CN115821171A - Trace B element-doped modified high-strength high-plasticity multi-component alloy, and preparation method and application thereof - Google Patents
Trace B element-doped modified high-strength high-plasticity multi-component alloy, and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a trace B element doped modified high-strength high-plasticity multi-component alloy, a preparation method and application thereof, wherein the general formula of the multi-component alloy is Fe a Ni b Cr c Cu d Al e Ti f gB, wherein a, b, c, d, e and f are molar ratios, g is a mass fraction, a is more than or equal to 1.8 and less than or equal to 2.2, b is more than or equal to 0.8 and less than or equal to 1.2, c is more than or equal to 0.3 and less than or equal to 0.6, d is more than or equal to 0.1 and less than or equal to 0.4, e is more than or equal to 0.1 and less than or equal to 0.4, f is more than or equal to 0.1 and less than or equal to 0.3 (molar ratio), and g is more than or equal to 60ppm and less than or equal to 90ppm. The multicomponent alloy is doped with trace B element and then is subjected to simple thermal mechanical treatment, so that the precipitation of a coarse BCC-based Heusler phase at a crystal boundary is inhibited, the formation of a fine BCC-based Heusler phase in the crystal boundary is promoted, the stress concentration is relieved, and the comprehensive mechanical property of the alloy is greatly improved.
Description
Technical Field
The invention relates to a multicomponent alloy technology, in particular to a high-strength high-plasticity multicomponent alloy modified by doping trace B elements, a preparation method and application thereof.
Background
The high-entropy alloy or the multi-component alloy is widely concerned due to the special physical, chemical and mechanical properties of the alloy, and becomes a hotspot of metal alloy research, so as to become a structural and functional integrated material in the future. Although it is composed of 4 or more main elements, it can maintain a single-phase disordered solid solution structure in an as-cast state. Achieving both ultra-high strength and reliable ductility in multicomponent alloys of single face-centered cubic disordered solid solution structure remains a challenge. In order to provide excellent mechanical properties to a multicomponent alloy having a single face-centered cubic structure, it is generally necessary to strengthen a matrix phase having good toughness. Among the various conventional strengthening strategies, precipitation strengthening plays a crucial role, because the slow diffusion property of elements in multicomponent alloys provides unique opportunities for the formation of fine and stable nanoscale precipitation phases, which increase the strength of the alloys to new levels.
Generally, the methods for achieving this aim only focus on adjusting the alloy composition and the thermomechanical processing conditions, which are both cumbersome and costly. In contrast, it remains a great challenge to design a simple and low cost method to optimize the microstructure to achieve the best balance of strength and ductility for multi-component alloys.
Disclosure of Invention
The invention aims to provide a trace B element-doped modified high-strength high-plasticity Fe-Ni-Cr-Cu-Al-Ti-B multi-component alloy and a preparation method thereof, aiming at the problems that the design for improving the comprehensive mechanical property of the alloy is rarely reported by adopting an extremely low-content doping agent to adjust the microstructure at present. In the B-free state, a large amount of coarse BCC-based Heusler hard phases precipitate at grain boundaries of the alloy after thermomechanical treatment, which severely impairs the plasticity of the alloy. By doping the B element with extremely low content, under the same thermal mechanical treatment condition, the precipitation of a coarse hard phase at a grain boundary is inhibited, the formation of a fine BCC-based Heusler phase in the grain boundary is promoted, the stress concentration is relieved, and the comprehensive mechanical property of the alloy is greatly improved. The multicomponent alloy of the system has the characteristics of excellent strong plasticity balance and is expected to be widely applied to industrial production.
In order to realize the purpose, the invention adopts the technical scheme that: a trace B element doped modified high-strength high-plasticity multicomponent alloy with a general formula of Fe a Ni b Cr c Cu d Al e Ti f gB, wherein a, b, c, d, e and f are molar ratios, g is a mass fraction, a is more than or equal to 1.8 and less than or equal to 2.2, b is more than or equal to 0.8 and less than or equal to 1.2, c is more than or equal to 0.3 and less than or equal to 0.6, d is more than or equal to 0.1 and less than or equal to 0.4, e is more than or equal to 0.1 and less than or equal to 0.4,0.1≤f≤0.3、60ppm≤g≤90ppm。
Further, the general formula Fe a Ni b Cr c Cu d Al e Ti f -the gB multicomponent alloy composition satisfies the following condition: a: b: d: f =20:10:2:1, c: e =5:3, and g is more than or equal to 60ppm and less than or equal to 90ppm.
Furthermore, in the general formula, a is more than or equal to 1.9 and less than or equal to 2.1, b is more than or equal to 0.9 and less than or equal to 1.1, c is more than or equal to 0.4 and less than or equal to 0.5, d is more than or equal to 0.1 and less than or equal to 0.2, e is more than or equal to 0.3 and less than or equal to 0.4, f is more than or equal to 0.1 and less than or equal to 0.2, and g is more than or equal to 60ppm and less than or equal to 90ppm.
The invention also discloses a preparation method of the trace B element doped modified high-strength high-plasticity multi-component alloy, which comprises the following steps:
stacking single raw materials of Ni, cr, cu, al, ti and Fe-B intermediate alloy according to the weight ratio, and smelting by using a vacuum arc smelting furnace to obtain a multi-component alloy button ingot; and placing the multi-component alloy button ingot in a vacuum heat treatment furnace, carrying out homogenization heat treatment, and then sequentially carrying out large-deformation cold rolling and high-temperature aging heat treatment to obtain the trace B element-doped modified high-strength high-plasticity multi-component alloy.
Further, the purity of the selected metal simple substance raw materials, namely Ni, cr, cu, al and Ti, is more than or equal to 99.95 wt%; the purity of the selected Fe-B master alloy raw material is more than or equal to 99wt.%.
Furthermore, when the alloy raw materials are smelted, the Fe-B intermediate alloy raw materials are placed at the lowest part of the copper crucible so as not to be blown away by the instant arc and influence the B content, and the Fe-B intermediate alloy is covered by the metal simple substance raw materials of Ni, cr, cu, al and Ti.
Further, the vacuum pumping of the vacuum melting furnace is 2.9 multiplied by 10 -3 ～3.2×10 -3 pa, and then reversely filling high-purity argon to-0.06-0.05 MPa.
Further, when the alloy button ingot is smelted, the current is added to 200-250A, the smelting time is 60-80 s, and the repeated smelting and turning times are 5-6 times, so that the uniformity of the tissue structure is ensured.
Further, the selected equipment for the homogenization heat treatment, the cold rolling and the high-temperature aging heat treatment are a GSL tubular heat treatment furnace, a two-roll cold rolling mill and a MITR table box furnace respectively.
Further, the homogenization heat treatment process comprises the following steps: homogenizing at 1100-1200 deg.c for 4-8 hr and water quenching; a cold rolling process: a large deformation amount of 80 to 90%; high-temperature aging heat treatment process: the annealing temperature is 650-1100 ℃, the aging time is 1-20 h, and the water quenching is carried out.
Furthermore, the tensile strength of the multicomponent alloy is greatly improved through simple thermal mechanical treatment after trace B element doping, meanwhile, the fracture toughness is maintained at a higher level, modification is carried out within an acceptable cost control range, and the balance of strength and plasticity is realized.
The invention also discloses the application of the trace B element doped modified high-strength high-plasticity multi-component alloy in the fields of hard tool materials, tank armors, transformers, machine tools, jet aircraft engines, aircraft engine combined blades or engine casings.
Compared with the prior art, the trace B element doped modified high-strength high-plasticity Fe-Ni-Cr-Cu-Al-Ti-B multi-component alloy has the following advantages:
1. the multicomponent alloy is doped with trace B element and then is subjected to thermo-mechanical treatment in the prior art, so that the precipitation of a coarse BCC-based Heusler phase at a grain boundary is inhibited, the formation of a fine BCC-based Heusler phase in the grain boundary is promoted, the nucleation points of a crack source are reduced, the stress concentration is relieved, and the balance of strength and plasticity is realized.
2. The multicomponent alloy of the invention not only has excellent comprehensive mechanical property, but also has more uniform organization structure after being modified by doping trace B element, has few casting defects, and greatly improves the problem of difficult casting forming of the multicomponent alloy.
3. The trace B element doped modified high-strength high-plasticity Fe-Ni-Cr-Cu-Al-Ti-B multi-component alloy has the advantages of simple preparation process, easy acquisition of selected materials and wide development prospect in industrial production of the Fe-based multi-component alloy by modification within the acceptable cost control range.
4. The multicomponent alloy of the invention has excellent mechanical property under the B-free state, and the yield strength, the tensile strength and the elongation are 793.8MPa, 1153.1MPa and 25.2 percent respectively. After the modification by doping trace B element, the yield strength and the tensile strength of the multicomponent alloy are greatly improved to 1153.1MPa and 1442.7MPa respectively, and the elongation at break is still kept at a higher level of 21.3%.
Drawings
FIG. 1 is a microstructure of the multicomponent alloy of example 1 and comparative example 1 of the present invention in the same thermomechanically treated state, wherein (a) is the B-free state of comparative example 1 and (B) is the B state of example 1 at 60 ppm;
FIG. 2 is an XRD pattern of the multicomponent alloy obtained in example 1 of the present invention and comparative example 1 under the same thermo-mechanical treatment condition;
FIG. 3 is a tensile engineering stress-strain curve of the multicomponent alloy obtained in example 1 of the present invention and comparative example 1 under the same thermomechanically treated condition.
FIG. 4 shows the microstructure of the multicomponent alloy obtained in example 2 of the present invention and comparative example 2 in the same thermomechanically treated state, wherein (a) is the B-free state of comparative example 2 and (B) is the B state of example 2 containing 90 ppm;
FIG. 5 is an XRD pattern of the multicomponent alloy obtained in example 2 of the present invention and comparative example 2 under the same thermo-mechanical treatment condition;
FIG. 6 is a tensile engineering stress-strain curve of the multicomponent alloys obtained in inventive example 2 and comparative example 2 under the same thermomechanically treated condition.
Detailed Description
The invention is further illustrated by the following examples:
example 1
The embodiment discloses a trace B element-doped modified high-strength high-plasticity Fe-Ni-Cr-Cu-Al-Ti-B multi-component alloy with a general formula of Fe 2 NiCr 0.5 Cu 0.2 Al 0.3 Ti 0.1 -60ppm B multicomponent alloy composition.
In this embodiment, the preparation method of the trace B element-doped modified high-strength high-plasticity multi-component alloy comprises the following steps: according to the weight ratioThe Fe-B intermediate alloy raw material is placed at the lowest part of a copper crucible so as not to be blown away by an instantaneous arc to influence the B content, the Fe-B intermediate alloy is covered by the elementary metal raw materials of Ni, cr, cu, al and Ti, the purity of the selected elementary metal raw materials of Ni, cr, cu, al and Ti is more than or equal to 99.95 wt%, and the purity of the selected Fe-B intermediate alloy raw material is more than or equal to 99 wt%. Vacuum pumping to 3.0 × 10 -3 pa, and then reversely filling high-purity argon to-0.06 MPa.
When the alloy ingot is smelted, the current is added to 250A, the smelting time is 70s, and the alloy ingot is repeatedly turned and smelted for 6 times to ensure the uniformity of the structure. Finally obtaining the as-cast state doped 60ppm B modified Fe 2 NiCr 0.5 Cu 0.2 Al 0.3 Ti 0.1 A multi-component alloy button ingot. Placing the multi-component alloy button ingot in a GSL tubular heat treatment furnace, selecting a homogenization heat treatment process at 1200 ℃ for 4h, and performing water quenching; the cold rolling was repeated 2 times with a cold rolling deformation of 90% and a cold rolling amount of 0.1mm per pass. Then annealing at high temperature of 1000 ℃ for 1h, and water quenching; then low-temperature annealing is carried out for 700 ℃ multiplied by 20h, and water quenching is carried out. Finally 60ppm B of Fe in the thermomechanically treated state was obtained 2 NiCr 0.5 Cu 0.2 Al 0.3 Ti 0.1 A multi-component alloy.
Comparative example 1
The general formula of the alloy of the comparative example is Fe 2 NiCr 0.5 Cu 0.2 Al 0.3 Ti 0.1 The preparation method is basically the same as that of example 1, except that the Fe-B master alloy raw material is replaced with a metallic simple substance raw material Fe.
FIG. 1 shows the microstructure of the multicomponent alloy obtained in example 1 and comparative example 1 in the same thermomechanically treated state. It was found that the alloy, after being doped with 60ppm of B, was subjected to the same thermo-mechanical treatment, which suppressed the precipitation of coarse BCC-based Heusler phases at grain boundaries, while promoting the formation of fine BCC-based Heusler phases within grain boundaries. FIG. 2 shows XRD patterns of the multi-component alloys obtained in example 1 and comparative example 1 in the same thermo-mechanically treated state, the multi-component alloys having identical phase structures in the 0B and 60ppm B containing states, both comprised of FCC and BCC phases. FIG. 3 is a tensile engineering stress-strain curve of the multicomponent alloy obtained in example 1 and comparative example 1 under the same thermomechanically treated condition. The multicomponent alloy can be found to have excellent mechanical properties in the 0B state, and the yield strength, the tensile strength and the elongation are 793.8MPa, 1153.1MPa and 25.2 percent respectively. After the modification by doping 60ppm B, the precipitation of a coarse hard phase at a grain boundary is inhibited, the formation of a fine Heusler phase in the grain boundary is promoted, the stress concentration is relieved, the yield strength and the tensile strength of the alloy are improved and respectively increased to 961.1MPa and 1270.9MPa, and the fracture elongation is still kept at a higher level of 22.7%.
Example 2
The embodiment discloses a trace B element-doped modified high-strength high-plasticity Fe-Ni-Cr-Cu-Al-Ti-B multi-component alloy with a general formula of Fe 2 NiCr 0.5 Cu 0.2 Al 0.3 Ti 0.1 -90ppm B multicomponent alloy composition.
In this embodiment, the preparation method of the trace B element doped modified high-strength high-ductility Fe-Ni-Cr-Cu-Al-Ti-B multicomponent alloy comprises the following steps: the Fe-B intermediate alloy raw material is placed at the lowest part of a copper crucible so as to prevent the Fe-B intermediate alloy raw material from being blown away by an instantaneous arc to influence the B content, the Fe-B intermediate alloy is covered by metal elementary raw materials of Ni, cr, cu, al and Ti, the purity of the selected metal elementary raw materials of Ni, cr, cu, al and Ti is more than or equal to 99.95 wt%, and the purity of the selected Fe-B intermediate alloy raw material is more than or equal to 99 wt%. Vacuum pumping to 3.0 × 10 -3 pa, and then reversely filling high-purity argon to-0.06 MPa.
When the alloy ingot is smelted, the current is added to 250A, the smelting time is 70s, and the alloy ingot is repeatedly turned and smelted for 6 times to ensure the uniformity of the structure. Finally obtaining the modified Fe doped with 90ppm of B under the cast state 2 NiCr 0.5 Cu 0.2 Al 0.3 Ti 0.1 A multi-component alloy button ingot. Placing the obtained multi-component alloy button ingot in a GSL tubular heat treatment furnace, selecting a homogenization heat treatment process to be 1200 ℃ for 4h, and performing water quenching; the cold rolling was repeated 2 times with a cold rolling deformation of 90% and a cold rolling amount of 0.1mm per pass. Then annealing at high temperature of 1000 ℃ for 1h, and water quenching; then low-temperature annealing is carried out for 700 ℃ multiplied by 20h, and water quenching is carried out. Finally, fe in thermomechanically treated state containing 90ppm of B is obtained 2 NiCr 0.5 Cu 0.2 Al 0.3 Ti 0.1 A multi-component alloy.
Comparative example 2
The general formula of the alloy of the comparative example is Fe 2 NiCr 0.5 Cu 0.2 Al 0.3 Ti 0.1 The preparation method is basically the same as that of example 2, except that the raw material of the Fe-B master alloy is replaced with a metallic simple substance raw material Fe.
FIG. 4 shows the microstructure of the multicomponent alloy obtained in example 2 and comparative example 2 in the same thermomechanically treated state. Similar to example 1, it was found that the alloy after doping with 90ppm B was subjected to the same thermo-mechanical treatment, suppressing precipitation of coarse BCC-based Heusler phases at grain boundaries, and simultaneously promoting formation of fine BCC-based Heusler phases within grain boundaries. FIG. 5 shows XRD patterns of the multi-component alloys obtained in example 2 and comparative example 2 under the same thermo-mechanical treatment conditions, the multi-component alloys having identical phase structures in the 0B and 90ppm B-containing conditions, both of which are composed of FCC and BCC phases, but with the addition of 90ppm B reduced (110) BCC The intensity of the peaks indicates a relatively low content of BCC phase therein. FIG. 6 is a tensile engineering stress-strain curve of the multicomponent alloys obtained in example 2 and comparative example 2 under the same thermomechanically treated condition. The multicomponent alloy can be found to have excellent mechanical properties in the 0B state, and the yield strength, the tensile strength and the elongation are 793.8MPa, 1153.1MPa and 25.2 percent respectively. After the modification by doping 90ppm B, the precipitation of a coarse hard phase at a grain boundary is inhibited, the formation of a fine Heusler phase in the grain boundary is promoted, and the stress concentration is relieved, so that the yield strength and the tensile strength of the alloy are greatly improved to be respectively increased to 1153.1MPa and 1442.7MPa, and the fracture elongation is still kept at a higher level of 21.3%. In conclusion, the Fe-Ni-Cr-Cu-Al-Ti-B multicomponent alloy modified by doping trace B element has excellent strength-plasticity balance, so that the Fe-Ni-Cr-Cu-Al-Ti-B multicomponent alloy has wide development prospect in the field of engineering structures.
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 trace B element doped modified high-strength high-plasticity multi-component alloy is characterized in that the general formula is Fe a Ni b Cr c Cu d Al e Ti f -gB, wherein a, b, c, d, e and f are molar ratios, g is a mass fraction, a is more than or equal to 1.8 and less than or equal to 2.2, b is more than or equal to 0.8 and less than or equal to 1.2, c is more than or equal to 0.3 and less than or equal to 0.6, d is more than or equal to 0.1 and less than or equal to 0.4, e is more than or equal to 0.1 and less than or equal to 0.4, f is more than or equal to 0.1 and less than or equal to 0.3, and g is more than or equal to 60ppm and less than or equal to 90ppm.
2. The trace B element-doped modified high-strength high-plasticity multi-component alloy as claimed in claim 1, wherein the general formula is Fe a Ni b Cr c Cu d Al e Ti f -a in gB: b: d: f =20:10:2:1, c: e =5:3, and g is more than or equal to 60ppm and less than or equal to 90ppm.
3. A preparation method of the trace B element-doped modified high-strength high-plasticity multi-component alloy as claimed in claim 1 or 2 is characterized by comprising the following steps:
stacking single raw materials of Ni, cr, cu, al, ti and Fe-B intermediate alloy according to the weight ratio, and smelting by using a vacuum arc smelting furnace to obtain a multi-component alloy button ingot; placing the multi-component alloy button ingot into a vacuum heat treatment furnace, carrying out homogenization heat treatment, and then sequentially carrying out large-deformation cold rolling and high-temperature aging heat treatment to obtain the trace B element doped modified high-strength high-plasticity multi-component alloy.
4. The method for preparing the trace B element-doped modified high-strength high-plasticity multi-component alloy according to claim 3, wherein the purity of selected metal elementary raw materials, namely Ni, cr, cu, al and Ti, is more than or equal to 99.95 wt%; the purity of the selected Fe-B master alloy raw material is more than or equal to 99wt.%.
5. The method for preparing the trace B element-doped modified high-strength high-plasticity multi-component alloy as claimed in claim 3, wherein when the alloy raw materials are smelted, the Fe-B intermediate alloy raw materials are placed at the lowest part of a copper crucible, and the Fe-B intermediate alloy is covered by the elemental metal raw materials of Ni, cr, cu, al and Ti.
6. The method for preparing the trace B element-doped modified high-strength high-plasticity multi-component alloy as claimed in claim 3, wherein the vacuumizing of a vacuum melting furnace is 2.9 x 10 -3 ～3.2×10 -3 pa, and then reversely filling high-purity argon to-0.06-0.05 MPa.
7. The method for preparing the trace B element-doped modified high-strength high-plasticity multi-component alloy according to claim 3, wherein when the alloy button ingot is smelted, the current is added to 200-250A, the smelting time is 60-80 s, and the repeated smelting and turning times are 5-6 times.
8. The method for preparing the trace B element-doped modified high-strength high-plasticity multi-component alloy according to claim 3, wherein the selected equipment for the homogenization heat treatment, the cold rolling and the high-temperature aging heat treatment are a GSL tubular heat treatment furnace, a two-roll cold rolling mill and a MITR bench box furnace respectively.
9. The method for preparing the trace B element-doped modified high-strength high-plasticity multi-component alloy according to claim 3, wherein the homogenizing heat treatment process comprises the following steps: homogenizing at 1100-1200 deg.c for 4-8 hr, and water quenching; the cold rolling process comprises the following steps: a large deformation amount of 80 to 90%; the high-temperature and low-temperature annealing heat treatment process comprises the following steps: annealing temperature is 650-1100 ℃, aging time is 1-20 h, and water quenching is carried out.
10. Use of the B element doped modified high strength high plasticity multicomponent alloy of claim 1 or 2 in the field of hard tool materials, tank armor, transformers, machine tools, jet engines, aircraft engine composite blades or engine casings.
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| CN114293087A (en) * | 2022-01-04 | 2022-04-08 | 中国科学院兰州化学物理研究所 | Single-phase high-entropy alloy with micron/nano-crystalline grain composite structure |
| CN115141967A (en) * | 2022-06-13 | 2022-10-04 | 哈尔滨工业大学（深圳） | High-entropy alloy composite material and preparation method and application thereof |
| CN115354202A (en) * | 2022-07-05 | 2022-11-18 | 西北工业大学 | High-toughness material suitable for differential backfill spot welding tool and preparation method |
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