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CN-122013136-A - Three-dimensional graphene basalt fiber composite material and preparation method thereof

CN122013136ACN 122013136 ACN122013136 ACN 122013136ACN-122013136-A

Abstract

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

Inventors

  • HU YANLING
  • JIANG YANG
  • JI HUAYU
  • ZHAO BANGHAO
  • LIN YIXIAN
  • ZHANG XUHONG

Assignees

  • 厦门理工学院

Dates

Publication Date
20260512
Application Date
20260205
Priority Date
20260126

Claims (10)

  1. 1. The three-dimensional graphene basalt fiber composite material is characterized by comprising the following components: basalt fiber cloth substrate; the graphene layer is formed by vertical graphene sheets, the diameter of the graphene sheets is between 200 nm and 1000 nm, and the thickness of the graphene sheets is within 10 nm.
  2. 2. The three-dimensional graphene basalt fiber composite material according to claim 1, wherein the three-dimensional graphene basalt fiber composite material is prepared by a PECVD tube furnace, wherein the direction of an electric field emitted by plasma of the PECVD tube furnace is perpendicular to the surface of the basalt fiber cloth substrate, so that the graphene layer is vertically grown on the basalt fiber cloth substrate.
  3. 3. The three-dimensional graphene basalt fiber composite material according to claim 1, wherein the time for the front surface on which the graphene layer is formed to rise from room temperature 22 ℃ to 67 ℃ is 30 seconds under the irradiation of 100 mW/cm 2 simulated sunlight, the temperature is stabilized at 81.3 ℃ after 5 minutes of irradiation, the time for the front surface to rise from room temperature 22 ℃ to 90 ℃ is 30 seconds under the irradiation of 155 mW/cm2 of simulated sunlight, and the temperature is stabilized at 105.5 ℃ after 5 minutes.
  4. 4. The three-dimensional graphene basalt fiber composite of claim 1, wherein the three-dimensional graphene basalt fiber composite has a contact angle measured at 2 microliter drops of water of greater than 150 degrees and a contact angle measured at 5 microliter drops of water of 149.7 degrees.
  5. 5. A method of preparing a three-dimensional graphene basalt fiber composite material according to any one of claims 1 to 4, comprising: step S1, cleaning basalt fiber cloth, drying, cutting, shaping and fixing the dried basalt fiber cloth, pushing the basalt fiber cloth into a furnace tube prepared by a PECVD tube furnace, and sealing the furnace body; Step S2, taking the basalt fiber as a substrate in a PECVD tube furnace, and introducing argon, reducing gas and gaseous carbon source for reaction, wherein in the reaction process, the electric field direction of plasma in the PECVD tube furnace is perpendicular to the basalt fiber cloth, and then a graphene layer is vertically grown along the electric field direction; And step S3, cooling after the reaction is finished, and opening the furnace body to obtain the three-dimensional graphene basalt fiber composite material.
  6. 6. The method for preparing the three-dimensional graphene basalt fiber composite material according to claim 5, wherein the step S1 specifically comprises: sequentially using deionized water and ethanol to clean basalt fiber cloth respectively; placing the cleaned basalt fiber cloth into an oven for drying; Cutting the dried basalt fiber cloth into a barrel shape, winding the basalt fiber cloth into a circle with the same size as the barrel-shaped inner wall, supporting the barrel-shaped inner wall by a quartz ring, fixing the quartz ring on a quartz boat, pushing the quartz boat into a furnace tube, and sealing the furnace body.
  7. 7. The method for preparing the three-dimensional graphene basalt fiber composite material according to claim 5, further comprising, before the reaction: Plasma treatment is carried out on the surface of basalt fiber cloth, wherein the treatment process is as follows: Pumping the vacuum degree to the air pressure of 10-200pa; Filling argon gas with a concentration of 10-100sccm and reducing gas with a concentration of 1-100sccm; the plasma is started, the running power is started from 100W and gradually adjusted to 200W, so that the plasma is turned off after cleaning is carried out for 10-30 min.
  8. 8. The method for preparing the three-dimensional graphene basalt fiber composite material according to claim 5, wherein step S2 specifically comprises: argon is filled, and the temperature is gradually increased to a target reaction temperature T1; maintaining the target reaction temperature T1 for a preset time, closing argon gas filling, filling reducing gas at a filling flow rate of 1-100sccm, filling a gaseous carbon source, slowly increasing the filling speed from 0 to 1-100sccm, starting plasma with power of 150-500W, and enabling the electric field direction to be perpendicular to the surface of the basalt fiber cloth.
  9. 9. The method for preparing the three-dimensional graphene basalt fiber composite material according to claim 5, wherein the gaseous carbon source comprises methane, ethane, propane, acetylene and ethanol, and the reducing gas is hydrogen.
  10. 10. The method for preparing the three-dimensional graphene basalt fiber composite material according to claim 8, wherein the target reaction temperature T1 is 400-700 ℃, and the preset time is 10-60 minutes.

Description

Three-dimensional graphene basalt fiber composite material and preparation method thereof Technical Field The invention relates to the technical field of composite materials, in particular to a three-dimensional graphene basalt fiber composite material and a preparation method thereof. Background By virtue of the characteristics of high carrier mobility, excellent thermal conductivity, mechanical strength and the like, the graphene becomes a research hotspot in the fields of global material science and industry, and the large-scale application of the graphene has important significance in promoting the strategic and emerging industry upgrading of new energy sources, electronic devices and the like. Chemical Vapor Deposition (CVD) technology is considered as the most industrially potential method for preparing graphene because it can prepare large-area, high-quality graphene films. However, the traditional CVD process relies on metals such as copper and nickel as catalytic substrates, and the graphene film with atomic-scale thickness is peeled off and transferred to a target substrate through a complex transfer process, which is easy to cause film pollution, damage and folding, and remarkably deteriorates the electrical and mechanical properties of the graphene film, thus becoming a core bottleneck for limiting the practical application of the graphene film. In order to overcome the problem, liu Zhongfan academy proposes a concept of a super-Mononene material in 2024, namely, a continuous graphene layer ('graphene skin') is grown on the surface of a traditional engineering material in situ, so that the function coordination of graphene and a substrate material is realized, the transfer bottleneck is avoided, and a new path of vectorization is opened up for the industrialized application of the graphene. However, current research on Mononene materials is still focused on specific substrates such as quartz fibers, alumina, and the like. This is because the nonmetallic substrate is less catalytically active and the thermal decomposition of the carbon precursor is promoted by a high temperature (> 1000 ℃) CVD process to grow graphene. Quartz fibers, while resistant to high temperature processing, have severely limited the large-scale application of composite materials at high cost (> 100 yuan per square meter). The basalt fiber is a low-cost inorganic fiber prepared by taking natural basalt ore (SiO 2+Al2O3 is about 70%) as a raw material and carrying out melt wire drawing, has the comprehensive properties of high temperature resistance (-269-700 ℃), high strength, excellent insulativity, corrosion resistance and the like, is rich in raw materials and low in cost, and has market quotation of about 1/10 of that of quartz fiber, thus being an ideal candidate substrate for replacing the quartz fiber. At present, most basalt fiber/graphene composite materials in the market mostly adopt bonding mixtures of graphene oxide powder and basalt fibers, and the bonding force is poor. Some researches, such as a Chinese patent CN 1058197110B, utilize the catalysis of reduced iron atoms on the surface of basalt fiber by means of a CVD technology, crack a carbon source on the surface of basalt fiber at high temperature, grow a graphene film with the thickness of 0.3-100 nm in situ, and the prepared graphene/basalt composite material has the characteristics of high mechanical strength, high conductivity and hydrophobicity, but does not have good photo-thermal effect, and has uncertain superhydrophobic and icephobic capabilities, so that the application of the graphene/basalt composite material is limited. Disclosure of Invention The invention provides a three-dimensional graphene basalt fiber composite material and a preparation method thereof, and aims to improve at least one of the technical problems. In order to solve the technical problems, the invention provides a three-dimensional graphene basalt fiber composite material, which comprises the following components: basalt fiber cloth substrate; The graphene layer is formed by vertical graphene sheets, the diameter of the graphene sheets is between 200 nm and 1000 nm, and the thickness of the graphene sheets is within 10 nm. The three-dimensional graphene basalt fiber composite material is prepared through a PECVD tube furnace, wherein the direction of an electric field emitted by plasma of the PECVD tube furnace is perpendicular to the surface of the basalt fiber cloth substrate, so that the graphene layer is vertically grown on the basalt fiber cloth substrate. Preferably, the three-dimensional graphene basalt fiber composite material has the advantages that under the illumination of 100 mW/cm 2 simulated sunlight, the time for the front surface on which a graphene layer is formed to rise from room temperature 22 ℃ to 67 ℃ is 30 seconds, the temperature is stabilized at 81.3 ℃ after 5 minutes of illumination, under the illumination of 155 mW/cm2 simulated sunlight, the time