CN115216663A - Heterogeneous high-toughness graphene reinforced aluminum-based composite material and preparation method thereof - Google Patents

Heterogeneous high-toughness graphene reinforced aluminum-based composite material and preparation method thereof Download PDF

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CN115216663A
CN115216663A CN202210852216.5A CN202210852216A CN115216663A CN 115216663 A CN115216663 A CN 115216663A CN 202210852216 A CN202210852216 A CN 202210852216A CN 115216663 A CN115216663 A CN 115216663A
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aluminum
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graphene
composite material
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CN115216663B (en
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于欢
韩业金
王荣荣
周吉学
李航
马百常
张素卿
吴建华
唐守秋
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New Material Institute of Shandong Academy of Sciences
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium

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  • Powder Metallurgy (AREA)

Abstract

The invention relates to a heterogeneous graphene reinforced aluminum-based composite material and a preparation method thereof. According to the invention, through heterogeneous configuration, back stress strengthening is introduced, the processing and hardening capacity of the material is enhanced, the strength and plasticity of the material are improved, and cost reduction and efficiency improvement of the graphene reinforced aluminum-based composite material are realized.

Description

Heterogeneous high-toughness graphene reinforced aluminum-based composite material and preparation method thereof
Technical Field
The invention relates to the technical field of preparation of metal matrix composites, in particular to a heterogeneous graphene reinforced aluminum matrix composite and a preparation method thereof.
Background
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The material compounding breaks through the defect that the monomer material cannot obtain comprehensive performance, and becomes an important direction for the research and development of new materials. The graphene material is compounded with the structural functional material aluminum, so that the mechanical and physical properties of the material can be obviously optimized, and the graphene material is considered as an ideal reinforcement material. However, compared with metal aluminum and its alloy, graphene is expensive, which results in an increase in material cost, and therefore, the greatest difficulty in the application of graphene reinforced aluminum matrix composite is to reduce the material cost on the basis of ensuring the mechanical and physical properties of the material. The heterogeneous material has the characteristics of macroscopic uniformity and microscopic non-uniformity, a back stress strengthening mechanism is introduced, the processing and hardening capacity of the material is enhanced, and the strength and the plasticity of the material can be improved. Compared with homogeneous graphene reinforced aluminum matrix composite materials, the heterogeneous configuration is expected to improve the reinforcing efficiency of graphene and realize cost reduction and efficiency improvement of the materials.
The prior published literature reports that the improvement of the material strength and plasticity through the heterogeneous configuration design focuses on the regulation and control of the heterogeneous grain structure of the metal matrix, the heterogeneous component composition is generally powder bodies in different ball milling states or powder bodies in a ball milling state and a non-ball milling state, the component with a fine grain structure plays a strengthening role, and the following defects exist: (1) A large number of crystal boundaries exist in the fine-grained matrix, so that diffuse scattering in the conduction process is intensified, and the physical properties of electric conduction and heat conduction of the material are reduced; (2) The bonding strength of the reinforcing phase in the powder body component and the matrix is low, and the reinforcing effect of the reinforcing body is weakened; (3) The mechanical ball milling causes damage to graphene, the number of defects is increased, and the physical properties of the material are influenced; (4) The mechanical ball milling efficiency is low, and the requirement of industrial production is difficult to meet.
Disclosure of Invention
In order to solve the technical problems, the invention provides a heterogeneous high-strength and high-toughness graphene reinforced aluminum matrix composite and a preparation method thereof. Through heterogeneous configuration, back stress strengthening is introduced, the processing and hardening capacity of the material is enhanced, the strength and plasticity of the material are improved, and cost reduction and efficiency improvement of the graphene reinforced aluminum-based composite material are realized.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a heterogeneous high-toughness graphene reinforced aluminum-based composite material, which comprises the following steps:
(1) Mechanically stirring and mixing graphene and aluminum-based powder in an organic solvent to obtain a mixed solution;
(2) Performing solid-liquid separation on the mixed solution by utilizing spray drying to realize the drying of the mixed powder;
(3) Preparing the mixed powder into a graphene reinforced aluminum-based composite material by adopting a powder pressing and sintering method;
(4) Crushing the graphene reinforced aluminum-based composite material by mechanical crushing to obtain scrap A;
(5) Uniformly mixing the scraps A and the aluminum-based powder by using a powder mixer to obtain heterogeneous mixed powder B;
(6) Pressing the heterogeneous mixed powder B, and then pre-sintering;
(7) And extruding and forming the sintered blank to obtain the heterogeneous high-strength and high-toughness graphene reinforced aluminum-based composite material.
Further, in the step (1), the aluminum-based powder is aluminum or aluminum alloy powder, and the average particle size is 1 to 200 μm.
Further, in the step (1), the graphene has a sheet diameter of less than 100 μm and a thickness of less than 20nm.
The mass fraction of the graphene in the graphene reinforced aluminum matrix composite material is 0.1-5%.
Furthermore, in the step (3), the pressing pressure is higher than 100MPa, the sintering temperature is between 400 and 650 ℃, and the sintering time is 0.5 to 10 hours.
Further, in the step (4), the size of the crushed chips A is less than 5mm × 2mm × 1mm (length × width × thickness).
Further, in the step (5), the mass fraction of the crushed scrap A in the mixed powder B is 10-90%, and the aluminum-based powder is pure aluminum or aluminum alloy powder.
Further, in the step (6), the pressing pressure is higher than 100MPa, the sintering temperature is between 400 and 650 ℃, and the sintering time is 0.5 to 10 hours.
Further, in the step (7), the extrusion ratio is more than 4, the temperature of the extruded blank is 400-600 ℃, and the extrusion speed is 1-20 mm/s.
In a second aspect of the invention, the heterogeneous high-toughness graphene reinforced aluminum matrix composite material prepared by the preparation method is provided.
The method adopts a preformed blank and a mechanical crushing process to obtain few/no-defect graphene reinforced aluminum-based composite material scraps; the graphene reinforced aluminum-based composite material is added into aluminum and aluminum alloy powder, and the controllable configuration of the heterogeneous high-toughness graphene reinforced aluminum-based composite material can be realized by adjusting the graphene content, the size and the proportion of the reinforced component and the granularity of the aluminum powder, so that the differential customization of the mechanical property, the physical property and the material cost of the material is met; the graphene and the matrix are combined under the action of two thermal coupling in the pre-forming stage and the non-homogeneous powder forming stage, the interface combination state is improved, and the enhancement effect of the graphene on the aluminum matrix is improved.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, based on the difference of mechanical properties between the graphene reinforced aluminum-based component and the aluminum-based component without the addition of the graphene, a back stress strengthening mechanism is introduced, and compared with the traditional material which introduces back stress strengthening through non-uniform grain structures (mixing fine grains with coarse grains), the diffuse scattering effect caused by grain boundary increase is effectively weakened, and the physical properties of electric conduction and heat conduction of the material are improved.
(2) According to the invention, the graphene reinforcement and the aluminum matrix are combined under the action of twice thermal coupling, so that the interface bonding strength is improved, and the reinforcing effect of graphene on the aluminum matrix is improved.
(3) The aluminum-based composite material with uniformly distributed graphene is used as the intermediate alloy and added into the aluminum-based powder in the form of mechanical broken fragments, so that the method is suitable for industrial production, meets the requirements on diversification of mechanical properties, physical properties and material cost, and has the advantages of simple process flow and wide application prospect.
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The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
Fig. 1 is a raman spectrum of graphene in example 1 of the present invention.
Fig. 2 is a scanning electron microscope image of the aluminum matrix composite material with uniformly distributed graphene prepared in example 1 of the present invention.
FIG. 3 is a scanning electron microscope photograph of a pre-sintered compact in inventive example 2.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Example 1
The embodiment of the invention provides a preparation method of a heterogeneous high-toughness graphene reinforced aluminum matrix composite, which comprises the following steps:
(1) Mechanically stirring graphene and aluminum-based powder in an organic solvent.
The graphene sheet diameter is 20 micrometers, the thickness is 5nm, the mass fraction of the graphene in the graphene reinforced aluminum-based composite material is 0.5%, the aluminum-based powder is pure aluminum powder, and the average particle size is 1.5 micrometers.
(2) And carrying out solid-liquid separation on the mixed solution by utilizing spray drying to realize the drying of the mixed powder.
(3) And preparing the aluminum matrix composite material with uniformly distributed graphene by adopting powder pressing and sintering.
The pressing pressure is 200MPa, the sintering temperature is 600 ℃, and the sintering time is 6h.
(4) And (3) crushing the graphene reinforced aluminum-based composite material by turning to obtain scrap A.
The average size of the crumbs A after crushing was 5 mm. Times.0.5 mm. Times.0.2 mm (length. Times.width. Times.thickness).
(5) And uniformly mixing the A and the aluminum-based powder by using a powder mixer to obtain heterogeneous mixed powder B.
The mass fraction of the crushed scrap A in the mixed powder B is 75%, and the aluminum-based powder is pure aluminum powder.
(6) The powder B is pressed and subsequently presintered.
The pressing pressure is 200MPa, the sintering temperature is 500 ℃, and the sintering time is 1h.
(7) And (3) extruding and forming the sintered blank to obtain the heterogeneous high-strength and high-toughness graphene reinforced aluminum-based composite material, wherein the mechanical and electrical properties of the material are listed in Table 1.
The extrusion ratio is 10, the temperature of the extruded blank is 500 ℃, and the extrusion speed is 5mm/s.
The graphene powder obtained in step (1) of the first embodiment and the composite powder obtained in step (2) of the first embodiment were tested by using a raman spectrometer, and the results are shown in fig. 1. The intensity ratio of the D peak to the G peak of the initial graphene powder is 0.1019, and the intensity ratio of the D peak to the G peak of the composite material powder prepared by mechanical stirring is 0.0646, so that the defect of the graphene can be repaired by the mechanical stirring process.
The scanning electron microscope is used for the aluminum matrix composite material with uniformly distributed graphene in the step (3) of the first embodiment, and the result is shown in fig. 2 (a). As can be seen from fig. 2 (a): the graphene is uniformly dispersed and distributed in the aluminum matrix without agglomeration.
The scrap B from step (4) of the first example was observed by a scanning electron microscope, and the result is shown in FIG. 2 (B). As can be seen from fig. 2 (b): the crumb B was relatively uniform in size with an average size of 5mm by 0.5mm by 0.2mm (length by width by thickness).
Comparative example 1
This comparative example is substantially the same as example 1 except that graphene is not added. The method comprises the following specific steps:
(1) The aluminum-based powder is mechanically stirred in an organic solvent.
The aluminum-based powder is pure aluminum powder with the average particle size of 1.5 mu m.
(2) And carrying out solid-liquid separation on the mixed solution by utilizing spray drying to realize the drying of the mixed powder.
(3) The aluminum-based material is prepared by powder pressing and sintering.
The pressing pressure is 500MPa, the sintering temperature is 600 ℃, and the sintering time is 6h.
(4) The aluminum-based material is crushed by turning to obtain chips A.
The average size of the crumbs A after crushing was 5 mm. Times.0.5 mm. Times.0.2 mm (length. Times.width. Times.thickness).
(5) And (3) uniformly mixing the A with the aluminum-based powder by using a powder mixer to obtain heterogeneous mixed powder B.
The mass fraction of the crushed scrap A in the mixed powder B is 75%, and the aluminum-based powder is pure aluminum powder.
(6) The powder B is pressed and subsequently presintered.
The pressing pressure is 200MPa, the sintering temperature is 500 ℃, and the sintering time is 1h.
(7) The sintered blank was extruded to obtain an aluminum-based material having the mechanical and electrical properties shown in Table 1.
The extrusion ratio is 10, the extrusion blank temperature is 500 ℃, and the extrusion speed is 5mm/s.
Comparative example 2
The method comprises the following specific steps:
(1) The aluminium-based powder is compacted and subsequently presintered.
The aluminum-based powder is pure aluminum powder, the average particle size is 1.5 mu m, the pressing pressure is 200MPa, the sintering temperature is 500 ℃, and the sintering time is 1h.
(2) The sintered blank was extruded to obtain an aluminum-based material, the mechanical and electrical properties of which are shown in Table 1.
The extrusion ratio is 10, the extrusion blank temperature is 500 ℃, and the extrusion speed is 5mm/s.
Comparative example 3
(1) Mechanically stirring graphene and aluminum-based powder in an organic solvent.
The graphene sheet diameter is 20 micrometers, the thickness is 5nm, the mass fraction of the graphene in the graphene reinforced aluminum-based composite material is 0.5%, the aluminum-based powder is pure aluminum powder, and the average particle size is 1.5 micrometers.
(2) And carrying out solid-liquid separation on the mixed solution by utilizing spray drying to realize the drying of the mixed powder.
(3) And preparing the aluminum matrix composite material with uniformly distributed graphene by powder pressing and sintering.
The pressing pressure is 200MPa, the sintering temperature is 500 ℃, and the sintering time is 1h.
(4) And (3) extruding and forming the sintered blank to obtain the heterogeneous high-toughness graphene reinforced aluminum-based composite material, wherein the mechanical and electrical properties of the material are listed in the table 1.
The extrusion ratio is 10, the temperature of the extruded blank is 500 ℃, and the extrusion speed is 5mm/s.
Example 2
The preparation method of the heterogeneous high-toughness graphene reinforced aluminum-based composite material provided by the embodiment is basically the same as that of the embodiment 1, and the difference is that: the mass fraction of the graphene in the graphene reinforced aluminum matrix composite material is 1%.
The method comprises the following steps:
(1) Mechanically stirring graphene and aluminum-based powder in an organic solvent.
The graphene sheet diameter is 20 micrometers, the thickness is 5nm, the mass fraction of the graphene in the graphene reinforced aluminum-based composite material is 1%, the aluminum-based powder is pure aluminum powder, and the average particle size is 1.5 micrometers.
(2) And carrying out solid-liquid separation on the mixed solution by utilizing spray drying to realize the drying of the mixed powder.
(3) And preparing the aluminum matrix composite material with uniformly distributed graphene by powder pressing and sintering.
The pressing pressure is 200MPa, the sintering temperature is 600 ℃, and the sintering time is 6h.
(4) And (3) crushing the graphene reinforced aluminum-based composite material by turning to obtain scrap A.
The average size of the crumbs A after crushing was 5 mm. Times.0.5 mm. Times.0.2 mm (length. Times.width. Times.thickness).
(5) And (3) uniformly mixing the A with the aluminum-based powder by using a powder mixer to obtain heterogeneous mixed powder B.
The mass fraction of the crushed scrap A in the mixed powder B is 75%, and the aluminum-based powder is pure aluminum powder.
(6) The powder B is pressed and subsequently presintered.
The pressing pressure is 200MPa, the sintering temperature is 500 ℃, and the sintering time is 1h.
(7) And (3) extruding and forming the sintered blank to obtain the heterogeneous high-toughness graphene reinforced aluminum-based composite material, wherein the mechanical and electrical properties of the material are listed in table 1.
The extrusion ratio is 10, the temperature of the extruded blank is 500 ℃, and the extrusion speed is 5mm/s.
The observation of the pre-sintered compact of step (6) of the second example using a scanning electron microscope showed the result shown in FIG. 3. Through the pressing and sintering processes, the aluminum-based composite material with uniformly distributed graphene is well combined with a pure aluminum interface, and defects such as holes and cracks are not found.
Example 3
The preparation method of the heterogeneous high-toughness graphene reinforced aluminum-based composite material provided by the embodiment is basically the same as that of the embodiment 1, and the difference is that:
the mass fraction of the crushed scrap A in the mixed powder B is 25%.
The mechanical and electrical properties of the obtained heterogeneous high-toughness graphene reinforced aluminum matrix composite are listed in table 1.
Example 4
The preparation method of the heterogeneous high-toughness graphene reinforced aluminum-based composite material provided by the embodiment is basically the same as that of the embodiment 1, and the difference is that:
the mass fraction of the crushed scrap A in the mixed powder B is 50%.
The heterogeneous high-strength and toughness graphene reinforced aluminum-based composite material is obtained, and the mechanical and electrical properties of the material are listed in table 1 (wherein the weight percentage of the graphene is based on the total mass of the composite material).
TABLE 1 Room temperature mechanical and electrical Properties of the composites
Figure BDA0003755085810000091
According to the preparation method of the heterogeneous high-toughness graphene reinforced aluminum-based composite material, a back stress strengthening mechanism is utilized, on the premise that the mechanical property and the conductivity of the material are guaranteed, the addition amount of graphene in the composite material can be reduced to the maximum extent, the graphene strengthening effect and performance advantages are fully exerted, cost reduction and efficiency improvement of the graphene reinforced aluminum-based composite material are realized, and the potential of large-scale application is realized.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited thereto, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or equivalents thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. Although the present invention has been described with reference to the specific embodiments, it should be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.

Claims (10)

1. A preparation method of a heterogeneous high-toughness graphene reinforced aluminum matrix composite is characterized by comprising the following steps:
(1) Mechanically stirring and mixing graphene and aluminum-based powder in an organic solvent to obtain a mixed solution;
(2) Carrying out solid-liquid separation on the mixed solution by utilizing spray drying to realize the drying of the mixed powder;
(3) Preparing the mixed powder into a graphene reinforced aluminum-based composite material by adopting a powder pressing and sintering method;
(4) Crushing the graphene reinforced aluminum-based composite material by mechanical crushing to obtain scrap A;
(5) Uniformly mixing the scraps A and the aluminum-based powder by using a powder mixer to obtain heterogeneous mixed powder B;
(6) Pressing the heterogeneous mixed powder B, and then pre-sintering;
(7) And extruding and forming the sintered blank to obtain the heterogeneous high-strength and high-toughness graphene reinforced aluminum-based composite material.
2. The production method according to claim 1, wherein in the step (1), the aluminum-based powder is aluminum or aluminum alloy powder and has an average particle diameter of 1 to 200 μm.
3. The method according to claim 1, wherein in the step (1), the graphene has a sheet diameter of less than 100 μm and a thickness of less than 20nm.
4. The preparation method according to claim 1, wherein the mass fraction of the graphene in the graphene reinforced aluminum matrix composite is 0.1-5%.
5. The method according to claim 1, wherein in the step (3), the pressing pressure is higher than 100MPa, the sintering temperature is 400-650 ℃, and the sintering time is 0.5-10 h.
6. The method according to claim 1, wherein in the step (4), the crushed pieces A have a size of less than 5mm x 2mm x 1mm (length x width x thickness).
7. The method according to claim 1, wherein in the step (5), the mass fraction of the crushed chips A in the heterogeneous mixed powder B is 10 to 90%.
8. The method according to claim 1, wherein in the step (6), the pressing pressure is higher than 100MPa, the sintering temperature is 400-650 ℃, and the sintering time is 0.5-10 h.
9. The method according to claim 1, wherein in the step (7), the extrusion ratio is more than 4, the temperature of the extrusion billet is 400 to 600 ℃, and the extrusion speed is 1 to 20mm/s.
10. The heterogeneous high-strength and toughness graphene reinforced aluminum matrix composite material prepared by the preparation method according to any one of the preceding claims.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111515403A (en) * 2020-05-18 2020-08-11 山东省科学院新材料研究所 Method for preparing graphene reinforced aluminum matrix composite powder in short process
CN112387977A (en) * 2020-08-14 2021-02-23 南昌航空大学 Preparation method of graphene/aluminum composite material
AU2021105915A4 (en) * 2021-08-19 2021-10-21 Wuhan Research Institute Of Materials Protection Graphene reinforced aluminum matrix composite material with high conductivity and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111515403A (en) * 2020-05-18 2020-08-11 山东省科学院新材料研究所 Method for preparing graphene reinforced aluminum matrix composite powder in short process
CN112387977A (en) * 2020-08-14 2021-02-23 南昌航空大学 Preparation method of graphene/aluminum composite material
AU2021105915A4 (en) * 2021-08-19 2021-10-21 Wuhan Research Institute Of Materials Protection Graphene reinforced aluminum matrix composite material with high conductivity and preparation method thereof

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Inventor after: Zhou Jixue

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