CN115233072A - Ti-V-Zr-Nb-Al-Ta-Hf light high-strength high-entropy alloy and preparation method thereof - Google Patents
Ti-V-Zr-Nb-Al-Ta-Hf light high-strength high-entropy alloy and preparation method thereof Download PDFInfo
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Abstract
The invention provides a Ti-V-Zr-Nb-Al-Ta-Hf light high-strength high-entropy alloy and a preparation method thereof, wherein the general formula of the light high-strength high-entropy alloy is Ti a V b Zr c Nb d Al e Ta f Hf g Wherein a, b, c, d, e, f and g are molar ratios, a is more than or equal to 3.0 and less than or equal to 4.0, b is more than or equal to 0.5 and less than or equal to 1.5, c is more than or equal to 0.5 and less than or equal to 1.0, d is more than or equal to 0 and less than or equal to 1.0, e is more than or equal to 0 and less than or equal to 1.0, f is more than or equal to 0 and less than or equal to 0.5, and d, e, f and g are not 0 simultaneously. The invention also discloses a preparation method of the light high-strength high-entropy alloy. The light-weight high-strength high-entropy alloy has the low density of the traditional light-weight alloy and the high strength of materials such as steel, does not need a complex heat treatment process and a deformation strengthening process, and has excellent oxidation resistance.
Description
Technical Field
The invention relates to an alloy technology, in particular to a Ti-V-Zr-Nb-Al-Ta-Hf light high-strength high-entropy alloy and a preparation method thereof.
Background
The high-temperature alloy parts currently used in the aerospace field are continuously and rapidly developed towards large, complex and thin-walled directions, so that the requirements on the overall quality and comprehensive mechanical properties of the material are more strict, the material is generally required to have both low density and good mechanical properties, and even special properties such as high-temperature oxidation resistance, corrosion resistance and the like under extreme conditions are required, so that the development of casting high-temperature alloys is provided with opportunity and challenges are provided. The existing common light alloy materials such as magnesium alloy, aluminum alloy and the like have low density but low strength, and are difficult to be used as high-temperature parts in the aerospace field. The nickel-based alloy is widely applied to aerospace engines by virtue of excellent high-temperature mechanical properties, but the mass of the aircraft is increased due to the high density of the nickel-based alloy, and the flying speed of the aircraft is limited. Part of high-temperature titanium alloy can have two performances, but the limit service temperature is still limited within 600 ℃, and the bottleneck of development is difficult to break through by depending on the design idea of the traditional alloy. The invention utilizes the concept of common reinforcement of multiple principal elements of the high-entropy alloy to realize high entropy of the titanium alloy. The alloy which has low density and high strength and can work under complex working conditions is developed, and the alloy has important significance for the development of the fields of aerospace and the like.
Disclosure of Invention
The invention aims to provide a Ti-V-Zr-Nb-Al-Ta-Hf series light high-strength high-entropy alloy aiming at the problems that the yield strength of the traditional light alloy is low and the density of steel or nickel-based alloy is high, wherein the alloy has the low density of the traditional light alloy and the high strength of materials such as steel, and the like, and the excellent performance is obtained without complex heat treatment process and deformation strengthening process and has excellent oxidation resistance.
In order to realize the purpose, the invention adopts the technical scheme that: ti-V-Zr-Nb-Al-Ta-Hf light high-strength high-entropy alloy with general formula of Ti a V b Zr c Nb d Al e Ta f Hf g Wherein a, b, c, d, e, f and g are molar ratios, a is more than or equal to 3.0 and less than or equal to 4.0, b is more than or equal to 0.5 and less than or equal to 1.5, c is more than or equal to 0.5 and less than or equal to 1.0, d is more than or equal to 0 and less than or equal to 1.0, e is more than or equal to 0 and less than or equal to 1.0, f is more than or equal to 0 and less than or equal to 0.5, and d, e, f and g are not 0 at the same time.
Furthermore, a is more than or equal to 3.4 and less than or equal to 3.8, b is more than or equal to 1.0 and less than or equal to 1.5, c is more than or equal to 0.5 and less than or equal to 1.0, d is more than or equal to 0 and less than or equal to 1.0, e is more than or equal to 0 and less than or equal to 1.0, f is more than or equal to 0 and less than or equal to 0.4, g is more than or equal to 0 and less than or equal to 0.4, and d, e, f and g are not 0 at the same time.
Further, the Ti-V-Zr-Nb-Al-Ta-Hf light high-strength high-entropy alloy is of a single-phase BCC structure.
Further, the density of the Ti-V-Zr-Nb-Al-Ta-Hf light high-strength high-entropy alloy is less than 5.5g/cm 3 。
The invention also discloses a preparation method of the light high-strength high-entropy alloy, which comprises the following steps: sequentially stacking Ti, V, zr, nb, al, hf and Ta elements, and then adopting vacuum electromagnetic suspension induction melting or vacuum arc melting to obtain the light high-strength high-entropy alloy.
Furthermore, when the alloy is smelted, raw materials are placed according to the principle that the high melting point is above and the low melting point is below, the Ti, V, al and Zr are placed below, and the Hf, nb and Ta are placed at the top.
Furthermore, in the smelting process, in order to prevent the alloy from being oxidized in the smelting process, the smelting equipment needs to be vacuumized to 5 multiplied by 10 -3 Pa to 3X 10 -3 Pa, then back flushing argon to 0.03 to 0.05MPa.
Further, during vacuum arc melting, the alloy ingot is turned and melted for six to eight times, and the molten state is kept for about 100s each time, so that the components are uniform.
Further, during vacuum electromagnetic suspension induction smelting, the alloy ingot is overturned and smelted for five to six times to ensure that the components are uniform.
Furthermore, the elements of Ti, V, zr, nb, al, ta and Hf all adopt industrial grade pure raw materials with the purity of more than 99.5 wt.%.
The components of the light high-strength high-entropy alloy are verified by phase diagram simulation, and the formula is scientific and reasonable. The preparation method for directly obtaining excellent performance by casting is simple and easy to implement. Compared with the prior art, the light high-strength high-entropy alloy has the following advantages:
1. the light-weight high-strength high-entropy alloy comprises specific element selection and combination, and the concept of high entropy of titanium alloy is adopted, and the density of the alloy is far lower than that of alloys such as steel and the like due to the fact that a large amount of Ti element is added; the addition of a proper amount of Al element can increase the corrosion resistance and the oxidation resistance of the alloy, and the formation of intermetallic compounds can not influence the plasticity of the alloy; the addition of Nb, hf and Ta elements can improve the average melting point of the alloy and increase the lattice distortion of the alloy, thereby improving the room-temperature and high-temperature strength of the alloy.
2. The alloy has excellent mechanical property in an as-cast state, and an ingot obtained under the conditions of vacuum induction melting or vacuum arc melting is of a single-phase BCC structure, and the crystal structure is simple and stable and is easy to study.
3. Compared with nickel-based high-temperature alloy, the light high-strength high-entropy alloy has remarkable density advantage, and the density of the alloy series is 5.5g/cm measured by an Archimedes drainage method 3 And the following.
4. The hardness of the light high-strength high-entropy alloy reaches 360HV in an as-cast state, the tensile yield strength at room temperature is more than 1.2GPa at most, and the ultrahigh yield strength of the alloy far exceeds that of the traditional light alloy after deformation and heat treatment.
5. The elongation after fracture of the light high-strength high-entropy alloy is about 8-16%, and the alloy has better plasticity than a plurality of light high-entropy alloys with complex intermetallic compounds. The specific yield strength is about 220MPa cm 3 ·g -1 . The alloy has excellent strong plastic fit and high specific strength in an as-cast state, far exceeds the prior high-entropy alloy, and has great advantages even compared with the traditional light titanium alloy.
6. The light high-strength high-entropy alloy has excellent oxidation resistance, and oxidation weight gain is less than 1.0mg/cm after 40 hours when the oxidation resistance is tested at the constant temperature of 600 DEG C 2 After the oxidation resistance test is carried out at 700 ℃, the oxidation weight gain is less than 10mg/cm after 40 hours 2 . The oxidation resistance is reduced at 800 ℃, but the good oxidation resistance is still kept.
7. The light high-strength high-entropy alloy is insensitive to component proportion, the influence of micro change of the component proportion on the overall performance of the alloy is small, the preparation method of the alloy is simple, and the alloy can be prepared by adopting conventional vacuum arc melting or vacuum electromagnetic suspension induction melting. The alloy can have excellent mechanical properties without any heat treatment process and deformation strengthening process, and has great potential for continuously improving the properties through subsequent processes.
In conclusion, the light-weight high-strength high-entropy alloy has the low density of the traditional light-weight alloy and the high strength of materials such as steel, does not need a complex heat treatment process and a deformation strengthening process, and has excellent oxidation resistance. The preparation process is simple and economical, and has wide application prospect in the fields of aerospace and the like.
Drawings
FIG. 1 shows as-cast Ti of example 1 3.6 V 1.2 Zr 0.8 XRD diffraction analysis diagram of Nb lightweight high-strength high-entropy alloy;
FIG. 2 shows as-cast Ti of example 1 3.6 V 1.2 Zr 0.8 A tensile true stress-true strain curve of the Nb lightweight high-strength high-entropy alloy measured at room temperature;
FIG. 3 shows as-cast Ti of example 1 3.6 V 1.2 Zr 0.8 An oxidation weight gain curve of the Nb lightweight high-strength high-entropy alloy at the constant temperature of 600 ℃,700 ℃ and 800 ℃;
FIG. 4 shows as-cast Ti of example 2 3.6 V 1.2 Zr 0.8 NbAl 0.6 XRD diffraction analysis of light high-strength high-entropy alloyAnalyzing the graph;
FIG. 5 shows as-cast Ti of example 2 3.6 V 1.2 Zr 0.8 NbAl 0.6 A tensile true stress-true strain curve of the light high-strength high-entropy alloy measured at room temperature;
FIG. 6 shows as-cast Ti of example 2 3.6 V 1.2 Zr 0.8 NbAl 0.6 The tensile fracture morphology of the light high-strength high-entropy alloy is 70 times of magnification;
FIG. 7 shows as-cast Ti of example 2 3.6 V 1.2 Zr 0.8 NbAl 0.6 The tensile fracture morphology of the light high-strength high-entropy alloy is 1000 times in magnification;
FIG. 8 shows as-cast Ti of example 2 3.6 V 1.2 Zr 0.8 NbAl 0.6 A microstructure and morphology diagram of the light high-strength high-entropy alloy;
FIG. 9 shows as-cast Ti of example 2 3.6 V 1.2 Zr 0.8 NbAl 0.6 The oxidation weight gain curve of the light high-strength high-entropy alloy at the constant temperature of 600 ℃,700 ℃ and 800 ℃;
FIG. 10 shows as-cast Ti of example 3 3.6 V 1.2 Zr 0.8 Nb 0.6 Al 0.6 XRD diffraction analysis chart of light high-strength high-entropy alloy;
FIG. 11 shows as-cast Ti of example 3 3.6 V 1.2 Zr 0.8 Nb 0.6 Al 0.6 A tensile true stress-true strain curve of the light high-strength high-entropy alloy measured at room temperature;
FIG. 12 shows as-cast Ti of example 3 3.6 V 1.2 Zr 0.8 Nb 0.6 Al 0.6 The tensile fracture morphology of the light high-strength high-entropy alloy is 70 times of magnification;
FIG. 13 shows as-cast Ti of example 3 3.6 V 1.2 Zr 0.8 Nb 0.6 Al 0.6 The tensile fracture morphology of the light high-strength high-entropy alloy is 1000 times in magnification;
FIG. 14 shows as-cast Ti of example 3 3.6 V 1.2 Zr 0.8 Nb 0.6 Al 0.6 A microstructure topography of the light high-strength high-entropy alloy;
FIG. 15 shows a schematic view ofEXAMPLE 4 As-cast Ti 3.6 V 1.2 Zr 0.8 Nb 0.2 Al 0.6 Ta 0.2 Hf 0.2 XRD diffraction analysis chart of light high-strength high-entropy alloy;
FIG. 16 shows as-cast Ti of example 4 3.6 V 1.2 Zr 0.8 Nb 0.2 Al 0.6 Ta 0.2 Hf 0.2 A tensile true stress-true strain curve of the light high-strength high-entropy alloy measured at room temperature;
FIG. 17 shows as-cast Ti of example 4 3.6 V 1.2 Zr 0.8 Nb 0.2 Al 0.6 Ta 0.2 Hf 0.2 The oxidation weight gain curve of the light high-strength high-entropy alloy at the constant temperature of 600 ℃,700 ℃ and 800 ℃;
FIG. 18 shows as-cast Ti of example 4 3.6 V 1.2 Zr 0.8 Nb 0.2 Al 0.6 Ta 0.2 Hf 0.2 The light high-strength high-entropy alloy has the surface oxide layer appearance after being kept at the constant temperature of 600 ℃ for 20 hours;
FIG. 19 shows as-cast Ti of example 4 3.6 V 1.2 Zr 0.8 Nb 0.2 Al 0.6 Ta 0.2 Hf 0.2 The light high-strength high-entropy alloy has the surface oxide layer appearance after being kept at the constant temperature of 800 ℃ for 20 hours.
Detailed Description
The invention is further illustrated by the following examples:
example 1
This example discloses a Ti a V b Zr c Nb d Al e Ta f Hf g A light high-strength high-entropy alloy with the general formula of Ti 3.6 V 1.2 Zr 0.8 Nb, and Al, ta, and Hf elements are not present in the composition.
Ti 3.6 V 1.2 Zr 0.8 The specific preparation method of Nb is as follows: stacking raw materials Ti, V, zr and Nb in sequence according to a molar ratio shown in a general formula, wherein the proportion of Ti element is higher, zr, V and Nb are selected, and all elements are selected from industrial grade pure raw materials with the purity of more than 99.5 wt%. Then vacuum arc melting or vacuum electromagnetic suspension induction melting is adopted, when the alloy is melted and matched, the Ti, V and Zr are put below, and the Nb is put at the mostVacuum-pumping to 5 × 10 -3 Pa, then back flushing argon to 0.05MPa. And during arc melting, each alloy ingot is melted for at least six times so as to ensure uniform components.
FIG. 1 is an XRD diffraction analysis chart of the as-cast lightweight high-strength high-entropy alloy of example 1, which proves that the alloy shows the crystal structure of single-phase BCC in the as-cast state. FIG. 2 is a tensile true stress-true strain curve of the as-cast lightweight high-strength high-entropy alloy of example 1 at room temperature, with a yield strength of about 780MPa and a tensile plasticity of about 10%. FIG. 3 is an oxidation weight gain curve at 600 deg.C, 700 deg.C, 800 deg.C of the as-cast lightweight high-strength high-entropy alloy of example 1, wherein the constant temperature weight gain at 600 deg.C is less than 1.0mg/cm during the long-time oxidation process of 40 hours 2 The weight gain at the constant temperature of 700 ℃ is about 10mg/cm 2 The weight gain at constant temperature of 800 ℃ is about 40mg/cm 2 。
Example 2
This example discloses a light weight, high strength and high entropy alloy with general formula of Ti 3.6 V 1.2 Zr 0.8 NbAl 0.6 . The preparation method of the light-weight high-strength high-entropy alloy is the same as that of the embodiment 1.
In this example, al is added to the alloy in comparison with example 1, but the amount of Al added is not so high as to prevent the formation of intermetallic compounds and to lower the mechanical properties. The addition of Al element can reduce the overall density of the alloy and improve the oxidation resistance of the alloy, and can increase the lattice distortion and improve the strength of the alloy.
As shown in FIG. 4, the alloys described in this example and example 1 both have a single-phase BCC structure in the as-cast state, and the addition of Al does not change the crystal structure type of the alloy. FIG. 5 is a room temperature tensile true stress-true strain curve for example 2. Compared with example 1, the yield strength of example 2 is about 950MPa, the elongation after fracture exceeds 10 percent, and the density is reduced to 5.4g/cm 3 . FIGS. 6 and 7 show the macro and micro morphology of the tensile fracture of example 2, wherein the macro surface of the fracture is dark gray, and a large number of dimples are present on the micro surface. It can be judged from the microstructure morphology of fig. 8 that the as-cast alloy has component segregation, and the EDS result shows that this segregation is Zr element segregation. Ti (titanium) 3.6 V 1.2 Zr 0.8 NbAl 0.6 The alloy exhibits Ti in comparative example 1 3.6 V 1.2 Zr 0.8 The Nb alloy has more excellent oxidation resistance, and as shown in figure 9, the Nb alloy hardly increases the weight before and after the heat preservation for 40 hours at 600 ℃, and the oxidation resistance performance at 700 ℃ and 800 ℃ is better than that of the example 1.
Example 3
This example discloses a light-weight, high-strength, high-entropy alloy with general formula of Ti 3.6 V 1.2 Zr 0.8 Nb 0.6 Al 0.6 . The preparation method of the light-weight high-strength high-entropy alloy is the same as that of the embodiment 1.
Compared with the embodiment 1, the embodiment not only adds Al element, but also reduces the proportion of Nb, and reduces the alloy density to 5.2g/cm 3 。
Fig. 10 shows the change of Nb element in the system, which still presents a single-phase BCC structure. FIG. 11 is a room temperature tensile curve of the alloy of example 3, wherein the yield strength of the alloy of example 3 is improved to approximately 1.0GPa as the Nb element is reduced compared with the alloys of examples 1 and 2. The fracture morphology of FIGS. 12, 13 reveals Ti 3.6 V 1.2 Zr 0.8 Nb 0.6 Al 0.6 Severe necking of the alloy, but good plasticity of the alloy is reflected from the sides. The microstructure diagram of fig. 14 shows typical characteristic dendrites of the cast alloy, illustrating the presence of compositional segregation in the alloy.
Example 4
This example discloses a light weight, high strength and high entropy alloy with general formula of Ti 3.6 V 1.2 Zr 0.8 Nb 0.2 Al 0.6 Ta 0.2 Hf 0.2 . The preparation method of the light-weight high-strength high-entropy alloy is the same as that of the embodiment 1.
Compared with the embodiment 1, the embodiment adds Al element, reduces the proportion of Nb, and adds proper amount of Hf and Ta elements, thereby further increasing the lattice distortion and improving the overall strength of the alloy, and the alloy density is about 5.5g/cm 3 。
FIG. 15 shows that the Hf and Ta element system still presents a single-phase BCC structure after the Hf and Ta elements are added to the system. FIG. 16 is the room temperature tensile curve of the alloy of example 4,with the reduction of Nb element and the addition of Hf and Ta elements, the yield strength of the alloy is remarkably improved to about 1.2GPa, and the alloy has tensile plasticity of about 15 percent. The combination of strong plasticity far exceeds most of traditional light alloys and light high-entropy alloys. It is worth noting that such excellent mechanical properties can be obtained only in the as-cast state of the alloy. The antioxidant ability thereof was investigated, and FIG. 17 is Ti 3.6 V 1.2 Zr 0.8 Nb 0.2 Al 0.6 Ta 0.2 Hf 0.2 Oxidation weight gain curve of alloy at 600 deg.C, 700 deg.C, 800 deg.C. With Ti in example 2 3.6 V 1.2 Zr 0.8 NbAl 0.6 The alloy is similar, has excellent oxidation resistance at 600 ℃, and has better performance at 700 ℃ and 800 ℃. This patent also discloses Ti 3.6 V 1.2 Zr 0.8 Nb 0.2 Al 0.6 Ta 0.2 Hf 0.2 The appearance of the oxidized surface of the alloy after being oxidized for 20h, fig. 18 is the appearance of the alloy after being oxidized at 600 ℃, and fig. 19 is the appearance of the alloy after being oxidized at 800 ℃, so that the surface is relatively flat after being oxidized at 600 ℃, and the surface has only slight cracks and falls. Compared with the oxide film at 800 ℃, the surface has larger unevenness, but still has a more complete oxide film.
The invention is not limited to the description of the light weight, high strength and high entropy alloy of any of examples 1 to 4. The multi-principal-element high-entropy alloy is different from the traditional alloy taking one element as a base body, and is insensitive to component change in most cases, especially for the single-phase BCC high-entropy alloy, a solid solution is formed by a plurality of elements, and the mechanical property cannot be greatly changed by properly changing the components. The room temperature tensile curves of examples 1-4 support the above statements, and the alloy always maintains excellent mechanical properties with the addition or content change of Al, nb, ta and Hf elements. The unpublished data also show that appropriate changes of elements such as Ti, zr, V and the like are not obvious to change the mechanical properties. Therefore, the content ratio of the elements in the present invention fluctuates within an appropriate range.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A Ti-V-Zr-Nb-Al-Ta-Hf light high-strength high-entropy alloy is characterized in that the general formula is Ti a V b Zr c Nb d Al e Ta f Hf g Wherein a, b, c, d, e, f and g are molar ratios, a is more than or equal to 3.0 and less than or equal to 4.0, b is more than or equal to 0.5 and less than or equal to 1.5, c is more than or equal to 0.5 and less than or equal to 1.0, d is more than or equal to 0 and less than or equal to 1.0, e is more than or equal to 0 and less than or equal to 1.0, f is more than or equal to 0 and less than or equal to 0.5, and d, e, f and g are not 0 at the same time.
2. The Ti-V-Zr-Nb-Al-Ta-Hf based light weight, high strength and high entropy alloy as claimed in claim 1, wherein a is 3.4. Ltoreq. A.ltoreq.3.8, b is 1.0. Ltoreq.1.5, c is 0.5. Ltoreq. C.ltoreq.1.0, d is 0. Ltoreq. D.ltoreq.1.0, e is 0. Ltoreq. F.ltoreq.0.4, g is 0. Ltoreq. G.ltoreq.0.4, and d, e, f and g are not 0 at the same time.
3. The Ti-V-Zr-Nb-Al-Ta-Hf light weight, high strength and high entropy alloy of claim 1, wherein the Ti-V-Zr-Nb-Al-Ta-Hf light weight, high strength and high entropy alloy is a single phase BCC structure.
4. The Ti-V-Zr-Nb-Al-Ta-Hf light weight, high strength and high entropy alloy as claimed in claim 1, wherein the density of the Ti-V-Zr-Nb-Al-Ta-Hf light weight, high strength and high entropy alloy is less than 5.5g/cm 3 。
5. A preparation method of the light-weight high-strength high-entropy alloy as claimed in any one of claims 1 to 4, characterized by comprising the following steps: sequentially stacking Ti, V, zr, nb, al, hf and Ta elements, and then adopting vacuum electromagnetic suspension induction melting or vacuum arc melting to obtain the light high-strength high-entropy alloy.
6. The method for preparing the light-weight, high-strength and high-entropy alloy as claimed in claim 5, wherein the Ti, V, al and Zr are placed below and the Hf, nb and Ta are placed on the top during alloy melting.
7. The method for preparing the light-weight high-strength high-entropy alloy as claimed in claim 5, wherein in the smelting process, the smelting equipment needs to be vacuumized to 5 x 10 -3 Pa to 3X 10 -3 Pa, then back flushing argon to 0.03 to 0.05MPa.
8. The method for preparing the light-weight high-strength high-entropy alloy as claimed in claim 5, wherein during vacuum arc melting, the alloy ingot is turned and melted for six to eight times, and the time of each time of the melting state is kept for about 100s.
9. The preparation method of the light-weight high-strength high-entropy alloy according to claim 5, wherein the alloy ingot is overturned and melted for five to six times during vacuum electromagnetic suspension induction melting.
10. The method for preparing the light-weight high-strength high-entropy alloy according to claim 5, wherein the elements Ti, V, zr, nb, al, ta and Hf are all industrial grade pure raw materials with the purity of more than 99.5 wt.%.
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| CN109666811A (en) * | 2019-01-29 | 2019-04-23 | 大连理工大学 | A kind of radiation resistance high-entropy alloy and preparation method thereof |
| CN111549270A (en) * | 2020-05-22 | 2020-08-18 | 北京工业大学 | Low-density high-strength high-plasticity high-entropy alloy material and preparation method thereof |
| CN113652591A (en) * | 2021-07-22 | 2021-11-16 | 中国科学院金属研究所 | Ti-rich high-entropy alloy with high specific strength, high plasticity and high toughness and preparation thereof |
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