Three-dimensional graphene basalt fiber composite material and preparation method thereof

Abstract

The invention provides a three-dimensional graphene basalt fiber composite material and a preparation method thereof. The three-dimensional graphene basalt fiber composite material comprises a basalt fiber cloth substrate; the graphene layer is deposited on the surface of the basalt fiber cloth substrate in a vertical growth manner; the graphene layer is composed of a vertical graphene sheet, the diameter of the graphene sheet ranges from 200 nm to 1000 nm, and the thickness of the graphene sheet is within 10 nm. The three-dimensional graphene basalt fiber composite material disclosed by the invention has excellent photo-thermal performance, electric heating performance, super-hydrophobic performance and ice hydrophobicity, so that the three-dimensional graphene basalt fiber composite material can be applied to some scenes with high photo-thermal / electric heating requirements or high hydrophobic / ice hydrophobicity requirements.

Description

Technical Field

[0001] This invention relates to the field of composite materials technology, and more specifically, to a three-dimensional graphene basalt fiber composite material and its preparation method. Background Technology

[0002] Graphene, with its high carrier mobility, excellent thermal conductivity, and mechanical strength, has become a research hotspot in global materials science and industry. Its large-scale application is of great significance for promoting the upgrading of strategic emerging industries such as new energy and electronic devices. Chemical vapor deposition (CVD) technology is considered the most industrially promising method for preparing graphene films because it can produce large-area, high-quality graphene films. However, traditional CVD processes rely on metals such as copper and nickel as catalytic substrates, and involve a complex transfer process to peel off and transfer atomically thin graphene films to the target substrate. This process is prone to film contamination, damage, and folding, significantly degrading its electrical and mechanical properties, becoming a core bottleneck limiting the practical application of graphene films.

[0003] To overcome this problem, Academician Liu Zhongfan's team proposed the concept of "super graphene materials" in 2024. This involves growing a continuous graphene layer ("graphene skin") in situ on the surface of traditional engineering materials, achieving functional synergy between graphene and the substrate material while circumventing transfer bottlenecks. This opens up a new "carrier-based" path for the industrial application of graphene. However, current research on graphene materials still focuses on specific substrates such as quartz fiber and alumina. This is because non-metallic substrates have weak catalytic activity, requiring high-temperature (>1000℃) CVD processes to promote the thermal decomposition of carbon precursors to grow graphene. Although quartz fiber can withstand high-temperature processing, its high cost (>100 yuan / square meter) severely restricts the large-scale application of composite materials. Basalt fiber, a low-cost inorganic fiber made from natural basalt ore (SiO2+Al2O3≈70%) through melt drawing, not only possesses comprehensive properties such as high temperature resistance (-269℃~700℃), high strength, excellent insulation and corrosion resistance, but also has abundant raw materials and low price. Its market price is only about 1 / 10 of that of quartz fiber, making it an ideal candidate substrate to replace quartz fiber.

[0004] Currently, most commercially available basalt fiber / graphene composite materials use a binder mixture of graphene oxide powder and basalt fiber, resulting in poor bonding strength. Some studies, such as Chinese patent CN 1058197110B, utilize CVD technology to catalyze the reduction of iron atoms on the surface of basalt fibers, pyrolyzing the carbon source on the basalt fiber surface at high temperatures to grow graphene films with a thickness of 0.3–100 nm in situ. The prepared graphene / basalt composite material possesses high mechanical strength, high electrical conductivity, and hydrophobic properties, but it lacks good photothermal effects, and its superhydrophobic and ice-repellent capabilities are uncertain, limiting its applications. Summary of the Invention

[0005] This invention provides a three-dimensional graphene basalt fiber composite material and its preparation method, aiming to improve at least one of the above-mentioned technical problems.

[0006] To address the aforementioned technical problems, this invention provides a three-dimensional graphene basalt fiber composite material, comprising:

[0007] Basalt fiber cloth substrate; A graphene layer is deposited on the surface of the basalt fiber cloth substrate in a vertical growth manner; the graphene layer is composed of vertical graphene sheets with a diameter between 200 nm and 1000 nm and a thickness of less than 10 nm.

[0008] Preferably, the three-dimensional graphene basalt fiber composite material is prepared by PECVD tube furnace; wherein the direction of the electric field emitted by the plasma of the PECVD tube furnace is perpendicular to the surface of the basalt fiber cloth substrate, thereby vertically growing the graphene layer on the basalt fiber cloth substrate.

[0009] Preferably, the three-dimensional graphene basalt fiber composite material has a strength of 100 mW / cm². 2 Under simulated sunlight, the front side with the graphene layer formed took 30 seconds to rise from room temperature of 22°C to 67°C, and the temperature stabilized at 81.3°C after 5 minutes of illumination. Under simulated sunlight of 155 mW / cm2, the front side took 30 seconds to rise from room temperature of 22°C to 90°C, and the temperature stabilized at 105.5°C after 5 minutes.

[0010] Preferably, the contact angle of the three-dimensional graphene basalt fiber composite material is greater than 150 degrees when 2 microliters of water droplets are dropped, and is 149.7 degrees when 5 microliters of water droplets are dropped.

[0011] This invention also provides a method for preparing the three-dimensional graphene basalt fiber composite material as described above, comprising: Step S1: Clean and dry the basalt fiber cloth, cut, shape and fix the dried basalt fiber cloth, push it into the furnace tube prepared by PECVD tube furnace, and seal the furnace body; Step S2: In a PECVD tube furnace, using the basalt fiber as a substrate, argon, reducing gas and gaseous carbon source are introduced to carry out the reaction; wherein, during the reaction, the electric field direction of the plasma in the PECVD tube furnace is perpendicular to the basalt fiber cloth, and graphene layer is grown perpendicularly along the electric field direction. Step S3: After the reaction is complete, cool down and open the furnace to obtain a three-dimensional graphene basalt fiber composite material.

[0012] Preferably, step S1 specifically includes: The basalt fiber cloth was cleaned with deionized water and ethanol in turn. The cleaned basalt fiber cloth is placed in an oven to dry; The dried basalt fiber cloth is cut into a barrel shape, wound into a circle the same size as the inner wall of the barrel, supported by a quartz ring inside the barrel, fixed on a quartz boat, pushed into the furnace tube, and the furnace body is sealed.

[0013] Preferably, the reaction further includes: The surface of basalt fiber cloth is subjected to plasma treatment, the treatment process of which is as follows: Evacuate the vacuum to a pressure of 10-200 Pa; Fill with argon gas at 10-100 sccm and reducing gas at 1-100 sccm; Start the plasma, starting with a power of 100W and gradually adjusting it to 200W. Clean for 10-30 minutes, then turn off the plasma.

[0014] Preferably, step S2 specifically includes: Argon gas is introduced and the temperature is gradually increased to the target reaction temperature T1; Maintain the target reaction temperature T1 for a preset time, and during the temperature holding period: turn off argon gas charging, and charge reducing gas at a flow rate of 1-100 sccm; charge gaseous carbon source, and slowly increase the charging rate from 0 to 1-100 sccm; start plasma with a power of 150W-500W, and the electric field direction is perpendicular to the surface of basalt fiber cloth.

[0015] Preferably, the gaseous carbon source includes methane, ethane, propane, acetylene, and ethanol, and the reducing gas is hydrogen.

[0016] Preferably, the target reaction temperature T1 is 400-700℃, and the preset time is 10-60 minutes.

[0017] The three-dimensional graphene basalt fiber composite material based on this embodiment has excellent photothermal properties, electrothermal properties, as well as superhydrophobic and icing-repellent properties, making it applicable to some scenarios with high requirements for photothermal / electrothermal properties or high requirements for hydrophobic / icing-repellent properties. Attached Figure Description

[0018] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present invention and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained from these drawings without creative effort.

[0019] Figure 1 In the image: (a) is a photograph of a basalt fiber cloth substrate; (b) is a photograph of a three-dimensional graphene basalt fiber composite material.

[0020] Figure 2 These are scanning electron microscope (SEM) images of the surface of the three-dimensional graphene basalt fiber composite material provided in the embodiments of the present invention at different magnifications.

[0021] Figure 3 This is a flowchart of the preparation method of the three-dimensional graphene basalt fiber composite material provided in the embodiments of the present invention.

[0022] Figure 4 These are the surface Raman spectra of the three-dimensional graphene basalt fiber composite materials of Examples 1, 2 and 3.

[0023] Figure 5 This is a comparison graph showing the change of surface temperature over time under simulated sunlight irradiation of different intensities for Examples 1, Comparative Examples 1, 2a, and 3a.

[0024] Figure 6 In the figures: (a) shows the test results of the surface static contact angle and roll-off angle of Example 2, Comparative Example 1, Comparative Example 2b, and Comparative Example 3b; (b) shows a comparison of the push-pull test of the ice bonding force of the copper cable covered in Example 2 and the copper cable covered in Comparative Example 1; (c) shows the bottom photos of the two copper cables after the push-pull test of the ice bonding force of the copper cable.

[0025] Figure 7 These are the electrothermal test results from Example 3. Detailed Implementation

[0026] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of the present invention, not all of them. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention. Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely represents selected embodiments of the invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.

[0027] The first embodiment of the present invention provides a three-dimensional graphene basalt fiber composite material, comprising: Basalt fiber cloth substrate.

[0028] In this embodiment, a photograph of the basalt fiber cloth substrate can be referred to. Figure 1 (a). Among them, basalt fiber has the advantages of high tensile strength and good mechanical properties; high dielectric constant and good insulation properties; low thermal conductivity and good flame retardancy, high temperature and low temperature resistance; good chemical stability, acid and alkali resistance and strong corrosion resistance; high sound absorption coefficient, strong electromagnetic radiation resistance and low cost, etc., so it is very suitable for large-scale continuous production.

[0029] A graphene layer is deposited on the surface of the basalt fiber cloth substrate in a vertical growth manner; the graphene layer is composed of vertically shaped graphene sheets.

[0030] In this embodiment, the sample image of the three-dimensional graphene basalt fiber composite material can be referenced. Figure 1 (b), such as Figure 1 As shown in (b), the surface of the three-dimensional graphene basalt fiber composite material loses the metallic luster of the basalt fiber and turns pure black.

[0031] In this embodiment, the surface scanning electron microscope images of the three-dimensional graphene basalt fiber composite material at different magnifications can be referenced. Figure 2 (The left side is magnified 10,000 times, and the right side is magnified 5,000 times), from Figure 2 As can be seen, the vertical graphene sheets on the basalt fiber cloth substrate form a three-dimensional structure. The diameter and density of the vertical graphene sheets are related to the CVD process. In this embodiment, specifically, the diameter of the vertical graphene sheets is between 200 nm and 1000 nm, and the thickness is less than 10 nm.

[0032] In this embodiment, the three-dimensional graphene basalt fiber composite material can be prepared by PECVD tube furnace. For example... Figure 3 As shown, the preparation process is described in detail below: Step S1: Clean and dry the basalt fiber cloth, cut and shape the dried basalt fiber cloth, push it into the furnace tube prepared by PECVD tube furnace, and seal the furnace body.

[0033] Specifically, step S1 includes: S11, the basalt fiber cloth was cleaned with deionized water and ethanol in sequence.

[0034] The cleaning time can be set according to actual needs, such as about 5 minutes.

[0035] S12, put the cleaned basalt fiber cloth into the drying oven for drying.

[0036] The drying temperature can be set to around 80℃.

[0037] S13. Cut the dried basalt fiber cloth into a barrel shape, wind it into a circle the same size as the inner wall of the barrel, support the inside of the barrel with a quartz ring, fix it on a quartz boat, push it into the furnace tube, and seal the furnace body.

[0038] In this embodiment, since basalt fiber itself has poor thermal conductivity, it is placed against the hot wall of the quartz ring, which makes it easier for the temperature of the basalt fiber cloth substrate to reach the target reaction temperature set by the furnace, thereby improving the growth efficiency of the graphene layer.

[0039] Step S2: In a PECVD tube furnace, using the basalt fiber as a substrate, argon, reducing gas and gaseous carbon source are introduced to carry out the reaction; wherein, during the reaction, the electric field direction of the plasma in the PECVD tube furnace is perpendicular to the basalt fiber cloth, and graphene layer is grown perpendicularly along the electric field direction. In this embodiment, specifically, the surface of the basalt fiber cloth needs to be treated before the reaction. The treatment process is as follows: The vacuum level is evacuated to a pressure of 10-200 Pa.

[0040] Argon gas is introduced at 10-100 sccm, and reducing gas is introduced at 1-100 sccm.

[0041] Start the plasma in the PECVD tube furnace, starting the power from 100W and gradually adjusting it to 200W. Clean for 10-30 minutes, then turn off the plasma.

[0042] In this embodiment, after the surface treatment of the basalt fiber cloth is completed, the next step of the deposition reaction can be carried out. The reaction process is as follows: Argon gas is introduced and the temperature is gradually increased to the target reaction temperature T1.

[0043] Specifically, the target reaction temperature T1 is 400-700℃.

[0044] Maintain the target reaction temperature T1 for a preset time, and during the temperature holding period: turn off argon gas charging, and charge reducing gas at 1-100 sccm; charge gaseous carbon source, and slowly increase the charging rate from 0 to 1-100 sccm; start plasma, with a power of 150W-500W, and the electric field direction is perpendicular to the surface of basalt fiber cloth.

[0045] In this embodiment, the plasma serves two purposes: firstly, it controls the growth direction of the graphene layer. Because the electric field generated by the plasma is automatically perpendicular to the substrate surface, a graphene layer perpendicular to the surface of the basalt fiber cloth can be grown. Secondly, it effectively decomposes the gaseous carbon source, lowering the chemical reaction barrier and allowing the entire reaction system to undergo carbon source decomposition at a lower temperature. For example, in this embodiment, by using plasma, the target reaction temperature T1 can be controlled at 400-700℃, which is lower than the melting temperature of the basalt fiber cloth.

[0046] Specifically, the preset time is 10-60 minutes, the gaseous carbon source includes methane, ethane, propane, acetylene, and ethanol, and the reducing gas is hydrogen.

[0047] Step S3: After the reaction is complete, cool down and open the furnace to obtain a three-dimensional graphene basalt fiber composite material.

[0048] The process can be configured to shut down the plasma and remove the three-dimensional graphene basalt fiber composite material after cooling to 200°C.

[0049] In this embodiment, the three-dimensional graphene basalt fiber composite material prepared based on the above preparation method has excellent photothermal properties, electrothermal properties, as well as superhydrophobic and ice-repellent properties.

[0050] The photothermal properties, electrothermal properties, superhydrophobic properties, and ice-repellent properties of the three-dimensional graphene basalt fiber composite material of the present invention will be illustrated below with some more detailed embodiments.

[0051] The present invention provides the following embodiments and comparative examples for comparative illustration.

[0052] Example 1 In this embodiment, the gaseous carbon source is methane with a flow rate of 10 sccm, the reducing gas is hydrogen with a flow rate of 20 sccm, and the target reaction temperature T1 is set to 700℃. After the reaction, a graphene basalt fiber composite material is obtained.

[0053] Example 2 In this embodiment, the substrate is a basalt fiber cloth substrate, the gaseous carbon source is methane with a flow rate of 20 sccm, the reducing gas is hydrogen with a flow rate of 10 sccm, and the target reaction temperature T1 is set to 650℃.

[0054] Example 3 In this embodiment, the gaseous carbon source is methane with a flow rate of 100 sccm, the reducing gas is hydrogen with a flow rate of 50 sccm, and the target reaction temperature T1 is set to 600℃.

[0055] Comparative Example 1 This comparative example is raw basalt fiber cloth that has not undergone CVD deposition.

[0056] Comparative Example 2a The substrate selected for this comparative example is quartz fiber cloth, and all other process parameters are the same as those in Example 1.

[0057] Comparative Example 3a The substrate selected for this comparative example is a pure copper mesh, and all other process parameters are the same as those in Example 1.

[0058] Comparative Example 2b The substrate selected for this comparative example is quartz fiber cloth, and all other process parameters are the same as those in Example 2.

[0059] Comparative Example 3b The substrate selected for this comparative example is a pure copper mesh, and all other process parameters are the same as in Example 2.

[0060] First, the growth of the graphene layer on the basalt fiber cloth substrate was verified: like Figure 4 As shown, Figure 4 The images show the surface Raman spectra of the three-dimensional graphene-basalt fiber composite materials prepared in Examples 1-3 above. The surface Raman spectra indicate that graphene layers were grown on basalt fiber cloth substrates in all three examples. Furthermore, according to I... D / I G The proportions of the defect concentrations in the graphene layers are: Example 1 < Example 2 < Example 3.

[0061] In addition, from Figure 2 It can be seen that the graphene layer grows vertically on the basalt fiber cloth substrate.

[0062] Next, the photothermal effects of Example 1 and the comparative example are compared: Table 1 shows a comparison of the photothermal effects of Example 1, Comparative Example 1, Comparative Example 2a, and Comparative Example 3a: Table 1: Comparison of photothermal effects between Example 1 and the comparative example

[0063] like Figure 5 As shown, Figure 5 This is a comparison chart of the photothermal performance of Example 1 and Comparative Examples 1, 2a, and 3a. Figure 5 Table 1 shows that, compared to Comparative Example 1, Comparative Example 2a, and Comparative Example 3a, Example 1 exhibits a stronger and faster photothermal response: at 100 mW / cm 2 Under simulated sunlight (1 Sun) illumination, Example 1 took only 30 seconds to rise from room temperature (22°C) to 67°C, and the temperature stabilized at around 81.3°C after 5 minutes of illumination; at 155 mW / cm 2 Under simulated sunlight (1.5 Sun) illumination, the front side only takes 30 seconds to rise from room temperature (22℃) to 90℃, and the temperature stabilizes at around 105.5℃ after 5 minutes. Its heating rate and heating capacity are significantly higher than those of the comparative examples.

[0064] Then, the hydrophobic and ice-repellent effects of Example 2 and the comparative example are compared: Table 2 shows a comparison of the hydrophobicity and icing-repellency of Example 2, Comparative Example 1, Comparative Example 2b, and Comparative Example 3b: Table 2: Comparison of hydrophobicity and hydrophobic effect between Example 2 and the comparative example

[0065] As can be seen from Table 2, compared with Comparative Examples 1, 2b, and 3b, Example 2 is more hydrophobic, and only Example 2 exhibits ice-repellent properties (Table 2).

[0066] Specifically, the first is hydrophobicity, such as Figure 6 As shown in (a), compared to the superhydrophilicity of ordinary basalt fiber cloth (i.e., Comparative Example 1), Example 2 exhibits superhydrophobicity: the contact angle measured when 2 microliters of water droplets fall is greater than 150 degrees, and the contact angle measured when 5 microliters of water droplets fall is 149.7 degrees. Although Comparative Examples 2b and 3b also exhibit some hydrophobicity, their contact angles are significantly smaller than those of Example 2, indicating that their hydrophobicity is lower than that of Example 2.

[0067] To verify the ice-repellency, copper cables covered with basalt fiber cloth (Comparative Example 1) and copper cables covered with basalt fiber cloth (Example 2) were glued to the ice surface after being soaked in water at the bottom. After freezing for 24 hours, the copper cables were pushed down at a constant speed using a force gauge, and the change in pushing force over time was recorded. The results are shown in the figure. Figure 6 As shown in (b), combined with the two subsequent photographs of the bottom of the copper cables ( Figure 6 (c) It is very obvious that Example 2 has strong icing-repellent properties, while Comparative Example 1 has no icing-repellent properties. The same method was used to verify that Comparative Examples 2b and 3b also had no icing-repellent properties.

[0068] Finally, the electrothermal properties were verified: like Figure 7 Example 3 was cut into strips 3.5 cm long and 2 cm wide, with conductive adhesive applied to both sides. A DC voltage was applied, and the surface temperature of Example 2 was tested using an infrared thermal imaging thermometer. The results showed that Example 3 had a higher conductivity and a significant electrothermal effect: when the voltage across the two ends was 20V, the surface temperature of Example 3 was 44℃; when the voltage across the two ends was 99V, the surface temperature of Example 3 could reach 338℃.

[0069] The above comparison shows that the three-dimensional graphene basalt fiber composite material of the present invention has good photothermal properties, superhydrophobicity, icing-repellency, and electrothermal properties. These properties enable the three-dimensional graphene basalt fiber composite material of the present invention to have more application scenarios. For example, because this embodiment has good photothermal properties, it can be applied to textiles to achieve a heat preservation effect by converting absorbed light into heat or by absorbing infrared radiation emitted by the human body and converting it into heat to achieve an active heat preservation effect.

[0070] For example, due to the photothermal, electrothermal, superhydrophobic, and icing-repellent properties of this embodiment, it simultaneously possesses the capabilities of active icing (active icing is the melting of surface ice and snow caused by photothermal or electrothermal processes) and passive icing (making it difficult for ice to adhere through the material's own special physical or chemical properties, such as low surface energy and special microstructure). Therefore, it is expected to be applied in de-icing facilities, photothermal (electrothermal) systems (seawater desalination, brine desalination, wastewater treatment), and photothermal (electrothermal) housing heating. It can also be applied to the surfaces of products with high icing-repellent requirements, such as the leading edge of aircraft wings, engine air intake lips, wind turbine blades, power transmission lines and towers, ships, and rearview mirrors and antennas of automobiles.

[0071] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the invention by those skilled in the art. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the invention should be included within the scope of protection of the invention.

Claims

1. A three-dimensional graphene-basalt fiber composite material, characterized in that, include: Basalt fiber cloth substrate; A graphene layer is deposited on the surface of the basalt fiber cloth substrate in a vertical growth manner; the graphene layer is composed of vertical graphene sheets with a diameter between 200 nm and 1000 nm and a thickness of less than 10 nm.

2. The three-dimensional graphene basalt fiber composite material according to claim 1, characterized in that, The three-dimensional graphene basalt fiber composite material is prepared by PECVD tube furnace; wherein the direction of the electric field emitted by the plasma of the PECVD tube furnace is perpendicular to the surface of the basalt fiber cloth substrate, thereby vertically growing the graphene layer on the basalt fiber cloth substrate.

3. The three-dimensional graphene basalt fiber composite material according to claim 1, characterized in that, The three-dimensional graphene basalt fiber composite material has a strength of 100 mW / cm². 2 Under simulated sunlight, the front side with the graphene layer formed took 30 seconds to rise from room temperature of 22°C to 67°C, and the temperature stabilized at 81.3°C after 5 minutes of illumination. Under simulated sunlight of 155 mW / cm2, the front side took 30 seconds to rise from room temperature of 22°C to 90°C, and the temperature stabilized at 105.5°C after 5 minutes.

4. The three-dimensional graphene basalt fiber composite material according to claim 1, characterized in that, The contact angle of the three-dimensional graphene basalt fiber composite material was greater than 150 degrees when 2 microliters of water were dropped, and 149.7 degrees when 5 microliters of water were dropped.

5. A method for preparing a three-dimensional graphene basalt fiber composite material as described in any one of claims 1 to 4, characterized in that, include: Step S1: Clean and dry the basalt fiber cloth, cut, shape and fix the dried basalt fiber cloth, push it into the furnace tube prepared by PECVD tube furnace, and seal the furnace body; Step S2: In a PECVD tube furnace, using the basalt fiber as a substrate, argon, reducing gas and gaseous carbon source are introduced to carry out the reaction; wherein, during the reaction, the electric field direction of the plasma in the PECVD tube furnace is perpendicular to the basalt fiber cloth, and graphene layer is grown perpendicularly along the electric field direction. Step S3: After the reaction is complete, cool down and open the furnace to obtain a three-dimensional graphene basalt fiber composite material.

6. The method for preparing a three-dimensional graphene basalt fiber composite material according to claim 5, characterized in that, Step S1 specifically includes: The basalt fiber cloth was cleaned with deionized water and ethanol in turn. The cleaned basalt fiber cloth is placed in an oven to dry; The dried basalt fiber cloth is cut into a barrel shape, wound into a circle the same size as the inner wall of the barrel, supported by a quartz ring inside the barrel, fixed on a quartz boat, pushed into the furnace tube, and the furnace body is sealed.

7. The method for preparing a three-dimensional graphene basalt fiber composite material according to claim 5, characterized in that, The reaction also includes: The surface of basalt fiber cloth is subjected to plasma treatment, the treatment process of which is as follows: Evacuate the vacuum to a pressure of 10-200 Pa; Fill with argon gas at 10-100 sccm and reducing gas at 1-100 sccm; Start the plasma, starting with a power of 100W and gradually adjusting it to 200W. Clean for 10-30 minutes, then turn off the plasma.

8. The method for preparing a three-dimensional graphene basalt fiber composite material according to claim 5, characterized in that, Step S2 specifically includes: Argon gas is introduced and the temperature is gradually increased to the target reaction temperature T1; Maintain the target reaction temperature T1 for a preset time, and during the temperature holding period: turn off argon gas charging, and charge reducing gas at a flow rate of 1-100 sccm; charge gaseous carbon source, and slowly increase the charging rate from 0 to 1-100 sccm; start plasma with a power of 150W-500W, and the electric field direction is perpendicular to the surface of basalt fiber cloth.

9. The method for preparing a three-dimensional graphene basalt fiber composite material according to claim 5, characterized in that, The gaseous carbon source includes methane, ethane, propane, acetylene, and ethanol, and the reducing gas is hydrogen.

10. The method for preparing a three-dimensional graphene basalt fiber composite material according to claim 8, characterized in that, The target reaction temperature T1 is 400-700℃, and the preset time is 10-60 minutes.

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