CN106948031A - The preparation method of ultra-fine tow silicon carbide fibre - Google Patents
The preparation method of ultra-fine tow silicon carbide fibre Download PDFInfo
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- CN106948031A CN106948031A CN201710307212.8A CN201710307212A CN106948031A CN 106948031 A CN106948031 A CN 106948031A CN 201710307212 A CN201710307212 A CN 201710307212A CN 106948031 A CN106948031 A CN 106948031A
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- silicon carbide
- carbide fibre
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- 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
- D01F9/10—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material by decomposition of organic substances
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
Abstract
The present invention provides a kind of preparation method of ultra-fine tow silicon carbide fibre, raw material will be used as using Polycarbosilane (PCS), from the small silk number spinneret that hole count is less than 200, continuous P CS fibers are made by melt spinning, continuous P CS fibers are subjected to radiation annealing processing and are changed into PCS fusion-free fibres, by PCS fusion-free fibres by pre-burning under more than 1000 DEG C inert atmospheres, then by being burnt eventually under more than 1400 DEG C inert atmospheres, prepare the SiC fibers of ultra-fine tow.The ultra-fine tow silicon carbide fibre prepared, on the basis of 11 12 μm of fibre diameter is ensured, number of fiber is controlled below 200.
Description
Technical field
The present invention relates to high-performance ceramic fiber technical field, a kind of system of ultra-fine tow silicon carbide fibre is specifically related to
Preparation Method.
Background technology
The core of Nuclear Safety is to prevent that the radioactive fission product in reactor from leaking into the environment of surrounding.Core fires
Expect that involucrum is one of key core part of power producer, its effect is to prevent the effusion of fission product, keep fuel rod
Integrality.Cladding materials is operated under high temperature and radiation parameter, and operating condition is very harsh, it is desirable to which material has small neutron
The characteristic such as absorption cross-section, high thermal conductivity factor, intensity height, good toughness, corrosion-resistant, Flouride-resistani acid phesphatase, heat endurance be good.Nuclear energy it is advanced
Property, security reliability and economy and the performance of cladding materials used are closely related.The current second generation and three generations's nuclear reactor are more
Using zircaloy as cladding materials, but because zircaloy can be undergone phase transition more than 450 DEG C, more than 1093 DEG C can occur zirconium with water
Water reacts, and reduces material hardness, makes material easy to wear, long-term also because of hydrogen abstraction reaction cladding materials to be caused crisp using zircaloy
Change.Particularly under major accident operating mode, the reaction of zirconium water can produce substantial amounts of hydrogen, and detonation can occur under given conditions or quick-fried
It is fried, seriously jeopardize the integrality of nuclear island factory building and facility.U.S.'s Three Mile Island nuclear accident and Fukushima, Japan core all demonstrate zircaloy
The limitation of core structural material.
Relative to Zirconium alloy material, SiC fiber reinforcement SiC based composites (SiC/SiC) are applied to have in cladding materials
There is the advantage of following aspect：
1) heat resistance is good, can be used for a long time in the environment of 800 DEG C in nuclear reactor environment as cladding materials, short
Phase can bear 1200 DEG C of high temperature, improve the security of reactor；
2) slowing down absorptance is good, and parasitic thermal neutron absorbs cross section compared with zircaloy reduction by more than 15%, using same uranium
During 235 fuel (enrichment 5%), fuel burn-up can bring up to 70000MWD/tU by 60000MWD/tU；
3) hardness is high, can effectively reduce due to the abrasion that fragment in cooling agent and grid exist and caused, extend fuel
Rod service life and reactor normal working hours.
Just because of these features of SiC/SiC composites, SiC/SiC composites fuel can is in nuclear power system field
Have broad application prospects.
At present, SiC/SiC composites are as the research in terms of nuclear fuel pencil cladding also in the starting stage, and existing core fires
The design size of charge bar cladding tubes：External diameter about 10mm, wall thickness design about 0.8mm, using " sandwich " interlayer structure form, centre
Layer choosing is supported with SiC/SiC composites there is provided main mechanical property, and thickness is 0.4~0.6mm；The both sides choosing in intermediate layer
With CVD SiC coatings.
At present, the SiC fibers of external commercialization include：The Nicalon series SiC fibers of Japanese carbon company, Japan
The Tyranno series SiC fibers and the Sylramic fibers of COI Ceramic companies of the U.S. of Yu Buxingchan companies.Wherein,
Nicalon a diameter of 12-14 μm of silicon carbide fibres of series, number of fiber is 0.5K.In Tyranno series SiC fibers, LOX
M fibers, ZMI fibers and SA-1 fibre diameters are 10-11 μm, and number of fiber is 0.8K；S and SA-3 fibre diameters are 7.5-8.5 μ
M, number of fiber is 1.6K.Sylramic fibre diameters are 10 μm, and number of fiber is 1.6K.The life of domestic SiC fibers mainly
Producing unit includes the National University of Defense technology, Xiamen University and Suzhou Cerafil Ceramic Fiber Co., Ltd..Wherein, the National University of Defense technology produces
KD series SiC fibers it is main based on 0.5K and 1K, fibre diameter is 11-12 μm；Xiamen University mainly produces 0.5K SiC
Fiber, fibre diameter is 12-14 μm；Suzhou Cerafil Ceramic Fiber Co., Ltd. mainly produces 1K SiC fibers, and fibre diameter is
11-12μm。
From above-mentioned existing SiC fibers situation：Although the diameter and tow of SiC fibers prepared by domestic and international constituent parts are deposited
In difference, but take fibre bundle number and diameter influence into consideration, fiber linear density is closer to, typically in 180-300g/km
Scope, fiber linear density is approached, and tow sectional area is close, can be that follow-up braiding and the development of SiC/SiC composites are provided
It is convenient.
It is different from the demand of the part such as Aeronautics and Astronautics, when SiC/SiC composites are applied to nuclear fuel pencil cladding, pipeline
The wall thickness of component only has 0.4-0.6mm, and the thickness in monolayer scope of the SiC fibre bundles produced both at home and abroad at present is in 0.3-
0.5mm, can be used in the fiber of carrying less than 2 layers on composite material conduit section.Therefore, more filaments bundles are prepared
SiCSiC/SiC composite fibers, are premise and the basis for preparing nuclear fuel pencil cladding SiC/SiC composites.At present,
The production of SiC fibers yet there are no document report below 0.5K numbers.
The content of the invention
It is an object of the invention to provide a kind of preparation method of ultra-fine tow silicon carbide fibre, the invention solves existing
Bearing capacity can not meet nuclear fuel pencil cladding and want when SiC/SiC composite fibers are used directly as nuclear fuel pencil cladding
Ask；Existing SiC/SiC composite fibers diameter is excessively thick, and the skill of nuclear fuel pencil cladding intensity requirement can not be met after thickness
Art problem.
The silicon carbide fibre thinner in order to obtain tow：One kind is to reduce fibre diameter, and another is to reduce number of fiber.
An aspect of of the present present invention provides a kind of preparation method of ultra-fine tow silicon carbide fibre, comprises the following steps：It is right
Polycarbosilane (PCS) precursor carries out melt spinning, radiation annealing processing and obtains PCS fusion-free fibres, right under an inert atmosphere
The PCS fusion-free fibres sequentially carry out pre-burning and burnt eventually, prepare the SiC fibers of ultra-fine tow；The softening point of the PCS
For 200-250 DEG C, molecular weight distribution index is less than 4, and oxygen content is less than 0.5wt%；Spinneret used in the fusing spinning step
Plate hole number is less than 200；Fusing spinning step parameter：It is 400-800m/ minutes to receive silk speed, and pressure is 0.2-0.6MPa, temperature
Spend for 270-320 DEG C.The calcined temperature is more than 1000 DEG C；The temperature of burning eventually is more than 1400 DEG C.
The step of not being described in detail in this method is operated by existing method.On the one hand this method is entered by small silk number spinneret
Row PCS melt spinnings, prepare the PCS fibers of small silk number；Two be by PCS fibers by cross-linking radiation, pre-burning after, pass through
Burn eventually and prepare ultra-fine tow SiC fibers.Softening point, the molecular distribution for the PCS that polycondensation reaction is obtained are reset to cracking simultaneously
Coefficient and oxygen content are controlled, so that small silk number spinneret is passed through, so as to obtain the PCS fibers of small silk number.So as to
It ensure that the silk number and filament diameter of final gained silicon carbide fibre reach requirement.So as to which the obtained nuclear fuel pencil cladding that can meet will
The material asked.Coordinate fusing spinning step parameter while using small silk number spinneret, gained silicon carbide fibre can just expired
The requirement of sufficient nuclear fuel pencil cladding.By controlling to burn eventually and calcined temperature so that the high temperature strength of gained fusion-free fibre is obtained
To raising.
PCS used can be it is commercially available and meet the softening point, the finished product of molecular weight distribution index requirement, can also be by following
Step is prepared：Take polydimethylsiloxane 1000g to be placed in reactor, be passed through after high pure nitrogen displaced air, be slowly heated
To 460 DEG C, and at such a temperature, heat preservation hot depolymerizes 4 hours.Crude product is dissolved in after dimethylbenzene and filtered, and is again heated to 350 DEG C,
Filtrate carries out vacuum distillation 30 minutes at 350 DEG C, and light yellow resin shape Polycarbosilane PCS is obtained after cooling.
Further, spinneret hole count is 50~200.Using this thread number, the more preferable carborundum of mechanical property can be obtained fine
Dimension.The intensity of gained silicon carbide fibre reaches maximum.
Further, the aperture of spinneret is 15-25 μm.It can guarantee that filament diameter reaches requirement in gained fibre bundle.
Further, radiation annealing parameter：Irradiation dose is to be incubated 1-2 hours at 15-25MGry, 450-500 DEG C of temperature.
Be conducive to improving the monofilament mechanical strength of gained fiber.
Further, calcined temperature is 1000-1400 DEG C.Advantageously reduce the oxygen content of resulting materials.
Further, the parameter of step is burnt eventually：Temperature is 1400-1800 DEG C, and tension force 0.05-0.8N is burnt eventually, wire is burnt eventually
Speed is 0.5-4m/ minutes；Inert atmosphere used is nitrogen, the argon that purity is more than 99.999% in burn in step and eventually burning step
Gas or helium.
Whole burn herein refers to control filametntary tension force during burning eventually by putting gauze frame, controlled by five roller drawing-offs
Filametntary wire travelling speed during burning eventually.
Another aspect of the present invention additionally provides a kind of ultra-fine tow silicon carbide fibre, is prepared by above-mentioned method.
Further, the filament strength of ultra-fine tow silicon carbide fibre is more than 2.8GPa, and synnema intensity is more than 2.5GPa, fine
Tie up oxygen content and be less than 1wt%, the monofilament of the ultra-fine tow silicon carbide fibre is strong after being incubated 1 hour under 1400 DEG C of inert atmospheres
Spend retention rate and be more than 80%.
Further, the thickness of the ultra-fine tow silicon carbide fibre is 0.05-0.1mm after compacting.Obtained carbonization
Silica fibre thickness meets nuclear fuel pencil cladding requirement, while having required mechanical property.
The technique effect of the present invention：
1st, the present invention provides the preparation method of ultra-fine tow silicon carbide fibre, by from the small silk that hole count is less than 200
Number spinneret, the quantity to gained continuous P CS fibers is controlled, and prepares a diameter of 11-12 μm, number of fiber is 200
The SiC fibers of following ultra-fine tow.
2. the present invention provides the preparation method of ultra-fine tow silicon carbide fibre, technique is simple and convenient to operate, is not required to increase high
Expensive equipment, just it can be implemented using the production equipment of current second generation continuous SiC fiber.
3. the present invention provide in ultra-fine tow silicon carbide fibre, it is fine with good mechanical property and resistance to elevated temperatures
Tie up filament strength and be more than 2.8GPa, synnema intensity is more than 2.5GPa, and fiber oxygen content is less than under 1wt%, 1400 DEG C of inert atmospheres
Strength retention ratio is more than 80% after being incubated 1 hour.
4. the present invention provide in ultra-fine tow silicon carbide fibre, compacted depth scope is in 0.05-0.1mm, fiber lousiness
And little breakage, compliance is very good, is to prepare SiC/SiC composite nuclear fuel pencil claddings with good woven performance
Suitable reinforcement fibers.
The specific various embodiments that refer to the preparation method proposition according to the ultra-fine tow silicon carbide fibre of the present invention
It is described below, will be apparent in terms of the above and other for causing the present invention.
Brief description of the drawings
Fig. 1 is the light photo for the ultra-fine tow silicon carbide fibre that the embodiment of the present invention 1 is prepared.
Embodiment
The accompanying drawing for constituting the part of the application is used for providing a further understanding of the present invention, schematic reality of the invention
Apply example and its illustrate to be used to explain the present invention, do not constitute inappropriate limitation of the present invention.
Embodiment
Material and instrument used are commercially available in following examples.
Embodiment 1
Take polydimethylsiloxane 1000g to be placed in reactor, be passed through after high pure nitrogen displaced air, be heated slowly to 460
DEG C, and heat preservation hot depolymerizes 4 hours at such a temperature.Crude product is dissolved in after dimethylbenzene and filtered, and is again heated to 350 DEG C, filtrate
Vacuum distillation 30 minutes is carried out at 350 DEG C, light yellow resin shape Polycarbosilane PCS is obtained after cooling, its softening point is 208-231
DEG C, molecular weight distribution index 2.6, oxygen content 0.35wt%.
The PCS of synthesis is placed in melt spinning device (spinneret hole count is 200 holes, and aperture is 20 μm), in High Purity Nitrogen
Gas shielded, under the conditions of 300 DEG C, with 600m/ minutes speed melt spinnings, prepares 200 continuous P CS fibers, fiber is average
13.0 μm of diameter.
PCS fibers are passed through into radiation annealing, irradiation dose selects 15MGry, and annealing temperature selects 450 DEG C, soaking time choosing
With 2h, PCS fusion-free fibres are made.By the pre-burning under 1200 DEG C, high pure nitrogen protective condition of PCS fusion-free fibres, obtain pre-
Burn fiber.
By pre-burning fiber under 1600 DEG C, high-purity argon gas protective condition, continuously burnt eventually with 2m/ minutes speed, tension force is burnt eventually
Control prepares 200 SiC fibers in 0.8N.
The performance of fiber is as shown in table 1 prepared by embodiment 1.
The key property of SiC fibers (200) prepared by the embodiment 1 of table 1
Fiber lousiness and little breakage prepared by embodiment 1, compliance are very good, with good woven performance.Fiber
Thickness in monolayer is about 0.15mm.It is the suitable reinforcement fibers for preparing SiC/SiC composite nuclear fuel pencil claddings.
Embodiment 2
PCS preparation method is same as Example 1.
The PCS of synthesis is placed in melt spinning device (spinneret hole count is 100 holes, and aperture is 15 μm), in High Purity Nitrogen
Gas shielded, under the conditions of 300 DEG C, with 400m/ minutes speed melt spinnings, prepares 0.1K continuous P CS fibers, fiber is average
11.9 μm of diameter.
PCS fibers are passed through into radiation annealing, irradiation dose selects 20MGry, and annealing temperature selects 500 DEG C, soaking time choosing
With 1h, PCS fusion-free fibres are made.By the pre-burning under 1000 DEG C, high-purity argon gas protective condition of PCS fusion-free fibres, obtain pre-
Burn fiber.
By pre-burning fiber under 1400 DEG C, high-purity argon gas protective condition, continuously burnt eventually with 4m/ minutes speed, tension force is burnt eventually
Control prepares 0.1K SiC fibers in 0.2N.
The performance of fiber is as shown in table 2 prepared by embodiment 2.
The key property of SiC fibers (0.1K) prepared by the embodiment 2 of table 2
Fiber lousiness and little breakage prepared by embodiment 2, compliance are very good, with good woven performance.Fiber
Thickness in monolayer is about 0.11mm.It is the suitable reinforcement fibers for preparing SiC/SiC composite nuclear fuel pencil claddings.
Embodiment 3
PCS preparation method is same as Example 1.
The PCS of synthesis is placed in melt spinning device (spinneret hole count is 50 holes, and aperture is 25 μm), in high pure nitrogen
Protect, under the conditions of 300 DEG C, with 800m/ minutes speed melt spinnings, prepare 0.05K continuous P CS fibers, fiber is average
15.3 μm of diameter.
PCS fibers are passed through into radiation annealing, irradiation dose selects 25MGry, and annealing temperature selects 500 DEG C, soaking time choosing
With 2h, PCS fusion-free fibres are made.By the pre-burning under 1400 DEG C, high-purity helium protective condition of PCS fusion-free fibres, obtain pre-
Burn fiber.
By pre-burning fiber under 1800 DEG C, high-purity helium protective condition, continuously burnt eventually with 0.5m/ minutes speed, burn open eventually
Power is controlled in 0.05N, prepares 0.05K SiC fibers.
The performance of fiber is as shown in table 3 prepared by embodiment 3.
The key property of SiC fibers (0.05K) prepared by the embodiment 3 of table 3
Fiber lousiness prepared by embodiment 3 and broken end are less, and compliance is preferable, with preferable woven performance.Fiber
Thickness in monolayer is about 0.08mm.It may be used as the reinforcing fiber of SiC/SiC composite nuclear fuel pencil claddings.
From the result of embodiment 1~3 can be seen that can from PCS precursors, by regulating and controlling spinneret hole quantity,
Control spinning temperature, the technological parameter such as speed, prepare small silk number PCS fibers, then process radiation annealing realize it is non-fusible, in advance
Burn and prepare ultra-fine tow SiC fibers after burning eventually.
SiC fibers are prepared using the inventive method, without changing main process equipment prepared by current SiC fibers, and
The fibrous mechanical property of preparation is excellent, and oxygen content is low, and tow is thin, and lousiness and little breakage, compliance are good, are woven with good
Performance, is the suitable reinforcement fibers for preparing SiC/SiC composite nuclear fuel pencil claddings, is had in advanced nuclear energy field good
Application prospect, can also be applied to the field such as high-performance weaponry, Aeronautics and Astronautics ultra-thin Si C/SiC composite structures
The development of part.
Those skilled in the art will be clear that the scope of the present invention is not restricted to example discussed above, it is possible to which it is carried out
Some changes and modification, the scope of the present invention limited without departing from appended claims.Although oneself is through in accompanying drawing and explanation
The present invention is illustrated and described in book in detail, but such explanation and description are only explanations or schematical, and it is nonrestrictive.
The present invention is not limited to the disclosed embodiments.
By to accompanying drawing, the research of specification and claims, when implementing the present invention, those skilled in the art can be with
Understand and realize the deformation of the disclosed embodiments.In detail in the claims, term " comprising " is not excluded for other steps or element,
And indefinite article " one " or " one kind " be not excluded for it is multiple.The some measures quoted in mutually different dependent claims
The fact does not mean that the combination of these measures can not be advantageously used.Any reference marker in claims is not constituted pair
The limitation of the scope of the present invention.
Claims (9)
1. a kind of preparation method of ultra-fine tow silicon carbide fibre, it is characterised in that comprise the following steps：PCS is sequentially carried out
Melt spinning, radiation annealing processing obtain PCS fusion-free fibres, and the PCS fusion-free fibres are sequentially entered under an inert atmosphere
Row pre-burning and eventually burning, prepare the SiC fibers of ultra-fine tow；
Spinning jet used hole count is less than 200 in the fusing spinning step；
The temperature of burning eventually is more than 1400 DEG C；
The calcined temperature is more than 1000 DEG C；
Polycondensation reaction is reset through the cracking and obtains PCS, and the softening point of the PCS is 200-250 DEG C, and molecular weight distribution index is small
In 4, oxygen content is less than 0.5wt%；
The fusing spinning step parameter：It is 400-800m/ minutes to receive silk speed, and pressure is 0.2-0.6MPa, and temperature is 270-
320℃。
2. the preparation method of ultra-fine tow silicon carbide fibre according to claim 1, it is characterised in that the spinneret hole
Number is 50~200.
3. the preparation method of ultra-fine tow silicon carbide fibre according to claim 1, it is characterised in that the spinneret
Aperture is 15-25 μm.
4. the preparation method of ultra-fine tow silicon carbide fibre according to claim 1, it is characterised in that the radiation annealing
Parameter：Irradiation dose is to be incubated 1-2 hours at 15-25MGry, 450-500 DEG C of temperature.
5. the preparation method of ultra-fine tow silicon carbide fibre according to claim 1, it is characterised in that the calcined temperature
For 1000-1400 DEG C.
6. the preparation method of ultra-fine tow silicon carbide fibre according to claim 1, it is characterised in that described to burn step eventually
Parameter：Temperature is 1400-1800 DEG C, and tension force 0.05-0.8N is burnt eventually, and it is 0.5-4m/ minutes that wire travelling speed is burnt eventually；
Inert atmosphere used is nitrogen, argon gas or the helium that purity is more than 99.999% in the burn in step and the step of burning eventually
Gas.
7. a kind of ultra-fine tow silicon carbide fibre, it is characterised in that by method system such as according to any one of claims 1 to 6
It is standby to obtain.
8. ultra-fine tow silicon carbide fibre according to claim 7, it is characterised in that the ultra-fine tow silicon carbide fibre
Filament strength be more than 2.8GPa, synnema intensity be more than 2.5GPa, oxygen content be less than 1wt%, under 1400 DEG C of inert atmospheres protect
The filament strength retention rate of temperature ultra-fine tow silicon carbide fibre after 1 hour is more than 80%.
9. ultra-fine tow silicon carbide fibre according to claim 7, it is characterised in that the ultra-fine tow carbonization after compacting
The thickness of silica fibre is 0.05-0.1mm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109695071A (en) * | 2018-12-27 | 2019-04-30 | 苏州赛力菲陶纤有限公司 | A kind of durothermic method of raising continuous carbofrax fibre |
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