CN106087112A - A kind of surface has the preparation method of the continuous SiC fiber of carbon-coating - Google Patents

A kind of surface has the preparation method of the continuous SiC fiber of carbon-coating Download PDF

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CN106087112A
CN106087112A CN201610571309.5A CN201610571309A CN106087112A CN 106087112 A CN106087112 A CN 106087112A CN 201610571309 A CN201610571309 A CN 201610571309A CN 106087112 A CN106087112 A CN 106087112A
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carbon
sic fiber
coating
fiber
preparation
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CN106087112B (en
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苟燕子
王浩
王军
王应德
简科
王小宙
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National University of Defense Technology
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/10Artificial 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
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/10Chemical after-treatment of artificial filaments or the like during manufacture of carbon
    • D01F11/16Chemical after-treatment of artificial filaments or the like during manufacture of carbon by physicochemical methods

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Inorganic Fibers (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Ceramic Products (AREA)

Abstract

The present invention provides the preparation method of the continuous SiC fiber that a kind of surface has carbon-coating, and the continuous SiC fiber carbon layer on surface thickness that the method prepares by controlling heating schedule, sintering temperature, temperature retention time and vacuum in sintering process is uniform.

Description

A kind of surface has the preparation method of the continuous SiC fiber of carbon-coating
Technical field
The present invention relates to continuous SiC fiber technical field, be specifically related to a kind of surface and there is the continuous SiC fiber of carbon-coating Preparation method.
Background technology
Continuous SiC fiber has high intensity, high-modulus, high temperature resistant, antioxidation, creep resistant, a series of excellences such as corrosion-resistant Performance, may be used for the fiber reinforcement of the matrixes such as metal, resin, pottery, to prepare high-performance composite materials, in aviation The fields such as space flight, weaponry and nuclear industry are with a wide range of applications.Northeastern Japan university professor Yajima develops the earliest Go out precursor pyrolysis and hot pressing and prepare high-performance continuous SiC fiber (Yajima S, Hasegawa Y, Okamura K, Matsuzawa T,Development of high tensile strength silicon carbide fiber using an Organosilicon polymer precursor.Nature, 1978,273:525-527.), its typical preparation flow is: By organosilicon polymer Pintsch process, reset polycondensation reaction and prepare Polycarbosilane (PCS) as precursor, then PCS is depended on Through melt spinning, cure treatment, pyrolysis be inorganization etc., technical process prepares continuous SiC fiber to sequence.At present, continuous SiC Fiber has been realized in industrialized production, and the SiC ceramic matrix composite material strengthened by continuous SiC fiber has been widely used in aviation The fields such as the heat-resistant part of airspace engine, nuclear reactor material.
Prepare carbon coating on continuous SiC fiber surface, contribute to improving the intensity of continuous SiC fiber further, improving fibre Dimension and the interface of matrices of composite material, and low-fiber resistivity drops.CN201310085507.7 discloses a kind of use Chemical vapour deposition technique (CVD) prepares the method for the continuous SiC fiber of rich surface carbon structure, by high temperature process furnances two ends Use inert atmosphere to carry out sealing gland, and inside arrival end sealing gland, be passed through the gaseous mixture of gaseous alkanes and noble gas, make poly-carbon Silane fusion-free fibre realizes surface deposited carbon layer during high temperature pyrolysis.Patent CN02140433.X discloses a seed coat Core bicomponent fibre method prepares the production technology of continuous carbofrax fibre, is first dissolved by high molecular polymer and makes in a solvent Skin liquid, is then dissolved or dispersed in solvent makes core liquid by dispersant, high molecular polymer, SiC powder, sintering aid, will Skin liquid and core liquid are extruded from the micropore of core-sheath spinning pack under stress, solidify, stretch, are obtained fibril after drying.Will Fibril low-temperature oxidation in atmosphere processes, and in argon gas atmosphere, high temperature sintering obtains that core is SiC fiber and skin zone is carbon Continuous fiber.Patent CN201380026420.0 discloses use and contains Fluohydric acid. and nitric acid, but the aqueous without acetic acid is sour Solution carries out chemical treatment to SiC fiber, thus removes the silicon dioxide being present in fiber surface, and formed≤100nm Microporous carbonaceous layer.
From method therefor in above prior art, with prior aries such as CVD, sheath-core bicomponent method and etching methods Preparing carbon-coating at SiC fiber surface, process conditions are complicated, and are difficult to control the carbon-coating uniformity that fiber surface is formed, therefore, Seriously constrain surface and there is the industrialized production of continuous SiC fiber and the application of carbon-coating.
Summary of the invention
It is an object of the invention to provide the preparation method that a kind of surface has the continuous SiC fiber of carbon-coating, this invention solution Prior art of having determined prepares carbon-coating at SiC fiber surface, and process conditions are complicated, and are difficult to control to what SiC fiber surface was formed The technical problem of carbon-coating uniformity.
The present invention provides the preparation method of the continuous SiC fiber that a kind of surface has carbon-coating, comprises the following steps: by inorganic SiC fiber is incubated 0.5~10 after being warming up to more than 1300 DEG C according to the programming rate of 150~600 DEG C/h in vacuum environment Hour, prepared surface has the SiC fiber of carbon-coating.
Further, the vacuum of vacuum environment is less than 1.01 × 105Pa。
Further, it is warming up to more than 1300 DEG C refer to be warming up to 1300~1900 DEG C.
Further, programming rate is 200~500 DEG C/h.
Further, the preparation of inorganic SiC fiber comprises the following steps: the fusion-free fibre will prepared by PCS polymer Under gaseous environment, rise to 1000~1500 DEG C according to the programming rate of 50~200 DEG C/h, be incubated 0.5~2 hour, system ?;Gas is the group of the one or any kind composition in nitrogen, argon, helium, hydrogen or ammonia.
Another aspect of the present invention additionally provides the surface that a kind of said method prepares, and to have the continuous SiC of carbon-coating fine Dimension, there is carbon-coating in continuous SiC fiber surface.
Further, the thickness of carbon-coating is 1nm~4.5 μm.
Hinge structure, the technique effect of the present invention:
1, the surface that the present invention provides has the preparation method of continuous SiC fiber of carbon-coating, by controlling in sintering process Heating schedule and the thickness of continuous SiC fiber carbon layer on surface prepared of sintering temperature, temperature retention time and vacuum at 1nm~ 4.5 μm on a large scale in adjustable, and the thickness of the formed carbon-coating of this fiber surface is uniformly, without projection or other polymorphic structures, and And be tightly combined with fiber core, thus ensure that the continuous SiC fiber finally given remains in that good mechanical property, ginseng See accompanying drawing 3.
2, the surface that the present invention provides has the preparation method of continuous SiC fiber of carbon-coating, uses routine prepared by fiber Equipment just can be implemented, it is easy to accomplish industrialized production, and the production that continuous SiC fiber that surface have carbon-coating can be greatly lowered becomes This.
3, the surface that the present invention provides has a preparation method of continuous SiC fiber of carbon-coating, simple process, easy to operate, Being easily achieved industrialized production, preparation cost low, obtained continuous SiC fiber mechanical property and heat resistance are good, and surface tool There is carbon-coating.
4, the surface that the present invention provides has the continuous SiC fiber of carbon-coating, and it is continuously adjustable that this fiber surface exists thickness Carbon-coating, so that this fiber has the mechanical property of excellence, and has excellent heat resistance.
Specifically refer to the various realities that the preparation method of the continuous SiC fiber that the surface according to the present invention has carbon-coating proposes Execute the described below of example, by apparent for the above and other aspect making the present invention.
Accompanying drawing explanation
Fig. 1 is that the cross-sectional scans Electronic Speculum of the inorganic SiC fiber prepared in the preferred embodiment of the present invention 1 step (1) is shone Sheet (SEM);
Fig. 2 be in the preferred embodiment of the present invention 1 in step (1) the inorganic SiC fiber of preparation by fiber surface to fibre core The element distribution plots schematic diagram in portion;
Fig. 3 is the cross-sectional scans that the surface prepared in the preferred embodiment of the present invention 1 has the continuous SiC fiber of carbon-coating Electromicroscopic photograph;
Fig. 4 is that in the preferred embodiment of the present invention 1, the surface of preparation has the continuous SiC fiber of carbon-coating by fiber surface to fibre The element distribution plots schematic diagram of dimension core;
Fig. 5 is to drop after the continuous SiC fiber prepared in comparative example 1 is incubated 1 hour at 1800 DEG C in argon gas atmosphere Surface scan electromicroscopic photograph to room temperature.
Detailed description of the invention
The accompanying drawing of the part constituting the application is used for providing a further understanding of the present invention, and the present invention's is schematic real Execute example and illustrate for explaining the present invention, being not intended that inappropriate limitation of the present invention.
The surface that the present invention provides has the preparation method of the continuous SiC fiber of carbon-coating, comprises the following steps: by inorganic SiC fiber is incubated 0.5~10 after being warming up to more than 1300 DEG C according to the programming rate of 150~600 DEG C/h in vacuum environment Hour, prepare described surface and there is the SiC fiber of carbon-coating.
The method that the present invention provides is by the heating schedule in the sintering process to inorganic SiC fiber, sintering temperature, insulation Time and vacuum are controlled, and the oxygen in SiC fiber and element silicon are removed from outside to inside, thus remain at fiber surface Descend carbon, prepared surface and had uniformly and the continuous SiC fiber of thickness continuously adjustabe carbon-coating.And the continuous SiC of gained Fiber also has good mechanical property and heat resistance.The method is by controlling temperature retention time under vacuum conditions, in target Enable to SiC fiber at temperature (i.e. more than 1300 DEG C) and become fiber C, in the extreme case, be equivalent to carbon layer on surface Thickness be exactly the radius of this fiber.
The most inorganic SiC fiber refer to PCS fusion-free fibre through organic-inorganic convert after, mainly by SiC, freedom Carbon and SiCxOyThe SiC fiber of amorphous equal composition.Can be commercially available prod or be prepared by existing conventional method Arrive.
Being preferably, vacuum is less than 1.01 × 105Pa.Now along with the reduction of vacuum, the oxygen in inorganic SiC fiber and The removing speed of element silicon is accelerated, and easier can form carbon-coating at fiber surface.By controlling vacuum within the range, energy Preferably by oxygen and the element silicon removing of SiC fiber sheath, thus form thicker carbon-coating.
Preferably, it is warming up to more than 1300 DEG C refer to be warming up to 1300~1900 DEG C.After being warming up to this temperature, can be conducive to Formed carbon-coating strengthens the mechanical property of gained fiber.
Preferably, programming rate is 200~500 DEG C/h.The resistance to of gained fiber can be improved further by this ramp Warm nature energy.
Preferably, the preparation of inorganic SiC fiber comprises the following steps: existed by the fusion-free fibre prepared by PCS polymer Under gaseous environment, rise to 1000~1500 DEG C according to the programming rate of 50~200 DEG C/h, be incubated 0.5~2 hour, prepare; Gas is the group of the one or any kind composition in nitrogen, argon, helium, hydrogen or ammonia.Inorganic SiC is prepared by this condition Fiber, can improve the mechanical property of gained inorganic SiC fiber, and can regulate and control that it is elementary composition, is more beneficial for follow-up preparation The attachment of the carbon-coating obtained, improves mechanical property and the resistance to elevated temperatures of final continuous SiC fiber.
PCS polymer used herein refers to through cracking and be reset the poly-carbon silicon that conversion obtains by polydimethylsiloxane Alkane, or by Polycarbosilane and ferrocene, FeCl3、AlCl3、Al(AcAc)3、Al(OR)3、B(OR)3、Ti(OR)4、Zr (OR)4、Zr(AcAc)4In (R=Me, Et, Pt, Bt or Ph) one or more compounds reaction prepare containing Fe, Al, B, The Polycarbosilane of the heterogeneous elements such as Ti or Zr, or other contains the preceramic polymer of SiC ceramic of Si and C element.When So PCS polymer can also be this commercially available series products.
The fusion-free fibre prepared by PCS polymer herein refers to be first passed through melt spinning by PCS polymer, dry method is spun The spinning modes such as silk, wet spinning, electrostatic spinning prepare PCS fibril, the most again PCS fibril are placed in non-fusible place In reason device, it is passed through air or reactive atmosphere cross-links, or use electron beam irradiation to cross-link, prepare non-fusible fibre Dimension.
Another aspect of the present invention additionally provides a kind of surface prepared as stated above and has the continuous SiC of carbon-coating Fiber.This fiber is owing to have employed above-mentioned preparation method so that the thickness of gained carbon-coating is 1nm~4.5 μm, thus realizes at this Interior continuously adjustabe, and thickness is uniform, and also carbon-coating is tightly combined with SiC fiber core so that it is there is more excellent power Learn performance and resistance to elevated temperatures, thus gained fiber is different from existing continuous SiC fiber.
Preferably, the carbon layers having thicknesses on gained continuous SiC fiber surface be 1nm~4.5 μm on a large scale in adjustable.
Concrete the method comprises the following steps:
(1) fusion-free fibre prepared by PCS polymer is placed in graphite furnace, is passed through gas, according to 50~200 DEG C/ Hour programming rate rise to 1000~1500 DEG C, be incubated 0.5~2 hour, prepare inorganic SiC fiber;
(2) inorganic SiC fiber is placed in pyrographite stove, is evacuated to certain vacuum degree, then according to 150~600 DEG C/h programming rate rise to 1300~1900 DEG C, be incubated 0.5~10 hour, prepared surface has the SiC fiber of carbon-coating.
Further, in step (1), described gas refers to one or several in nitrogen, argon, helium, hydrogen, ammonia Gaseous mixture.Certain vacuum degree is meant less than 1.01 × 105Pa is i.e. less than a normal atmosphere.
The method that the present invention provides is by PCS fusion-free fibre, by inorganization process, high temperature under vacuum Burn till, thus surface must be arrived there is the continuous SiC fiber of carbon-coating.
Embodiment
In following example, material used and instrument are commercially available.
Reference example 1
By by the polydimethylsiloxane Polycarbosilane that process cracking and rearrangement conversion obtain under constant-pressure and high-temperature, (softening point is 215 DEG C, number-average molecular weight is 1.68 × 103G/mol, molecular weight distribution index is 2.82) it is placed in the molten cylinder of melt spinning device In, under nitrogen atmosphere is protected, it is heated to 320 DEG C, after it is melted into improving uniformity of melt completely, at 289 DEG C, 0.4MPa Pressure under, carry out drawing-off spinning with the speed of 400m/ minute, obtain the continuous P CS fibril that average diameter is 12um.Will PCS fibril prepares fusion-free fibre afterwards through electron beam irradiation (electron beam line is 3mA, and total exposure time is 9 hours).
Embodiment 1
(1) fusion-free fibre of preparation in reference example 1 is placed in graphite furnace, is passed through the gaseous mixture (hydrogen of nitrogen and hydrogen It is 85% that gas accounts for the volume ratio of gaseous mixture), rise to 1000 DEG C with the programming rate of 80 DEG C/h, be incubated 1 hour, prepare inorganic SiC fiber.(2) inorganic SiC fiber is placed in pyrographite stove, evacuation, makes vacuum reach 6Pa, then according to 300 DEG C/h programming rate rise to 1900 DEG C, be incubated 1 hour, prepared surface has the continuous SiC fiber of carbon-coating.
Fig. 1 is the cross-sectional scans electromicroscopic photograph of the inorganic SiC fiber of preparation in the embodiment of the present invention 1 step (1), can by figure Seeing, fibre section smooth even, fiber surface does not has obvious carbon-coating interface.
Fig. 2 be in the embodiment of the present invention 1 in step (1) the inorganic SiC fiber of preparation by fiber surface to fiber core Element distribution plots, as seen from the figure, although in the range of fiber surface 10nm, rich carbon is oxygen-enriched, but from the scope of 10 to 200nm In, fiber composition is Silicon-rich, and therefore, the surface further demonstrating gained inorganic SiC fiber does not has carbon-coating.
Fig. 3 is the cross-sectional scans electromicroscopic photograph of the continuous SiC fiber that the surface of preparation has carbon-coating in the embodiment of the present invention 1 (SEM), as seen from the figure, this fiber surface and core have obvious interface to occur, illustrate that this fiber surface defines uniform carbon Layer.
Fig. 4 is that in the embodiment of the present invention 1, the surface of preparation has the continuous SiC fiber of carbon-coating by fiber surface to fibre core The element distribution plots in portion, in the range of surface to core 200nm, is that the content of carbon, silicon and oxygen almost can be ignored not entirely Meter.It follows that formed carbon-coating at Fig. 3 continuous SiC fiber fiber surface, and it can be seen from figure 3 that this carbon-coating dense uniform, About thickness about 1 μm.
Embodiment 2
The inorganic SiC fiber of preparation in embodiment 1 step (1) is placed in pyrographite stove, evacuation, makes vacuum reach To 28Pa, rising to 1800 DEG C according to the programming rate of 260 DEG C/h, be incubated 1 hour, prepared surface has the continuous SiC of carbon-coating Fiber.
Embodiment 3
The inorganic SiC fiber of preparation in embodiment 1 step (1) is placed in pyrographite stove, evacuation, makes vacuum reach To 350Pa, rising to 1700 DEG C according to the programming rate of 230 DEG C/h, be incubated 2 hours, prepared surface has the continuous of carbon-coating SiC fiber.
Embodiment 4
(1) fusion-free fibre of preparation in reference example 1 is placed in graphite furnace, is passed through nitrogen, with the liter of 150 DEG C/h Temperature speed rises to 1500 DEG C, is incubated 1 hour, prepares inorganic SiC fiber.(2) inorganic SiC fiber is placed in pyrographite stove, Evacuation, makes vacuum reach 80Pa, rises to 1700 DEG C according to the programming rate of 200 DEG C/h, is incubated 1 hour, prepares surface There is the continuous SiC fiber of carbon-coating.
Reference example 2
By by the PCS polymer of Polycarbosilane and the synthesis of 2% aluminium acetylacetonate, (softening point is 217 DEG C, and number-average molecular weight is 4110g/mol, molecular weight distribution index is 1.81) be placed in the molten cylinder of melt spinning device, heat under inert atmosphere protection Be warming up to 362 DEG C, after it is melted into improving uniformity of melt completely, 287 DEG C, under the pressure of 0.5MPa, with the speed of 420m/ minute Degree carries out drawing-off spinning, obtains the PCS fibril that average diameter is 13um.PCS fibril is placed in air curing and processes dress Carry out cure treatment in putting, within 1 hour, rise to 100 DEG C and be incubated 2 hours, then rising to 210 with the programming rate of 12 DEG C/h DEG C, it is down to room temperature after being incubated 1 hour at 210 DEG C and prepares fusion-free fibre.
Reference example 1 is the PCS polymer that the cracking polymerization of usual polydimethylsiloxane is formed.It is poly-carbon silicon referring to example 2 The PCS polymer formed after alkane and acetylacetone,2,4-pentanedione reactive aluminum.
Embodiment 5
(1) fusion-free fibre of preparation in reference example 2 is placed in graphite furnace, is passed through nitrogen, with the liter of 120 DEG C/h Temperature speed rises to 1300 DEG C, is incubated 1 hour, prepares inorganic SiC fiber.(2) inorganic SiC fiber is placed in pyrographite stove, Evacuation, makes vacuum reach 5000Pa, rises to 1900 DEG C according to the programming rate of 200 DEG C/h, is incubated 1 hour, prepares table Mask has the continuous SiC fiber of carbon-coating.
Embodiment 6
(1) fusion-free fibre of preparation in reference example 2 is placed in graphite furnace, is passed through nitrogen, with the liter of 110 DEG C/h Temperature speed rises to 1300 DEG C, is incubated 1 hour, prepares inorganic SiC fiber.(2) inorganic SiC fiber is placed in pyrographite stove, Evacuation, makes vacuum reach 800Pa, rises to 1600 DEG C according to the programming rate of 200 DEG C/h, is incubated 0.5 hour, prepares Surface has the continuous SiC fiber of carbon-coating.
Embodiment 7
(1) being placed in graphite furnace by the fusion-free fibre of preparation in reference example 2, (hydrogen accounts for mixing to be passed through nitrogen and hydrogen The volume ratio of gas is 25%), rise to 1500 DEG C with the programming rate of 200 DEG C/h, be incubated 0.5 hour, prepare inorganic SiC fine Dimension.(2) inorganic SiC fiber is placed in pyrographite stove, evacuation, makes vacuum reach 0.002Pa, according to 600 DEG C/h Programming rate rise to 1900 DEG C, be incubated 10 hours, prepared surface has the continuous SiC fiber of carbon-coating.
Embodiment 8
(1) being placed in graphite furnace by the fusion-free fibre of preparation in reference example 2, (ammonia accounts for mixing to be passed through argon and ammonia The volume ratio of gas is 10%), rise to 1000 DEG C with the programming rate of 50 DEG C/h, be incubated 2 hours, prepare inorganic SiC fiber. (2) inorganic SiC fiber is placed in pyrographite stove, evacuation, makes vacuum reach 5Pa, according to the intensification of 150 DEG C/h Speed rises to 1300 DEG C, is incubated 1 hour, and prepared surface has the continuous SiC fiber of carbon-coating.
Embodiment 9
Difference with embodiment 4 is: vacuum is 5.0 × 104Pa。
Comparative example 1
Difference with embodiment 2 is: inorganic SiC fiber in vacuum environment according to the programming rate liter of 100 DEG C/h Temperature is incubated after 1000 DEG C.
Comparative example 2
Difference with embodiment 2 is: inorganic SiC fiber in vacuum environment according to the programming rate liter of 350 DEG C/h Temperature is incubated after 2000 DEG C.
Embodiment 1~8 and comparative example 1~2 in the mechanics of gained continuous SiC fiber and heat resistance be shown in Table 1.Fiber Diameter measured by micrometer caliper, and the mechanical property of fiber is recorded by ultimate fibre electronics strength tester.Melted highly basic dissolves sample Product, analyze the silicone content in fiber with colorimetric determination, and carbon and oxygen content are surveyed by C/S analyser and N/O analyser the most respectively ?.
The surface prepared in embodiment 2 has the continuous SiC fiber of carbon-coating, is incubated in argon gas atmosphere at 1800 DEG C Being down to room temperature after 1 hour, recording its strength retention ratio is 82%, and this fiber has the resistance to elevated temperatures of excellence.
Although fiber intensity is higher obtained by comparative example 1, but because its preparation temperature is the lowest, there is not carbon-coating in surface.At argon Being down to room temperature after being incubated 1 hour at 1800 DEG C in gas atmosphere, this fiber turns green efflorescence, and as shown in Figure 5, in comparative example, 1 gained is fine Dimension structure is at such a temperature by high temperature, no longer fine and close, loses intensity completely.
The fiber obtained in comparative example 2, although surface has carbon-coating, but owing to preparation temperature is the highest, fibre strength is significantly Decline (seeing table 1), had a strong impact on the application of fiber.
Table 1 embodiment 1~8 and comparative example 1~2 in the mechanics of gained continuous SiC fiber and heat resistance table
As shown in Table 1, the method that the present invention provides can prepare surface and have the carbon-coating of uniform thickness, and oxygen content also can simultaneously Preferably controlled, so that the combination property such as the mechanical property of gained fiber and resistance to elevated temperatures is superior to comparative example 1 ~gained fiber in 2.Carbon layers having thicknesses, under different sintering conditions, can carry out artificial adjustment so that it is have controllability.
Those skilled in the art will understand that the scope of the present invention is not restricted to example discussed above, it is possible to carries out it Some changes and amendment, the scope of the present invention limited without deviating from appended claims.Although in accompanying drawing and explanation Book illustrates and describes the present invention in detail, but such explanation and description are only explanations or schematic, and 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 are permissible Understand and realize the deformation of the disclosed embodiments.In detail in the claims, term " includes " being not excluded for other steps or element, And indefinite article " " or " a kind of " are not excluded for multiple.Some measure quoted in mutually different dependent claims The fact does not means that the combination of these measures can not be advantageously used.It is right that any reference marker in claims is not constituted The restriction of the scope of the present invention.

Claims (7)

1. a surface has the preparation method of continuous SiC fiber of carbon-coating, it is characterised in that comprise the following steps: by inorganic SiC fiber is incubated 0.5~10 after being warming up to more than 1300 DEG C according to the programming rate of 150~600 DEG C/h in vacuum environment Hour, prepare described surface and there is the SiC fiber of carbon-coating.
Surface the most according to claim 1 has the preparation method of the continuous SiC fiber of carbon-coating, it is characterised in that described The vacuum of vacuum environment is less than 1.01 × 105Pa。
Surface the most according to claim 1 has the preparation method of the continuous SiC fiber of carbon-coating, it is characterised in that described It is warming up to more than 1300 DEG C refer to be warming up to 1300~1900 DEG C.
Surface the most according to claim 1 has the preparation method of the continuous SiC fiber of carbon-coating, it is characterised in that described Programming rate is 200~500 DEG C/h.
5. have the preparation method of the continuous SiC fiber of carbon-coating according to the surface according to any one of Claims 1 to 4, it is special Levying and be, the preparation of described inorganic SiC fiber comprises the following steps: by the fusion-free fibre prepared by PCS polymer at gas Under environment, rise to 1000~1500 DEG C according to the programming rate of 50~200 DEG C/h, be incubated 0.5~2 hour, prepare;
Described gas is the group of the one or any kind composition in nitrogen, argon, helium, hydrogen or ammonia.
6. the surface that method as according to any one of Claims 1 to 5 prepares has a continuous SiC fiber for carbon-coating, It is characterized in that, there is carbon-coating in described continuous SiC fiber surface.
Surface the most according to claim 6 has the continuous SiC fiber of carbon-coating, it is characterised in that the thickness of described carbon-coating For 1nm~4.5 μm.
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JP2020066812A (en) * 2018-10-23 2020-04-30 日本特殊陶業株式会社 Composite fiber and fiber bundle

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