CN114807712A - High-entropy alloy reinforced aluminum-based composite material and preparation method thereof - Google Patents
High-entropy alloy reinforced aluminum-based composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-entropy alloy reinforced aluminum matrix composite and a preparation method thereof; the invention adopts CoCrFeNiMn high-entropy alloy as a reinforcing phase and 7075 aluminum alloy as a matrix. The preparation method comprises the following steps: (1) ball milling and mixing the powder to obtain composite material powder; (2) preparing a composite material block by spark plasma sintering; (3) and carrying out hot extrusion on the composite material block to prepare the CoCrFeNiMn/7075Al composite material. According to the invention, CoCrFeNiMn high-entropy alloy particles are used as a reinforcing phase, the CoCrFeNiMn high-entropy alloy particles have good wettability with 7075 aluminum alloy, and the high-entropy alloy and an aluminum matrix have good interface combination through a preparation process combining spark plasma sintering and hot extrusion, so that the composite material with fine grains and excellent comprehensive mechanical properties is prepared.
Description
Technical Field
The invention relates to the field of aluminum-based composite materials, in particular to a high-entropy alloy reinforced aluminum-based composite material and a preparation method thereof.
Background
The particle reinforced aluminum matrix composite material has the advantages of high specific strength, high specific rigidity and the like, and is widely concerned in the industries of aerospace, transportation and the like. High strength, high wear resistant ceramic particles (e.g. SiC, Al) 2 O 3 TiC, etc.) are the most commonly used reinforcements in aluminum matrix composites, however, ceramic particles have poor interface bonding with the matrix due to poor wettability with the aluminum matrix, mismatched thermal expansion coefficient, poor interface reaction, etc., cracks usually rapidly propagate at the interface, and finally the plasticity of the ceramic particle reinforced aluminum matrix composite is poor.
To solve this problem, metal particles have been proposed as a reinforcement for aluminum matrix composites, which have better compatibility with the aluminum matrix and a better matching coefficient of thermal expansion. The commonly used metal particles are amorphous alloys and high-entropy alloys. The high-entropy alloy is a novel alloy system which has more than four main elements and the atomic ratios of the elements are nearly equal, and is different from the traditional alloy in that the high-entropy alloy generally forms a simple solid solution structure (such as an FCC structure, a BCC structure, a HCP structure and the like) instead of a complex intermetallic compound, so that the high-entropy alloy has higher strength, hardness and excellent thermal stability, wherein the single-phase FCC high-entropy alloy generally has better plasticity, and the BCC high-entropy alloy has higher strength. The CoCrFeNiMn high-entropy alloy is used as an FCC single-phase solid solution, has better plasticity, is combined with aluminum alloy to prepare a composite material, has more excellent strong plasticity matching, and particularly for high-strength 7-series aluminum alloy, the CoCrFeNiMn/7075Al composite material can realize the improvement of strength and simultaneously retain certain plasticity. Compared with amorphous alloy, the high-entropy alloy reinforced aluminum matrix composite has the advantages of wider processing temperature range and better strong plastic fit.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings of the prior art and provides a high-entropy alloy reinforced aluminum matrix composite and a preparation method thereof. The CoCrFeNiMn high-entropy alloy has the structure of FCC single-phase solid solution, has excellent plasticity compared with high-entropy alloys with BCC and HCP structures, and can realize good matching of strong plasticity. The CoCrFeNiMn high-entropy alloy reinforced aluminum-based composite material prepared by the method has high strength, good plasticity, excellent mechanical property and stable property.
The invention is realized by the following technical scheme:
a high-entropy alloy reinforced aluminum matrix composite material comprises:
the composite material takes CoCrFeNiMn high-entropy alloy as a reinforcing phase and 7075 aluminum alloy as a matrix;
the volume fraction of the CoCrFeNiMn high-entropy alloy is 3-10%;
the 7075 aluminum alloy is 90-97% in volume fraction.
The CoCrFeNiMn high-entropy alloy has the same atomic ratio of each element.
A preparation method of a high-entropy alloy reinforced aluminum matrix composite material comprises the following steps: the preparation method comprises the following preparation steps:
the method comprises the following steps: preparation of composite powder
Taking CoCrFeNiMn high-entropy alloy powder and 7075 aluminum matrix powder according to a preset volume fraction, and putting the CoCrFeNiMn high-entropy alloy powder and the 7075 aluminum matrix powder into a ball-milling tank filled with inert protective gas for sealing and mixing to obtain composite powder;
step two: sintered compact
Placing the composite powder prepared in the step one into a graphite die, and then carrying out spark plasma sintering so as to sinter and form the composite powder in the die and obtain a sintering blank coating sheath;
step three: hot extrusion molding
And (4) covering and sheathing the sintered blank prepared in the step two, placing the sintered blank in a resistance furnace, preserving heat at the hot extrusion temperature, carrying out hot extrusion, and carrying out air cooling to room temperature to obtain the high-entropy alloy reinforced 7075 aluminum-based composite material.
In the first step, the technological parameters of sealing and mixing in the ball milling tank are as follows: the ball material mass ratio is 8: 1-15: 1, the rotating speed is 100 r/min-300 r/min, and the ball milling mixing time is 10-40 h, so that the composite powder is obtained.
In the second step, the parameters of the spark plasma sintering process are as follows: the sintering pressure is 20-50 MPa, the sintering temperature is 475-550 ℃, the heat preservation time is 4-8 min, and the vacuum degree is less than 8 Pa.
In the third step, the sheath is prepared by turning the bar material in the 7075-T6 state.
In the third step, the blank heat preservation temperature is 300-450 ℃, the heat preservation time is 20-30 min, the temperature of the hot extrusion die is 280-430 ℃, the temperature of the extrusion nozzle is 270-420 ℃, and the extrusion nozzles with different inner diameters are utilized to obtain samples prepared by different extrusion ratios, wherein the extrusion ratio is 13-20.
In the third step, the extrusion angle of the hot extrusion nozzle is 120 ℃, the joint of the conical surface and the cylindrical surface is in smooth transition by an arc and is provided with a chamfer angle of 2-4 degrees.
Compared with the prior art, the invention has the following advantages and effects:
the CoCrFeNiMn high-entropy alloy reinforced aluminum-based composite material is prepared by adopting a discharge plasma sintering and hot extrusion combined mode, the composite material overcomes the problems of poor wettability, mismatched thermal expansion coefficient and the like in the conventional ceramic particle reinforced aluminum-based composite material, and meanwhile, the aluminum-based composite material with excellent comprehensive mechanical property and good interface combination is prepared by virtue of excellent strong plasticity of the CoCrFeNiMn high-entropy alloy.
Drawings
FIG. 1 is a metallographic structure morphology diagram of a CoCrFeNiMn/7075Al composite material prepared in example 1.
FIG. 2 shows the room temperature tensile fracture of the CoCrFeNiMn/7075Al composite prepared in example 1.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1:
firstly, the method comprises the following steps: according to the preset volume fraction, CoCrFeNiMn high-entropy alloy particles and 7075 aluminum matrix powder (the volume fraction of the high-entropy alloy is 5%) are placed into a ball-milling tank filled with inert protective gas to be hermetically mixed, the ball-material ratio is 10:1, and the mixture is mixed for 10 hours at the ball-milling speed of 250r/min to obtain composite powder.
II, secondly: and (3) placing the composite powder into a graphite mold, wherein graphite carbon paper is arranged between the graphite mold and the composite powder. And placing the graphite mold filled with the composite powder in a discharge plasma sintering furnace, vacuumizing until the vacuum degree in a hearth is less than 8Pa, setting sintering parameters, and sintering.
Thirdly, the method comprises the following steps: the specific sintering parameters are as follows: the sintering pressure is 30MPa, the sintering temperature is 500 ℃, and the heat preservation time is 8 min.
Fourthly, the method comprises the following steps: and (3) coating the blank obtained after spark plasma sintering with a sheath prepared from 7075 aluminum alloy, and performing hot extrusion molding.
Fifthly: the hot extrusion parameters were: putting the blank into a resistance furnace for heat preservation at the temperature of 400 ℃ for 20min, wherein the temperature of an extrusion die is 380 ℃, the temperature of an extrusion nozzle is 370 ℃, and the extrusion ratio is 16: 1;
sixthly, the method comprises the following steps: in the step (5) of the embodiment, the metallographic structure of the CoCrFeNiMn/7075Al composite material is as shown in FIG. 1, and the high-entropy alloy particles are well bonded with the interface of the aluminum matrix.
Seventhly, the method comprises the following steps: the yield strength, tensile strength and elongation of the CoCrFeNiMn/7075Al composite material in step (5) of this example were measured by using the method of GB/T228-: the yield strength is 403MPa, the tensile strength is 542MPa, and the elongation is 8%.
Eighthly: in the step (5) of this example, the tensile fracture of the CoCrFeNiMn/7075Al composite material is shown in fig. 2, which shows that there exists a high-entropy particle spalling phenomenon at the tensile fracture and a dimple with different depths at a part of the tensile fracture.
Example 2:
firstly, the method comprises the following steps: according to the preset volume fraction, placing CoCrFeNiMn high-entropy alloy particles and 7075 aluminum matrix powder (the volume fraction of the high-entropy alloy is 3%) into a ball-milling tank filled with inert protective gas, sealing and mixing, wherein the ball-material ratio is 8:1, and mixing is carried out for 20 hours at the ball-milling speed of 300r/min, so as to obtain the composite powder.
II, secondly: and (3) placing the composite powder into a graphite mold, wherein graphite carbon paper is arranged between the graphite mold and the composite powder. And placing the graphite mold filled with the composite powder in a discharge plasma sintering furnace, vacuumizing until the vacuum degree in a hearth is less than 8Pa, setting sintering parameters, and sintering.
Thirdly, the method comprises the following steps: the specific sintering parameters are as follows: the sintering pressure is 20MPa, the sintering temperature is 475 ℃, and the heat preservation time is 4 min.
Fourthly, the method comprises the following steps: and (3) coating the blank obtained after spark plasma sintering with a sheath prepared from 7075 aluminum alloy, and performing hot extrusion molding.
Fifthly: the hot extrusion parameters were: putting the blank into a resistance furnace for heat preservation at 300 ℃ for 20min, wherein the temperature of an extrusion die is 280 ℃, the temperature of an extrusion nozzle is 270 ℃, and the extrusion ratio is 13: 1;
sixthly, the method comprises the following steps: the yield strength, tensile strength and elongation of the CoCrFeNiMn/7075Al composite material in step (5) of this example were measured by using the method of GB/T228-: the yield strength is 316MPa, the tensile strength is 465MPa, and the elongation is 13.2 percent.
Example 3:
firstly, the method comprises the following steps: according to the preset volume fraction, placing CoCrFeNiMn high-entropy alloy particles and 7075 aluminum matrix powder (the volume fraction of the high-entropy alloy is 10%) into a ball-milling tank filled with inert protective gas, sealing and mixing, wherein the ball-material ratio is 15:1, and mixing is carried out for 40h at the ball-milling speed of 100r/min to obtain composite powder.
II, secondly: and (3) placing the composite powder into a graphite mold, wherein graphite carbon paper is arranged between the graphite mold and the composite powder. And placing the graphite mold filled with the composite powder in a discharge plasma sintering furnace, vacuumizing until the vacuum degree in a hearth is less than 8Pa, setting sintering parameters, and sintering.
Thirdly, the method comprises the following steps: the specific sintering parameters are as follows: the sintering pressure is 50MPa, the sintering temperature is 550 ℃, and the heat preservation time is 8 min.
Fourthly, the method comprises the following steps: and (3) coating the blank obtained after spark plasma sintering with a sheath prepared from 7075 aluminum alloy, and performing hot extrusion molding.
Fifthly: the hot extrusion parameters were: putting the blank into a resistance furnace for heat preservation at the temperature of 450 ℃ for 30min, wherein the temperature of an extrusion die is 430 ℃, the temperature of an extrusion nozzle is 420 ℃, and the extrusion ratio is 20: 1;
sixthly, the method comprises the following steps: the yield strength, tensile strength and elongation of the CoCrFeNiMn/7075Al composite material in step (5) of this example were measured by using the method of GB/T228-: the yield strength is 367MPa, the tensile strength is 498MPa, and the elongation is 7.8 percent.
In conclusion, the CoCrFeNiMn high-entropy alloy is used as a reinforcing phase, the aluminum matrix composite material is prepared by adopting the discharge plasma sintering and hot extrusion combined process, the problems of poor wettability, poor interface bonding and the like of the traditional ceramic particle reinforced aluminum matrix composite material are solved, good interface bonding is obtained, the yield strength is improved, a certain elongation is kept, and good strong-plasticity matching is obtained.
As described above, the present invention can be preferably realized.
The embodiments of the present invention are not limited to the above-described embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and they are included in the scope of the present invention.
Claims (8)
1. A high-entropy alloy reinforced aluminum matrix composite is characterized in that:
the composite material takes CoCrFeNiMn high-entropy alloy as a reinforcing phase and 7075 aluminum alloy as a matrix;
the volume fraction of the CoCrFeNiMn high-entropy alloy is 3-10%;
the 7075 aluminum alloy is 90-97% in volume fraction.
2. The high-entropy alloy-reinforced aluminum-based composite material according to claim 1, wherein:
the CoCrFeNiMn high-entropy alloy has the same atomic ratio of each element.
3. The preparation method of the high-entropy alloy reinforced aluminum-based composite material as claimed in any one of claims 1 to 2, which is characterized by comprising the following preparation steps:
the method comprises the following steps: preparation of composite powder
Taking CoCrFeNiMn high-entropy alloy powder and 7075 aluminum matrix powder according to a preset volume fraction, and putting the CoCrFeNiMn high-entropy alloy powder and the 7075 aluminum matrix powder into a ball-milling tank filled with inert protective gas for sealing and mixing to obtain composite powder;
step two: sintered compact
Filling the composite powder prepared in the step one into a graphite die, and then performing spark plasma sintering to sinter and form the composite powder in the die to obtain a sintering blank coating sheath;
step three: hot extrusion molding
And (4) covering and sheathing the sintered blank prepared in the step two, placing the sintered blank in a resistance furnace, preserving heat at the hot extrusion temperature, carrying out hot extrusion, and carrying out air cooling to room temperature to obtain the high-entropy alloy reinforced 7075 aluminum-based composite material.
4. The preparation method of the high-entropy alloy reinforced aluminum matrix composite material according to claim 3, wherein in the first step, the process parameters of sealing and mixing in the ball milling tank are as follows:
the ball material mass ratio is 8: 1-15: 1, the rotating speed is 100 r/min-300 r/min, and the ball milling mixing time is 10-40 h, so that the composite powder is obtained.
5. The preparation method of the high-entropy alloy-reinforced aluminum-based composite material according to claim 3, characterized in that: in the second step, the parameters of the spark plasma sintering process are as follows:
the sintering pressure is 20-50 MPa, the sintering temperature is 475-550 ℃, the heat preservation time is 4-8 min, and the vacuum degree is less than 8 Pa.
6. A method for preparing a high-entropy alloy-reinforced aluminum-based composite material according to any one of claims 3 to 5, characterized in that:
in the third step, the sheath is prepared by turning the bar material in the 7075-T6 state.
7. The preparation method of the high-entropy alloy-reinforced aluminum-based composite material according to claim 6, characterized in that:
in the third step, the blank heat preservation temperature is 300-450 ℃, the heat preservation time is 20-30 min, the temperature of the hot extrusion die is 280-430 ℃, the temperature of the extrusion nozzle is 270-420 ℃, and the extrusion nozzles with different inner diameters are utilized to obtain samples prepared by different extrusion ratios, wherein the extrusion ratio is 13-20.
8. The preparation method of the high-entropy alloy-reinforced aluminum-based composite material according to claim 7, characterized in that:
in the third step, the extrusion angle of the hot extrusion nozzle is 120 ℃, the joint of the conical surface and the cylindrical surface is in smooth transition by an arc and is provided with a chamfer angle of 2-4 degrees.
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