Spatial net structure high-entropy alloy reinforced aluminum matrix composite and preparation method thereof

Abstract

The invention relates to the technical field of metal material processing, and particularly discloses a high-entropy alloy reinforced aluminum-based composite material with a spatial net structure and a preparation method thereof.The composite material takes an aluminum alloy as a matrix and takes an AlFeCoCrNi high-entropy alloy as a reinforcement, the mass ratio of the high-entropy alloy to the aluminum alloy is 1: 10, and the preparation method comprises the steps that 10% AlFeCoCrNi / 5086Al mixed powder is obtained through a V-shaped powder mixer; in a vacuum glove box, the powder is laid in a cylindrical rubber tube with the diameter of 20 mm in a crossed mode according to the ratio of 10% AlFeCoCrNi / 5086Al to pure Al powder being 2: 1, and layered powder is formed; and carrying out cold isostatic pressing to form a layered structure, and extruding and forming the composite material bar with the layered structure at 460 DEG C through an equal channel angular extrusion die. And cutting into 2 mm slices through linear cutting, polishing and grinding surface processing traces, and carrying out ultrasonic cleaning. And finally, the two layers are staggered, the 2mm composite material with the three-dimensional space net structure is obtained through cold rolling forming, and the rolling ratio is 2: 1.

Description

Technical Field

[0001] The invention relates to the technical field of metal material processing, in particular to a spatial network structure high entropy alloy reinforced aluminum-based composite material and a preparation method thereof. Background Art

[0002] High entropy alloy is an alloy composed of five or more main elements, and the atomic content of each element is between 5% and 35%. It breaks the design concept of traditional alloys based on one or two metal elements. It has excellent comprehensive performance and is hailed as one of the most promising materials in the future. At present, the research on high entropy alloys is mainly focused on the performance of single-phase solid solutions such as CoCrFeNi and CrFeNiCu, and the preparation methods used are mostly arc melting. Arc melting will inevitably cause problems such as thermal expansion, separation of components and interface separation, which will lead to many defects such as voids in the prepared high entropy alloys, and it is easy to show an inverted strength-toughness relationship, that is, while increasing strength, it will lead to a sharp decrease in plasticity and toughness, which will greatly limit the development of high entropy alloy systems and preparation processes.

[0003] In the prior art, some aluminum alloys are prepared by isostatic sintering. As is well known, cold rolling is a method of cold rolling and pressing a sheet material after pickling to remove the oxide scale. It is a method of preparing particle-reinforced metal matrix composite materials.

[0004] The Chinese invention patent application with publication number CN114807712A discloses a method for preparing a high entropy alloy particle reinforced aluminum-based composite material, comprising the steps of milling mixed powder to obtain composite material powder; preparing a composite material block by spark plasma sintering; and hot extruding the composite material block to prepare a CoCrFeNiMn / 7075Al composite material. The obtained aluminum alloy has good mechanical properties, with a tensile strength of 435MPa and an elongation of 11.2%.

[0005] The Chinese invention patent application with publication number CN114309625A discloses a method for preparing a high entropy alloy particle reinforced aluminum-based composite material, wherein high entropy alloy powder is mixed with aluminum alloy powder, ball-milled and pressed into shape, the molded part is first sintered, and then hot-extruded to obtain a high entropy alloy reinforced aluminum-based composite material. The high entropy alloy reinforced aluminum-based composite material has a high strength and toughness, with a tensile strength of more than 780MPa and a fracture toughness of 30MPa·m 1 / 2 above.

[0006] High entropy alloy reinforced aluminum-based composites have the advantages of high specific strength, high specific modulus and corrosion resistance, and have been widely used in aerospace and marine equipment. However, the hardness and wear resistance of aluminum alloys are generally not high. At present, aluminum-based composites prepared by using SiC, Al2O3, B4C, etc. as reinforcement phases can effectively improve the hardness and other properties of aluminum alloys, but ceramic particles as reinforcement phases have disadvantages such as poor interface bonding and poor wettability, which affects the application of aluminum-based composites in aerospace and marine equipment.

[0007] At present, there are few reports at home and abroad on the method of obtaining 10% AlFeCoCrNi / 5086Al layered structure by cold isostatic pressing preforming - obtaining 10% AlFeCoCrNi / 5086Al layered structure by equal-diameter angular extrusion - obtaining 10% AlFeCoCrNi / 5086Al network structure high entropy alloy composite materials. Therefore, it is necessary to propose a method for preparing a spatial network structure high entropy alloy reinforced aluminum-based composite material to prepare a high entropy alloy reinforced aluminum-based composite material with superior performance to meet the application of aerospace and marine equipment materials. Summary of the invention

[0008] The purpose of the present invention is to provide a spatial network structure high entropy alloy reinforced aluminum-based composite material and a preparation method thereof in view of the defects of the prior art, so as to solve the problems raised by the above-mentioned background technology.

[0009] To achieve the above object, the present invention provides the following technical solution: a method for preparing a spatial network structure high entropy alloy reinforced aluminum-based composite material, the specific steps are as follows:

[0010] S01. The high entropy alloy and 5086 aluminum are fully mixed in a TG-2 type V-type powder mixer at a mass ratio of 1:10, wherein the high entropy alloy powder used has a molar ratio of 5mol% to 35mol% of Al, 5mol% to 35mol% of Fe, 5mol% to 35mol% of Ni, 5mol% to 35mol% of Co, and 5mol% to 35mol% of Cr;

[0011] S02, 10% AlFeCoCrNi / 5086Al and pure aluminum powder are uniformly filled into a rubber tube with a diameter of 20 mm in a ratio of 1:1, and preformed by LDJ200 / 600-300 type cold isostatic pressing;

[0012] S03, extruding the preformed composite material rod through a YJ32-315A hydraulic press and a homemade equal-diameter angular extrusion die at 460°C to obtain a 10% AlFeCoCrNi / 5086Al layered structure, and then cutting the extruded rod into 1 mm uniform thin slices through a DK7735 taper wire cutting machine, polishing and grinding to remove surface processing marks, and finally ultrasonically cleaning in anhydrous ethanol;

[0013] S04. The cleaned composite material is pickled to remove the oxide scale, and then rolled on a JK-GYJ-100B electric roller mill for multiple passes with a rolling ratio of 2:1 to obtain a sheet with a thickness of 2 mm.

[0014] As a preferred technical solution of the present invention, the weighing of each metal powder in step S01 is carried out in a vacuum glove box, and the particle size of each metal powder is 10 to 50 μm.

[0015] As a preferred technical solution of the present invention, the mixing of the metal powders in step S01 is performed under an inert gas atmosphere.

[0016] As a preferred technical solution of the present invention, in step S01, the metal powders are mixed in the TG-2 V-type powder mixer for 10 hours at a rotation speed of 100 r / min, using 10-50 μm AlFeNiCoCr powder and 10-50 μm 5086 aluminum powder.

[0017] As a preferred technical solution of the present invention, in step S02, the powder layer thickness is controlled by mass ratio. The density of the 10% AlFeCoCrNi / 5086Al composite material is measured by the Archimedean principle drainage method to be the same as the density of pure Al. The materials are weighed in a vacuum glove box according to an equal mass ratio, and 3 g of powder is spread on each layer and filled into a rubber tube, and then compacted to obtain a layered powder with a length of about 20 cm, which is then preformed by cold isostatic pressing.

[0018] As a preferred technical solution of the present invention, in step S03, the cold isostatically preformed rod is extruded at 460°C in an equal-diameter angular extrusion die, and a 4 cm long 20 mm diameter copper plug is placed at the lower end during the extrusion process, so that the composite material obtains greater deformation resistance during the extrusion process and makes the force more uniform; then, the extruded rod is cut into 1 mm uniform thin slices by wire cutting, and the surface processing marks are removed by polishing and grinding, and finally ultrasonically cleaned in anhydrous ethanol.

[0019] A spatial network structure high entropy alloy particle reinforced aluminum-based composite material, the composite material is based on an aluminum alloy as a matrix and a high entropy alloy as a reinforcement phase, and is prepared by the preparation method described in any one of claims 1 to 6, the mass ratio of the high entropy alloy to aluminum is 1:10, and the high entropy alloy is an AlFeNiCoCr series high entropy alloy.

[0020] As a preferred technical solution of the present invention, the composite material has a hardness of 200-350 HV, a tensile strength of 340-360 MPa, and an elongation of 20%-27%.

[0021] Compared with the prior art, the present invention has the following beneficial effects:

[0022] The invention provides a space high entropy alloy particle reinforced aluminum-based composite material, which takes aluminum as a matrix and a high entropy alloy as a reinforcement, and is prepared by the preparation method of the invention, wherein the mass ratio of the high entropy alloy to the aluminum alloy is 1:10, and the high entropy alloy is an AlFeNiCoCr series high entropy alloy, which has good hardness and strength and can meet the application of aerospace and marine equipment materials.

[0023] The advantages of the composite material are as follows: the hardness of the composite material is 200-350 HV, the tensile strength is 340-360 MPa, and the elongation is 20%-27%.

[0024] The specific advantages of the preparation method are as follows:

[0025] 1. The metal elements Al, Fe, Ni, Co, and Cr contained in the high entropy alloy powder are all non-precious metals, and the production cost is low;

[0026] 2. 5086Al and AlFeNiCoCr high entropy alloy are fully prepared to obtain 10% AlFeNiCoCr3 / 5086Al;

[0027] 3. Using AlFeNiCoCr high entropy alloy powder particles as reinforcement, 5086 aluminum and pure aluminum as matrix, and equal-diameter angular extrusion-cold rolling to prepare a mesh structure aluminum-based composite material with the advantages of high strength and high toughness. The high strength of the composite material is mainly improved by the high entropy alloy as a reinforcement. The addition of high entropy alloy makes it easier to achieve solid solution strengthening, and the large deformation of cold rolling makes it easier to achieve grain refinement and dislocation strengthening. The re-stretching deformation is mainly divided into three stages. The first stage is provided by pure aluminum for property deformation, because pure aluminum has low strength but good plasticity. When the yield of pure aluminum is reached, it enters the second stage. The second stage is provided by the 5086 aluminum matrix. Now plastic deformation occurs in the matrix. When the dislocation moves and encounters high entropy alloy particles, it will pass through the high entropy alloy particles. The third stage is the 10% AlFeNiCoCr / 5086Al / Al collaborative deformation stage. When the strength reaches the strength limit of the interface between 10% AlFeNiCoCr / 5086Al and pure aluminum, ductile fracture occurs at the interface;

[0028] 4. The preparation process is simple and the molding cycle is short, and particle-reinforced aluminum-based composite materials with a mesh structure having high strength and toughness can be obtained. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 XRD pattern of 10%AlFeNiCoCr / 5086Al / Al composite material;

[0030] Figure 2 XRD diagram of 10% AlFeNiCoCr / 5083Al / Al spatial network structure composite material;

[0031] Figure 3 Schematic diagram of the microstructure of 10% AlFeNiCoCr / 5083Al / Al spatial network structure composite material;

[0032] Figure 4 This is a process flow chart for preparing 10% AlFeNiCoCr / 5083Al / Al spatial network structure composite material. DETAILED DESCRIPTION

[0033] The preferred embodiments of the present invention are described in detail below in conjunction with the accompanying drawings so that the advantages and features of the present invention can be more easily understood by those skilled in the art, thereby making a clearer and more definite definition of the protection scope of the present invention.

[0034] like Figure 4 As shown, the preparation method of the spatial network structure high entropy alloy reinforced aluminum-based composite material of the present invention comprises the following steps:

[0035] S01. In a vacuum glove box, weigh 20 g of AlFeNiCoCr high entropy alloy and 180 g of 5086 aluminum, add them into a TG-2 V-type powder mixing tank, and mix them thoroughly for 10 hours at a speed of 100 r / min.

[0036] S02. In a vacuum glove box, 10% AlFeCoCrNi / 5086Al and pure aluminum powder were uniformly filled into a rubber tube with a diameter of 20 mm in a ratio of 2:1. Each layer of powder was compacted once, and the mass of each layer was 3±0.01 g. Finally, it was preformed by LDJ200 / 600-300 cold isostatic pressing;

[0037] S03, the preformed composite material rod is extruded into a 10% AlFeCoCrNi / 5086Al layered structure by a YJ32-315A hydraulic press and a homemade equal-diameter angular extrusion die at 460°C. Before extrusion, the 10% AlFeCoCrNi / 5086Al / Al rod is kept warm in the equal-diameter angular extrusion die for 30 minutes, and a copper rod with a diameter of 20mm and a length of 4cm is placed at its lower end. After extrusion, the pressure is maintained for 3 minutes to prevent the composite material from rebounding due to plastic deformation. The extruded rod is then cut into 1mm uniform thin slices by a DK7735 taper wire cutting machine, and the surface processing marks are removed by polishing and grinding. Finally, it is ultrasonically cleaned (in anhydrous ethanol) for 5 minutes.

[0038] S04. The cleaned composite material is pickled to remove the oxide scale. The acid used is diluted sulfuric acid to remove the oxide layer and impurities on the surface. Then it is rolled on the K-GYJ-100B electric roller mill for multiple passes, with a single pressing amount of 0.1mm and a rolling ratio of 2:1, to obtain a sheet with a thickness of about 2mm.

[0039] The high entropy alloy particle reinforced aluminum matrix composite material prepared by the above preparation method has 5086 aluminum and pure aluminum as the matrix, high entropy alloy as the reinforcement phase, the mass ratio of high entropy alloy to aluminum is 1:10, and the high entropy alloy is AlFeNiCoCr series high entropy alloy. The hardness of the composite material tested by HV-30 Vickers hardness tester is 200-350HV; the tensile strength tested by UTM5305 universal testing machine is 340-360MPa, and the elongation measured by extensometer is 20%-27%.

[0040] The preparation method of the present invention and the components and properties of the composite material will be specifically described below in conjunction with Examples 1 to 2. The following examples are only used to illustrate the present invention in detail and do not limit the protection scope of the present invention in any form.

[0041] Example 1: A method for preparing a spatial network structure high entropy alloy reinforced aluminum-based composite material, the specific steps are as follows:

[0042] S01, preparing 10% AlFeNiCoCr / 5086Al mixed powder;

[0043] In a vacuum glove box, weigh 20 g of AlFeNiCoCr high entropy alloy and then weigh 180 g of 5086 aluminum, add them into a TG-2 V-type powder mixing tank, and mix them thoroughly for 10 hours at a rotation speed of 100 r / min.

[0044] Preforming of S02, 10% AlFeNiCoCr / 5086Al / Al layered composites;

[0045] In a vacuum glove box, 10% AlFeCoCrNi / 5086Al and pure aluminum powder were uniformly filled into a rubber tube with a diameter of 20 mm in a ratio of 2:1, 10% AlFeCoCrNi / 5086Al: pure Al = 2:1, and each layer of powder was compacted once; finally, it was preformed by LDJ200 / 600-300 cold isostatic pressing.

[0046] S03, equal channel angular extrusion 10% AlFeNiCoCr / 5086Al / Al layered composite molding;

[0047] The preformed composite material rod was extruded by a YJ32-315A hydraulic press and a homemade equal-diameter angular extrusion die at 460°C to obtain a 10% AlFeCoCrNi / 5086Al layered structure. Before extrusion, the 10% AlFeCoCrNi / 5086Al / Al rod was kept warm in the equal-diameter angular extrusion die for 30 minutes, the extrusion speed was 10mm / s, and a copper rod with a diameter of 20mm and a length of 4cm was placed at its lower end. After extrusion, the pressure was maintained for 3 minutes to prevent the composite material from rebounding due to plastic deformation. The extruded rod was then cut into 1mm uniform thin slices by a DK7735 taper wire cutting machine, and the surface processing marks were removed by polishing and grinding. Finally, it was ultrasonically cleaned (in anhydrous ethanol) for 5 minutes.

[0048] S04, cold rolling treatment;

[0049] The cleaned composite material is pickled to remove the oxide scale. The acid used is diluted sulfuric acid to remove the oxide layer and impurities on the surface. Then it is rolled on the K-GYJ-100B electric roller mill for multiple passes, with a single pressing amount of 0.1mm and a rolling ratio of 2:1, to obtain a sheet with a thickness of about 2mm.

[0050] The high entropy alloy particle reinforced aluminum matrix composite material prepared by the above preparation method has 5086 aluminum and pure aluminum as the matrix, high entropy alloy as the reinforcement phase, the mass ratio of high entropy alloy to aluminum is 1:10, and the high entropy alloy is AlFeNiCoCr series high entropy alloy. The hardness of the composite material tested by HV-30 Vickers hardness tester is 200-350HV; the tensile strength tested by UTM5305 universal testing machine is 340-360MPa, and the elongation measured by extensometer is 20%-27%.

[0051] Example 2: A method for preparing a spatial network structure high entropy alloy reinforced aluminum-based composite material, the specific steps are as follows:

[0052] S01, preparing 10% AlFeNiCoCr / 5086Al mixed powder;

[0053] In a vacuum glove box, weigh 20 g of AlFeNiCoCr high entropy alloy and then weigh 180 g of 5086 aluminum, add them into a TG-2 V-type powder mixing tank, and mix them thoroughly for 10 hours at a rotation speed of 100 r / min.

[0054] S02, preparing premixed powder;

[0055] In a vacuum glove box, 10% AlFeCoCrNi / 5086Al and pure aluminum powder were uniformly filled into a rubber tube with a diameter of 20 mm in a ratio of 3:3, 10% AlFeCoCrNi / 5086Al: pure Al = 3:3, and compaction was performed every time two layers of powder were filled; finally, pre-formed by LDJ200 / 600-300 cold isostatic pressing.

[0056] S03, equal channel angular extrusion 10% AlFeNiCoCr / 5086Al / Al layered composite molding;

[0057] The preformed composite material rod was extruded by a YJ32-315A hydraulic press and a homemade equal-diameter angular extrusion die at 460°C to obtain a 10% AlFeCoCrNi / 5086Al layered structure. Before extrusion, the 10% AlFeCoCrNi / 5086Al / Al rod was kept warm in the equal-diameter angular extrusion die for 30 minutes, the extrusion speed was 10mm / s, and a copper rod with a diameter of 20mm and a length of 4cm was placed at its lower end. After extrusion, the pressure was maintained for 3 minutes to prevent the composite material from rebounding due to plastic deformation. The extruded rod was then cut into 1mm uniform thin slices by a DK7735 taper wire cutting machine, and the surface processing marks were removed by polishing and grinding. Finally, it was ultrasonically cleaned (in anhydrous ethanol) for 5 minutes.

[0058] S04, cold rolling treatment;

[0059] The cleaned composite material is pickled to remove the oxide scale. The acid used is diluted sulfuric acid to remove the oxide layer and impurities on the surface. Then it is rolled on the K-GYJ-100B electric roller mill for multiple passes, with a single pressing amount of 0.1mm and a rolling ratio of 2:1, to obtain a sheet with a thickness of about 2mm.

[0060] The high entropy alloy particle reinforced aluminum matrix composite material prepared by the above preparation method has 5086 aluminum and pure aluminum as the matrix, high entropy alloy as the reinforcement phase, the mass ratio of high entropy alloy to aluminum is 1:10, and the high entropy alloy is an AlFeNiCoCr series high entropy alloy. The hardness of the composite material tested by the HV-30 Vickers hardness tester is 190-300HV; the tensile strength tested by the UTM5305 universal testing machine is 300-330MPa, and the elongation measured by the extensometer is 20%-25%.

[0061] The above embodiments only express the implementation methods of the present invention, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, and these all belong to the protection scope of the present invention.

Claims

1. A method for preparing a spatial network structure high entropy alloy reinforced aluminum-based composite material, characterized in that: The specific steps are as follows: S01. The high entropy alloy and 5086 aluminum are fully mixed in a TG-2 type V-type powder mixer at a mass ratio of 1:10, wherein the high entropy alloy powder used has a molar ratio of 5mol% to 35mol% of Al, 5mol% to 35mol% of Fe, 5mol% to 35mol% of Ni, 5mol% to 35mol% of Co, and 5mol% to 35mol% of Cr; S02, 10% AlFeCoCrNi / 5086Al and pure aluminum powder are uniformly filled into a rubber tube with a diameter of 20 mm in a ratio of 1:1, and preformed by LDJ200 / 600-300 type cold isostatic pressing; S03, extruding the preformed composite material rod through a YJ32-315A hydraulic press and a homemade equal-diameter angular extrusion die at 460°C to obtain a 10% AlFeCoCrNi / 5086Al layered structure, and then cutting the extruded rod into 1 mm uniform thin slices through a DK7735 taper wire cutting machine, polishing and grinding to remove surface processing marks, and finally ultrasonically cleaning in anhydrous ethanol; S04. The cleaned composite material is pickled to remove the oxide scale, and then rolled on a JK-GYJ-100B electric roller mill for multiple passes with a rolling ratio of 2:1 to obtain a sheet with a thickness of 2 mm.

2. The method for preparing the spatial network structure high entropy alloy reinforced aluminum-based composite material according to claim 1, characterized in that: The weighing of each metal powder in step S01 is carried out in a vacuum glove box, and the particle size of each metal powder is 10 to 50 μm.

3. The method for preparing the spatial network structure high entropy alloy reinforced aluminum-based composite material according to claim 2, characterized in that: The mixing of the metal powders in step S01 is performed under an inert gas atmosphere.

4. The method for preparing the spatial network structure high entropy alloy reinforced aluminum-based composite material according to claim 1, characterized in that: In step S01, the metal powders are mixed in a TG-2 V-type powder mixer for 10 hours at a rotation speed of 100 r / min, using 10-50 μm AlFeNiCoCr powder and 10-50 μm 5086 aluminum powder.

5. The method for preparing the spatial network structure high entropy alloy reinforced aluminum-based composite material according to claim 1, characterized in that: In step S02, the powder layer thickness is controlled by the mass ratio. The density of the 10% AlFeCoCrNi / 5086Al composite material is measured by the Archimedean principle and the drainage method, and is the same as the density of pure Al. The materials are weighed in a vacuum glove box according to the same mass ratio, and 3 g of powder is spread on each layer and filled into a rubber tube. The powder is then compacted to obtain a layered powder with a length of about 20 cm, and finally preformed by cold isostatic pressing.

6. The method for preparing the spatial network structure high entropy alloy reinforced aluminum-based composite material according to claim 1, characterized in that: In step S03, the cold isostatically preformed rod is extruded at 460°C in an equal-diameter angular extrusion die. During the extrusion process, a 4 cm long and 20 mm diameter copper plug is placed at the lower end to allow the composite material to obtain greater deformation resistance during the extrusion process and make the force more uniform. Then, the extruded rod is cut into 1 mm uniform thin slices by wire cutting, and the surface processing marks are removed by polishing and grinding, and finally ultrasonically cleaned in anhydrous ethanol.

7. A spatial network structure high entropy alloy particle reinforced aluminum matrix composite material, characterized in that: The composite material is based on an aluminum alloy as a matrix and a high entropy alloy as a reinforcement phase, and is prepared by the preparation method described in any one of claims 1 to 6, the mass ratio of the high entropy alloy to aluminum is 1:10, and the high entropy alloy is an AlFeNiCoCr series high entropy alloy.

8. The spatial network structure high entropy alloy particle reinforced aluminum-based composite material according to claim 7, characterized in that: The composite material has a hardness of 200-350 HV, a tensile strength of 340-360 MPa, and an elongation of 20%-27%.

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