A method for preparing a graphene-reinforced copper-based composite wire

Abstract

A method for preparing graphene-reinforced copper-based composite wires. This invention employs a chemical plating process to deposit silver onto the surface of graphene, obtaining silver-plated graphene powder. By controlling the silver content in the silver-plated graphene powder between 15.3 wt% and 34.7 wt%, the high-temperature conductivity of the graphene-reinforced copper-based composite wires is effectively improved, while maintaining minimal change in the tensile strength of the copper-based composite wires. The copper-based composite wires prepared using this method maintain a conductivity above 70% IACS even at a temperature rise of 150°C, demonstrating broad application prospects in conductor materials for heating equipment.

Description

Technical Field

[0001] This invention belongs to the field of copper-based new materials, specifically relating to a method for preparing graphene-reinforced copper-based composite wires. Background Technology

[0002] With industrial development and the emergence of many new fields, higher demands are being placed on conductor materials. Pure copper wire has gained widespread attention due to its excellent electrical and thermal conductivity. The conductivity of pure copper at room temperature typically exceeds 100% IACS; however, under elevated temperatures, the increased scattering of free electrons caused by atomic oscillations leads to a significant decrease in the conductivity of pure copper. For example, at 150°C, the conductivity of pure copper drops to approximately 68% IACS. Therefore, the industry urgently needs to develop high-quality conductive materials that can operate under elevated temperatures. In view of this, the purpose of this invention is to obtain a conductor material with excellent high-temperature conductivity. Summary of the Invention

[0003] The purpose of this invention is to provide a method for preparing graphene-reinforced copper-based composite wires, aiming to obtain copper-based composite wires with excellent high-temperature conductivity and tensile strength.

[0004] The technical solution of the present invention is as follows:

[0005] A method for preparing a graphene-reinforced copper-based composite wire includes the following steps:

[0006] Weigh graphene and form a solution system, then stir and disperse it at 300-350 r / min for 30-60 min; prepare a 0.3-0.5 g / mL silver nitrate solution, mix it with the graphene solution and stir magnetically for 30-60 min, then add a 0.15-0.30 g / mL glucose solution as a reducing agent, heat to about 80-95℃, and stir at a constant temperature to allow the reaction to proceed fully, thus obtaining silver-containing graphene composite powder. Finally, reduce it under a mixed atmosphere of hydrogen / argon to obtain silver-plated graphene powder. By adjusting the amount of graphene, the proportion of silver in the silver-plated graphene powder is 15.3-34.7 wt%.

[0007] Graphene silver-plated powder and copper powder are ground and mixed at a mass ratio of 1:1.82-2.11, then loaded into an oxygen-free copper tube. The copper tube is then forged to an outer diameter of Φ6-8mm using a rotary forging machine. After that, it is drawn in multiple passes on a drawing machine to obtain a wire with a diameter of Φ1-1.2mm. Finally, it is vacuum annealed at 320-330℃ for 2-3 hours to relieve stress, thus obtaining a graphene-reinforced copper-based composite wire.

[0008] Preferably, the stirring speed is 350 r / min.

[0009] Preferably, the annealing temperature is 320℃.

[0010] Preferably, the annealing time is 2 hours.

[0011] Preferably, the concentration of the silver nitrate solution is 0.5 g / mL.

[0012] Preferably, the concentration of the glucose solution is 0.30 g / mL.

[0013] Preferably, the silver content in the graphene silver-plated powder is 23.4 wt%.

[0014] This invention utilizes a chemical plating process to deposit silver onto the surface of graphene, resulting in silver-plated graphene powder that significantly improves the high-temperature conductivity of graphene-reinforced copper-based composite wires. Simultaneously, an appropriate silver content has little effect on the tensile strength of the graphene-reinforced copper-based composite wires; however, excessive silver content negatively impacts tensile strength. Therefore, in practice, the silver content in the silver-plated graphene powder should be controlled between 15.3 wt% and 34.7 wt%. Detailed Implementation

[0015] The technical effects of the present invention will be verified through specific embodiments below, but the implementation of the present invention is not limited thereto.

[0016] Example 1

[0017] Graphene was weighed and a solution was formed. The solution was stirred and dispersed at 300 r / min for 30 min. A 0.3 g / mL silver nitrate solution was prepared and mixed with the graphene solution. The mixture was then magnetically stirred for 30 min. A 0.15 g / mL glucose solution was added dropwise as a reducing agent. The temperature was raised to 80℃ and stirred at a constant temperature to allow the reaction to proceed fully, resulting in silver-containing graphene composite powder. Finally, the powder was reduced in a mixed atmosphere of hydrogen and argon to obtain silver-plated graphene powder. By adjusting the amount of graphene, the silver content in the silver-plated graphene powder was adjusted to 15.3 wt%.

[0018] Graphene silver-plated powder and copper powder were ground and mixed at a mass ratio of 1:1.82, and then loaded into an oxygen-free copper tube. The copper tube was then forged to an outer diameter of Φ6mm using a rotary forging machine. After that, it was drawn in multiple passes on a drawing machine to obtain a wire with a diameter of Φ1mm. Finally, it was vacuum annealed at 320℃ for 2 hours to eliminate stress, thus obtaining a graphene-reinforced copper-based composite wire.

[0019] Example 2

[0020] Graphene was weighed and a solution was formed. The solution was stirred and dispersed at 300 r / min for 30 min. A 0.3 g / mL silver nitrate solution was prepared and mixed with the graphene solution. The mixture was then magnetically stirred for 30 min. A 0.15 g / mL glucose solution was added dropwise as a reducing agent. The temperature was raised to 80 °C and stirred at a constant temperature to allow the reaction to proceed fully, resulting in silver-containing graphene composite powder. Finally, the powder was reduced in a mixed atmosphere of hydrogen and argon to obtain silver-plated graphene powder. By adjusting the amount of graphene, the silver content in the silver-plated graphene powder was adjusted to 18.5 wt%.

[0021] Graphene silver-plated powder and copper powder were ground and mixed at a mass ratio of 1:1.82, and then loaded into an oxygen-free copper tube. The copper tube was then forged to an outer diameter of Φ6mm using a rotary forging machine. After that, it was drawn in multiple passes on a drawing machine to obtain a wire with a diameter of Φ1mm. Finally, it was vacuum annealed at 320℃ for 2 hours to eliminate stress, thus obtaining a graphene-reinforced copper-based composite wire.

[0022] Example 3

[0023] Graphene was weighed and a solution was formed. The solution was stirred and dispersed at 300 r / min for 30 min. A 0.3 g / mL silver nitrate solution was prepared and mixed with the graphene solution. The mixture was then magnetically stirred for 30 min. A 0.15 g / mL glucose solution was added dropwise as a reducing agent. The temperature was raised to 80 °C and stirred at a constant temperature to allow the reaction to proceed fully, resulting in silver-containing graphene composite powder. Finally, the powder was reduced in a mixed atmosphere of hydrogen and argon to obtain silver-plated graphene powder. By adjusting the amount of graphene, the silver content in the silver-plated graphene powder was adjusted to 23.4 wt%.

[0024] Graphene silver-plated powder and copper powder were ground and mixed at a mass ratio of 1:1.82, and then loaded into an oxygen-free copper tube. The copper tube was then forged to an outer diameter of Φ6mm using a rotary forging machine. After that, it was drawn in multiple passes on a drawing machine to obtain a wire with a diameter of Φ1mm. Finally, it was vacuum annealed at 320℃ for 2 hours to eliminate stress, thus obtaining a graphene-reinforced copper-based composite wire.

[0025] Example 4

[0026] Graphene was weighed and a solution was formed. The solution was stirred and dispersed at 300 r / min for 30 min. A 0.3 g / mL silver nitrate solution was prepared and mixed with the graphene solution. The mixture was then magnetically stirred for 30 min. A 0.15 g / mL glucose solution was added dropwise as a reducing agent. The temperature was raised to 80 °C and stirred at a constant temperature to allow the reaction to proceed fully, resulting in silver-containing graphene composite powder. Finally, the powder was reduced in a mixed atmosphere of hydrogen and argon to obtain silver-plated graphene powder. By adjusting the amount of graphene, the silver content in the silver-plated graphene powder was adjusted to 29.6 wt%.

[0027] Graphene silver-plated powder and copper powder were ground and mixed at a mass ratio of 1:1.82, and then loaded into an oxygen-free copper tube. The copper tube was then forged to an outer diameter of Φ6mm using a rotary forging machine. After that, it was drawn in multiple passes on a drawing machine to obtain a wire with a diameter of Φ1mm. Finally, it was vacuum annealed at 320℃ for 2 hours to eliminate stress, thus obtaining a graphene-reinforced copper-based composite wire.

[0028] Example 5

[0029] Graphene was weighed and a solution was formed. The solution was stirred and dispersed at 300 r / min for 30 min. A 0.3 g / mL silver nitrate solution was prepared and mixed with the graphene solution. The mixture was then magnetically stirred for 30 min. A 0.15 g / mL glucose solution was added dropwise as a reducing agent. The temperature was raised to 80 °C and stirred at a constant temperature to allow the reaction to proceed fully, resulting in silver-containing graphene composite powder. Finally, the powder was reduced in a mixed atmosphere of hydrogen and argon to obtain silver-plated graphene powder. By adjusting the amount of graphene, the silver content in the silver-plated graphene powder was adjusted to 34.7 wt%.

[0030] Graphene silver-plated powder and copper powder were ground and mixed at a mass ratio of 1:1.82, and then loaded into an oxygen-free copper tube. The copper tube was then forged to an outer diameter of Φ6mm using a rotary forging machine. After that, it was drawn in multiple passes on a drawing machine to obtain a wire with a diameter of Φ1mm. Finally, it was vacuum annealed at 320℃ for 2 hours to eliminate stress, thus obtaining a graphene-reinforced copper-based composite wire.

[0031] Comparative Example 1

[0032] Graphene powder and copper powder were ground and mixed at a mass ratio of 1:1.82, then loaded into an oxygen-free copper tube. The copper tube was then forged to an outer diameter of Φ6mm using a rotary forging machine. After that, it was drawn in multiple passes on a drawing machine to obtain a wire with a diameter of Φ1mm. Finally, it was vacuum annealed at 320℃ for 2 hours to eliminate stress, thus obtaining a graphene-reinforced copper-based composite wire.

[0033] Comparative Example 2

[0034] Graphene was weighed and a solution was formed. The solution was stirred and dispersed at 300 r / min for 30 min. A 0.3 g / mL silver nitrate solution was prepared and mixed with the graphene solution. The mixture was then magnetically stirred for 30 min. A 0.15 g / mL glucose solution was added dropwise as a reducing agent. The temperature was raised to 80 °C and stirred at a constant temperature to allow the reaction to proceed fully, resulting in silver-containing graphene composite powder. Finally, the powder was reduced in a mixed atmosphere of hydrogen and argon to obtain silver-plated graphene powder. By adjusting the amount of graphene, the silver content in the silver-plated graphene powder was made to be 60 wt%.

[0035] Graphene silver-plated powder and copper powder were ground and mixed at a mass ratio of 1:1.82, and then loaded into an oxygen-free copper tube. The copper tube was then forged to an outer diameter of Φ6mm using a rotary forging machine. After that, it was drawn in multiple passes on a drawing machine to obtain a wire with a diameter of Φ1mm. Finally, it was vacuum annealed at 320℃ for 2 hours to eliminate stress, thus obtaining a graphene-reinforced copper-based composite wire.

[0036] Next, we evaluated the high-temperature (150°C) conductivity and room-temperature tensile strength of the graphene-reinforced copper-based composite wires in Examples 1-5 and Comparative Examples 1-2. To ensure the comparability of the samples, the experimental conditions were made completely identical except for the silver content in the graphene silver-plated powder. The experimental results are shown in Table 1.

[0037] Table 1 Experimental data for each sample

[0038] serial number Conductivity at 150℃ / IACS% Room temperature tensile strength / MPa Example 1 71.31 272 Example 2 73.60 269 Example 3 75.63 277 Example 4 74.17 273 Example 5 73.19 275 Comparative Example 1 68.55 268 Comparative Example 2 70.44 251 Stress-relieved annealed pure copper wire 68％ 273

[0039] As shown in Table 1, the silver-plated graphene powder obtained by electroless plating significantly improves the high-temperature conductivity of graphene-reinforced copper-based composite wires. Meanwhile, an appropriate silver content has little effect on the tensile strength of the graphene-reinforced copper-based composite wires; however, excessive silver content negatively impacts tensile strength. Therefore, in practice, the silver content in the silver-plated graphene powder should be controlled between 15.3 wt% and 34.7 wt%.

[0040] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the technical principles of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A method for preparing graphene-reinforced copper-based composite wire, characterized in that, The preparation method includes the following steps: Graphene was weighed and a solution was formed. The solution was stirred and dispersed at 300-350 r / min for 30-60 min. A 0.3-0.5 g / mL silver nitrate solution was prepared and mixed with the graphene solution. The mixture was then magnetically stirred for 30-60 min. A 0.15-0.30 g / mL glucose solution was added dropwise as a reducing agent. The temperature was raised to 80-95℃, and the mixture was stirred at a constant temperature to ensure a complete reaction, resulting in silver-containing graphene composite powder. Finally, the powder was reduced in a mixed atmosphere of hydrogen and argon to obtain silver-plated graphene powder. By adjusting the amount of graphene, the silver content in the silver-plated graphene powder was adjusted to 18.5-34.7 wt%. Graphene silver-plated powder and copper powder are ground and mixed at a mass ratio of 1:1.82-2.11, then loaded into an oxygen-free copper tube. The copper tube is then forged to an outer diameter of Φ6-8mm using a rotary forging machine. After that, it is drawn in multiple passes on a drawing machine to obtain a wire with a diameter of Φ1-1.2mm. Finally, it is vacuum annealed at 320-330℃ for 2-3 hours to relieve stress, thus obtaining a graphene-reinforced copper-based composite wire.

2. A preparation method as described in claim 1, characterized in that, The stirring speed is 350 r / min.

3. A preparation method as described in claim 1, characterized in that, The annealing temperature is 320℃.

4. A preparation method as described in claim 1, characterized in that, The annealing time is 2 hours.

5. A preparation method as described in claim 1, characterized in that, The concentration of the silver nitrate solution is 0.5 g / mL.

6. A preparation method as described in claim 1, characterized in that, The concentration of the glucose solution is 0.30 g / mL.

7. A preparation method as described in claim 1, characterized in that, The silver content in the graphene silver-plated powder is 23.4 wt%.