CN108193325A - High temperature resistant SiC fibers containing zirconium and preparation method thereof - Google Patents
High temperature resistant SiC fibers containing zirconium and preparation method thereof Download PDFInfo
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- CN108193325A CN108193325A CN201711449898.0A CN201711449898A CN108193325A CN 108193325 A CN108193325 A CN 108193325A CN 201711449898 A CN201711449898 A CN 201711449898A CN 108193325 A CN108193325 A CN 108193325A
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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
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/24—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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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
- D01D5/084—Heating filaments, threads or the like, leaving the spinnerettes
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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Abstract
The present invention relates to a kind of High temperature resistant SiC fibers containing zirconium and preparation method thereof.Preparation method includes step：S101：Yttrium oxide is dissolved in ethyl alcohol, heat and is stirred evenly, obtains the first solution；S102：First solution is mixed and stirred evenly with nano zircite dispersion liquid, obtains the second solution；S103：Polycarbosilane is dissolved in dimethylbenzene, is added in the second solution ＆ stir, is heated to solvent later and volatilizees completely, obtain powdery product；S104：By powdery product through melt spinning and cure treatment, cross filament beam is obtained；S105：By cross filament beam high temperature sintering under an inert atmosphere, it is cooled to room temperature later, obtains silicon carbide fibre.Zirconium oxide and yttrium oxide are introduced in the preparation process of silicon carbide fibre of the present invention, utilize the phase transformation volume expansion of zirconium oxide and the temperature flowing of yttrium oxide, it prepares that intensity is high, silicon carbide fibre of stable performance under high temperature, good application prospect is presented in high-temperature fields such as aerospaces.
Description
Technical field
The present invention relates to high-performance fiber technical fields, and in particular to a kind of High temperature resistant SiC fibers containing zirconium and its preparation
Method.
Background technology
Silicon carbide (SiC) fiber is the excellent ceramic fibre of a kind of high-strength and high-modulus, high temperature resistance.Based on its excellent object
Mechanics and high temperature resistance are managed, silicon carbide fibre has extremely wide in the national defence such as Aeronautics and Astronautics, weaponry leading-edge field
Application prospect；Therefore, also it is always contraband of the western countries to China.Based on this, research silicon carbide fibre prepares skill
Art breaks foreign technology block, realizes the autonomous production of silicon carbide fibre, will promote China's advanced composite material and weapon dress
Standby research application level and the important leverage of the military strength and comprehensive strength that improve China.
The preparation method of silicon carbide fibre is precursor mainly using Polycarbosilane (PCS) in traditional technology, by molten
Melt spinning, cure treatment, high temperature firing technique are prepared.However, the performance of SiC fibers is very quick to high-temperature process temperature
Sense；It is generally acknowledged that：Under high-temperature condition, with the raising of temperature, the β-SiC microcrystalline grain Size growths in silicon carbide fibre are fine
Dimension is internal to there is apparent hole and micro-crack, so as to which fibre strength drastically declines.
Based on this, providing a kind of preparation method of novel silicon carbide fibre is particularly important.
Invention content
For the defects in the prior art, the present invention is intended to provide a kind of High temperature resistant SiC fibers containing zirconium and its preparation side
Method.High temperature resistant SiC fibers containing zirconium provided by the invention have many advantages, such as that intensity is high, has stable high-temperature performance, not only can be
It is used, and performance is held essentially constant in 1200 DEG C of environment above, thus good application prospect is presented in high-temperature field.
Specifically, zirconium oxide and yttrium oxide are introduced in a manner of physical blending in SiC fiber manufacturing process, using zirconium oxide in high temperature
The volume expansion that lower phase transformation generates inhibits growing up for β-SiC microcrystalline grains；It is formed at high temperature using sintering aid yttrium oxide
The ceramic phase of good fluidity, face crack in the silicon carbide fibre sintering process that heals, so as to prepare, intensity is high, high-temperature behavior
Stable silicon carbide fibre.
For this purpose, the present invention provides following technical solution：
In a first aspect, the present invention provides a kind of preparation method of the silicon carbide fibre containing zirconium, include the following steps：S101：It will
Yttrium oxide is dissolved in ethyl alcohol, is heated and is stirred evenly, and obtains the first solution；S102：First solution and nano zircite are disperseed
Liquid is mixed and stirred for uniformly, obtaining the second solution；S103：Polycarbosilane is dissolved in dimethylbenzene, obtains third solution；Poly- carbon silicon
The preferred softening point of alkane is 240~280 DEG C, and molecular weight is 2500~3200；The second solution is added in third solution later and is stirred
It mixes uniformly, the solution after stirring evenly is heated to solvent later and is volatilized completely, obtains powdery product；Specific operation process
In, it heats while stirring, until solvent volatilizees completely；S104：By powdery product through melt spinning and cure treatment, obtain
Cross filament beam；Wherein, melt spinning is specially：Powdery product is placed in melt spinning cylinder, in N2Or 2~4h under Ar atmosphere
280~300 DEG C are heated to, is then forced into 2~4MPa, melt flow is flowed out by strainer, spinneret, obtains fibre bundle；It is non-fusible
Processing is specially：Fibre bundle is put into wire tray in air environment, 1~2h is warming up to 180~200 DEG C and keeps the temperature 2~4h, then
N2Or 2~3h is warming up to 420~460 DEG C under Ar atmosphere, keeps the temperature 6~8h.S105：By cross filament beam high temperature under an inert atmosphere
Sintering, is cooled to room temperature, obtains silicon carbide fibre containing zirconium later.Specifically, the preparation method of nano zircite dispersion liquid is：It takes
A certain amount of nano zircite is added in deionized water, and the mass ratio of nano zircite and deionized water is (1~10):3000；
It adds in 0.03~0.5wt% isopropanols later or PEG makees dispersant, with NaOH adjusting solution ph to 10 or so, ultrasonic vibration
30min, subsequent 1~2h of magnetic agitation, obtains nano zircite dispersion liquid.
Preferably, in S101, the mass ratio of yttrium oxide and ethyl alcohol is 1：(5~10), the temperature of heating is 40~45 DEG C, is stirred
Rate is mixed as 200~300r/min, mixing time is 30~40min.
Preferably, in S102, the volume ratio of the first solution and nano zircite dispersion liquid is 1：(10~20), stir speed (S.S.)
For 200~300r/min, mixing time is 90~120min.
Preferably, in S103, the mass ratio of Polycarbosilane and dimethylbenzene is 1：(5~10), third solution and the second solution
Volume ratio be (5~10)：1, stir speed (S.S.) is 300~400r/min.
Preferably, in S105, inert gas N2And/or Ar, and the flow of inert gas is 100~200ml/min.
Preferably, in S105, high temperature sintering is cooled to room temperature and specifically includes later：With the rate liter of 100~200 DEG C/h
Temperature keeps the temperature 2~4h to 1000~1200 DEG C；1700~1800 DEG C then are warming up to the rate of 500~600 DEG C/h, heat preservation 0.5
~1h；Room temperature is down to the rate of 100~200 DEG C/h later.
Second aspect, using containing the zirconium silicon carbide fibre provided by the invention being prepared.
The third aspect, silicon carbide fibre containing zirconium provided by the invention the high-temperature fields such as aerospace application, and especially
The application being above in 1200 DEG C of environment.
Above-mentioned technical proposal provided by the invention has the following advantages：
(1) applicant has found by numerous studies：High temperature resistant SiC fibers containing zirconium provided by the invention have intensity it is high,
The advantages that having stable high-temperature performance can not only use, but also performance is held essentially constant in 1200 DEG C of environment above, in high temperature
Field has a good application prospect.
(2) in SiC fiber manufacturing process provided by the invention, zirconium oxide and yttrium oxide are introduced in a manner of physical blending,
Using the zirconium oxide volume expansion that phase transformation generates at high temperature, inhibit growing up for β-SiC microcrystalline grains；It is aoxidized using sintering aid
The ceramic phase for the good fluidity that yttrium is formed at high temperature, heal silicon carbide fibre sintering process in face crack, so as to prepare
Go out the silicon carbide fibre that intensity is high, has stable high-temperature performance.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description
It obtains significantly or is recognized by the practice of the present invention.
Specific embodiment
The embodiment of technical solution of the present invention will be described in detail below.Following embodiment is only used for clearer
Illustrate technical scheme of the present invention, therefore be only used as example, and be not intended to limit the protection scope of the present invention and limit the scope of the invention.
Experimental method in following embodiments is conventional method unless otherwise specified.
Test material used in following embodiments is to be commercially available from conventional reagent shop unless otherwise specified.
Quantitative test in following embodiment, is respectively provided with three repeated experiments, and data are the average value of three repeated experiments
Or mean+SD.
The present invention provides a kind of preparation method of the silicon carbide fibre containing zirconium, includes the following steps：
S101：Yttrium oxide is dissolved in ethyl alcohol, is heated to 40~50 DEG C, and stir evenly, obtains the first solution.Wherein,
The mass ratio of yttrium oxide and ethyl alcohol is 1：(5~10), the temperature of heating is 40~45 DEG C, and stir speed (S.S.) is 200~300r/min,
Mixing time is 30~40min.
S102：First solution and nano zircite dispersion liquid are mixed and stirred for uniformly, obtaining the second solution.Wherein,
The volume ratio of one solution and nano zircite dispersion liquid is 1：(10~20), stir speed (S.S.) be 200~300r/min, mixing time
For 90~120min.The preparation method of nano zircite dispersion liquid is：By nano zircite and deionized water according to (1~
10)：3000 mass ratio stirs evenly, and adds in 0.03~0.5wt% isopropanols later or PEG makees dispersant, adjusted with NaOH
For solution ph to 10 or so, ultrasonic vibration 30min, subsequent 1~2h of magnetic agitation obtain nano zircite dispersion liquid.
S103：Polycarbosilane is dissolved in dimethylbenzene, obtains third solution；The second solution is added in third solution and is stirred
It mixes uniformly, the solution after stirring evenly is heated to 60~80 DEG C later, is stirred continuously to solvent and volatilizees completely, is obtained powdered
Product.Wherein, the mass ratio of Polycarbosilane and dimethylbenzene is 1：The volume ratio of (5~10), third solution and the second solution is (5
~10)：1, stir speed (S.S.) is 300~400r/min.
S104：By powdery product through melt spinning and cure treatment, cross filament beam is obtained.Wherein, melt spinning
Specially：Powdery product is placed in melt spinning cylinder, in N2Or 2~4h is heated to 280~300 DEG C under Ar atmosphere, then adds
2~4MPa is depressed into, melt flow is flowed out by strainer, spinneret, obtains fibre bundle；Cure treatment is specially：Fibre bundle is put into
In air environment, 1~2h is warming up to 180~200 DEG C and keeps the temperature 2~4h, subsequent N wire tray2Or 2~3h is warming up under Ar atmosphere
420~460 DEG C, keep the temperature 6~8h.
S105：Cross filament beam is placed in sintering furnace, under an inert atmosphere high temperature sintering, is cooled to room temperature later, obtained
To silicon carbide fibre containing zirconium.Wherein, inert gas N2And/or Ar, and the flow of inert gas is 100~200ml/min；It is high
Temperature sintering, is cooled to room temperature and specifically includes later：1000~1200 DEG C are warming up to the rate of 100~200 DEG C/h, heat preservation 2~
4h；1700~1800 DEG C then are warming up to the rate of 500~600 DEG C/h, keeps the temperature 0.5~1h；Later with 100~200 DEG C/h
Rate be down to room temperature.
It illustrates With reference to embodiment：
Embodiment one
The present embodiment provides a kind of preparation methods of silicon carbide fibre containing zirconium, include the following steps：
S101：Yttrium oxide powder is dissolved in ethyl alcohol.Wherein, the mass ratio of yttrium oxide and ethyl alcohol is 1:5.It is heated to 40
DEG C, it is stirred with 200r/min rates, mixing time 40min obtains the first solution.
S102：First solution and nano zircite dispersion liquid are mixed and stirred for uniformly, obtaining the second solution.Wherein,
The volume ratio of one solution and nano zircite dispersion liquid is 1：10, stir speed (S.S.) 200r/min, mixing time 90min.It receives
Rice Zirconium oxide dispersion liquid preparation method be：By nano zircite and deionized water according to 1：3000 mass ratio stirring is equal
It is even, 0.03wt% isopropanols are added in later and make dispersant, with NaOH adjusting solution ph to 10, ultrasonic vibration 30min, subsequent magnetic
Power stirs 2h, obtains nano zircite dispersion liquid.
S103：Polycarbosilane is dissolved in dimethylbenzene, obtains third solution；The second solution is added in third solution and is stirred
It mixes uniformly, the solution after stirring evenly is heated to 80 DEG C later, is stirred to solvent with the rate of 400r/min and volatilized completely, obtained
To powdery product.Wherein, the mass ratio of Polycarbosilane and dimethylbenzene is 1：5, third solution and the volume ratio of the second solution are
5：1.
S104：Powdery product is placed in melt spinning cylinder, in N22h is heated to 280 DEG C under atmosphere, is then forced into
4MPa, melt flow are flowed out by strainer, spinneret, obtain fibre bundle；Fibre bundle is put into wire tray in air environment, 2h is warming up to
200 DEG C and 4h is kept the temperature, subsequent N22h is warming up to 420 DEG C under atmosphere, keeps the temperature 6h, obtains cross filament beam.
S105：Cross filament beam is placed in sintering furnace, in the N that flow is 100ml/min2Under atmosphere, with 100 DEG C/h's
Rate is warming up to 1000 DEG C, keeps the temperature 4h；1700 DEG C then are warming up to the rate of 500 DEG C/h, keeps the temperature 0.5h；Later with 100 DEG C/
The rate of h is down to room temperature, obtains silicon carbide fibre containing zirconium.
Embodiment two
The present embodiment provides a kind of preparation methods of silicon carbide fibre containing zirconium, include the following steps：
S101：Yttrium oxide powder is dissolved in ethyl alcohol.Wherein, the mass ratio of yttrium oxide and ethyl alcohol is 1:10.It is heated to 50
DEG C, it is stirred with 200r/min rates, mixing time 40min obtains the first solution.
S102：First solution and nano zircite dispersion liquid are mixed and stirred for uniformly, obtaining the second solution.Wherein,
The volume ratio of one solution and nano zircite dispersion liquid is 1：15, stir speed (S.S.) 300r/min, mixing time 120min.It receives
Rice Zirconium oxide dispersion liquid preparation method be：By nano zircite and deionized water according to 10：3000 mass ratio stirring is equal
It is even, 0.5wt% isopropanols are added in later and make dispersant, with NaOH adjusting solution ph to 10, ultrasonic vibration 30min, subsequent magnetic
Power stirs 1h, obtains nano zircite dispersion liquid.
S103：Polycarbosilane is dissolved in dimethylbenzene, obtains third solution；The second solution is added in third solution and is stirred
It mixes uniformly, the solution after stirring evenly is heated to 60 DEG C later, is stirred to solvent with the rate of 400r/min and volatilized completely, obtained
To powdery product.Wherein, the mass ratio of Polycarbosilane and dimethylbenzene is 1：10, third solution and the volume ratio of the second solution are
10：1.
S104：Powdery product is placed in melt spinning cylinder, in N24h is heated to 300 DEG C under atmosphere, is then forced into
2MPa, melt flow are flowed out by strainer, spinneret, obtain fibre bundle；Fibre bundle is put into wire tray in air environment, 1h is warming up to
180 DEG C and 2h is kept the temperature, subsequent N23h is warming up to 460 DEG C under atmosphere, keeps the temperature 8h, obtains cross filament beam.
S105：Cross filament beam is placed in sintering furnace, in the case where flow is the Ar atmosphere of 200ml/min, with 200 DEG C/h's
Rate is warming up to 1200 DEG C, keeps the temperature 2h；1800 DEG C then are warming up to the rate of 600 DEG C/h, keeps the temperature 1h；Later with 200 DEG C/h
Rate be down to room temperature, obtain silicon carbide fibre containing zirconium.
Comparative example one
It should be noted that the comparative example on the basis of embodiment two, is formed by changing relative parameters setting.Specifically
Ground, this comparative example provide a kind of preparation method of the silicon carbide fibre containing zirconium, include the following steps：
S1：Polycarbosilane is dissolved in dimethylbenzene, obtains third solution；Nano zircite dispersion is added in third solution
Liquid simultaneously stirs evenly, and the solution after stirring evenly is heated to 60 DEG C later, is stirred with the rate of 400r/min complete to solvent
Volatilization, obtains powdery product.Wherein, the mass ratio of Polycarbosilane and dimethylbenzene is 1：10, third solution and nano zircite
The volume ratio of dispersion liquid is 10：1.The preparation method of nano zircite dispersion liquid is：By pressing for nano zircite and deionized water
According to 10：3000 mass ratio stirs evenly, later add in 0.5wt% isopropanols make dispersant, with NaOH adjust solution ph to
10, ultrasonic vibration 30min, subsequent magnetic agitation 1h obtain nano zircite dispersion liquid.
S2：Powdery product is placed in melt spinning cylinder, in N24h is heated to 300 DEG C under atmosphere, is then forced into 2MPa,
Melt flow is flowed out by strainer, spinneret, obtains fibre bundle；Fibre bundle is put into wire tray in air environment, 1h is warming up to 180 DEG C
And 2h is kept the temperature, subsequent N23h is warming up to 460 DEG C under atmosphere, keeps the temperature 8h, obtains cross filament beam.
S3：Cross filament beam is placed in sintering furnace, in the case where flow is the Ar atmosphere of 200ml/min, with the speed of 200 DEG C/h
Rate is warming up to 1200 DEG C, keeps the temperature 2h；1800 DEG C then are warming up to the rate of 600 DEG C/h, keeps the temperature 1h；Later with 200 DEG C/h's
Rate is down to room temperature, obtains silicon carbide fibre containing zirconium.
In addition, in order to preferably highlight the advantage of technical solution of the present invention, measure each embodiment and comparative example and be carbonized containing zirconium
The normal temperature strength and elasticity modulus of silica fibre work after 10h in addition, measuring respectively silicon carbide fibre containing zirconium under 1200 DEG C of environment
Strength retention ratio, concrete outcome are as shown in table 1.
The capabilities list of 1 each embodiment silicon carbide fibre containing zirconium of table
| Normal temperature strength/GPa | Elasticity modulus/GPa | Strength retention ratio/% | |
| Embodiment one | 3.3 | 218 | 98 |
| Embodiment two | 3.2 | 220 | 95 |
| Comparative example one | 2.6 | 198 | 71 |
Certainly, in addition to the situation that embodiment one and embodiment two are enumerated, prepared by the weight percent of other raw material components
Each condition and parameter in journey etc. are also possible.
High temperature resistant SiC fibers containing zirconium provided by the invention have many advantages, such as that intensity is high, have stable high-temperature performance, and not only may be used
To be used in 1200 DEG C of environment above, and performance is held essentially constant, thus presents good application in high-temperature field
Prospect.Specifically, zirconium oxide and yttrium oxide are introduced in a manner of physical blending in SiC fiber manufacturing process, utilizes zirconium oxide
The volume expansion that phase transformation generates at high temperature inhibits growing up for β-SiC microcrystalline grains；Using sintering aid yttrium oxide at high temperature
The ceramic phase of the good fluidity of formation, face crack in the silicon carbide fibre sintering process that heals are high, high so as to prepare intensity
The silicon carbide fibre that warm nature can be stablized.
In the description of the present invention, it is to be understood that term " first ", " second " are only used for description purpose, and cannot
It is interpreted as indicating or implies relative importance or imply the quantity of the technical characteristic indicated by indicating.Define as a result, " the
One ", one or more this feature can be expressed or be implicitly included to the feature of " second ".In the description of the present invention,
" multiple " are meant that two or more, unless otherwise specifically defined.
In the description of this specification, reference term " one embodiment ", " example ", " is specifically shown " some embodiments "
The description of example " or " some examples " etc. means specific features, structure, material or the spy for combining the embodiment or example description
Point is contained at least one embodiment of the present invention or example.In the present specification, schematic expression of the above terms are not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office
It is combined in an appropriate manner in one or more embodiments or example.In addition, without conflicting with each other, the skill of this field
Art personnel can tie the different embodiments or examples described in this specification and the feature of different embodiments or examples
It closes and combines.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, those of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changes, replacing and modification.
Claims (9)
1. the preparation method of a kind of silicon carbide fibre containing zirconium, which is characterized in that include the following steps：
S101：Yttrium oxide is dissolved in ethyl alcohol, heat and is stirred evenly, obtains the first solution；
S102：First solution and nano zircite dispersion liquid are mixed and stirred for uniformly, obtaining the second solution；
S103：Polycarbosilane is dissolved in dimethylbenzene, obtains third solution；Second solution is added in the third solution
And stir evenly, the solution after stirring evenly is heated to solvent later volatilizees completely, obtains powdery product；
S104：By the powdery product through melt spinning and cure treatment, cross filament beam is obtained；
S105：By cross filament beam high temperature sintering under an inert atmosphere, it is cooled to room temperature later, obtains described being carbonized containing zirconium
Silica fibre.
2. the preparation method of the silicon carbide fibre according to claim 1 containing zirconium, it is characterised in that：
In the S101, the mass ratio of the yttrium oxide and the ethyl alcohol is 1：(5~10), the temperature of heating is 40~45 DEG C,
Stir speed (S.S.) is 200~300r/min, and mixing time is 30~40min.
3. the preparation method of the silicon carbide fibre according to claim 1 containing zirconium, it is characterised in that：
In the S102, the volume ratio of first solution and nano zircite dispersion liquid is 1：(10~20), stir speed (S.S.) are
200~300r/min, mixing time are 90~120min.
4. the preparation method of the silicon carbide fibre according to claim 1 containing zirconium, it is characterised in that：
In the S103, the mass ratio of the Polycarbosilane and the dimethylbenzene is 1：(5~10), the third solution with it is described
The volume ratio of second solution is (5~10)：1, stir speed (S.S.) is 300~400r/min.
5. the preparation method of the silicon carbide fibre according to claim 1 containing zirconium, it is characterised in that：
In the S105, inert gas N2And/or Ar, and the flow of the inert gas is 100~200ml/min.
6. the preparation method of the silicon carbide fibre according to claim 1 containing zirconium, it is characterised in that：
In the S105, the high temperature sintering is cooled to room temperature and specifically includes later：It is warming up to the rate of 100~200 DEG C/h
1000~1200 DEG C, keep the temperature 2~4h；Then 1700~1800 DEG C are warming up to the rate of 500~600 DEG C/h, heat preservation 0.5~
1h；Room temperature is down to the rate of 100~200 DEG C/h later.
7. the silicon carbide fibre containing zirconium being prepared according to any one of claim 1~6 the method.
8. silicon carbide fibre containing zirconium described in claim 7 is in the application of high-temperature field.
9. application of the silicon carbide fibre containing zirconium in the environment higher than 1200 DEG C described in claim 7.
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|---|---|---|---|---|
| CN109608201A (en) * | 2019-01-28 | 2019-04-12 | 江西嘉捷信达新材料科技有限公司 | Silicon carbide/boron nitride fiber and its preparation method and application |
| CN109761610A (en) * | 2019-01-28 | 2019-05-17 | 江西嘉捷信达新材料科技有限公司 | Silicon carbide fibre and its preparation method and application |
| CN109811429A (en) * | 2019-01-28 | 2019-05-28 | 江西嘉捷信达新材料科技有限公司 | Silicon carbide fibre and the preparation method and application thereof containing nano aluminum nitride and metallic nickel |
| CN109809820A (en) * | 2019-01-28 | 2019-05-28 | 江西嘉捷信达新材料科技有限公司 | Zirconium carbide, nanometer silicon carbide composite fibre enhancing silicon carbide fibre and preparation method thereof |
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| CN109811429B (en) * | 2019-01-28 | 2021-07-27 | 江西嘉捷信达新材料科技有限公司 | Silicon carbide fiber containing nano aluminum nitride and metal nickel, and preparation method and application thereof |
| CN109809820B (en) * | 2019-01-28 | 2021-11-02 | 江西嘉捷信达新材料科技有限公司 | Zirconium carbide and silicon carbide nano composite fiber reinforced silicon carbide fiber and preparation method thereof |
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