CN110938896B - Conductive ceramic fiber based on silicon carbide and preparation method thereof - Google Patents
Conductive ceramic fiber based on silicon carbide and preparation method thereof Download PDFInfo
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- CN110938896B CN110938896B CN201911248767.5A CN201911248767A CN110938896B CN 110938896 B CN110938896 B CN 110938896B CN 201911248767 A CN201911248767 A CN 201911248767A CN 110938896 B CN110938896 B CN 110938896B
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Abstract
The invention discloses a conductive ceramic fiber based on silicon carbide and a preparation method thereof, wherein the conductivity of the conductive ceramic fiber is 102～104S/m, tensile strength of 0.4-2.8 GPa and modulus of 60-280 GPa; the preparation method is carried out continuouslyAnd (3) taking the SiC fiber as a raw material, and heating, preserving heat and cooling under a vacuum condition to obtain the conductive ceramic fiber. The conductive ceramic fiber provided by the invention has excellent conductivity, and simultaneously, the mechanical property of the conductive ceramic fiber can meet the application requirement and has good flexibility; the preparation method provided by the invention has the advantages of wide raw material source, simple preparation process and convenience in operation, and can realize large-scale preparation of the conductive fiber.
Description
Technical Field
The invention relates to the technical field of conductive fibers, in particular to a silicon carbide-based conductive ceramic fiber and a preparation method thereof.
Background
The conductive fiber not only has excellent electrical properties, but also has knittability, and is widely applied in the fields of antistatic, flexible sensors, electromagnetic shielding and the like. Particularly, the rapid development of wearable electronic products in recent years directly promotes the application requirements of the conductive fibers in the field of wearable electronic products.
The conductive fibers may be classified into organic conductive fibers, metal conductive fibers and inorganic non-metal conductive fibers according to their material characteristics. The organic conductive fiber includes various polymer fibers having a pi-conjugated structure in the main chain, such as polypyrrole fibers, polythiophene fibers, polyaniline fibers, and the like. However, the conductive polymer is difficult to synthesize and spin due to a conjugated structure in the main chain of the polymer, and the preparation cost is high. In addition, metal compound, carbon black particles, graphene, carbon nanotubes and other conductive substances can be coated on the surface of common organic fibers or doped in the fibers by methods such as sputtering coating, physical adsorption, chemical reaction, blend spinning and the like to form coating type conductive fibers or composite type conductive fibers. The coating type fiber has good conductivity, but the conductive material on the surface layer of the fiber is easily removed in the post-processing. The composite conductive fiber is easy to cohere and good in processability, is widely used for industrial production, but has poor high-temperature resistance. The metal conductive fiber is formed by preparing metal such as aluminum, copper, silver and the like into a fiber shape by a melting-drawing method, a cutting method, a drawing method and the like, has very excellent conductivity and can approach to pure metal, but the metal conductive fiber has high preparation difficulty and poor processability and is difficult to form conductive fiber with a fine diameter. At present, inorganic nonmetal conductive fibers mainly comprise carbon fibers, have the advantages of excellent conductivity, fine diameter, high strength, wear resistance, corrosion resistance and the like, but have poor oxidation resistance.
Disclosure of Invention
The invention provides a silicon carbide-based conductive ceramic fiber and a preparation method thereof, which are used for overcoming the defects of difficulty in synthesis and spinning, no high temperature resistance, easy falling of conductive substances, poor processability and the like in the prior art, and provide a novel inorganic nonmetal conductive fiber, and meanwhile, the conductive ceramic fiber is low in preparation difficulty and simple in technological process.
In order to achieve the above object, the present invention provides a silicon carbide-based conductive ceramic fiber having a conductivity of 102～104S/m, tensile strength of 0.4-2.8 GPa, and modulus of 60-280 GPa.
In order to achieve the above object, the present invention also provides a method for preparing a silicon carbide-based conductive ceramic fiber, comprising the steps of:
heating the continuous SiC fibers from room temperature to a set temperature at a heating rate of 100-600 ℃/h under a vacuum condition, then preserving heat for 1-5 h at the set temperature, and naturally cooling to obtain the conductive ceramic fibers.
Compared with the prior art, the invention has the beneficial effects that:
1. the conductivity of the conductive ceramic fiber provided by the invention is 102～104S/m, tensile strength of 0.4-2.8 GPa, and modulus of 60-280 GPa. The conductivity of the conductive ceramic fiber provided by the invention can be 102～104The S/m is regulated and controlled in a large range, and meanwhile, the mechanical property of the composite material can meet the application requirement, and the composite material is thin in diameter and good in flexibility.
2. According to the preparation method of the conductive ceramic fiber, the core part of the obtained conductive fiber is silicon carbide, so that the fiber has good high temperature resistance, oxidation resistance, corrosion resistance and other properties. In addition, the preparation method provided by the invention does not damage the cross-sectional shape of the raw material SiC fiber, so that the prepared conductive ceramic fiber also has good appearance.
3. The preparation method of the conductive ceramic fiber provided by the invention has the advantages of wide raw material source, simple preparation process and convenience in operation, and can realize large-scale preparation of the conductive fiber.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a surface scanning electron micrograph of the continuous conductive ceramic fiber prepared in example 5;
FIG. 2 is a scanning electron micrograph of a cross-section of the continuous conductive ceramic fiber prepared in example 5;
fig. 3 is a high-angle annular dark field image, a carbon and silicon elemental distribution diagram of the continuous conductive ceramic fiber powder sample prepared in example 5.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the technical solutions in the embodiments of the present invention may be combined with each other, but it must be based on the realization of those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination of technical solutions should not be considered to exist, and is not within the protection scope of the present invention.
The drugs/reagents used are all commercially available without specific mention.
The invention provides a conductive ceramic fiber based on silicon carbide, which has the conductivity of 102～104S/m, tensile strength of 0.4-2.8 GPa, and modulus of 60-280 GPa.
The invention also provides a preparation method of the conductive ceramic fiber based on the silicon carbide, which comprises the following steps:
heating the continuous SiC fibers from room temperature to a set temperature at a heating rate of 100-600 ℃/h under a vacuum condition, then preserving heat for 1-5 h at the set temperature, and naturally cooling to obtain the conductive ceramic fibers.
Preferably, the oxygen content of the continuous SiC fibers is less than 5wt%, and the proper continuous SiC fibers are selected to ensure that the finally prepared fiber products have excellent performance.
Preferably, the continuous SiC fiber is a continuous SiC fiber doped with Zr, Al, Fe, Ag, Cu, Au, Hf, Re, Nb, B, Ti, N, Ta and/or Ir.
The preparation method can adopt SiC fiber raw materials with different forms, can prepare conductive fibers with corresponding forms, and has wide application range.
Preferably, the continuous SiC fiber has a tensile strength of 1.5GPa or more and a modulus of 260GPa or more. The raw materials with excellent performance are selected to ensure that the obtained conductive ceramic fiber has excellent performance.
Preferably, the set temperature is 1500-1800 ℃. The fiber obtained by controlling the temperature within the range of 1500-1800 ℃ has more excellent conductivity.
Preferably, the vacuum condition refers to the pressure of the environment being less than 50Pa, so as to facilitate the formation of the conductive layer on the surface of the fiber.
Silicon carbide is known as a semiconductor, and thus ceramic fibers of silicon carbide prepared by a precursor conversion method have poor electrical conductivity. The invention improves the conductivity of the silicon carbide fiber through high-temperature heat treatment, so that the silicon carbide fiber becomes a good conductor. Therefore, the invention provides a novel inorganic nonmetal conductive fiber, namely a conductive ceramic fiber based on silicon carbide, which has the advantages of high temperature resistance, oxidation resistance, low density, good flexibility, low preparation difficulty, simple operation and easy realization of industrial production.
Example 1
The embodiment provides a preparation method of a silicon carbide-based conductive ceramic fiber, which comprises the following steps:
placing KD-II type second generation continuous SiC fiber (tensile strength is 2.73GPa, modulus is 290GPa, oxygen content is lower than 3 wt%) in a graphite furnace, vacuumizing, heating from room temperature to 1500 ℃ at the heating rate of 300 ℃/h, then preserving heat for 1h at 1500 ℃, naturally cooling, cooling in the furnace, and taking out the product to obtain the conductive ceramic fiber.
The conductive ceramic fiber prepared in this example had a tensile strength of 2.62GPa, a modulus of 279GPa, and an electrical conductivity of 4.3X 102S/m。
The electrical conductivity of the fibers was measured and calculated by a high resistivity meter. The tensile strength and modulus of the fibers were measured using a universal tester (original tensile length 25 mm).
Example 2
In this embodiment, a method for preparing a silicon carbide-based conductive ceramic fiber is provided, and compared with embodiment 1, the temperature rise and temperature preservation temperature in this embodiment is 1600 ℃, and other processes are the same as those in embodiment 1.
The conductive ceramic fiber prepared in the embodiment has the tensile strength of 2.4GPa, the modulus of 271GPa and the conductivity of 9.2 multiplied by 102S/m。
Example 3
In this embodiment, a method for preparing a silicon carbide-based conductive ceramic fiber is provided, and compared with embodiment 1, the temperature rise and temperature preservation temperature in this embodiment is 1700 ℃, and other processes are the same as those in embodiment 1.
The conductive ceramic fiber prepared in the embodiment has the tensile strength of 2.26GPa, the modulus of 256GPa and the conductivity of 1.6 multiplied by 103S/m。
Example 4
The embodiment provides a preparation method of a silicon carbide-based conductive ceramic fiber, which comprises the following steps:
placing KD-SA type aluminum-containing third-generation continuous SiC fiber (with tensile strength of 2.1GPa, modulus of 360GPa and oxygen content of less than 1 wt%) in a graphite furnace, vacuumizing, heating from room temperature to 1800 ℃ at a heating rate of 100 ℃/h, preserving heat at 1800 ℃ for 1h, naturally cooling, cooling in the furnace, and taking out the product to obtain the conductive ceramic fiber.
The conductive ceramic fiber prepared by the embodiment has the tensile strength of 0.84GPa, the modulus of 208GPa and the conductivity of 1.5 multiplied by 104S/m。
Example 5
The embodiment provides a preparation method of a conductive ceramic fiber based on silicon carbide, compared with embodiment 4, the heat preservation time of the embodiment is 2h, and other processes are the same as embodiment 4.
The conductive ceramic fiber prepared in the embodiment has the tensile strength of 0.57GPa, the modulus of 198GPa and the conductivity of 2.9 multiplied by 104S/m。
Fig. 1 is a scanning electron micrograph of a surface of the continuous conductive ceramic fiber prepared in this example, and fig. 2 is a scanning electron micrograph of a cross-section of the continuous conductive ceramic fiber prepared in this example. As can be seen from fig. 1 and 2, the conductive ceramic fiber has a complete shape, a smooth and uniform surface, and a circular cross section, wherein the dense part of the fiber core mainly comprises silicon carbide, and the loose part close to the surface mainly comprises graphite. Fig. 3 is a high-angle annular dark field image, a carbon and silicon element distribution diagram of the continuous conductive ceramic fiber powder sample prepared in this example, and it can be seen from the figure that the conductive ceramic fiber contains carbon as a main component and a small amount of silicon, and the silicon exists in the form of silicon carbide. It is understood that the high-temperature treatment converts the portion of the raw material SiC fiber near the surface into graphite that can conduct electricity, and therefore, the conductivity of the entire fiber is improved.
Example 6
The embodiment provides a preparation method of a conductive ceramic fiber based on silicon carbide, compared with embodiment 4, the heat preservation time of the embodiment is 5h, and other processes are the same as embodiment 4.
The conductive ceramic fiber prepared in the embodiment has the tensile strength of 0.42GPa, the modulus of 68GPa and the conductivity of 4.3 multiplied by 104S/m。
Comparing examples 1 to 3 and 4 to 6, it can be seen that the higher the heating and heat-insulating temperature and the longer the heat-insulating time, the higher the conductivity of the obtained conductive ceramic fiber, but as the temperature increases, the mechanical properties of the conductive ceramic fiber decrease, so that in order to obtain a conductive ceramic fiber whose mechanical properties and conductive properties meet the application requirements, the heating and heat-insulating temperature and heat-insulating time need to be strictly controlled.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (5)
1. A preparation method of a silicon carbide-based conductive ceramic fiber is characterized by comprising the following steps:
heating the continuous SiC fibers from room temperature to a set temperature at a heating rate of 100-600 ℃/h under a vacuum condition, then preserving heat at the set temperature for 1-5 h, and naturally cooling to obtain the conductive ceramic fibers;
the set temperature is 1500-1800 ℃; the vacuum condition refers to the pressure of the environment being less than 50 Pa; the core part of the conductive ceramic fiber is silicon carbide, and the rest is graphite; the conductive ceramic fiber has a conductivity of 102~104S/m, tensile strength of 0.4-2.8 GPa, and modulus of 60-280 GPa.
2. The method of making electrically conductive ceramic fibers of claim 1 wherein the oxygen content of the continuous SiC fibers is less than 5 wt%.
3. The method of making a conductive ceramic fiber of claim 1 wherein the continuous SiC fiber is Zr, Al, Fe, Ag, Cu, Au, Hf, Re, Nb, B, Ti, N, Ta and/or Ir doped continuous SiC fiber.
4. The method of producing the conductive ceramic fiber according to claim 2 or 3, wherein the continuous SiC fiber has a tensile strength of 1.5 to 2.8GPa and a modulus of 260 to 280 GPa.
5. A silicon carbide-based conductive ceramic fiber produced by the production method according to any one of claims 1 to 4.
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| CN101994169B (en) * | 2010-09-14 | 2014-04-02 | 苏州赛力菲陶纤有限公司 | Continuous silicon carbide fiber preparation method and production device |
| CN105155041B (en) * | 2015-10-20 | 2017-07-07 | 中国人民解放军国防科学技术大学 | A kind of preparation method of the continuous SiC fiber that resistivity can be on a large scale regulated and controled |
| CN105568427B (en) * | 2016-03-01 | 2018-02-02 | 江苏赛菲新材料有限公司 | A kind of high resistivity continuous carbofrax fibre and preparation method thereof |
| CN109456065B (en) * | 2019-01-07 | 2021-05-28 | 中国人民解放军国防科技大学 | Preparation method of SiC ceramic fiber |
| CN110106583B (en) * | 2019-05-24 | 2021-06-11 | 中国人民解放军国防科技大学 | Preparation method of SiC fibers with low boron content |
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