CN105622172B - The fiber surface of non-oxidized substance fiber reinforced ceramic matrix composites is prepared in situ (C-SiC)nOr the method for SiC coatings - Google Patents
The fiber surface of non-oxidized substance fiber reinforced ceramic matrix composites is prepared in situ (C-SiC)nOr the method for SiC coatings Download PDFInfo
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
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- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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Abstract
The present invention relates to a kind of fiber surfaces of non-oxidized substance fiber reinforced ceramic matrix composites to be prepared in situ (C SiC)nOr the method for SiC coatings, the preparation method include：Fiber surface using chemical vapor infiltration in fiber preform forms one layer C layers；Using Si or SiO as silicon source, the C layer segments of fiber surface are made using chemical vapor infiltration or are completely reformed into SiC.The present invention uses Si or SiO as that as the sources Si, can prepare (C SiC) n or SiC coatings to avoid using organic silicon source of high cost, or generate the generation of toxic corrosive tail gas HCl, have the characteristics that at low cost, environmental-friendly.
Description
Technical field
The present invention relates to the technologies of preparing of coat of silicon carbide, and in particular to a kind of non-oxidized substance fiber reinforced ceramic-base is compound
The fiber surface of material is prepared in situ (C-SiC)nOr the method for SiC coatings.
Background technology
Fiber reinforced ceramic matrix composites be it is a kind of fiber is combined into the high-performance composite materials to be formed with ceramic matrix,
Have the characteristics that high temperature resistant, corrosion-resistant, high reliability, is had been widely used in aerospace field.Fiber reinforced ceramic
In based composites, fiber and ceramic matrix all have higher modulus, but toughness is relatively low as main composition phase.The two is multiple
But it is Presence of an interface between the two to have higher toughness, important reason after conjunction.Interface is the important composition portion of composite material
Point, it is to influence toughness of material, high temperature resistant, corrosion-resistant and high reliability importance.Interface main function is that crackle is prevented to expand
The deflection of crackle is opened up or caused, crack propagation energy is consumed, with the reliability of reinforcing material.
SiC has the characteristics that high temperature resistant, anti-oxidant, modulus is high, coefficient of thermal expansion is low, is well suited as fiber coat material
Material, the i.e. interface of fiber and matrix.Has a large amount of research report at present to prepare SiC coatings, using before organic containing Si
Drive body and H2CVI is reacted to prepare.The cost of the organic precursor of use is higher toxic, and the tail gas generated is also toxic, has
Corrosivity.(C-SiC)nThe extension of crackle can be more efficiently prevented compared with individual SiC interface coatings.
It has been had been reported that in related patents currently, preparing SiC coatings with fiber C reaction in-situ using Si
(CN101560728A), but patent directly uses fiber C to form SiC coatings with Si vapor reactions, and this preparation method can cause
Low-fiber performance drops in the erosion of fiber.And combined with the coating of SiC can be stronger for fiber, and when crack propagation, is difficult to play
The effect of Anticrack.Fiber is only limitted to fiber C in patent, and for SiC, SiCN or SiBCN etc., other non-oxidized substances are fine
Dimension is difficult to be applicable in, nor can be formed (C-SiC)nCoating.
Invention content
In view of the problems of the existing technology, it is desirable to provide it is a kind of it is at low cost, the small, universality of pollution is strong is prepared in situ
The method of SiC coatings, to form SiC or (C-SiC) in multiple fibernCoating, and solve to prepare at present and be deposited in SiC coatings
Cost and pollution problem.
Present invention firstly provides a kind of fiber surfaces of non-oxidized substance fiber reinforced ceramic matrix composites, and SiC is prepared in situ
Or the preparation method of C-SiC coatings, the preparation method include：
(1) chemical vapor infiltration is used to form one layer C layers in the fiber surface of fiber preform；
(2) using Si or SiO as silicon source, the C layer segments of fiber surface is made using chemical vapor infiltration or are completely reformed into
SiC。
The present invention also provides a kind of fiber surface of non-oxidized substance fiber reinforced ceramic matrix composites and is prepared in situ first
(C- SiC)nThe preparation method of coating, the preparation method include：
(1) chemical vapor infiltration is used to form one layer C layers in the fiber surface of fiber preform；
(2) using Si or SiO as silicon source, the C layer segments of fiber surface is made using chemical vapor infiltration or are completely reformed into
SiC；
Above steps may be repeated multiple times (1) and (2) are to obtain (C-SiC)nCoating.
The present invention uses Si or SiO for as the sources Si, Si is polycrystalline Si powder or Si blocks, and Si can come from the remaining of photovoltaic industry
Material realizes waste utilization.SiO uses Si and SiO2Reaction is formed, SiO2Also there is the price of relative moderate.Therefore the present invention can be with
It avoids preparing (C-SiC) n or SiC coatings using organic silicon source of high cost, or generates the production of toxic corrosive tail gas HCl
It is raw, have the characteristics that at low cost, environmental-friendly.
In the present invention, C layers of the thickness can be 0.05-5 μm, and the coating of this thickness range can effectively enhance composite material
Reliability, and can avoid erosions of the Si or SiO to fiber.
In the present invention, in step (1), isothermal CVI, isothermal forced flow CVI, temperature gradient can be used in chemical vapor infiltration
CVI, forced flow temperature gradient CVI, pulse CVI.
In the present invention, in step (1), carbon source can be used alkane, alkene, alkynes or aromatic hydrocarbon, for example, methane, ethane, propane,
Butane, acetylene, benzene, carbon source flow are 1~100mL/ minutes.
In the present invention, in step (1), carrier gas used in chemical vapor infiltration can be argon gas, carrier gas flux can be 100~
1500mL/ minutes, carrier gas temperature range can be 800~1200 DEG C, and processing time can be 0.5 hour or more.
In the present invention, in step (2), chemical vapor infiltration can be used isothermal forced flow CVI, temperature gradient CVI, force
Flowing temperature gradient CVI, preferably forced flow temperature gradient CVI.
In the present invention, in step (2), carrier gas used in chemical vapor infiltration can be argon gas, carrier gas stream can be 100~
1500mL/ minutes, processing time can be 0.5 hour or more.
In the present invention, in step (2), with Si and SiO2Reaction forms SiO as silicon source, Si and SiO2It is heated to 1200 DEG C
It is above to generate silicon source steam, after carrier gas is heated to same temperature, then mix with the silicon source steam.
In the present invention, in step (2), in step (2), using Si as silicon source, Si is heated to 1400 DEG C or more and generates silicon source
Steam after carrier gas is heated to same temperature, then is mixed with the silicon source steam.
Description of the drawings
Fig. 1 shows the SEM pictures of the fiber C of the different amplification covered without coating in embodiment 1；
Fig. 2 shows the SEM pictures for the fiber C that SiC coatings in embodiment 2 cover；
Fig. 3 shows the SEM pictures for the fiber C that SiC coatings cover in embodiment 3；
Fig. 4 shows to be prepared for (C-SiC) in embodiment 41The SEM figures of SiC/SiC composite materials are prepared after coating using PIP
Piece.
Specific implementation mode
Hereinafter, being further illustrated the present invention with reference to attached drawing and following embodiments, it should be appreciated that attached drawing and following embodiments
It is merely to illustrate the present invention, is not intended to limit the present invention.
To form SiC or (C-SiC) in multiple fibernCoating, and solve to prepare cost present in SiC coatings at present
And pollution problem, the present invention propose a kind of method that SiC coatings are prepared in situ at low cost, pollution is small, universality is strong.I.e., originally
SiC or (C-SiC) is prepared in situ in a kind of fiber surface of non-oxidized substance fiber reinforced ceramic matrix composites of disclosure of the inventionn
The method of (n=1,2,3 ...) coating.Chemical vapor infiltration (Chemical Vapor Infiltration, CVI are used first
Amorphous or crystalline state C are formed in the fiber surface of precast body.SiC coatings are then prepared by the way of CVI, wherein silicon source is SiO
Or Si.The thickness of SiC coatings is at 0.05-5 μm.The above process, which is repeated several times, can prepare (C-SiC)nCoating.The present invention's avoids
(C-SiC) n or SiC coatings are prepared using organic silicon source of high cost, or generate the generation of toxic corrosive tail gas HCl,
Have the characteristics that at low cost, environmental-friendly.Specifically, the method for the present invention may include following steps.
First, choose fiber preform, can be used worked out with carbon, silicon carbide, SiCN or SiBCN fibers to be formed it is prefabricated
Body.The volume fraction of fiber can be 10~50vol.% in fiber preform.
Fiber preform is put into cvd furnace, using CVI in precast body fiber surface deposited carbon layer.Deposition carbon source used
Alkane, unsaturated hydrocarbon (alkene, alkynes, aromatic hydrocarbon) can be used, for example, methane, ethane, propane, butane, acetylene, benzene.
The flow of carbon source is controllable to 1~100mL/ minutes.Can be selected with isothermal CVI, isothermal forced flow CVI, temperature gradient CVI,
Forced flow temperature gradient CVI, pulse CVI.
Carrier gas used can be argon gas.It can be 800-1200 DEG C to deposit (processing) temperature, be 0.5h or more, deposition shape when deposition
At C layer thickness be 0.05-5 μm.
Then use CVI reaction in-situs to prepare SiC coatings, by carrier gas Ar gases be further heated to after certain temperature with
SiO or Si steams converge, preferably SiO, and gas is pumped into stove, and gas is reacted with the C of the precast body surface of heating layers, in advance
The temperature of body processed should be not less than the temperature of carrier gas.The CVI times are in 0.5h or more.Isothermal forced flow CVI, temperature ladder can be selected
CVI, forced flow temperature gradient CVI are spent, preferably forced flow temperature gradient CVI prepares SiC coatings.
It should be understood that the temperature of fiber preform is not less than the temperature of carrier gas, further for the CVI with temperature gradient, in advance
Ascendant trend is presented along carrier gas direction in the temperature of body processed.
It should be understood that SiC coatings use polysilicon Si powder or Si block of the purity 99% or more, purity is 99% or more
SiO2.Si and SiO2Reaction forms SiO.The preferred SiO of silicon source.Si or SiO is reacted with C prepares the existing a large amount of reports of SiC, therefore
The present invention is feasible method.
When SiC coating CVI, carrier gas Ar to first pass through be heated to silicon source steam phase it is synthermal after, can be with silicon source steam
Converge.
Progress can be repeated several times in the above process, to prepare (C-SiC)nCoating.
It, can be by precast body by CVI, organic precursor dipping pyrolytic process (PIP) or liquid-phase silicone after interface coating is formed
Infiltration process (LSI) forms fibre reinforced composites.
Some exemplary embodiments are enumerated further below so that the present invention is better described.It should be understood that the present invention is in detail
The above embodiment and following embodiment stated are only illustrative of the invention and is not intended to limit the scope of the invention, this field
Some the nonessential modifications and adaptations made of technical staff's the above according to the present invention belong to the protection of the present invention
Range.In addition, specific proportioning, the time etc. in following technological parameters are also only exemplary, those skilled in the art can be upper
It states and selects suitable value in the range of limiting.
Embodiment 1
Fiber volume fraction is that the carbon fiber precast body of 30vol.% is placed in cvd furnace, and Fig. 1 is that the C of non-seal coat is fine
The scanning electron microscopic picture of dimension.CVI carbon-coatings use propane for carbon source, and Ar is carrier gas, the flow of the two be respectively 100ml/min and
1000 ml/min deposit 10h, the carbon layers having thicknesses of deposition are 0.5 μm under the conditions of 900 DEG C.SiC coatings are prepared in situ in CVI, pure
Degree is heated to 1450 DEG C for 99.9% Si powder, and carrier gas Ar is heated to 1450 DEG C, after the two is converged, and it is heavy that mixed gas is pumped into
In product stove.SiC coatings are prepared with isothermal forced flow CVI, the pressure of CVI is 150kPa, and temperature is 1700 DEG C, time 2h,
The SiC thickness of formation is 0.35 μm.It then passes through LSI and fine and close carbon fibre reinforced composite is prepared.
Embodiment 2
Fiber volume fraction is that the carbon fiber precast body of 25vol.% is placed in cvd furnace.Using forced flow temperature gradient
CVI prepares carbon-coating, and butane is carbon source, and Ar is carrier gas, and the flow of the two is respectively 30ml/min and 1000ml/min, sample front
800 DEG C of temperature, pressure 150kPa, under the conditions of 1200 DEG C of rear end temperature, pressure 10kPa, for 24 hours, the carbon-coating of deposition is about deposition
0.3μm.SiC coatings are prepared in situ in CVI, the SiO for being 99% by Si powder and purity that purity is 99%2Mixture is heated to
1200 DEG C, carrier gas Ar is heated to 1200 DEG C, after the two is converged, and mixed gas is pumped into cvd furnace.It is forced with temperature gradient
It flows CVI and prepares SiC coatings, the forefront pressure of CVI is 180kPa, temperature is 1200 DEG C, and rear part temperature is 1300 DEG C, pressure
The SiC thickness of 20kPa, sedimentation time 4h, formation are about 0.3 μm, shown in Fig. 2.It then passes through PIP and carbon fiber is prepared
Enhance composite material of silicon carbide.
Embodiment 3
Fiber volume fraction is that the carbon fiber precast body of 20vol.% is placed in cvd furnace.Pulse CVI prepares carbon-coating, deposition
It is evacuated to 0.7kPa in stove, keeps 5s, then uses acetylene for carbon source, Ar is carrier gas, and the flow of the two is respectively 75ml/
Min and 1000ml/min, gas is filled in stove, until pressure 5kPa, keeps 100s.It repeats the above process, in 1200 DEG C of conditions
Under, 8h is deposited, the carbon layers having thicknesses of deposition are about 2 μm.SiC coatings are prepared in situ in CVI, Si powder and purity by purity for 99.9%
For 99.9% SiO2Mixture is heated to 1250 DEG C, and carrier gas Ar is heated to 1250 DEG C, after the two is converged, and mixed gas is pumped into
Into cvd furnace.SiC coatings are prepared with temperature gradient forced flow CVI, the pressure of CVI is 180kPa, and sample front temperature is
1250 DEG C, rear part temperature is 1300 DEG C, pressure 5kPa, sedimentation time 6h, about 2 μm of the SiC thickness of formation, shown in Fig. 3.
It then passes through LSI and carbon fibre reinforced silicon carbide composite material is prepared.
Embodiment 4
Fiber volume fraction is that the silicon carbide fibre precast body of 10vol.% is placed in cvd furnace.CVI carbon-coatings, using ethane
For carbon source, Ar is carrier gas, and the flow of the two is respectively 90ml/min and 1000ml/min, under the conditions of 1100 DEG C, is deposited for 24 hours,
The carbon layers having thicknesses of deposition are 3 μm.SiC coatings are prepared in situ in CVI, are 99.9% by Si powder and purity that purity is 99.9%
SiO2Mixture is heated to 1230 DEG C, and carrier gas Ar is heated to 1230 DEG C, after the two is converged, and mixed gas is pumped into cvd furnace
It is interior.SiC coatings are prepared with temperature gradient CVI, sample front temperature is 1230 DEG C, and rear part temperature is 1270 DEG C, and sedimentation time is
12h.The SiC thickness that reaction is formed is 2 μm, forms C-SiC coatings.It then passes through PIP and silicon carbide fibre enhancing carbon is prepared
SiClx composite material, shown in Fig. 4.
Embodiment 5
Fiber volume fraction is that the SiBCN fiber preforms of 15vol.% are placed in cvd furnace.CVI carbon-coatings, using methane
For carbon source, Ar is carrier gas, and the flow of the two is respectively 1ml/min and 100ml/min, under the conditions of 1150 DEG C, deposits 0.5h,
The carbon layers having thicknesses of deposition are 0.05 μm.SiC coatings are prepared in situ in CVI, are 99.9% by Si powder and purity that purity is 99.9%
SiO2Mixture is heated to 1210 DEG C, and carrier gas Ar is heated to 1210 DEG C, after the two is converged, and mixed gas is pumped into cvd furnace
It is interior.SiC coatings are prepared with forced flow CVI, the pressure of CVI is 200kPa, and sample temperature is 1210 DEG C, sedimentation time 16h,
The SiC thickness of formation is 0.05 μm.It then passes through PIP and the silicon carbide fiber reinforced composite materials of SiBCN is prepared.
Embodiment 6
Fiber volume fraction is that the SiCN fiber preforms of 15vol.% are placed in cvd furnace.CVI carbon-coatings, use butane for
Carbon source, Ar are carrier gas, and the flow of the two is respectively 20ml/min and 500ml/min, under the conditions of 950 DEG C, deposit 96h, deposition
Carbon layers having thicknesses be 5 μm.SiC coatings are prepared in situ in CVI, the SiO for being 99.9% by Si powder and purity that purity is 99.9%2
Mixture is heated to 1205 DEG C, and carrier gas Ar is heated to 1205 DEG C, after the two is converged, and mixed gas is pumped into cvd furnace.With
Temperature gradient CVI prepares SiC coatings, and the pressure of CVI is 100kPa, and sample front temperature is 1205 DEG C, rear part temperature 1250
DEG C, sedimentation time is that for 24 hours, the SiC thickness of formation is 5 μm.Then passing through CVI, that SiCN is prepared is silicon carbide fiber reinforced multiple
Condensation material.
Embodiment 7
Fiber volume fraction is that the SiBCN fiber preforms of 40vol.% are placed in cvd furnace.CVI carbon-coatings, use benzene for
Carbon source, Ar are carrier gas, and the flow of the two is respectively 35ml/min and 1500ml/min, under the conditions of 1050 DEG C, deposit 84h, sink
Long-pending carbon layers having thicknesses are 2.5 μm.SiC coatings are prepared in situ in CVI, and the Si powder that purity is 99.999% is heated to 1420 DEG C, is carried
Gas Ar is heated to 1420 DEG C, after the two is converged, and mixed gas is pumped into cvd furnace.With temperature gradient forced flow CVI systems
The pressure of standby SiC coatings, CVI is 175kPa, and sample front temperature is 1420 DEG C, and rear part temperature is 1450 DEG C, and sedimentation time is
The SiC thickness of 48h, formation are 2.5 μm.CVI prepares the BN coatings that thickness is 0.3 μm, obtains SiC-BN composite coatings.It is passed through after
It crosses PIP and the silicon carbide fiber reinforced composite materials of SiBCN is prepared.
Claims (7)
1. the system of SiC or C-SiC coatings is prepared in situ in a kind of fiber surface of non-oxidized substance fiber reinforced ceramic matrix composites
Preparation Method, which is characterized in that the preparation method includes：
（1）Fiber surface using chemical vapor infiltration in the fiber preform of non-seal coat forms one layer of C layers of amorphous；Step
（1）In, amorphous C layers of the thickness is 0.05-5 μm, and the fiber of fiber preform is carbon, silicon carbide, SiCN or SiBCN fine
Dimension；
（2）Using SiO as silicon source, the amorphous C layer segments of fiber surface are made using chemical vapor infiltration or are completely reformed into SiC；Step
Suddenly（2）In, carrier gas used in chemical vapor infiltration is argon gas, and carrier gas flux is 100~1500mL/minute, processing time 0.5
Hour or more；With Si and SiO2Reaction forms SiO as silicon source, Si and SiO2It is heated to 1200 DEG C to 1250 DEG C and generates silicon source steaming
Gas after carrier gas is heated to same temperature, then is mixed with the silicon source steam.
2. a kind of fiber surface of non-oxidized substance fiber reinforced ceramic matrix composites is prepared in situ (C-SiC)nThe preparation of coating
Method, which is characterized in that the preparation method includes：
（1）Fiber surface using chemical vapor infiltration in the fiber preform of non-seal coat forms one layer of C layers of amorphous；Step
（1）In, amorphous C layers of the thickness is 0.05-5 μm, and the fiber of fiber preform is carbon, silicon carbide, SiCN or SiBCN fine
Dimension；
（2）Using SiO as silicon source, the amorphous C layer segments of fiber surface are made using chemical vapor infiltration or are completely reformed into SiC；Step
Suddenly（2）In, carrier gas used in chemical vapor infiltration is argon gas, and carrier gas flux is 100~1500mL/minute, processing time 0.5
Hour or more；With Si and SiO2Reaction forms SiO as silicon source, Si and SiO2It is heated to 1200 DEG C to 1250 DEG C and generates silicon source steaming
Gas after carrier gas is heated to same temperature, then is mixed with the silicon source steam；Above steps may be repeated multiple times（1）With（2）To obtain
It states (C-SiC)nCoating.
3. preparation method according to claim 1 or 2, which is characterized in that step（1）In, chemical vapor infiltration uses etc.
Warm CVI, isothermal forced flow CVI, temperature gradient CVI, forced flow temperature gradient CVI, pulse CVI.
4. preparation method according to claim 1 or 2, which is characterized in that step（1）In, carbon source using alkane, alkene,
Alkynes or aromatic hydrocarbon, carbon source flow are 1~100mL/minute.
5. preparation method according to claim 4, which is characterized in that step（1）In, carbon source is using methane, ethane, third
Alkane, butane, acetylene, benzene.
6. preparation method according to claim 1 or 2, which is characterized in that step（1）In, chemical vapor infiltration is used to be carried
Gas is argon gas, and carrier gas flux is 100~1500mL/minute, ranging from 800~1200 DEG C of carrier gas temperature, processing time 0.5
Hour or more.
7. preparation method according to claim 1 or 2, which is characterized in that step（2）In, chemical vapor infiltration uses etc.
Warm forced flow CVI, temperature gradient CVI, forced flow temperature gradient CVI.
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| CN109053207B (en) * | 2018-10-16 | 2020-12-29 | 航天特种材料及工艺技术研究所 | Yttrium silicate modified silicon carbide fiber reinforced silicon carbide composite material and preparation method thereof |
| EP3962631A1 (en) * | 2019-05-01 | 2022-03-09 | King Abdullah University of Science and Technology | Hybrid inorganic oxide-carbon molecular sieve membranes |
| CN111943726B (en) * | 2020-08-11 | 2022-10-04 | 航天特种材料及工艺技术研究所 | High-performance C/SiBCN composite material and preparation method and application thereof |
| CN112299865A (en) * | 2020-11-19 | 2021-02-02 | 航天特种材料及工艺技术研究所 | Modified C/SiC composite material and preparation method thereof |
| CN115849955B (en) * | 2023-01-09 | 2023-08-01 | 中国人民解放军国防科技大学 | Continuous SiBCN ceramic fiber containing BNC in-situ coating and preparation method and application thereof |
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| CN101555139A (en) * | 2009-05-20 | 2009-10-14 | 中国人民解放军国防科学技术大学 | Method for preparing SiCf/SiC compound material by combination of chemical vapor carbon deposition process and gas phase siliconizing process |
| CN104817337A (en) * | 2015-04-20 | 2015-08-05 | 陕西科技大学 | Multi-scale-structure SiC/C porous composite ceramic and preparation method thereof |
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| CN100371302C (en) * | 2006-05-26 | 2008-02-27 | 中国科学院上海硅酸盐研究所 | Method for preparing carbon-fiber reinforced silicon carbonate base composite by gas-phase siliconizing technology |
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| CN101555139A (en) * | 2009-05-20 | 2009-10-14 | 中国人民解放军国防科学技术大学 | Method for preparing SiCf/SiC compound material by combination of chemical vapor carbon deposition process and gas phase siliconizing process |
| CN104817337A (en) * | 2015-04-20 | 2015-08-05 | 陕西科技大学 | Multi-scale-structure SiC/C porous composite ceramic and preparation method thereof |
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