wire cutting, and the test pieces were cut through 180#, 400#, 800#Polishing on No. 1200, no. 2000, no. 3000 and No. 5000 sand paper, ultrasonically cleaning the polished sample for 15min, and drying at 1X 10 -3 s -1 Is stretched at the strain rate of (c).
FIG. 20 shows the obtained homogeneous Nb 24 Zr 30 Ti 34 Al 9 Ta 3 The scanning electron microscope structure diagram of the alloy can show that after cold rolling annealing treatment, the alloy structure is compact and the grain size distribution is uniform;
FIG. 21 shows the obtained homogeneous Nb 24 Zr 30 Ti 34 Al 9 Ta 3 The tensile engineering stress-engineering strain curve of the alloy has room temperature tensile yield strength as high as 1088MPa and 34.4% tensile elongation after recrystallization annealing treatment.
Comparative example 1
For as-cast Nb obtained in example 1 32 Zr 29.5 Ti 28 Al 8 Ta 2.5 Carrying out hot rolling deformation treatment on the alloy: the as-cast alloy was cut into 8mm thick lath-shaped specimens, and the hot rolling temperature was 1050 ℃, the holding time was 30min, the single pass rolling reduction was 10%, and when the hot rolling deformation of the alloy was about 40%, the alloy appeared to crack, so the as-cast alloy of example 1 was not suitable for hot rolling structure control under the condition that the hot rolling temperature was 1050 ℃, and the rolling deformation was 40% when the holding time was 30 min.
The invention realizes that the room temperature tensile elongation of the light high-strength multi-component refractory alloy reaches 30.0-50.0%, has room temperature tensile yield strength of 900-1200 MPa, can realize direct cold rolling-annealing treatment at room temperature to realize tissue regulation, is beneficial to deformation processing, and can realize large-size sample preparation.
The near equimolar ratio of Nb, ti and Zr ensures that the alloy has high solid solubility and improves the yield strength of the alloy; compared with other elements in the alloy system, ta element has higher Young's modulus which is about 3.5 times of Ti element and 7 times of Al, nb and Zr elements, and the solid solution strengthening effect of the alloy is obviously enhanced while the weight is kept to be light by a small amount of addition. Meanwhile, ta has excellent plasticity, corrosion resistance and high-temperature performance, and is beneficial to improving the strength, plasticity and thermal stability of the alloy.
According to the invention, the light-weight element Al is introduced into the multi-component refractory alloy, and the Al element proportion is reasonably selected on the premise of ensuring that the alloy structure is a single-phase solid solution, so that the low-density multi-component refractory alloy is obtained, and the alloy density rho=6.20-6.70 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Meanwhile, the addition of Al element induces the formation of a large amount of ordered phases, and a BCC/B2 structure similar to the gamma/gamma' of the commercial nickel-based superalloy is formed, so that the nickel-based superalloy has great commercial potential.
The invention provides a light high-strength multi-component refractory alloy with ultrahigh room temperature tensile ductility, which takes Nb, ti and Zr refractory elements as main materials, and simultaneously adds oxidizing element Al, so that a compact oxide film or passivation protection layer is easily formed on the surface of the alloy, the diffusion rate of oxygen atoms is blocked preferentially, the high-temperature corrosion resistance of the alloy is obviously improved, and the alloy is expected to become a new generation of high-temperature structural material.
The invention provides a light high-strength multi-component refractory alloy with ultrahigh room temperature tensile ductility, which has uniform structure, can directly carry out large deformation cold rolling to regulate and control the structure without intermediate annealing treatment, has simple process flow and obviously reduces energy consumption and cost.
According to the invention, through designing the proportion of Nb, ti, zr, ta and Al elements, the room-temperature elongation rate is up to 30.0-50.0% in the light high-strength multi-component refractory alloy, and the room-temperature yield strength has the strong-plasticity matching combination of 900-1200 MPa, and the structure regulation and control can be realized through direct cold rolling-short-time annealing treatment at room temperature, so that the deformation processing is facilitated, and the preparation of large-size samples can be realized; the Al element proportion is reasonably selected to obtain the density rho=6.20-6.70 g/cm 3 A light-weight high-strength multi-component refractory alloy; meanwhile, addition of Al induces formation of a large amount of ordered phases to form a BCC/B2 structure, so that the method has great commercial potential; the addition of near-equal atomic ratios of Nb, ti and Zr ensures that the alloy has high solid solubility and improves the yield strength of the alloy; ta has excellent plasticity, corrosion resistance and high temperature performance, and the addition of Ta is beneficial to improving the strength, plasticity and thermal stability of the alloy; at high temperature, al element is easy to form a compact oxide film or passivation protection layer on the surface of the alloy, so that the diffusion rate of oxygen atoms is preferentially blocked, and the high temperature of the alloy is obviously improvedThe corrosion resistance is expected to become a new generation of high temperature structural material.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered in the scope of the claims of the present invention.
Claims (10)
1. A light high-strength multi-component refractory alloy is characterized in that: the alloy comprises 22.0 to 38.0 percent of Nb, 26.0 to 36.0 percent of Ti, 23.0 to 32.0 percent of Zr, 5.0 to 10.0 percent of Al and 2.0 to 3.5 percent of Ta by atom percent;
wherein the sum of the atomic percentages of Nb, ti and Zr is less than or equal to 93.0 percent and more than or equal to 87.5 percent; the sum of the atomic percentages of Al and Ta is less than or equal to 12.5 percent and more than or equal to 7.0 percent; the sum of the atomic percentages of the components is 100 percent;
the random state of the alloy is a BCC/B2 coherent structure, wherein the size of B2 is 0.5-2.5 nm.
2. A lightweight high strength multi-component refractory alloy as set forth in claim 1 wherein: the alloy comprises 24.0-36.5% of Nb, 28.0-34.0% of Ti, 25.0-30.0% of Zr, 6.0-9.0% of Al and 2.5-3.0% of Ta by atomic percentage.
3. The as-cast light-weight high strength multi-component refractory alloy of claim 1 or 2, wherein: the alloy has the following characteristics:
(a) The density of the alloy is 6.00-6.80 g/cm 3 ；
(b) The tensile yield strength of the multi-component refractory alloy at room temperature is 800-1100 MPa;
(c) The elongation percentage of the multi-component refractory alloy at room temperature is 6.5 to 35.0 percent.
4. A preparation method of a light high-strength multi-component refractory alloy is characterized by comprising the following steps of: comprising the steps of (a) a step of,
the alloy according to any one of claims 1 to 3, wherein the alloy is obtained by melting the components in a vacuum or inert gas atmosphere.
5. The method for preparing the light high-strength multi-component refractory alloy according to claim 4, wherein the method comprises the following steps: smelting under the vacuum condition, and maintaining the vacuum degree in the furnace at 1-0.0001 Pa; smelting under the protection of inert gas, charging inert gas and maintaining the gas pressure at 0.000001-0.05 MPa.
6. A preparation method of a light high-strength multi-component refractory alloy with ultrahigh room temperature tensile ductility is characterized by comprising the following steps of: comprising the steps of directly cold-rolling and annealing the cast light high-strength multi-component refractory alloy obtained by the preparation method of claim 4 or 5 to obtain the homogeneous alloy with compact structure.
7. The method for preparing a lightweight high strength multi-component refractory alloy having ultra-high room temperature tensile ductility as claimed in claim 6, wherein: the direct cold rolling is carried out, the multi-pass cold rolling is carried out, the single-pass rolling reduction is less than or equal to 25%, and the total rolling reduction is 40-100%.
8. The method for producing a lightweight high strength multi-component refractory alloy having ultra-high room temperature tensile ductility as claimed in claim 6 or 7, wherein: and the annealing treatment is carried out under vacuum or inert gas atmosphere, the annealing temperature is 800-1200 ℃, the annealing time is 5-30 min, and then quenching is carried out immediately.
9. The homogeneous light-weight high-strength multi-component refractory alloy with ultra-high room temperature tensile ductility obtained by the preparation method according to any one of claims 6 to 8.
10. The homogeneous light weight high strength multi-component refractory alloy having ultra-high room temperature tensile ductility according to claim 9, wherein: the alloy has the following characteristics:
(a) The density of the alloy is 6.00-6.80 g/cm 3 ；
(b) The tensile yield strength of the multi-component refractory alloy at room temperature is 800-1200 MPa;
(c) The elongation percentage of the multi-component refractory alloy at room temperature is 15.0-50.0%.
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