Hollow silicon carbide ceramic fiber as well as preparation method and application thereof

The hollow silicon carbide ceramic fiber is prepared by using cheap silicone resin, which solves the problems of high cost and complex process and realizes the preparation of highly crystalline hollow structure, which is suitable for high-temperature thermal insulation and catalytic adsorption materials.

CN120738801AActive Publication Date: 2025-10-03NAT UNIV OF DEFENSE TECH
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Patent Information

Application Number
CN202511264078.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-09-05
Publication Date
2025-10-03
Estimated Expiration
2045-09-05

AI Technical Summary

Technical Problem

The existing preparation methods of hollow silicon carbide ceramic fibers are costly and complex, making industrial production difficult.

Method used

Using cheap silicone resin as a precursor, hollow silicon carbide ceramic fibers are prepared through melt spinning, thermal crosslinking, thermal decomposition, sintering and decarburization treatment. The spinning diameter and grain growth are controlled to avoid structural collapse and form a highly crystalline hollow structure.

Benefits of technology

The low-cost and simple process for preparing high-crystalline hollow silicon carbide ceramic fibers has been achieved. The fibers are suitable for high-temperature thermal insulation and catalytic adsorption materials, have good mechanical properties, and are suitable for industrial production.

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Abstract

The invention relates to a hollow silicon carbide ceramic fiber as well as a preparation method and application thereof. The preparation method of the hollow silicon carbide ceramic fiber comprises the following steps: carrying out melt spinning on organic silicon resin in an inert atmosphere; carrying out thermal cross-linking curing treatment at a preset temperature; raising the temperature to a preset temperature at a preset temperature raising speed in an inert atmosphere, and carrying out thermal decomposition; raising the temperature to a preset temperature at a preset temperature raising speed in an inert atmosphere, and carrying out sintering treatment to generate a silicon carbide-carbon ceramic composite fiber with a carbon-rich core part; raising the temperature to a preset temperature at a preset temperature raising speed, and carrying out oxidation and decarbonization treatment to ensure that free carbon in the fiber is removed, so as to generate the silicon carbide ceramic fiber with a hollow structure. The preparation method is low in cost and simple in process, and the prepared hollow silicon carbide ceramic fiber is relatively good in mechanical property, and is suitable for the fields of high-temperature thermal insulation materials and catalytic adsorption materials compared with silicon carbide fibers with compact morphology in the prior art.
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Description

Technical Field

[0001] The present invention belongs to the technical field of fiber materials, and in particular relates to a hollow silicon carbide ceramic fiber and a preparation method and application thereof. Background Art

[0002] Silicon carbide fiber has the advantages of high temperature resistance, oxidation resistance, corrosion resistance and good mechanical properties. It also has good compatibility with composite matrices such as metals, ceramics, and polymers. It is an ideal reinforcing material and has broad application prospects in fields such as aerospace and nuclear industry.

[0003] In addition to the aforementioned advantages, silicon carbide hollow ceramic fibers also possess a unique hollow structure and morphology, making them suitable for use as high-temperature thermal insulation materials and catalytic adsorption materials. Current methods for preparing silicon carbide hollow ceramic fibers include: using polycarbosilane as a raw material for precursor blending to produce polymer mixed fibers, followed by high-temperature heat treatment to produce hollow fibers (e.g., patent CN109023590B); using strong oxidants or halogenation reactions to crosslink polycarbosilane fibrils, followed by high-temperature sintering to produce hollow fibers (e.g., CN110117842B, CN108456949B); and customizing fiber spinning spinnerets to control the morphology of polycarbosilane fibrils to produce silicon carbide hollow fibers (e.g., CN2700346 Y). However, these methods are associated with high costs and complex and demanding preparation processes.

[0004] In summary, there is an urgent need to provide a hollow silicon carbide ceramic fiber with low cost and simple process, as well as a preparation method and application thereof. Summary of the Invention

[0005] The purpose of the present invention is to provide a hollow silicon carbide ceramic fiber with low cost and simple process, and a preparation method and application thereof.

[0006] The above object is achieved through the following technical solution: A method for preparing hollow silicon carbide ceramic fiber, comprising the following steps: S1, melt spinning: silicone resin is melted in an inert atmosphere and spun to form polymer fibrils; S2, cross-linking and curing: performing a thermal cross-linking and curing treatment on the polymer fibrils at a predetermined temperature to obtain infusible fibers; S3, thermal decomposition: thermally decomposing the infusible fibers at a predetermined heating rate to a predetermined temperature in an inert atmosphere to generate inorganic ceramic fibers; S4, sintering: sintering the inorganic ceramic fiber at a predetermined heating rate to a predetermined temperature in an inert atmosphere to generate a silicon carbide-carbon ceramic composite fiber having a carbon-rich core; S5, decarburization: heating the silicon carbide-carbon ceramic composite fiber to a predetermined temperature at a predetermined heating rate to perform an oxidation decarburization treatment to generate a hollow silicon carbide ceramic fiber.

[0007] The present invention uses a cheap organic silicon resin as a precursor to transform and prepare ceramic fibers. The organic silicon resin is melted in an inert atmosphere and formed into polymer fibrils of a predetermined diameter under predetermined process conditions. The polymer is subjected to a thermal crosslinking and curing treatment at a predetermined temperature, and the side hydroxyl groups condense to form a three-dimensional Si-O-Si network (crosslinking degree greater than 85%). Then, in the inert atmosphere, the infusible fibers are thermally decomposed at a predetermined heating rate to a predetermined temperature, and the relevant groups are cracked and volatilized, leaving an amorphous SiOC ceramic skeleton to generate inorganic ceramic fibers. Then, in the inert atmosphere, the fibers are sintered at a predetermined heating rate to a predetermined temperature, and a carbon thermal reduction reaction occurs. Free carbon migrates to the core to form a carbon-rich region, and β-SiC grains of a predetermined size grow in the outer shell. Finally, decarburization is performed. At a predetermined temperature, the carbon in the core is selectively oxidized to form a hollow structure, while the outer shell retains complete β-SiC crystals, thereby generating a high-crystalline silicon carbide ceramic fiber with a hollow structure.

[0008] This invention uses an organic silicone resin as a precursor and produces highly crystalline, hollow silicon carbide ceramic fibers through controlled spinning, infusibility, inorganicization, high-temperature sintering, and high-temperature post-treatment processes. The production cost is significantly lower than that of polycarbosilane and its modified precursors commonly used in the prior art. Thermal crosslinking is used to infusibly render the polymer fibrils, followed by high-temperature heat treatment to produce highly crystalline silicon carbide hollow ceramic fibers. The resulting ceramic fibers exhibit superior mechanical properties and, compared to existing electron beam irradiation infusibility techniques, offer a simpler process, easier operation, and lower manufacturing costs.

[0009] As a further preferred technical solution, the sintering conditions in step S4 are as follows: in an inert atmosphere, the inorganic ceramic fiber is subjected to high-temperature sintering at a rate of 0.5°C / min to 10°C / min, increasing from 1500°C to 1900°C, and holding the temperature for 1 to 3 hours, to obtain a silicon carbide-carbon ceramic composite fiber with a carbon-rich core, wherein the silicon carbide phase is β-SiC crystal. Sintering under these conditions drives the growth of β-SiC grains, controls the grain size, and avoids abnormal grain growth; ensures a dense fiber surface without structural collapse, achieves high crystallinity, and ensures a carbon-rich core.

[0010] Preferably, a further technical solution is that the decarburization conditions in step S5 are: heating to 700°C to 1000°C in dry air at a heating rate of 0.5°C / min to 10°C / min, and holding at this temperature for 0 to 3 hours. Under such conditions, high-temperature oxidative decarburization can remove free carbon from the fiber while ensuring that the fiber structure does not collapse, achieving precise control of the hollow structure. The decarburization temperature matches the carbon diffusion rate, ensuring a hollow structure with uniform fiber wall thickness.

[0011] Preferably, a further technical solution is that the melt spinning conditions in step S1 are: heating at a temperature of 150°C to 200°C for 0.5 to 1 hour in an inert atmosphere, at a pressure of 0.1 MPa to 1 MPa, and at a spinning speed of 100 to 900 r / min. The spinning pressure of 0.1 MPa to 1 MPa controls the rheological properties of the melt, and the spinning speed of 100 to 900 r / min regulates the fiber diameter. Melt spinning under these conditions can ensure the production of continuous fibers, achieve product diameter uniformity, ensure continuous spinning, avoid fiber breakage or paralleling, and the resulting fibers have uniform diameter and a smooth surface.

[0012] Preferably, a further technical solution is that the crosslinking and curing conditions in step S2 are: a treatment temperature of 90°C to 250°C and a treatment time of 2 hours to 10 hours. Crosslinking and curing under these conditions can ensure that the original fibers will not melt and filament under subsequent thermal decomposition and high-temperature sintering conditions, thereby maintaining structural integrity.

[0013] Preferably, in step S3, the thermal decomposition process is carried out under the following conditions: heating the fiber to a temperature of 800°C to 1300°C at a heating rate of 0.5°C / min to 10°C / min in an inert atmosphere, and holding the temperature for 0 to 3 hours. Thermal decomposition under these conditions ensures a smooth fiber surface, no structural collapse, and maintains adequate mechanical properties.

[0014] As a preferred embodiment, a further technical solution is that the organic silicone resin is an organic silicone polymer having Si—O bonds as the main chain and side groups including methyl and phenyl groups.

[0015] Select silicone resins with side groups containing methyl (-CH3) and phenyl (-C6H5) groups (such as methylphenyl silicone resin). The methyl groups provide a high carbon residue (generating free carbon after cracking), while the phenyl groups enhance thermal stability. Methyl groups crack to generate free carbon (the source of the core carbon phase), while the phenyl groups inhibit high-temperature melting. Selecting this precursor also avoids the technical problem of uneven composition caused by high-temperature disproportionation of Si-C bonds in polycarbosilane.

[0016] As a further preferred technical solution, the inert atmosphere is nitrogen or argon with a purity of ≥99.99%. This prevents oxidation degradation and premature consumption of the carbon phase, while also reducing the inhibition of SiC lattice growth by oxygen impurities and ensuring crystallization quality.

[0017] To achieve the above objectives, the present invention further provides a hollow silicon carbide ceramic fiber, characterized by being produced by any of the aforementioned methods for producing hollow silicon carbide ceramic fibers. The hollow silicon carbide ceramic fiber produced by the present invention exhibits superior mechanical properties and, compared to the denser morphology of existing silicon carbide fibers, is suitable for use in high-temperature thermal insulation materials and catalytic adsorption materials.

[0018] To achieve the above objectives, the present invention also provides an application of a hollow silicon carbide ceramic fiber, wherein the hollow silicon carbide ceramic fiber is applied to the fields of high-temperature thermal insulation materials and catalytic adsorption materials.

[0019] Compared with the existing technology, the present invention has the following technical advantages: 1. Low cost: Using cheap silicone resin as a precursor to convert and prepare ceramic fibers, the production cost is much lower than that of polycarbosilane and its modified precursors; 2. Precise structural control: By controlling the spinning, infusibility, inorganicization, high-temperature sintering and high-temperature post-treatment processes, high crystallinity and controllable hollow morphology can be achieved through carbon phase migration → selective decarburization; 3. Process compatibility: The entire process does not require special equipment (such as expensive electron irradiation equipment), is easy to implement, and has the characteristics of simple process, convenient operation, and low manufacturing cost, making it suitable for industrial production; 4. The prepared hollow silicon carbide ceramic fiber has good mechanical properties and is more suitable for the fields of high-temperature thermal insulation materials and catalytic adsorption materials compared to the dense morphology of silicon carbide fibers in the existing technology.

[0020] The present invention utilizes the molecular structure characteristics of silicone resin and solves the industry pain points of high cost and complex process in a simple way through an innovative process chain of melt spinning, cross-linking, cracking, sintering and selective decarbonization. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] The accompanying drawings, which constitute a part of the present invention, are used to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute improper limitations on the present invention.

[0022] Figure 1 This is a scanning electron microscope image of the hollow silicon carbide ceramic fiber prepared in Example 1 of the present invention; Figure 2 This is the XRD pattern of the hollow silicon carbide ceramic fiber prepared in Example 1 of the present invention. DETAILED DESCRIPTION

[0023] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts shall fall within the scope of protection of the present invention.

[0024] In addition, the technical solutions between the various embodiments of the present invention can be combined with each other, but it must be based on the fact that ordinary technicians in this field can implement it. When the combination of technical solutions is mutually contradictory or cannot be implemented, it should be deemed that such a combination of technical solutions does not exist and is not within the scope of protection required by the present invention.

[0025] Unless otherwise specified, all drugs / reagents used were commercially available.

[0026] Example 1 Preparation of high-crystalline silicon carbide hollow ceramic fibers, this embodiment includes the following steps: (1) 5 g of solid silicone resin (Si-O bond as the main chain, side groups containing methyl and phenyl silicone polymer) was placed in the spinning cylinder of a melt spinning device, and high-purity nitrogen was introduced to replace the air in the spinning cylinder at 60 °C. The spinning cylinder was heated to 190 °C and kept warm for 0.5 h. The melt spinning was carried out at a speed of 600 r / min under a pressure of 0.5 MPa to obtain polymer fibrils. (2) Place the polymer fibers in a quartz tube furnace, heat to 120°C, and keep warm for 3 hours to obtain infusible fibers; (3) The infusible fiber was placed in a quartz tube furnace, vacuumed, and high-purity nitrogen was introduced to replace the air in the quartz tube furnace three times. The temperature was raised to 1100 °C at a rate of 50 °C / h, and the temperature was kept at this temperature for 1 h to obtain inorganic ceramic fiber; (4) The inorganic ceramic fiber was placed in a graphite furnace, vacuumed, and high-purity nitrogen was introduced to replace the air in the graphite furnace three times. The temperature was raised to 1900 °C at a heating rate of 60 °C / h and kept at this temperature for 1 h to obtain silicon carbide-carbon ceramic composite fiber; (5) The silicon carbide-carbon ceramic composite fiber is placed in a muffle furnace, heated to 800°C at a heating rate of 5°C / min, and kept at this temperature for 1 hour to obtain a silicon carbide ceramic fiber with a high crystalline hollow structure.

[0027] The scanning electron microscope image of the hollow silicon carbide ceramic fiber obtained in this embodiment is as follows: Figure 1As shown in FIG, the hollow structured silicon carbide ceramic fiber is characterized by scanning electron microscopy. The morphology is hollow and is composed of silicon carbide grains with a grain size greater than 200 nm. Figure 2 As shown in FIG, XRD characterization shows that the fiber phase is β-SiC, and the oxygen content thereof is tested by an oxygen and nitrogen analyzer, which is less than 1%.

[0028] Example 2 (1) 5 g of solid silicone resin (Si-O bond as the main chain, side groups containing methyl and phenyl silicone polymer) was placed in the spinning cylinder of a melt spinning device, high-purity nitrogen was introduced, the air was replaced at 60 ° C, heated to 190 ° C, kept warm for 0.5 h, and melt-spun at a speed of 600 r / min under a pressure of 0.5 MPa to obtain polymer fibrils; (2) Place the polymer fibers in a quartz tube furnace, heat to 150°C, and keep warm for 1 hour to obtain infusible fibers; (3) The infusible fiber is placed in a quartz tube furnace, vacuumed, and high-purity nitrogen is introduced to replace the air three times. The temperature is raised to 1100°C at a heating rate of 50°C / h, and the temperature is kept at this temperature for 1 hour to obtain inorganic ceramic fiber; (4) The inorganic ceramic fiber was placed in a graphite furnace, vacuumed, and high-purity nitrogen was introduced to replace the air three times. The temperature was raised to 1900°C at a heating rate of 60°C / h, and the temperature was kept at this temperature for 1 hour to obtain silicon carbide-carbon ceramic composite fiber; (5) The silicon carbide-carbon ceramic composite fiber was placed in a muffle furnace, heated to 800°C at a heating rate of 5°C / min, and kept at this temperature for 1 hour to obtain highly crystalline silicon carbide hollow ceramic fiber.

[0029] Scanning electron microscopy (SEM) analysis of the hollow silicon carbide ceramic fiber obtained in this example revealed a hollow morphology composed of silicon carbide grains larger than 200 nm. XRD analysis confirmed the fiber phase to be β-SiC. An oxygen and nitrogen analyzer was used to measure the oxygen content, which was less than 1%. The characterization results were essentially the same as those for Example 1 and are not shown separately.

[0030] Example 3 (1) 5 g of solid silicone resin (Si-O bond as the main chain, side groups containing methyl and phenyl silicone polymer) was placed in the spinning cylinder of a melt spinning device, high-purity nitrogen was introduced, the air was replaced at 60 ° C, heated to 190 ° C, kept warm for 0.5 h, and melt-spun at a speed of 600 r / min under a pressure of 0.5 MPa to obtain polymer fibrils; (2) Place the polymer fibers in a quartz tube furnace, heat to 180°C, and keep warm for 1 hour to obtain infusible fibers; (3) The infusible fiber is placed in a quartz tube furnace, vacuumed, and high-purity nitrogen is introduced to replace the air three times. The temperature is raised to 1100°C at a heating rate of 50°C / h, and the temperature is kept at this temperature for 1 hour to obtain inorganic ceramic fiber; (4) The inorganic ceramic fiber was placed in a graphite furnace, vacuumed, and high-purity nitrogen was introduced to replace the air three times. The temperature was raised to 1900°C at a heating rate of 60°C / h, and the temperature was kept at this temperature for 1 hour to obtain silicon carbide-carbon ceramic composite fiber; (5) The silicon carbide-carbon ceramic composite fiber is placed in a muffle furnace, heated to 800°C at a heating rate of 5°C / min, and kept at this temperature for 1 hour to obtain highly crystalline silicon carbide hollow ceramic fiber.

[0031] Scanning electron microscopy (SEM) analysis of the hollow silicon carbide ceramic fiber obtained in this example revealed a hollow morphology composed of silicon carbide grains larger than 200 nm. XRD analysis confirmed the fiber phase to be β-SiC. An oxygen and nitrogen analyzer was used to measure the oxygen content, which was less than 1%. The characterization results were essentially the same as those for Example 1 and are not shown separately.

[0032] Example 4 (1) 5 g of solid silicone resin (Si-O bond as the main chain, side groups containing methyl and phenyl silicone polymer) was placed in the spinning cylinder of a melt spinning device, and high-purity nitrogen was introduced to replace the air at 60 °C. The mixture was heated to 200 °C and kept warm for 0.5 h. The melt spinning was carried out at a speed of 300 r / min under a pressure of 1 MPa to obtain polymer fibrils. (2) Place the polymer fibrils in a quartz tube furnace, heat to 90°C, and keep warm for 10 hours to obtain infusible fibers; (3) The infusible fiber was placed in a quartz tube furnace, vacuumed, and high-purity nitrogen was introduced to replace the air three times. The temperature was raised to 800°C at a heating rate of 30°C / h, and the temperature was kept at this temperature for 3 hours to obtain inorganic ceramic fiber; (4) The inorganic ceramic fiber was placed in a graphite furnace, vacuumed, and high-purity nitrogen was introduced to replace the air three times. The temperature was raised to 1500°C at a heating rate of 60°C / h and kept at this temperature for 3 h to obtain silicon carbide-carbon ceramic composite fiber; (5) The silicon carbide-carbon ceramic composite fiber was placed in a muffle furnace, heated to 700°C at a heating rate of 10°C / min, and kept at this temperature for 3 hours to obtain highly crystalline silicon carbide hollow ceramic fiber.

[0033] Scanning electron microscopy (SEM) analysis of the hollow silicon carbide ceramic fiber obtained in this example revealed a hollow morphology composed of silicon carbide grains larger than 200 nm. XRD analysis confirmed the fiber phase to be β-SiC. An oxygen and nitrogen analyzer was used to measure the oxygen content, which was less than 1%. The characterization results were essentially the same as those for Example 1 and are not shown separately.

[0034] Example 5 (1) 5 g of solid silicone resin (Si-O bond as the main chain, side groups containing methyl and phenyl silicone polymer) was placed in the spinning cylinder of a melt spinning device, and high-purity nitrogen was introduced to replace the air at 60 °C. The mixture was heated to 200 °C and kept warm for 0.5 h. The melt spinning was carried out at a speed of 900 r / min under a pressure of 0.1 MPa to obtain polymer fibrils. (2) Place the polymer fibers in a quartz tube furnace, heat to 250°C, and keep warm for 2 hours to obtain infusible fibers; (3) The infusible fiber is placed in a quartz tube furnace, vacuumed, and high-purity nitrogen is introduced to replace the air three times. The temperature is raised to 1100°C at a heating rate of 600°C / h, and the temperature is kept at this temperature for 1 hour to obtain inorganic ceramic fiber; (4) The inorganic ceramic fiber was placed in a graphite furnace, vacuumed, and high-purity nitrogen was introduced to replace the air three times. The temperature was raised to 1900°C at a heating rate of 30°C / h, and the temperature was kept at this temperature for 1h to obtain silicon carbide-carbon ceramic composite fiber; (5) The silicon carbide-carbon ceramic composite fiber is placed in a muffle furnace, heated to 1000°C at a heating rate of 10°C / min, and kept at this temperature for 1 hour to obtain highly crystalline silicon carbide hollow ceramic fiber.

[0035] Scanning electron microscopy (SEM) analysis of the hollow silicon carbide ceramic fiber obtained in this example revealed a hollow morphology composed of silicon carbide grains larger than 200 nm. XRD analysis confirmed the fiber phase to be β-SiC. An oxygen and nitrogen analyzer was used to measure the oxygen content, which was less than 5%. The characterization results were essentially the same as those in Example 1 and are not shown separately.

[0036] Example 6 (1) 5 g of solid silicone resin (Si-O bond as the main chain, side groups containing methyl and phenyl silicone polymer) was placed in the spinning cylinder of a melt spinning device, high-purity nitrogen was introduced, the air was replaced at 60 ° C, heated to 150 ° C, kept warm for 0.5 h, and melt-spun at a speed of 100 r / min under a pressure of 0.5 MPa to obtain polymer fibrils; (2) Place the polymer fibers in a quartz tube furnace, heat to 250°C, and keep warm for 1 hour to obtain infusible fibers; (3) The infusible fiber is placed in a quartz tube furnace, vacuumed, and high-purity nitrogen is introduced to replace the air three times. The temperature is raised to 1100°C at a heating rate of 50°C / h, and the temperature is kept at this temperature for 1 hour to obtain inorganic ceramic fiber; (4) The inorganic ceramic fiber was placed in a graphite furnace, vacuumed, and high-purity nitrogen was introduced to replace the air three times. The temperature was raised to 1900°C at a heating rate of 60°C / h and kept at this temperature for 1 h to obtain silicon carbide-carbon ceramic composite fiber; (5) The silicon carbide-carbon ceramic composite fiber is placed in a muffle furnace, heated to 1000°C at a heating rate of 5°C / min, and kept at this temperature for 1 hour to obtain highly crystalline silicon carbide hollow ceramic fiber.

[0037] Scanning electron microscopy (SEM) analysis of the hollow silicon carbide ceramic fiber obtained in this example revealed a hollow morphology composed of silicon carbide grains larger than 200 nm. XRD analysis confirmed the fiber phase to be β-SiC. An oxygen and nitrogen analyzer was used to measure the oxygen content, which was less than 5%. The characterization results were essentially the same as those in Example 1 and are not shown separately.

[0038] For ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention, and these improvements and modifications should also be considered as the scope of protection of the present invention.

Claims

1. A method for preparing hollow silicon carbide ceramic fiber, characterized in that: The steps include: S1, melt spinning: silicone resin is melted in an inert atmosphere and spun to form polymer fibrils; S2, cross-linking and curing: performing a thermal cross-linking and curing treatment on the polymer fibrils at a predetermined temperature to obtain infusible fibers; S3, thermal decomposition: thermally decomposing the infusible fibers at a predetermined heating rate to a predetermined temperature in an inert atmosphere to generate inorganic ceramic fibers; S4, sintering: sintering the inorganic ceramic fiber at a predetermined heating rate to a predetermined temperature in an inert atmosphere to generate a silicon carbide-carbon ceramic composite fiber having a carbon-rich core; S5, decarburization: heating the silicon carbide-carbon ceramic composite fiber to a predetermined temperature at a predetermined heating rate to perform an oxidation decarburization treatment to generate a hollow silicon carbide ceramic fiber.

2. The method for preparing hollow silicon carbide ceramic fiber according to claim 1, wherein: The sintering conditions in step S4 are as follows: in an inert atmosphere, the inorganic ceramic fiber is sintered at a temperature of 1500°C to 1900°C at a temperature of 0.5°C / min to 10°C / min, and the temperature is kept for 1 h to 3 h to obtain a silicon carbide-carbon ceramic composite fiber with a carbon-rich core, wherein the silicon carbide phase is β-SiC crystal.

3. The method for preparing hollow silicon carbide ceramic fiber according to claim 2, wherein: The decarburization conditions in step S5 are: heating to 700° C. to 1000° C. at a heating rate of 0.5° C. / min to 10° C. / min in dry air, and holding time of 0 h to 3 h.

4. The method for preparing hollow silicon carbide ceramic fiber according to claim 1, wherein: The melt spinning conditions in step S1 are: heating at a temperature of 150° C. to 200° C. for 0.5 h to 1 h in an inert atmosphere, and melt spinning at a speed of 100 r / min to 900 r / min under a pressure of 0.1 MPa to 1 MPa.

5. The method for preparing hollow silicon carbide ceramic fiber according to claim 4, characterized in that: The cross-linking and curing conditions in step S2 are: a treatment temperature of 90° C. to 250° C., and a treatment time of 1 hour to 10 hours.

6. The method for preparing the hollow silicon carbide ceramic fiber according to claim 5, wherein: The thermal decomposition conditions in step S3 are: in an inert atmosphere, heating to 800° C. to 1300° C. at a heating rate of 0.5° C. / min to 10° C. / min, and holding time of 0 h to 3 h.

7. The method for preparing the hollow silicon carbide ceramic fiber according to any one of claims 1 to 6, characterized in that: The organic silicon resin is an organic silicon polymer with Si-O bonds as the main chain and side groups including methyl and phenyl groups.

8. The method for preparing the hollow silicon carbide ceramic fiber according to claim 7, wherein: The inert atmosphere is nitrogen or argon with a purity of ≥99.99%.

9. A hollow silicon carbide ceramic fiber, characterized in that: The hollow silicon carbide ceramic fiber is prepared by the preparation method of any one of claims 1 to 8.

10. An application of a hollow silicon carbide ceramic fiber, characterized in that: The hollow silicon carbide ceramic fiber described in claim 9 is applied to the fields of high-temperature thermal insulation materials and catalytic adsorption materials.

Citation Information

Patent Citations

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