CN103387405B - Preparation method of silicon carbide and silicon carbide composite material member - Google Patents

Preparation method of silicon carbide and silicon carbide composite material member Download PDF

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CN103387405B
CN103387405B CN201310287547.XA CN201310287547A CN103387405B CN 103387405 B CN103387405 B CN 103387405B CN 201310287547 A CN201310287547 A CN 201310287547A CN 103387405 B CN103387405 B CN 103387405B
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silicon carbide
preparation
polycarbosilane
carbon siclx
precast body
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CN103387405A (en
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李军平
张国兵
胡继东
赵彦伟
冯志海
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China Academy of Launch Vehicle Technology CALT
Aerospace Research Institute of Materials and Processing Technology
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Aerospace Research Institute of Materials and Processing Technology
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Abstract

The invention relates to a preparation method of silicon carbide and silicon carbide composite material member, especially relates to a preparation method of deformed silicon carbide and silicon carbide composite material member, and belongs to the technology field of ceramic matrix composite material. The impregnation phase and the precursor used in the preparation method not only comprise the solid PCS, but also comprise the liquid PCS, which is more cheap, so the technology matching property of the member is stronger, the densification efficiency of the member is improved to some degree, the cost is reduced and the preparation period of the member is shortened. The impregnation phase has little harm to the environment and the operators, and only a general type ventilation device is needed.

Description

A kind of preparation method of silicon carbide/carbon SiClx composite element
Technical field
The present invention relates to a kind of preparation method of silicon carbide/carbon SiClx composite element, particularly a kind of preparation method of special-shaped silicon carbide/carbon SiClx composite element, belongs to technology field of ceramic matrix composite material.
Background technology
As everyone knows, Continuous Fiber Reinforced Ceramic Matrix Composites has the features such as high temperature resistant, the high rigidity of stupalith, corrosion-resistant, high abrasion concurrently, and the enhancing of continuous fibre is on good terms and is effectively improved the obdurability of matrix material.For silicon carbide/carbon SiClx matrix material, because its fiber and matrix are silicon carbide, thermal mismatch problem can not be there is between the two, and its density is low, intensity is high, good rigidity, material itself then have resistance to elevated temperatures, particularly excellent intrinsic high-temperature oxidation resistance.Therefore, this material has broad application prospects at the high-technology field such as aerospace, nuclear industry.
The preparation method of silicon carbide/carbon SiClx matrix material mainly comprises following four kinds: chemical vapor infiltration (CVI), impregnating slurry pressure sintering (HP), nm immersion and instantaneous eutectic phase method (NITE) and polymer infiltration and pyrolysis method (PIP).Wherein HP and NITE method all needs to there is hot pressing process in the processing step later stage, has larger process limitation for the special-shaped material members particularly with complicated shape of preparation; And comparatively large for the damage of silicon carbide fiber, composite materials property aspect can be subject to larger negative impact.Meanwhile, for CVI technique, it can pass through technical arrangement plan, controls the heterogeneous composite material of Formed SiClx or carbon modified SiClx in silicon carbide fiber precast body, has certain process advantage.But CVI technique preparation cycle is long, very high to equipment and process control overflow, for preparing heavy wall (>=10mm), larger-size special-shaped component is comparatively difficult.Polymer infiltration and pyrolysis method, also known as polymer impregnation pyrolysis conversion method, is development in recent years one of prevailing technology preparing ceramic matric composite rapidly.It can by design and the molecular structure controlling organic precursor for the preparation of the ceramic matrix with specific components; Matrix material preparation temperature is lower, particularly has obvious advantage for preparing complicated shape heavy wall silicon carbide/carbon SiClx matrix material.Certainly, adopt PIP method also to there is the longer and prices of raw and semifnished materials costliness of preparation cycle and wait engineer applied problem.
Summary of the invention
The object of the invention is the preparation method in order to propose a kind of silicon carbide/carbon SiClx composite element, the method cost is low, the cycle is short, and prepared matrix material has excellent intrinsic antioxidant property.This invention for shortening composite element preparation cycle, reduce costs and all have important practical significance.
The object of the invention is to be achieved through the following technical solutions.
The preparation method of a kind of silicon carbide/carbon SiClx composite element of the present invention, step is:
1) preparation of silicon carbide fiber precast body: adopt Two-dimensional Carbon SiClx cloth laying or 3 D weaving technique to prepare silicon carbide fiber precast body, the preparation of profiling/clean whole size can be realized;
2) chemical Vapor deposition process prepares RESEARCH OF PYROCARBON interfacial layer: using methane, propane, propylene or acetylene gas as deposition carbon source, diluent gas is argon gas, silicon carbide fiber precast body step 1) obtained is placed in carbon laydown stove and deposits, at the surface deposition RESEARCH OF PYROCARBON interfacial layer of silicon carbide fiber; Processing parameter is as follows: depositing temperature is 850-1400 DEG C, and deposition pressure is 0.1-20KPa, and depositing time is 1-100 hour.Wherein the RESEARCH OF PYROCARBON interfacial layer thickness on silicon carbide fiber surface is 0.05-5 μm; Before deposition, specific frock is adopted to carry out " the dimension shape " of precast body; Described specific frock is the mating shapes with silicon carbide fiber precast body;
3) matrix densification: adopt PIP method to step 2) the silicon carbide fiber precast body that obtains carries out densification, obtains silicon carbide/carbon SiClx matrix material.
Above-mentioned steps 3) in the step of PIP method be: pressure impregnation is carried out to silicon carbide fiber precast body, is then cured, after having solidified, obtain base substrate; Pintsch process conversion is carried out to base substrate; The infiltration pyrolysis process finally circulating above-mentioned.Wherein, impregnation pressure is 0.1-10MPa, and dipping time is 1-10 hour, and dipping temperature is 20-120 DEG C; Solidification value is between 160-550 DEG C, and set time is 1-10 hour; The outlet temperature of Pintsch process is 900-1600 DEG C, and the time is 1-10 hour; The cycle index of infiltration pyrolysis is 5-15 time, finally realizes the matrix densification of matrix material.
Above-mentioned steps 3) in PIP method pressure impregnation time the dipping that uses comprise mutually in solid-state Polycarbosilane (PCS), the liquid PCS of liquid PCS(containing a kind of group in silico ethylene base, silene propyl group, silicon propargyl, silicon ethynylene group or mixed group of more than two kinds) or the mixture of solid-state PCS and liquid PCS, flood mutually and can also comprise solvent, solvent is tetrahydrofuran (THF), toluene, dimethylbenzene, divinylbenzene (DVB) or hexane, and wherein divinylbenzene also has the effect of crosslinking and curing agent simultaneously.Reasonably combined according to solvent and solute, and coordinate the round of dipping, the mass ratio of solvent and PCS is 0-5.
In the component of described dipping phase, can also comprise functionality ceramic powder, described functionality ceramic powder comprises active filler as Ti, Zr, Hf, Al, Si or B, or inert filler is as SiC powder, B 4c, TiB 2, TiC, ZrB 2, ZrC, HfB 2, HfC or Al 2o 3; The mode of blended, the solution movement blended under agitation of wet ball grinding or ultrasonic wave solution blending is adopted to carry out blended; Wherein functionality ceramic powder is micro-nano magnitude, and the functionality ceramic powder added accounts for the 0.05%-0.5% of PCS and solvent total mass.
Above-mentioned steps 3) in PIP law technology route step in, roughing operation can be added in the process of circulation infiltration pyrolysis, also can adopt the mode that clean whole size is shaping.In the later stage of densification, if when the rate of body weight gain of composites is less than 1%, densification terminates.
Beneficial effect
Dipping phase used in the present invention, the presoma adopted is except comprising solid-state PCS, and also comprise relatively cheap liquid PCS, process matching is stronger, and efficiency of densification can be improved to some extent, can reduce the cost simultaneously and shorten manufacturing cycle of material members.Simultaneously, when using liquid PCS, owing to itself being that (viscosity in case of heating can be thinning for thickness, be applicable to flood) or viscosity lower than the liquid of 1000 centipoises (under room temperature), can use not even with poisonous benzene homologues equal solvent less, whole steeping process can complete in room temperature or lower temperature (lower than 100 DEG C), the poisonous and harmful produced, inflammable and explosive material can decrease, the preferred harm to environment and operator of the dipping phase therefore in this invention is little, only needs the environmental practices such as universal ventilation installation.
Accompanying drawing explanation
Fig. 1 be the embodiment of the present invention 1 obtain silicon carbide/carbon SiClx matrix material flexural strength test after cross-section morphology stereoscan photograph;
Fig. 2 be the embodiment of the present invention 2 obtain silicon carbide/carbon SiClx matrix material flexural strength test after cross-section morphology stereoscan photograph;
Fig. 3 is the surface topography stereoscan photograph after the silicon carbide/carbon SiClx matrix material ablation that obtains of the embodiment of the present invention 4;
Fig. 4 is the cross-section morphology stereoscan photograph after the silicon carbide/carbon SiClx matrix material ablation that obtains of the embodiment of the present invention 4.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
A preparation method for silicon carbide/carbon SiClx composite element, step is:
1) preparation of silicon carbide fiber precast body: adopt Two-dimensional Carbon SiClx cloth laying or 3 D weaving technique to prepare silicon carbide fiber precast body;
2) chemical Vapor deposition process prepares RESEARCH OF PYROCARBON interfacial layer: using methane, propane, propylene or acetylene gas as deposition carbon source, diluent gas is argon gas, silicon carbide fiber precast body step 1) obtained is placed in carbon laydown stove and deposits, at the surface deposition RESEARCH OF PYROCARBON interfacial layer of silicon carbide fiber; Processing parameter is as follows: depositing temperature is 850-1400 DEG C, and deposition pressure is 0.1-20KPa, and depositing time is 1-100 hour.Wherein the RESEARCH OF PYROCARBON interfacial layer thickness on silicon carbide fiber surface is 0.05-5 μm;
3) matrix densification: adopt PIP method to step 2) the silicon carbide fiber precast body that obtains carries out densification, obtains silicon carbide/carbon SiClx matrix material; The step of PIP method is: carry out pressure impregnation to silicon carbide fiber precast body, be then cured, obtain base substrate after having solidified; Pintsch process conversion is carried out to base substrate.
Step 2) in before deposition, adopt the maintenance with the frock of the mating shapes of silicon carbide fiber precast body, precast body being carried out to shape.
Circulation step 3) in infiltration pyrolysis process, when matrix material rate of body weight gain is less than 1%, densification terminates.
In step 3), impregnation pressure is 0.1-10MPa, and dipping time is 1-10 hour, and dipping temperature is 20-120 DEG C; Solidification value is between 160-550 DEG C, and set time is 1-10 hour; The outlet temperature of Pintsch process is 900-1600 DEG C, and the time is 1-10 hour.
The dipping used during PIP method pressure impregnation in step 3) is Polycarbosilane mutually; Polycarbosilane is solid-state Polycarbosilane, liquid Polycarbosilane or the mixture of solid-state Polycarbosilane and liquid Polycarbosilane.
Containing a kind of group in silico ethylene base, silene propyl group, silicon propargyl, silicon ethynylene group or mixed group of more than two kinds in described liquid Polycarbosilane.
Described dipping mutually in also comprise solvent, solvent is the one in tetrahydrofuran (THF), toluene, dimethylbenzene, divinylbenzene or hexane, and the solvent added and the mass ratio of Polycarbosilane are a, 0 < a≤5.
Described dipping also comprises functionality ceramic powder mutually, and described functionality ceramic powder comprises active filler Ti, Zr, Hf, Al, Si or B, or inert filler SiC powder, B 4c, TiB 2, TiC, ZrB 2, ZrC, HfB 2, HfC or Al 2o 3; The functionality ceramic powder added accounts for the 0.05%-0.5% of Polycarbosilane and solvent total mass
The mode of blended, the solution movement blended under agitation of wet ball grinding or ultrasonic wave solution blending is adopted to carry out blended to functionality ceramic powder, Polycarbosilane and solvent.
Functionality ceramic powder is micro-nano magnitude.
Embodiment 1
A preparation method for silicon carbide/carbon SiClx composite element, comprises following step:
1) take continuous carbofrax fibre as raw material, be first made into plain, then adopt sewing process at the auxiliary lower obtained arc precast body of graphite frock;
2) take methane as carbon-source gas, precast body step 1) obtained is placed in cvd furnace and carries out chemical vapour deposition, at the silicon carbide fiber surface deposition RESEARCH OF PYROCARBON interfacial layer of precast body.The processing condition of chemical vapour deposition are: depositing temperature is 900 DEG C, and deposition pressure is 0.15KPa, and depositing time is 40 hours.Wherein the interfacial layer thickness of RESEARCH OF PYROCARBON is 0.17 μm;
3) adopt the mode of vacuum aided, after the dipping prepared is preheated to 60 DEG C mutually, is incorporated into and deposited in the silicon carbide fiber precast body of RESEARCH OF PYROCARBON interfacial layer, final impregnation pressure is 3MPa.Wherein, dipping mutually in be 1:0.2 containing the mass ratio of liquid PCS and DVB of vinyl, and by the liquid PCS solution of vinyl for preparing and silicon carbide powder blended with weight ratio 1:0.5, the median size of silicon carbide powder is 0.5 μm; Ball milling forms final dipping phase after 4 hours;
4) what flood phase is solidificated in N 2carry out in atmosphere, solidification holding temperature is 200 DEG C and 400 DEG C, and soaking time is respectively 3h and 5h; Pintsch process carries out in an ar atmosphere, and burning temperature is eventually 1000 DEG C, and soaking time is 10 hours;
5) mode of circulation infiltration pyrolysis is adopted to carry out densification in the sample of above-mentioned process, cycle index is 10 times, and sample rate of body weight gain is less than 0.1%, namely achieves the densification of material, obtain final arc silicon carbide/carbon SiClx composite element, its density is 2.3g/cm 3, the flexural strength with stove flat board is 402MPa, and modulus in flexure is 95Gpa.As shown in Figure 1, matrix material presents comparatively significantly spike protein gene to cross-section morphology after the test of its flexural strength, illustrates that continuous fibre has brought reinforced effects into play, shows comparatively significantly ductile rupture characteristic.
Embodiment 2
A preparation method for silicon carbide/carbon SiClx composite element, comprises following step:
1) take continuous carbofrax fibre as raw material, be first made into five heddle satin cloth, then adopt the mode of two-dimentional laying to form T-shaped precast body in graphite frock;
2) take propane as carbon-source gas, precast body is placed in cvd furnace and carries out chemical vapour deposition, at the silicon carbide fiber surface deposition RESEARCH OF PYROCARBON interfacial layer of precast body.The processing condition of chemical vapour deposition are: depositing temperature is 1200 DEG C, and deposition pressure is 1.0KPa, and depositing time is 20 hours.Wherein the interfacial layer thickness of RESEARCH OF PYROCARBON is about 0.15 μm;
3) adopt the mode of vacuum aided, be incorporated into mutually by the dipping prepared and deposited in the silicon carbide precast body of RESEARCH OF PYROCARBON interfacial layer, final impregnation pressure is 2MPa.Wherein, dipping mutually in be 1:0.8 containing the mass ratio of the liquid PCS and solid-state PCS of propargyl, and by the solution for preparing and silicon carbide powder blended with weight ratio 1:0.2, ball milling forms final dipping phase after 10 hours;
4) what flood phase is solidificated in N 2carry out in atmosphere, solidification holding temperature is 150 DEG C and 350 DEG C, and soaking time is respectively 2h and 5 hour; Pintsch process carries out in an ar atmosphere, and burning temperature is eventually 1200 DEG C, and soaking time is 2 hours;
5) adopted by the sample of above-mentioned process the mode of circulation infiltration pyrolysis to carry out densification (wherein flooding phase composite slightly to adjust), cycle index is 8 times, and sample rate of body weight gain is less than 0.1%, namely achieves the densification of material.
6) by precision work, obtain final silicon carbide/carbon SiClx composite element, its density is 2.25g/cm 3, the flexural strength with stove flat board is 370MPa, and modulus in flexure is 82GPa, cross-section morphology after the test of its flexural strength as shown in Figure 2, matrix material presents comparatively significantly spike protein gene, illustrates that continuous fibre has brought reinforced effects into play, shows comparatively significantly ductile rupture characteristic.
Embodiment 3
A preparation method for silicon carbide/carbon SiClx composite element, comprises following step:
1) take continuous carbofrax fibre as raw material, adopt three-dimensional four-way craft woven to become thrust chamber precast body (band graphite inner core);
2) take acetylene as carbon-source gas, precast body is placed in cvd furnace and carries out chemical vapour deposition, at the silicon carbide fiber surface deposition RESEARCH OF PYROCARBON interfacial layer of precast body.The processing condition of chemical vapour deposition are: depositing temperature is 1000 DEG C, and deposition pressure is 4.0KPa, and depositing time is 30 hours.Wherein the interfacial layer thickness of RESEARCH OF PYROCARBON is about 0.23 μm;
3) adopt the mode of vacuum aided, be incorporated into mutually by the dipping prepared and deposited in the silicon carbide precast body of RESEARCH OF PYROCARBON interfacial layer, final impregnation pressure is 1MPa.Wherein, dipping mutually in blended with weight ratio 1:0.1:0.1 containing the liquid PCS of propargyl and silicon carbide, Zr powder, ball milling forms final dipping phase after 10 hours;
4) what flood phase is solidificated in N 2carry out in atmosphere, solidification holding temperature is 180 DEG C and 420 DEG C, and soaking time is respectively 1h and 2 hour; Pintsch process carries out in an ar atmosphere, and burning temperature is eventually 1300 DEG C, and soaking time is 2 hours;
5) adopted by the sample of above-mentioned process the mode of circulation infiltration pyrolysis to carry out densification (wherein flooding phase composite slightly to adjust), cycle index is 9 times, and sample rate of body weight gain is less than 0.1%, namely achieves the densification of material.
6) by precision work, obtain final silicon carbide/carbon SiClx composite element, its density is 2.32g/cm 3, the flexural strength with stove flat board is 356MPa, and modulus in flexure is 89GPa.
Embodiment 4
A preparation method for silicon carbide/carbon SiClx composite element, comprises following step:
1) take continuous carbofrax fibre as raw material, first prepare silicon carbide without latitude cloth and net tire, then by replacing the mode of laying without latitude cloth and net tire, successively superpose, successively amplify, and successively adopt acupuncture to fix the imitative type stereo fabric forming L-type, and undertaken " d type " by graphite frock;
2) take acetylene as carbon-source gas, precast body is placed in cvd furnace and carries out chemical vapour deposition, at the silicon carbide fiber surface deposition RESEARCH OF PYROCARBON interfacial layer of precast body.The processing condition of chemical vapour deposition are: depositing temperature is 1050 DEG C, and deposition pressure is 0.4KPa, and depositing time is 4 hours.Wherein the interfacial layer thickness of RESEARCH OF PYROCARBON is about 0.08 μm;
3) adopt the mode of vacuum aided, be incorporated into mutually by the dipping prepared and deposited in the silicon carbide precast body of RESEARCH OF PYROCARBON interfacial layer, final impregnation pressure is 4MPa.Wherein, flood mutually containing allylic liquid PCS and silicon carbide, ZrB 2powder is blended with weight ratio 1:0.05:0.2, and ball milling forms final dipping phase after 10 hours;
4) what flood phase is solidificated in N 2carry out in atmosphere, solidification heat preservation zone is 180 DEG C and 350 DEG C, and soaking time is respectively 2h and 2 hour; Pintsch process carries out in an ar atmosphere, and burning temperature is eventually 1500 DEG C, and soaking time is 2 hours;
5) carry out the later stage of matrix densification at infiltration pyrolysis, according to the situation of weightening finish with surface " sealing of hole ", add 2 rough machined operations;
6) adopted by the sample of above-mentioned process the mode of circulation infiltration pyrolysis to carry out densification (wherein flooding phase composite slightly to adjust), cycle index is 8 times, and sample rate of body weight gain is less than 0.1%, namely achieves the densification of material.
7) by precision work, obtain final silicon carbide/carbon SiClx composite element, its density is 2.38g/cm 3, the flexural strength with stove flat board is 337MPa, and modulus in flexure is 85GPa.
8) 800s(surface temperature is examined to be 1450 DEG C with stove flat board (surface is without oxidation resistant coating) electric arc tunnel ablation test), the linear ablative rate of test specimen is 1.0 × 10 -5– 8.2 × 10 -5mm/s, shows excellent intrinsic antioxidant property.As shown in Figures 3 and 4, after ablation examination, material shows the silicon-dioxide oxide film defining one deck densification, thus effectively prevents oxygen to the diffusion of material internal for surface after its ablation and cross-section morphology; This oxidated layer thickness only has tens microns simultaneously, shows the intrinsic antioxidant characteristics of silicon carbide/carbon SiClx matrix material excellence at such a temperature.
The above; be only the embodiment of the best of the present invention, but protection scope of the present invention is not limited thereto, any those skilled in the art of being familiar with are in the technical scope that the present invention covers; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.The content be not described in detail in specification sheets of the present invention belongs to the known technology of professional and technical personnel in the field.

Claims (8)

1. a preparation method for silicon carbide/carbon SiClx composite element, is characterized in that step is:
1) preparation of silicon carbide fiber precast body: adopt Two-dimensional Carbon SiClx cloth laying or 3 D weaving technique to prepare silicon carbide fiber precast body;
2) chemical Vapor deposition process prepares RESEARCH OF PYROCARBON interfacial layer: using methane, propane, propylene or acetylene gas as deposition carbon source, diluent gas is argon gas, by step 1) the silicon carbide fiber precast body that obtains is placed in carbon laydown stove and deposits, at the surface deposition RESEARCH OF PYROCARBON interfacial layer of silicon carbide fiber; Processing parameter is as follows: depositing temperature is 850-1400 DEG C, and deposition pressure is 0.1-20KPa, and depositing time is 1-100 hour; Wherein the RESEARCH OF PYROCARBON interfacial layer thickness on silicon carbide fiber surface is 0.05-5 μm;
3) matrix densification: adopt PIP method to step 2) the silicon carbide fiber precast body that obtains carries out densification, obtains silicon carbide/carbon SiClx matrix material; The step of PIP method is: carry out pressure impregnation to silicon carbide fiber precast body, be then cured, obtain base substrate after having solidified; Pintsch process conversion is carried out to base substrate;
Step 2) in before deposition, adopt the maintenance with the frock of the mating shapes of silicon carbide fiber precast body, precast body being carried out to shape;
Step 3) in impregnation pressure be 0.1-10MPa, dipping time is 1-10 hour, and dipping temperature is 20-120 DEG C; Solidification value is between 160-550 DEG C, and set time is 1-10 hour; The outlet temperature of Pintsch process is 900-1600 DEG C, and the time is 1-10 hour.
2. the preparation method of a kind of silicon carbide/carbon SiClx composite element according to claim 1, is characterized in that: circulation step 3) in infiltration pyrolysis process, when matrix material rate of body weight gain is less than 1%, densification terminates.
3. the preparation method of a kind of silicon carbide/carbon SiClx composite element according to claim 1, is characterized in that: step 3) in PIP method pressure impregnation time the dipping that uses be Polycarbosilane mutually; Polycarbosilane is solid-state Polycarbosilane, liquid Polycarbosilane or the mixture of solid-state Polycarbosilane and liquid Polycarbosilane.
4. the preparation method of a kind of silicon carbide/carbon SiClx composite element according to claim 3, is characterized in that: containing a kind of group in silico ethylene base, silene propyl group, silicon propargyl, silicon ethynylene group or mixed group of more than two kinds in described liquid Polycarbosilane.
5. the preparation method of a kind of silicon carbide/carbon SiClx composite element according to claim 3, it is characterized in that: described dipping mutually in also comprise solvent, solvent is the one in tetrahydrofuran (THF), toluene, dimethylbenzene, divinylbenzene or hexane, the solvent added and the mass ratio of Polycarbosilane are a, 0 < a≤5.
6. the preparation method of a kind of silicon carbide/carbon SiClx composite element according to claim 5, it is characterized in that: described dipping also comprises functionality ceramic powder mutually, described functionality ceramic powder comprises active filler Ti, Zr, Hf, Al, Si or B, or inert filler SiC powder, B 4c, TiB 2, TiC, ZrB 2, ZrC, HfB 2, HfC or Al 2o 3; The functionality ceramic powder added accounts for the 0.05%-0.5% of Polycarbosilane and solvent total mass.
7. the preparation method of a kind of silicon carbide/carbon SiClx composite element according to claim 6, is characterized in that: adopt the mode of blended, the solution movement blended under agitation of wet ball grinding or ultrasonic wave solution blending to carry out blended to functionality ceramic powder, Polycarbosilane and solvent.
8. the preparation method of a kind of silicon carbide/carbon SiClx composite element according to claim 6, is characterized in that: functionality ceramic powder is micro-nano magnitude.
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CN116813363A (en) * 2023-05-15 2023-09-29 北京航空航天大学 Antioxidant SiC f /SiC-HfB 2 Preparation method of composite material
CN117285371B (en) * 2023-11-23 2024-03-01 北京天仁道和新材料有限公司 Ultrahigh-temperature ceramic matrix composite material and preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1803715A (en) * 2006-01-24 2006-07-19 中国人民解放军国防科学技术大学 Method for preparing silicon carbide fiber reinforced silicon carbide composite material
CN102249721A (en) * 2011-05-20 2011-11-23 中国人民解放军国防科学技术大学 Method for preparing carbon-fiber-reinforced silicon carbide composite material
CN102276279A (en) * 2011-06-10 2011-12-14 中国人民解放军国防科学技术大学 Preparation method of silicon carbide fiber reinforced silicon carbide composite material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1803715A (en) * 2006-01-24 2006-07-19 中国人民解放军国防科学技术大学 Method for preparing silicon carbide fiber reinforced silicon carbide composite material
CN102249721A (en) * 2011-05-20 2011-11-23 中国人民解放军国防科学技术大学 Method for preparing carbon-fiber-reinforced silicon carbide composite material
CN102276279A (en) * 2011-06-10 2011-12-14 中国人民解放军国防科学技术大学 Preparation method of silicon carbide fiber reinforced silicon carbide composite material

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