CN115821141A - Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy and preparation method thereof - Google Patents
Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
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Abstract
The invention discloses a Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy and a preparation method thereof, and relates to a Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy and a preparation method thereof. The invention aims to solve the problems of low hardness and poor wear resistance of the existing high-entropy alloy, and the Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy consists of Al, co, cr, fe, ni and Sc elements, and has the expression of (AlCoCrFeNi) 100‑x Sc x And x is 1 or 2, wherein Al, co, cr, fe and Ni are in equal atomic ratio. The alloy is prepared by adopting an arc melting method, and the Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy designed by the invention has the characteristics of high hardness, excellent wear resistance and the like. The invention is applied to the field of high-entropy alloy.
Description
Technical Field
The invention relates to a Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy and a preparation method thereof.
Background
High entropy alloys, an advanced metallic material, are composed of a plurality of constituent elements, each element content being between 5-35 at.%. By virtue of the characteristic of high configuration entropy, the high-entropy alloy often forms a single-phase solid solution instead of a large amount of intermetallic phases, so that the defects of the traditional alloy are avoided. Therefore, the high-entropy alloy has excellent comprehensive properties, namely enough hardness and strength, and excellent corrosion resistance, irradiation resistance and high-temperature oxidation resistance. The high-entropy alloy has great potential in practical application, and is particularly applied to the key fields of aviation, aerospace, chemical engineering, energy sources and the like.
In fact, multiphase high entropy alloys with similar structures have good overall properties. Therefore, alCoCrFeNi high entropy alloys with a dual phase BCC structure have received much attention. However, the AlCoCrFeNi high-entropy alloy does not have good castability, and shows great structural nonuniformity in the casting process, thereby causing the problem of poor castability. Eutectic high entropy alloys are known to have good castability. From a mechanical properties point of view, the combination of primary phase and eutectic region gives the best combination of strength and ductility compared to a fully eutectic structure. The AlCoCrFeNi high-entropy alloy with the dual-phase structure has higher ductility but lower hardness, and the Laves phase draws wide attention in the industrial field by virtue of the inherent advantage of high hardness. Thus, if hypoeutectic high entropy alloys with a composite BCC/Laves phase structure could be prepared, they would have superior hardness, wear resistance and castability, sweeping obstacles for their technical applications.
Disclosure of Invention
The invention aims to solve the problems of low hardness and poor wear resistance of the conventional high-entropy alloy, and provides a Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy and a preparation method thereof.
The invention relates to a Laves phase precipitation modified AlCoCrFeNi biphase high-entropy alloy which consists of Al, co, cr, fe, ni and Sc elements and has the expression (AlCoCrFeNi) 100-x Sc x And x is 1 or 2, wherein Al, co, cr, fe and Ni are in equal atomic ratio.
The preparation method of the Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy is carried out according to the following steps: 1. according to the expression (AlCoCrFeNi) 100-x Sc x Weighing Al, co, cr, fe, ni and Sc according to the atomic percentage to obtain raw materials; wherein x is 1 or 2, al, co, cr, fe, ni are equal atomic ratio;
2. pretreating raw materials and a titanium block, adding the raw materials into a crucible of a smelting furnace in the sequence of Al, sc, ni, co, fe and Cr from bottom to top, adding the titanium block into another crucible of the smelting furnace, vacuumizing the smelting furnace, introducing argon for protection, smelting the titanium block, smelting the raw materials, and cooling to obtain an alloy ingot;
3. repeatedly smelting the alloy ingot for 6-8 times, and cooling to obtain a Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy; wherein the alloy ingot is turned over each time of melting.
The invention has the beneficial effects that:
(1) According to the invention, rare earth Sc element is introduced into AlCoCrFeNi two-phase high-entropy alloy, and the mixed enthalpies of the Sc element and Al, co, cr, fe and Ni elements are respectively as follows: -38kJ/mol, -30kJ/mol, 1kJ/mol, -11kJ/mol and-39 kJ/mol, and the electronegativities of the elements Sc, al, co, cr, fe and Ni are respectively as follows: 1.36, 1.61, 1.88, 1.66, 1.83 and 1.91.
According to the invention, the characteristics of large atomic radius of Sc, large negative mixing enthalpy with other component elements, large electronegativity difference and the like are utilized, so that a hard Laves phase is precipitated at the crystal boundary of the AlCoCrFeNi alloy, and the hard Laves phase modified AlCoCrFeNi is prepared; the primary phase of the components is BCC phase, and the eutectic structure at the grain boundary comprises BCC and Laves phases which alternately grow.
(2) The light high-entropy alloy designed by the invention can be obtained by using a conventional arc melting preparation method. The preparation process is simple, convenient to operate and high in repeatability.
(3) The Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy designed by the invention has the characteristics of high hardness, excellent wear resistance and the like, is a preferred material for wear-resistant load-bearing structural members applied under various complex working conditions, and promotes the practical application of the high-entropy alloy.
Drawings
FIG. 1 is an XRD pattern of the high entropy alloys prepared in examples 1 and 2 and comparative example 1, wherein a pattern b is a partial enlarged view of a pattern a;
FIG. 2 is an SEM image of high entropy alloys prepared in examples 1 and 2 and comparative example 1;
FIG. 3 is a graph of alloy Vickers hardness for high entropy alloys prepared in examples 1 and 2 and comparative example 1;
FIG. 4 is a graph of wear rate data for alloys of the high entropy alloys prepared in examples 1 and 2 and comparative example 1.
Detailed Description
The technical solution of the present invention is not limited to the specific embodiments listed below, and includes any combination of the specific embodiments.
The first embodiment is as follows: the Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy in the embodiment is composed of Al, co, cr, fe, ni and Sc elements, and has the expression of (AlCoCrFeNi) 100-x Sc x And x is 1 or 2, wherein Al, co, cr, fe and Ni are in equal atomic ratio.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the Laves phase precipitation modified AlCoCrFeNi two-phase high entropy alloy consists of, in atomic percent, 19.8% Al, 19.8% Co, 19.8% Cr, 19.8% Fe, 19.8% Ni and 1% Sc, expressed as (AlCoCrFeNi) 99 Sc 1 . The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the Laves phase precipitation modified AlCoCrFeNi dual-phase high entropy alloy consists of, in atomic percent, 19.6% of Al, 19.6% of Co, 19.6% of Cr, 19.6% of Fe, 19.6% of Ni and 2% of Sc, expressed as (AlCoCrFeNi) 98 Sc 2 . OthersThe same as in the first or second embodiment.
The fourth concrete implementation mode: the preparation method of the Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy in the embodiment is carried out according to the following steps: 1. according to the expression (AlCoCrFeNi) 100-x Sc x Weighing Al, co, cr, fe, ni and Sc according to the atomic percentage to obtain raw materials; wherein x is 1 or 2, al, co, cr, fe, ni are equal atomic ratio;
2. pretreating raw materials and a titanium block, adding the raw materials into a crucible of a smelting furnace in the sequence of Al, sc, ni, co, fe and Cr from bottom to top, adding the titanium block into another crucible of the smelting furnace, vacuumizing the smelting furnace, introducing argon for protection, smelting the titanium block, smelting the raw materials, and cooling to obtain an alloy ingot;
3. repeatedly smelting the alloy ingot for 6-8 times, and cooling to obtain a Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy; wherein the alloy ingot is turned over during each melting.
In the smelting process, the metal titanium block is firstly smelted, and the residual oxygen in the chamber of the electric arc furnace chamber is adsorbed, so that the oxidation behavior in the smelting process is further reduced.
The fifth concrete implementation mode: the fourth difference between this embodiment and the specific embodiment is that: step one weigh Al, co, cr, fe, ni and Sc in proportions such that 19.8 atomic percent Al, 19.8% Co, 19.8% Fe, 19.8% Ni and 1% Sc. The rest is the same as the fourth embodiment.
The sixth specific implementation mode: the fourth or fifth difference between the present embodiment and the specific embodiment is that: step one weighing Al, co, cr, fe, ni and Sc at a ratio of 19.6 atomic percent Al, 19.6% Co, 19.6% Cr, 19.6% Fe, 2% Sc. The others are the same as the fourth or fifth embodiments.
The seventh embodiment: this embodiment differs from one of the fourth to sixth embodiments in that: and the pretreatment in the second step comprises grinding, polishing, cleaning and drying. The rest is the same as one of the fourth to sixth embodiments.
The specific implementation mode eight: this embodiment and the fourth to seventh embodimentsOne difference is that: in the second step, the vacuum is pumped to 5 multiplied by 10 -3 And introducing protective gas high-purity argon to-0.05 MPa after Pa. The rest is the same as one of the fourth to seventh embodiments.
The specific implementation method nine: this embodiment is different from the fourth to eighth embodiment in that: and the current intensity is 450-550A during smelting in the second step. The rest is the same as the fourth to eighth embodiments.
The detailed implementation mode is ten: this embodiment is different from one of the fourth to ninth embodiments in that: and step three, cooling for 20-30min along with the furnace after the last smelting. The others are the same as in one of the fourth to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
example 1 Laves phase precipitation modification of AlCoCrFeNi two-phase high entropy alloy expressed as (AlCoCrFeNi) by atomic percent consisting of 19.8% Al, 19.8% Co, 19.8% Cr, 19.8% Fe, 19.8% Ni and 1% Sc 99 Sc 1 。
The preparation method comprises the following steps:
(1) Weighing Sc blocks, al blocks, co sheets, cr blocks, fe particles and Ni particles according to the atomic ratio to obtain raw materials; the purity of the raw materials is more than 99.95 percent.
(2) Polishing, cleaning and pretreating the selected raw materials and the metal titanium block to remove oxides and impurities on the surface of the metal raw materials, specifically, firstly polishing by using a grinding wheel and abrasive paper, then ultrasonically cleaning in an ethanol solution, and drying for later use;
(3) Sequentially placing the processed raw materials into a crucible of a non-consumable vacuum arc furnace according to the sequence of Al, sc, ni, co, fe and Cr, simultaneously placing a metallic titanium block into another crucible of the non-consumable vacuum arc furnace, and vacuumizing to 5 multiplied by 10 -3 Pa, filling protective gas high-purity argon to-0.05 MPa, repeatedly vacuumizing, filling argon, washing for 3 times, then performing arc-striking smelting, firstly melting a metallic titanium block, with the smelting current of 450A for 3min, adsorbing residual oxygen in an arc furnace chamber in the smelting process, further reducing the oxidation behavior in the smelting process, then smelting an alloy ingot with the smelting current of 550A for 5min, and cooling to obtain the alloy ingot；
(4) And (4) overturning the primary alloy ingot by using a manipulator of the furnace, continuing to smelt again after overturning, and repeatedly smelting for 7 times. Ensuring the uniformity of alloy components, and obtaining Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy (AlCoCrFeNi) after multiple times of smelting is finished and cooling 99 Sc 1 。
Example 2 Laves phase precipitation modification of AlCoCrFeNi Dual-phase high entropy alloy consists of, in atomic percent, 19.6% Al, 19.6% Co, 19.6% Cr, 19.6% Fe, 19.6% Ni and 2% Sc, expressed as (AlCoCrFeNi) 98 Sc 2 。
The preparation method comprises the following steps:
(1) Weighing the Sc blocks, the Al blocks, the Co sheets, the Cr blocks, the Fe particles and the Ni particles according to the atomic ratio to obtain raw materials; the purity of the raw materials is more than 99.95 percent.
(2) Polishing, cleaning and pretreating the selected raw materials and the metal titanium block to remove oxides and impurities on the surface of the metal raw materials, specifically, firstly polishing by using a grinding wheel and abrasive paper, then ultrasonically cleaning in an ethanol solution, and drying for later use;
(3) Sequentially placing the processed raw materials into a crucible of a non-consumable vacuum arc furnace according to the sequence of Al, sc, ni, co, fe and Cr, simultaneously placing a metallic titanium block into another crucible of the non-consumable vacuum arc furnace, and vacuumizing to 5 multiplied by 10 -3 Pa, filling protective gas high-purity argon to-0.05 MPa, repeatedly vacuumizing, filling argon, washing for 3 times, then performing arc striking smelting, firstly melting a metal titanium block, with the smelting current of 450A for 3min, adsorbing residual oxygen in an arc furnace chamber in the smelting process, further reducing the oxidation behavior in the smelting process, then smelting an alloy ingot with the smelting current of 550A for 5min, and cooling to obtain the alloy ingot;
(4) And (3) overturning the primary molten alloy ingot by using a manipulator of the furnace, continuously smelting again after overturning, and repeatedly smelting for 7 times. Ensuring the uniformity of alloy components, and cooling to obtain Laves phase precipitation modified AlCoCrFeNi biphase high-entropy alloy (AlCoCrFeNi) after multiple times of smelting 98 Sc 2 。
Comparative example 1 an AlCoCrFeNi high entropy alloyThe atomic percent consists of 20% Al, 20% Co, 20% Cr, 20Fe and 20% Ni, expressed as Al 20 Co 20 Cr 20 Fe 20 Ni 20 Or AlCoCrFeNi.
The preparation method comprises the following steps:
(1) Weighing Al blocks, co sheets, cr blocks, fe particles and Ni particles according to the atomic ratio to obtain raw materials; the purity of the raw materials is more than 99.95 percent.
(2) Polishing, cleaning and pretreating the selected raw materials and the metal titanium block to remove oxides and impurities on the surface of the metal raw materials, specifically, firstly polishing by using a grinding wheel and abrasive paper, then ultrasonically cleaning in an ethanol solution, and drying for later use;
(3) Sequentially putting the processed raw materials into a crucible of a non-consumable vacuum electric arc furnace according to the sequence of Al, ni, co, fe and Cr, simultaneously putting a metal titanium block into another crucible of the non-consumable vacuum electric arc furnace, and vacuumizing to 5 multiplied by 10 -3 Pa, introducing protective gas high-purity argon to-0.05 MPa, then carrying out arc striking smelting, firstly melting a metal titanium block, wherein the smelting current is 450A, the time is 3min, adsorbing oxygen remained in an arc furnace chamber in the smelting process, further reducing the oxidation behavior in the smelting process, then smelting an alloy ingot, wherein the smelting current is 550A, the time is 5min, and cooling to obtain the alloy ingot;
(4) And (4) overturning the primary alloy ingot by using a manipulator of the furnace, continuing to smelt again after overturning, and repeatedly smelting for 7 times. The uniformity of alloy components is ensured, and AlCoCrFeNi high-entropy alloy is obtained after multiple times of smelting.
FIG. 1 shows the XRD diffraction patterns of the high entropy alloys of examples 1 and 2 and comparative example 1; wherein, the O is BBC (A2), □ is BBC (B2), and the T is Laves phase. As can be seen from FIG. 1, examples 1 and 2 and comparative example 1 both contained a BCC phase. With the gradual introduction of Sc element, an XRD diffraction peak is shifted negatively, and scandium atoms cause more serious lattice distortion to an AlCoCrFeNi matrix. The XRD diffraction pattern of example 2 exhibited Laves phases as compared to comparative example 1, wherein the Laves phases are (Ni, co) 2 Sc。
Based on scanning electron microscope (AlCoCrFeNi) 100-x Sc x Microstructure of alloy sampleThe structure was observed, and the results are shown in FIG. 2. It can be seen that the comparative examples are homogeneous in texture and exhibit a single-phase BCC structure. For example 1, a hypoeutectic structure consisting of primary phase BCC and eutectic regions, including BCC phase and Laves phase, alternately grown, appeared. Furthermore, the Laves phase in example 1 was not found in the corresponding XRD patterns because the Laves phase content was too low. For example 2, the content of the Laves phase in the alloy system is obviously increased. The addition of scandium reduces the grain size, mainly because the large atomic radius of scandium is repelled by primary phase BCC and segregates to the grain boundary, laves phase is formed at the grain boundary, and the Laves phase separated out at the grain boundary hinders the growth of the primary BCC phase and further induces grain refinement.
FIG. 3 shows the results of microhardness of the high entropy alloys of examples 1 and 2 and comparative example 1. The results show that scandium addition has a strong correlation with the hardness of the alloy. As the atomic percent Sc content increases, the volume fraction of the Laves phase gradually increases from 0vol.% to 8.1vol.%, and the microhardness increases from 508HV (comparative example 1) to 632HV (example 2). The increase in microhardness of examples 1 and 2 is mainly due to solid solution strengthening, second phase strengthening and fine grain strengthening.
Based on HT-1000 ball disk type friction and wear instrument pair (AlCoCrFeNi) 100-x Sc x The high-entropy alloy is subjected to a 5N dry friction and wear experiment, and the friction pair is Si 3 N 4 The slip speed was 300rpm and the slip time was 30 minutes. FIG. 4 shows the wear rate results for the high entropy alloys of examples 1 and 2 and comparative example. The wear rates of the high-entropy alloys of examples 1 and 2 and the comparative example are 3.96X 10 -5 m 3 ·N -1 ·m -1 、3.41×10 -5 m 3 ·N -1 ·m -1 、6.72×10 -5 m 3 ·N -1 ·m -1 . Therefore, the wear rate is greatly reduced along with the increase of the hardness of the high-entropy alloy, which is consistent with Archard's law, namely, the wear resistance and the hardness of the material are in a positive correlation relationship. It can be seen that the wear resistance of examples 1, 2 is greatly improved.
Claims (10)
1. A Laves phase precipitation modified AlCoCrFeNi biphase high-entropy alloy is characterized in that the alloy consists of Al, co, cr, fe, ni and Sc elements, and the expression is (AlCoCrFeNi) 100-x Sc x And x is 1 or 2, wherein Al, co, cr, fe and Ni are in equal atomic ratio.
2. The Laves phase modified AlCoCrFeNi dual phase high entropy alloy of claim 1, wherein the Laves phase modified AlCoCrFeNi dual phase high entropy alloy comprises, in atomic percent, 19.8% al, 19.8% co, 19.8% cr, 19.8% fe, 19.8% ni and 1% sc composition, expressed as (AlCoCrFeNi) 99 Sc 1 。
3. A Laves phase modified AlCoCrFeNi dual phase high entropy alloy of claim 1, wherein the Laves phase modified AlCoCrFeNi dual phase high entropy alloy comprises, in atomic percent, 19.6% al, 19.6% co, 19.6% cr, 19.6% fe, 19.6% ni and 2% sc, expressed as (AlCoCrFeNi) 98 Sc 2 。
4. The preparation method of the Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy as claimed in claim 1, characterized in that the preparation method comprises the following steps: 1. according to the expression (AlCoCrFeNi) 100-x Sc x Weighing Al, co, cr, fe, ni and Sc according to the atomic percentage to obtain raw materials; wherein x is 1 or 2, al, co, cr, fe, ni are equal atomic ratio;
2. pretreating raw materials and a titanium block, adding the raw materials into a crucible of a smelting furnace in the sequence of Al, sc, ni, co, fe and Cr from bottom to top, adding the titanium block into another crucible of the smelting furnace, vacuumizing the smelting furnace, introducing argon for protection, smelting the titanium block, smelting the raw materials, and cooling to obtain an alloy ingot;
3. repeatedly smelting the alloy ingot for 6-8 times, and cooling to obtain a Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy; wherein the alloy ingot is turned over each time of melting.
5. A method of producing a Laves phase segregation modified AlCoCrFeNi two-phase high entropy alloy according to claim 4, characterized in that step one weighs Al, co, cr, fe, ni and Sc in proportions such as 19.8% by atomic percent Al, 19.8% Co, 19.8% by weight of Cr, 19.8% by weight of Fe, 19.8% by weight of Ni and 1% by weight of Sc.
6. The method of claim 4, wherein the first step comprises weighing Al, co, cr, fe, ni and Sc at a ratio of 19.6 at% Al, 19.6 at% Co, 19.6 at% Cr, 19.6 at% Fe, 19.6 at% Ni, 2 at% Sc.
7. The method for preparing the Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy as claimed in claim 4, wherein the pretreatment in the second step is grinding and polishing, cleaning and drying.
8. The method for preparing the Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy as claimed in claim 4, wherein in the second step, the vacuum pumping is performed until the temperature is 5 x 10 -3 And introducing protective gas high-purity argon to-0.05 MPa after Pa.
9. The preparation method of the Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy according to claim 4, wherein the current intensity in the second step of smelting is 450-550A.
10. The preparation method of the Laves phase precipitation modified AlCoCrFeNi two-phase high-entropy alloy as claimed in claim 4, wherein the step three is carried out after the last melting and is cooled with the furnace for 20-30min.
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| CN116479303A (en) * | 2023-04-20 | 2023-07-25 | 哈尔滨工业大学 | Al-Co-Cr-Fe-Ni-Ta high-strength high-entropy alloy applied in high-temperature environment and preparation method thereof |
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