CN108395253A - A kind of preparation method of silicon boron nitrogen carbon beryllium ceramic fibre - Google Patents
A kind of preparation method of silicon boron nitrogen carbon beryllium ceramic fibre Download PDFInfo
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- CN108395253A CN108395253A CN201810148504.6A CN201810148504A CN108395253A CN 108395253 A CN108395253 A CN 108395253A CN 201810148504 A CN201810148504 A CN 201810148504A CN 108395253 A CN108395253 A CN 108395253A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62272—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on non-oxide ceramics
- C04B35/62277—Fibres based on carbides
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- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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Abstract
The present invention relates to a kind of preparation methods of silicon boron nitrogen carbon beryllium ceramic fibre, including：Prepared by the silicon boron nitrogen carbon matrix precursor containing beryllium element, prepared by presoma as-spun fibre, prepared by silicon boron nitrogen carbon beryllium ceramic fibre.The present invention is simple, and reaction condition is mild, at low cost；The silicon boron nitrogen carbon beryllium ceramic fibre surface being prepared is smooth, even tissue, compact structure, has good mechanical property, thermal stability, antioxygenic property and absorbing property.
Description
Technical field
The invention belongs to the preparation field of ceramic fibre, more particularly to a kind of preparation side of silicon boron nitrogen carbon beryllium ceramic fibre
Method.
Background technology
Continuous Fiber Reinforced Ceramic Matrix Composites have higher specific strength, specific modulus and excellent thermal stability
The advantages that, it is widely used in the high-end fields such as aerospace.With the development of aerospace cause, to the resistance to height of ceramic matric composite
Mild antioxygenic property requirement is higher and higher, and it is the key that improve its performance then to prepare suitable reinforcing fiber.Silicon boron nitrogen carbon
Ceramic fibre is by its high-melting-point, Strong oxdiative ability and excellent high-temperature stability by the extensive pass of military project and civil field
Note.But under high-temperature oxidation environment, the boron element (B) in silicon boron nitrogen carbon ceramic material can generate boron oxide gaseous volatilization and subtract
Its weak antioxygenic property, affects it and is further widely used.The elements such as aluminium (Al), zirconium (Zr) are introduced to form multicomponent material
System is the effective ways for the comprehensive performance for improving silicon boron nitrogen carbon ceramic material.
Chinese patent CN105801866A (publication date 2016.07.27) discloses a kind of borosilicate azane ceramics containing aluminium
The preparation method of precursor, this method are that solid PVDF hollow fiber membrane is dissolved in dimethylbenzene, are then tried again with organometallic aluminium
Agent is fully reacted, and heats and held for some time, distillation obtain the boron nitrogen silane elder generation containing aluminium element of yellow after being cooled to room temperature
Drive body, the advantages of this method is that raw material sources are reliable, it can be achieved that each element is uniformly distributed, and inhibits the growth of SiC crystal, the party
The shortcomings that method is oxide layer easy fracture under high temperature, and antioxygenic property reduces, and there are decomposition reaction, mechanical property in forming process
Can be relatively low, and the hardness of the obtained borosilicate azane ceramics containing aluminium is relatively low.
Chinese patent CN101492285B (publication date 2009.07.29) discloses a kind of preparation method of fibre containing beryllium,
This method is to contain beryllium compound, organic polymer as raw material, presoma containing beryllium be made, then continuous fiber is made through melt spinning
Or staple fiber is made in centrifugal drying silk, blowing process, above-mentioned fiber progress cure treatment is obtained fusion-free fibre, then protect in atmosphere
Shield is lower to carry out high temperature firing, and continuous fiber containing beryllium or staple fiber is made.The advantages of this method is that technological process is simple, is suitble to batch
Production, it is to be improved that the disadvantages of this method is that fiber high temperature is stablized, and allows for the system due to being free of boron element (B) and contain
There is the system containing boron element (B) to compare, recrystallization temperature wants low 300~400 DEG C, and conductivity at high temperature reduces.
Metallic beryllium (Be) and boron (B) belong to a period of element, but beryllium (Be) is more easy to lose electronics relative to boron (B), because
The generation for being more prone to generate heat safe beryllium oxide when this is aoxidized and inhibiting boron oxide gas, increases to a certain extent
The inoxidizability and high temperature oxidation stability of system.And Be-B ionic bonds have compared with the covalent bond in silicon boron nitrogen carbon material it is higher
Thermal conductivity, modulus and conductivity.
Invention content
Technical problem to be solved by the invention is to provide a kind of preparation method of silicon boron nitrogen carbon beryllium ceramic fibre, this method
Simply, reaction condition is mild, at low cost, and the silicon boron nitrogen carbon beryllium ceramic fibre surface being prepared is smooth, even tissue, and structure causes
It is close, there is good mechanical property, thermal stability, antioxygenic property and absorbing property.
A kind of preparation method of silicon boron nitrogen carbon beryllium ceramic fibre of the present invention, is as follows：
(1) by nitrogen source, boron source, silicon source, beryllium source and solvent with molar ratio be 12:2:2:1~0.5:120~160 mixing, are stirred
Reaction is mixed, the silicon boron nitrogen carbon matrix precursor containing beryllium element, melt spinning are obtained, winding obtains presoma as-spun fibre；
(2) presoma as-spun fibre in step (1) under the conditions of mixed gas is subjected to cure treatment, obtained crosslinked
Then fusion-free fibre cracks in a nitrogen atmosphere, be cooled to room temperature, obtains silicon boron nitrogen carbon beryllium ceramic fibre.
Nitrogen source is hexamethyldisilazane in the step (1)；Boron source is boron chloride；Silicon source is dichloro methyl silane；
Beryllium source is dichloride beryllium；Solvent is anhydrous n-hexane.
Mixing carries out under the conditions of -45~-15 DEG C in the step (1).
It is stirred to react specially in the step (1)：8-12h is stirred, 80~130 DEG C is warming up to 3~5 DEG C/min, protects
6~12h of temperature, then it is warming up to 200~220 DEG C with 3~5 DEG C/min, heat preservation 12~for 24 hours.
The temperature of melt spinning is 100~120 DEG C in the step (1).
The speed wound in the step (1) is 100-500m/min.
It is 1 that mixed gas, which is volume ratio, in the step (2):1-2:1 active gases and inert gas, inert gas are
Nitrogen or argon gas, active gases are ammonia or boron chloride.
The speed that is passed through of mixed gas is 100~300ml/min in the step (2).
The condition of cure treatment is in the step (2)：With 2~3 DEG C/min be warming up to 300~400 DEG C and keep the temperature 3~
6h。
The condition of cracking is in the step (2)：1200~1400 DEG C are warming up to 3~5 DEG C/min, soaking time 4
~8h.
The present invention passes through a step using hexamethyldisilazane, boron chloride, dichloro methyl silane, dichloride beryllium as raw material
Method polycondensation obtains the poly- silicon boron nitrogen carbon matrix precursor containing beryllium element, and presoma obtains as-spun fibre after melt spinning, by nascent fibre
Dimension carries out cure treatment, then Pintsch process obtains silicon boron nitrogen carbon beryllium ceramic fibre under an inert atmosphere.
Advantageous effect
(1) present invention is simple, and reaction condition is mild, at low cost；
(2) the silicon boron nitrogen carbon beryllium ceramic fibre surface that the present invention is prepared is smooth, and even tissue, compact structure has
Good mechanical property, thermal stability, antioxygenic property and absorbing property.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
(1) at -15 DEG C, by 1.2mol hexamethyldisilazane, 0.2mol boron chlorides, 0.2mol dichloro methyl silanes
Co-dissolve is in 15mol anhydrous n-hexanes in three-necked flask with 0.1mol dichloride berylliums, after stirring 12h, with 3 DEG C/min's
Heating rate heating heating three-necked flask keeps the temperature 6h, then be warming up to 220 DEG C with 3 DEG C/min speed, keeps the temperature 12h, obtain to 100 DEG C
To the silicon boron nitrogen carbon matrix precursor containing beryllium element, it is heated to 100 DEG C in a nitrogen environment, melt spinning is carried out, with 200m/min's
Winding speed collects a diameter of 20~26 μm of silicon boron nitrogen carbon beryllium presoma as-spun fibre.
(2) as-spun fibre in step (1) is put into tube furnace, volume ratio is passed through as 2 with the speed of 250mL/min:1
Ammonia and nitrogen composition mixed gas, with the heating rate of 3 DEG C/min be warming up to 350 DEG C reaction 5h, obtain silicon boron nitrogen carbon
Beryllium presoma fusion-free fibre, the Pintsch process under nitrogen atmosphere protection are warming up to 1300 DEG C instead with the heating rate of 5 DEG C/min
5h is answered, room temperature is cooled to, obtains silicon boron nitrogen carbon beryllium ceramic fibre.The fiber can keep noncrystalline state at 1800 DEG C, at 1500 DEG C
Not oxidized, tensile strength 1.1GPa is less than -8dB in 8.0~18.0GHz frequency range internal reflection rates, has good wave absorbtion
Energy.
Embodiment 2
(1) at -45 DEG C, by 6mol hexamethyldisilazane, 1mol boron chlorides, 1mol dichloro methyl silanes and
Co-dissolve is in 75mol anhydrous n-hexanes in three-necked flask for 0.25mol dichloride berylliums, after stirring 12h, with 4 DEG C/min's
Heating rate heating heating three-necked flask keeps the temperature 7h, then be warming up to 220 DEG C with 3 DEG C/min speed, keeps the temperature 14h, obtain to 120 DEG C
To the silicon boron nitrogen carbon matrix precursor containing beryllium element, it is heated to 110 DEG C in a nitrogen environment, melt spinning is carried out, with 300m/min's
Winding speed collects a diameter of 20~26 μm of silicon boron nitrogen carbon beryllium presoma as-spun fibre.
(2) as-spun fibre in step (1) is put into tube furnace, volume ratio is passed through as 1 with the speed of 150ml/min:1
The mixed gas of ammonia and nitrogen composition is warming up to 300 DEG C of reaction 6h with the heating rate of 3 DEG C/min, obtains silicon boron nitrogen carbon beryllium
Presoma fusion-free fibre, the Pintsch process under nitrogen atmosphere protection, 1200 DEG C of reactions are warming up to the heating rate of 5 DEG C/min
6h is cooled to room temperature, obtains silicon boron nitrogen carbon beryllium ceramic fibre.The fiber can keep noncrystalline state at 1800 DEG C, at 1500 DEG C not
It is aoxidized, tensile strength 1.2GPa, is less than -8dB in 8.0~18.0GHz frequency range internal reflection rates, there is good wave absorbtion
Energy.
Claims (10)
1. a kind of preparation method of silicon boron nitrogen carbon beryllium ceramic fibre, is as follows：
(1) by nitrogen source, boron source, silicon source, beryllium source and solvent with molar ratio be 12:2:2:1~0.5:120~160 mixing, stirring are anti-
It answers, obtains the silicon boron nitrogen carbon matrix precursor containing beryllium element, melt spinning, winding obtains presoma as-spun fibre；
(2) presoma as-spun fibre in step (1) under the conditions of mixed gas is subjected to cure treatment, obtains crosslinked not melting
Chemical fibre is tieed up, and is then cracked in a nitrogen atmosphere, is cooled to room temperature, obtains silicon boron nitrogen carbon beryllium ceramic fibre.
2. a kind of preparation method of silicon boron nitrogen carbon beryllium ceramic fibre described in accordance with the claim 1, which is characterized in that the step
(1) nitrogen source is hexamethyldisilazane in；Boron source is boron chloride；Silicon source is dichloro methyl silane；Beryllium source is dichloride beryllium；It is molten
Agent is anhydrous n-hexane.
3. a kind of preparation method of silicon boron nitrogen carbon beryllium ceramic fibre described in accordance with the claim 1, which is characterized in that the step
(1) mixing carries out under the conditions of -45~-15 DEG C in.
4. a kind of preparation method of silicon boron nitrogen carbon beryllium ceramic fibre described in accordance with the claim 1, which is characterized in that the step
(1) it is stirred to react specially in：8-12h is stirred, 80~130 DEG C is warming up to 3~5 DEG C/min, keeps the temperature 6~12h, then with 3~5
DEG C/min is warming up to 200~220 DEG C, heat preservation 12~for 24 hours.
5. a kind of preparation method of silicon boron nitrogen carbon beryllium ceramic fibre described in accordance with the claim 1, which is characterized in that the step
(1) temperature of melt spinning is 100~120 DEG C in.
6. a kind of preparation method of silicon boron nitrogen carbon beryllium ceramic fibre described in accordance with the claim 1, which is characterized in that the step
(1) speed wound in is 100-500m/min.
7. a kind of preparation method of silicon boron nitrogen carbon beryllium ceramic fibre described in accordance with the claim 1, which is characterized in that the step
(2) it is 1 that mixed gas, which is volume ratio, in:1-2:1 active gases and inert gas, inert gas are nitrogen or argon gas, activity
Gas is ammonia or boron chloride.
8. a kind of preparation method of silicon boron nitrogen carbon beryllium ceramic fibre described in accordance with the claim 1, which is characterized in that the step
(2) speed that is passed through of mixed gas is 100~300ml/min in.
9. a kind of preparation method of silicon boron nitrogen carbon beryllium ceramic fibre described in accordance with the claim 1, which is characterized in that the step
(2) condition of cure treatment is in：It is warming up to 300~400 DEG C with 2~3 DEG C/min and keeps the temperature 3~6h.
10. a kind of preparation method of silicon boron nitrogen carbon beryllium ceramic fibre described in accordance with the claim 1, which is characterized in that the step
Suddenly the condition of cracking is in (2)：1200~1400 DEG C are warming up to 3~5 DEG C/min, soaking time is 4~8h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109825902A (en) * | 2019-01-31 | 2019-05-31 | 中南大学 | A kind of silicon carbide fibre and preparation method thereof and equipment with the distribution of heterogeneous element gradient |
| CN109837612A (en) * | 2019-01-28 | 2019-06-04 | 江西嘉捷信达新材料科技有限公司 | Beryllium, silicon carbide/boron nitride fiber of hafnium codope and the preparation method and application thereof |
| CN118222866A (en) * | 2024-03-21 | 2024-06-21 | 哈尔滨工业大学 | Preparation method of high-strength interface-combined beryllium-aluminum composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109837612A (en) * | 2019-01-28 | 2019-06-04 | 江西嘉捷信达新材料科技有限公司 | Beryllium, silicon carbide/boron nitride fiber of hafnium codope and the preparation method and application thereof |
| CN109837612B (en) * | 2019-01-28 | 2021-08-27 | 江西嘉捷信达新材料科技有限公司 | Beryllium and hafnium co-doped silicon carbide/boron nitride fiber and preparation method and application thereof |
| CN109825902A (en) * | 2019-01-31 | 2019-05-31 | 中南大学 | A kind of silicon carbide fibre and preparation method thereof and equipment with the distribution of heterogeneous element gradient |
| CN109825902B (en) * | 2019-01-31 | 2021-04-23 | 中南大学 | Silicon carbide fiber with heterogeneous element radial gradient distribution and preparation method and equipment thereof |
| CN118222866A (en) * | 2024-03-21 | 2024-06-21 | 哈尔滨工业大学 | Preparation method of high-strength interface-combined beryllium-aluminum composite material |
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