CN110357648A - A method of preparing multistage multiple dimensioned fiber reinforced ceramic matric composite - Google Patents

A method of preparing multistage multiple dimensioned fiber reinforced ceramic matric composite Download PDF

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CN110357648A
CN110357648A CN201910618383.1A CN201910618383A CN110357648A CN 110357648 A CN110357648 A CN 110357648A CN 201910618383 A CN201910618383 A CN 201910618383A CN 110357648 A CN110357648 A CN 110357648A
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multiple dimensioned
multistage
fiber reinforced
fiber
matric composite
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姜卓钰
焦健
杨金华
周怡然
吕晓旭
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AECC Beijing Institute of Aeronautical Materials
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AECC Beijing Institute of Aeronautical Materials
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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Abstract

The present invention is a kind of method for preparing multistage multiple dimensioned fiber reinforced ceramic matric composite, in this method, first in fiber surface deposited interfacial layer, and nanometer reinforcement is prepared in the fiber surface with interfacial TCO layer, obtain multistage multiple dimensioned fiber, mixed solution is prepared simultaneously as slurry, and slurry is introduced into multistage multiple dimensioned fiber by wet process preimpregnation preparation method for material and obtains prepreg；By prepreg cutting, paving, hot-forming obtain precast body；Precast body high temperature carbonization is obtained into porous body, melting siliconising is finally carried out using silicon powder embedding porous body, obtains multistage multiple dimensioned fiber reinforced ceramic matric composite；The density of the multiple dimensioned fiber reinforced ceramic matric composite of multistage prepared using the above method is up to 2.7g/cm3, within 5%, bending strength and fracture toughness have to be significantly improved controlled porosity.

Description

A method of preparing multistage multiple dimensioned fiber reinforced ceramic matric composite
Technical field
The present invention is a kind of method for preparing multistage multiple dimensioned fiber reinforced ceramic matric composite, belongs to fiber reinforced pottery The preparation technical field of porcelain based composites.
Background technique
Ceramic matric composite refers to that dispersed phase is introduced in ceramic matrix forms reinforcement, and ceramic matrix is continuous phase Composite material, the heat resistance having had, density is low, insensitive to crackle, catastrophic failure will not occur, therefore sending out Have in the engine thermals end pieces such as motivation blade, machine lock, the high low pressure turbine disk, flameholder and ejector exhaust pipe important Using effectively improving the working efficiency of engine.
Continuous Fiber Reinforced Ceramic Matrix Composites, hole and crackle during applied at elevated temperature due to being formed in matrix The defects of, cause material fragility big, damage toughness is insufficient, and fatigue life is short, it is difficult to meet next-generation engine material fatigability The demand of energy.Therefore research attempts using the technological approaches such as nanofiber multistage toughening at this stage, exploitation is more resistant to high temperature, higher The ceramic matric composite of damage tolerance.
Nanofiber is introduced into material matrix as the second reinforcement, can pass through the toughenings machine such as crack deflection and bridging System, the multiple dimensioned toughening effect for improving reinforced phase, improves oxidation resistent susceptibility, mechanical property of ceramic matric composite etc..
In recent years, related research institutes both domestic and external prepared the ceramic base of unidirectional reinforcement toughening in prepreg infiltration process Major progress is achieved in terms of composite material, using the ceramic matric composite and component of technique preparation have reached it is higher at Ripe degree, GE company, the U.S. has been examined by application layer using the ceramic base composite material member of technique preparation, therefore is developed pre- The process of the multistage multiple dimensioned fiber reinforced ceramic matric composite of leaching material infiltration process preparation will have great importance.
Summary of the invention
The present invention is exactly directed to next-generation engine for the demand of ceramic matric composite more high fatigue property, proposes A kind of method of the multistage multiple dimensioned fiber reinforced ceramic matric composite of prepreg infiltration process preparation, i.e., introduce on fiber and receive Meter level reinforcement prepares multistage multiple dimensioned fiber, then prepares multistage multiple dimensioned fiber using prepreg-infiltration process and increases Tough ceramic matric composite develops the ceramic matric composite more resistant to high temperature, more high damage tolerance.
The purpose of the present invention is what is realized by following technological approaches:
It is as follows that this kind prepares the step of method of multistage multiple dimensioned fiber reinforced ceramic matric composite:
Step 1: the preparation of precursor slurry
Silicon carbide powder, phenolic resin, silicon powder are uniformly mixed with ethyl alcohol according to 1: 1~3: 1~3: 5~10 mass ratioes, Precursor slurry is obtained after ball milling, for use；
Step 2: preparing boundary layer on continuous-filament woven fabric surface
The type of boundary layer is the compound of one or more of pyrolytic carbon (PyC), boron nitride (BN) or silicon carbide (SiC) Boundary layer；
Step 3: preparing multistage multi-scale reinforcing body on continuous-filament woven fabric surface
Step 4: the preparation of multistage multiple dimensioned fiber prepreg material
After the precursor slurry prepared in step 1 is introduced into completion step 3 by wet process prepreg preparation process Continuous-filament woven fabric in, obtain multistage multiple dimensioned fiber prepreg material；
Step 5: the preparation of multistage multiple dimensioned fiber reinforced precast body
The multiple dimensioned fiber prepreg material of multistage in step 4 is placed in heat pressing and molding mold and is formed, hot-forming temperature It is 150~400 DEG C, briquetting pressure is about 1~5MPa, and the dwell time is about 1~5h, and multistage multiple dimensioned fibre is obtained after pressure maintaining Tie up toughening precast body；
Step 6: the preparation of multistage multiple dimensioned fiber reinforcement porous body
The multiple dimensioned fiber reinforced precast body of multistage that step 5 obtains is put into high temperature furnace and is heated to 1200 DEG C, is obtained more The multiple dimensioned fiber reinforcement porous body of grade；
Step 7: the preparation of multistage multiple dimensioned fiber reinforced ceramic matric composite
The multiple dimensioned fiber reinforcement porous body of multistage prepared in step 6 is put into graphite crucible, is seeped using high-temperature fusion The mode of silicon obtains multistage multiple dimensioned fiber reinforced ceramic matric composite.
In a kind of implementation, the Ball-milling Time in step 1 is 1~5 hour.
In a kind of implementation, single layer interfacial layer thickness described in step 2 is 100~500nm, and boundary layer overall thickness is about 1 ~2 μm.
In a kind of implementation, the fiber is silicon carbide fibre or carbon fiber, and the continuous-filament woven fabric is that two dimension is fine Tie up fabric or unidirectional narrow fabrics.
In a kind of implementation, in the method for the multistage multi-scale reinforcing body of continuous-filament woven fabric surface preparation described in step 3 For growth in situ nanometer silicon carbide fiber, introduces nanometer silicon carbide fiber or introduce nanometer silicon carbide whiskers.
Further, the growth in situ nanometer silicon carbide fiber is with Si powder, SiO2Powder, C are raw material, using gas phase in situ Reaction method grows nano SiC fiber in continuous fiber surface, and the reaction temperature for preparing nano SiC fiber is 1400 DEG C -1500 DEG C.
Further, the introducing nanometer silicon carbide fiber or introducing nanometer silicon carbide whiskers are to add it to dehydrated alcohol In the mixed solution of polyethylene glycol, the mass ratio of dehydrated alcohol and polyethylene glycol is 20: 1~5, using the method for ultrasonic vibration Disperse 1~5h, use glass to stir during ultrasonic disperse, completes the screen filtration for using 100~500 mesh after dispersing, obtain To nanometer silicon carbide fiber or nanometer silicon carbide whiskers mixed solution, mixed solution is then brushed into continuous-filament woven fabric surface On, it dries.
In a kind of implementation, introducing described in step 4 is using the method repeatedly brushed, then by prepreg in room 10~30h is dried under temperature.
In a kind of implementation, hot-forming mode described in step 5 is that hot press is pressed and molded, autoclave is hot pressed into Type or vacuum bag are hot-forming.
In a kind of implementation, the technological temperature for melting siliconising is 1400~1800 DEG C.
The advantages of technical solution of the present invention and feature are as follows:
1. the present invention prepares multistage multiple dimensioned fibre by preparing nanometer silicon carbide reinforcement on continuous-filament woven fabric surface Dimension, and using the multistage multiple dimensioned fiber reinforced ceramic matric composite of prepreg infiltration process preparation, process cycle is shorter, controllably Property it is higher, in engineer application have apparent advantage；
2. the present invention improves nano silicon carbide by growing or introducing nanometer reinforcement in continuous-filament woven fabric surface in situ The uniformity that silica fibre or whisker are distributed in multistage multiple dimensioned fiber reinforced ceramic matric composite, convenient for control nanometer enhancing The content of body has apparent advantage in implementation process；
3. dispersing nanometer silicon carbide reinforcement in organic solvent present invention introduces when nanometer reinforcement, avoiding and expecting Nanometer reinforcement is caused to damage due to factors such as mechanical ball mills in slurry mixing, also avoid nanofiber in slurry with solid The tangled up and knotted of particle utmostly plays the toughening effect of nanofiber, thus also with apparent excellent on toughening effect Gesture；
Specific embodiment
Embodiment 1
It is as follows that this kind prepares the step of method of multistage multiple dimensioned fiber reinforced ceramic matric composite:
Step 1: silicon carbide powder, phenolic resin, silicon powder than are uniformly mixed with ethyl alcohol according to 1:3:1:5 mass fraction, Obtain slurry within ball milling 5 hours, for use；
Step 2: being deposited as continuous fiber reinforcement in silicon carbide fibre fabric surface using silicon carbide fibre fabric BN/SiC/PyC boundary layer, single layer interfacial layer thickness are about 400nm；
Step 3: with Si powder and SiO2Powder is raw material, using in continuous SiC fiber fabric surface growth in situ nano SiC Multistage multiple dimensioned fiber is prepared in fiber, and the reaction temperature that gas phase reaction in situ prepares nano SiC fiber is 1450 DEG C；
Step 4: by wet process prepreg preparation process by slurry provisioned in step 1 uniformly brushes arrive step 3 it is made On the standby multiple dimensioned fiber of multistage.It needs strict control to introduce the amount of slurry in dipping process, using the method repeatedly brushed, protects Demonstrate,prove the uniformity of slurry distribution in prepreg；Then by prepreg naturally dry 12h, multistage multiple dimensioned SiC fiber prepreg is obtained Material；
Step 5: the multiple dimensioned SiC fiber prepreg material of multistage prepared in step 4 is cut, paving；And it is paving is good Prepreg is placed in compression molding die and is pressed and molded.Forming temperature is 300 DEG C, and briquetting pressure is about 5MPa, dwell time About 3h obtains multistage multiple dimensioned fiber reinforced precast body；
It is obtained Step 6: the multiple dimensioned fiber reinforced precast body of multistage prepared in step 5 is put into heat treatment in high temperature furnace The porous body of multistage multiple dimensioned silicon carbide fibre enhancing, the preparation temperature of porous body is about 1200 DEG C；
Step 7: the porous body prepared in step 6 is put into graphite crucible, obtained by the way of high-temperature fusion siliconising To the ceramic matric composite of multistage multiple dimensioned toughening, melting siliconising preparation temperature is about 1500 DEG C.After the technique, obtain The fine and close multiple dimensioned fiber reinforced ceramic matric composite of multistage.
After the technique, the fine and close multiple dimensioned fiber reinforced ceramic matric composite of multistage is obtained, density is reachable 2.7g/cm3, within 5%, the fracture toughness and fracture elongation of composite material have to be significantly improved controlled porosity.
Embodiment 2
It is as follows that this kind prepares the step of method of multistage multiple dimensioned fiber reinforced ceramic matric composite:
Step 1: silicon carbide powder, phenolic resin, silicon powder and ethyl alcohol is more mixed than uniformly according to 1:2:1.5:7 mass fraction It closes, and ball milling 5 hours obtain slurry, for use；
Step 2: being deposited as continuous fiber reinforcement in silicon carbide fibre fabric surface using silicon carbide fibre fabric PyC/SiC/PyC boundary layer, single layer interfacial layer thickness are about 500nm；
Step 3: the mixed solution of dehydrated alcohol and polyethylene glycol is prepared than the ratio for 20:1 according to mass fraction, and Nano SiC fiber is added in mixed solution, 2h is dispersed using ultrasonic vibration+churned mechanically method, obtains nano silicon carbide Silica fibre mixed solution；
Step 4: mixed solution obtained by step 3 is evenly coated in continuous carbofrax fibre fabric surface, and by silicon carbide Fabric dries, and multistage multiple dimensioned silicon carbide fibre is obtained after solvent volatilizees completely；
Step 5: precursor slurry provisioned in step 1 is homogeneously introduced to step by wet process prepreg preparation process On the multiple dimensioned silicon carbide fibre of multistage prepared by four.Strict control is needed to introduce the amount of slurry in dipping process, using multiple The method of brushing guarantees the uniformity of slurry distribution in prepreg；Then by prepreg naturally dry 12h, multistage more rulers are obtained Spend silicon carbide fibre prepreg；
Step 6: the multiple dimensioned silicon carbide fibre prepreg of multistage prepared in step 5 is cut, paving；And it is paving is good Prepreg be placed in heat pressing and molding mold, it is hot-forming using autoclave.Being pressed and molded temperature is 300 DEG C, briquetting pressure About 5MPa, dwell time are about 3h, obtain multistage multiple dimensioned toughening precast body.
It is heat-treated to obtain multistage more rulers Step 7: the resin base precast body prepared in step 6 is put into high temperature furnace high temperature Silicon carbide fibre toughening porous body is spent, the preparation temperature of porous body is about 1200 DEG C.
Step 8: the porous body prepared in step 7 is put into graphite crucible, obtained by the way of high-temperature fusion siliconising To multistage multiple dimensioned fiber reinforced ceramic matric composite, melting siliconising preparation temperature is about 1500 DEG C.After the technique, Obtain the ceramic matric composite of the closely knit multiple dimensioned toughening of multistage.

Claims (10)

1. a kind of method for preparing multistage multiple dimensioned fiber reinforced ceramic matric composite, it is characterised in that: the step of this method It is as follows:
Step 1: the preparation of precursor slurry
Silicon carbide powder, phenolic resin, silicon powder are uniformly mixed with ethyl alcohol according to 1: 1~3: 1~3: 5~10 mass ratioes, ball milling After obtain precursor slurry, for use；
Step 2: preparing boundary layer on continuous-filament woven fabric surface
The type of boundary layer is the compound interface of one or more of pyrolytic carbon (PyC), boron nitride (BN) or silicon carbide (SiC) Layer；
Step 3: preparing multistage multi-scale reinforcing body on continuous-filament woven fabric surface
Step 4: the preparation of multistage multiple dimensioned fiber prepreg material
The precursor slurry prepared in step 1 is introduced into the company after completing step 3 by wet process prepreg preparation process In continuous fabric, multistage multiple dimensioned fiber prepreg material is obtained；
Step 5: the preparation of multistage multiple dimensioned fiber reinforced precast body
The multiple dimensioned fiber prepreg material of multistage in step 4 is placed in heat pressing and molding mold and is formed, hot-forming temperature is 150~400 DEG C, briquetting pressure is about 1~5MPa, and the dwell time is about 1~5h, and multistage multiple dimensioned fiber is obtained after pressure maintaining Toughening precast body；
Step 6: the preparation of multistage multiple dimensioned fiber reinforcement porous body
The multiple dimensioned fiber reinforced precast body of multistage that step 5 obtains is put into high temperature furnace and is heated to 1200 DEG C, it is more to obtain multistage Scale fiber reinforcement porous body；
Step 7: the preparation of multistage multiple dimensioned fiber reinforced ceramic matric composite
The multiple dimensioned fiber reinforcement porous body of multistage prepared in step 6 is put into graphite crucible, using high-temperature fusion siliconising Mode obtains multistage multiple dimensioned fiber reinforced ceramic matric composite.
2. the method for the multistage multiple dimensioned fiber reinforced ceramic matric composite of preparation according to claim 1, feature exist In: the Ball-milling Time in step 1 is 1~5 hour.
3. the method for the multistage multiple dimensioned fiber reinforced ceramic matric composite of preparation according to claim 1, feature exist In: single layer interfacial layer thickness described in step 2 is 100~500nm, and boundary layer overall thickness is about 1~2 μm.
4. the method for the multistage multiple dimensioned fiber reinforced ceramic matric composite of preparation according to claim 1, feature exist In: the fiber is silicon carbide fibre or carbon fiber, and the continuous-filament woven fabric is two-dimensional fiber fabric or unidirectional narrow fabrics.
5. the method for the multistage multiple dimensioned fiber reinforced ceramic matric composite of preparation according to claim 1, feature exist In: it in the method that continuous-filament woven fabric surface prepares multistage multi-scale reinforcing body is growth in situ nano silicon carbide described in step 3 Silica fibre introduces nanometer silicon carbide fiber or introduces nanometer silicon carbide whiskers.
6. the method for the multistage multiple dimensioned fiber reinforced ceramic matric composite of preparation according to claim 5, feature exist In: the growth in situ nanometer silicon carbide fiber is with Si powder, SiO2Powder, C are raw material, using gas-phase reaction method in situ continuous Fiber surface grows nano SiC fiber, and the reaction temperature for preparing nano SiC fiber is 1400 DEG C -1500 DEG C.
7. the method for the multistage multiple dimensioned fiber reinforced ceramic matric composite of preparation according to claim 5, feature exist In:
The introducing nanometer silicon carbide fiber or introducing nanometer silicon carbide whiskers are to add it to dehydrated alcohol and polyethylene glycol Mixed solution in, the mass ratio of dehydrated alcohol and polyethylene glycol is 20: 1~5,1~5h is dispersed using the method for ultrasonic vibration, It uses glass to stir during ultrasonic disperse, completes the screen filtration for using 100~500 mesh after dispersing, obtain nano silicon carbide Silica fibre or nanometer silicon carbide whiskers mixed solution, mixed solution is then brushed on continuous-filament woven fabric surface, dry.
8. the method for the multistage multiple dimensioned fiber reinforced ceramic matric composite of preparation according to claim 1, feature exist In: introducing described in step 4 is that prepreg is then dried 10~30h at room temperature using the method repeatedly brushed.
9. the method for the multistage multiple dimensioned fiber reinforced ceramic matric composite of preparation according to claim 1, feature exist In: hot-forming mode described in step 5 is hot press compression molding, autoclave is hot-forming or vacuum bag is hot-forming.
10. the method for the multistage multiple dimensioned fiber reinforced ceramic matric composite of preparation according to claim 1, feature exist In: the technological temperature for melting siliconising is 1400~1800 DEG C.
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Cited By (9)

* Cited by examiner, † Cited by third party
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CN111039687A (en) * 2019-12-13 2020-04-21 中国航空制造技术研究院 Damage-free hole making method for continuous fiber reinforced ceramic matrix composite
CN111170754A (en) * 2020-02-08 2020-05-19 西北工业大学 Composite material with Si-Y-C ternary ceramic matrix and preparation method thereof
CN111606715A (en) * 2020-05-14 2020-09-01 湖南太子新材料科技有限公司 Preparation method of silicon carbide fiber reinforced silicon carbide composite material
CN113061036A (en) * 2021-03-05 2021-07-02 华中科技大学 Carbon fiber-SiC whisker reinforced SiSiC composite material with complex structure and preparation method thereof
CN113307643A (en) * 2021-06-02 2021-08-27 中国航空制造技术研究院 SiC based on one-way beltfPreparation method of/SiC composite material
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CN111039687A (en) * 2019-12-13 2020-04-21 中国航空制造技术研究院 Damage-free hole making method for continuous fiber reinforced ceramic matrix composite
CN111170754A (en) * 2020-02-08 2020-05-19 西北工业大学 Composite material with Si-Y-C ternary ceramic matrix and preparation method thereof
CN111606715A (en) * 2020-05-14 2020-09-01 湖南太子新材料科技有限公司 Preparation method of silicon carbide fiber reinforced silicon carbide composite material
CN113061036A (en) * 2021-03-05 2021-07-02 华中科技大学 Carbon fiber-SiC whisker reinforced SiSiC composite material with complex structure and preparation method thereof
WO2022183527A1 (en) * 2021-03-05 2022-09-09 华中科技大学 Complex-structure carbon fiber-sic whisker-reinforced sisic composite material and preparation method therefor
CN113307643A (en) * 2021-06-02 2021-08-27 中国航空制造技术研究院 SiC based on one-way beltfPreparation method of/SiC composite material
CN113735604A (en) * 2021-09-29 2021-12-03 湖北瑞宇空天高新技术有限公司 Multilayer ceramic matrix composite for aeroengine thermal structural member and preparation method thereof
CN116354737A (en) * 2023-04-03 2023-06-30 合肥富维康新材料有限公司 Method for precisely controlling volume fraction of SiC fibers in MI-SiC/SiC composite material
CN116375487A (en) * 2023-04-03 2023-07-04 合肥富维康新材料有限公司 Preparation method of low-porosity SiC fiber unidirectional prepreg tape
CN116768642A (en) * 2023-08-17 2023-09-19 成都飞机工业（集团）有限责任公司 Preparation method of long spiral fiber toughened ceramic matrix composite

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Application publication date: 20191022