CN114836668B - CoCrFeMnNiAl high-entropy alloy and preparation method thereof - Google Patents

CoCrFeMnNiAl high-entropy alloy and preparation method thereof Download PDF

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CN114836668B
CN114836668B CN202210479103.5A CN202210479103A CN114836668B CN 114836668 B CN114836668 B CN 114836668B CN 202210479103 A CN202210479103 A CN 202210479103A CN 114836668 B CN114836668 B CN 114836668B
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entropy alloy
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CN114836668A (en
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喇培清
杜明宸
金静
余海存
盛捷
柏泽民
高云滕
杜琳琳
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Lanzhou University of Technology
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/23—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces involving a self-propagating high-temperature synthesis or reaction sintering step
    • 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
    • C22C1/03—Making non-ferrous alloys by melting using master alloys
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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
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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Abstract

The CoCrFeMnNiAl high-entropy alloy comprises the following components in percentage by atom: co 27~29,Cr 17~18,Fe 15~19,Mn 4~1,Ni 23~29,Al 7~10. The method comprises the following steps: step (1) weighing the reaction materials according to a preset proportion, and placing the reaction materials into a planetary ball mill for ball milling; step (2), pressing the ball-milled reaction materials into cake-shaped blanks on a press; step (3) putting the cake-shaped blank into a reaction kettle, putting an ignition agent on the blank, filling protective gas for gas washing, then filling the protective gas for pressure maintaining, and continuously heating until the system is subjected to self-propagating reaction to obtain a base metal alloy; step (4) carrying out vacuum induction secondary smelting on the base metal alloy to obtain an ingot; and (5) carrying out solution treatment at 1150 ℃ for 30min after carrying out hot rolling of the cast ingot at 1200 ℃ for 50% of deformation, and carrying out water cooling.

Description

CoCrFeMnNiAl high-entropy alloy and preparation method thereof
Technical Field
The invention relates to a preparation technology of CoCrFeMnNiAl high-entropy alloy.
Background
The fused salt photo-thermal power generation (Concentrated solar power, CSP) technology not only can effectively provide power, but also can greatly reduce CO in the global scope 2 Emissions, one of the most competitive alternatives to fossil fuels, is receiving increasing attention. Molten chloride salts have been proposed as candidate dielectric materials for heat transfer fluids (Heat transfer fluids, HTF) and thermal energy storage (Thermal energy storage, TES) in next generation CSP power plants with the advantages of low cost, low melting point, high boiling point, good heat transfer properties, etc. However, the chloride molten salt has extremely strong corrosiveness to pipes of heat storage and heat transfer systems, and the existing structural materials (namely iron-based and nickel-based alloys) have poor corrosion resistance to the chloride molten salt at high temperature. Therefore, the development of a novel alloy serving in a high-temperature chloride molten salt corrosion environment is significant.
Compared with the traditional alloy, the high-entropy alloy has more excellent performances of high strength, high plasticity, high corrosion resistance, high wear resistance and the like. Related researches indicate that the Al element can well improve the corrosion resistance of the alloy to the high-temperature molten salt, mainly because the formed aluminum oxide film has good compactness, the aluminum oxide film is not easy to fall off in the high-temperature chloride molten salt, and the corrosion resistance can be reduced due to preferential dissolution of the Cr element in the chloride molten salt.
At present, the high-entropy alloy is prepared by adopting a vacuum arc furnace smelting method, and the vacuum arc furnace smelting method has the defects of complex preparation process and larger energy consumption, and the high-entropy alloy can be uniformly prepared by repeatedly smelting for several times, so that the obtained bulk material is smaller.
Disclosure of Invention
The invention aims to provide a preparation method of a CoCrFeMnNiAl high-entropy alloy.
The invention relates to a CoCrFeMnNiAl high-entropy alloy and a preparation method thereof, wherein the CoCrFeMnNiAl high-entropy alloy comprises the following components in percentage by atom: co 27~29,Cr 17~18,Fe 15~19,Mn 4~1,Ni 23~29,Al 7~10.
The preparation method of the CoCrFeMnNiAl high-entropy alloy comprises the following steps:
step (1) weighing the reaction materials according to a preset proportion, and placing the reaction materials into a planetary ball mill for ball milling;
step (2) pressing the ball-milled reaction materials into cake-shaped blanks with the diameter of 80mm and the height of about 50mm on a pressing machine;
step (3) putting the cake-shaped blank into a reaction kettle, putting an ignition agent on the blank, filling protective gas for gas washing, then filling the protective gas for pressure maintaining, and continuously heating until the system is subjected to self-propagating reaction to obtain a base metal alloy;
step (4) carrying out vacuum induction secondary smelting on the base metal alloy to obtain an ingot;
and (5) carrying out solution treatment at 1150 ℃ for 30min after carrying out hot rolling of the cast ingot at 1200 ℃ for 50% of deformation, and carrying out water cooling.
The invention has the beneficial effects that: the invention has simple process flow, simplifies production equipment and is simple to operate; compared with the existing technology for preparing high-entropy alloy by using a vacuum arc furnace smelting method, the technology is simple, has low energy consumption and has commercial production scale; according to the invention, on the basis of the high-entropy alloy with the equal molar ratio of CoCrFeMnNi, the heat insulation temperature is reduced by adding the diluent, and the Al content is regulated and controlled.
Drawings
FIG. 1 is the XRD patterns of examples 1, 2, and 3; FIG. 2 is the XRD patterns of examples 4, 5, and 6; fig. 3, 4, 5, 6, 7 and 8 are metallographic structure diagrams of examples 1, 2, 3, 4, 5 and 6, respectively; fig. 9, 10, 11, 12, 13, and 14 are SEM tissue morphology diagrams of examples 1, 2, 3, 4, 5, and 6, respectively.
Detailed Description
The invention relates to a CoCrFeMnNiAl high-entropy alloy and a preparation method thereof, wherein the CoCrFeMnNiAl high-entropy alloy comprises the following components in percentage by atom: co 27~29,Cr 17~18,Fe 15~19,Mn 4~1,Ni 23~29,Al 7~10.
The preparation method of the CoCrFeMnNiAl high-entropy alloy comprises the following steps:
step (1) weighing the reaction materials according to a preset proportion, and placing the reaction materials into a planetary ball mill for ball milling;
step (2) pressing the ball-milled reaction materials into cake-shaped blanks with the diameter of 80mm and the height of about 50mm on a pressing machine;
step (3) putting the cake-shaped blank into a reaction kettle, putting an ignition agent on the blank, filling protective gas for gas washing, then filling the protective gas for pressure maintaining, and continuously heating until the system is subjected to self-propagating reaction to obtain a base metal alloy;
step (4) carrying out vacuum induction secondary smelting on the base metal alloy to obtain an ingot;
and (5) carrying out solution treatment at 1150 ℃ for 30min after carrying out hot rolling of the cast ingot at 1200 ℃ for 50% of deformation, and carrying out water cooling.
The preparation method comprises the following steps of (1) ball milling parameters: the duration is 8h, alumina ball milling beads are selected, the ball-material ratio is 2:1, and the rotating speed is 80r/min; the pressure of the press is 70 MPa.
In the preparation method, in the step (2), the reactant raw material adopted in the reactant is Co 2 O 3 、Cr 2 O 3 、Fe 2 O 3 、MnO 2 NiO (or Ni) and Al powder.
According to the preparation method, in the step (3), the preheating temperature is 280-340 ℃, the protective atmosphere is argon, and the air pressure is 4-6 Mpa.
In the preparation method, in the step (4), the preheating time is 60min, and the vacuum degree is 10 -2 Pa, maintaining for 10min for alloying.
In the preparation method, in the step (5), the hot rolling is heated to 1200 ℃ at a speed of 10 ℃/min and is kept for 30min, the reduction of each pass is 0.3mm, and the temperature is kept for 5min after the furnace is returned for each pass. The solution treatment is heated to 1150 ℃ at a heating speed of 10 ℃/min, and the solution is preserved for 30min and quenched.
According to the design of the CoCrFeMnNi high-entropy alloy with the equal molar ratio, the heat insulation temperature is changed by adding the diluent to change the Al content, the base metal alloy is prepared by the aluminothermic method, and then the secondary smelting is carried out by vacuum medium frequency induction smelting, so that the internal defects prepared by the aluminothermic method are eliminated, and the bulk alloy material with qualified quality is obtained. The high-temperature corrosion resistance and the high-temperature creep resistance are improved, and the cost is reduced. The preparation process is simple, environment-friendly, low in cost and suitable for mass production.
The following are specific embodiments of the present invention, and the technical solutions of the present invention will be further described with reference to the embodiments, but the present invention is not limited to these embodiments:
example 1:
the preparation method of the initial casting blank by the aluminothermic method comprises the following steps:
table 1 example 1 cocrfenmnnial high entropy alloy reactant material ratio (wt.%)
(1) And (3) batching: 1kg of reaction raw materials are weighed according to the mixture ratio of the reaction materials shown in the table 1, and each raw material is evenly mixed into four parts;
(2) Ball milling: putting the uniformly mixed reaction materials into a QM-ISP4 planetary ball mill for ball milling at the rotating speed of 80r/min and the ball milling time of 8h, wherein the ball mill steering is changed every 2 h to prevent caking, and the ball mill is made of Al 2 O 3 Ball-to-material ratio 1:2;
(3) And (3) preparing by an aluminothermic method: after ball milling, the reaction materials are put into a mould, a hydraulic press is used for applying pressure of 70MPa, and after pressure maintaining is carried out for 4 min, the materials are pressed into a round cake-shaped green body with the diameter of about 80mm and the thickness of about 50 mm. Placing the pressed embryo in a copper crucible, placing a 2 g ignition agent sheet above the embryo, placing the copper crucible in a closed reaction kettle for gas washing, introducing 5 MPa argon as protective gas, heating by electrifying, igniting the ignition agent when the temperature in the kettle is increased to 280 ℃ or more, initiating thermit reaction, rapidly increasing the pressure and the temperature in the kettle at the moment, and closing a heating switch after the reaction starts. Cooling the product to room temperature along with the furnace under the protection of argon atmosphere, opening the reaction kettle, taking out the product, and coating Al on the alloy 2 O 3 And wrapping the layers, and breaking the wrapping layers to obtain the block alloy.
The preparation method of the vacuum medium-frequency induction smelting secondary smelting comprises the following steps:
(1) Preparing a base material: the CoCrFeMnNiAl high-entropy alloy prepared by the aluminothermic method is processed into a strip with the width of 10 mm by wire cutting, and stains on the surface are polished off, so that the introduction of impurities is prevented;
(2) Vacuum medium-frequency induction smelting: preheating a diffusion pump of an intermediate frequency induction furnace for 40-50 min in the smelting process, then placing a block alloy into a magnesia-alumina spinel crucible with the volume of 3 kg, placing a metal trapezoid mould with a release agent preheated to 300 ℃ in advance into a smelting furnace, and opening a vacuum system to ensure the vacuum degree to be 10 -2 And after Pa, starting a smelting system, sequentially adjusting the heating power from 0 kw at a gradient of 5 kw, keeping for 5min after each adjustment to ensure uniform heating, reducing the heating power to 5 kw after observing that the bulk alloy is completely melted into liquid through an observation port, keeping the temperature for 10min to ensure uniform components, turning over a crucible, pouring molten metal into a mold, and taking out after cooling.
And (5) testing the room temperature mechanical properties. Hardness test the hardness test system was fully automatic with a WILSON-VH1102, load 300 g, load time 12 s, and 10 points per sample were averaged and expressed as Vickers hardness HV 0.3. The tensile test was performed on an Shimadzu AGS-X300 kN electronic universal tester at a tensile rate of 0.5 mm/min with displacement loading, and 3 parallel experiments were performed on each component sample. The results showed 169.8 HV0.3 hardness, 470.98 MPa tensile strength and 44.07% elongation.
Example 2:
the reaction materials of this example are shown in Table 2, and the preparation steps are the same as those of example 1, and the results of the room temperature mechanical property test are: hardness 210.2 HV0.3, tensile strength 522.39 MPa, elongation 40.03%.
Table 2 example 2 cocrfenmnnial high entropy alloy reactant material ratio (wt.%)
Example 3:
the reaction materials of this example are shown in Table 3, and the preparation steps are the same as those of example 1, and the results of the room temperature mechanical property test are: hardness 188.4 HV0.3, tensile strength 525.05 MPa and elongation 48.86%.
Table 3 example 3 cocrfenmnnial high entropy alloy reactant material ratio (wt.%)
Example 4:
the cocrfenmnnial high-entropy alloy ingot obtained in example 1 was hot rolled, the hot rolling steps being:
cutting a plate with the thickness of 5 mm from the high-entropy alloy cast ingot of example 1 by wire cutting, heating the plate to 1200 ℃ from room temperature by a box furnace at the heating rate of 10 ℃/min and preserving heat for 30min, carrying out hot rolling by a two-roll cold-hot rolling mill, wherein the reduction of the rolling temperature is 0.3mm per pass, placing the plate into the box furnace for preserving heat for 2 min for each pass, the rolling deformation is 50%, obtaining a hot-rolled plate with the thickness of 2.5 mm, placing the hot-rolled plate cooled at room temperature into the box furnace, heating the plate to 1150 ℃ at the same heating rate and preserving heat for 30min, carrying out solid solution treatment, taking out and then cooling by water.
The same room temperature mechanical property test and 800℃high temperature tensile property test as in example 1 were performed. 800. High-temperature stretching at the temperature of between 0.2 and mm per minute is carried out on an AGS-X300 kN electronic universal tester, and 3 groups of parallel experiments are carried out on each component by adopting a displacement loading mode. The test data are shown in Table 4:
TABLE 4 example 4CoCrFeMnNiAl high entropy alloy Hot rolled mechanical Properties
Example 5:
the CoCrFeMnNiAl high entropy alloy obtained in example 2 was subjected to hot rolling treatment, and the preparation procedure was the same as that of example 4, and the mechanical property data are shown in Table 5.
TABLE 5 example 5 CoCrFeMnNiAl high entropy alloy Hot rolled mechanical Properties
Example 6:
the CoCrFeMnNiAl high entropy alloy obtained in example 3 was subjected to hot rolling treatment, and the preparation procedure was the same as that of example 4, and the mechanical property data are shown in Table 6.
TABLE 6 example 6 CoCrFeMnNiAl high entropy alloy Hot rolled mechanical Properties
The data show that the invention realizes the preparation of the CoCrFeMnNiAl high entropy alloy with different Al contents.
The above description is merely an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions easily come within the technical scope of the present invention as those skilled in the art will readily come to be included in the scope of the present invention. The protection scope of the present invention is subject to the protection scope of the claims.

Claims (1)

1. The preparation method of the CoCrFeMnNiAl high-entropy alloy comprises the following components in percentage by atom: 27-29 parts of Co, 17-18 parts of Cr, 15-19 parts of Fe, 4-1 parts of Mn, 23-29 parts of Ni and 7-10 parts of Al;
the method is characterized by comprising the following steps of:
step (1) weighing the reaction materials according to a preset proportion, and placing the reaction materials into a planetary ball mill for ball milling;
step (2), pressing the ball-milled reaction materials into cake-shaped blanks with the diameter of 80mm and the height of 50mm on a press;
step (3) putting the cake-shaped blank into a reaction kettle, putting an ignition agent on the blank, filling protective gas for gas washing, then filling the protective gas for pressure maintaining, and continuously heating until the system is subjected to self-propagating reaction to obtain a base metal alloy;
step (4) carrying out vacuum induction secondary smelting on the base metal alloy to obtain an ingot;
step (5), hot rolling the cast ingot at 1200 ℃ for 50% of deformation, performing solution treatment at 1150 ℃ for 30min, and water-cooling;
the ball milling parameters in the step (1): the duration is 8 hours, alumina ball milling beads are selected, the ball-material ratio is 2:1, and the rotating speed is 80r/min; pressurizing the press to 70MPa;
in the reaction material in the step (2), the adopted reactant raw material is Co 2 O 3 、Cr 2 O 3 、Fe 2 O 3 、MnO 2 NiO and Al powders;
the preheating temperature of the step (3) is 280-340 ℃, the protective atmosphere is argon, and the air pressure is 4-6 MPa; preheating time of step (4) is 60min, and vacuum degree is 10 -2 Pa, maintaining for 10min for alloying;
the hot rolling is heated to 1200 ℃ at a speed of 10 ℃/min and is kept at the temperature for 30min, the reduction of each pass is 0.3mm, and the temperature is kept for 5min after furnace return; the solution treatment is heated to 1150 ℃ at a heating speed of 10 ℃/min, and the solution is preserved for 30min and quenched.
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AlCrFeNiTi高熵合金热稳定性的研究;农智升;李宏宇;王继杰;;稀有金属材料与工程(01);全文 *
Surface segregation in Cr-Mn-Fe-Co-Ni high entropy alloys;Alberto Ferrari等;Applied Surface Science;第1-7页 *
热处理对Al_(0.5)CoCrCuFeNi高熵合金显微组织与硬度的影响;杨上金;吴波;刘灯宪;赵春凤;钭舒适;吴育锋;陈祖华;;金属热处理(11);全文 *

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