Multi-component synergistically reinforced aluminum-based composite material and preparation method thereof

Abstract

The invention discloses a multi-component synergistically reinforced aluminum-based composite material and a preparation method thereof, and belongs to the technical field of metal-based composite materials. According to the invention, aluminum powder, magnesium powder and zinc oxide powder are used as raw materials, and the multi-component reinforced phase and precipitated phase synergistically reinforced aluminum-based composite material is prepared through segmented ball milling, cold pressing, reactive sintering, hot extrusion and heat treatment processes. The preparation method of the multi-component synergistically reinforced aluminum-based composite material is advanced in process, and compounding and alloying of the matrix can be achieved at the same time. The prepared aluminum-based composite material has excellent mechanical properties, the tensile strength of the aluminum-based composite material can reach 760 MPa, the yield strength of the aluminum-based composite material can reach 653 MPa, and the ductility of the aluminum-based composite material can reach 3.5%.

Description

Technical Field

[0001] The present invention belongs to the technical field of metal matrix composite materials, and in particular relates to a multi-component synergistically reinforced aluminum matrix composite material and a preparation method thereof. Background Art

[0002] As an important lightweight material, aluminum-based composite materials have a series of excellent properties such as high specific strength, high specific modulus, and good electrical and thermal conductivity, and play an irreplaceable role in the fields of national defense, aerospace, and electronic power. With the rapid development of modern industrial level, higher requirements are put forward for the comprehensive mechanical properties of aluminum-based composite materials.

[0003] According to the different ways of introducing the reinforcing phase, aluminum-based composite materials can be divided into external addition method and in-situ self-generation method. Aluminum-based composite materials prepared by external addition method usually cause a series of problems such as insufficient reinforcing phase-matrix interface bonding strength, poor interface reaction, and easy agglomeration and difficult dispersion of reinforcing phase. Aluminum-based composite materials prepared by in-situ reaction can achieve good interface bonding and ensure its excellent mechanical properties. Furthermore, based on the strategy of compositeization and alloying, the preparation of multi-component synergistically strengthened aluminum-based composite materials can achieve further optimization and improvement of material properties. Among them, the Al-Mg-ZnO composite material system can achieve the synergistic improvement of the performance of aluminum-based composite materials by reinforcing phase and precipitate through in-situ reaction and heat treatment technology.

[0004] However, aluminum-based composites prepared by traditional casting methods have a series of unfavorable factors, such as the reaction temperature is too high, resulting in coarsening of the internal structure of the composite material, and the energy mismatch between the enhanced phase interfaces induces grain boundary segregation, which makes it very difficult to prepare high-performance aluminum-based composites. Summary of the invention

[0005] In view of the above technical problems, the present invention proposes a multi-component synergistically reinforced aluminum-based composite material and a preparation method thereof. The method can utilize the synergistic enhancement effect of the multi-component reinforcement phase and the precipitation phase to effectively improve the comprehensive mechanical properties of the aluminum-based composite material, while avoiding the problems of microstructure coarsening and grain boundary segregation caused by the traditional casting method.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] A method for preparing a multi-component synergistically reinforced aluminum-based composite material comprises the following steps:

[0008] Aluminum powder, magnesium powder and stearic acid are subjected to a first-stage ball milling treatment under an argon protective atmosphere to obtain an aluminum powder / magnesium powder composite powder; zinc oxide powder and stearic acid are then added to a ball milling jar for a second-stage ball milling treatment to prepare an aluminum powder / magnesium powder / zinc oxide powder composite powder;

[0009] The obtained aluminum powder / magnesium powder / zinc oxide powder composite powder is subjected to cold pressing, normal pressure high temperature sintering, hot extrusion, solid solution and aging treatment to obtain an aluminum-based composite material with multi-component synergistic strengthening.

[0010] Furthermore, the amounts of the raw materials in the aluminum powder / magnesium powder / zinc oxide powder composite powder are as follows: 1-7 wt. % of magnesium powder, 7 wt. % of zinc oxide, 1 wt. % of stearic acid, and the rest of aluminum powder, based on 100 wt. %.

[0011] Furthermore, the conditions of the first stage ball milling treatment are: ball milling speed 500 rpm, time 6-8 hours, cooling treatment after ball milling for 24 hours;

[0012] The conditions of the second stage ball milling treatment are: ball milling speed of 200 rpm, time of 2 h, and then running at 500 rpm for 6 h.

[0013] Furthermore, the cold pressing forming conditions are: a pressure of 600 MPa, a holding time of 5 min, and the formed cold pressed blank is a cylindrical block with a diameter of 20 mm.

[0014] Furthermore, the atmospheric high temperature sintering specifically refers to: passing argon into the quartz tube for 10 minutes, heating to 773K at a sintering heating rate of 10K / min, and then heating to 1023K at a sintering heating rate of 5K / min, keeping warm for 1-2 hours, continuously passing argon during the sintering process and cooling to room temperature.

[0015] Furthermore, the parameters of the hot extrusion are: temperature of 803K, holding time of 30min, pressure of 600MPa, extrusion ratio of 16:1, and finally a hot extruded rod with a diameter of 5mm is obtained.

[0016] Furthermore, the solid solution specifically refers to: solid solution at 753K for 4-6h and water quenching.

[0017] Furthermore, the conditions of the aging treatment are: aging temperature is 393K, and time is 20-50h.

[0018] The invention also discloses a multi-component synergistically reinforced aluminum-based composite material prepared by the preparation method.

[0019] Compared with the prior art, the present invention has the following advantages and technical effects:

[0020] The present invention uses aluminum powder, magnesium powder and zinc oxide powder as raw materials, and prepares a multi-component reinforcement phase (the multi-component reinforcement phase MgAl2O4 and MgO are formed by in-situ reaction of Al powder, Mg powder and ZnO powder) and a precipitation phase (precipitation phase MgZn2, Mg 32(AlZn) 49 Aluminum-based composite materials that are synergistically strengthened (formed through aging precipitation) (by preparing a composite material of a multi-component reinforcement phase and a precipitation phase to exert the effects of solid solution strengthening, second phase strengthening and load transfer strengthening, thereby improving the performance of the composite material). The preparation method of the multi-component synergistically strengthened aluminum-based composite material provided by the present invention has advanced technology and can simultaneously realize the compositeization and alloying of the matrix. The prepared aluminum-based composite material has excellent mechanical properties, and its tensile strength can reach 760MPa, its yield strength can reach 653MPa, and its elongation can reach 3.5%. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] The drawings constituting a part of the present application are used to provide a further understanding of the present application. The illustrative embodiments and descriptions of the present application are used to explain the present application and do not constitute an improper limitation on the present application. In the drawings:

[0022] Figure 1 The process flow chart of preparing the multi-component synergistically reinforced aluminum-based composite material of the present invention;

[0023] Figure 2 The SEM morphology of the composite powder after segmented ball milling in Example 1 of the present invention; (a) is the macroscopic morphology of the composite powder; (b) is the high-magnification morphology of the composite powder;

[0024] Figure 3 Characterization images of the multi-component synergistically strengthened aluminum-based composite material prepared in Example 1 of the present invention; (a) is the EBSD image of sample S1; (b) is the TEM image of sample S1; (c) is the HRTEM image of the MgZn2 phase in sample S1; (d) is the MgZn2 phase in sample S1 32 (AlZn) 49 HRTEM images of the phase;

[0025] Figure 4 Engineering stress-strain curves of peak aging aluminum-based composite materials with different magnesium contents prepared in Examples 1-2 and Comparative Examples 1-2 of the present invention. DETAILED DESCRIPTION

[0026] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as limiting the present invention, but should be understood as a more detailed description of certain aspects, features, and embodiments of the present invention.

[0027] It should be understood that the terms described in the present invention are only for describing special embodiments and are not intended to limit the present invention. In addition, for the numerical range in the present invention, it should be understood that each intermediate value between the upper and lower limits of the scope is also specifically disclosed. Each smaller range between the intermediate value in any stated value or stated range and any other stated value or intermediate value in the described range is also included in the present invention. The upper and lower limits of these smaller ranges can be independently included or excluded in the scope.

[0028] Unless otherwise indicated, all technical and scientific terms used herein have the same meanings as those generally understood by those skilled in the art. Although the present invention describes only preferred methods and materials, any methods and materials similar or equivalent to those described herein may also be used in the implementation or testing of the present invention. All documents mentioned in this specification are incorporated by reference to disclose and describe the methods and / or materials associated with the documents. In the event of a conflict with any incorporated document, the content of this specification shall prevail.

[0029] It will be apparent to those skilled in the art that various modifications and variations may be made to the specific embodiments of the present invention description without departing from the scope or spirit of the present invention. Other embodiments derived from the present invention description will be apparent to those skilled in the art. The present invention description and examples are exemplary only.

[0030] The words “include,” “including,” “have,” “contain,” etc. used in this document are open-ended terms, meaning including but not limited to.

[0031] The present invention is based on the Al-Mg-ZnO system, which can realize the composite and alloying of the matrix. The reaction sintering and heat treatment process can be used to prepare a multi-component reinforcement phase and a precipitate phase to synergistically strengthen the aluminum-based composite material, thereby achieving a significant improvement in mechanical properties. The specific technical solution is as follows:

[0032] A method for preparing a multi-component synergistically reinforced aluminum-based composite material comprises the following steps:

[0033] (1) performing a first-stage ball milling treatment on aluminum powder, magnesium powder and a portion of stearic acid under an argon protective atmosphere to obtain an aluminum powder / magnesium powder composite powder; then adding zinc oxide powder and the remaining portion of stearic acid into a ball milling jar to perform a second-stage ball milling treatment to prepare an aluminum powder / magnesium powder / zinc oxide powder composite powder;

[0034] (2) The obtained aluminum powder / magnesium powder / zinc oxide powder composite powder is subjected to cold pressing, normal pressure high temperature sintering, hot extrusion, solid solution and aging treatment to obtain an aluminum-based composite material with multi-component synergistic strengthening.

[0035] In step (1) of some preferred embodiments of the present invention, the amount of each raw material in the aluminum powder / magnesium powder / zinc oxide powder composite powder is calculated as 100wt.% as follows: magnesium powder 1-7wt.%, zinc oxide 7wt.%, stearic acid 1wt.%, and the rest is aluminum powder. The preferred amount is: magnesium powder 5-7wt.%, zinc oxide 7wt.%, stearic acid 1wt.%, and the rest is aluminum powder.

[0036] In some preferred embodiments of the present invention, in step (1), the conditions of the first stage ball milling treatment are: ball milling speed of 500 rpm, time of 6-8 hours, preferably 8 hours, and cooling treatment for 24 hours after the ball milling is completed; the conditions of the second stage ball milling treatment are: ball milling speed of 200 rpm, time of 2 hours, and then running at 500 rpm for 6 hours.

[0037] The present invention adopts a segmented ball milling process, and the raw material powder can not only form a smaller size and a well-combined lamellar structure, but also can realize pre-alloying of the raw material through the energy input of high-energy ball milling, reduce the activation energy of the reaction in the subsequent sintering process, and promote the reaction.

[0038] In step (2) of some preferred embodiments of the present invention, the cold pressing forming conditions are: pressure 600 MPa, holding time 5 min, and the formed cold pressed blank is a cylindrical block with a diameter of 20 mm.

[0039] In step (2) of some preferred embodiments of the present invention, the atmospheric high temperature sintering specifically refers to: passing argon into the quartz tube for 10 minutes, heating to 773K at a sintering heating rate of 10K / min, and then heating to 1023K at a sintering heating rate of 5K / min, keeping warm for 1-2 hours, preferably 1 hour, and continuously passing argon during the sintering process and cooling to room temperature.

[0040] In step (2) of some preferred embodiments of the present invention, the hot extrusion parameters are: temperature 803K, holding time 30min, pressure 600MPa, extrusion ratio 16:1, and finally a hot extruded rod with a diameter of 5mm is obtained.

[0041] In step (2) of some preferred embodiments of the present invention, the solution treatment specifically refers to: solution treatment at 753K for 4-6 hours and water quenching, preferably solution treatment for 4 hours.

[0042] In step (2) of some preferred embodiments of the present invention, the conditions of the aging treatment are: aging temperature is 393K, time is 20-50h, preferably 20-22h.

[0043] The above-mentioned preparation method can be used to prepare an aluminum-based composite material with multi-component synergistic reinforcement.

[0044] The "room temperature" in the present invention refers to 20-30°C unless otherwise specified.

[0045] The raw materials used in the present invention are all purchased from the market.

[0046] The technical solution of the present invention is further illustrated by the following embodiments.

[0047] Example 1

[0048] A method for preparing a multi-component synergistically reinforced aluminum-based composite material, the process flow is as follows Figure 1 As shown, the specific steps are as follows:

[0049] (1) 87 wt.% aluminum powder, 5 wt.% magnesium powder and 0.5 wt.% stearic acid were subjected to a first-stage ball milling treatment under an argon protective atmosphere, and then cooled for 24 hours to obtain an aluminum powder / magnesium powder composite powder; the first-stage ball milling parameters were: a ball milling speed of 500 rpm and a ball milling time of 8 hours; then 7 wt.% zinc oxide powder and 0.5 wt.% stearic acid were added to the ball milling jar and subjected to a second-stage ball milling treatment to prepare an aluminum powder / magnesium powder / zinc oxide powder composite powder; the second-stage ball milling parameters were: a ball milling speed of 200 rpm and a ball milling time of 2 hours, and then the ball milling was run at a speed of 500 rpm for 6 hours; the SEM morphology of the aluminum powder / magnesium powder / zinc oxide powder composite powder after ball milling is as follows Figure 2 As shown;

[0050] (2) The aluminum powder / magnesium powder / zinc oxide powder composite powder obtained in step (1) is cold pressed, the applied pressure is 600 MPa, the holding time is 5 min, and the cold pressed blank is a cylindrical block with a diameter of 20 mm; then the cold pressed block is subjected to normal pressure high temperature sintering and hot extrusion treatment; during normal pressure high temperature sintering, argon gas is introduced into the quartz tube for 10 min, and the sintering heating rate is 10 K / min to 773 K, and then the sintering heating rate is 5 K / min to 1023 K, and the temperature is kept for 1 h. During the sintering process, argon gas is continuously introduced and cooled to room temperature; the hot extrusion temperature is 803 K, the holding time is 30 min, the pressure is set to 600 MPa, the extrusion ratio is 16:1, and a hot extruded rod with a diameter of 5 mm is obtained;

[0051] (3) The hot extruded rod obtained in step (2) was solution treated at 753 K for 4 h and water quenched, and then aged at 393 K for 22 h (peak aging) to obtain a multi-component synergistically strengthened aluminum-based composite material (denoted as S1).

[0052] Figure 3 Characterization images of the multi-component synergistically strengthened aluminum-based composite material prepared in Example 1, (a) is the EBSD image of sample S1; (b) is the TEM image of sample S1; (c) is the HRTEM image of the MgZn2 phase in sample S1; (d) is the MgZn2 phase in sample S132 (AlZn) 49 HRTEM image of the phase. It can be seen that there are in-situ synthesized MgAl2O4, MgO reinforcement phase and heat-treated MgZn2, Mg 32 (AlZn) 49 of the precipitated phase.

[0053] Example 2

[0054] A method for preparing a multi-component synergistically reinforced aluminum-based composite material, the process flow is as follows Figure 1 As shown, the specific steps are as follows:

[0055] (1) 85 wt.% aluminum powder, 7 wt.% magnesium powder and 0.5 wt.% stearic acid were subjected to a first-stage ball milling treatment under an argon protective atmosphere to obtain an aluminum powder / magnesium powder composite powder; the first-stage ball milling parameters were: a ball milling speed of 500 rpm and a ball milling time of 8 h; then 7 wt.% zinc oxide powder and 0.5 wt.% stearic acid were added to the ball milling jar and subjected to a second-stage ball milling treatment to obtain an aluminum powder / magnesium powder / zinc oxide powder composite powder; the second-stage ball milling parameters were: a ball milling speed of 200 rpm and a ball milling time of 2 h, followed by running at a ball milling speed of 500 rpm for 6 h;

[0056] (2) Same as Example 1;

[0057] (3) The hot extruded rod obtained in step (2) is solution treated at 753 K for 4 h and water quenched, and then aged at 393 K for 20 h (peak aging) to obtain a multi-component synergistically strengthened aluminum-based composite material (denoted as S2).

[0058] Comparative Example 1

[0059] A method for preparing a multi-component synergistically reinforced aluminum-based composite material, the specific steps are as follows:

[0060] (1) 91wt.% aluminum powder, 1wt.% magnesium powder and 0.5wt.% stearic acid were subjected to a first-stage ball milling treatment under an argon protective atmosphere to obtain an aluminum powder / magnesium powder composite powder; the first-stage ball milling parameters were: a ball milling speed of 500rpm and a ball milling time of 8h; then 7wt.% zinc oxide powder and 0.5wt.% stearic acid were added to the ball milling jar and subjected to a second-stage ball milling treatment to obtain an aluminum powder / magnesium powder / zinc oxide powder composite powder; the second-stage ball milling parameters were: a ball milling speed of 200rpm and a ball milling time of 2h, followed by running at a ball milling speed of 500rpm for 6h;

[0061] (2) Same as Example 1;

[0062] (3) The hot extruded rod obtained in step (2) was solution treated at 753 K for 4 h and water quenched, and then aged at 393 K for 8 h (peak aging) to obtain a multi-component synergistically strengthened aluminum-based composite material (denoted as S3).

[0063] Comparative Example 2

[0064] A method for preparing a multi-component synergistically reinforced aluminum-based composite material, the specific steps are as follows:

[0065] (1) 89 wt.% aluminum powder, 3 wt.% magnesium powder and 0.5 wt.% stearic acid were subjected to a first-stage ball milling treatment under an argon protective atmosphere to obtain an aluminum powder / magnesium powder composite powder; the first-stage ball milling parameters were: a ball milling speed of 500 rpm and a ball milling time of 8 h; then 7 wt.% zinc oxide powder and 0.5 wt.% stearic acid were added to the ball milling jar and subjected to a second-stage ball milling treatment to obtain an aluminum powder / magnesium powder / zinc oxide powder composite powder; the second-stage ball milling parameters were: a ball milling speed of 200 rpm and a ball milling time of 2 h, followed by running at a ball milling speed of 500 rpm for 6 h;

[0066] (2) Same as Example 1;

[0067] (3) The hot extruded rod obtained in step (2) was solution treated at 753 K for 4 h and water quenched, and then aged at 393 K for 14 h (peak aging) to obtain a multi-component synergistically strengthened aluminum-based composite material (denoted as S4).

[0068] Performance Test:

[0069] The alloy materials prepared in Examples 1-2 and Comparative Examples 1-2 were processed by wire cutting into standard tensile specimens, and tensile properties were tested on a universal tensile testing machine, where the tensile rate was 0.5 mm / min. The test results are shown in Tables 1 and Figure 4 .

[0070] Table 1 Mechanical properties of peak-aging aluminum matrix composites with different magnesium contents

[0071]

[0072] From Table 1 and Figure 4 It can be seen that the aluminum-based composite materials prepared by the methods of Examples 1 and 2 of the present invention have excellent mechanical properties. The performance of the samples prepared by the present invention is jointly determined by the Mg content and the aging time. The different aging times for different samples are due to the different peak aging caused by the different magnesium contents. Therefore, the present invention focuses on controlling different magnesium contents to prepare different samples. At a lower Mg content, sufficient reinforcement phase and precipitation phase cannot be formed to exert a strengthening effect.

[0073] The above are only preferred specific implementations of the present application, but the protection scope of the present application is not limited thereto. Any changes or substitutions that can be easily thought of by a person skilled in the art within the technical scope disclosed in the present application should be included in the protection scope of the present application. Therefore, the protection scope of the present application should be based on the protection scope of the claims.

Claims

1. A method for preparing a multi-component synergistically reinforced aluminum-based composite material, characterized in that: The following steps are involved: Aluminum powder, magnesium powder and part of stearic acid are subjected to a first-stage ball milling treatment under an argon protective atmosphere to obtain an aluminum powder / magnesium powder composite powder; zinc oxide powder and the remaining part of stearic acid are then added to a ball milling jar for a second-stage ball milling treatment to prepare an aluminum powder / magnesium powder / zinc oxide powder composite powder; The obtained aluminum powder / magnesium powder / zinc oxide powder composite powder is subjected to cold pressing, normal pressure high temperature sintering, hot extrusion, solid solution and aging treatment to obtain an aluminum-based composite material with multi-component synergistic strengthening.

2. The method for preparing the multi-component synergistically reinforced aluminum-based composite material according to claim 1, characterized in that: The amounts of the raw materials in the aluminum powder / magnesium powder / zinc oxide powder composite powder are as follows: 1-7 wt. % of magnesium powder, 7 wt. % of zinc oxide, 1 wt. % of stearic acid, and the rest of aluminum powder, based on 100 wt. %.

3. The method for preparing the multi-component synergistically reinforced aluminum-based composite material according to claim 1, characterized in that: The first stage of ball milling treatment method is: ball milling at a rotation speed of 500 rpm for 6-8 hours, and cooling treatment for 24 hours after the ball milling is completed; The method of the second stage ball milling treatment is: ball milling at a rotation speed of 200 rpm for 2 hours, and then running at 500 rpm for 6 hours.

4. The method for preparing the multi-component synergistically reinforced aluminum-based composite material according to claim 1, characterized in that: The cold pressing forming conditions are: pressure 600 MPa, holding time 5 min, and the formed cold pressed blank is a cylindrical block with a diameter of 20 mm.

5. The method for preparing the multi-component synergistically reinforced aluminum-based composite material according to claim 1, characterized in that: The atmospheric high temperature sintering specifically refers to: introducing argon into the quartz tube for 10 minutes, heating to 773K at a sintering heating rate of 10K / min, then heating to 1023K at a sintering heating rate of 5K / min, keeping warm for 1-2 hours, and cooling to room temperature.

6. The method for preparing a multi-component synergistically reinforced aluminum-based composite material according to claim 1, characterized in that: The parameters of the hot extrusion are: temperature 803K, holding time 30min, pressure 600MPa, extrusion ratio 16:1, and finally a hot extruded rod with a diameter of 5mm is obtained.

7. The method for preparing a multi-component synergistically reinforced aluminum-based composite material according to claim 1, characterized in that: The solid solution conditions are: solid solution at 753K for 4-6 hours and water quenching.

8. The method for preparing a multi-component synergistically reinforced aluminum-based composite material according to claim 1, characterized in that: The aging treatment conditions are: aging temperature 393K, time 20-50h.

9. A multi-component synergistically reinforced aluminum-based composite material prepared by the preparation method according to any one of claims 1 to 8.

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