CN108723371B - Preparation method of high-entropy alloy reinforced aluminum matrix composite - Google Patents
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Abstract
The invention discloses a high-entropy alloy reinforced aluminum matrix composite and a preparation method thereof. The preparation process comprises the steps of designing a high-entropy alloy system with high hardness, and preparing high-entropy alloy powder by vacuum high-energy ball milling after calculating the mixture ratio; adding aluminum alloy powder according to the mixture ratio and mixing the aluminum alloy powder; the high-entropy alloy reinforced aluminum matrix composite material is prepared by adopting a hot extrusion technology. The obtained composite material can improve the bonding strength of the reinforcing phase and the interface of the aluminum alloy matrix, so that the composite material has good mechanical property.
Description
Technical Field
The invention belongs to the technical field of metal matrix composite materials, and particularly relates to a high-entropy alloy reinforced aluminum alloy composite material and a preparation method thereof.
Background
The bulk high-entropy alloy (HEA) has a series of excellent mechanical properties different from the traditional crystalline alloy, such as high strength, high hardness, low elastic modulus, large elastic strain limit and the like, so that the alloy is considered to be a structural material with great potential. However, the high brittleness allows the HEA material to fracture catastrophically in a catastrophic manner without significant room temperature macroscopic plastic deformation; the high brittleness and high hardness bring great difficulty to the processing of the material. These severely limit the large-scale application of HEA as an advanced structural material in engineering. Therefore, the problems of room temperature brittleness and difficult processing are developed to become important bottleneck of the application of the HEA material.
Disclosure of Invention
In order to overcome the defects, the invention provides a high-entropy alloy reinforced aluminum-based composite material and a preparation method thereof, which can improve the plasticity of the composite material while maintaining the excellent strength and hardness of the composite material.
In order to achieve the purpose, the invention adopts the following technical scheme:
the high-entropy alloy reinforced aluminum-based composite material is characterized in that aluminum alloy is used as a matrix, high-entropy alloy is used as a reinforcing phase, and the high-entropy alloy is high-entropy alloy powder with a body-centered cubic structure.
The high-entropy alloy is a body-centered cubic solid solution (BCC) alloy system generated by alloy components according to an atomic ratio; in the high-entropy alloy, the purity of metal powder of Al, Fe, Cr, Co, Ni, Cu and Ti is more than 99.9%, and the granularity is less than or equal to 45 mu m. The matrix is aluminum alloy powder, the purity of the aluminum alloy powder is more than 99.9%, and the granularity is less than or equal to 300 mu m. The composite aluminum alloy substrate may be a 2-series to 5-series aluminum alloy.
In the composite material, the mass content of the high-entropy alloy is 10-40wt%, and the mass content of the aluminum alloy powder is 60-90 wt%.
The preparation method of the high-entropy alloy reinforced aluminum matrix composite is characterized by comprising the following steps of:
1) selecting raw materials: the purity of the metal powder of Al, Fe, Cr, Co, Ni, Cu and Ti is more than 99.9 percent, and the particle size is less than or equal to 45 mu m; the purity of the aluminum alloy powder is more than 99.9 percent, and the granularity is less than or equal to 300 mu m; weighing each metal powder;
2) putting the weighed metal powder into a stainless steel vacuum grinding tank, vacuumizing, filling inert gas, and carrying out mechanical alloying in a high-energy ball mill, wherein the dry grinding speed is 300-500 r/min, the dry grinding time is 40-50 h, the wet grinding time is 2-5 h, and the wet grinding speed is 100-300 r/min; dry grinding is carried out firstly, and then wet grinding is carried out; after wet grinding, opening a vacuum tank, carrying out vacuum drying for 24-36 h, and then carrying out ball milling for 1-2 h at a speed of 50-100 r/min to prepare high-entropy alloy powder;
3) preparing composite material powder: adding the aluminum alloy powder weighed in proportion into the high-entropy alloy powder obtained in the step 2), and mechanically mixing for 3-5 hours at the speed of 150-200 r/min to prepare composite material powder; in the composite material powder, the mass content of the high-entropy alloy is 10-40wt%, and the mass content of the aluminum alloy powder is 60-90 wt%;
4) hot extrusion forming: and (3) carrying out cold pressing on the composite material to obtain an ingot blank, and then carrying out hot extrusion at the extrusion temperature of 400-600 ℃ and the extrusion ratio of 10-15 to finally obtain the high-entropy alloy reinforced aluminum-based composite material.
The purity of the Al, Fe, Cr, Co, Ni, Cu and Ti metal powder is more than 99.9 percent, and the granularity is less than or equal to 45 mu m; the granularity of the aluminum alloy powder is less than or equal to 200 mu m.
Further, the preparation method comprises the following specific steps:
a) putting each metal powder to be ball-milled into a stainless steel milling tank, taking a stainless steel ball as a milling body, and carrying out ball milling according to the ball powder mass ratio of not less than 10: 1; before ball milling, firstly, vacuumizing for 10min by using a vacuum machine, and then filling argon gas with the pressure of 0.5MPa as protective gas; the rotating speed of the ball mill is 350r/min, and the rotating direction needs to be adjusted once every 60 min;
b) adding absolute ethyl alcohol into the powder which is subjected to dry grinding for 45 hours, and carrying out wet grinding for 5 hours; after the ball milling is finished, taking out the ball milling tank, opening the vacuum drying oven, then opening the cover of the ball milling tank, leaving a certain gap, putting the ball milling tank into the drying oven, and closing the oven door; vacuumizing by using a vacuum machine, adjusting the temperature to 50 ℃, drying for 24 hours, and taking out; putting the dried powder into a ball mill, ball-milling for 2h at the rotating speed of 120r/min, screening the prepared high-entropy alloy composite powder, and taking out for later use;
c) densification of the composite material: placing 20wt% of the high-entropy alloy composite powder obtained in the step 2) and 80wt% of 6061 aluminum alloy powder into a ball milling tank for mechanical powder mixing; carrying out extrusion forming on the composite material powder; and (3) carrying out cold pressing to obtain an ingot blank with the diameter of 13.5mm and the height of 23mm, and then carrying out hot extrusion at the extrusion temperature of 450 ℃ at the extrusion ratio of 11.4 to finally obtain the aluminum-based composite material with the diameter of 4mm and the length of 135 mm.
And testing the high-entropy alloy composite material by adopting an XRD (X-ray diffraction), a TEM (transverse electric-magnetic field), a mechanical property testing machine and the like.
According to the high-entropy alloy reinforced aluminum-based composite material, the high-entropy alloy body with the alloy reinforcement body mainly comprising the body-centered cubic solid solution (BCC) with high strength and high hardness is subjected to high-energy ball milling to obtain the high-entropy alloy, and the high-entropy alloy is subjected to segregation on the aluminum alloy grain boundary to generate metal phase reinforcement; in the heating and pressurizing densification processes, the high-entropy alloy phase and the aluminum alloy phase form an interface bonding mechanism with certain diffusion while keeping respective crystal structures, so that the high-entropy alloy reinforced aluminum alloy composite material is strongly plastic bonded, and the high-entropy alloy reinforced aluminum matrix composite material with high strength and high toughness is prepared.
Drawings
FIG. 1 is a schematic view of a high-entropy alloy-reinforced aluminum-based composite material of example 1 obtained by hot extrusion;
FIG. 2 is an XRD analysis of the composite material prepared in example 1;
FIG. 3 is a stress-strain plot of the composite of example 1;
FIG. 4 is a schematic view of a high entropy alloy reinforced aluminum matrix composite of example 2;
fig. 5 is an XRD analysis pattern of the composite material prepared in example 2.
Detailed Description
The invention is further illustrated by the following examples and figures.
Selection of raw materials: al, Fe, Cr, Co, Ni and Cu metal powder with the purity of 99.99 percent is weighed according to the following table 1, and the granularity is less than or equal to 45 mu m. Table 1 shows the mass of the selected metal components in g for the composite material.
TABLE 1 quality of selected metal components for preparing composite materials
Example 1
(1) Preparing composite powder: the prepared FeNiCoCrCuAl is prepared according to the above table2.8The powder (subscript is mol ratio) is mechanically alloyed in a high-energy ball mill, the dry milling rotating speed is 350r/min, the wet milling time is 5h after the dry milling is 40h, and the wet milling is rotatedThe speed is 300r/min, and the body-centered cubic structure high-entropy alloy FeNiCoCrCuAl is prepared2.8And (3) powder. The method comprises the following specific steps:
a) putting the powder to be ball-milled into a stainless steel milling tank, and ball-milling by taking a stainless steel ball as a milling body according to the ball powder mass ratio of not less than 10: 1. Before ball milling, firstly, vacuumizing for 10min by using a vacuum machine, and then filling argon gas with the pressure of 0.5MPa as protective gas; the rotation speed of the ball mill is 350r/min, and the rotation direction needs to be adjusted once every 60 min.
b) And adding absolute ethyl alcohol into the powder which is ball-milled for 45 hours to carry out wet milling for 5 hours. After the ball milling is finished, the ball milling tank is taken out, the vacuum drying oven is opened, the cover of the ball milling tank is opened, a certain gap is reserved, and the box door is closed after the ball milling tank is placed into the drying oven. Vacuumizing by a vacuum machine, adjusting the temperature to 50 ℃, drying for 24 hours, and taking out. And putting the dried powder into a ball mill, performing ball milling for 2h at the rotating speed of 120r/min, screening the prepared high-entropy alloy composite powder, and taking out the powder for later use.
(2) Densification of the composite material: placing the high-entropy alloy composite powder (20 wt%) and 6061 aluminum alloy powder (80 wt%) in a ball milling tank for mechanical powder mixing; and carrying out extrusion forming on the composite material powder. Firstly, cold pressing is carried out to obtain an ingot blank with the diameter of 13.5mm and the height of 23mm, then hot extrusion is carried out, the extrusion temperature is 450 ℃, the extrusion ratio is 11.4, and finally the aluminum-based composite material with the diameter of 4mm and the length of 135mm shown in figure 1 is obtained.
(3) And (5) characterizing the structure and the performance, and testing the sample by adopting an XRD (X-ray diffraction) and mechanical property testing machine and the like. XRD analysis showed that both the aluminum alloy and the high entropy alloy maintained their respective crystallographic structures (fig. 2). With reference to fig. 1, endogenous TiC particles are distributed at the grain boundary and extrude fcc solid solution grains in the alloy densification process, resulting in the occurrence of deformation twin crystals; the compressive yield strength, breaking strength and plastic strain of the composite material reach 350.6251 Mpa, 470.7533 Mpa and 16.0617% (fig. 3), respectively, and the average microhardness is 129.9Hv (hot extrusion 6061 aluminum alloy hardness 48.66 Hv) compared with 6061 aluminum alloy shown in table 2 below.
TABLE 2 tensile test data sheet
| Tensile strength (MPa) | Bent 4 degree of strength (MPa) | Elongation (%) | |
| Aluminium alloy | 189.6592 | 156.7139 | 16.6409 |
| Composite material | 470.7533 | 350 .6251 | 16.0617 |
Example 2
Preparing composite powder: the prepared TiFeNiCoCrCuAl is prepared according to the above table 12(subscript is molar ratio) to prepare high-entropy alloy powder, and the specific steps refer to example 1.
The alloy matrix of the composite material is 7075 aluminum alloy, and the preparation process of the composite material refers to example 1. The physical pattern and XRD analysis of the composite material are shown in FIGS. 4 and 5. XRD analysis showed that both the aluminum alloy and the high-entropy alloy maintained their respective crystallographic structures (fig. 5). The compressive yield strength, the breaking strength and the plastic strain of the composite material respectively reach 354.5251 MPa, 469.7032 MPa and 16.165 percent.
Example 3
Preparing composite powder: ti prepared as in Table 1 above1.5The FeNiCoCrCuAl (subscript is a molar ratio) is used for preparing the high-entropy alloy powder, and the specific steps refer to example 1.
The alloy matrix of the composite material is 7075 aluminum alloy, and the preparation process of the composite material refers to example 1.
The high-entropy alloy reinforced aluminum matrix composite material takes high-entropy alloy particles as a reinforcing phase. Firstly, designing a high-strength high-hardness high-entropy alloy system according to the design principle of the high-entropy alloy; proportioning alloys according to design components, and preparing high-entropy alloy powder with a body-centered cubic structure by adopting a mechanical alloying technology and vacuum ball milling; fully and mechanically mixing the prepared high-entropy alloy powder with the selected aluminum alloy powder; the high-strength high-toughness high-entropy alloy composite material is prepared by adopting a process of performing hot extrusion on a preformed blank.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the scope of the invention.
Claims (1)
1. The preparation method of the high-entropy alloy reinforced aluminum-based composite material is characterized in that the high-entropy alloy reinforced aluminum-based composite material takes 6061 aluminum alloy as a matrix, high-entropy alloy as a reinforcing phase and high-entropy alloy as high-entropy alloy powder with a body-centered cubic structure; the high-entropy alloy powder selects metal components with the following mass: 75.6 parts of Al, 56 parts of Fe, 52 parts of Cr, 59 parts of Co, 59 parts of Ni and 64 parts of Cu; the metal components generate body-centered cubic solid solution high-entropy alloy according to the atomic ratio;
the preparation method comprises the following steps:
1) selecting raw materials: the high-entropy alloy powder is made of Al, Fe, Cr, Co, Ni, Cu and Ti metal powder with the purity of 99.9 percent and the granularity of less than or equal to 45 mu m; the purity of 6061 aluminum alloy powder is more than 99.9 percent, and the granularity is less than or equal to 200 mu m; weighing each metal powder;
2) preparing high-entropy alloy powder: a) putting metal powder for the high-entropy alloy to be ball-milled into a stainless steel milling tank, and ball-milling according to a ball powder mass ratio of not less than 10:1 by taking a stainless steel ball as a milling body; before ball milling, firstly, vacuumizing for 10min by using a vacuum machine, and then filling argon gas with the pressure of 0.5MPa as protective gas; the rotating speed of the ball mill is 350r/min, and the rotating direction needs to be adjusted once every 60 min;
b) adding absolute ethyl alcohol into the powder which is subjected to dry grinding for 45 hours, and carrying out wet grinding for 5 hours; after the ball milling is finished, taking out the ball milling tank, opening the vacuum drying oven, then opening the cover of the ball milling tank, leaving a certain gap, putting the ball milling tank into the drying oven, and closing the oven door; vacuumizing by using a vacuum machine, adjusting the temperature to 50 ℃, drying for 24 hours, and taking out; putting the dried powder into a ball mill, ball-milling for 2h at the rotating speed of 120r/min, screening the prepared high-entropy alloy powder, and taking out for later use;
3) densification of the composite material: placing 20wt% of the high-entropy alloy powder obtained in the step 2) and 80wt% of 6061 aluminum alloy powder into a ball milling tank for mechanical powder mixing; carrying out extrusion forming on the composite material powder; and (3) performing cold pressing to obtain an ingot blank with the diameter of 13.5mm and the height of 23mm, and then performing hot extrusion at the extrusion temperature of 450 ℃ at the extrusion ratio of 11.4 to finally obtain the high-entropy alloy reinforced aluminum-based composite material with the diameter of 4mm and the length of 135 mm.
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