A nano-bamboo joint-nanowire dual-component composite film and a preparation method thereof

Abstract

The application discloses a kind of nano bamboo joint-nanowire dual-component composite film and preparation method thereof, comprising the following steps: 1) poly-silazane, ferrocene and xylene are uniformly mixed, and solution A is obtained;2) after solidification, again ground into powder B;3) powder B is laid in substrate, and then heat treatment is carried out, after cooling, sample C is obtained;4) sample C is placed in chemical vapor deposition furnace, after heating, natural gas and argon are introduced, and then heat preservation is carried out, and sample D is obtained;5) tetraethyl orthosilicate, anhydrous ethanol and deionized water are uniformly mixed, and then pH value is adjusted, to obtain solution E;6) sample D is immersed in solution E and soaked, and then dried to obtain sample F;7) sample F is heat treated to obtain sample G;8) sample G is oxidized to obtain nano bamboo joint-nanowire dual-component composite film, and the fire-resistant film prepared by the method has a longer fire-resistant time at 1000 DEG C.

Description

Technical Field

[0001] This invention relates to a refractory film and its preparation method, specifically to a nano-bamboo joint-nanowire bicomponent composite film and its preparation method. Background Technology

[0002] Refractory materials can slow the spread of fire, providing valuable time for fire suppression. Flexible refractory films can be easily bent and folded, enabling them to accommodate complex circuit component structures and irregularly shaped parts, providing comprehensive and reliable fire protection. Therefore, flexible refractory insulation materials are increasingly attracting the attention of researchers in fields such as fire protection and electronic circuits. Currently, researchers have prepared flexible refractory films with preliminary fire-resistant and heat-insulating effects. However, existing refractory films are generally composed of single-phase nanowires, and due to differences in nanowire preparation temperatures, it is often difficult to achieve a composite of bicomponent nanostructures. Therefore, the preparation of refractory films with bicomponent nanowires is of great significance. Silicon nitride and silicon carbide nanowires, with their low coefficient of thermal expansion, excellent thermal stability, and good chemical stability, have become ideal materials for preparing bicomponent nanowire refractory films.

[0003] Reference 1, "Y. Liu, L. Zhang, R. Zhang, S. Shao, L. Sun, X. Wan, T. Wang, Thermalinsulating and fire-retardant Si3N4 nanowire membranes resistant to high temperatures up to 1300℃, Journal of Materials Science & Technology, 155(2023)82-88," reports a high-temperature resistant and heat-insulating single silicon nitride nanowire refractory film. This film can withstand a temperature of 1000 degrees Celsius for 20 seconds.

[0004] Reference 2, "F.-F. Chen, Y.-J. Zhu, Z.-C. Xiong, T.-W. Sun, Y.-Q. Shen, Highly Flexible Superhydrophobic and Fire-Resistant Layered Inorganic Paper, ACS Applied Materials & Interfaces, 8(2016) 34715-34724," reports a single hydroxyapatite nanowire flame-retardant paper with fire-resistant properties. This flame-retardant paper can withstand a high temperature of 650 degrees Celsius for 5 minutes.

[0005] Reference 3, “S.He,K.Li,Q.Liu,S.Gu,Q.Song,Flexible SiC-nanowire membrane reinforced pyrocarbon profiled joints with significantly improved thermal shock resistance,Ceramics International,45(2019)2241-2249,” reports a flexible silicon carbide nanowire membrane with a single silicon carbide nanowire.

[0006] The above literature has prepared nanoscale refractory materials, but the above refractory materials only use one type of nanowire and do not achieve the composite of two-phase nanowires, and the refractory time at 1000℃ is relatively short. Summary of the Invention

[0007] The purpose of this invention is to overcome the shortcomings of the prior art and provide a nano-bamboo joint-nanowire bicomponent composite film and its preparation method. The refractory film prepared by this method has a long refractory time at 1000℃.

[0008] To achieve the above objectives, this invention discloses a method for preparing a nano-bamboo joint-nanowire bicomponent composite thin film, comprising the following steps:

[0009] 1) Mix polysilazane, ferrocene and xylene evenly to obtain solution A;

[0010] 2) Allow solution A to stand and solidify, then grind it into powder B;

[0011] 3) Spread powder B evenly on the substrate, then perform heat treatment, and after cooling, peel the product off the substrate surface to obtain sample C;

[0012] 4) Place sample C in a chemical vapor deposition furnace, heat it up, then introduce natural gas and argon gas, and then keep it at the temperature to obtain sample D;

[0013] 5) Mix tetraethyl orthosilicate, anhydrous ethanol and deionized water evenly, and then adjust the pH value to obtain solution E;

[0014] 6) Immerse sample D in solution E, then dry it to obtain sample F;

[0015] 7) Heat-treat sample F to obtain sample G;

[0016] 8) Sample G was oxidized to obtain a nano-bamboo joint-nanowire bicomponent composite film.

[0017] In step 1), the mass ratio of polysilazane to ferrocene is (7-10):1, and the volume ratio of xylene to polysilazane is (2-5):1.

[0018] The substrate is U-shaped graphite paper.

[0019] The specific process of heat treatment in step 3) is as follows: heat treatment in a high-temperature furnace for 2-4 hours, wherein the temperature during the heat treatment process is 1350℃-1550℃ and the nitrogen pressure is 0.10MPa-0.30MPa.

[0020] The specific operation of step 4) is as follows:

[0021] Sample C was placed in a chemical vapor deposition furnace and heated to 1000℃-1100℃. Natural gas was then introduced at a flow rate of (0.6-1) L / min, and argon gas was introduced at a flow rate of (2.2-2.6) L / min. The mixture was then kept at this temperature for 1-3 hours to obtain sample D.

[0022] In step 5), the pH is adjusted to 4-6 using hydrochloric acid solution.

[0023] In step 5), the mass ratio of tetraethyl orthosilicate to anhydrous ethanol is (2-5):1, and the mass ratio of anhydrous ethanol to deionized water is (1-4):1.

[0024] The soaking time in step 6) is 4-7 hours.

[0025] The specific operation of step 7) is as follows:

[0026] Sample F was placed in a high-temperature furnace for heat treatment for 1-4 hours to obtain sample G. The temperature during the heat treatment process was 1500℃-1700℃, and the argon gas pressure was 0.10MPa-0.30MPa.

[0027] The specific operation of step 8) is as follows:

[0028] Sample G was placed in an oxidation furnace at 500℃-800℃ and oxidized in air for 1-3 hours. After cooling, a nano-bamboo joint-nanowire bicomponent composite film was obtained.

[0029] This invention discloses a nano-bamboo joint-nanowire bicomponent composite film, which is prepared based on the preparation method of the nano-bamboo joint-nanowire bicomponent composite film.

[0030] The present invention has the following beneficial effects:

[0031] The present invention describes a nano-bamboo joint-nanowire bicomponent composite film and its preparation method. Specifically, a silicon nitride nanowire film is used as the substrate. A carbon layer is introduced through chemical vapor deposition, a silicon source is introduced using a sol-gel method, and silicon carbide nano-bamboo joints are prepared through high-temperature treatment. Finally, excess carbon layers are removed through oxidation treatment, thereby preparing a refractory film with a dual-phase nanostructure of silicon carbide nano-bamboo joints and silicon nitride nanowires, achieving the composite preparation of bicomponent nanowires. It should be noted that the core of this invention lies in: a) the design of the carbon layer. Without the carbon layer, the silicon carbide nano-bamboo joint-silicon nitride nanowire bicomponent composite cannot be achieved, and a bicomponent film cannot be obtained. The carbon layer's function is to withstand the high temperature of 1500℃-1700℃ during the high-temperature synthesis of the silicon carbide nano-bamboo joints, protecting the silicon nitride nanowires and preventing high-temperature damage; b) the high-temperature oxidation treatment process of 500℃-800℃. Without this high-temperature oxidation treatment process, a rigid material is obtained instead of a film. The principle of high-temperature oxidation treatment is that the carbon layer oxidizes into carbon dioxide and carbon monoxide at high temperatures, causing the carbon layer to lose its rigidity. Simultaneously, this temperature does not reach the damage temperature of silicon carbide nano-stripes and silicon nitride nanowires, thus not affecting their morphology and microstructure. The performance characteristics of the bicomponent refractory film are: it can withstand 1000℃ for up to 1200 seconds without damage, representing a 60-fold improvement over the maximum high-temperature resistance test results of existing technologies; it can achieve a minimum insulation temperature of 450℃ for a 670℃ alcohol lamp; the maximum temperature difference between the front and back of the refractory film is 220℃, and the temperature reduction can reach up to 32%. Attached Figure Description

[0032] Figure 1 Optical image of the nano-bamboo joint-nanowire bicomponent composite film prepared in Example 3;

[0033] Figure 2 The phase diagram is shown for the nano-bamboo joint-nanowire bicomponent composite film prepared in Example 3.

[0034] Figure 3 This is a transmission electron microscope (TEM) image of the nano-bamboo joint-nanowire bicomponent composite film prepared in Example 3;

[0035] Figure 4 Optical image of the nano-bamboo joint-nanowire bicomponent composite film prepared in Example 3 after a 1000°C fire resistance test for 1200 seconds;

[0036] Figure 5 Optical image of the nano-bamboo joint-nanowire bicomponent composite film prepared in Example 3 for thermal insulation testing;

[0037] Figure 6 Optical image of the unsuccessful fabrication of the nano-bamboo joint-nanowire bicomponent composite film in Example 5;

[0038] Figure 7 Example 6 failed to successfully prepare a nano-bamboo joint-nanowire bicomponent composite film, and the final result was an optical image of a rigid material. Detailed Implementation

[0039] To enable those skilled in the art to better understand the present invention, 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 merely some embodiments of the present invention, not all embodiments, and are not intended to limit the scope of the present invention. Furthermore, in the following description, descriptions of well-known structures and technologies are omitted to avoid unnecessary confusion regarding the concepts disclosed in the present invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort should fall within the scope of protection of the present invention.

[0040] The accompanying drawings show structural schematic diagrams according to embodiments disclosed in this invention. These drawings are not drawn to scale, and some details have been enlarged for clarity, and some details may have been omitted. The shapes of the various regions and layers shown in the drawings, as well as their relative sizes and positional relationships, are merely exemplary and may deviate from reality due to manufacturing tolerances or technical limitations. Furthermore, those skilled in the art can design regions / layers with different shapes, sizes, and relative positions as needed.

[0041] The preparation method of the nano-bamboo joint-nanowire bicomponent composite film of the present invention includes the following steps:

[0042] 1) Mix polysilazane, ferrocene and xylene uniformly to obtain solution A, wherein the mass ratio of polysilazane to ferrocene is (7-10):1, and the volume ratio of xylene to polysilazane is (2-5):1;

[0043] 2) Let solution A stand for 5-7 days to solidify, then grind it into powder B in a mortar;

[0044] 3) Spread powder B evenly in U-shaped graphite paper, and then place it in a high-temperature furnace for heat treatment for 2-4 hours. The temperature during the heat treatment process is 1350℃-1550℃, and the nitrogen pressure is 0.10MPa-0.30MPa. Then cool it with the furnace, and then peel the product off the surface of the U-shaped graphite paper to obtain sample C.

[0045] 4) Place sample C in a chemical vapor deposition furnace, heat it to 1000℃-1100℃, then introduce natural gas at a flow rate of (0.6-1) L / min and argon at a flow rate of (2.2-2.6) L / min, and then keep it at this temperature for 1-3 hours to obtain sample D.

[0046] 5) Mix tetraethyl orthosilicate, anhydrous ethanol and deionized water evenly, then adjust the pH value to 4-6 with hydrochloric acid solution, stir evenly to obtain solution E, wherein the mass ratio of tetraethyl orthosilicate to anhydrous ethanol is (2-5):1, and the mass ratio of anhydrous ethanol to deionized water is (1-4):1.

[0047] 6) Immerse sample D in solution E for 4-7 hours, then place it in a drying oven to dry, thus obtaining sample F;

[0048] 7) Place sample F in a high-temperature furnace for heat treatment for 1-4 hours to obtain sample G. The temperature during the heat treatment process is 1500℃-1700℃, and the argon gas pressure is 0.10MPa-0.30MPa.

[0049] 8) Place sample G in an oxidation furnace at 500℃-800℃ and oxidize it in air for 1-3 hours. After cooling, a nano-bamboo joint-nanowire bicomponent composite film is obtained.

[0050] Example 1

[0051] The operation process in this embodiment is as follows:

[0052] 1) Mix polysilazane, ferrocene and xylene uniformly to obtain solution A, wherein the mass ratio of polysilazane to ferrocene is 7:1 and the volume ratio of xylene to polysilazane is 2:1.

[0053] 2) Let solution A stand for 5 days to solidify, then grind it into powder B in a mortar;

[0054] 3) Spread powder B evenly in U-shaped graphite paper, and then place it in a high-temperature furnace for heat treatment for 2 hours. The temperature during the heat treatment process is 1350℃ and the nitrogen pressure is 0.10MPa. Then cool it with the furnace, and then peel the product off the surface of the U-shaped graphite paper to obtain sample C.

[0055] 4) Place sample C in a chemical vapor deposition furnace, heat it to 1000℃, then introduce natural gas at a flow rate of 0.6 L / min and argon at a flow rate of 2.2 L / min, and then hold it at this temperature for 1 hour to obtain sample D;

[0056] 5) Mix tetraethyl orthosilicate, anhydrous ethanol and deionized water evenly, then adjust the pH value to 4 with hydrochloric acid solution, and stir evenly to obtain solution E, wherein the mass ratio of tetraethyl orthosilicate to anhydrous ethanol is 2:1 and the mass ratio of anhydrous ethanol to deionized water is 1:1.

[0057] 6) Immerse sample D in solution E for 4 hours, then dry it in a drying oven to obtain sample F;

[0058] 7) Sample F was placed in a high-temperature furnace for heat treatment for hours to obtain sample G, wherein the temperature during the heat treatment process was 1500℃ and the argon gas pressure was 0.10MPa;

[0059] 8) Place sample G in an oxidation furnace at 500℃ and oxidize it in air for 1 hour. After cooling, a nano-bamboo joint-nanowire bicomponent composite film is obtained.

[0060] Example 1 successfully prepared a nano-bamboo joint-nanowire bicomponent composite film. It achieved no damage after withstanding 1000 degrees Celsius for 1000 seconds. It also achieved a 550-degree Celsius insulation level from a 670-degree Celsius alcohol lamp, with a temperature difference of 120 degrees Celsius between the front and back sides of the refractory film, representing an 18% temperature reduction.

[0061] Example 2

[0062] The specific operation of this embodiment is as follows:

[0063] 1) Mix polysilazane, ferrocene and xylene uniformly to obtain solution A, wherein the mass ratio of polysilazane to ferrocene is 10:1 and the volume ratio of xylene to polysilazane is 5:1.

[0064] 2) Let solution A stand for 7 days to solidify, then grind it into powder B in a mortar;

[0065] 3) Spread powder B evenly in U-shaped graphite paper, and then place it in a high-temperature furnace for heat treatment for 4 hours. The temperature during the heat treatment process is 1550℃ and the nitrogen pressure is 0.30MPa. Then cool it with the furnace, and then peel the product off the surface of the U-shaped graphite paper to obtain sample C.

[0066] 4) Place sample C in a chemical vapor deposition furnace, heat it to 1100℃, then introduce natural gas at a flow rate of 1L / min and argon at a flow rate of 2.6L / min, and then hold it at this temperature for 3 hours to obtain sample D.

[0067] 5) Mix tetraethyl orthosilicate, anhydrous ethanol and deionized water evenly, then adjust the pH value to 6 with hydrochloric acid solution, and stir evenly to obtain solution E, wherein the mass ratio of tetraethyl orthosilicate to anhydrous ethanol is 5:1 and the mass ratio of anhydrous ethanol to deionized water is 4:1.

[0068] 6) Immerse sample D in solution E for 7 hours, then dry it in a drying oven to obtain sample F;

[0069] 7) Sample F was placed in a high-temperature furnace for heat treatment for 4 hours to obtain sample G. The temperature during the heat treatment process was 1700℃ and the argon gas pressure was 0.30MPa.

[0070] 8) Place sample G in an oxidation furnace at 800℃ and oxidize it in air for 3 hours. After cooling, a nano-bamboo joint-nanowire bicomponent composite film is obtained.

[0071] Example 2 successfully prepared a nano-bamboo joint-nanowire bicomponent composite film. It achieved resistance to 1000°C for 1100 seconds without damage. It also achieved a 510°C insulation performance against a 670°C alcohol lamp, with a temperature difference of 160°C between the front and back sides of the refractory film, representing a 24% temperature reduction.

[0072] Example 3

[0073] The operation process in this embodiment is as follows:

[0074] 1) Mix polysilazane, ferrocene and xylene uniformly to obtain solution A, wherein the mass ratio of polysilazane to ferrocene is 9:1 and the volume ratio of xylene to polysilazane is 4:1.

[0075] 2) Let solution A stand for 6 days to solidify, then grind it into powder B in a mortar;

[0076] 3) Spread powder B evenly in U-shaped graphite paper, and then place it in a high-temperature furnace for heat treatment for 3 hours. The temperature during the heat treatment process is 1450℃ and the nitrogen pressure is 0.20MPa. Then cool it with the furnace, and then peel the product off the surface of the U-shaped graphite paper to obtain sample C.

[0077] 4) Place sample C in a chemical vapor deposition furnace, heat it to 1070℃, then introduce natural gas at a flow rate of 0.8 L / min and argon at a flow rate of 2.4 L / min, and then hold it at this temperature for 2 hours to obtain sample D;

[0078] 5) Mix tetraethyl orthosilicate, anhydrous ethanol and deionized water evenly, then adjust the pH value to 5 with hydrochloric acid solution, and stir evenly to obtain solution E, wherein the mass ratio of tetraethyl orthosilicate to anhydrous ethanol is 2:1, and the mass ratio of anhydrous ethanol to deionized water is 1.5:1.

[0079] 6) Immerse sample D in solution E for 6 hours, then dry it in a drying oven to obtain sample F;

[0080] 7) Sample F was placed in a high-temperature furnace for heat treatment for 2 hours to obtain sample G. The temperature during the heat treatment process was 1600℃ and the argon gas pressure was 0.20MPa.

[0081] 8) Place sample G in an oxidation furnace at 600℃ and oxidize it in air for 2 hours. After cooling, a nano-bamboo joint-nanowire bicomponent composite film is obtained.

[0082] refer to Figures 1 to 5Example 3 successfully prepared a nano-bamboo joint-nanowire bicomponent composite film. It achieved resistance to 1000 degrees Celsius for 1200 seconds without damage. It also achieved a 450-degree Celsius insulation level from a 670-degree Celsius alcohol lamp, with a temperature difference of 220 degrees Celsius between the front and back sides of the refractory film, representing a 32% temperature reduction.

[0083] Example 4

[0084] The operation process in this embodiment is as follows:

[0085] 1) Mix polysilazane, ferrocene and xylene uniformly to obtain solution A, wherein the mass ratio of polysilazane to ferrocene is 8:1 and the volume ratio of xylene to polysilazane is 3:1.

[0086] 2) Let solution A stand for 7 days to solidify, then grind it into powder B in a mortar;

[0087] 3) Spread powder B evenly in U-shaped graphite paper, and then place it in a high-temperature furnace for heat treatment for 2.5 hours. The temperature during the heat treatment process is 1500℃ and the nitrogen pressure is 0.25MPa. Then cool it with the furnace, and then peel the product off the surface of the U-shaped graphite paper to obtain sample C.

[0088] 4) Place sample C in a chemical vapor deposition furnace, heat it to 1050℃, then introduce natural gas at a flow rate of 0.7 L / min and argon at a flow rate of 2.5 L / min, and then hold it at this temperature for 1.5 hours to obtain sample D;

[0089] 5) Mix tetraethyl orthosilicate, anhydrous ethanol and deionized water evenly, then adjust the pH value to 6 with hydrochloric acid solution, and stir evenly to obtain solution E, wherein the mass ratio of tetraethyl orthosilicate to anhydrous ethanol is 3:1 and the mass ratio of anhydrous ethanol to deionized water is 2:1.

[0090] 6) Immerse sample D in solution E for 5 hours, then dry it in a drying oven to obtain sample F;

[0091] 7) Sample F was placed in a high-temperature furnace for heat treatment for 3 hours to obtain sample G. The temperature during the heat treatment process was 1600℃ and the argon gas pressure was 0.25MPa.

[0092] 8) Place sample G in an oxidation furnace at 700℃ and oxidize it in air for 1.5 hours. After cooling, a nano-bamboo joint-nanowire bicomponent composite film is obtained.

[0093] Example 4 successfully prepared a nano-bamboo joint-nanowire bicomponent composite film. It achieved no damage after withstanding 1000 degrees Celsius for 900 seconds. It also achieved a 495-degree Celsius insulation level under a 670-degree Celsius alcohol lamp, with a temperature difference of 175 degrees Celsius between the front and back sides of the refractory film, representing a 26% temperature reduction.

[0094] Example 5

[0095] The operation process in this embodiment is as follows:

[0096] 1) Mix polysilazane, ferrocene and xylene uniformly to obtain solution A, wherein the mass ratio of polysilazane to ferrocene is 9:1 and the volume ratio of xylene to polysilazane is 4:1.

[0097] 2) Let solution A stand for 6 days to solidify, then grind it into powder B in a mortar;

[0098] 3) Spread powder B evenly in U-shaped graphite paper, and then place it in a high-temperature furnace for heat treatment for 3 hours. The temperature during the heat treatment process is 1450℃ and the nitrogen pressure is 0.20MPa. Then cool it with the furnace, and then peel the product off the surface of the U-shaped graphite paper to obtain sample C.

[0099] 4) Mix tetraethyl orthosilicate, anhydrous ethanol and deionized water evenly, then adjust the pH value to 5 with hydrochloric acid solution, and stir evenly to obtain solution D, wherein the mass ratio of tetraethyl orthosilicate to anhydrous ethanol is 2:1, and the mass ratio of anhydrous ethanol to deionized water is 1.5:1.

[0100] 5) Immerse sample C in solution D for 6 hours, then dry it in a drying oven to obtain sample E;

[0101] 6) Sample E was placed in a high-temperature furnace for heat treatment for 2 hours to obtain sample H. The temperature during the heat treatment process was 1600℃ and the argon gas pressure was 0.20MPa. Sample H consisted of scattered fragments.

[0102] Example 5 failed to successfully prepare a nano-bamboo joint-nanowire bicomponent composite film. This example did not fully follow the preparation process proposed in this invention, and therefore could not produce a sample. Because step 4) of the carbon layer design process proposed in this invention was missing, it was also impossible to protect the silicon nitride nanowires at high temperatures, resulting in the inability to prepare a complete film sample; only scattered fragments were obtained, such as... Figure 6 As shown.

[0103] Example 6

[0104] The operation process in this embodiment is as follows:

[0105] 1) Mix polysilazane, ferrocene and xylene uniformly to obtain solution A, wherein the mass ratio of polysilazane to ferrocene is 9:1 and the volume ratio of xylene to polysilazane is 4:1.

[0106] 2) Let solution A stand for 6 days to solidify, then grind it into powder B in a mortar;

[0107] 3) Spread powder B evenly in U-shaped graphite paper, heat treat for 3 hours at a temperature of 1450℃ and a nitrogen pressure of 0.20MPa. After the furnace cools down, peel the product off the surface of the U-shaped graphite paper to obtain sample C.

[0108] 4) Place sample C in a chemical vapor deposition furnace, heat it to 1070℃, then introduce natural gas at a flow rate of 0.8 L / min and argon at a flow rate of 2.4 L / min, and keep it at this temperature for 2 hours to obtain sample D;

[0109] 5) Mix tetraethyl orthosilicate, anhydrous ethanol and deionized water evenly, wherein the mass ratio of tetraethyl orthosilicate to anhydrous ethanol is 2:1 and the mass ratio of anhydrous ethanol to deionized water is 1.5:1. Then adjust the pH of the solution to 5 with hydrochloric acid solution and stir evenly to obtain solution E.

[0110] 6) Immerse sample D in solution E for 6 hours, then dry it in a drying oven to obtain sample F;

[0111] 7) The sample F was heat-treated for 2 hours at a temperature of 1600℃ and an argon pressure of 0.20MPa. The final sample was a rigid material, not a flexible film.

[0112] Example 6 failed to successfully prepare a nano-bamboo joint-nanowire bicomponent composite film. This example did not fully follow the preparation process, and the final result was a rigid material because it lacked step 8) of the oxidation process in air atmosphere proposed in this invention. Therefore, a flexible film could not be prepared, and only a rigid material without flexibility was obtained. Figure 7 As shown.

[0113] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit it. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art should understand that modifications or equivalent substitutions can still be made to the specific implementation of the present invention. Any modifications or equivalent substitutions that do not depart from the spirit and scope of the present invention should be covered within the scope of protection of the claims of the present invention.

Claims

1. A method for preparing a nano-bamboo joint-nanowire bicomponent composite thin film, characterized in that, Includes the following steps: 1) Mix polysilazane, ferrocene, and xylene evenly to obtain solution A; 2) Allow solution A to stand and solidify, then grind it into powder B; 3) Spread powder B evenly on the substrate, then perform heat treatment, and after cooling, peel the product off the substrate surface to obtain the sample silicon nitride nanowire film. 4) The silicon nitride nanowire film sample was placed in a chemical vapor deposition furnace, heated, and then natural gas and argon were introduced. After holding at the temperature, carbon layer design was performed to obtain sample D. 5) Mix tetraethyl orthosilicate, anhydrous ethanol and deionized water evenly, and then adjust the pH value to obtain solution E; 6) Immerse sample D in solution E, then dry it to obtain sample F; 7) Heat-treat sample F to obtain sample G; 8) Sample G was oxidized to obtain a silicon carbide nano-bamboo joint-silicon nitride nanowire bicomponent composite film; The specific operation of step 8) is as follows: Sample G was placed in an oxidation furnace at 500℃-800℃ and oxidized in air for 1-3 hours. After cooling, a nano-bamboo joint-nanowire bicomponent composite film was obtained.

2. The method for preparing the nano-bamboo joint-nanowire bicomponent composite film according to claim 1, characterized in that, In step 1), the mass ratio of polysilazane to ferrocene is (7-10):1, and the volume ratio of xylene to polysilazane is (2-5):

1.

3. The method for preparing the nano-bamboo joint-nanowire bicomponent composite film according to claim 1, characterized in that, The substrate is U-shaped graphite paper.

4. The method for preparing the nano-bamboo joint-nanowire bicomponent composite film according to claim 1, characterized in that, The specific process of heat treatment in step 3) is as follows: heat treatment in a high-temperature furnace for 2-4 hours, wherein the temperature during the heat treatment process is 1350℃-1550℃ and the nitrogen pressure is 0.10 MPa-0.30 MPa.

5. The method for preparing the nano-bamboo joint-nanowire bicomponent composite film according to claim 1, characterized in that, The specific operation of step 4) is as follows: The silicon nitride nanowire film sample was placed in a chemical vapor deposition furnace and heated to 1000℃-1100℃. Natural gas was then introduced at a flow rate of (0.6-1) L / min, and argon gas was introduced at a flow rate of (2.2-2.6) L / min. The temperature was then maintained for 1-3 hours to obtain sample D.

6. The method for preparing the nano-bamboo joint-nanowire bicomponent composite film according to claim 1, characterized in that, In step 5), the pH is adjusted to 4-6 using hydrochloric acid solution; In step 5), the mass ratio of tetraethyl orthosilicate to anhydrous ethanol is (2-5):1, and the mass ratio of anhydrous ethanol to deionized water is (1-4):

1.

7. The method for preparing the nano-bamboo joint-nanowire bicomponent composite film according to claim 1, characterized in that, The soaking time in step 6) is 4-7 hours.

8. The method for preparing the nano-bamboo joint-nanowire bicomponent composite film according to claim 1, characterized in that, The specific operation of step 7) is as follows: Sample F was placed in a high-temperature furnace for heat treatment for 1-4 hours to obtain sample G. The temperature during the heat treatment process was 1500℃-1700℃, and the argon gas pressure was 0.10 MPa-0.30 MPa.

9. A nano-bamboo joint-nanowire bicomponent composite film, characterized in that, It was prepared according to the preparation method of the nano-bamboo joint-nanowire bicomponent composite film according to any one of claims 1-8.

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