CN113930653A - Quaternary high-entropy alloy containing nanoparticle structure and preparation method thereof - Google Patents
Quaternary high-entropy alloy containing nanoparticle structure and preparation method thereof Download PDFInfo
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- CN113930653A CN113930653A CN202111195500.1A CN202111195500A CN113930653A CN 113930653 A CN113930653 A CN 113930653A CN 202111195500 A CN202111195500 A CN 202111195500A CN 113930653 A CN113930653 A CN 113930653A
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- 239000000956 alloy Substances 0.000 title claims abstract description 116
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 114
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000003723 Smelting Methods 0.000 claims abstract description 35
- 238000002844 melting Methods 0.000 claims abstract description 34
- 230000008018 melting Effects 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 34
- 238000001816 cooling Methods 0.000 claims abstract description 25
- -1 aluminum-chromium-iron-nickel Chemical compound 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 44
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 23
- 229910052786 argon Inorganic materials 0.000 claims description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 18
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- 239000011651 chromium Substances 0.000 claims description 9
- 229910052804 chromium Inorganic materials 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- 239000013078 crystal Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 210000001787 dendrite Anatomy 0.000 claims description 6
- 238000005204 segregation Methods 0.000 abstract description 8
- 239000000155 melt Substances 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 description 17
- 239000000498 cooling water Substances 0.000 description 15
- 239000002184 metal Substances 0.000 description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 9
- 229910052802 copper Inorganic materials 0.000 description 9
- 239000010949 copper Substances 0.000 description 9
- 238000001878 scanning electron micrograph Methods 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000005266 casting Methods 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 5
- 238000011049 filling Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 5
- 229910052721 tungsten Inorganic materials 0.000 description 5
- 239000010937 tungsten Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 238000005201 scrubbing Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 229910000828 alnico Inorganic materials 0.000 description 3
- 229910052729 chemical element Inorganic materials 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000010891 electric arc Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910002059 quaternary alloy Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 229910018507 Al—Ni Inorganic materials 0.000 description 1
- 229910019589 Cr—Fe Inorganic materials 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910001325 element alloy Inorganic materials 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000005303 weighing 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
-
- C—CHEMISTRY; METALLURGY
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention provides a quaternary high-entropy alloy containing a nano-particle structure and a preparation method thereof, belonging to the technical field of high-entropy alloy materials. The method comprises the steps of sequentially placing raw materials from bottom to top according to the sequence of the melting points of the raw materials from low to high, then smelting and cooling to obtain the quaternary high-entropy alloy containing the nano-particle structure; the smelting times are 3-6 times; cooling after each smelting in a water cooling mode; the quaternary high-entropy alloy is an aluminum-chromium-iron-nickel quaternary high-entropy alloy. The invention adopts a water cooling mode to accelerate the cooling rate of the melt, reduce the cooling time and control the element segregation, so that the quaternary high-entropy alloy has higher compressive strength and good ductility. The results of the examples show that the aluminum-chromium-iron-nickel quaternary high-entropy alloy provided by the invention has the hardness of 247.76HV, the compressive strength of 1807.01MPa, the yield strength of 1205.08MPa and the elongation of 16.21%.
Description
Technical Field
The invention relates to the technical field of high-entropy alloy materials, in particular to a quaternary high-entropy alloy containing a nanoparticle structure and a preparation method thereof.
Background
High entropy alloys are alloys formed from a variety of equivalent or about equivalent metals and are considered considerable in material science and engineering because of the many desirable properties that high entropy alloys may possess. The traditional five-element high-entropy alloy researched at present usually uses a large amount of high-cost elements such as cobalt, titanium and the like, and the application and development of the high-entropy alloy are severely restricted. Therefore, the preparation of the cobalt-free low-cost quaternary high-entropy alloy with a high-quality structure and good mechanical properties has very important significance. Compared with a four-element alloy, the five-element high-entropy alloy has lower fluidity, the mixing enthalpy among elements in the system is more complex, and the element distribution condition is less influenced by the mixing enthalpy among the elements, so that the structure of the five-element high-entropy alloy cannot be influenced in the preparation process of the traditional melting five-element high-entropy alloy, and the five-element high-entropy alloy has higher strength and good ductility; the mixed enthalpy of two elements in the quaternary alloy system is the lowest, and the quaternary alloy has the attribute of better fluidity, so that the elements in the system are easily gathered in pairs to cause element segregation, the mechanical property of the quaternary high-entropy alloy is greatly influenced, and great challenge is brought to the technological method of the quaternary high-entropy alloy.
Therefore, how to overcome the element segregation in the quaternary high-entropy alloy and make the quaternary high-entropy alloy have higher compressive strength and good ductility becomes a technical problem to be solved in the field.
Disclosure of Invention
The invention aims to provide a quaternary high-entropy alloy containing a nano-particle structure and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a quaternary high-entropy alloy containing a nano-particle structure, which comprises the following steps:
placing the raw materials from bottom to top in sequence according to the sequence of the melting points of the raw materials from low to high, then smelting and cooling to obtain the quaternary high-entropy alloy containing the nano-particle structure; the smelting times are 3-6 times; cooling after each smelting in a water cooling mode; the quaternary high-entropy alloy is an aluminum-chromium-iron-nickel quaternary high-entropy alloy.
Preferably, the atomic ratio of the aluminum, chromium, iron and nickel in the aluminum, chromium, iron and nickel quaternary high-entropy alloy is 1: 1: 1: 1.
preferably, the raw material includes aluminum particles, chromium particles, iron particles, and nickel particles.
Preferably, the atmosphere for smelting is argon.
Preferably, the purity of the argon is more than or equal to 99.5 percent.
Preferably, the initial current of the melting is 30A.
Preferably, the final current of the smelting is ≦ 400A.
Preferably, the air pressure for smelting is 0.8-0.9 air pressure.
The invention provides the quaternary high-entropy alloy containing the nano-particle structure, which is prepared by the preparation method and consists of dendritic crystals and nano-particles among the dendritic crystals; the dendrites have a face centered cubic structure; the nanoparticles have a body centered cubic structure.
Preferably, the shape of the nano particles is spherical, and the particle size of the nano particles is 1-3 μm.
The invention provides a preparation method of a quaternary high-entropy alloy containing a nano-particle structure, which comprises the following steps: placing the raw materials from bottom to top in sequence according to the sequence of the melting points of the raw materials from low to high, then smelting and cooling to obtain the quaternary high-entropy alloy containing the nano-particle structure; the smelting times are 3-6 times; cooling after each smelting in a water cooling mode; the quaternary high-entropy alloy is an aluminum-chromium-iron-nickel quaternary high-entropy alloy. According to the invention, the raw materials are sequentially arranged from bottom to top according to the sequence of the melting points of the raw materials in the quaternary high-entropy alloy from low to high, so that the outermost high-melting-point metal is ensured to be melted first, and then the metal liquid wraps the lower-layer low-melting-point metal, so that metal elements with different melting points can be completely melted; the alloy is cooled in a water cooling mode in the smelting process, so that the cooling rate of a melt can be increased, the cooling time is shortened, the element segregation in the alloy is controlled, and the quaternary high-entropy alloy has higher compressive strength and good ductility. The results of the embodiments show that the quaternary high-entropy alloy provided by the invention is composed of dendritic crystals and interdendritic nanoparticles, the dendritic crystals have a face-centered cubic structure, the nanoparticles have a body-centered cubic structure, the overall morphology of the quaternary high-entropy alloy is a long-range disordered dendritic crystal and interdendritic structure, and the disordered structure proves that the elements are uniformly distributed, so that the preparation method overcomes the element segregation, the quaternary high-entropy alloy has the hardness of 247.76HV, the compressive strength of 1807.01MPa, the yield strength of 1205.08MPa and the elongation of 16.21%, meets the strength and plasticity requirements of the service of metal parts, and is not inferior to the traditional cobalt-containing quinary high-entropy alloy in yield strength alone.
Drawings
FIG. 1 is a schematic view showing the construction of a vacuum arc melting furnace used in the present invention;
in FIG. 1, 1 is a cooling water temperature display screen, 2 is a cooling water switch, 3 is a cooling water tank, 4 is a cooling water pipe, 5 is a suction casting furnace chamber, 6 is a suction casting crucible, 7 is a stirring metal spoon, 8 is a mechanical arm fixing device, 9 is a mechanical arm, 10 is a furnace chamber, 11 is argon gas, 12 is a tungsten electrode gun rod, 13 is an arc striking switch, 14 is a lifting switch, 15 is an outer guide wire, 16 is a lifter top, 17 is a lifter device, 18 is an electromagnetic stirring switch, 19 is a furnace lamp switch, 20 is a potential regulator, 21 is a grip type controller, 22 is an observation mirror, 23 is an arc torch head, 24 is a vacuum arc melting furnace, 25 is a water-cooled copper crucible, 26 is a high-entropy alloy, 27 is a vacuum gauge, 28 is an argon gas switch, 29 is a vacuum pump, 30 is a melting current display screen, 31 is a vacuum degree display screen, 32 is a molecular pump switch, 33 is a mechanical pump switch, 34 is a vacuum furnace master switch, 35 is an argon bottle;
FIG. 2 is an X-ray diffraction pattern of an AlCrFe-Ni quaternary high-entropy alloy prepared in example 1;
FIG. 3 is an SEM image of an AlCrFeNi quaternary high entropy alloy prepared in example 1;
FIG. 4 is an SEM image of the interdendritic region of the AlCrFeNi quaternary high entropy alloy prepared in example 1;
FIG. 5 is an engineering stress-strain curve for the AlCrFe-Ni quaternary high entropy alloy prepared in example 1;
FIG. 6 is an SEM image of an AlCrFeNi quaternary high entropy alloy prepared in example 2;
FIG. 7 is an SEM image of an AlCrFeNi quaternary high-entropy alloy prepared in example 3;
FIG. 8 is an SEM image of an AlCrFe-Ni quaternary high entropy alloy prepared in example 4;
FIG. 9 is an SEM image of an AlCrFeNi quaternary high entropy alloy prepared in example 5.
Detailed Description
The invention provides a preparation method of a quaternary high-entropy alloy containing a nano-particle structure, which comprises the following steps:
placing the raw materials from bottom to top in sequence according to the sequence of the melting points of the raw materials from low to high, then smelting and cooling to obtain the quaternary high-entropy alloy containing the nano-particle structure; the smelting times are 3-6 times; cooling after each smelting in a water cooling mode; the quaternary high-entropy alloy is an aluminum-chromium-iron-nickel quaternary high-entropy alloy.
In the invention, the quaternary high-entropy alloy is an aluminum-chromium-iron-nickel quaternary high-entropy alloy, and the atomic ratio of aluminum, chromium, iron and nickel in the aluminum-chromium-iron-nickel quaternary high-entropy alloy is preferably 1: 1: 1: 1. in the present invention, the raw material preferably includes aluminum particles, chromium particles, iron particles, and nickel particles. In the present invention, the particle size of the raw material is not particularly limited, and may be selected according to the technical common knowledge of those skilled in the art.
The present invention preferably pre-treats the feedstock prior to placement. In the present invention, the pretreatment is preferably performed in the following manner: and putting the raw materials into absolute ethyl alcohol for ultrasonic cleaning, then putting the raw materials into a mixed solution of acetone and absolute ethyl alcohol for ultrasonic cleaning, and finally carrying out vacuum drying to obtain the pretreated raw materials. According to the invention, the raw materials are pretreated by the process, so that impurities in the raw materials can be removed, and the content of the impurities in the high-entropy alloy is reduced.
In the present invention, the melting is preferably performed in a vacuum arc melting furnace. The invention preferably carries out cleaning, raw material placing, vacuumizing and argon filling treatment on the vacuum arc melting furnace in sequence before melting.
In the present invention, the cleaning is preferably performed by scrubbing the melting bath and the water-cooled copper mold auxiliary melting bath in the furnace and the inner wall of the furnace chamber with absolute ethyl alcohol, and then polishing the tip of the tungsten electrode gun rod with a grinder. The invention can clean the interior of the melting chamber through cleaning, and simultaneously ensure the stability of current and successfully complete arc striking.
In the invention, the raw materials are placed from bottom to top in sequence according to the sequence of the melting point of the raw materials from low to high. The raw materials are placed in the mode, so that the outermost high-melting-point metal can be guaranteed to be melted first, and then the lower-layer low-melting-point metal is wrapped by the molten metal, so that metal elements with different melting points can be completely melted, and the probability of element segregation is further reduced.
In the invention, the vacuumizing is preferably to turn on a vacuum pump to evacuate the air in the vacuum arc melting furnace so that the pressure in the furnace reaches 5X 10-3And Pa, closing the vacuum pump, opening an argon valve, and repeating the operation for 3-5 times. The invention can better remove the air in the cavity of the vacuum arc melting furnace by vacuumizing.
In the invention, the argon filling is preferably performed by filling high-purity argon so as to keep the pressure in the furnace at 0.8-0.9. The invention can protect the raw materials and the alloy from being oxidized by filling argon.
In the present invention, the atmosphere for the melting is preferably a protective atmosphere, more preferably high-purity argon; the air pressure for smelting is preferably 0.8-0.9 air pressure. The invention adopts the mode for smelting, and can prevent oxygen element and other impurities from being introduced in the smelting process.
In the present invention, the initial current of the melting is preferably 30A, and the final current is preferably ≦ 400A. In the present invention, the manner of increasing the initial current to the final current is preferably a gradient increase, and the current is preferably 50A for each increase in the gradient increase. The smelting temperature can be more stable through the mode.
In the invention, the number of times of melting is 3 to 6, preferably 5. Through multiple times of smelting, the invention can further ensure that all components in the alloy are uniformly mixed and reduce element segregation.
After the smelting is finished, the invention preferably opens the air release valve, and opens the furnace door after the internal and external air pressures are balanced, so as to obtain the high-entropy alloy cast ingot. The process can avoid potential safety hazards caused by different pressures inside and outside the furnace.
After the high-entropy alloy-containing cast ingot is obtained, the front surface, the back surface and the periphery of the high-entropy alloy cast ingot are preferably polished by 200-mesh abrasive paper to clean the surface of the cast ingot, then the cast ingot is scrubbed by absolute ethyl alcohol, and finally the cast ingot is dried in a vacuum drying oven at 80-120 ℃ for 5-20 min to obtain the quaternary high-entropy alloy containing the nano-particle structure. According to the invention, the impurities on the surface of the high-entropy alloy can be removed by polishing and scrubbing the high-entropy alloy cast ingot.
The preparation method is simple, and the existing device can be used for production.
The invention provides the quaternary high-entropy alloy containing the nano-particle structure, which is prepared by the preparation method in the technical scheme, and the quaternary high-entropy alloy containing the nano-particle structure is composed of dendritic crystal structures composed of face-centered cubic structures and interdendritic nano-particles composed of body-centered cubic structures. In the invention, the shape of the interdendritic nanoparticles is preferably spherical, and the size of the interdendritic nanoparticles is preferably 1-3 μm. The quaternary high-entropy alloy containing the nano-particle structure provided by the invention has higher compressive strength and good ductility.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a quaternary high-entropy alloy containing a nanoparticle structure comprises the following steps:
(1) according to the atomic ratio of aluminum, chromium, iron and nickel of 1: 1: 1: 1, weighing 6.966 +/-0.001 g of aluminum particles, 13.424 +/-0.001 g of chromium particles, 14.458 +/-0.001 g of iron particles and 15.152 +/-0.001 g of nickel particles, respectively placing the aluminum particles, the chromium particles, the iron particles and the nickel particles in a beaker, adding 300mL of absolute ethyl alcohol, ultrasonically cleaning for 35min by adopting a magnetic vibration device, then ultrasonically cleaning for 20min by using a mixed solution of acetone and absolute ethyl alcohol in sequence, placing the cleaned raw material in a vacuum drying oven for drying at the drying temperature of 200 ℃ for 30min to obtain the raw material;
(2) scrubbing a smelting pool and a water-cooling copper mold auxiliary smelting pool in the vacuum arc smelting furnace and the inner wall of a furnace chamber by using absolute ethyl alcohol, then polishing the tip of a tungsten electrode gun rod by using a grinder, sequentially placing the raw materials obtained in the step (1) from bottom to top according to the sequence of the melting points of the raw materials from low to high, starting a vacuum pump, evacuating air in the vacuum arc smelting furnace to enable the pressure in the furnace to reach 5 multiplied by 10-3Pa, closing the vacuum pump, opening an argon valve, repeating the operation for 3 times to remove the air in the cavity, and then filling high-purity argon to keep the pressure in the furnace at 0.8;
(3) the arc torch head is aligned to a titanium ingot in an auxiliary molten pool to complete arc striking, the current is controlled to be 30A, and after the current is stabilized, the current is gradually increased in an increasing gradient of 50A and is stabilized to be slightly lower than 400A; rapidly aligning an electric arc gun head to an alloy element in a main molten pool to rotatably smelt an upper layer raw material into a liquid state and wrap a lower layer raw material, smelting all metal raw materials into the liquid state through a handle type controller, standing for 30s to keep the metal raw materials in an overheat flowing state after deep metal liquid vortex occurs, and immediately closing electric arc current; opening a cooling water switch of a main molten pool, standing for 30s after the cast ingot is cooled to be blocky, turning over the cast ingot by using a mechanical arm after the surface of the cast ingot shows metallic luster, repeatedly smelting for 5 times, opening a vent valve, opening a furnace door after the internal and external air pressures are balanced to obtain a high-entropy alloy cast ingot, wherein the size of the high-entropy alloy cast ingot is phi 30mm multiplied by 15 mm;
(4) polishing the front surface, the back surface and the periphery of the high-entropy alloy cast ingot obtained in the step (3) by using 200-mesh abrasive paper to clean the surface of the cast ingot, then scrubbing by using absolute ethyl alcohol, and finally drying the cast ingot in a vacuum drying oven at 100 ℃ for 10min to obtain a quaternary high-entropy alloy containing a nano-particle structure;
the structure of the vacuum arc melting furnace is shown in figure 1, 1 is a cooling water temperature display screen, 2 is a cooling water switch, 3 is a cooling water tank, 4 is a cooling water pipe, 5 is a suction casting furnace chamber, 6 is a suction casting crucible, 7 is a stirring metal spoon, 8 is a mechanical arm fixing device, 9 is a mechanical arm, 10 is a furnace chamber, 11 is argon gas, 12 is a tungsten electrode gun rod, 13 is an arc striking switch, 14 is a lifting switch, 15 is an outer guide wire, 16 is a lifter top, 17 is a lifter device, 18 is an electromagnetic stirring switch, 19 is a furnace lamp switch, 20 is a potential regulator, 21 is a handle controller, 22 is an observation mirror, 23 is an arc gun head, 24 is a vacuum arc melting furnace, 25 is a water-cooling copper crucible, 26 is a high-entropy alloy, 27 is a vacuum gauge, 28 is an argon switch, 29 is a vacuum pump, 30 is a melting current display screen, 31 is a vacuum degree display screen, and 32 is a molecular pump switch, 33 is a mechanical pump switch, 34 is a main switch of the vacuum furnace, and 35 is an argon bottle;
the vacuum arc melting furnace 24 comprises a furnace chamber 10, an elevator device 17 and a mechanical arm 9;
the left side of the furnace chamber 10 is provided with a vacuum pump 29 and an argon bottle 35, and the right side is connected with a cooling water tank 3;
the handle controller 21 is mounted on the elevator device 17;
the tungsten electrode gun rod 12 and the electric arc gun head 23 are connected with a handle type controller 21;
the handle type controller 21 is provided with an electromagnetic stirring switch 18, an arc striking switch 13, a furnace lamp switch 19, a lifting switch 14, a potential regulator 20 and a cooling water switch 2;
a lifter top 16 on the lifter device 17 is connected with an outer guide wire 15 and is connected with a power supply of a vacuum arc melting furnace 24;
a mechanical arm 9 in the furnace chamber 10 is fixed by a mechanical arm fixing device 8 and is connected with a material turning metal spoon 7, and the material turning metal spoon 7 mainly turns over a high-entropy alloy 26 in a water-cooled copper crucible 25;
the lower part of the vacuum arc melting furnace 24 is provided with a water-cooled copper crucible 25, the lower part of the water-cooled copper crucible 25 is provided with a cooling water pipe 4 for cooling the high-entropy alloy 26, and the cooling water pipe 4 is connected with a cooling water tank 3 and a cooling water temperature display screen 1;
the right part of the water-cooled copper crucible 25 is a suction casting crucible 6, and the lower part of the suction casting crucible 6 is connected with a suction casting furnace chamber 5;
the vacuum pump 29 is provided with a smelting current display screen 30, a vacuum degree display screen 31, a molecular pump switch 32, a mechanical pump switch 34, a mechanical pump switch 33 and a vacuum meter 27.
Example 2
High purity argon gas was introduced in the step (2) to maintain the pressure in the furnace at 0.9 atmosphere, and the other conditions were the same as in example 1.
Example 3
High purity argon gas was introduced in the step (2) to maintain the pressure in the furnace at 0.9 atmosphere, and the other conditions were the same as in example 1.
Example 4
High purity argon gas was introduced in the step (2) to maintain the pressure in the furnace at 0.9 atmosphere, and the other conditions were the same as in example 1.
Example 5
The same as in example 1.
Comparative example 1
Patent CN 110144476A-A preparation method of aluminum-cobalt-chromium-iron-nickel high-entropy alloy, wherein a quaternary aluminum-cobalt-iron-nickel high-entropy alloy cooled along with a furnace is used, the Vickers hardness of the quaternary aluminum-cobalt-iron-nickel high-entropy alloy is 232HV, and the yield strength is 432 MPa.
Comparative example 2
The patent CN 110172630A-a quaternary hypoeutectic high-entropy alloy with good strong plasticity matching and a preparation method thereof, wherein the yield strength of the quaternary Al14Co28Cr28Ni30 high-entropy alloy is 480MPa, and the ultimate strength is about 1000 MPa.
Comparative example 3
In a patent CN 201910837304.6-Al-Co-Cr-Ni quaternary high-entropy alloy system and an Al18Co24Cr20Ni38 quaternary high-entropy alloy in the preparation method thereof, the ultimate strength of the high-entropy alloy is 1005MPa, and the ductility is 8.2%.
The crystal structure of the aluminum-chromium-iron-nickel quaternary high-entropy alloy prepared in example 1 was analyzed by an X-ray diffractometer, and the X-ray diffraction pattern obtained is shown in fig. 2. As can be seen from fig. 2, the alnico quaternary high-entropy alloy consists of face-centered cubic and body-centered cubic solid solutions, no complex mesophase or intermetallic compound is formed, and the diffraction peak intensity of the face-centered cubic structure is higher, which indicates that the alnico quaternary high-entropy alloy contains a large amount of face-centered cubic structures and a small amount of body-centered cubic structures.
The scanning electron microscope is used for analyzing the microstructure and chemical elements of the aluminum-chromium-iron-nickel quaternary high-entropy alloy prepared in example 1, and an SEM image is shown in FIG. 3. As can be seen from fig. 3, due to the rapid cooling effect of the copper mold, the alloy exhibits a dendrite structure, the dendrite structure is a face centered cubic structure, the face centered cubic structure is composed of a Cr-Fe phase, the interdendritic structure is a body centered cubic structure composed of spherical nanoparticles, the body centered cubic structure is composed of an Al-Ni phase, if element segregation occurs, the aggregation of the same elements will cause the arrangement of the structural morphology in a long range ordered distribution, while in the structure of fig. 3, the overall morphology of the quaternary high-entropy alloy can be clearly seen as a long range disordered dendrite and interdendritic structure, which indicates that the distribution of the elements is uniform.
Microscopic morphology and chemical element analysis were performed on the interdendritic regions of the alnico quaternary high-entropy alloy prepared in example 1 with a scanning electron microscope, and the obtained SEM image is shown in fig. 4. As can be seen from FIG. 4, the nanoparticles between the dendrites are spherical and have a size of about 1-3 μm.
The mechanical properties of the quaternary Al-Cr-Fe-Ni high-entropy alloy prepared in example 1 were analyzed by a microcomputer controlled electronic universal tester, and the obtained engineering stress-strain curve is shown in FIG. 5. By analyzing the graph shown in FIG. 5, the ultimate compression strength of the aluminum-chromium-iron-nickel quaternary high-entropy alloy is 1807.01MPa, the yield strength reaches 1205.08MPa, the elongation reaches 16.21%, the hardness of the aluminum-chromium-iron-nickel quaternary high-entropy alloy is measured to reach 247.76HV by performing a hardness test on the aluminum-chromium-iron-nickel quaternary high-entropy alloy by using a Vickers hardness tester, and the aluminum-chromium-iron-nickel quaternary high-entropy alloy is proved to have high compression strength, good ductility and excellent mechanical properties.
As can be seen from the comparison of the mechanical properties of the aluminum-chromium-iron-nickel quaternary high-entropy alloy prepared in the embodiment 1 and the quaternary high-entropy alloys prepared in the comparative examples 1-3, the preparation method provided by the invention can improve the hardness, yield strength, ultimate strength and ductility of the quaternary high-entropy alloy, so that the quaternary high-entropy alloy has higher strength and good ductility.
The scanning electron microscope is used for analyzing the microstructure and chemical elements of the aluminum-chromium-iron-nickel quaternary high-entropy alloy prepared in the embodiments 2 to 5, and the obtained SEM images are shown in FIGS. 6 to 9. As can be seen from the graphs in FIGS. 2 to 5, the aluminum-chromium-iron-nickel quaternary high-entropy alloy prepared by the preparation method disclosed by the invention has a nanoparticle structure, so that the high-entropy alloy prepared by the preparation method disclosed by the invention has excellent mechanical properties.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a quaternary high-entropy alloy containing a nanoparticle structure comprises the following steps:
placing the raw materials from bottom to top in sequence according to the sequence of the melting points of the raw materials from low to high, then smelting and cooling to obtain the quaternary high-entropy alloy containing the nano-particle structure; the smelting times are 3-6 times; cooling after each smelting in a water cooling mode; the quaternary high-entropy alloy is an aluminum-chromium-iron-nickel quaternary high-entropy alloy.
2. The preparation method according to claim 1, wherein the atomic ratio of AlCrFe-Ni in the AlCrFe-Ni quaternary high-entropy alloy is 1: 1: 1: 1.
3. the method of claim 2, wherein the raw material includes aluminum particles, chromium particles, iron particles, and nickel particles.
4. The method of claim 1, wherein the smelting atmosphere is argon.
5. The method of claim 4, wherein the purity of the argon gas is greater than or equal to 99.5%.
6. The method of claim 1, wherein the initial current for the melting is 30A.
7. The method of claim 6, wherein the final current of the smelting is ≤ 400A.
8. The method according to claim 1, wherein the pressure of the smelting is 0.8 to 0.9.
9. The quaternary high-entropy alloy containing the nano-particle structure prepared by the preparation method of any one of claims 1 to 8, wherein the quaternary high-entropy alloy containing the nano-particle structure is composed of dendritic crystals and inter-dendritic nanoparticles; the dendrites have a face centered cubic structure; the nanoparticles have a body centered cubic structure.
10. The quaternary high-entropy alloy containing the nanoparticle structure according to claim 9, wherein the nanoparticles are spherical in shape and have a particle size of 1-3 μm.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105648297A (en) * | 2016-01-18 | 2016-06-08 | 南京工程学院 | Preparation method for high-entropy alloy composite material with externally-added nanometer ceramic phase reinforced and toughened |
| CN109576519A (en) * | 2018-12-27 | 2019-04-05 | 中北大学 | A kind of preparation method of iron copper manganese nickel high-entropy alloy |
| CN110172628A (en) * | 2019-04-18 | 2019-08-27 | 中北大学 | A kind of preparation method of the good aluminium ferro-cobalt nickel chromium triangle high-entropy alloy of corrosion resistance |
| 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 |
| CN113186443A (en) * | 2021-04-08 | 2021-07-30 | 南京理工大学 | Aluminum-cobalt-chromium-iron-nickel high-entropy alloy containing nano strengthening phase gamma' phase and preparation method thereof |
-
2021
- 2021-10-14 CN CN202111195500.1A patent/CN113930653A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105648297A (en) * | 2016-01-18 | 2016-06-08 | 南京工程学院 | Preparation method for high-entropy alloy composite material with externally-added nanometer ceramic phase reinforced and toughened |
| CN109576519A (en) * | 2018-12-27 | 2019-04-05 | 中北大学 | A kind of preparation method of iron copper manganese nickel high-entropy alloy |
| CN110172628A (en) * | 2019-04-18 | 2019-08-27 | 中北大学 | A kind of preparation method of the good aluminium ferro-cobalt nickel chromium triangle high-entropy alloy of corrosion resistance |
| 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 |
| CN113186443A (en) * | 2021-04-08 | 2021-07-30 | 南京理工大学 | Aluminum-cobalt-chromium-iron-nickel high-entropy alloy containing nano strengthening phase gamma' phase and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 李云凯: "《金属材料学》", 31 January 2019, 北京理工大学出版社 * |
| 陈霄: "AlxCrFeNi四组元合金的微观组织与性能研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
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