CN111500917A - High-strength and high-toughness medium-entropy high-temperature alloy and preparation method thereof - Google Patents
High-strength and high-toughness medium-entropy high-temperature alloy and preparation method thereof Download PDFInfo
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- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
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Abstract
The invention discloses a high-strength and high-toughness medium-entropy high-temperature alloy and a preparation method thereof, wherein the alloy comprises the following chemical components, by weight, 28.5-32.5% of Cr, 31.5-33.4% of Co, 32-35% of Ni, 0.5-6% of Al, 0-6% of Ti, 0-3% of Ta, 0.02-0.12% of C, 0.002-0.015% of B, 0.005-0.12% of Zr, 0.005-0.15% of RE, more than or equal to 2% and less than or equal to Al + Ti + Ta and less than or equal to 6% of Ta, wherein RE is any one of rare earth elements of Ce, L a and Y.
Description
Technical Field
The invention belongs to the technical field of medium-entropy high-temperature alloys, and relates to a high-strength high-toughness medium-entropy high-temperature alloy and a preparation method thereof.
Background
The high-entropy alloy is a novel alloy material which is developed in recent years and is different from the traditional alloy, and consists of 5-13 main elements, wherein the constituent elements have equal or approximately equal atomic ratios. After solidification of the multi-principal element high-entropy alloy, a complex intermetallic compound is not formed, but a simple FCC or BCC solid solution is formed. The high-entropy alloy has a thermodynamic high-entropy effect, a structural lattice distortion effect, a kinetic delayed diffusion effect and a performance cocktail effect. By utilizing the effects, the components of the alloy are reasonably designed, and the alloy has good comprehensive characteristics of high hardness, high strength, good wear resistance, corrosion resistance, high-temperature oxidation resistance and the like.
Although high entropy alloys are excellent in performance, generally the toughness and toughness match is poor. For example, the FeCoNiCrMn high-entropy alloy can achieve 60% of stretch forming, but the tensile strength is lower than 500 MPa; the compression strength of AlCoCrFeNiTi0.5 high-entropy alloy reaches 3200MPa, but almost has no tensile plasticity. The addition of Ti and Al in a small amount can promote the precipitation of a second phase, thereby strengthening the performance of the high-entropy alloy, but the toughness matching can not be improved for all high-entropy alloys. For example, for AlFeCrCoCu alloy, the addition of Ti can significantly increase the hardness of the alloy, but has almost no tensile plasticity. The existing AlCrFeNiV system high-entropy alloy has certain obdurability matching effect, but is not enough for practical application. It is for these reasons that the development and engineering applications of high entropy alloys are limited.
At present, research in the field of high-entropy alloy is more and more transferred to medium-entropy alloy. The CrCoNi medium entropy alloy is a single Face Centered Cubic (FCC) solid solution and has more excellent strength and plasticity than FeCoNiCrMn high entropy alloy. In addition, the alloy has high Cr content and better oxidation resistance and corrosion resistance. However, the medium entropy alloy is only solid solution strengthened, and the high temperature strength is still low. Therefore, how to further improve the strength of the alloy by strengthening means such as dislocation strengthening, precipitation strengthening and the like and promote the application of the alloy in the field of high-temperature structural materials is a problem which needs to be solved at present.
Disclosure of Invention
The invention aims to solve the problems of insufficient strength and the like of the CrCoNi intermediate entropy alloy, negotiate the relationship between strength and plasticity, and provide the intermediate entropy high-temperature alloy with high strength and toughness and the preparation method thereof. The method is formulated by adding a proper amount of alloy strengthening elements, reasonable hot working and a solution aging heat treatment process, and the obtained high-strength-toughness medium-entropy high-temperature alloy keeps higher strength and plasticity on the premise of keeping better hot working performance. Therefore, the key technology for solving the problems is selection and dosage of alloy elements, optimization of a processing and preparation process and selection of a solution aging heat treatment process.
The invention is realized by the following technical scheme:
the high-strength high-toughness medium-entropy high-temperature alloy comprises, by weight, 28.5-32.5% of Cr28, 31.5-33.4% of Co, 32-35% of Ni, 0.5-6% of Al, 0-6% of Ti, 0-3% of Ta, 0.02-0.12% of C, 0.002-0.015% of B, 0.005-0.12% of Zr, 0.005-0.15% of RE, and more than or equal to 2% and less than or equal to 6% of Al + Ti + Ta, wherein RE is any one of rare earth elements Ce, L a and Y.
The invention relates to a high-strength and high-toughness medium-entropy high-temperature alloy and a preparation method thereof, wherein the preparation method comprises the following steps:
1) mixing Cr, Co, Ni, Al, Ti, Ta, B, Zr, C and RE according to a proportion, putting the mixture into a smelting furnace for smelting, refining at a high temperature of 1550-1650 ℃ for 15-30 min, and casting into an alloy ingot;
2) forging the alloy ingot to form an electrode bar, remelting the electrode bar, and crystallizing the remelted alloy ingot;
3) forging the heavy fusion ingot to prepare an alloy bar;
4) and carrying out solid solution and aging heat treatment on the alloy bar.
The smelting is vacuum induction furnace smelting;
the forged electrode bar is forged into an electrode bar at the temperature of 800-1250 ℃, and the forging ratio is 3-5;
the remelting is vacuum arc furnace remelting or vacuum electroslag remelting;
the forging alloy bar is formed by cogging and forging alloy square billets 1 at the temperature of 800-1250 ℃, and the forging ratio is 3-5. After surface grinding and defect flaw detection treatment, forging the alloy square blank 1 into an alloy blank 2 at the temperature of 800-1250 ℃, wherein the forging ratio is 5-8, tempering the alloy blank 2 at the temperature of 800-1250 ℃ for 25-30 min, rounding the alloy blank 2 at the forging ratio of 1-5 into a square blank 3, tempering the alloy blank 3 at the temperature of 800-1250 ℃ for 25-30 min, and rinsing the alloy blank into a round bar at the forging ratio of 1-5.
The solid solution heat treatment process comprises the steps of firstly heating to 800-920 ℃, preserving heat for 1-2 hours, continuously heating to 1050-1200 ℃, preserving heat for 1-4 hours, and air cooling to obtain a solid solution alloy;
the aging system is to perform heat preservation for 5-20 hours at 700-950 ℃ and perform air cooling.
The alloy of the invention comprehensively considers the influence of alloy elements on the high-temperature mechanical property, the hot working property and the oxidation resistance of the alloy during component design, and the specific consideration factors are as follows:
cr: mainly enter a gamma matrix to play a role in solid solution strengthening, and can also precipitate granular M on a grain boundary23C6Carbide strengthens the grain boundaries and another important function of Cr is to protect the alloy surface from O, S, salt action, which causes oxidation and hot corrosion. The existing alloy with better corrosion resistance generally has higher Cr content. However, since Cr is an element that promotes the formation of a brittle sigma-type harmful phase and excessively high Cr content deteriorates the structural stability of the alloy, the Cr content is 28.5 to 32.5%.
Co: the alloy is mainly dissolved in a gamma matrix in a solid mode, plays a role in solid solution strengthening, reduces stacking fault energy of the matrix, reduces the solubility of Al and Ti in the matrix, increases the number of gamma 'phases, improves the dissolution temperature of the gamma' phases, and obviously improves the creep resistance of the alloy. Therefore, the content of Co is 31.5-33.4%.
Ni: the gamma ' phase forming element obviously expands the two-phase area of gamma/gamma ', improves the stability of alloy structure and improves the complete dissolving temperature of the gamma ' phase to a certain extent. However, if the Ni content is too high, the chemical composition of the gamma' phase will be closer to that of Ni3Since Al increases the coarsening rate, the Ni content is 32-35%.
Al, Ti and Ta: al, Ti and Ta are main elements forming gamma' phase, and can greatly improve the precipitation strengthening effect of the alloy. Meanwhile, the addition of Al element can form Al on the surface of the alloy2O3The protective film is beneficial to improving the oxidation resistance of the alloy, Ti is beneficial to improving the corrosion resistance, Ta obviously improves the complete dissolution temperature, volume fraction and stability of a gamma' phase, and enhances the high-temperature mechanical property of the alloy, but excessive Al and Ti can separate out harmful β phases and are not beneficial to tissue stability.
C: the grain boundary strengthening element is also a strong deoxidizer, is beneficial to deoxidation in the alloy smelting process, improves the purity of the alloy and improves the processability of the alloy. Meanwhile, C can react with partial refractory element performance carbide, so that the supersaturation degree of a matrix is reduced, and the structure stability is facilitated. However, the content of C is too high, which forms continuous and network-distributed carbide on the grain boundary and is not beneficial to the mechanical property of the alloy, so that the content of C is 0.02-0.12%.
B and Zr: and B is a crystal boundary strengthening element, can increase the plasticity of the alloy, is beneficial to the coordinated deformation of the crystal boundary in the hot working process, and can improve the oxidation resistance and creep resistance of the alloy. However, if the content of B is too high, large block boride is easy to form in the grain boundary, which is not favorable for the mechanical property of the alloy. Zr is also a crystal boundary strengthening element, has an important effect on purifying crystal boundaries, and improves the plasticity and creep resistance of the alloy. However, too high Zr content is not favorable for the mechanical properties of the alloy. Therefore, B is 0.002 to 0.015% and Zr is 0.005 to 0.12%.
The RE, Ce, L a and Y rare earth elements can play a good role in deoxidation, desulfurization and degassing in the alloy smelting process, purify and strengthen grain boundaries and improve the processing performance of the alloy, can also be used as microalloying elements to be segregated in the grain boundaries and play a role in strengthening the grain boundaries, and in addition, the Ce, L a and Y are used as active elements to improve the oxidation resistance of the alloy and improve the surface stability, but too high rare earth elements can form a large amount of large-particle oxides in the grain boundaries and are not beneficial to the processing performance of the alloy, so the RE is 0.005-0.15%.
Al + Ti + Ta: al, Ti and Ta are all gamma 'phase forming elements, and the content of the elements directly influences the volume fraction and the complete dissolution temperature of the gamma' phase, so that the high-temperature mechanical property of the alloy is determined. However, the too high contents of Al, Ti and Ta are not good for the processing performance of the alloy, so that the content of Al, Ti and Ta is controlled to be more than or equal to 2 percent and less than or equal to 6 percent.
The invention has the following beneficial effects:
1) the alloy has high strength. Cr, Co and Ni are added in equal molar atomic percentage, so that a higher entropy value is kept, and a strong solid solution strengthening effect is achieved; in addition, three gamma 'phase forming elements of Al, Ti and Ta are added, so that the alloy has a precipitation strengthening effect of a stably existing nano gamma' phase at 700-850 ℃, and the high-temperature mechanical property of the alloy is obviously improved by reasonably matching C, B and Zr crystal boundary strengthening elements; meanwhile, by adjusting the hot working process parameters and the heat treatment system, more twin crystals exist in the alloy, and the strength of the alloy is further improved through twin crystal strengthening;
2) the alloy has good hot workability. The alloy has a wider hot working window of 330-390 ℃, and has less surface cracks, good plasticity and high yield in the alloy forging process. By controlling Al + Ti + Ta to be less than or equal to 6%, the aging strengthening effect is fully achieved, the alloy is ensured to have good hot working performance, and the gamma' phase is controlled to be in nanoparticle dispersion distribution. By adding RE rare earth elements, the grain boundary is purified, and the hot processing performance of the grain boundary is improved;
3) the alloy has good oxidation resistance. Adding 28.5-32.5% of Cr to produce Cr on the surface of alloy2O3The oxidation resistance is improved; in addition, the oxidation resistance of the alloy is further improved by adding the RE element;
4) the alloy has the advantages of less harmful impurity elements, high purity, less internal defects and good uniformity of component structure. Through reasonable addition of C, RE alloy elements, better effects of deoxidation, denitrification and desulfurization are achieved. The high vacuum refining is adopted to further reduce the gas content and improve the purity and the hot workability of the alloy. By adopting a smelting and remelting duplex smelting mode, the contents of non-metallic inclusions, gas and sulfur in the alloy are reduced, the segregation of alloy components is reduced, the uniformity of component structures is ensured, and the mechanical property of the alloy is further improved.
5) The alloy has the advantages that the content of noble metals such as Ta and the like is controlled, the alloy cost and the alloy density are controlled, and the alloy density is 8.1-8.3 g/cm3The alloy is lower than most existing cobalt-based wrought superalloy and is equivalent to advanced nickel-based wrought superalloy, so that the alloy can be used as a candidate material for high-temperature components of aircraft engines and industrial gas turbines, and has a good application prospect.
Drawings
Fig. 1 is an optical micrograph of alloy 2.
FIG. 2 is a tensile engineering stress-strain curve of alloy 1 and alloy 2 at a high temperature of 700 ℃.
Detailed Description
Table 1 shows the alloy compositions of the examples and some of the reference alloy compositions (in weight percent). It is apparent that the embodiments described below are only a part of the embodiments of the present invention, and not all of them. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
TABLE 1
Example 1
Weighing Cr, Co, Ni, Al, Ti, Ta, B, Zr, C and RE raw materials according to the components shown in the alloys 1-3 in the table 1, putting the raw materials into a 50kg vacuum induction smelting furnace for smelting, carrying out high-temperature refining for 15min at the refining temperature of 1650 ℃, and casting into alloy ingots; the alloy ingot is forged into an electrode bar at the temperature of 800 ℃ with the forging ratio of 3. Remelting in a vacuum arc furnace, and crystallizing to obtain a remelted alloy ingot; and forging the heavy-fusion gold ingot at 800 ℃, cogging and forging to obtain an alloy square billet 1, wherein the forging ratio is 3. After surface grinding and defect flaw detection treatment, forging the alloy square billet 1 into an alloy billet 2 at the temperature of 800 ℃, wherein the forging ratio is 5, tempering the alloy billet 2 at the temperature of 800 ℃ for 30min, rounding the alloy billet 2 at the forging ratio of 1 into a square billet 3, tempering the alloy billet 3 at the temperature of 800 ℃ for 30min, and rinsing the alloy billet into an alloy bar at the forging ratio of 1. Firstly carrying out solution heat treatment on the alloy bar, wherein the process comprises the following steps: firstly heating to 800 ℃, preserving heat for 2h, continuously heating to 1050 ℃, preserving heat for 4h, and air cooling to obtain solid solution alloy; and then carrying out aging treatment, wherein the aging treatment process comprises the steps of keeping the temperature for 5 hours at 700 ℃, and cooling in air.
Table 2 shows the tensile properties at 700 ℃ for alloys 1 to 3 and comparative alloys
| Alloy brand | Rm/MPa | Rp0.2/MPa | A％ |
| Alloy 1 | 812 | 495 | 23 |
| Alloy 2 | 939 | 620 | 18 |
| Alloy 3 | 813 | 554 | 20 |
| Comparative alloy GH605 | 504 | 338 | 20 |
| Comparative alloy GH4169 | 808 | 540 | 6 |
Example 2
Weighing Cr, Co, Ni, Al, Ti, Ta, B, Zr, C and RE raw materials according to the components shown in alloy 4-6 in the table 1, putting the raw materials into a 50kg vacuum induction smelting furnace for smelting, carrying out high-temperature refining for 30min at the refining temperature of 1550 ℃, and casting into alloy ingots; the alloy ingot was forged to an electrode bar at 1250 ℃ with a forging ratio of 5. Remelting in a vacuum arc furnace, and crystallizing to obtain a remelted alloy ingot; and forging the heavy-fusion gold ingot at 1250 ℃, and cogging and forging to obtain an alloy square billet 1 with a forging ratio of 5. After surface grinding and defect flaw detection treatment, forging the alloy square billet 1 into an alloy billet 2 at 1250 ℃, wherein the forging ratio is 8, tempering the alloy billet 2 at 1250 ℃ for 25min, rounding the alloy billet 2 into a square billet 3 at the forging ratio of 5, tempering the alloy billet 3 at 1250 ℃ for 25min, and rinsing the alloy billet into an alloy bar at the forging ratio of 5. Firstly carrying out solution heat treatment on the alloy bar, wherein the process comprises the following steps: heating to 920 ℃, preserving heat for 1h, continuing heating to 1050 ℃, preserving heat for 1h, and air cooling to obtain solid solution alloy; and then carrying out aging treatment, wherein the aging treatment process comprises the steps of keeping the temperature for 5 hours at 950 ℃, and cooling in air.
Table 3 shows the tensile properties at 700 ℃ for alloys 4-6 and comparative alloys
| Alloy brand | Rm/MPa | Rp0.2/MPa | A％ |
| Alloy 4 | 840 | 510 | 20 |
| Alloy 5 | 857 | 522 | 19 |
| Alloy 6 | 907 | 562 | 21 |
| Comparative alloy GH605 | 504 | 338 | 20 |
| Comparative alloy GH4169 | 808 | 540 | 6 |
Example 3
Weighing Cr, Co, Ni, Al, Ti, Ta, B, Zr, C and RE raw materials according to the components shown in alloy 7-9 in the table 1, putting the raw materials into a 50kg vacuum induction smelting furnace for smelting, carrying out high-temperature refining for 25min at 1600 ℃, and casting into alloy ingots; the alloy ingot was forged to an electrode rod at a temperature of 1150 ℃ at a forging ratio of 4. Remelting in a vacuum arc furnace, and crystallizing to obtain a remelted alloy ingot; and forging the heavy-fusion gold ingot at the forging temperature of 1150 ℃, and cogging and forging the heavy-fusion gold ingot into an alloy square billet 1 with the forging ratio of 4. After surface grinding and defect flaw detection treatment, forging the alloy square billet 1 into an alloy billet 2 at the temperature of 1150 ℃, wherein the forging ratio is 6, tempering the alloy billet 2 at the temperature of 1150 ℃ for 28min, rounding the alloy billet 2 at the forging ratio of 3 into a square billet 3, tempering the alloy billet 3 at the temperature of 1150 ℃ for 28min, and rinsing the alloy billet into an alloy bar at the forging ratio of 3. Firstly carrying out solution heat treatment on the alloy bar, wherein the process comprises the following steps: firstly heating to 850 ℃, preserving heat for 2h, continuously heating to 1200 ℃, preserving heat for 1h, and air cooling to obtain solid solution alloy; and then carrying out aging treatment, wherein the aging treatment process comprises the steps of keeping the temperature for 20 hours at 950 ℃, and cooling in air.
Table 4 shows the tensile properties at 700 ℃ for alloys 7 to 9 and comparative alloys
The present invention is not limited to the above-described preferred embodiments, which are not intended to limit the scope of the invention. All equivalent changes and modifications made according to the content of the claims of the present application shall be within the technical scope of the present invention.
Claims (8)
1. The high-strength high-toughness medium-entropy high-temperature alloy is characterized by comprising the following chemical components, by weight, 28.5-32.5% of Cr, 31.5-33.4% of Co, 32-35% of Ni, 0.5-6% of Al, 0-6% of Ti, 0-3% of Ta, 0.02-0.12% of C, 0.002-0.015% of B, 0.005-0.12% of Zr, 0.005-0.15% of RE, more than or equal to 2% of Al + Ti + Ta, and less than or equal to 6%, wherein RE is any one of rare earth elements Ce, L a and Y.
2. The preparation method of the high-strength-toughness medium-entropy high-temperature alloy as claimed in claim 1, characterized by comprising the following steps:
1) mixing Cr, Co, Ni, Al, Ti, Ta, B, Zr, C and RE according to a proportion, putting the mixture into a smelting furnace for smelting, refining at a high temperature of 1550-1650 ℃ for 15-30 min, and casting into an alloy ingot;
2) forging the alloy ingot to form an electrode bar, remelting the electrode bar, and crystallizing the remelted alloy ingot;
3) forging the heavy fusion ingot to prepare an alloy bar;
4) and carrying out solid solution and aging heat treatment on the alloy bar.
3. The method for preparing the high-strength high-toughness medium-entropy high-temperature alloy as claimed in claim 2, wherein the smelting is vacuum induction furnace smelting.
4. The preparation method of the high-strength-toughness medium-entropy high-temperature alloy as claimed in claim 2, wherein the forged electrode rod is forged into an electrode rod at a temperature of 800-1250 ℃, and the forging ratio is 3-5.
5. The method of claim 2, wherein the remelting is vacuum arc furnace remelting or vacuum electroslag remelting.
6. The preparation method of the high-strength-toughness medium-entropy high-temperature alloy as claimed in claim 2, wherein the forging alloy bar is formed by cogging and forging an alloy billet 1 at a temperature of 800-1250 ℃, and the forging ratio is 3-5. After surface grinding and defect flaw detection treatment, forging the alloy square blank 1 into an alloy blank 2 at the temperature of 800-1250 ℃, wherein the forging ratio is 5-8, tempering the alloy blank 2 at the temperature of 800-1250 ℃ for 25-30 min, rounding the alloy blank 2 at the forging ratio of 1-5 into a square blank 3, tempering the alloy blank 3 at the temperature of 800-1250 ℃ for 25-30 min, and rinsing the alloy blank into a round bar at the forging ratio of 1-5.
7. The preparation method of the high-strength-toughness medium-entropy high-temperature alloy as claimed in claim 2, wherein the solution heat treatment process comprises the steps of firstly heating to 800-920 ℃, preserving heat for 1-2 hours, continuously heating to 1050-1200 ℃, preserving heat for 1-4 hours, and air cooling to obtain a solid solution alloy.
8. The preparation method of the high-strength-toughness medium-entropy high-temperature alloy as claimed in claim 2, wherein the aging system is to keep the temperature at 700-950 ℃ for 5-20 h and cool the alloy in air.
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