A fullerene ash reinforced 6013 aluminum-based composite material and its preparation method

Abstract

The present invention belongs to the field of materials and provides a fullerene ash reinforced 6013 aluminum-based composite material and a preparation method thereof, comprising: preparing a fullerene ash reinforced 6013 aluminum-based composite material by a stirring casting method, and the extruded profile having excellent mechanical properties after T6 treatment. Fullerene ash particles are an ideal reinforcing phase for metal-based composite materials and can play a good strengthening role on aluminum alloys. Fullerene ash particles have a significant inhibitory effect on the growth of α-Al grains and a significant hindering effect on the diffusion of alloying elements in the solid solution process. The mechanical performance indicators such as aging peak hardness, yield strength, and tensile strength of the fullerene ash reinforced 6013 composite material are all higher than those of the 6013 alloy. This is attributed to the strengthening and grain refinement effects of the fullerene ash.

Description

Technical Field

[0001] The invention belongs to the field of materials, and in particular relates to a fullerene ash reinforced 6013 aluminum-based composite material and a preparation method thereof. Background Art

[0002] The information disclosed in this background technology section is only intended to enhance understanding of the overall background of the invention and should not necessarily be regarded as an admission or any form of suggestion that the information constitutes the prior art already known to those skilled in the art.

[0003] Carbon nanoparticles, including graphene, fullerenes, carbon nanotubes, titanium carbide, and silicon carbide, are excellent reinforcements for aluminum alloys. The development of carbon nanoparticle-reinforced aluminum-based composites is a hot topic in both research and industry.

[0004] Patent CN114855021A discloses a method for preparing a fullerene ash-modified diamond particle-reinforced aluminum-based composite material. The method specifically includes: dispersing the fullerene ash; uniformly mixing the ultrasonically dispersed fullerene ash with aluminum powder and diamond particles; drying the mixed powder; and finally preparing the fullerene-modified diamond / aluminum composite material. However, this technology is primarily targeted at electronic packaging materials, developing diamond / fullerene synergistically reinforced aluminum-based composite materials. The preparation method utilizes a sintering process, a powder metallurgy method primarily intended to improve the material's thermal conductivity. This functional composite material cannot meet the technical requirements for manufacturing structural materials. Summary of the Invention

[0005] In order to solve the above problems, the present invention provides a fullerene ash reinforced 6013 aluminum-based composite material and a preparation method thereof.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions:

[0007] The first aspect of the present invention provides a method for preparing a fullerene ash reinforced 6013 aluminum-based composite material, comprising:

[0008] Dispersing fullerene ash in an ethanol solution, then adding water and performing ultrasonic treatment to obtain a fullerene ash suspension;

[0009] Pure aluminum powder is added to the fullerene ash suspension, mixed evenly, and dried to obtain a fullerene ash and aluminum powder mixed powder;

[0010] Cold pressing, sintering and extruding the mixed powder of fullerene ash and aluminum powder to obtain a fullerene ash aluminum composite material rod;

[0011] An alloy material is prepared according to a composition of Si 0.72-0.75 wt.%, Fe 0-0.01 wt.%, Cu 1.1-1.2 wt.%, Mn 0.2-0.3 wt.%, Mg 0.89-0.90 wt.%, Cr 0-0.01 wt.%, Zn 0-0.01 wt.%, Ti 0-0.01 wt.%, Fullerene 0.3-0.04 wt.%, and the balance Al; the alloy is smelted, the alloy is kept warm after melting, and then refined with argon gas, and the temperature is kept warm after refining, and then the temperature is cooled to 710-720° C., a fullerene ash aluminum composite material rod is added, the temperature is kept warm, and the alloy is cast into a mold to obtain a fullerene ash reinforced 6013 aluminum-based composite ingot;

[0012] Extruding the composite material ingot to obtain a fullerene ash reinforced 6013 composite material profile;

[0013] The profile is subjected to T6 treatment, the solution temperature is 565-580℃, kept warm for 2-3h, and water quenched to obtain the product.

[0014] This invention uses a stir casting method, primarily utilizing the strengthening effect of fullerene ash, to create a structural material with excellent mechanical properties. A stir casting method was used to prepare a fullerene ash-reinforced 6013 aluminum-based composite material. After extrusion, the T6 treatment yielded the following mechanical properties:

[0015] Table 1 Mechanical properties

[0016]

[0017] The second aspect of the present invention provides a fullerene ash reinforced 6013 aluminum-based composite material prepared by the above method.

[0018] The third aspect of the present invention provides the application of the above-mentioned fullerene ash reinforced 6013 aluminum-based composite material in the field of materials.

[0019] Beneficial effects of the present invention

[0020] (1) Fullerene ash particles are spherical particles of about 40 nm, which are ideal strengthening phases for metal matrix composites and can play a good strengthening role for aluminum alloys.

[0021] (2) Fullerene ash particles have a significant inhibitory effect on the growth of α-Al grains and a significant hindering effect on the diffusion of alloying elements in the solid solution process.

[0022] (3) The mechanical properties of fullerene ash reinforced 6013 composite materials, such as peak hardness, yield strength, and tensile strength, are higher than those of 6013 alloy, which is attributed to the strengthening and grain refinement effects of fullerene ash.

[0023] (4) The preparation method of the present invention is simple, practical, and easy to promote. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] The accompanying drawings, which constitute a part of the present invention, are used to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their description are used to explain the present invention and do not constitute improper limitations on the present invention.

[0025] Figure 1 It is a metal mold;

[0026] Figure 2 Comparison of fullerene ash before and after dispersion: (a) morphology before dispersion, (b) morphology after ultrasonic dispersion;

[0027] Figure 3 Morphologies of pure Al and fullerene ash / Al mixed powders: (a), (b) pure Al powder, (c), (d), (e) 10 wt.% fullerene ash / Al mixed powders;

[0028] Figure 4 Cold pressed blocks and extruded rods of 3wt.% fullerene-containing raw gray aluminum composites: (a) cold pressed blocks; (b) extruded rods; (c) microstructure of cold pressed blocks; (d, e) microstructures of extruded rods;

[0029] Figure 5 For extrusion testing and extrusion bars;

[0030] Figure 6 OM images of 6013 aluminum alloy and composite materials after solution treatment at 565℃ for different times: (a) 6013, 60 min; (b) MMC, 60 min; (c) 6013, 120 min; (d) MMC, 120 min; (e) 6013, 120 min; (f) MMC, 120 min;

[0031] Figure 7 For SEM and EDS result analysis;

[0032] Figure 8 The hardness values ​​after aging at 200℃ for different times;

[0033] Figure 9 The hardness values ​​are obtained after aging at 190℃ for different times. DETAILED DESCRIPTION

[0034] It should be noted that the following detailed descriptions are exemplary and intended to provide further explanation of the present invention. Unless otherwise specified, all technical and scientific terms used in the present invention have the same meanings as those commonly understood by those skilled in the art to which the present invention belongs.

[0035] The first aspect of the present invention provides a method for preparing a fullerene ash reinforced 6013 aluminum-based composite material, comprising:

[0036] Dispersing fullerene ash in an ethanol solution, then adding water and performing ultrasonic treatment to obtain a fullerene ash suspension;

[0037] Pure aluminum powder is added to the fullerene ash suspension, mixed evenly, and dried to obtain a fullerene ash and aluminum powder mixed powder;

[0038] Cold pressing, sintering and extruding the mixed powder of fullerene ash and aluminum powder to obtain a fullerene ash aluminum composite material rod;

[0039] An alloy material is prepared according to a composition of Si 0.72-0.75 wt.%, Fe 0-0.01 wt.%, Cu 1.1-1.2 wt.%, Mn 0.2-0.3 wt.%, Mg 0.89-0.90 wt.%, Cr 0-0.01 wt.%, Zn 0-0.01 wt.%, Ti 0-0.01 wt.%, Fullerene 0.3-0.04 wt.%, and the balance Al; the alloy is smelted, the alloy is kept warm after melting, and then refined with argon gas, and the temperature is kept warm after refining, and then the temperature is cooled to 710-720° C., a fullerene ash aluminum composite material rod is added, the temperature is kept warm, and the alloy is cast into a mold to obtain a fullerene ash reinforced 6013 aluminum-based composite ingot;

[0040] Extruding the composite material ingot to obtain a fullerene ash reinforced 6013 composite material profile;

[0041] The profile is subjected to T6 treatment, the solution temperature is 565-580℃, kept warm for 2-3h, and water quenched to obtain the product.

[0042] In some embodiments, the ultrasonic power is 1700-1800w, and the treatment time is 3-5min.

[0043] In some embodiments, the aluminum powder has a particle size of 7-10 μm.

[0044] In some embodiments, the cold pressing parameters are 20 to 22 tons of force and 3 to 5 minutes of pressure maintenance.

[0045] In some embodiments, the sintering parameters are 600-650° C. and 120-130 min.

[0046] In some embodiments, the extrusion die is preheated to a temperature of 300-320°C.

[0047] In some embodiments, the melting temperature is 740-750°C, the alloy is kept warm for 25-30 minutes after melting, and is refined using argon. After refining, the temperature is continued to be kept warm for 15-20 minutes, and the temperature is cooled to 710-720°C. 3-5 wt.% fullerene raw gray aluminum composite material rods are added, and the temperature is continued to be kept warm for 15-20 minutes before being cast into a mold.

[0048] In some embodiments, the specific parameters of extrusion are homogenization temperature of 550-560°C, holding temperature for 12-15 hours, air cooling, reheating to 500-510°C after cooling, holding temperature for 120-130 minutes before extrusion, and preheating temperature of the extrusion die at 450-460°C;

[0049] In some embodiments, the aging temperature is 190-200° C., and the holding time is 3.6-4 hours.

[0050] The present invention will be further described in detail below with reference to specific embodiments. It should be noted that the specific embodiments are intended to explain the present invention rather than to limit it.

[0051] Example 1 Experimental method

[0052] 3 g of fullerene ash was dispersed in 50 ml of ethanol solution, and then 450 ml of deionized water was added for ultrasonic treatment at an ultrasonic power of 1700 W for 5 min to obtain a fullerene ash suspension.

[0053] 97g of atomized pure aluminum powder was added to the fullerene ash suspension and mechanically stirred. The aluminum powder had a particle size of 7-10μm. After drying, a 3wt.% fullerene ash and aluminum powder mixture was obtained.

[0054] The mixed powder was cold pressed, sintered, and extruded. The cold pressing parameters were 20 tons of pressure for 5 minutes, the sintering parameters were 600°C for 120 minutes, and the extrusion die was preheated to 300°C. A 3 wt.% fullerene-containing aluminum composite rod was obtained.

[0055] 6013 aluminum alloy and composite materials were prepared according to the composition in Table 2. The melting temperature was 740°C. After melting, the alloy was kept warm for 30 minutes and refined using argon. After refining, the temperature was kept warm for another 15 minutes. The temperature was then lowered to 720°C. 3 wt.% fullerene ash aluminum composite rods were added. The temperature was kept warm for another 15 minutes and cast into a metal mold. The mold dimensions are as follows: Figure 1 As shown, a fullerene ash reinforced 6013 aluminum matrix composite ingot was obtained.

[0056] Table 2 Nominal composition of Fullerene / 6013 composites

[0057]

[0058] The composite ingot was extruded. Specific parameters included a homogenization temperature of 550°C, a 12-hour hold, and air cooling. After cooling, it was reheated to 500°C and held for 120 minutes before extrusion. The extrusion die was preheated to 450°C. This yielded a 0.3 wt.% fullerene-reinforced 6013 composite profile.

[0059] The profiles were subjected to T6 treatment, solution temperature 565℃, holding temperature for 2h, water quenching, aging temperature 190℃, holding temperature for 4h.

[0060] Experimental results of Example 2

[0061] Figure 2 The morphology of fullerene ash before and after dispersion is compared. Figure 2 It can be seen that ultrasound has a good dispersing effect on fullerene ash. Before dispersion, fullerene ash is irregular and fluffy particles ( Figure 2 a) The edges and interior contain numerous voids. The fullerene ash is composed of small, nanoscale particles, which are bonded together by van der Waals forces to form larger particles. After ultrasonic dispersion, the fullerene ash is nanoparticles. SEM results indicate the following: 1. The fullerene ash is a carbonaceous material with poor wettability with aluminum. Due to interfacial tension, the aluminum melt has difficulty penetrating the edges and internal voids, resulting in weak interfacial bonding. 2. The large particles are loose aggregates of smaller particles aggregated by van der Waals forces, resulting in poor bonding strength and inability to strengthen the aluminum alloy matrix. 3. The fullerene ash in the aluminum alloy matrix acts as a crack source, similar to an initial crack, significantly damaging the tensile strength of the aluminum alloy.

[0062] Figure 3 This is a mixture of fullerene ash and aluminum powder. The fullerene ash adheres to the surface of pure aluminum powder. The macroscopic distribution is relatively uniform, with some localized agglomeration.

[0063] Figure 4 These are cold-pressed blocks and extruded rods of 3wt.% fullerene ash aluminum composite materials. In the cold-pressed blocks, the material density is low, and the aluminum powder has a certain degree of deformation. In the extruded rods, the fullerene ash is relatively evenly distributed, and is in the form of spherical particles of about 40nm. There are agglomerations in some local locations, and the agglomerate size is less than 1μm. During the preparation of the composite material, agglomeration is difficult to avoid, but no large-scale agglomerations were found, and it will not cause much damage to the mechanical properties. During the extrusion process, no obvious deformation was found in the fullerene ash particles, and they still maintained a spherical morphology, indicating that the strengthening phase has a high hardness. The 40nm spherical phase will have a good strengthening effect on the aluminum alloy.

[0064] A 0.3wt.% fullerene ash reinforced 6013 aluminum matrix composite was prepared by stir casting and extrusion test was carried out. The composite showed good surface quality and high smoothness after extrusion.

[0065] Figure 6 The metallographic images of 6013 alloy and composite material after solution at 565℃ for different time periods. Figure 6 It can be seen that the fullerene ash has a significant inhibitory effect on the grain growth during the solid solution process, resulting in a smaller grain size in the composite material and a large amount of residual unsolvated strengthening phase in the composite material.

[0066] EDS analysis shows that the unsolution strengthened phase is Al-Cu phase ( Figure 7 Energy dispersive spectrometry (EDS) analysis of the α-Al phase is shown in Table 3. As can be seen from the experimental results, Mn and C were not detected in either alloy, with their contents exceeding the lower limit of EDS detection. Mg and Si content showed little difference between the two alloys. Cu had a higher solubility level in the 6013 alloy (1.68 wt.%) and a lower level in the composite (1.42 wt.%).

[0067] Table 3 EDS results of 6013 and composite materials after solution treatment at 565℃ for 60 min

[0068]

[0069] Hardness testing of the 6013 aluminum alloy and the composite material after solution treatment is performed, and the results are shown in Table 4. It can be seen that the hardness of both the 6013 aluminum alloy and the composite material decreases with increasing solution treatment time. The composite material's hardness remains slightly higher than that of the 6013 aluminum alloy. The hardness of the 6013 aluminum alloy decreases more significantly with increasing solution treatment time.

[0070] Table 4 Brinell hardness values ​​after solution

[0071]

[0072] Based on the above experimental results, the addition of fullerene ash hinders the solid solution of alloying elements into the α-Al matrix. The present inventors believe that this effect is particularly pronounced for Cu. Fullerene ash can hinder the growth of α-Al grains during the solid solution process. Due to the higher solid solubility of elements in 6013, its hardness is lower. The composite material's higher hardness than 6013 is attributed to the following three factors:

[0073] 1. Strengthening effect of undissolved Al-Cu binary phase;

[0074] 2. Strengthening effect of fullerene ash on the matrix;

[0075] 3. α-Al grain refinement effect.

[0076] 6013 aluminum alloy and composite materials were kept at 565℃ for 120min, then water quenched and aged. The aging temperatures were 200℃ and 190℃, and the aging times were 1h, 2h, 3h, and 4h, respectively. After aging, they were air-cooled and their hardness was tested. The results are shown in Tables 5, 6, and Figure 8 、 Figure 9 shown.

[0077] Table 5 Hardness values ​​after aging at 200℃ for different times

[0078]

[0079]

[0080] Table 6 Hardness values ​​after aging at 190℃ for different times

[0081]

[0082] The experimental results show that the solution treatment process has a significant impact on the subsequent aging process. The composite material reaches peak hardness sooner, and after reaching peak hardness, the hardness decreases with increasing aging time. The peak hardness of the 6013 aluminum alloy after aging is 130 HV, while the peak hardness of the composite material is 138 HV.

[0083] Ageing strengthening is the re-precipitation of dissolved elements to form a nanoparticle-reinforced matrix. Defects such as dislocations and vacancies are the nucleation sites of nano-precipitates. When there are more dislocations in the matrix, the aging process is easier to proceed. When fullerene ash reinforcement particles are present in the composite material, a large number of "geometrically required dislocations" will form around the particles during the water quenching process after solutionization due to the different thermal expansion coefficients between the reinforcement particles and the matrix. Therefore, the composite material reaches its peak hardness at a faster rate during the aging process. After the hardness reaches its peak, the merging and growth of the nano-precipitates will reduce the dispersion strengthening effect. Therefore, the hardness decreases with the extension of the aging time.

[0084] After 6013 and composite material T6 were treated, the solution process was 565℃ for 120min, water quenching, aging temperature was 190℃, and tensile tests were carried out. The results are shown in Table 7.

[0085] Table 7 Tensile properties of 6013 and composite materials after T6 treatment

[0086]

[0087] The tensile strength of the composite material is slightly higher than that of 6013 alloy, which is attributed to the strengthening effect of fullerene ash on the matrix and the refinement of α-Al grains.

[0088] The foregoing description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Those skilled in the art will readily appreciate that various modifications and variations of the present invention are possible. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention are intended to be within the scope of protection of the present invention.

Claims

1. A method for preparing a fullerene ash reinforced 6013 aluminum-based composite material, characterized in that: include: Dispersing fullerene ash in an ethanol solution, then adding water and performing ultrasonic treatment to obtain a fullerene ash suspension; Before dispersion, the fullerene ash was irregular and fluffy particles with many gaps at the edges and inside. The fullerene ash was composed of small nano-sized particles, which were bonded by van der Waals forces to form large particles. After ultrasonic dispersion, the fullerene ash was spherical particles of 40 nm. Pure aluminum powder is added to the fullerene ash suspension, mixed evenly, and dried to obtain a fullerene ash and aluminum powder mixed powder; Cold pressing, sintering and extruding the mixed powder of fullerene ash and aluminum powder to obtain a fullerene ash aluminum composite material rod; An alloy material is prepared according to a composition of Si 0.72-0.75wt.%, Fe 0-0.01wt.%, Cu 1.1-1.2wt.%, Mn 0.2-0.3wt.%, Mg 0.89-0.90wt.%, Cr 0-0.01wt.%, Zn 0-0.01wt.%, Ti 0-0.01wt.%, Fullerene 0.3-0.04wt.%, and the balance Al, the alloy is melted, the alloy is kept warm after melting, and then refined with argon gas, and the temperature is continued to be kept after refining, and then the temperature is cooled to 710-720°C, a fullerene ash aluminum composite material rod is added, the temperature is continued to be kept, and the alloy is cast into a mold to obtain a fullerene ash reinforced 6013 aluminum-based composite ingot; Extruding the composite material ingot to obtain a fullerene ash reinforced 6013 aluminum-based composite material profile; The profile is subjected to T6 treatment, with a solution temperature of 565~580℃, holding temperature for 2~3h, and water quenching. The aging temperature is 190~200℃, and holding temperature for 3.6~4h.

2. The method for preparing the fullerene ash reinforced 6013 aluminum-based composite material according to claim 1, wherein: The ultrasonic power is 1700-1800w, and the treatment time is 3-5min.

3. The method for preparing the fullerene ash reinforced 6013 aluminum-based composite material according to claim 1, wherein: The particle size of aluminum powder is 7-10μm.

4. The method for preparing the fullerene ash reinforced 6013 aluminum-based composite material according to claim 1, wherein: The cold pressing parameters are 20~22 tons of force and holding pressure for 3~5 minutes.

5. The method for preparing the fullerene ash reinforced 6013 aluminum-based composite material according to claim 1, wherein: The sintering parameters are 600~650℃ and holding time for 120~130min.

6. The method for preparing the fullerene ash reinforced 6013 aluminum-based composite material according to claim 1, wherein: The extrusion die preheating temperature is 300~320℃.

7. The method for preparing the fullerene ash reinforced 6013 aluminum-based composite material according to claim 1, wherein: The melting temperature is 740~750℃. After the alloy is melted, it is kept warm for 25~30 minutes and refined with argon. After refining, it is kept warm for 15~20 minutes, cooled to 710~720℃, 3~5wt.% fullerene ash aluminum composite material rod is added, and it is kept warm for 15~20 minutes before being cast into a mold.

8. The method for preparing the fullerene ash reinforced 6013 aluminum-based composite material according to claim 1, wherein: The specific parameters of extrusion are homogenization temperature of 550~560℃, holding temperature for 12~15h, air cooling, reheating to 500~510℃ after cooling, holding temperature for 120~130min before extrusion, and preheating temperature of extrusion die at 450~460℃.

9. A fullerene ash reinforced 6013 aluminum-based composite material prepared by the method according to any one of claims 1 to 8.

10. Use of the fullerene ash reinforced 6013 aluminum-based composite material according to claim 9 in the field of materials.

Images