CN114645180B - Double-phase reinforced aluminum alloy and preparation method thereof - Google Patents

Double-phase reinforced aluminum alloy and preparation method thereof Download PDF

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CN114645180B
CN114645180B CN202210153260.7A CN202210153260A CN114645180B CN 114645180 B CN114645180 B CN 114645180B CN 202210153260 A CN202210153260 A CN 202210153260A CN 114645180 B CN114645180 B CN 114645180B
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苏文学
王宏明
程成
李桂荣
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Abstract

The invention discloses a two-phase particle reinforced aluminum alloy and a preparation method thereof, belonging to the field of metal materials. The two-phase particles are respectively FeCoNiCrMn high-entropy alloy strengthening phase and Al 2 O 3 The ceramic strengthening phase particles and the matrix are pure aluminum. The preparation method comprises the steps of preparing high-entropy alloy powder by high-energy ball milling; fully mixing pure aluminum powder, high-entropy alloy powder and aluminum oxide particles, obtaining a green body through cold isostatic pressing, and heating the green body in a microwave smelting furnace to obtain a FeCoNiCrMn high-entropy alloy strengthening phase and Al 2 O 3 An aluminum alloy with ceramic strengthening phase dual-phase strengthening. The advantages of the invention are: the reinforced phase of the double-phase reinforcement reserves the reinforcement characteristics and advantages of a single reinforced phase, has obvious synergistic reinforcement effect, eliminates the cluster defect of a particle phase by virtue of a synergistic mixing effect, and refines crystal grains at the aluminum crystal boundary by virtue of dispersion distribution, thereby realizing the synchronous improvement of the properties such as the hardness, the strength and the plasticity of the composite material, and meeting the application in the fields of aerospace and transportation.

Description

Double-phase reinforced aluminum alloy and preparation method thereof
Technical Field
The invention belongs to the field of metal materials, and particularly relates to a two-phase particle reinforced aluminum alloy and a preparation method thereof.
Background
The multiphase composite reinforced aluminum alloy has excellent high-temperature mechanical property, good wear resistance, low thermal expansion coefficient, simple preparation process and low reinforcement cost, and thus becomes the research focus of high-end aluminum materials. The ceramic phase has excellent performances such as high temperature resistance, wear resistance, high strength and hardness, but the ceramic phase has high brittleness, so that the ceramic phase is poor in wettability with a matrix interface, low in interface bonding strength and the like when used as a reinforcement, the hardness and strength of the aluminum material are improved, and the plasticity and toughness of the material are inevitably reduced, so that the application range of the aluminum alloy in high-end fields is limited.
As an innovative alloy system, the high-entropy alloy is an alloy consisting of 5 or more than 5 elements and composed according to an equal molar ratio or an approximately equal molar ratio, and researches of numerous scholars find that the high-entropy alloy has more ideal properties compared with the traditional alloy, such as high toughness, high temperature resistance, good corrosion resistance, good wear resistance and the like, so that the high-entropy alloy is valued in the field of materials science. Researches find that the thermal expansion coefficients of the high-entropy alloy and the aluminum matrix are similar, and the natural interface bonding characteristic between metal and metal is realized, so that the interface wettability and the interface compatibility of the high-entropy alloy and the aluminum matrix are good. The high-entropy alloy is added to cooperate with the hard ceramic particles while the strength and the hardness of the material are not reduced, so that the interface combination between the reinforcement and the matrix can be obviously improved, and the performances of the material, such as plastic toughness, wear resistance, elastic modulus and the like, can be improved.
At present, a dual-phase or multi-phase hybrid reinforced aluminum alloy material is reported, but a high-entropy alloy and ceramic combination is not reported as a composite reinforced phase for preparing a dual-phase reinforced aluminum alloy, so that in order to continuously improve the performance of an aluminum alloy material and expand the high-end application range of the aluminum alloy, a new system and a new method aiming at aluminum alloy reinforcement and performance improvement are necessary to be developed, and a high-strength and high-toughness aluminum alloy with higher performance is prepared, so that the method has important significance in the fields of aerospace, transportation and the like.
Disclosure of Invention
The invention aims to provide an aluminum alloy reinforced by combining a high-entropy alloy reinforcing phase and a ceramic particle reinforcing phase and a preparation method thereof.
The invention is realized by the following technical scheme:
the double-phase reinforced aluminum alloy is characterized in that a reinforcing phase of the double-phase reinforced aluminum alloy is a FeCoNiCrMn high-entropy alloy reinforcing phase and Al 2 O 3 A ceramic strengthening phase, wherein the FeCoNiCrMn high-entropy alloy strengthening phase accounts for 15 percent of the total mass fraction of the dual-phase strengthened aluminum alloy, and Al 2 O 3 The ceramic strengthening phase accounts for 2-8% of the total mass fraction of the two-phase reinforced aluminum alloy, and the matrix of the two-phase reinforced aluminum alloy is aluminum.
Further, the FeCoNiCrMn high-entropy alloy strengthening phase is in a sheet shape in an aluminum matrix, and the Al is 2 O 3 The ceramic reinforcing phase is spherical.
Further, the aluminum alloy has a hardness of 109.3 to 128.5HV, a yield strength of 291.5 to 319.2MPa, and an elongation of 41.2 to 46.7%.
The preparation method of the double-phase reinforced aluminum alloy is characterized by comprising the following steps of:
(1) Preparing materials: weighing 15% and 2% -8% of FeCoNiCrMn high-entropy alloy strengthening phase powder and Al 2 O 3 Ceramic powders, and pure aluminum powders;
(2) Preparing two-phase reinforced aluminum alloy powder: after mixing the weighed powders, mechanically alloying the powders by adopting a planetary ball mill under the protection of argon gas, and drying the powders to prepare the two-phase reinforced aluminum alloy powder with the average grain diameter of 5 mu m;
(3) Preparing a green compact: placing the prepared two-phase reinforced aluminum alloy powder in a die, and carrying out static pressure forming, wherein the static pressure is 500MPa, and the static pressure time is 10s, so as to obtain a green body;
(5) Microwave sintering: and (3) placing the green body in a microwave heating furnace, sintering under the protection of argon, keeping the sintering temperature at 460-500 ℃ for 1-3 h, and then cooling to below 200 ℃ along with the furnace to complete sintering to obtain the biphase reinforced aluminum alloy.
Further, the FeCoNiCrMn high-entropy alloy strengthening phase is prepared from iron, cobalt, nickel, chromium and manganese powders with the purity of more than 99.9% according to an equal molar ratio, and is prepared into the high-entropy alloy powder with the particle size range of 5-15 mu m and irregular sheet shape by adopting a planetary ball mill mechanical alloying method under the protection of argon.
Further, the mechanical alloying parameters of the FeCoNiCrMn high-entropy alloy powder are as follows: pre-ball milling for 4 to 6 hours at the rotating speed of 120r/min; setting the ball milling time to be 72 to 96h, and setting the rotating speed to be 280 to 360r/min; the ball-milling jar and the ball of grinding are the steel, and the ball material ratio is 5.
Further, said Al 2 O 3 The ceramic reinforcing phase is 1 to 3 mu m in size and is a regular spherical particle.
Further, the mechanical alloying parameters of the dual-phase reinforced aluminum alloy powder in the step (2) are as follows: setting the ball milling time to be 6-10 h, setting the rotating speed to be 120-160r/min, wherein the ball milling tank and the grinding balls are made of steel, and the ball-to-material ratio is 5.
Further, the drying process of the double-phase reinforced aluminum alloy powder in the step (2) is completed in a vacuum drying oven, and the drying temperature is 70-75 ℃.
Further, the heating rate of the microwave oven in the step (5) for sintering is 40 to 55 ℃/min.
The main advantages of the invention are: the high-entropy alloy with metal characteristics and the alumina ceramic with typical ceramic characteristics are combined to be used as the composite strengthening phase of the aluminum alloy, the two strengthening phases can keep the advantages of the two strengthening phases when the aluminum alloy is strengthened, the effects of synergistic strengthening and hybrid strengthening are achieved, and the performance of the material is greatly improved.
The action mechanism of the high-entropy alloy and ceramic composite reinforced aluminum alloy is as follows:
(1) Adding high entropy alloy can balance Al 2 O 3 The deformation nonuniformity between the ceramic particles and the Al matrix provides a good bonding interface, and when the material is acted by external force, the load can be effectively transferred to the particles, so that the stress concentration on the matrix is released, the possibility of Al matrix fracture is reduced, and the mechanical property of the composite material is improved.
(2) Due to Al 2 O 3 The ceramic particles have excellent performance, the tensile strength, the compressive strength and the bending strength of the material are improved by adding the ceramic particles, and the alumina ceramic particles are hard in texture and also serve as grinding agents to a certain extent in the ball milling process, so that the ceramic particles have positive effects on grain refinement and particle dispersion distribution.
(3) The reinforcing phase and the aluminum matrix have good wettability, smooth and clean interface, no obvious reaction layer and high interface bonding strength.
(4) The FeCoNiCrMn high-entropy alloy phase and the alumina ceramic phase reinforce the aluminum alloy, and various strengthening mechanisms exist, including fine grain strengthening, particle strengthening, dislocation strengthening, interface strengthening and the like. FeCoNiCrMn and Al 2 O 3 The elastic modulus of the composite material is higher, so that the composite material has higher elastic modulus, and the plasticity and toughness potential of the particle reinforced aluminum-based composite material are fully exerted.
(5) The preparation method can prepare FeCoNiCrMn high-entropy alloy and Al with uniform particle dispersion and fine microstructure 2 O 3 The ceramic reinforced aluminum alloy has good hardness, strength and wear resistance, and can meet the application in the fields of aerospace and transportation.
Meanwhile, the microwave sintering heating technology adopted by the invention has the characteristics of rapid heating, uniform heating and the like. The sintering temperature is combined with the thermal expansion characteristics of the high-entropy alloy, the aluminum oxide and the aluminum matrix, the dual-phase reinforced aluminum alloy obtained under the adopted sintering temperature condition has higher density, and under the temperature range, the phenomena of element diffusion, grain growth, grain interface stripping and the like during sintering are avoided to a great extent, and the positive influence is exerted on the performance of the composite material.
Drawings
FIG. 1 is FeCoNiCrMn + Al obtained in example 1 2 O 3 XRD pattern of the two-phase reinforced aluminum alloy.
FIG. 2 is FeCoNiCrMn + Al obtained in example 1 2 O 3 SEM image of the two-phase reinforced aluminum alloy.
FIG. 3 is FeCoNiCrMn + Al obtained in example 2 2 O 3 SEM image of the two-phase reinforced aluminum alloy.
FIG. 4 is FeCoNiCrMn + Al obtained in example 3 2 O 3 SEM image of the two-phase reinforced aluminum alloy.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention is further described in detail below with reference to the accompanying drawings. It will be understood that these examples are intended to illustrate the invention, and are not intended to limit the scope of the invention in any way; in the following examples, various procedures and methods not described in detail are conventional methods well known in the art.
Example 1:
preparation ofFeCoNiCrMn high-entropy alloy and Al 2 O 3 The ceramic phase composite reinforced aluminum alloy comprises 15 percent of FeCoNiCrMn high-entropy alloy reinforcing phase and Al, wherein the addition amount of the FeCoNiCrMn high-entropy alloy reinforcing phase accounts for the total mass fraction of the dual-phase reinforced aluminum alloy 2 O 3 The ceramic strengthening phase accounts for 2 percent of the total mass fraction of the two-phase reinforced aluminum alloy, and the matrix of the two-phase reinforced aluminum alloy is aluminum.
The preparation process of the two-phase reinforced aluminum alloy comprises the following steps:
step 1: mixing iron, cobalt, nickel, chromium and manganese powders with the purity of more than 99.9 percent according to an equal molar ratio, and then filling the mixture into a stainless steel ball milling tank, wherein the weight ratio of the ball powders is 5:1, adding stainless steel balls, wherein the stainless steel balls are divided into three sizes of 15mm, 10mm and 5mm according to a mass ratio of 1:3:5 weigh the large and medium size pellets. Adding anhydrous ethanol into the ball milling tank in an amount of 60 wt% of the mixed powder to ensure the uniformity of the powder in the ball milling tank, vacuumizing the ball milling tank, and performing ball milling for 5 hours in advance by using a planetary ball mill under the protection of argon at a rotating speed of 120r/min; setting the ball milling time to be 96h and the rotating speed to be 360r/min; the ball milling tank and the milling balls are made of steel, the ball-to-material ratio is 5.
Step 2: weighing the FeCoNiCrMn high-entropy alloy powder obtained in the step 1 and alumina according to the mass percentages of 15wt.% and 2wt.%, and the balance being pure aluminum. The alumina is regular spherical particles with the particle diameter of 1-3 mu m.
And step 3: preparing composite powder by high-energy ball milling: mixing the weighed two types of reinforcement powder with matrix aluminum powder, and then filling the mixture into a stainless steel ball milling tank, wherein the weight ratio of the ball powder is 5:1, adding stainless steel balls, wherein the stainless steel balls are divided into three sizes of 15mm, 10mm and 5mm according to a mass ratio of 1:2:4. the amount of absolute ethyl alcohol added into the ball-milling tank is 60wt.% of the mixed powder so as to ensure the uniformity of the powder in the ball-milling tank, then the ball-milling tank is vacuumized, a planetary ball mill is adopted under the protection of argon, the ball-milling time is set to 10 hours, the rotating speed is 160r/min, the ball-milling tank and the grinding balls are made of steel, the ball-to-material ratio is 5 2 O 3 ) The average particle size of the p/Al composite powder was 5 μm. Then a vacuum drying oven is adopted for carrying outDrying, and setting the temperature of a drying oven at 73 ℃.
And 4, step 4: preparing a green compact: drying the composite powder obtained in the step (3), placing the dried composite powder into a mold, and carrying out static pressure forming, wherein the static pressure is 450MPa, and the static pressure time is 10s, so as to obtain a green body;
and 5: microwave sintering: and (4) placing the green body obtained in the step (4) into a microwave smelting furnace, heating to 490 ℃ at the heating rate of 45 ℃/min, preserving the heat for 2 hours, carrying out the heating process under the protection of argon, and slowly cooling to below 200 ℃ to obtain the two-phase reinforced aluminum alloy.
And (3) detection results: feCoNiCrMn + Al prepared in example 1 2 O 3 The XRD and SEM of the two-phase reinforced aluminum alloy are shown in figures 1 and 2, and the figures show that particles of the obtained material are dispersedly distributed at the grain boundary of an aluminum matrix, the interface is smooth and clean, no obvious reaction layer exists, the pores and defects are low, and the results of standard performance tests show that the hardness of the two-phase reinforced aluminum alloy reaches 109.3HV, the yield strength is 291.5MPa, the elongation is 41.2%, the performance of the material is greatly improved, and the material has obvious technical effects.
In the embodiment 2 and the embodiment 3, the FeCoNiCrMn high-entropy alloy is kept accounting for 15 percent of the total mass fraction of the dual-phase reinforced aluminum alloy, and Al is added 2 O 3 Mass fraction of ceramic strengthening phase, and the same process and parameters as in example 1 were used to prepare FeCoNiCrMn + Al 2 O 3 A composite material. FeCoNiCrMn + Al obtained in examples 1 to 3 2 O 3 The performance index of the composite material is shown in table 1.
TABLE 1
Examples Al 2 O 3 Content of (A)wt.%) Hardness (HV) Yield strength (MPa) Elongation (%)
Example 1 2 109.3 291.5 41.2
Example 2 5 120.0 311.6 45.0
Example 3 8 128.5 319.2 46.7
From the test data shown in Table 1, it is shown that FeCoNiCrMn + Al prepared according to the present invention 2 O 3 The hardness, yield strength and elongation of the composite material are all improved along with the increase of the alumina ceramic reinforcing phase.
The examples are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any obvious modifications, substitutions or variations can be made by those skilled in the art without departing from the spirit of the present invention.

Claims (8)

1. A dual-phase reinforced aluminum alloy is characterized in that the dual-phase reinforced aluminum alloy is reinforcedThe phases are FeCoNiCrMn high-entropy alloy strengthening phase and Al 2 O 3 A ceramic strengthening phase, wherein the FeCoNiCrMn high-entropy alloy strengthening phase accounts for 15 percent of the total mass fraction of the dual-phase strengthened aluminum alloy, and Al 2 O 3 The ceramic strengthening phase accounts for 2-8% of the total mass fraction of the dual-phase reinforced aluminum alloy, and the matrix of the dual-phase reinforced aluminum alloy is aluminum;
the FeCoNiCrMn high-entropy alloy strengthening phase is in a sheet shape in an aluminum matrix, and the Al is 2 O 3 The ceramic strengthening phase is spherical;
the hardness of the aluminum alloy reaches 109.3 to 128.5HV, the yield strength is 291.5 to 319.2MPa, and the elongation is 41.2 to 46.7%.
2. A method for producing a dual-phase reinforced aluminum alloy as recited in claim 1, comprising the steps of:
(1) Preparing materials: weighing FeCoNiCrMn high-entropy alloy strengthening phase powder and Al according to the mass percent of 15 percent and 2-8 percent 2 O 3 Ceramic powders, and pure aluminum powders;
(2) Preparing two-phase reinforced aluminum alloy powder: after mixing the weighed powders, mechanically alloying the powders by adopting a planetary ball mill under the protection of argon gas, and drying the powders to prepare the two-phase reinforced aluminum alloy powder with the average grain diameter of 5 mu m;
(3) Preparing a green compact: placing the prepared two-phase reinforced aluminum alloy powder in a mold, and carrying out static pressure forming, wherein the static pressure is 350 to 500MPa, and the static pressure time is 10s, so as to obtain a green body;
(5) Microwave sintering: and (3) placing the green body in a microwave heating furnace, sintering under the protection of argon, keeping the sintering temperature at 460-500 ℃ for 1-3 h, and then cooling to below 200 ℃ along with the furnace to complete sintering to obtain the biphase reinforced aluminum alloy.
3. The preparation method of the FeCoNiCrMn high-entropy alloy powder is characterized in that the FeCoNiCrMn high-entropy alloy strengthening phase is prepared from iron, cobalt, nickel, chromium and manganese powders with the purity of more than 99.9% according to an equimolar ratio, and the high-entropy alloy powder with the particle size range of 5-15 μm and irregular sheet shapes is prepared by a mechanical alloying method of a planetary ball mill under the protection of argon.
4. The preparation method according to claim 3, wherein the FeCoNiCrMn high entropy alloy powder mechanical alloying parameters are as follows: pre-ball milling for 4 to 6 hours at the rotating speed of 120r/min; setting the ball milling time to be 72 to 96h, and setting the rotating speed to be 280 to 360r/min; the ball-milling jar and the ball of grinding are the steel, and the ball material ratio is 5.
5. The method of claim 2, wherein: the Al is 2 O 3 The ceramic reinforcing phase has a size of 1-3 μm and is in the form of regular spherical particles.
6. The method of claim 2, wherein: the mechanical alloying parameters of the double-phase reinforced aluminum alloy powder in the step (2) are as follows: setting the ball milling time to be 6-10 h, setting the rotating speed to be 120-160r/min, wherein the ball milling tank and the grinding balls are made of steel, and the ball-to-material ratio is 5.
7. The method of claim 2, wherein: and (3) completing the drying process of the double-phase reinforced aluminum alloy powder in the step (2) in a vacuum drying box, wherein the drying temperature is 70-75 ℃.
8. The method of claim 2, wherein: and (5) the heating rate of the sintering in the microwave heating furnace is 40-55 ℃/min.
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