CN114836668A - CoCrFeMnNiAl high-entropy alloy and preparation method thereof - Google Patents
CoCrFeMnNiAl high-entropy alloy and preparation method thereof Download PDFInfo
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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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- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- 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
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- 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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- 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
A CoCrFeMnNiAl high-entropy alloy and a preparation method thereof comprise the following components in atomic percentage: 27-29 Co, 17-18 Cr, 15-19 Fe, 4-1 Mn, 23-29 Ni, 7-10 Al. The method comprises the following steps: weighing reaction materials according to a preset proportion, and placing the reaction materials in a planetary ball mill for ball milling; pressing the ball-milled reaction materials into a cake-shaped blank on a press machine; 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 a system generates a self-propagating reaction to obtain a base metal alloy; performing vacuum induction secondary smelting on the base metal alloy to obtain an ingot; and (5) carrying out hot rolling on the cast ingot at 1200 ℃ for 50% of deformation, carrying out solution treatment at 1150 ℃ for 30min, and carrying out water cooling.
Description
Technical Field
The invention relates to a preparation technology of a CoCrFeMnNiAl high-entropy alloy.
Background
The fused salt solar thermal 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. Chloride fused salt has been proposed as a candidate dielectric material for Heat Transfer Fluids (HTF) and Thermal Energy Storage (TES) in next generation CSP power stations, with advantages of low cost, low melting point, high boiling point, good Heat transfer performance, etc. However, the chloride molten salt has extremely strong corrosivity to heat storage and transfer system pipes, and the existing structural materials (namely iron-based and nickel-based alloys) have poor chloride molten salt corrosion resistance at high temperature. Therefore, the development of novel alloys serving in a high-temperature chloride molten salt corrosion environment is of great significance.
Compared with the traditional alloy, the high-entropy alloy has more excellent performances such as high strength, high plasticity, high corrosion resistance, high wear resistance and the like. Related researches indicate that the Al element can well improve the high-temperature molten salt corrosion resistance of the alloy, mainly because an alumina film formed by the Al element has good compactness and is not easy to fall off in high-temperature chloride molten salt, and the corrosion resistance can be reduced by preferential dissolution of the Cr element in the chloride molten salt.
At present, a vacuum arc furnace smelting method is adopted for preparing the block high-entropy alloy, has the defects of complex preparation process and large energy consumption, and can ensure that the components of the high-entropy alloy are uniform and the obtained block material is small only by repeatedly smelting for several times.
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 atomic percentage: 27-29 Co, 17-18 Cr, 15-19 Fe, 4-1 Mn, 23-29 Ni, 7-10 Al.
The preparation method of the CoCrFeMnNiAl high-entropy alloy comprises the following steps:
weighing reaction materials according to a preset proportion, and placing the reaction materials in a planetary ball mill for ball milling;
pressing the ball-milled reaction materials into cake-shaped blanks with the diameter of 80 mm and the height of about 50 mm on a press machine;
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 a system generates a self-propagating reaction to obtain a base metal alloy;
performing vacuum induction secondary smelting on the base metal alloy to obtain an ingot;
and (5) carrying out hot rolling on the cast ingot at 1200 ℃ for 50% of deformation, carrying out solution treatment at 1150 ℃ for 30min, and carrying out water cooling.
The invention has the beneficial effects that: the invention has simple process flow, simplified production equipment and simple operation; compared with the currently used process for preparing the high-entropy alloy by a vacuum arc furnace smelting method, the process is simple, the energy consumption is low, and the commercial production scale is realized; according to the invention, on the basis of the CoCrFeMnNi high-entropy alloy with the equal molar ratio, the adiabatic temperature is reduced by adding the diluent, and meanwhile, the Al content is regulated and controlled.
Drawings
FIG. 1 is an XRD pattern for examples 1, 2, 3; FIG. 2 is an XRD pattern for examples 4, 5, 6; FIGS. 3, 4, 5, 6, 7 and 8 are metallographic structure diagrams of examples 1, 2, 3, 4, 5 and 6, respectively; fig. 9, fig. 10, fig. 11, fig. 12, fig. 13, and fig. 14 are SEM texture maps 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 atomic percentage: 27-29 Co, 17-18 Cr, 15-19 Fe, 4-1 Mn, 23-29 Ni, 7-10 Al.
The invention discloses a preparation method of a CoCrFeMnNiAl high-entropy alloy, which comprises the following steps:
weighing reaction materials according to a preset proportion, and placing the reaction materials in a planetary ball mill for ball milling;
pressing the ball-milled reaction materials into cake-shaped blanks with the diameter of 80 mm and the height of 50 mm on a press machine;
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 a system generates a self-propagating reaction to obtain a base metal alloy;
performing vacuum induction secondary smelting on the base metal alloy to obtain an ingot;
and (5) carrying out hot rolling on the cast ingot at 1200 ℃ for 50% of deformation, carrying out solution treatment at 1150 ℃ for 30min, and carrying out water cooling.
The preparation method comprises the following steps of (1) ball milling parameters: the time is 8 hours, alumina ball grinding beads are selected, the ball material ratio is 2:1, and the rotating speed is 80 r/min; the pressure of the press is 70 MPa.
In the preparation method, the reactant material adopted in the reaction material in the step (2) 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 pressure is 4-6 Mpa.
The preparation method comprises the step (4) of preheating for 60 min and vacuum degree of 10 -2 Pa, keeping alloying for 10 min.
According to the preparation method, in the step (5), the hot rolling is carried out, the temperature is increased to 1200 ℃ at the speed of 10 ℃/min, the heat preservation is carried out for 30min, the reduction of each pass is 0.3 mm, and the heat preservation is carried out for 5 min after each pass is re-melted. The solution treatment is carried out by heating to 1150 ℃ at the heating speed of 10 ℃/min and preserving the temperature for 30min for water quenching.
According to the design of the CoCrFeMnNi high-entropy alloy with the equal molar ratio, the content of Al is changed by adding the diluent to change the adiabatic temperature, the base metal alloy is prepared by an aluminothermic method, and then secondary smelting is carried out by vacuum medium-frequency induction smelting, so that the internal defects of the aluminothermic method are eliminated, and the block 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 large-scale production.
The following are specific examples of the present invention and the technical solutions of the present invention will be further described with reference to the examples, but the present invention is not limited to the examples:
example 1:
an initial casting blank is prepared by an aluminothermic method, and the preparation steps are as follows:
table 1 example 1 cocrfelmnial high entropy alloy reaction mass mix (wt.%) of cocrfelminal
(1) Preparing materials: weighing 1kg of reaction raw materials according to the reaction material proportion shown in Table 1, and evenly mixing each raw material by dividing into four parts on average;
(2) ball milling: putting the uniformly mixed reaction materials into a QM-ISP4 planetary ball mill for ball milling at the rotating speed of 80 r/min for 8 hours, wherein the turning direction of the ball mill is changed every 2 hours to prevent agglomeration, and the ball milling beads are made of Al 2 O 3 The ball material ratio is 1: 2;
(3) the preparation by the aluminothermic method comprises the following steps: after the ball milling is finished, the reaction materials are placed into a die, an oil pressure press is used for applying pressure of 70 MPa, and after pressure maintaining is carried out for 4 min, the materials are pressed into round cake-shaped green bodies with the diameter of about 80 mm and the thickness of about 50 mm. Placing the pressed blank in a copper crucible, placing 2 g of ignition agent sheet above the blank, placing the copper crucible in a closed reaction kettle for gas washing, introducing 5 MPa argon as protective gas, heating by electrifying, and igniting the ignition agent when the temperature in the kettle rises to more than 280 deg.CAnd initiating aluminothermic reaction, wherein the pressure and the temperature in the kettle are quickly increased, and after the reaction starts, closing the heating switch. Cooling the generated product to room temperature along with the furnace under the protection of argon atmosphere, opening the reaction kettle, taking out the product, and coating a layer of Al on the alloy 2 O 3 And (4) coating the layers, and breaking the coated layers to obtain the block alloy.
Vacuum intermediate frequency induction melting and secondary smelting, which comprises the following preparation steps:
(1) preparing a base material: processing CoCrFeMnNiAl high-entropy alloy prepared by a thermite method into a strip with the width of 10 mm by linear cutting, and polishing away stains on the surface to prevent the introduction of impurities;
(2) vacuum intermediate frequency induction smelting: preheating a diffusion pump of a medium-frequency induction furnace for 40-50 min in a smelting process, putting a block alloy into a magnesia-alumina spinel crucible with the volume of 3 kg, putting a metal trapezoidal die which is brushed with a release agent and preheated to 300 ℃ in advance into the smelting furnace, opening a vacuum system, and ensuring that the vacuum degree is 10 -2 And (2) opening a smelting system after Pa, sequentially adjusting the heating power from 0 kw at a gradient of 5 kw, keeping for 5 min after each adjustment to ensure uniform heating, adjusting the heating power to 5 kw to keep the temperature for 10 min to ensure uniform components after the block alloy is completely molten into liquid through an observation port, turning over the crucible, pouring the molten metal into a mold, and taking out after cooling.
The mechanical properties of the material at room temperature are tested. The hardness test adopts a WILSON-VH1102 type full-automatic microhardness test system, the load is 300 g, the loading time is 12 s, 10 points of each sample measurement are averaged, and the average value is expressed by Vickers hardness HV 0.3. The tensile test was carried out on an Shimadzu AGS-X300 kN electronic universal tester with a tensile rate of 0.5 mm/min, and 3 sets of parallel experiments were carried out on each component sample in a displacement loading manner. The results showed 169.8 HV0.3 of hardness, 470.98 MPa of tensile strength and 44.07% of elongation.
Example 2:
the reaction mass of this example is shown in Table 2, the procedure for its preparation is the same as in example 1, and the room temperature mechanical properties test results are: the hardness is 210.2 HV0.3, the tensile strength is 522.39 MPa, and the elongation is 40.03%.
Table 2 example 2 cocrfelmnial high entropy alloy reaction mass mix (wt.%) of cocrfelminal
Example 3:
the reaction mass of this example is shown in Table 3, the procedure for its preparation is the same as in example 1, and the room temperature mechanical properties test results are: hardness 188.4 HV0.3, tensile strength 525.05 MPa, and elongation 48.86%.
Table 3 example 3 cocrfelmnial high entropy alloy reaction mass mix (wt.%) of cocrfelminal
Example 4:
the CoCrFeMnNiAl high-entropy alloy cast ingot obtained in the example 1 is subjected to hot rolling, and the hot rolling step comprises:
a plate with the thickness of 5 mm is cut from the high-entropy alloy ingot casting in example 1 by linear cutting, the high-entropy alloy ingot casting is heated to 1200 ℃ from room temperature by a box furnace at the heating rate of 10 ℃/min and is kept warm for 30min, hot rolling is carried out by a two-roll cold-hot rolling mill, the reduction is 0.3 mm per pass, the high-entropy alloy ingot casting is placed into the box furnace for keeping warm for 2 min per pass in order to prevent the reduction of the rolling temperature, the rolling deformation is 50 percent, a hot rolled plate with the thickness of 2.5 mm is obtained, the hot rolled plate cooled at room temperature is placed into the box furnace to be heated to 1150 ℃ at the same heating rate and is kept warm for 30min, solid solution treatment is carried out, and the hot rolled plate is taken out and cooled by water.
The same room temperature mechanical properties test and 800 ℃ high temperature tensile properties test as in example 1 were carried out. The high-temperature stretching at 800 ℃ is carried out on an AGS-X300 kN electronic universal tester, the stretching speed is 0.2 mm/min, a displacement loading mode is adopted, and 3 groups of parallel experiments are carried out on each component. The test data is shown in table 4:
TABLE 4 example 4CoCrFeMnNiAl high entropy alloy hot rolling state mechanical property
Example 5:
the CoCrFeMnNiAl high-entropy alloy obtained in example 2 is subjected to hot rolling treatment, the preparation steps are the same as those of example 4, and the mechanical property data are shown in Table 5.
TABLE 5 example 5 CoCrFeMnNiAl high entropy alloy hot rolled state mechanical properties
Example 6:
the CoCrFeMnNiAl high-entropy alloy obtained in example 3 was hot-rolled according to the same preparation procedure as in example 4, and the mechanical property data are shown in Table 6.
TABLE 6 example 6 CoCrFeMnNiAl high entropy alloy hot rolling state mechanical property
The data show that the invention realizes the preparation of CoCrFeMnNiAl high-entropy alloys with different Al contents.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are 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 (7)
1. A CoCrFeMnNiAl high-entropy alloy is characterized by comprising the following components in atomic percentage: 27-29 Co, 17-18 Cr, 15-19 Fe, 4-1 Mn, 23-29 Ni, 7-10 Al.
2. The preparation method of the CoCrFeMnNiAl high-entropy alloy as claimed in claim 1, characterized by comprising the steps of:
weighing reaction materials according to a preset proportion, and placing the reaction materials in a planetary ball mill for ball milling;
pressing the ball-milled reaction materials into cake-shaped blanks with the diameter of 80 mm and the height of 50 mm on a press machine;
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 a system generates a self-propagating reaction to obtain a base metal alloy;
performing vacuum induction secondary smelting on the base metal alloy to obtain an ingot;
and (5) carrying out hot rolling on the cast ingot at 1200 ℃ for 50% of deformation, carrying out solution treatment at 1150 ℃ for 30min, and carrying out water cooling.
3. The preparation method of the CoCrFeMnNiAl high-entropy alloy as claimed in claim 2, characterized in that: the ball milling parameters in the step (1): the time is 8 hours, alumina ball grinding beads are selected, the ball material ratio is 2:1, and the rotating speed is 80 r/min; the pressure of the press is 70 MPa.
4. The preparation method of the CoCrFeMnNiAl high-entropy alloy as claimed in claim 2, characterized in that: in the reaction materials 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 (or Ni) and Al powder.
5. The preparation method of the CoCrFeMnNiAl high-entropy alloy as claimed in claim 2, characterized in that: and (3) preheating at 280-340 ℃, wherein the protective atmosphere is argon, and the pressure is 4-6 MPa.
6. The preparation method of the CoCrFeMnNiAl high-entropy alloy as claimed in claim 2, characterized in that: the preheating time of the step (4) is 60 min, and the vacuum degree is 10 -2 Pa, keeping alloying for 10 min.
7. The preparation method of the CoCrFeMnNiAl high-entropy alloy as claimed in claim 2, characterized in that: the hot rolling in the step (5) is carried out, the temperature is increased to 1200 ℃ at the speed of 10 ℃/min, the heat preservation is carried out for 30min, the reduction of each pass is 0.3 mm, and the heat preservation is carried out for 5 min after each pass is returned to the furnace; the solution treatment is carried out by heating to 1150 ℃ at the heating speed of 10 ℃/min and preserving the temperature for 30min for water quenching.
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| CN115894043A (en) * | 2022-11-08 | 2023-04-04 | 深圳市蓝海永兴实业有限公司 | High-entropy MAlB ceramic material and preparation method thereof |
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| CN107760963A (en) * | 2017-10-26 | 2018-03-06 | 福建工程学院 | A kind of nitrogenous FeCoCrNiMn high-entropy alloys and preparation method thereof |
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| CN107760963A (en) * | 2017-10-26 | 2018-03-06 | 福建工程学院 | A kind of nitrogenous FeCoCrNiMn high-entropy alloys and preparation method thereof |
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| ALBERTO FERRARI等: "Surface segregation in Cr-Mn-Fe-Co-Ni high entropy alloys", APPLIED SURFACE SCIENCE, pages 1 - 7 * |
| 农智升;李宏宇;王继杰;: "AlCrFeNiTi高熵合金热稳定性的研究", 稀有金属材料与工程, no. 01 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115894043A (en) * | 2022-11-08 | 2023-04-04 | 深圳市蓝海永兴实业有限公司 | High-entropy MAlB ceramic material and preparation method thereof |
| CN115894043B (en) * | 2022-11-08 | 2023-10-27 | 深圳市蓝海永兴实业有限公司 | High-entropy MAlB ceramic material and preparation method thereof |
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