A two-dimensional nanomaterial reinforced copper-based composite material and its preparation method
By combining discharge plasma sintering and hot rolling technology, MXene reinforced copper-based composite materials were prepared, solving the problems of complex preparation process, low output rate and insufficient performance in the prior art, and achieving high-performance composite materials preparation.
Patent Information
- Application Number
- CN202410280456.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-03-12
- Publication Date
- 2025-06-17
- Estimated Expiration
- 2044-03-12
AI Technical Summary
In the prior art, when preparing MXene reinforced copper-based composites, there are problems such as complex preparation process, low output rate, poor thermal expansion performance, and insufficient performance of electrical and thermal conductivity.
A single layer of MXene nanosheets were prepared by combining discharge plasma sintering technology and hot rolling process by combining ultrasonic dispersion and high-speed homogenization, and nanoscale Ni powder and ureagen intercalation agent were added, and then mixed with copper powder for ball milling and ball milling and drying, and finally plasma sintering and hot rolling were carried out.
The MXene reinforced copper-based composite material with excellent mechanical properties, high temperature stability and good electrical and thermal conductivity was achieved, which improved the density and Vickers hardness of the composite material.
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Figure CN118166234B_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of two-dimensional nanomaterials, and particularly relates to a two-dimensional nanomaterial (MXene)-reinforced copper-based composite material and a preparation method thereof. Background Art
[0002] Preparing ceramic fibers / particles as reinforcing phase materials for copper-based composite materials is an effective way to improve the properties of copper and its alloys. In particulate-reinforced copper-based composite materials, the reinforcing phase particles mainly include oxides, carbides, nitrides, silicides, etc. However, the final properties of copper-based composite materials are greatly affected by the ceramic fiber / particle reinforcing phase (factors such as size, shape, coefficient of thermal expansion, density, etc.). In order to obtain composite materials with high specific strength and excellent electrical conductivity, selecting a suitable reinforcing phase is an urgent task in the current research on copper-based composite materials.
[0003] Currently, due to its unique single-atom layer structure, graphene has excellent mechanical properties (fracture strength up to 130 GPa, Young's modulus about 1100 GPa), thermal conductivity (thermal conductivity about 5000 W / m·K), and electrical conductivity (electron mobility reaches 200000 cm 2 / V·s), and has a large specific surface area of about 2630 m 2 g -1 , making it widely regarded as a metal matrix reinforcing phase. However, two-dimensional nanomaterials such as graphene have poor high-temperature stability and are extremely prone to oxidation at 450°C to 500°C, resulting in the destruction of the original 2D structure, making it difficult to fully exert its excellent properties, and it is prone to agglomeration due to van der Waals forces and a large specific surface area. Two-dimensional carbonitride MXene is named after its similar two-dimensional layered structure to graphene. It is a series of two-dimensional nanomaterials of two-dimensional transition metal carbides, nitrides, or carbonitrides, which are obtained by chemical etching and exfoliation of the MAX phase. The mechanical properties of MXene are similar to those of graphene nanosheets, with van der Waals forces connecting between layers, having a relatively low shear strength, showing intrinsic self-lubricating properties, and MXene can still remain stable in an argon atmosphere at 1200°C without destroying the original 2D structure. In addition, MXene has good dispersibility in both aqueous solutions and organic solvents due to the presence of functional groups (-O, -OH, -F, etc.) on its surface, providing a prerequisite for its uniform dispersion.
[0004] However, when preparing single-layer MXene from multi-layer MXene, the existing technologies mainly include ball milling method and ultrasonic method. When preparing single-layer MXene nanosheets by the ball milling method, a large amount of loss is likely to occur during the preparation process, and the yield is only about 75% - 78%. Moreover, the ball milling time is too long, all of which need to be more than 24 hours. Impurities are likely to be introduced during the ball milling process, and the heat generated is also very likely to cause phase transformation of the material, resulting in a decline in the intrinsic properties of the MXene material. In addition, although the ultrasonic dispersion method can well retain the intrinsic properties and content of MXene, its dispersion effect is greatly limited, resulting in a small content of single-layer nanosheets and making it difficult to form a strong interfacial bond with the surface of the metal matrix.
[0005] According to the existing technology, the existing methods for preparing MXene-reinforced copper-based composites mainly include "molecular-level mixing + spark plasma sintering" and "molecular-level mixing + hot pressing sintering" hot pressing sintering technologies, which have the following problems: Molecular-level mixing mainly uses copper salts, and the preparation process is relatively complex. Simply using the spark plasma sintering technology (SPS) cannot guarantee the density of the composite material and the alignment direction of MXene. While using the hot pressing sintering technology, the sintering temperature is high and the holding time is long, resulting in coarse grains of the sintered sample and reducing the mechanical properties of the composite material. Summary of the Invention
[0006] In view of the above technical deficiencies and other problems, the invention proposes a two-dimensional nanomaterial MXene-reinforced copper-based composite material with excellent mechanical properties, high-temperature stability properties, electrical and thermal conductivity properties and a preparation method thereof. The invention combines the spark plasma sintering technology and the hot rolling process to prepare the MXene-reinforced copper-based composite material, and obtains a composite material with both excellent mechanical properties and electrical conductivity.
[0007] The technical solution to realize the present invention is: A two-dimensional nanomaterial-reinforced copper-based composite material and a preparation method thereof, including the following steps:
[0008] (1) Using multi-layer MXene as the raw material and absolute ethanol as the solvent, successively through ultrasonic treatment and the first homogenization treatment, adding nano-scale Ni powder, through the second homogenization treatment, adding a solid intercalating agent, and then through the third homogenization treatment, centrifuging to obtain a suspension containing single-layer MXene nanosheets;
[0009] (2) Adding pure copper powder to the suspension containing single-layer MXene nanosheets, and successively through homogenization treatment, ball milling, and drying to obtain MXene-Cu composite material powder;
[0010] (3) Performing plasma sintering on the MXene-Cu composite material powder;
[0011] (4) Finally, through hot rolling treatment, a two-dimensional nanomaterial-reinforced copper-based composite material is obtained.
[0012] Preferably, in step (1), the addition amount of nanoscale Ni powder is 10 wt% of the mass of MXene; the addition amount of the solid-state intercalating agent is 10 times the mass of MXene.
[0013] Preferably, in step (1), the ultrasonic treatment time is more than 5 minutes; the rotation speed of the homogenization treatment is 10000 rpm / min, the first homogenization treatment time is 20 min, the second homogenization treatment time is 30 min, and the third homogenization treatment time is 6 h.
[0014] Preferably, in step (2), in the MXene / Cu composite powder, the content of MXene is 0.2 - 1.5 wt%.
[0015] Preferably, in step (2), the rotation speed of the homogenization treatment is 10000 rpm / min, and the time is 2 h; the rotation speed of the ball milling treatment is 300 rpm / min, the time is 12 h, and the ball-to-material ratio is 4:1.
[0016] Preferably, in step (3), the plasma sintering temperature is 850 °C and the time is 6 min.
[0017] Preferably, in step (4), the hot rolling treatment temperature is 100 °C, the linear velocity is 30 mm / s, and it is rolled back and forth 5 times.
[0018] Compared with the prior art, the present invention prepares monolayer MXene nanosheets by a method combining ultrasonic dispersion and high-speed homogenization. During the preparation process, nanoscale Ni powder is added to further improve the wettability of MXene. The Ni-modified MXene process is simple, and the Ni particles collide violently with the MXene nanosheets under the action of a high-speed homogenizer, enabling the Ni particles to be well adsorbed on the surface of MXene. In addition, the added urea intercalating agent has a low cost, a simple acquisition method, and is easily removed in the centrifugal washing process, ensuring the purity of the MXene nanosheet solution. The present invention uses a ball milling method to mix monolayer MXene nanosheets and copper powder. This method further utilizes the violent collision between the matrix particles and the reinforcing phase material to disperse a small amount of multilayer MXene that has not been completely dispersed, enabling the monolayer MXene nanosheets to be evenly distributed in the matrix material. Then, the obtained composite powder is subjected to spark plasma sintering, and the sintered sample is subjected to hot rolling treatment, which can refine the grains of the composite material and reduce the grain gaps. Description of the Drawings
[0019] Figure 1 It is a schematic diagram of the powder mixing process of MXene-Cu composite powder.
[0020] Figure 2 Process flow chart for the preparation of MXene / Cu composite material
[0021] Figure 3 SEM images of the original powders, where (a) Cu powder; (b) Ni powder; (c) multi-layer MXene powder
[0022] Figure 4 XRD patterns of the original powders, where (a) Cu powder; (b) Ni powder; (c) multi-layer MXene powder
[0023] Figure 5 SEM images of few-layer MXene nanosheets after homogenization of multi-layer MXene, where (a) and (b) are at different magnifications
[0024] Figure 6 SEM images of 0.2wt.% MXene / Cu composite material powder at different magnifications, where (a) 500X; (b) and (c) are magnified images of 2000 times and 10000 times respectively within the yellow square in figure (a); (d) is the EDS spectrum at the position of the blue square in figure (b)
[0025] Figure 7 OM images of different samples, where (a) pure Cu; (b) 0.2wt% MXene / Cu composite material; (c) 0.4wt% MXene / Cu composite material; (d) 0.6wt% MXene / Cu composite material; (e) 1.5wt% MXene / Cu composite material
[0026] Figure 8 In (a) is the density curve of MXene / Cu composite material with the change of MXene content; (b) is the Vickers hardness diagram of MXene / Cu composite material with the change of MXene content Detailed implementation manners
[0027] The present invention prepares single-layer MXene nanosheets by the method of "high-speed homogenization + ultrasonic", obtains the composite powder of single-layer MXene nanosheets and copper powder by the method of "high-speed homogenization + ball milling", and then combines the "spark plasma sintering + hot rolling" technology to obtain a new composite material with both excellent mechanical properties and good electrical conductivity
[0028] Combined with Figure 2 , the specific steps for the present invention to prepare two-dimensional nanomaterial MXene-reinforced copper-based composite material are as follows:
[0029] Four kinds of MXene / Cu composites with different contents (0.2 wt.%, 0.4 wt.%, 0.6 wt.%, 1.5 wt.%) were prepared in this invention. 25 g of MXene / Cu composite powder with each content was prepared. The specific contents are shown in Table 1. In addition, 100 g of pure copper powder was weighed with an electronic balance and divided into four parts, each part being 25 g, which was used for comparative study at different sintering temperatures.
[0030] Table 1. Composition Table of MXene / Cu Composite Powder Content
[0031]
[0032] (1) Preparation of Single-Layer MXene Nanosheets
[0033] a. Pour the weighed multi-layer MXene (Ti3C2) into a beaker, and then add absolute ethanol to it to prepare a solution with a concentration of 1 mg / ml and perform ultrasonic treatment for 5 minutes at 40 °C.
[0034] b. After ultrasonic treatment, homogenize the solution with a high-speed homogenizer. The homogenization speed is 10000 rpm / min and the homogenization time is 20 min.
[0035] c. After step b is completed, continue to add Ni powder with a content of 10 wt% of MXene to the solution to improve the surface wettability of MXene. The homogenization speed is 10000 rpm / min and the homogenization time is 30 min.
[0036] d. After homogenization, add a solid intercalating agent (urea) to the solution. The added content is 10 times the content of MXene, and continue to perform homogenization treatment. The homogenization speed is 10000 rpm / min and the homogenization time is 6 h.
[0037] e. After the above steps are completed, the solid intercalating agent needs to be removed. Pour the solution into a centrifuge tube and centrifuge and wash it at 4000 rpm / min for 10 min in a centrifuge (LC-LX-L40B, Shanghai Lichen Bangxi Instrument Technology Co., Ltd.). A total of 4 times of centrifugation and washing are required.
[0038] f. After centrifugation is completed, pour off the supernatant. The remaining suspension contains the single-layer MXene nanosheets required for the experiment.
[0039] (2) Preparation of MXene / Cu Composite Powder
[0040] a. After the preparation of monolayer MXene nanosheets, weighed pure copper powder is added to the suspension containing monolayer MXene nanosheets, and a certain amount of absolute ethanol is added until the composite powder is completely immersed (in this invention, a 250 ml volumetric beaker is used, and absolute ethanol is added to the 250 ml graduation line). The prepared solution is homogenized by a high-speed homogenizer at a homogenization speed of 10,000 rpm / min for 2 h;
[0041] b. After homogenization, the solution containing the composite powder is poured into a 500 ml stainless steel ball milling jar with a ball-to-material ratio of 4:1 and about 100 g of stainless steel grinding balls. Then absolute ethanol is added to two-thirds of the ball milling jar for high-energy ball milling at a speed of 300 rpm / min for 12 h. Stop rotating for 20 min every 3 h (for heat dissipation of the ball milling jar), and change the rotation direction each time when stopping.
[0042] c. After ball milling, the grinding balls are separated from the solution, and the solution is vacuum dried at a drying temperature of 80 °C until all the absolute ethanol has evaporated. The composite powder is collected and ground for use. The mixing steps are as Figure 1 shown.
[0043] (3) Sintering of pure copper powder
[0044] a. Lay a layer of graphite paper on the bottom and side of the graphite mold;
[0045] b. Put the dried ground powder into a cylindrical graphite mold with a sintering diameter of 15 mm, then put the mold into a spark plasma sintering equipment, compact the mixed powder, and evacuate the plasma sintering equipment;
[0046] c. The compacted powder is heated in the sintering equipment at a heating rate of 150 °C / min, and the pressure at both ends of the mold is gradually increased to 50 MPa. When the sintering temperature reaches the sintering temperature (750 °C, 800 °C, 850 °C, 900 °C) and the sintering pressure reaches 50 MPa, keep it warm for 6 min;
[0047] d. After sintering, the sintered sample is cooled to room temperature in the furnace, and the sample is taken out.
[0048] (4) Sintering + hot rolling of MXene / Cu composite powder
[0049] a. Lay a layer of graphite paper on the bottom and side of 4 graphite molds;
[0050] b. After drying the composite powders with four contents, put them into 4 cylindrical graphite molds with a sintering diameter of 15 mm, then put the molds into a spark plasma sintering equipment, compact the mixed powder, and evacuate the plasma sintering equipment;
[0051] c. The compacted powder is heated in a sintering device at a heating rate of 150 °C / min, while the pressure at both ends of the mold is gradually increased to 50 MPa. When the sintering temperature reaches 850 °C and the sintering pressure reaches 50 MPa, it is kept warm for 6 min;
[0052] d. After sintering, the sintered sample is cooled to room temperature in the furnace and the sample is taken out.
[0053] e. The sintered sample is polished with a metallographic sample grinding and polishing machine at a rotation speed of 800 rpm / min and the sandpaper size is 400 mesh;
[0054] f. The sample is hot-rolled with a rolling mill (MSK-HRP-01, Hefei Kejing Materials Technology Co., Ltd.) at a temperature of 100 °C, a linear speed of 30 mm / s, and rolled back and forth 5 times.
[0055] Example 1
[0056] In this example, according to the specific operation process in step (3) of the above method, high-purity nanometer copper powder (99.99%, 500 nm) is used as the original powder, and no MXene reinforcement phase material is added. The dried powder is put into a graphite mold with a diameter of 15 mm, compacted and then sintered in a spark plasma device. The mold is heated to 750 °C at a speed of 150 °C / min, and pressure is applied to both ends of the compacted powder material during the heating process until 50 MPa, and then the pressure is kept unchanged. After the temperature reaches 750 °C, it is kept warm at this temperature for 6 min. After the sample sintering is completed, it is taken out, the surface of the sample is polished, and after the polishing is completed, it is hot-rolled at a temperature of 100 °C, a linear speed of 30 mm / s, and rolled back and forth 5 times.
[0057] Example 2
[0058] In this example, according to the specific operation process in step (3) of the above method, high-purity nanometer copper powder (99.99%, 500 nm) is used as the original powder, and no MXene reinforcement phase material is added. The dried powder is put into a graphite mold with a diameter of 15 mm, compacted and then sintered in a spark plasma device. The mold is heated to 800 °C at a speed of 150 °C / min, and pressure is applied to both ends of the compacted powder material during the heating process until 50 MPa, and then the pressure is kept unchanged. After the temperature reaches 800 °C, it is kept warm at this temperature for 6 min. After the sample sintering is completed, it is taken out, the surface of the sample is polished, and after the polishing is completed, it is hot-rolled at a temperature of 100 °C, a linear speed of 30 mm / s, and rolled back and forth 5 times.
[0059] Example 3
[0060] In this embodiment, according to the specific operation process in step (3) of the above method, high-purity nano copper powder (99.99%, 500 nm) is used as the original powder, and no MXene reinforcing phase material is added. The dried powder is placed in a graphite mold with a diameter of 15 mm, compacted, and then sintered in a spark plasma equipment. The mold is heated to 850 °C at a rate of 150 °C / min, and pressure is applied to both ends of the compacted powder material during the heating process until 50 MPa. Subsequently, the pressure is kept constant. When the temperature reaches 850 °C, it is held at this temperature for 6 min. After the sample sintering is completed, it is taken out, the surface of the sample is polished, and after polishing, hot rolling is carried out. The temperature is set at 100 °C, the linear velocity is 30 mm / s, and it is rolled back and forth 5 times.
[0061] Example 4
[0062] In this embodiment, according to the specific operation process in step (3) of the above method, high-purity nano copper powder (99.99%, 500 nm) is used as the original powder, and no MXene reinforcing phase material is added. The dried powder is placed in a graphite mold with a diameter of 15 mm, compacted, and then sintered in a spark plasma equipment. The mold is heated to 900 °C at a rate of 150 °C / min, and pressure is applied to both ends of the compacted powder material during the heating process until 50 MPa. Subsequently, the pressure is kept constant. When the temperature reaches 900 °C, it is held at this temperature for 6 min. After the sample sintering is completed, it is taken out, the surface of the sample is polished, and after polishing, hot rolling is carried out. The temperature is set at 100 °C, the linear velocity is 30 mm / s, and it is rolled back and forth 5 times.
[0063] Example 5
[0064] In this embodiment, according to the specific operation processes in steps (1), (2) and (4) of the above method, high-purity nano copper powder (99.99%, 500 nm) and multi-layer MXene (Ti3C2) are used as the original powder. 24.95 g of copper powder and 0.05 g of multi-layer MXene (0.2 wt.%) are weighed with an electronic balance. The multi-layer MXene nanosheets are ultrasonically dispersed, homogenized, centrifuged and washed to remove the supernatant. The copper powder and single-layer MXene nanosheets are mixed by high-speed homogenization and wet ball milling, and the composite powder is dried and ground to obtain the mixed powder for sintering. The dried and ground powder is placed in a graphite mold with a diameter of 15 mm, compacted, and then sintered in a spark plasma equipment. The mold is heated to 850 °C at a rate of 150 °C / min, and pressure is applied to both ends of the compacted powder material during the heating process until 50 MPa. Subsequently, the pressure is kept constant. When the temperature reaches 850 °C, it is held at this temperature for 6 min. After the sample sintering is completed, it is taken out, the surface of the sample is polished, and after polishing, hot rolling is carried out. The temperature is set at 100 °C, the linear velocity is 30 mm / s, and it is rolled back and forth 5 times.
[0065] Example 6
[0066] In this example, according to the specific operation processes in steps (1), (2) and (4) of the above method, high-purity nano copper powder (99.99%, 500 nm) and multi-layer MXene (Ti3C2) are used as the original powders. Weigh 24.9 g of copper powder and 0.1 g (0.4 wt.%) of multi-layer MXene with an electronic balance. After ultrasonic dispersion of the multi-layer MXene nanosheets, homogenize them, centrifuge and wash to remove the supernatant. Mix the copper powder and the single-layer MXene nanosheets by high-speed homogenization and wet ball milling, dry and grind the composite powder, and use it as the mixed powder for sintering. Put the dried and ground powder into a graphite mold with a diameter of 15 mm, compact it, and then sinter it in a spark plasma device. Heat the mold at a rate of 150 °C / min to 850 °C, and apply pressure to both ends of the compacted powder material during the heating process until 50 MPa, then keep the pressure constant. When the temperature reaches 850 °C, hold the temperature for 6 min. Take out the sample after sintering is completed, polish the surface of the sample, and then perform hot rolling after polishing. Set the temperature to 100 °C, the linear speed to 30 mm / s, and roll back and forth 5 times.
[0067] Example 7
[0068] In this example, according to the specific operation processes in steps (1), (2) and (4) of the above method, high-purity nano copper powder (99.99%, 500 nm) and multi-layer MXene (Ti3C2) are used as the original powders. Weigh 24.85 g of copper powder and 0.15 g (0.6 wt.%) of multi-layer MXene with an electronic balance. After ultrasonic dispersion of the multi-layer MXene nanosheets, homogenize them, centrifuge and wash to remove the supernatant. Mix the copper powder and the single-layer MXene nanosheets by high-speed homogenization and wet ball milling, dry and grind the composite powder, and use it as the mixed powder for sintering. Put the dried and ground powder into a graphite mold with a diameter of 15 mm, compact it, and then sinter it in a spark plasma device. Heat the mold at a rate of 150 °C / min to 850 °C, and apply pressure to both ends of the compacted powder material during the heating process until 50 MPa, then keep the pressure constant. When the temperature reaches 850 °C, hold the temperature for 6 min. Take out the sample after sintering is completed, polish the surface of the sample, and then perform hot rolling after polishing. Set the temperature to 100 °C, the linear speed to 30 mm / s, and roll back and forth 5 times.
[0069] Example 8
[0070] In this embodiment, according to the specific operation processes in the above method steps (1), (2) and (4), high-purity nano copper powder (99.99%, 500 nm) and multi-layer MXene (Ti3C2) are used as the original powders. 23.625 g of copper powder and 0.375 g (1.5 wt.%) of multi-layer MXene are weighed with an electronic balance. After ultrasonic dispersion of the multi-layer MXene nanosheets, they are homogenized, centrifuged and washed to remove the supernatant. The copper powder and the single-layer MXene nanosheets are mixed by high-speed homogenization and wet ball milling, and the composite powder is dried and ground to obtain the mixed powder for sintering. The dried and ground powder is put into a graphite mold with a diameter of 15 mm, compacted and then sintered in a spark plasma device. The mold is heated to 850 °C at a rate of 150 °C / min, and pressure is applied to both ends of the compacted powder material until 50 MPa during the heating process. Subsequently, the pressure is kept constant. When the temperature reaches 850 °C, it is held at this temperature for 6 min. After the sample sintering is completed, it is taken out, the surface of the sample is polished, and after polishing, hot rolling is carried out. The temperature is set at 100 °C, the linear speed is 30 mm / s, and it is rolled back and forth 5 times.
[0071] 2. Experimental results
[0072] Figure 3 (a)-(c) in are the original powder morphology diagrams of Cu powder, Ni powder, and multi-layer MXene respectively. It can be seen that both Cu powder and Ni powder are nanoscale to 500 nm, and MXene is a multi-layer powder in the shape of an accordion. Figure 4 (a)-(c) in are the XRD diagrams of the original powders Cu powder, Ni powder, and multi-layer MXene.
[0073] Figure 5 (a) and (b) in are the morphology diagrams of the single-layer MXene nanosheets prepared after the dispersion of MXene. From Figure 5 it can be seen that the diameter of the single-layer MXene nanosheets is about 1-2 μm, which indicates that the high-speed homogenization technology can effectively disperse the multi-layer MXene into few-layer or even single-layer MXene nanosheets.
[0074] Figure 6 (a) in is the 500-fold SEM image of the 0.2 wt.% MXene / Cu composite powder, Figure 6 (b) and (c) in are the 2000-fold and 10000-fold magnified images of the yellow square in (a) respectively, Figure 6 (d) in is the EDS energy spectrum analysis image of the blue square position in (b). It can be seen that the MXene reinforcement phase is evenly distributed in the Cu matrix without agglomeration. And through high-magnification electron microscopy (2000-fold, 10000-fold), it can be found that at the sintering temperature of 850 °C, MXene can still well maintain its original 2D structure.
[0075] Figure 7 are optical microscope images of the prepared samples with different compositions. From Figure 7 it can be seen that with the increase in the MXene content, the content of the reinforcement phase material in the matrix per unit volume increases significantly and is evenly distributed. Therefore, it can be confirmed that the MXene / Cu composite material sample contains MXene nanosheets and can maintain good stability at high temperatures. This is conducive to the formation of a good interfacial bond between the MXene reinforcement phase and the Cu matrix, helps stress transfer, and improves the properties of the composite material. (a) in Fig. 8 is the density curve of the MXene / Cu composite material with the change in the MXene content, Figure 8 and (b) in it is the Vickers hardness diagram of the MXene / Cu composite material with the change in the MXene content. The specific values of the density and hardness are shown in Table 2. From Figure 8 in (a) it can be seen that with the increase in the MXene content, the density of the composite material sample increases significantly, up to ∼99.78%, indicating that the added MXene can effectively improve the density of the composite material. From Figure 8 in (b) it can be seen that with the increase in the MXene content, the microhardness of the sample first increases and then decreases. When the MXene content is 0.4%, its Vickers hardness reaches the maximum value of 112 HV, which is ∼6% higher than that of pure copper.
[0076] Table 2. Density and Vickers hardness values of composite material samples with different MXene contents
[0077]
Claims
1. A method for preparing a two-dimensional nanomaterial reinforced copper-based composite material, characterized in that: The steps include: (1) Using multilayer MXene as raw material and anhydrous ethanol as solvent, ultrasonic treatment and the first homogenization treatment were performed in sequence, nano-sized Ni powder was added, the second homogenization treatment was performed, a solid intercalation agent was added, and the third homogenization treatment was performed. After centrifugation, a suspension containing single-layer MXene nanosheets was obtained; (2) adding pure copper powder to a suspension containing a single-layer MXene nanosheet, and obtaining a MXene-Cu composite material powder by homogenization, ball milling, and drying; (3) plasma sintering the MXene-Cu composite powder; (4) Finally, after hot rolling treatment, a two-dimensional nanomaterial reinforced copper-based composite material is obtained; Among them, the addition amount of nano-sized Ni powder is 10wt% of the mass of MXene; the addition amount of solid intercalation agent is 10 times the mass of MXene; the MXene content in MXene / Cu composite powder is 0.2~0.6wt%; In step (1), the ultrasonic treatment time is more than 5 minutes; the homogenization speed is 10000 rpm / min, the first homogenization time is 20 minutes, the second homogenization time is 30 minutes, and the third homogenization time is 6 hours; In step (2), the homogenization speed is 10000 rpm / min, the time is 2 h; the ball milling speed is 300 rpm / min, the time is 12 h, and the ball-to-material ratio is 4:1; In step (3), the plasma sintering temperature is 850°C and the time is 6 minutes; In step (4), the hot rolling treatment temperature is 100° C., the line speed is 30 mm / s, and the rolling is repeated 5 times.
2. A two-dimensional nanomaterial reinforced copper-based composite material prepared by the preparation method as claimed in claim 1.
Citation Information
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