GRAPHENE COPPER COMPOSITE MATERIAL PREPARATION METHOD BASED ON COMBINATION OF HOT PRESSING SINTERING AND CHEMICAL VAPOR DEPOSITION

Abstract

A graphene copper composite material preparation method based on a combination of hot pressing sintering and chemical vapor deposition, comprising: presetting multi-layer copper foil in a hot pressing chamber; preparing a graphene thin film on the surface of the copper foil by means of a chemical vapor deposition method to obtain a graphene copper composite material; and then performing hot pressing forming on the multi-layer graphene copper foil material to prepare the graphene copper composite material. Said material can replace a traditional copper material or silver material, is applied to a supercapacitor or a motor driving device, and has the effects of improving efficiency, reducing temperature rise, etc.

Claims

1. A graphene copper composite material preparation method, comprising: a) presetting multi-layers of copper foils in a hot pressing chamber; b) preparing a graphene thin film on the surface of the copper foil by means of a chemical vapor deposition process with methane as a carbon source to obtain a graphene copper raw material; and c) performing hot pressing sintering forming on the graphene copper raw material by means of a hot pressing sintering process to obtain a graphene copper composite material.

2. The graphene copper composite material preparation method of claim 1, wherein the spacing between layers of copper foils is controlled between 0.1 to 1 mm.

3. The graphene copper composite material preparation method of claim 1, wherein the copper foils have a purity of 99.9%, preferably 99.9% to 99.9999%.

4. The graphene copper composite material preparation method of claim 1, wherein each of the copper foils is a rolled copper foil with an orientation of (111).

5. The graphene copper composite material preparation method of claim 1, wherein the copper foil has a thickness of 15 to 25 M.

6. The graphene copper composite material preparation method of claim 1, wherein the method further includes the step of performing a hydrogen reduction treatment on the copper foil to remove gas adsorbed on the surface and oxide layer before depositing a graphene thin film.

7. The graphene copper composite material preparation method of claim 1, wherein the vapor deposition process is performed under at a temperature of 950 C. to 1020 C.; and/or, graphene is deposited on both the upper and lower sides of the copper foil, and the number of layers of the prepared graphene thin film is optionally 1 to 5 layers; and/or, the hot pressing sintering is performed under a hot pressing atmosphere of a high vacuum, a hot pressing temperature of 850 C. to 1050 C., and a pressure of 20 MPa to 60 MPa.

8. The graphene copper composite material preparation method of claim 1, wherein the total number of layers of the graphene copper composite material is 10 to 1000 layers.

9. The graphene copper composite material preparation method of claim 1, wherein the operation of the graphene thin film and hot pressing sintering in the preparation method are performed in a same chamber.

10. A graphene copper composite material prepared by the method of claim 1.

11. The graphene copper composite material preparation method of claim 2, wherein the copper foil has a purity of 99.9%, preferably 99.9% to 99.9999%.

12. The graphene copper composite material preparation method of claim 2, wherein the copper foil is a rolled copper foil with an orientation of (111).

13. The graphene copper composite material preparation method of claim 3, wherein the copper foil is a rolled copper foil with an orientation of (111).

14. The graphene copper composite material preparation method of claim 2, wherein the copper foil has a thickness of 15 to 25 M.

15. The graphene copper composite material preparation method of claim 3, wherein the copper foil has a thickness of 15 to 25 M.

16. The graphene copper composite material preparation method of claim 4, wherein the copper foil has a thickness of 15 to 25 M.

17. The graphene copper composite material preparation method of claim 2, wherein the method further includes the step of performing a hydrogen reduction treatment on the copper foil to remove gas adsorbed on the surface and oxide layer before depositing a graphene thin film.

18. The graphene copper composite material preparation method of claim 3, wherein the method further includes the step of performing a hydrogen reduction treatment on the copper foil to remove gas adsorbed on the surface and oxide layer before depositing a graphene thin film.

19. The graphene copper composite material preparation method of claim 4, wherein the method further includes the step of performing a hydrogen reduction treatment on the copper foil to remove gas adsorbed on the surface and oxide layer before depositing a graphene thin film.

20. The graphene copper composite material preparation method of claim 5, wherein the method further includes the step of performing a hydrogen reduction treatment on the copper foil to remove gas adsorbed on the surface and oxide layer before depositing a graphene thin film.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0027] FIG. 1 is a schematic structural diagram of all equipment for preparing the graphene copper composite material in the examples of the present application.

[0028] FIG. 2 is a physical photograph of the graphene copper composite material prepared in the examples of the present application.

[0029] FIG. 3 is a microstructure photograph of the graphene copper composite material prepared in Example 5 of the present application.

SPECIFIC MODES FOR CARRYING OUT THE EMBODIMENTS

[0030] The present application is described in detail below in conjunction with examples, but the protection scope of the present application is not limited to the following examples.

[0031] The graphene copper composite material in the following examples can be prepared using the equipment shown in FIG. 1. In FIG. 1, 1: upper press ram; 2: lower press ram; 3: pressing system; 4: deposition area of graphene thin films; 5: copper foils with high purity; 6: copper foil fixture.

[0032] The preparation method of the graphene copper composite material in the following examples is specifically as follows:

[0033] The present application adopts the following technical solutions:

[0034] Step A: loading materials, multi-layers of copper foils were preset in a hot pressing chamber, and the spacing between copper foils was controlled to a spacing between 0.1 to 1 mm using tooling fixtures; the thickness of copper foil was 25 m;

[0035] Step B: CVD process, methane was used as a carbon source to prepare graphene thin films on the surface of the copper foil preset in Step A; and

[0036] Step C: hot pressing sintering, molybdenum alloy press rams were installed on the upper and lower sides of multi-layer copper foil, and hot pressing sintering was performed using the graphene copper raw material prepared in step B to obtain a graphene copper composite material.

[0037] After further processing, the resulted graphene copper composite material was made into 20 mm (length)20 mm (width)1 mm (height).

[0038] FIG. 2 is a photograph of the graphene copper composite material prepared in the examples, wherein numbers 1 to 14 correspond to Examples 1 to 14.

[0039] FIG. 3 is a microstructure photograph of the graphene copper composite material prepared in Example 5 of the present application.

[0040] Table 1 lists the raw material components, preparation process parameters, and product performance parameters of Examples 1 to 14.

[0041] Graphene, as a conductive reinforcement material, has a composite effect and synergistic effect with copper material, and thereby achieving the effect of improving electrical conductivity. The results of Example 1 and Comparative Example 2 can indicate that the electrical performance of the copper-based composite material is increased from 100% IACS to 106% IACS, the temperature rise is decreased and the efficiency is increased after the addition of graphene.

[0042] It can be seen from the comparison between Example 2 and Example 11 that after the number of graphene layers exceeds 5, the properties of graphene change, and it will exist in the copper matrix in the form of free carbon, which is equivalent to the existence of impurity elements, thereby generating lattice defects and resulting in the decrease in conductivity.

[0043] It can be seen from the comparison results of Examples 11, 12, and 13 that as the purity of the raw materials increases, the electrical performance is improved.

[0044] It can be seen from the comparison results of Examples 2, 3, and 4 that the increase in the hot pressing temperature can improve the composite effect of copper and graphene, and improve the electrical conductivity.

[0045] For application verification, a flat-panel transformer test of the graphene-modified metal material was conducted, and the test results are shown in Table 1.

[0046] The thermal conductivity test was conducted in accordance with GB/T22588-2008; the tensile strength test was conducted in accordance with GB/T228.1-2010; the electrical conductivity test was conducted in accordance with T/CSTM 00591-2022; the efficiency test was conducted in accordance with the GB/18613-2016 Minimum allowable values of energy efficiency and energy efficiency grades for small and medium three-phase asynchronous motors; and temperature rise test was conducted under the following conditions: a voltage of 440 V, a current of 38 A, a frequency of 60 Hz, room temperature of 20 C., and stator winding temperature rise was detected.

[0047] The results show that the temperature rise is decreased by 2.4 C. and the efficiency is increased by 2.8%.

TABLE-US-00001 TABLE 1 Process control Product CVD process performance parameters Number of Deposition Hot pressing process Electrical Thermal Application verification Copper foil/ graphene temperature/ Pressure/ Temperature/ conductivity/ conductivity/ Temperature Efficiency/ Examples purity/% layers/N C. MPa C. Layer IACS % W/(m .Math. k) rise/ C. % 1 99.99 40 950 20 100 385 95 91 2 99.99 1 900 40 950 100 106 385 91.2 93.6 3 99.99 2 950 40 950 200 109 403 91.3 94.2 4 99.99 5 1020 40 950 200 110 392 90.4 92.4 5 99.99 2 950 40 800 200 112 415 89.3 92.2 6 99.99 2 950 40 1000 500 114 375 89.2 93.1 7 99.99 1 950 40 1030 300 110 408 89.4 94.4 8 99.99 1 950 25 950 100 110 410 89.5 93.4 9 99.99 2 950 55 950 800 107 383 91.4 92.3 10 99.99 5 950 40 950 100 110 403 88.3 97.2 11 99.999 2 950 40 950 200 115 400 88.2 97.4 12 99.99 18 950 40 950 200 102 380 94.5 92 13 95 2 950 40 950 200 98 375 96 91 14 99.99 2 1000 40 980 100 110 390 89.5 95

[0048] Although the present application has been described in detail with general descriptions and specific embodiments in the above context, it is obvious to a person skilled in the art that some modifications or improvements can be made based on the present application. Therefore, these modifications or improvements made without departing from the spirit of the present application shall fall within the protection scope claimed by the present application.