CN105755324A - High-entropy alloy with high strength and toughness and preparation method thereof - Google Patents
High-entropy alloy with high strength and toughness and preparation method thereof Download PDFInfo
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- CN105755324A CN105755324A CN201610116965.6A CN201610116965A CN105755324A CN 105755324 A CN105755324 A CN 105755324A CN 201610116965 A CN201610116965 A CN 201610116965A CN 105755324 A CN105755324 A CN 105755324A
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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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- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
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- 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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention discloses a high-entropy alloy with high strength and toughness and a preparation method thereof, and belongs to the field of metallic materials. The high-entropy alloy is AlaCrbFecNidVe according to a mole ratio; the method comprises: firstly, putting Al, Cr, Fe, Ni and V into a melting furnace, performing electric arc melting at a certain vacuum degree under the protection of a gas to obtain alloy liquid, and performing stirring and cooling to obtain an alloy ingot; and overturning the alloy ingot, and then performing electric arc melting, stirring and cooling to obtain the AlCrFeNiV high-entropy alloy. The high-entropy alloy is simple in structure, excellent in mechanical property, and relatively good in strength and toughness matching; and the method is simple and reliable, and is good in safety and high in economic value.
Description
Technical field
The present invention relates to a kind of high-entropy alloy having intensity and toughness concurrently and preparation method thereof, belong to metal material field.
Background technology
High-entropy alloy is the class novel alloy grown up in new alloy design concept in recent years.It is made up of four kinds and above essential element, can add minor element accordingly.Every kind of essential element molar content is more than 5%, and secondary addition element molar content is less than 5%.Being different from the single pivot of conventional alloys, the high-entropy alloy of many pivots has exclusive high entropic effect, big distortion of lattice effect, sluggish spreading effect and cocktail effect.These features make the comprehensive mechanical property excellence of high-entropy alloy, and high-entropy alloy breaches the development restriction of the single pivot of conventional alloys, and this has widened the research range of alloy greatly.
At present, the research of high-entropy alloy relates generally to design of alloy, phase formation mechenism, mainly comprises the impact of element alloy tissue, mechanical property, the heat treatment impact on high-entropy alloy tissue and performance, preparation and application etc..There are some researches show that the general plasticity of high intensity high-entropy alloy is very poor, and the high-entropy alloy common intensity of excellent plasticity is relatively low, is difficulty with the coupling of intensity and toughness.Such as AlCoCrFeNiTi0.5The compressive strength of high-entropy alloy is up to 3200MPa, but does not have stretching plastic；The stretching plastic of CoCrFeNi high-entropy alloy is more than 60%, but tensile strength is less than 500MPa.
Summary of the invention
For the problem of existing high-entropy alloy obdurability coupling difference, an object of the present invention is in that to provide a kind of high-entropy alloy having intensity and toughness concurrently, described high-entropy alloy excellent in mechanical performance, and obdurability coupling is better；The two of purpose are in that the preparation method providing a kind of high-entropy alloy having intensity and toughness concurrently, described method, and simple and reliable, safety is good, and economic worth is high.
The purpose of the present invention is realized by techniques below scheme:
A kind of high-entropy alloy having intensity and toughness concurrently, described high-entropy alloy is calculated in molar ratio as AlaCrbFecNidVe, wherein, a=0.5～1.0, b=0.9～1.0, c=0.8～1.0；D=1.5～3.0；E=0.1～0.3；
Described a, b, c, preferred a=0.5～0.75 of value of d and e, b=0.9, c=1.0, d=2.0～3.0 and e=0.2.
The preparation method of a kind of high-entropy alloy having intensity and toughness concurrently, described method specifically comprises the following steps that
(1) Al, Cr, Fe, Ni and V are placed in smelting furnace, under the protection of protective gas, in vacuum less than or equal to 1.0 × 103Carry out electric arc melting under MPa, obtain aluminium alloy, stirring, cooling, obtain alloy pig；
Wherein, described stirring is magnetic field agitation；The preferred argon of described protective gas；The preferred fine vacuum non-consumable arc-melting furnace of described smelting furnace；
Described Al, Cr, Fe, Ni and V purity are be more than or equal to 99.7wt%；
(2) electric arc melting in step (1), stirring and cooling procedure are repeated after being overturn by alloy pig；
(3) repeat step more than (2) 2 times, obtain the high-entropy alloy having intensity and toughness concurrently of the present invention.Beneficial effect
(1) excellent in mechanical performance of high-entropy alloy of the present invention, obdurability coupling is better；
(2) high-entropy alloy of the present invention has the heat stability of excellence, measures alloy heating through DSC and occurs without phase transformation to fusing；
(3) preparation method of the present invention is simple and reliable, and several elements of selection are all nontoxic and obtain conveniently, and safety is good, and economic worth is high.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) spectrogram of the high-entropy alloy that embodiment prepares；
Fig. 2 is the Al that embodiment 1 prepares0.5Cr0.9Fe0.8Ni1.5V0.1The optical microscope photograph of high-entropy alloy；
Fig. 3 is the Al that embodiment 2 prepares0.5Cr0.9FeNi2.5V0.2The optical microscope photograph of high-entropy alloy；
Fig. 4 is the AlCrFeNi that embodiment 3 prepares3.0V0.3The optical microscope photograph of high-entropy alloy；
Fig. 5 is the Al that embodiment 1 prepares0.5Cr0.9Fe0.8Ni1.5V0.1Scanning electron microscope (SEM) photo of high-entropy alloy；
Fig. 6 is the Al that embodiment 2 prepares0.5Cr0.9FeNi2.5V0.2Scanning electron microscope (SEM) photo of high-entropy alloy；
Fig. 7 is the AlCrFeNi that embodiment 3 prepares3.0V0.3Scanning electron microscope (SEM) photo of high-entropy alloy；
Fig. 8 is the tensile stress-strain curve of the high-entropy alloy that embodiment prepares；
Fig. 9 is the DSC heating curve of the high-entropy alloy that embodiment prepares；
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments in detail the present invention is described in detail, but is not limited to this.
The fine vacuum non-consumable arc-melting furnace used in following example is the DHL-400 type fine vacuum non-consumable arc-melting furnace that CAS Shenyang Scientific Instruments Co., Ltd. produces；
The Mechanics Performance Testing of gained high-entropy alloy, organizational structure and heat stability characterization information is as follows:
(1) material phase analysis: adopting Rigaku company SMARTLABX x ray diffractometer x to carry out material phase analysis, running voltage and electric current respectively 40KV and 190mA, x-ray source is CuK α (λ=0.1542nm) ray.
(2) microstructure: adopt Germany's AxioobserverA1m type research grade metallurgical microscope and HITACHIS4800 type cold field emission scanning electron microscope to carry out microstructure sign；
(3) quasi-static tensile Mechanics Performance Testing: adopt CMT4305 type computer electronic universal testing machine to carry out room temperature quasi-tensile test, test sample makes I-shaped part sample, strain rate 10 according to pertinent regulations in metal material tensile testing at ambient temperature (GB/T228.1-2010) national standard-3s-1；
(4) heat is analyzed: adopt differential scanning calorimetry (DSC) to carry out heat analysis, and it is Germany NETZSCHDSC404F3 that DSC tests instrument, and test sample is flake, diameter is 4mm, thickness is 0.5mm, and quality is less than 20mg, and test heating rate is 10K/s.
Simple substance Al described in following example, Cr, Fe, Ni and V purity be 99.9wt%.
Embodiment 1
The preparation method of a kind of high-entropy alloy having intensity and toughness concurrently, described high-entropy alloy is calculated in molar ratio as Al0.5Cr0.9Fe0.8Ni1.5V0.1；Described method specifically comprises the following steps that
(1) utilizing No. 60 SiC sand paper and abrasive machine to remove simple substance Al, Cr, Fe, Ni and V surface impurity and oxide, then use acetone to clean, weighing gross mass is the Al of 80g, Cr, Fe, Ni and V, and ultrasonic cleaning twice；
(2) Al after ultrasonic cleaning, Cr, Fe, Ni and V are placed in fine vacuum non-consumable arc-melting furnace, under the protection of argon, in vacuum less than or equal to 1.0 × 103Carry out electric arc melting under MPa, obtain aluminium alloy, stirring, cooling, obtain alloy pig；
(3) electric arc melting in step (1), stirring and cooling procedure are repeated after being overturn by alloy pig；
(4) repeat step (3) 2 times, obtain Al described in the present embodiment0.5Cr0.9Fe0.8Ni1.5V0.1High-entropy alloy.
With abrasive machine by gained Al0.5Cr0.9Fe0.8Ni1.5V0.1High-entropy alloy surface scale is removed, and then with acetone ultrasonic cleaning twice, cleaner alloy pig is placed in fine vacuum electric arc melting turnover casting and spun casting system, is cast in the mould of diameter 20mm and obtains Al after remelting0.5Cr0.9Fe0.8Ni1.5V0.1High-entropy alloy test specimens.
To described Al0.5Cr0.9Fe0.8Ni1.5V0.1High-entropy alloy test specimens carries out material phase analysis, and its X-ray diffraction (XRD) spectrogram is as it is shown in figure 1, it can be seen that Al0.5Cr0.9Fe0.8Ni1.5V0.1High-entropy alloy test specimens is made up of face-centered cubic (FCC), body-centered cubic (BCC) structure solid solution phase and ordered phase (BCC)；
To described Al0.5Cr0.9Fe0.8Ni1.5V0.1High-entropy alloy test specimens carries out Analysis on Microstructure, and its optical microscope photograph is as in figure 2 it is shown, scanning electron microscope (SEM) photo is as it is shown in figure 5, it can be seen that Al0.5Cr0.9Fe0.8Ni1.5V0.1High-entropy alloy shows as typical dendrite tissue；Wherein, in Fig. 2, Lycoperdon polymorphum Vitt is the interdendritic of BCC phase composition, and white is the arborescent structure of FCC phase composition；In Fig. 5, a-quadrant is the arborescent structure of FCC phase composition, and B district is the interdendritic of BCC phase composition, and interdendritic exists lamellar and bar-shaped two kinds of spinodal decomposition tissues；
To described Al0.5Cr0.9Fe0.8Ni1.5V0.1High-entropy alloy test specimens carries out quasi-static tensile Mechanics Performance Testing, and its tensile stress-strain curve is as shown in Figure 8, it is known that, Al0.5Cr0.9Fe0.8Ni1.5V0.1The room temperature tensile yield strength of high-entropy alloy is 404MPa, and tensile strength is 1142MPa, and fracture elongation is 22.7%；
To described Al0.5Cr0.9Fe0.8Ni1.5V0.1High-entropy alloy test specimens carries out heat analysis, and its DSC heating curve is as it is shown in figure 9, it can be seen that Al0.5Cr0.9Fe0.8Ni1.5V0.1High-entropy alloy occurs without phase transformation before heating to fusing, shows good heat stability.
Embodiment 2
The preparation method of a kind of high-entropy alloy having intensity and toughness concurrently, described high-entropy alloy is calculated in molar ratio as Al0.5Cr0.9FeNi2.5V0.2；Described method specifically comprises the following steps that
(1) utilizing No. 60 SiC sand paper and abrasive machine to remove simple substance Al, Cr, Fe, Ni and V surface impurity and oxide, then use acetone to clean, weighing gross mass is the Al of 80g, Cr, Fe, Ni and V, and ultrasonic cleaning twice；
(2) Al after ultrasonic cleaning, Cr, Fe, Ni and V are placed in fine vacuum non-consumable arc-melting furnace, under the protection of argon, in vacuum less than or equal to 1.0 × 103Carry out electric arc melting under MPa, obtain aluminium alloy, stirring, cooling, obtain alloy pig；
(3) electric arc melting in step (1), stirring and cooling procedure are repeated after being overturn by alloy pig；
(4) repeat step (3) 2 times, obtain Al described in the present embodiment0.5Cr0.9FeNi2.5V0.2High-entropy alloy.
With abrasive machine by gained Al0.5Cr0.9FeNi2.5V0.2High-entropy alloy surface scale is removed, and then with acetone ultrasonic cleaning twice, cleaner alloy pig is placed in fine vacuum electric arc melting turnover casting and spun casting system, is cast in the mould of diameter 20mm and obtains Al after remelting0.5Cr0.9FeNi2.5V0.2High-entropy alloy test specimens；
To described Al0.5Cr0.9FeNi2.5V0.2High-entropy alloy test specimens carries out material phase analysis, and its X-ray diffraction (XRD) spectrogram is as it is shown in figure 1, it can be seen that Al0.5Cr0.9FeNi2.5V0.2High-entropy alloy is made up of face-centered cubic (FCC) structure solid solution phase；
To described Al0.5Cr0.9FeNi2.5V0.2High-entropy alloy test specimens carries out Analysis on Microstructure, its optical microscope photograph as it is shown on figure 3, scanning electron microscope (SEM) photo as shown in Figure 6, it is known that, Al0.5Cr0.9FeNi2.5V0.2High-entropy alloy shows as typical dendrite tissue, and interdendritic exists the ball shaped nano precipitate being smaller in size than 100nm.
To described Al0.5Cr0.9FeNi2.5V0.2High-entropy alloy test specimens carries out quasi-static tensile Mechanics Performance Testing, and its tensile stress-strain curve is as shown in Figure 8, it is known that, Al0.5Cr0.9FeNi2.5V0.2The room temperature tensile yield strength of high-entropy alloy is 570MPa, and tensile strength is 873MPa, and fracture elongation is 46.7%；
To described Al0.5Cr0.9FeNi2.5V0.2High-entropy alloy test specimens carries out heat analysis, and its DSC heating curve is as it is shown in figure 9, it can be seen that Al0.5Cr0.9FeNi2.5V0.2High-entropy alloy occurs without phase transformation before heating to fusing, shows good heat stability.
Embodiment 3
The preparation method of a kind of high-entropy alloy having intensity and toughness concurrently, described high-entropy alloy is calculated in molar ratio as AlCrFeNi3.0V0.3；Described method specifically comprises the following steps that
(1) utilizing No. 60 SiC sand paper and abrasive machine to remove simple substance Al, Cr, Fe, Ni and V surface impurity and oxide, then use acetone to clean, weighing gross mass is the Al of 80g, Cr, Fe, Ni and V, ultrasonic cleaning twice；
(2) Al after ultrasonic cleaning, Cr, Fe, Ni and V are placed in fine vacuum non-consumable arc-melting furnace, under the protection of argon, in vacuum less than or equal to 1.0 × 103Carry out electric arc melting under MPa, obtain aluminium alloy, stirring, cooling, obtain alloy pig；
(3) electric arc melting in step (1), stirring and cooling procedure are repeated after being overturn by alloy pig；
(4) repeat step (3) 3 times, obtain AlCrFeNi described in the present embodiment3.0V0.3High-entropy alloy.
The AlCrFeNi that will prepare with abrasive machine3.0V0.3High-entropy alloy surface scale is removed, and then with acetone ultrasonic cleaning twice, cleaner alloy pig is placed in fine vacuum electric arc melting turnover casting and spun casting system, is cast in the mould of diameter 20mm and obtains AlCrFeNi after remelting3.0V0.3High-entropy alloy test specimens.
To described AlCrFeNi3.0V0.3High-entropy alloy test specimens carries out material phase analysis, and its X-ray diffraction (XRD) spectrogram is as it is shown in figure 1, it can be seen that AlCrFeNi3.0V0.3High-entropy alloy is made up of face-centered cubic (FCC), body-centered cubic (BCC) structure solid solution phase；
To described AlCrFeNi3.0V0.3High-entropy alloy test specimens carries out Analysis on Microstructure, and as shown in Figure 4, scanning electron microscope (SEM) photo is as it is shown in fig. 7, it can be seen that AlCrFeNi for its optical microscope photograph3.0V0.3High-entropy alloy shows as typical lamellar eutectic structure, and has primary phase to exist；
To the described AlCrFeNi prepared3.0V0.3High-entropy alloy test specimens carries out quasi-static tensile Mechanics Performance Testing, and its tensile stress-strain curve is as shown in Figure 8, it is known that, AlCrFeNi3.0V0.3The room temperature tensile yield strength of high-entropy alloy is 704MPa, and tensile strength is 1176MPa, and fracture elongation is 9.8%；
To described AlCrFeNi3.0V0.3High-entropy alloy test specimens carries out heat analysis, and its DSC heating curve is as it is shown in figure 9, it can be seen that AlCrFeNi3.0V0.3High-entropy alloy occurs without phase transformation before heating to fusing, shows good heat stability.
The present invention includes but not limited to above example, every any equivalent replacement carried out under the principle of spirit of the present invention or local improvement, all will be regarded as within protection scope of the present invention.
Claims (6)
1. the high-entropy alloy having intensity and toughness concurrently, it is characterised in that: described high-entropy alloy is calculated in molar ratio as AlaCrbFecNidVe, wherein, a=0.5～1.0, b=0.9～1.0, c=0.8～1.0；D=1.5～3.0；E=0.1～0.3.
2. a kind of high-entropy alloy having intensity and toughness concurrently according to claim 1, it is characterised in that: described a=0.5～0.75, b=0.9, c=1.0, d=2.0～3.0 and e=0.2.
3. the preparation method of the high-entropy alloy having intensity and toughness as claimed in claim 1 or 2 concurrently, it is characterised in that: described method specifically comprises the following steps that
(1) Al, Cr, Fe, Ni and V are placed in smelting furnace, under the protection of protective gas, in vacuum less than or equal to 1.0 × 103Carry out electric arc melting under MPa, obtain aluminium alloy, magnetic field agitation, cooling, obtain alloy pig；
(2) electric arc melting in step (1), stirring and cooling procedure are repeated after being overturn by alloy pig；
(3) repeat step more than (2) 2 times, described in obtaining, have the high-entropy alloy of intensity and toughness concurrently.
4. the preparation method of a kind of high-entropy alloy having intensity and toughness concurrently according to claim 3, it is characterised in that: described Al, Cr, Fe, Ni and V purity are be more than or equal to 99.7wt%.
5. the preparation method of a kind of high-entropy alloy having intensity and toughness concurrently according to claim 3, it is characterised in that: described protective gas is argon.
6. the preparation method of a kind of high-entropy alloy having intensity and toughness concurrently according to claim 3, it is characterised in that: described smelting furnace is fine vacuum non-consumable arc-melting furnace.
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| CN106086486A (en) * | 2016-08-12 | 2016-11-09 | 北京理工大学 | High-entropy alloy that a kind of obdurability coupling is good and preparation method thereof |
| CN107043884A (en) * | 2017-04-13 | 2017-08-15 | 贵州理工学院 | A kind of TiO particles enhancing CoCrCuFeNi high-entropy alloys and preparation method thereof |
| CN108193088A (en) * | 2017-12-29 | 2018-06-22 | 北京理工大学 | A kind of precipitation strength type AlCrFeNiV system high-entropy alloys and preparation method thereof |
| CN110468323A (en) * | 2019-08-20 | 2019-11-19 | 沈阳工业大学 | A kind of multi-principal elements alloy and preparation method thereof of high-strength plasticity and toughness |
| CN110512101A (en) * | 2019-10-08 | 2019-11-29 | 沈阳工业大学 | A kind of preparation method of the high-entropy alloy of the phase of chrome alum containing hard |
| CN111334698A (en) * | 2020-03-15 | 2020-06-26 | 沈阳工业大学 | Wear-resistant high-entropy alloy containing modulation and demodulation decomposition structure and capable of generating hard phase and preparation method of wear-resistant high-entropy alloy |
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| CN106086486B (en) * | 2016-08-12 | 2018-02-09 | 北京理工大学 | A kind of obdurability matches good high-entropy alloy and preparation method thereof |
| CN106086486A (en) * | 2016-08-12 | 2016-11-09 | 北京理工大学 | High-entropy alloy that a kind of obdurability coupling is good and preparation method thereof |
| CN107043884A (en) * | 2017-04-13 | 2017-08-15 | 贵州理工学院 | A kind of TiO particles enhancing CoCrCuFeNi high-entropy alloys and preparation method thereof |
| US11390938B2 (en) * | 2017-12-29 | 2022-07-19 | Beijing Institute Of Technology | Precipitation strengthening AlCrFeNiV system high entropy alloy and manufacturing method thereof |
| CN108193088A (en) * | 2017-12-29 | 2018-06-22 | 北京理工大学 | A kind of precipitation strength type AlCrFeNiV system high-entropy alloys and preparation method thereof |
| WO2019127610A1 (en) * | 2017-12-29 | 2019-07-04 | 北京理工大学 | Precipitation-enhanced alcrfeniv system high-entropy alloy and preparation method therefor |
| CN110468323A (en) * | 2019-08-20 | 2019-11-19 | 沈阳工业大学 | A kind of multi-principal elements alloy and preparation method thereof of high-strength plasticity and toughness |
| CN110512101A (en) * | 2019-10-08 | 2019-11-29 | 沈阳工业大学 | A kind of preparation method of the high-entropy alloy of the phase of chrome alum containing hard |
| CN111334698B (en) * | 2020-03-15 | 2021-04-20 | 沈阳工业大学 | Wear-resistant high-entropy alloy containing modulation and demodulation decomposition structure and capable of generating hard phase and preparation method of wear-resistant high-entropy alloy |
| CN111334698A (en) * | 2020-03-15 | 2020-06-26 | 沈阳工业大学 | Wear-resistant high-entropy alloy containing modulation and demodulation decomposition structure and capable of generating hard phase and preparation method of wear-resistant high-entropy alloy |
| CN114703415A (en) * | 2022-04-08 | 2022-07-05 | 青海大学 | High-entropy alloy based on interstitial solid solution and replacement solid solution strengthening effect and preparation method thereof |
| CN115821142A (en) * | 2022-10-25 | 2023-03-21 | 锑玛（苏州）精密工具股份有限公司 | FeCrNiVAl high-entropy alloy for nuclear power field machining cutter and preparation method and application thereof |
| CN115821142B (en) * | 2022-10-25 | 2024-06-11 | 锑玛（苏州）精密工具股份有限公司 | FECRNIVAL high-entropy alloy for nuclear power field machining tool, and preparation method and application thereof |
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