CN102910927A - Method for preparing self-healing silicon carbide ceramic-based composite material - Google Patents

Method for preparing self-healing silicon carbide ceramic-based composite material Download PDF

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CN102910927A
CN102910927A CN2012104651110A CN201210465111A CN102910927A CN 102910927 A CN102910927 A CN 102910927A CN 2012104651110 A CN2012104651110 A CN 2012104651110A CN 201210465111 A CN201210465111 A CN 201210465111A CN 102910927 A CN102910927 A CN 102910927A
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silicon carbide
carbide fiber
precast body
fiber precast
graphite jig
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CN102910927B (en
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邱海鹏
焦健
李秀倩
王宇
邹豪
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AVIC Beijing Aeronautical Manufacturing Technology Research Institute
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Abstract

The invention belongs to a preparation technology of a silicon carbide ceramic-based composite material and relates to the improvement on a method for preparing the self-healing silicon carbide fiber-reinforced ceramic-based composite material. The method is characterized by comprising the following steps of: preparing silicon carbide fiber precast body, preparing precursor steeping liquor; preparing silicon carbide fiber precast body interface layer; molding, vacuum steeping, drying, hot mold pressing, and cracking; steeping-drying-cracking with a die; and steeping-drying-cracking without the die. The method for preparing the self-healing silicon carbide ceramic-based composite material disclosed by the invention has the advantages that the process is simple, requirements on the device are low, the preparation period is short, the preparation cost is low, and the self-healing oxidation capacity resistance is strong.

Description

A kind of preparation method of self-sealing silicon carbide ceramic based composite material
Technical field
The invention belongs to the technology of preparing of carbon/silicon carbide ceramic matrix composite, relate to the improvement to the silicon carbide fiber reinforced ceramic matric composite preparation method of self-sealing silicon carbide.
Background technology
Silicon carbide fiber reinforced silicon carbide ceramic matric composite (SiC f/ SiC) in thyrite, add silicon carbide fiber to prepare as second-phase, its can be in breaking-down process by crack deflection, fibre breakage with the machine-processed receptivity such as extract, the intensity of strongthener and toughness.SiC fThe advantages such as/SiC has high specific strength, high ratio modulus, high rigidity, wear-resistant, anti-oxidant, anticorrosive, high-temperature stability is good, the desirable high-temperature structural materials of field a new generation such as aerospace and nuclear industry have been become, especially the indispensable thermal structure material of thrust-weight ratio 10 above aircraft engines has the significantly potentiality of loss of weight, raising use temperature and over-all properties.But, because SiC fContain certain free C in the matrix SiC of/SiC and the enhancing body SiC fiber, the thermal stresses that produces in preparation and use procedure can cause the SiC matrix to produce tiny crack, its inner residual hole of about 10% in this external material preparation process.Tiny crack and hole cause SiC f/ SiC at high temperature oxidizing medium can direct effect to material internal, weakened SiC fThe resistance of oxidation of/SiC, and then restricted SiC f/ SiC is in the application in interior high temperature resistant long-life high thrust-weight ratio aircraft engine field.
Often be used to improve SiC f/ SiC long lifetime antioxidation method has employing chemical vapor infiltration (CVI) preparation to have the multilayer (SiC-BC of self-healing function x) nMatrix [ patent: application number is 200910021047.5 ], but the CVI technological process is comparatively complicated, high to equipment requirements, preparation cycle is long, preparation cost is high.[ patent: application number is 200910049376.0 ] adopts boron powder, ZrB2, B4C etc. to contain boron substance as active filler, adopts slurry method and PIP method to carry out the development of self-healing ceramic matric composite.[ patent: application number is 201010013506.8 ] adopts the slurry Infiltration Technics to introduce the B4C particle, by liquid silicon infiltration technique Si introduced composite inner again, generates SiB4 and SiC with the B4C reaction in-situ.But adopt the method for active powder stuffing, be difficult to guarantee that active powder stuffing can be uniformly dispersed on the one hand in the organic precursor method steeping fluid, there is the infiltration bottleneck effect in active powder stuffing in steeping process on the other hand, has therefore weakened the self-healing anti-aging capability of ceramic matric composite.
Summary of the invention
The objective of the invention is: the preparation method who proposes the self-sealing silicon carbide ceramic based composite material that a kind of technique is simple, low for equipment requirements, preparation cycle is short, preparation cost is low, the self-healing anti-aging capability is strong.
Technical scheme of the present invention is: a kind of preparation method of self-sealing silicon carbide ceramic based composite material, it is characterized in that, and the step of preparation is as follows:
1, preparation silicon carbide fiber precast body: prepare the silicon carbide fiber precast body take continuous carbofrax fibre as starting material, its structure formation is: 2 dimension fiber layings, 2.5 dimension fibrages, 3 dimension fibrages or 3 dimension fiber needled felts;
2, preparation precursor steeping fluid: take Polycarbosilane and trimethylamine groups borine polymkeric substance as solute, prepare the precursor steeping fluid take dimethylbenzene as solvent, the weight percent that solute accounts for the precursor steeping fluid is 45%~60%, and the weight percent that Polycarbosilane accounts for solute is 60%~85%;
3, preparation silicon carbide fiber preform interface layer: the silicon carbide fiber precast body is placed in the chemical vapor deposition stove, take propane as source of the gas, preparation silicon carbide fiber precast body RESEARCH OF PYROCARBON interfacial layer, depositing temperature: 1000 ℃, gas flow: 1.0L/min, furnace pressure :≤2KPa, depositing time: 4~6h; Prepared RESEARCH OF PYROCARBON interfacial layer thickness is 0.1~0.5 μ m;
4, finalize the design: the silicon carbide fiber precast body is placed in the graphite jig finalize the design;
5, vacuum impregnation: graphite jig is put into vacuum impregnation equipment, the inner chamber of this vacuum impregnation equipment is communicated with the container that the precursor steeping fluid is housed by a pipeline with switch, switch on blinding off a line, inner chamber to vacuum impregnation equipment vacuumizes, until vacuum pressure is not higher than 0.01MPa, open the switch on the pipeline, the precursor steeping fluid is sucked in the encloses container by the pipeline with switch, flood graphite jig, switch on again blinding off a line, silicon carbide fiber precast body in the graphite jig is flooded, and dipping time is 10h~30h;
6, drying: after dipping is finished, graphite jig is taken out from vacuum impregnation equipment, place air, then at ambient temperature seasoning places baking oven with graphite jig, and oven dry is no less than 2h under 80 ℃~120 ℃ temperature;
7, hot moulding: graphite jig is put on the platform of thermocompressor, risen to 190 ℃~220 ℃ with the temperature rise rate of 10 ℃/min, be incubated 30 minutes, then give mould pressurizing to 3MPa~6MPa, pressurize and stopped heating are until naturally be cooled to release after the room temperature;
8, cracking: graphite jig is put into pyrolyzer, be evacuated to less than 1KPa, then the temperature rise rate with 10 ℃/min rises to 1050 ℃~1150 ℃, behind insulation 30min~60min, naturally is cooled to room temperature;
9, band mould impregnation drying cracking: the silicon carbide fiber precast body is no less than the cracking of 3 band mould impregnation dryings, and the process with the mould infiltration pyrolysis is at every turn: repeating step 5, step 6 and step 8;
10, go the cracking of mould impregnation drying: the silicon carbide fiber precast body is taken out from graphite jig, be no less than 10 times and go the cracking of mould impregnation drying, go the process of mould infiltration pyrolysis to be at every turn:
10.1, vacuum impregnation: the silicon carbide fiber precast body is put into vacuum impregnation equipment flood, vacuum pressure is not higher than 0.01MPa, and dipping time is 10h~30h;
10.2, drying: the dipping finish after, the silicon carbide fiber precast body is taken out from vacuum impregnation equipment, place air, at ambient temperature seasoning, then the silicon carbide fiber precast body is placed baking oven, oven dry is no less than 2h under 80 ℃~120 ℃ temperature;
10.3, cracking: the silicon carbide fiber precast body is put into pyrolyzer, be evacuated to less than 1kPa, then the temperature rise rate with 10 ℃/min rises to 1050 ℃~1150 ℃, the insulation 30min~60min after, naturally be cooled to room temperature.
Advantage of the present invention is: technique is simple, and is low for equipment requirements, and preparation cycle is short, and preparation cost is low, and the self-healing anti-aging capability is strong.
Embodiment
The below is described in further details the present invention.A kind of preparation method of self-sealing silicon carbide ceramic based composite material is characterized in that, the step of preparation is as follows:
1, preparation silicon carbide fiber precast body: prepare the silicon carbide fiber precast body take continuous carbofrax fibre as starting material, its structure formation is: 2 dimension fiber layings, 2.5 dimension fibrages, 3 dimension fibrages or 3 dimension fiber needled felts;
2, preparation precursor steeping fluid: take Polycarbosilane and trimethylamine groups borine polymkeric substance as solute, prepare the precursor steeping fluid take dimethylbenzene as solvent, the weight percent that solute accounts for the precursor steeping fluid is 45%~60%, and the weight percent that Polycarbosilane accounts for solute is 60%~85%;
3, preparation silicon carbide fiber preform interface layer: the silicon carbide fiber precast body is placed in the chemical vapor deposition stove, take propane as source of the gas, preparation silicon carbide fiber precast body RESEARCH OF PYROCARBON interfacial layer, depositing temperature: 1000 ℃, gas flow: 1.0L/min, furnace pressure :≤2KPa, depositing time: 4~6h; Prepared RESEARCH OF PYROCARBON interfacial layer thickness is 0.1~0.5 μ m;
4, finalize the design: the silicon carbide fiber precast body is placed in the graphite jig finalize the design;
5, vacuum impregnation: graphite jig is put into vacuum impregnation equipment, the inner chamber of this vacuum impregnation equipment is communicated with the container that the precursor steeping fluid is housed by a pipeline with switch, switch on blinding off a line, inner chamber to vacuum impregnation equipment vacuumizes, until vacuum pressure is not higher than 0.01MPa, open the switch on the pipeline, the precursor steeping fluid is sucked in the encloses container by the pipeline with switch, flood graphite jig, switch on again blinding off a line, silicon carbide fiber precast body in the graphite jig is flooded, and dipping time is 10h~30h;
6, drying: after dipping is finished, graphite jig is taken out from vacuum impregnation equipment, place air, then at ambient temperature seasoning places baking oven with graphite jig, and oven dry is no less than 2h under 80 ℃~120 ℃ temperature;
7, hot moulding: graphite jig is put on the platform of thermocompressor, risen to 190 ℃~220 ℃ with the temperature rise rate of 10 ℃/min, be incubated 30 minutes, then give mould pressurizing to 3MPa~6MPa, pressurize and stopped heating are until naturally be cooled to release after the room temperature;
8, cracking: graphite jig is put into pyrolyzer, be evacuated to less than 1kPa, then the temperature rise rate with 10 ℃/min rises to 1050 ℃~1150 ℃, behind insulation 30min~60min, naturally is cooled to room temperature;
9, band mould impregnation drying cracking: the silicon carbide fiber precast body is no less than the cracking of 3 band mould impregnation dryings, and the process with the mould infiltration pyrolysis is at every turn: repeating step 5, step 6 and step 8;
10, go the cracking of mould impregnation drying: the silicon carbide fiber precast body is taken out from graphite jig, be no less than 10 times and go the cracking of mould impregnation drying, go the process of mould infiltration pyrolysis to be at every turn:
10.1, vacuum impregnation: the silicon carbide fiber precast body is put into vacuum impregnation equipment flood, vacuum pressure is not higher than 0.01MPa, and dipping time is 10h~30h;
10.2, drying: the dipping finish after, the silicon carbide fiber precast body is taken out from vacuum impregnation equipment, place air, at ambient temperature seasoning, then the silicon carbide fiber precast body is placed baking oven, oven dry is no less than 2h under 80 ℃~120 ℃ temperature;
10.3, cracking: the silicon carbide fiber precast body is put into pyrolyzer, be evacuated to less than 1kPa, then the temperature rise rate with 10 ℃/min rises to 1050 ℃~1150 ℃, the insulation 30min~60min after, naturally be cooled to room temperature.
Embodiment 1
1, preparation silicon carbide fiber precast body: prepare 3 dimension fibrage silicon carbide fiber precast bodies take continuous carbofrax fibre as starting material.
2, preparation precursor steeping fluid: take Polycarbosilane and trimethylamine groups borine polymkeric substance as solute, prepare the precursor steeping fluid take dimethylbenzene as solvent, the weight percent that solute accounts for the precursor steeping fluid is 60%, and the weight percent that Polycarbosilane accounts for solute is 55%;
3, preparation silicon carbide fiber preform interface layer: the silicon carbide fiber precast body is placed in the chemical vapor deposition stove, take propane as source of the gas, preparation silicon carbide fiber precast body RESEARCH OF PYROCARBON interfacial layer, the processing condition of chemical vapour deposition are: propane flow 2L/min; N 2Flow 2L/min; Furnace pressure≤2KPa; 1000 ℃ of temperature; Depositing time 10h;
4, finalize the design: the silicon carbide fiber precast body is placed in the graphite jig finalize the design;
5, vacuum impregnation: graphite jig is put into vacuum impregnation equipment, the inner chamber of this vacuum impregnation equipment is communicated with the container that the precursor steeping fluid is housed by a pipeline with switch, switch on blinding off a line, inner chamber to vacuum impregnation equipment vacuumizes, until vacuum pressure is not higher than 0.01MPa, open the switch on the pipeline, the precursor steeping fluid is sucked in the encloses container by the pipeline with switch, flood graphite jig, switch on again blinding off a line, silicon carbide fiber precast body in the graphite jig is flooded, and dipping time is 25h;
6, drying: after dipping is finished, graphite jig is taken out from vacuum impregnation equipment, place air, then at ambient temperature seasoning places baking oven with graphite jig, and oven dry is no less than 2h under 80 ℃ of temperature;
7, hot moulding: graphite jig is put on the platform of thermocompressor, risen to 200 ℃ with the temperature rise rate of 10 ℃/min, be incubated 20 minutes, then give mould pressurizing to 4MPa, pressurize and stopped heating are until naturally be cooled to release after the room temperature;
8, cracking: graphite jig is put into pyrolyzer, be evacuated to less than 1kPa, then the temperature rise rate with 10 ℃/min rises to 1100 ℃, behind the insulation 60min, naturally is cooled to room temperature;
9, band mould impregnation drying cracking: the silicon carbide fiber precast body is no less than the cracking of 3 band mould impregnation dryings, and the process with the mould infiltration pyrolysis is at every turn: repeating step 5, step 6 and step 8;
10, go the cracking of mould impregnation drying: the silicon carbide fiber precast body is taken out from graphite jig, be no less than 10 times and go the cracking of mould impregnation drying, go the process of mould infiltration pyrolysis to be at every turn:
10.1, vacuum impregnation: the silicon carbide fiber precast body is put into vacuum impregnation equipment flood, vacuum pressure is not higher than 0.01MPa, and dipping time is 25h;
10.2, drying: after dipping is finished, the silicon carbide fiber precast body is taken out from vacuum impregnation equipment, place air, then at ambient temperature seasoning places baking oven with the silicon carbide fiber precast body, and oven dry is no less than 2h under 80 ℃ of temperature;
10.3, cracking: the silicon carbide fiber precast body is put into pyrolyzer, be evacuated to less than 1kPa, then the temperature rise rate with 10 ℃/min rises to 1100 ℃, the insulation 60min after, naturally be cooled to room temperature.
Embodiment 2
1, preparation silicon carbide fiber precast body: prepare 3 dimension fibrage silicon carbide fiber precast bodies take continuous carbofrax fibre as starting material.
2, preparation precursor steeping fluid: take Polycarbosilane and trimethylamine groups borine polymkeric substance as solute, prepare the precursor steeping fluid take dimethylbenzene as solvent, the weight percent that solute accounts for the precursor steeping fluid is 60%, and the weight percent that Polycarbosilane accounts for solute is 66.7%;
3, preparation silicon carbide fiber preform interface layer: the silicon carbide fiber precast body is placed in the chemical vapor deposition stove, take propane as source of the gas, preparation silicon carbide fiber precast body RESEARCH OF PYROCARBON interfacial layer, the processing condition of chemical vapour deposition are: propane flow 2L/min; N 2Flow 2L/min; Furnace pressure 2KPa; 1000 ℃ of temperature; Depositing time 5h;
4, finalize the design: the silicon carbide fiber precast body is placed in the graphite jig finalize the design;
5, vacuum impregnation: graphite jig is put into vacuum impregnation equipment, the inner chamber of this vacuum impregnation equipment is communicated with the container that the precursor steeping fluid is housed by a pipeline with switch, switch on blinding off a line, inner chamber to vacuum impregnation equipment vacuumizes, until vacuum pressure is not higher than 0.01MPa, open the switch on the pipeline, the precursor steeping fluid is sucked in the encloses container by the pipeline with switch, flood graphite jig, switch on again blinding off a line, silicon carbide fiber precast body in the graphite jig is flooded, and dipping time is 25h;
6, drying: after dipping is finished, graphite jig is taken out from vacuum impregnation equipment, place air, then at ambient temperature seasoning places baking oven with graphite jig, and oven dry is no less than 2h under 80 ℃ of temperature;
7, hot moulding: graphite jig is put on the platform of thermocompressor, risen to 200 ℃ with the temperature rise rate of 10 ℃/min, be incubated 20 minutes, then give mould pressurizing to 4MPa, pressurize and stopped heating are until naturally be cooled to release after the room temperature;
8, cracking: graphite jig is put into pyrolyzer, be evacuated to less than 1kPa, then the temperature rise rate with 10 ℃/min rises to 1100 ℃, behind the insulation 60min, naturally is cooled to room temperature;
9, band mould impregnation drying cracking: the silicon carbide fiber precast body is no less than the cracking of 3 band mould impregnation dryings, and the process with the mould infiltration pyrolysis is at every turn: repeating step 5, step 6 and step 8;
10, go the cracking of mould impregnation drying: the silicon carbide fiber precast body is taken out from graphite jig, be no less than 10 times and go the cracking of mould impregnation drying, go the process of mould infiltration pyrolysis to be at every turn:
10.1, vacuum impregnation: the silicon carbide fiber precast body is put into vacuum impregnation equipment flood, vacuum pressure is not higher than 0.01MPa, and dipping time is 25h;
10.2, drying: after dipping is finished, the silicon carbide fiber precast body is taken out from vacuum impregnation equipment, place air, then at ambient temperature seasoning places baking oven with the silicon carbide fiber precast body, and oven dry is no less than 2h under 80 ℃ of temperature;
10.3, cracking: the silicon carbide fiber precast body is put into pyrolyzer, be evacuated to less than 1kPa, then the temperature rise rate with 10 ℃/min rises to 1100 ℃, the insulation 60min after, naturally be cooled to room temperature.
Embodiment 3
1, preparation silicon carbide fiber precast body: prepare 2.5 dimension fibrage silicon carbide fiber precast bodies take continuous carbofrax fibre as starting material.
2, preparation precursor steeping fluid: take Polycarbosilane and trimethylamine groups borine polymkeric substance as solute, prepare the precursor steeping fluid take dimethylbenzene as solvent, the weight percent that solute accounts for the precursor steeping fluid is 60%, and the weight percent that Polycarbosilane accounts for solute is 80%;
3, preparation silicon carbide fiber preform interface layer: the silicon carbide fiber precast body is placed in the chemical vapor deposition stove, take propane as source of the gas, preparation silicon carbide fiber precast body RESEARCH OF PYROCARBON interfacial layer, the processing condition of chemical vapour deposition are: propane flow 2L/min; N 2Flow 2L/min; Furnace pressure≤2KPa; 1000 ℃ of temperature; Depositing time 5h;
4, finalize the design: the silicon carbide fiber precast body is placed in the graphite jig finalize the design;
5, vacuum impregnation: graphite jig is put into vacuum impregnation equipment, the inner chamber of this vacuum impregnation equipment is communicated with the container that the precursor steeping fluid is housed by a pipeline with switch, switch on blinding off a line, inner chamber to vacuum impregnation equipment vacuumizes, until vacuum pressure is not higher than 0.01MPa, open the switch on the pipeline, the precursor steeping fluid is sucked in the encloses container by the pipeline with switch, flood graphite jig, switch on again blinding off a line, silicon carbide fiber precast body in the graphite jig is flooded, and dipping time is 25h;
6, drying: after dipping is finished, graphite jig is taken out from vacuum impregnation equipment, place air, then at ambient temperature seasoning places baking oven with graphite jig, and oven dry is no less than 2h under 80 ℃ of temperature;
7, hot moulding: graphite jig is put on the platform of thermocompressor, risen to 200 ℃ with the temperature rise rate of 10 ℃/min, be incubated 20 minutes, then give mould pressurizing to 4MPa, pressurize and stopped heating are until naturally be cooled to release after the room temperature;
8, cracking: graphite jig is put into pyrolyzer, be evacuated to less than 1kPa, then the temperature rise rate with 10 ℃/min rises to 1100 ℃, behind the insulation 60min, naturally is cooled to room temperature;
9, band mould impregnation drying cracking: the silicon carbide fiber precast body is no less than the cracking of 3 band mould impregnation dryings, and the process with the mould infiltration pyrolysis is at every turn: repeating step 5, step 6 and step 8;
10, go the cracking of mould impregnation drying: the silicon carbide fiber precast body is taken out from graphite jig, be no less than 10 times and go the cracking of mould impregnation drying, go the process of mould infiltration pyrolysis to be at every turn:
10.1, vacuum impregnation: the silicon carbide fiber precast body is put into vacuum impregnation equipment flood, vacuum pressure is not higher than 0.01MPa, and dipping time is 25h;
10.2, drying: after dipping is finished, the silicon carbide fiber precast body is taken out from vacuum impregnation equipment, place air, then at ambient temperature seasoning places baking oven with the silicon carbide fiber precast body, and oven dry is no less than 2h under 80 ℃ of temperature;
10.3, cracking: the silicon carbide fiber precast body is put into pyrolyzer, be evacuated to less than 1kPa, then the temperature rise rate with 10 ℃/min rises to 1100 ℃, the insulation 60min after, naturally be cooled to room temperature.

Claims (1)

1. the preparation method of a self-sealing silicon carbide ceramic based composite material is characterized in that, the step of preparation is as follows:
1.1, preparation silicon carbide fiber precast body: prepare the silicon carbide fiber precast body take continuous carbofrax fibre as starting material, its structure formation is: 2 dimension fiber layings, 2.5 dimension fibrages, 3 dimension fibrages or 3 dimension fiber needled felts;
1.2, preparation precursor steeping fluid: take Polycarbosilane and trimethylamine groups borine polymkeric substance as solute, prepare the precursor steeping fluid take dimethylbenzene as solvent, the weight percent that solute accounts for the precursor steeping fluid is 45%~60%, and the weight percent that Polycarbosilane accounts for solute is 60%~85%;
1.3, preparation silicon carbide fiber preform interface layer: the silicon carbide fiber precast body is placed in the chemical vapor deposition stove, take propane as source of the gas, preparation silicon carbide fiber precast body RESEARCH OF PYROCARBON interfacial layer, depositing temperature: 1000 ℃, gas flow: 1.0L/min, furnace pressure :≤2KPa, depositing time: 4~6h; Prepared RESEARCH OF PYROCARBON interfacial layer thickness is 0.1~0.5 μ m;
1.4, typing: the silicon carbide fiber precast body placed in the graphite jig finalizes the design;
1.5, vacuum impregnation: graphite jig is put into vacuum impregnation equipment, the inner chamber of this vacuum impregnation equipment is communicated with the container that the precursor steeping fluid is housed by a pipeline with switch, switch on blinding off a line, inner chamber to vacuum impregnation equipment vacuumizes, until vacuum pressure is not higher than 0.01MPa, open the switch on the pipeline, the precursor steeping fluid is sucked in the encloses container by the pipeline with switch, flood graphite jig, switch on again blinding off a line, silicon carbide fiber precast body in the graphite jig is flooded, and dipping time is 10h~30h;
1.6, drying: after dipping is finished, graphite jig is taken out from vacuum impregnation equipment, place air, then at ambient temperature seasoning places baking oven with graphite jig, and oven dry is no less than 2h under 80 ℃~120 ℃ temperature;
1.7, hot moulding: graphite jig is put on the platform of thermocompressor, risen to 190 ℃~220 ℃ with the temperature rise rate of 10 ℃/min, be incubated 30 minutes, then give mould pressurizing to 3MPa~6MPa, pressurize and stopped heating are until naturally be cooled to release after the room temperature;
1.8, cracking: graphite jig is put into pyrolyzer, be evacuated to less than 1kPa, then the temperature rise rate with 10 ℃/min rises to 1050 ℃~1150 ℃, the insulation 30min~60min after, naturally be cooled to room temperature;
1.9, the cracking of band mould impregnation drying: the silicon carbide fiber precast body is no less than the cracking of 3 band mould impregnation dryings, and the process with the mould infiltration pyrolysis is at every turn: repeating step 1.5, step 1.6 and step 1.8;
1.10, go the cracking of mould impregnation drying: the silicon carbide fiber precast body is taken out from graphite jig, is no less than 10 times and goes the cracking of mould impregnation drying, go the process of mould infiltration pyrolysis to be at every turn:
1.10.1, vacuum impregnation: the silicon carbide fiber precast body is put into vacuum impregnation equipment flood, vacuum pressure is not higher than 0.01MPa, and dipping time is 10h~30h;
1.10.2, drying: the dipping finish after, the silicon carbide fiber precast body is taken out from vacuum impregnation equipment, place air, at ambient temperature seasoning, then the silicon carbide fiber precast body is placed baking oven, oven dry is no less than 2h under 80 ℃~120 ℃ temperature;
1.10.3, cracking: the silicon carbide fiber precast body is put into pyrolyzer, be evacuated to less than 1kPa, then the temperature rise rate with 10 ℃/min rises to 1050 ℃~1150 ℃, the insulation 30min~60min after, naturally be cooled to room temperature.
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CN110922191A (en) * 2019-12-20 2020-03-27 厦门大学 Silicon carbide polymer precursor ceramic defect healing method
CN112125679A (en) * 2020-09-17 2020-12-25 中航复合材料有限责任公司 Method for preparing omega-shaped stringer based on precursor impregnation cracking process
CN112125673A (en) * 2020-09-17 2020-12-25 中航复合材料有限责任公司 Method for preparing right-angle stringer based on precursor impregnation cracking process
CN113004044A (en) * 2019-12-20 2021-06-22 中核北方核燃料元件有限公司 SiC added with graphenefPreparation method of/SiC composite material
CN114113246A (en) * 2021-11-26 2022-03-01 航天特种材料及工艺技术研究所 Dielectric property test sample of polysilazane cracking product and preparation method and test method thereof
CN115180983A (en) * 2022-08-01 2022-10-14 航天特种材料及工艺技术研究所 High-entropy ceramic modification method of ceramic matrix composite and high-entropy modified composite prepared by same
CN115611649A (en) * 2022-08-11 2023-01-17 北京航空航天大学 Silicon carbide ceramic matrix composite material and preparation method and application thereof
CN115724675A (en) * 2022-11-16 2023-03-03 航天特种材料及工艺技术研究所 Impregnation-curing treatment method of polysilazane, composite material and preparation method thereof
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