CN109896864A - Method for preparing wave-absorbing continuous SiCN ceramic fiber - Google Patents
Method for preparing wave-absorbing continuous SiCN ceramic fiber Download PDFInfo
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- CN109896864A CN109896864A CN201910337268.7A CN201910337268A CN109896864A CN 109896864 A CN109896864 A CN 109896864A CN 201910337268 A CN201910337268 A CN 201910337268A CN 109896864 A CN109896864 A CN 109896864A
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Abstract
The invention discloses a preparation method of wave-absorbing continuous SiCN ceramic fiber, which comprises the following steps: s1: placing the polycarbosilane crosslinked fiber in a vacuum sintering furnace, and vacuumizing; s2: heating a vacuum sintering furnace, and then introducing a mixed gas of ammonia gas and helium gas; s3: continuously introducing the mixed gas, and keeping the pressure in the furnace unchanged; s4: continuing heating the vacuum sintering furnace, and stopping introducing the mixed gas into the vacuum sintering furnace; s5: reducing the pressure in the furnace, and simultaneously continuously heating the vacuum sintering furnace; s6: and stopping heating the vacuum sintering furnace, and obtaining the wave absorption type continuous SiCN ceramic fiber when the temperature is reduced to below 50 ℃. Compared with the prior art, the preparation method of the wave-absorbing continuous SiCN ceramic fiber provided by the invention is simple in process flow, and the prepared wave-absorbing continuous SiCN ceramic fiber has the resistivity of 104~108Omega cm, the lowest electromagnetic reflection loss reaches-63.7 dB, the thickness is that the effective absorption bandwidth reaches 4.20GHz, and the material not only has high resistivity, but also has excellent wave-absorbing performance of X wave band and Ku wave band.
Description
Technical field
The present invention relates to high-performance fiber preparation technical field, especially a kind of system for inhaling the continuous SiCN ceramic fibre of wave mode
Preparation Method.
Background technique
Microwave-absorbing ceramic fiber is the key raw material of high temperature Wave suction composite material, is the important material for realizing that high-temperature component is stealthy
Material.Since the C/Si atom of silicon carbide fibre raw material Polycarbosilane is relatively high, manufactured SiC fiber contains more free carbon,
The regulation of its composed structure is limited, is easy to prepare the ceramic fibre of low-resistivity, it is difficult to prepare resistivity higher than 10000 Ω cm
Microwave-absorbing ceramic fiber.
The absorbing property for promoting wave-absorption fibre, is on the one hand the reflection of electromagnetic wave to be reduced, and imports more electromagnetic waves
In material, on the other hand it is able to that the electromagnetic wave for importing material internal is made to be converted into heat by dielectric loss and polarization loss
Can, both sides overall effect makes being optimal of absorbing property of material.Therefore, simple high resistivity can only reduce reflection
Without can increase loss, although the big reflection electromagnetic wave of simple low-resistivity dielectric loss makes electromagnetic wave be difficult to import.It will
Fiber sheath is changed to nitride by enriched carbon layer, although resistivity can be dramatically increased, its interior free-carbon still can be to height
Absorbing property under the conditions of temperature brings adverse effect.
Summary of the invention
The present invention provides a kind of preparation method for inhaling the continuous SiCN ceramic fibre of wave mode, prepares in the prior art for overcoming
Microwave-absorbing ceramic fabric resistor rate be difficult to reach 10000 Ω cm or absorbing property under resistivity is high but its high temperature is impacted etc.
Defect realizes that the microwave-absorbing ceramic fabric resistor rate being prepared is 104~108Ω cm, and its absorbing property is not influenced.
To achieve the above object, the present invention propose it is a kind of inhale the continuous SiCN ceramic fibre of wave mode preparation method, including with
Lower step:
S1: Polycarbosilane cross filament is placed in vacuum sintering furnace, is vacuumized;
S2: being warming up to 300~500 DEG C for vacuum sintering furnace, is passed through the gaseous mixture of ammonia and helium later until vacuum is burnt
Knot furnace pressure is 85~95kPa;
S3: continue the gaseous mixture for being passed through ammonia and helium, while vacuum-sintering in-furnace temperature being heated up from 300~500 DEG C
To 800~1000 DEG C, and keeping vacuum-sintering furnace pressure is that 85~95kPa is constant, is stopped after temperature reaches 800~1000 DEG C
Ammonia and helium mix gas are only passed through into vacuum sintering furnace;
S4: control vacuum-sintering furnace pressure is 10~50Pa, while by vacuum-sintering in-furnace temperature from 800~1000 DEG C
It is warming up to 1300~1500 DEG C;
S5: stopping vacuum sintering furnace heating, is reduced to 50 DEG C to make pottery hereinafter, can be taken off the continuous SiCN of suction wave mode to its temperature
Porcelain fiber.
Compared with prior art, the beneficial effects of the present invention are as follows:
1, the continuous SiCN ceramic fibre preparation method of suction wave mode provided by the invention mainly makes Polycarbosilane cross filament
Raw material reacts to realize at high temperature under high pressure that with ammonia, the nitrogen in ammonia replaces Polycarbosilane cross filament raw material
In carbon, to reduce the C content in product, process flow is simple, it is easy to accomplish, and raw material sources are abundant, price just
Preferably.
2, the material being prepared using the method for the present invention is stripped of carbon while SiC/SiC is also obtainedxNy/Si3N4Three
Mingzhi's micro-structure, this is substantially reduced material C/Si atomic ratio of preparation, so that resistivity significantly improves, while SiC/
SiCxNy/Si3N4Sandwich micro-structure can reduce the reflection of electromagnetic wave, import more electromagnetic waves in material, the structure is also
The electromagnetic wave for importing material internal can be made to be converted into thermal energy, so that Absorbing Materials by dielectric loss and polarization loss
It is good.The resistivity of material that the present invention is prepared is 104~108Ω cm, dielectric constant is 8~20 within the scope of 8~18GHz,
Loss tangent is 0~0.5, and minimum ELECTROMAGNETIC REFLECTION loss reaches -63.7dB, is reached with a thickness of effective Absorber Bandwidth
4.20GHz, it is shown that excellent X-band and Ku wave band absorbing property.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
The structure shown according to these attached drawings obtains other attached drawings.
Fig. 1 is the SiC/SiC of one SiCN ceramic fibre of embodimentxNy/Si3N4Sandwich micro-structure TEM figure;
Fig. 2 is the absorbing property phenogram of one SiCN ceramic fibre of embodiment;
Fig. 3 is one SiCN ceramic fibre dielectric constant figure within the scope of 8~18GHz of embodiment;
Fig. 4 is one SiCN ceramic fibre of embodiment in 8~18GHz range internal loss angle tangent figure.
The embodiments will be further described with reference to the accompanying drawings for the realization, the function and the advantages of the object of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiment is only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts it is all its
His embodiment, shall fall within the protection scope of the present invention.
Without specified otherwise, used drug/reagent is commercially available.
The present invention proposes a kind of preparation method for inhaling the continuous SiCN ceramic fibre of wave mode, comprising the following steps:
S1: Polycarbosilane cross filament is placed in vacuum sintering furnace, is vacuumized;
In the step S1, the C/Si atomic ratio of the Polycarbosilane cross filament is weight in 1.5~2,1000 DEG C of nitrogen
It measures conservation rate and is higher than 80%, 400 DEG C will not melt deformation;Ceramic fibre with excellent absorbing property require to have certain SiC,
Si3N4The different compositions with C etc., the Polycarbosilane cross filament raw material of selection can provide Si, C, and Polycarbosilane cross filament raw material is high
SiC can be formed under temperature, part SiC becomes Si by atmosphere reaction later3N4, raw material can satisfy use demand and abundance,
It is cheap.
It is described to vacuumize, lower than 1Pa, to remove air to vacuum-sintering furnace pressure, preventing raw material and air reaction from introducing
Impurity.
S2: being warming up to 300~500 DEG C for vacuum sintering furnace, is passed through the gaseous mixture of ammonia and helium later until vacuum is burnt
Knot furnace pressure is 85~95kPa;
In the step S2, ammonia and helium volume ratio are (1:1)~(4:1) in the gaseous mixture;It is described to be passed through mixing
The flow of gas is 1~2L/min;
Ammonia in gaseous mixture is to react to make the nitrogen member in ammonia with Polycarbosilane cross filament raw material
Element replaces the carbon in Polycarbosilane cross filament raw material;Helium is to dilute ammonia, while helium is inert gas, no
The progress of meeting disturbing reaction;It is anti-that the control of ammonia and helium volume ratio and the control of mixed gas flow are provided to control gas phase
The degree answered controls the element composition of final SiCN fiber.
S3: continue the gaseous mixture for being passed through ammonia and helium, while vacuum-sintering in-furnace temperature being heated up from 300~500 DEG C
To 800~1000 DEG C, and keeping vacuum-sintering furnace pressure is that 85~95kPa is constant, is stopped after temperature reaches 800~1000 DEG C
Ammonia and helium mix gas are only passed through into vacuum sintering furnace;
In the step S3, the flow for being passed through gaseous mixture is 1~2L/min;The holding vacuum-sintering furnace pressure
Constant is to adjust to realize by vacuum pump sucking rate;
Keep vacuum-sintering furnace pressure be 85~95kPa it is constant be in order to make the operation stage fiber hydrolization come out contain
Carbon atmosphere is quickly discharged, while not accelerating its decomposition, and the too low meeting accelerated decomposition of pressure causes product defects more.
The heating rate is 1~2 DEG C/min.
Ammonia in this step, gaseous mixture reacts with Polycarbosilane cross filament raw material, the nitrogen in ammonia
Replace the carbon in Polycarbosilane cross filament raw material, thus the nitrogen content for reducing the carbon content of product, improving product.
S4: control vacuum-sintering furnace pressure is 10~50Pa, while by vacuum-sintering in-furnace temperature from 800~1000 DEG C
It is warming up to 1300~1500 DEG C;
In the step S4, the control vacuum-sintering furnace pressure is that 10~50Pa is adjusted by vacuum pump sucking rate
It realizes;The heating rate is 2~5 DEG C/min.
Reduce vacuum-sintering furnace pressure simultaneously continue increase in-furnace temperature be in order to prevent Carbon deposition in product surface.
S5: stopping vacuum sintering furnace heating, is reduced to 50 DEG C to make pottery hereinafter, can be taken off the continuous SiCN of suction wave mode to its temperature
Porcelain fiber.
The resistivity for inhaling the continuous SiCN ceramic fibre of wave mode is 104~108Ω cm, is situated between within the scope of 8~18GHz
Electric constant is 8~20, and loss tangent is 0~0.5, and minimum ELECTROMAGNETIC REFLECTION loss reaches -63.7dB, is absorbed with a thickness of effective
Bandwidth reaches 4.20GHz.
The carbon content for inhaling the continuous SiCN ceramic fibre of wave mode is 20~30wt%, nitrogen content is 10~20wt%, tool
There is SiC/SiCxNy/Si3N4Sandwich micro-structure.
1, TEM (transmission electron microscope): device model is Titan G2 60-300, after the grinding of gained fiber sample, ultrasound point
It dissipates in ethanol, is put into equipment after dripping on copper mesh and is tested.
2, it absorbing property: is calculated by dielectric constant and dielectric loss.
3, dielectric constant curve and dielectric loss curve: device model is Agilent N5230A vector network analyzer,
Be pressed under the conditions of 130 DEG C of 1MPa after gained fiber is mixed with ethylene oxide 22.86 × 10.16 × 3.0mm and 15.8 ×
The sample of 7.9 × 3.0mm, is tested by equipment.
Embodiment one
The present embodiment provides a kind of preparation methods for inhaling the continuous SiCN ceramic fibre of wave mode, comprising the following steps:
S1: being placed in vacuum sintering furnace for Polycarbosilane cross filament, vacuumize, and makes furnace pressure lower than 1Pa;
S2: being warming up to 400 DEG C for vacuum sintering furnace, later with the flow of 1.5L/min be passed through volume ratio 1:1 ammonia and
The gaseous mixture of helium is until vacuum-sintering furnace pressure is 85kPa;
S3: continue the gaseous mixture for being passed through ammonia and helium, while with the flow of 1.5L/min with the heating rate of 1 DEG C/min
Vacuum-sintering in-furnace temperature is warming up to 900 DEG C from 400 DEG C, and keeping vacuum-sintering furnace pressure is that 85kPa is constant, to temperature
Stop being passed through ammonia and helium mix gas into vacuum sintering furnace after reaching 900 DEG C;
S4: adjusting control vacuum-sintering furnace pressure by vacuum pump sucking rate is 50Pa, while with the heating of 2 DEG C/min
Vacuum-sintering in-furnace temperature is warming up to 1400 DEG C from 900 DEG C by rate;
S5: stopping vacuum sintering furnace heating, is reduced to 50 DEG C to make pottery hereinafter, can be taken off the continuous SiCN of suction wave mode to its temperature
Porcelain fiber.
Polycarbosilane cross filament raw material used, C/Si atomic ratio are that weight retention rate is higher than in 2,1000 DEG C of nitrogen
80%, 400 DEG C will not melt deformation.
The carbon content of the continuous SiCN ceramic fibre of the suction wave mode that the present embodiment is prepared is 28wt%, nitrogen content is
15wt% has SiC/SiCxNy/Si3N4Sandwich micro-structure, resistivity are 3.8 × 106Ω cm, within the scope of 8~18GHz
Dielectric constant is 14~17, and loss tangent is 0.2~0.4, and minimum ELECTROMAGNETIC REFLECTION loss reaches -63.7dB, with a thickness of having
Effect Absorber Bandwidth reaches 4.20GHz, it is shown that excellent X-band and Ku wave band absorbing property.
Fig. 1 be the present embodiment SiCN ceramic fibre micro-structure TEM figure, as seen from the figure its there are apparent sandwiches to press from both sides
Core structure, and sandwich of layers nitrogen, carbon distribution gradient;
Fig. 2 is the absorbing property phenogram of the SiCN ceramic fibre of the present embodiment, as seen from the figure its minimum ELECTROMAGNETIC REFLECTION damage
Consumption reaches -63.7dB, reaches 4.20GHz with a thickness of effective Absorber Bandwidth;
Fig. 3 is the dielectric constant curve of the SiCN ceramic fibre of the present embodiment, and dielectric constant is within the scope of 8~18GHz
12~18;
Fig. 4 is the dielectric loss curve of the SiCN ceramic fibre of the present embodiment, and dielectric loss is within the scope of 8~18GHz
0.2~0.4.
Embodiment two
The present embodiment provides a kind of preparation methods for inhaling the continuous SiCN ceramic fibre of wave mode, comprising the following steps:
S1: being placed in vacuum sintering furnace for Polycarbosilane cross filament, vacuumize, and makes furnace pressure lower than 1Pa;
S2: being warming up to 400 DEG C for vacuum sintering furnace, later with the flow of 2.0L/min be passed through volume ratio 4:1 ammonia and
The gaseous mixture of helium is until vacuum-sintering furnace pressure is 95kPa;
S3: continue the gaseous mixture for being passed through ammonia and helium, while with the flow of 2.0L/min with the heating of 1.5 DEG C/min speed
Vacuum-sintering in-furnace temperature is warming up to 900 DEG C from 400 DEG C by rate, and keeping vacuum-sintering furnace pressure is that 95kPa is constant, to temperature
Degree stops being passed through ammonia and helium mix gas into vacuum sintering furnace after reaching 900 DEG C;
S4: adjusting control vacuum-sintering furnace pressure by vacuum pump sucking rate is 50Pa, while with the heating of 5 DEG C/min
Vacuum-sintering in-furnace temperature is warming up to 1400 DEG C from 900 DEG C by rate;
S5: stopping vacuum sintering furnace heating, is reduced to 50 DEG C to make pottery hereinafter, can be taken off the continuous SiCN of suction wave mode to its temperature
Porcelain fiber.
Polycarbosilane cross filament used, C/Si atomic ratio are that weight retention rate is higher than in 1.5,1000 DEG C of nitrogen
80%, 400 DEG C will not melt deformation.
The carbon content of the continuous SiCN ceramic fibre of the suction wave mode that the present embodiment is prepared is 20wt%, nitrogen content is
20wt% has SiC/SiCxNy/Si3N4Sandwich micro-structure, resistivity are 6.3 × 108Ω cm, within the scope of 8~18GHz
Dielectric constant is 8~12, and loss tangent is 0~0.3, and minimum ELECTROMAGNETIC REFLECTION loss reaches -46.1dB, is inhaled with a thickness of effective
Take-up width reaches 3.79GHz, it is shown that excellent X-band and Ku wave band absorbing property.
Embodiment three
The present embodiment provides a kind of preparation methods for inhaling the continuous SiCN ceramic fibre of wave mode, comprising the following steps:
S1: being placed in vacuum sintering furnace for Polycarbosilane cross filament, vacuumize, and makes furnace pressure lower than 1Pa;
S2: being warming up to 400 DEG C for vacuum sintering furnace, later with the flow of 1.0L/min be passed through volume ratio 2:1 ammonia and
The gaseous mixture of helium is until vacuum-sintering furnace pressure is 90kPa;
S3: continue the gaseous mixture for being passed through ammonia and helium, while with the flow of 1.0L/min with the heating of 2.0 DEG C/min speed
Vacuum-sintering in-furnace temperature is warming up to 900 DEG C from 400 DEG C by rate, and keeping vacuum-sintering furnace pressure is that 90kPa is constant, to temperature
Degree stops being passed through ammonia and helium mix gas into vacuum sintering furnace after reaching 900 DEG C;
S4: adjusting control vacuum-sintering furnace pressure by vacuum pump sucking rate is 30Pa, while with the heating of 3 DEG C/min
Vacuum-sintering in-furnace temperature is warming up to 1400 DEG C from 900 DEG C by rate;
S5: stopping vacuum sintering furnace heating, is reduced to 50 DEG C to make pottery hereinafter, can be taken off the continuous SiCN of suction wave mode to its temperature
Porcelain fiber.
Polycarbosilane cross filament used, C/Si atomic ratio are that weight retention rate is higher than in 1.8,1000 DEG C of nitrogen
80%, 400 DEG C will not melt deformation.
The carbon content of the continuous SiCN ceramic fibre of the suction wave mode that the present embodiment is prepared is 30wt%, nitrogen content is
10wt% has SiC/SiCxNy/Si3N4Sandwich micro-structure, resistivity are 2.6 × 104Ω cm, within the scope of 8~18GHz
Dielectric constant is 15~20, and loss tangent is 0.2~0.5, and minimum ELECTROMAGNETIC REFLECTION loss reaches -39.4dB, with a thickness of having
Effect Absorber Bandwidth reaches 2.38GHz, it is shown that excellent X-band and Ku wave band absorbing property.
The above description is only a preferred embodiment of the present invention, is not intended to limit the scope of the invention, all at this
Under the inventive concept of invention, using equivalent structure transformation made by description of the invention and accompanying drawing content, or directly/use indirectly
It is included in other related technical areas in scope of patent protection of the invention.
Claims (9)
1. a kind of preparation method for inhaling the continuous SiCN ceramic fibre of wave mode, which comprises the following steps:
S1: Polycarbosilane cross filament is placed in vacuum sintering furnace, is vacuumized;
S2: being warming up to 300~500 DEG C for vacuum sintering furnace, is passed through the gaseous mixture of ammonia and helium later until vacuum sintering furnace
Interior pressure is 85~95kPa;
S3: continue the gaseous mixture for being passed through ammonia and helium, while vacuum-sintering in-furnace temperature is warming up to 800 from 300~500 DEG C
~1000 DEG C, and keep vacuum-sintering furnace pressure be 85~95kPa it is constant, stop after temperature reaches 800~1000 DEG C to
Ammonia and helium mix gas are passed through in vacuum sintering furnace;
S4: control vacuum-sintering furnace pressure is 10~50Pa, while vacuum-sintering in-furnace temperature being heated up from 800~1000 DEG C
To 1300~1500 DEG C;
S5: stopping vacuum sintering furnace heating, to its temperature be reduced to 50 DEG C hereinafter, can be taken off inhaling wave mode continuous SiCN ceramics fibre
Dimension.
2. a kind of preparation method for inhaling the continuous SiCN ceramic fibre of wave mode as described in claim 1, which is characterized in that the step
In rapid S1, the C/Si atomic ratio of the Polycarbosilane cross filament is that weight retention rate is higher than in 1.5~2,1000 DEG C of nitrogen
80%, 400 DEG C will not melt deformation.
3. a kind of preparation method for inhaling the continuous SiCN ceramic fibre of wave mode as described in claim 1, which is characterized in that the step
It is described to vacuumize to be lower than 1Pa to vacuum-sintering furnace pressure in rapid S1.
4. a kind of preparation method for inhaling the continuous SiCN ceramic fibre of wave mode as described in claim 1, which is characterized in that the step
In rapid S2, ammonia and helium volume ratio are (1:1)~(4:1) in the gaseous mixture;The flow for being passed through gaseous mixture be 1~
2L/min。
5. a kind of preparation method for inhaling the continuous SiCN ceramic fibre of wave mode as described in claim 1, which is characterized in that the step
In rapid S3, the flow for being passed through gaseous mixture is 1~2L/min;The heating rate is 1~2 DEG C/min.
6. a kind of preparation method for inhaling the continuous SiCN ceramic fibre of wave mode as described in claim 1, which is characterized in that the step
In rapid S3, the constant holding vacuum-sintering furnace pressure is to adjust to realize by vacuum pump sucking rate.
7. a kind of preparation method for inhaling the continuous SiCN ceramic fibre of wave mode as described in claim 1, which is characterized in that the step
In rapid S4, the control vacuum-sintering furnace pressure is that 10~50Pa is to adjust to realize by vacuum pump sucking rate;The liter
Warm rate is 2~5 DEG C/min.
8. a kind of preparation method of the continuous SiCN ceramic fibre of suction wave mode as described in claim 1~7, which is characterized in that institute
The resistivity for stating the suction continuous SiCN ceramic fibre of wave mode is 104~108Ω cm, within the scope of 8~18GHz dielectric constant be 8~
20, loss tangent is 0~0.5, and minimum ELECTROMAGNETIC REFLECTION loss reaches -63.7dB, is reached with a thickness of effective Absorber Bandwidth
4.20GHz。
9. a kind of preparation method for inhaling the continuous SiCN ceramic fibre of wave mode as claimed in claim 8, which is characterized in that the suction
The carbon content of the continuous SiCN ceramic fibre of wave mode is 20~30wt%, nitrogen content is 10~20wt%, has SiC/SiCxNy/
Si3N4Sandwich micro-structure.
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CN112851359A (en) * | 2021-01-22 | 2021-05-28 | 哈尔滨工业大学 | Absorption type SiBCN nano-fiber and preparation method thereof |
CN115340379A (en) * | 2021-05-14 | 2022-11-15 | 中国科学院化学研究所 | High-carbon-content silicon-boron-carbon-nitrogen ceramic fiber and preparation method and application thereof |
CN116041072A (en) * | 2023-01-09 | 2023-05-02 | 中国人民解放军国防科技大学 | Hollow SiCN ceramic fiber and preparation method and application thereof |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112851359A (en) * | 2021-01-22 | 2021-05-28 | 哈尔滨工业大学 | Absorption type SiBCN nano-fiber and preparation method thereof |
CN115340379A (en) * | 2021-05-14 | 2022-11-15 | 中国科学院化学研究所 | High-carbon-content silicon-boron-carbon-nitrogen ceramic fiber and preparation method and application thereof |
CN115340379B (en) * | 2021-05-14 | 2023-09-01 | 中国科学院化学研究所 | High-carbon-content silicon-boron-carbon-nitrogen ceramic fiber as well as preparation method and application thereof |
CN116041072A (en) * | 2023-01-09 | 2023-05-02 | 中国人民解放军国防科技大学 | Hollow SiCN ceramic fiber and preparation method and application thereof |
CN116041072B (en) * | 2023-01-09 | 2023-09-01 | 中国人民解放军国防科技大学 | Hollow SiCN ceramic fiber and preparation method and application thereof |
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