CN117070822A - Co-free CrFe 1.5 Ni 1.5 Nb x Eutectic medium-entropy alloy and preparation method thereof - Google Patents
Co-free CrFe 1.5 Ni 1.5 Nb x Eutectic medium-entropy alloy and preparation method thereof Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 85
- 239000000956 alloy Substances 0.000 title claims abstract description 85
- 230000005496 eutectics Effects 0.000 title claims abstract description 51
- 229910002467 CrFe Inorganic materials 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 230000008018 melting Effects 0.000 claims abstract description 54
- 238000002844 melting Methods 0.000 claims abstract description 54
- 239000000126 substance Substances 0.000 claims abstract description 48
- 239000002184 metal Substances 0.000 claims abstract description 45
- 229910052751 metal Inorganic materials 0.000 claims abstract description 45
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 229910052786 argon Inorganic materials 0.000 claims abstract description 10
- 238000010891 electric arc Methods 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 238000003723 Smelting Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 description 10
- 238000011010 flushing procedure Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005728 strengthening Methods 0.000 description 3
- 238000005266 casting Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000006023 eutectic alloy Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001068 laves phase Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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Abstract
The invention discloses Co-free CrFe 1.5 Ni 1.5 Nb x The eutectic entropy alloy comprises Cr, fe, ni and Nb in a molar ratio of 1:1.5:1.5: x, wherein x is more than 0.2 and less than 0.9; the method comprises the following steps: step 1, according to the mole ratio of 1:1.5:1.5: weighing pure Cr, fe, ni, nb metal simple substance, wherein x is more than 0.2 and less than 0.9; step 2, placing pure Cr, fe, ni, nb metal simple substances into a water-cooled crucible in a non-consumable arc melting furnace in sequence from low melting point to high melting point, repeatedly vacuumizing the non-consumable arc melting furnace, charging argon, repeatedly melting by utilizing an electric arc, and cooling to room temperature to obtain Co-free CrFe 1.5 Ni 1.5 Nb x The eutectic medium entropy alloy not only prepares the CrFe with low price and strong toughness 1.5 Ni 1.5 Nb x In eutectic crystalThe entropy alloy has simple and easily controlled preparation method.
Description
Technical Field
The invention relates to a medium entropy alloy, in particular to Co-free CrFe 1.5 Ni 1.5 Nb x Eutectic medium entropy alloy and a preparation method thereof.
Background
The medium-entropy alloy has high strength, high hardness, high wear resistance and excellent corrosion resistance, and the high-entropy alloy in single-phase FCC has good toughness but lower strength; the single-phase BCC has higher strength and poorer toughness, which limits the engineering application of the single-phase BCC, and meanwhile, the single-phase BCC has poorer fluidity and castability, and is easy to form metallurgical defects in different forms in cast ingots, which limits the engineering application of the single-phase BCC. The eutectic structure is formed through reasonable component design, and the eutectic medium entropy alloy can have the advantages of both the eutectic alloy and the medium entropy alloy, so that the alloy has good casting performance and excellent mechanical property and chemical property, thereby meeting the actual engineering production and application.
At present, coCrFeNi-based eutectic high-entropy alloy has excellent mechanical and chemical properties, which causes extensive research at home and abroad, and Jiang et al report that the eutectic high-entropy alloy CoCrFeNiTa consists of FCC phase and Laves phase 0.4 The breaking strength is up to 2290MPa, and the compressive strain is kept at 22.6%, so that the alloy has good toughness and coordination; jiang and Chandd et al report eutectic high entropy alloys CoCrFeNiNb 0.45 The microstructure of the alloy consists of fine regular lamellar FCC/Laves, the breaking strength of the alloy is 2200MPa, and the compressive strain is 17.5%; ye et al report that the eutectic medium entropy alloy CoCrFeNi-Nb 6 Ta 4 The room temperature fracture strength of the alloy is 2401MPa, and the compressive strain is 30%. Although the above reported eutectic high-entropy alloy has excellent mechanical properties, the alloy contains expensive and rare Co elements, so that the cost of the alloy is high, which severely limits the industrial application of the alloy, and therefore, on the basis of ensuring the excellent properties, the development of Co-free eutectic medium-entropy alloy is a key problem to be solved urgently.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a Co-free CrFe 1.5 Ni 1.5 Nb x The eutectic medium entropy alloy and the preparation method thereof not only prepare the CrFe with low price and strong toughness 1.5 Ni 1.5 Nb x The eutectic medium entropy alloy has simple and easily controlled preparation method.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
co-free CrFe 1.5 Ni 1.5 Nb x The eutectic entropy alloy comprises Cr, fe, ni and Nb in a molar ratio of 1:1.5:1.5: x, wherein 0.2 < x < 0.9.
Further, primary phase Laves and lamellar FCC/Laves eutectic are included.
Co-free CrFe 1.5 Ni 1.5 Nb x The preparation method of the eutectic entropy alloy comprises the following steps:
step 1, according to the mole ratio of 1:1.5:1.5: weighing pure Cr, fe, ni, nb metal simple substance, wherein x is more than 0.2 and less than 0.9;
step 2, placing pure Cr, fe, ni, nb metal simple substances into a water-cooled crucible in a non-consumable arc melting furnace in sequence from low melting point to high melting point, repeatedly vacuumizing the non-consumable arc melting furnace, charging argon, repeatedly melting by utilizing an electric arc, and cooling to room temperature to obtain Co-free CrFe 1.5 Ni 1.5 Nb x Eutectic mid-entropy alloy.
Further, the step 1 further comprises the steps of respectively placing the Cr, fe, ni, nb metal simple substance raw materials into absolute ethyl alcohol, cleaning for 15-20 min by utilizing ultrasonic waves, and drying by using a blower to obtain pure Cr, fe, ni, nb metal simple substances.
Further, the Cr, fe, ni, nb metal elemental raw materials are Cr flakes having a purity of 99.95%, fe particles having a purity of 99.95%, ni particles having a purity of 99.95%, and Nb blocks having a purity of 99.95%, respectively.
Further, the non-consumable arc melting furnace in the step 2 is provided with at least two water-cooled crucibles, wherein one water-cooled crucible is used for placing pure Cr, fe, ni, nb metal simple substance, and the other water-cooled crucible is internally provided with metal Ti simple substance for removing residual oxygen in the furnace.
Further, the step 2 repeatedly vacuumizes the non-consumable arc melting furnace until the vacuum degree in the furnace body is 3 multiplied by 10 -3 ～6×10 -3 Pa。
Further, in the step 2, after the non-consumable arc melting furnace is repeatedly vacuumized and flushed with argon, the air pressure in the furnace body is 0.05Pa.
Further, the process of repeatedly smelting by using the electric arc in the step 2 is as follows: firstly smelting Cr, fe, ni, nb metal simple substance for 4-5 min by utilizing an electric arc, obtaining an alloy cast ingot after cooling, re-remelting the alloy cast ingot for 4-5 min by utilizing the electric arc after overturning the alloy cast ingot, remelting for 5 times, and cooling to room temperature along with a furnace to obtain Co-free CrFe 1.5 Ni 1.5 Nb x Eutectic mid-entropy alloy.
Compared with the prior art, the invention has the following technical effects:
the chemical formula of the medium entropy alloy designed by the invention is CrFe 1.5 Ni 1.5 Nb x Wherein x is more than 0.2 and less than 0.9, and CrFe is a medium entropy alloy 1.5 Ni 1.5 Based on the method, the Co element in the existing eutectic medium-entropy alloy is replaced, and an eutectic structure is formed by adding Nb element, so that the production cost is reduced, and the toughness of the medium-entropy alloy is improved.
The invention utilizes vacuum arc melting technology to smelt the pre-configured metal simple substance, and improves the alloy by means of multiple toughening mechanisms such as solid solution strengthening, complex phase strengthening, eutectic interface toughening, fine grain toughening and the likeToughness, and the prepared intermediate entropy alloy is CrFe 1.5 Ni 1.5 Nb x The room temperature yield strength is 1448+/-39 MPa, the room temperature breaking strength can reach 2081+/-40 MPa, the room temperature breaking strength is high, the breaking strain is kept at 13.23+/-1.05%, the room temperature breaking strength has good plasticity, the room temperature breaking strength further has good casting performance, the room temperature breaking strength is not subjected to any heat treatment process and deformation strengthening process treatment, the large-size special-shaped component with uniform components, fine tissues and compact structures can be obtained through simple solidification, and the preparation method is simple and easy to control, and is suitable for large-scale engineering production and application.
Drawings
Fig. 1: co-free CrFe prepared in example 1 of the present invention 1.5 Ni 1.5 Nb 0.61 XRD pattern of entropy alloy in the eutectic;
fig. 2: co-free CrFe prepared in example 1 of the present invention 1.5 Ni 1.5 Nb 0.61 A low-magnification SEM image of the eutectic mid-entropy alloy;
fig. 3: co-free CrFe prepared in example 1 of the present invention 1.5 Ni 1.5 Nb 0.61 High-magnification SEM image of the eutectic mid-entropy alloy;
fig. 4: co-free CrFe prepared in example 1 of the present invention 1.5 Ni 1.5 Nb x Room temperature compressive stress-strain curve for an entropy alloy in a eutectic.
Detailed Description
The following examples illustrate the invention in further detail.
The Cr, fe, ni, nb metal simple substance raw materials selected in the embodiment 1 to the embodiment 5 of the invention are respectively Cr tablets with the purity of 99.95 percent, fe particles with the purity of 99.95 percent, ni particles with the purity of 99.95 percent and Nb blocks with the purity of 99.95 percent, and the chemical formula of the prepared Co-free medium entropy alloy is CrFe 1.5 Ni 1.5 Nb x Wherein x is more than 0.2 and less than 0.9.
Example 1
Step 1, respectively placing Cr, fe, ni, nb metal simple substance raw materials into absolute ethyl alcohol, cleaning for 15-20 min by utilizing ultrasonic waves, and drying by using a blower to obtain pure Cr, fe, ni, nb metal simple substance;
step 2, according to the mole ratio of 1:1.5:1.5: weighing pure Cr, fe, ni, nb metal simple substance by x, wherein x=0.61;
step 3, placing pure Cr, fe, ni, nb metal simple substances into one of the water-cooled crucibles in the non-consumable arc melting furnace in sequence from low melting point to high melting point, placing metal Ti simple substances for removing residual oxygen in the furnace into the other water-cooled crucible, and repeatedly vacuumizing the non-consumable arc melting furnace and flushing argon gas into the non-consumable arc melting furnace to ensure that the vacuum degree in the furnace body is 3 multiplied by 10 -3 Pa, the air pressure is 0.05Pa, an electromagnetic stirring switch is started, arc melting is started under electromagnetic stirring, melting is carried out for 4min, alloy cast ingots are obtained after cooling, arc remelting is carried out for 4min again after the alloy cast ingots are overturned, remelting is repeated for 5 times, and the alloy cast ingots are cooled to room temperature along with a furnace to obtain Co-free CrFe 1.5 Ni 1.5 Nb 0.61 Eutectic mid-entropy alloy.
As can be seen from FIG. 1, example 1 produced Co-free CrFe comprising both FCC and Laves alloy phase structures 1.5 Ni 1.5 Nb 0.61 Eutectic mid-entropy alloy.
As can be seen from FIGS. 2 and 3, co-free CrFe prepared in example 1 1.5 Ni 1.5 Nb 0.61 The entropy alloy in the eutectic consists of Laves primary phase and FCC/Laves eutectic lamellar sheets.
Co-free CrFe prepared from example 1 1.5 Ni 1.5 Nb x Taking three samples of the eutectic entropy alloy and sequentially taking the samples as a sample 1, a sample 2 and a sample 3 (sequentially marked as 1, 2 and 3), testing the mechanical properties of the samples at room temperature, and drawing a room temperature compression stress-strain curve, wherein specific mechanical property parameters are shown in a table 1; as can be seen from the room temperature compressive stress-strain curve of FIG. 4, co-free CrFe prepared in example 1 1.5 Ni 1.5 Nb x The breaking strength of the entropy alloy in the eutectic is 2081+/-40 MPa, the breaking strain is 13.23+/-1.05%, and after being treated by origin, the room temperature yield strength is 1448+/-39 MPa, and the alloy has good toughness.
Table 1: co-free CrFe prepared in example 1 1.5 Ni 1.5 Nb x Mechanical property parameter of eutectic medium-entropy alloy
Example 2
Step 1, respectively placing Cr, fe, ni, nb metal simple substance raw materials into absolute ethyl alcohol, cleaning for 15-20 min by utilizing ultrasonic waves, and drying by using a blower to obtain pure Cr, fe, ni, nb metal simple substance;
step 2, according to the mole ratio of 1:1.5:1.5: weighing pure Cr, fe, ni, nb metal simple substance by x, wherein x=0.21;
step 3, placing pure Cr, fe, ni, nb metal simple substances into one of the water-cooled crucibles in the non-consumable arc melting furnace in sequence from low melting point to high melting point, placing metal Ti simple substances for removing residual oxygen in the furnace into the other water-cooled crucible, and repeatedly vacuumizing the non-consumable arc melting furnace and flushing argon gas into the non-consumable arc melting furnace to ensure that the vacuum degree in the furnace body is 4 multiplied by 10 -3 Pa, the air pressure is 0.05Pa, an electromagnetic stirring switch is started, arc melting is started under electromagnetic stirring, the melting is carried out for 5min, alloy cast ingots are obtained after cooling, arc remelting is carried out for 5min after the alloy cast ingots are overturned, remelting is repeated for 5 times in this way, and the alloy cast ingots are cooled to room temperature along with a furnace to obtain Co-free CrFe 1.5 Ni 1.5 Nb 0.21 Eutectic mid-entropy alloy.
Example 3
Step 1, respectively placing Cr, fe, ni, nb metal simple substance raw materials into absolute ethyl alcohol, cleaning for 15-20 min by utilizing ultrasonic waves, and drying by using a blower to obtain pure Cr, fe, ni, nb metal simple substance;
step 2, according to the mole ratio of 1:1.5:1.5: weighing pure Cr, fe, ni, nb metal simple substance by x, wherein x=0.89;
step 3, placing pure Cr, fe, ni, nb metal simple substances into a non-consumable arc in sequence from low melting point to high melting pointPlacing metal Ti simple substance for removing residual oxygen in one water-cooled crucible in the smelting furnace, and then repeatedly vacuumizing and flushing argon into the non-consumable arc smelting furnace to make the vacuum degree in the furnace body be 5 multiplied by 10 -3 Pa, the air pressure is 0.05Pa, an electromagnetic stirring switch is started, arc melting is started under electromagnetic stirring, the melting is carried out for 5min, alloy cast ingots are obtained after cooling, arc remelting is carried out for 5min after the alloy cast ingots are overturned, remelting is repeated for 5 times in this way, and the alloy cast ingots are cooled to room temperature along with a furnace to obtain Co-free CrFe 1.5 Ni 1.5 Nb 0.89 Eutectic mid-entropy alloy.
Example 4
Step 1, respectively placing Cr, fe, ni, nb metal simple substance raw materials into absolute ethyl alcohol, cleaning for 15-20 min by utilizing ultrasonic waves, and drying by using a blower to obtain pure Cr, fe, ni, nb metal simple substance;
step 2, according to the mole ratio of 1:1.5:1.5: weighing pure Cr, fe, ni, nb metal simple substance by x, wherein x=0.4;
step 3, placing pure Cr, fe, ni, nb metal simple substances into one of the water-cooled crucibles in the non-consumable arc melting furnace in sequence from low melting point to high melting point, placing metal Ti simple substances for removing residual oxygen in the furnace into the other water-cooled crucible, and repeatedly vacuumizing the non-consumable arc melting furnace and flushing argon gas into the non-consumable arc melting furnace to ensure that the vacuum degree in the furnace body is 6 multiplied by 10 -3 Pa, the air pressure is 0.05Pa, an electromagnetic stirring switch is started, arc melting is started under electromagnetic stirring, melting is carried out for 4min, alloy cast ingots are obtained after cooling, arc remelting is carried out for 4min after the alloy cast ingots are overturned, remelting is repeated for 4 times in this way, and the alloy cast ingots are cooled to room temperature along with a furnace to obtain Co-free CrFe 1.5 Ni 1.5 Nb 0.4 Eutectic mid-entropy alloy.
Example 5
Step 1, respectively placing Cr, fe, ni, nb metal simple substance raw materials into absolute ethyl alcohol, cleaning for 15-20 min by utilizing ultrasonic waves, and drying by using a blower to obtain pure Cr, fe, ni, nb metal simple substance;
step 2, according to the mole ratio of 1:1.5:1.5: weighing pure Cr, fe, ni, nb metal simple substance by x, wherein x=0.5;
step 3, placing pure Cr, fe, ni, nb metal simple substances into one of the water-cooled crucibles in the non-consumable arc melting furnace in sequence from low melting point to high melting point, placing metal Ti simple substances for removing residual oxygen in the furnace into the other water-cooled crucible, and repeatedly vacuumizing the non-consumable arc melting furnace and flushing argon gas into the non-consumable arc melting furnace to ensure that the vacuum degree in the furnace body is 3 multiplied by 10 -3 Pa, the air pressure is 0.05Pa, an electromagnetic stirring switch is started, arc melting is started under electromagnetic stirring, the melting is carried out for 5min, alloy cast ingots are obtained after cooling, arc remelting is carried out for 5min after the alloy cast ingots are overturned, remelting is repeated for 5 times in this way, and the alloy cast ingots are cooled to room temperature along with a furnace to obtain Co-free CrFe 1.5 Ni 1.5 Nb 0.5 Eutectic mid-entropy alloy.
Claims (9)
1. Co-free CrFe 1.5 Ni 1.5 Nb x The eutectic entropy alloy is characterized in that the components comprise Cr, fe, ni and Nb, and the molar ratio of Cr, fe, ni and Nb is 1:1.5:1.5: x, wherein 0.2 < x < 0.9.
2. Co-free CrFe according to claim 1 1.5 Ni 1.5 Nb x An eutectic mid-entropy alloy comprising a Laves primary phase and FCC/Laves eutectic lamellae.
3. Co-free CrFe as claimed in claim 1 or 2 1.5 Ni 1.5 Nb x The preparation method of the eutectic entropy alloy is characterized by comprising the following steps of:
step 1, according to the mole ratio of 1:1.5:1.5: weighing pure Cr, fe, ni, nb metal simple substance, wherein x is more than 0.2 and less than 0.9;
step 2, placing pure Cr, fe, ni, nb metal simple substances into a water-cooled crucible in a non-consumable arc melting furnace in sequence from low melting point to high melting point, repeatedly vacuumizing the non-consumable arc melting furnace, charging argon, repeatedly melting by utilizing an electric arc, and cooling to room temperature to obtain Co-free CrFe 1.5 Ni 1.5 Nb x Eutectic mid-entropy alloy.
4. The Co-free CrFe according to claim 3 1.5 Ni 1.5 Nb x The preparation method of the eutectic entropy alloy is characterized by further comprising the step 1 of respectively placing Cr, fe, ni, nb metal simple substance raw materials into absolute ethyl alcohol, cleaning for 15-20 min by utilizing ultrasonic waves, and drying by using a blower to obtain pure Cr, fe, ni, nb metal simple substances.
5. Co-free CrFe according to claim 4 1.5 Ni 1.5 Nb x The preparation method of the eutectic entropy alloy is characterized in that the Cr, fe, ni, nb metal simple substance raw materials are Cr pieces with the purity of 99.95 percent, fe particles with the purity of 99.95 percent, ni particles with the purity of 99.95 percent and Nb blocks with the purity of 99.95 percent respectively.
6. The Co-free CrFe according to claim 3 1.5 Ni 1.5 Nb x The preparation method of the eutectic medium-entropy alloy is characterized in that the non-consumable arc melting furnace in the step 2 is internally provided with at least two water-cooled crucibles, wherein one water-cooled crucible is used for placing pure Cr, fe, ni, nb metal simple substance, and the other water-cooled crucible is internally provided with metal Ti simple substance for removing residual oxygen in the furnace.
7. The Co-free CrFe according to claim 3 1.5 Ni 1.5 Nb x The preparation method of the eutectic medium-entropy alloy is characterized in that the step 2 is to repeatedly vacuumize a non-consumable arc melting furnace until the vacuum degree in the furnace body is 3 multiplied by 10 -3 ～6×10 -3 Pa。
8. The Co-free CrFe according to claim 3 1.5 Ni 1.5 Nb x The preparation method of the eutectic medium-entropy alloy is characterized in that the step 2 is characterized in that after the non-consumable arc melting furnace is repeatedly vacuumized and argon is flushed, the air pressure in the furnace body is 0.05Pa.
9. The Co-free CrFe according to claim 3 1.5 Ni 1.5 Nb x The preparation method of the eutectic medium-entropy alloy is characterized in that the repeated smelting process of the step 2 by utilizing electric arcs is as follows: firstly smelting Cr, fe, ni, nb metal simple substance in a water-cooled crucible for 4-5 min by utilizing an electric arc, obtaining an alloy cast ingot after cooling, remelting the alloy cast ingot for 4-5 min again by utilizing the electric arc after overturning the alloy cast ingot, remelting for 5 times, and cooling to room temperature along with a furnace to obtain Co-free CrFe 1.5 Ni 1.5 Nb x Eutectic mid-entropy alloy.
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