CN110317073A - A kind of preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites - Google Patents
A kind of preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites Download PDFInfo
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Abstract
The present invention is a kind of preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites, micro/nano-scale reinforcement is mixed into precursor slurry prepares mixed slurry first by this method, and mixed slurry is brushed to the fiber surface containing boundary layer and obtains multistage fiber prepreg material, prepreg is cut, paving, hot pressing is for precast body, high-temperature process precast body obtains porous body, the porous body is then recycled to dipping in the precursor resin containing antioxidant composition, charing obtains half densification multistage toughening precast body, then densified using infiltration process, obtain the ceramic matric composite of multistage fiber coordination plasticizing, its anti-oxidant and toughness, which has, to be significantly improved.
Description
Technical field
The present invention is a kind of preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites, belongs to fiber increasing
The technology of preparing of tough ceramic matric composite.
Background technique
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 fiber interlayer and the brittle matrix of interfascicular as the second reinforcement, can pass through crack deflection
And the toughening mechanisms such as bridging, increase crack propagation distance, improves the brittleness of microcell matrix, the multiple dimensioned enhancing effect for improving reinforced phase
Fruit improves oxidation resistent susceptibility, mechanical property of ceramic matric composite etc., therefore nanometer reinforcement is also often applied to ceramic base
The performance of composite material optimizes.Micro/nano-scale reinforcement is introduced by matrix slurry using the method for ball milling mixing in the prior art
In, and using the methods of HIP sintering forming ceramic based composites, realize the toughened and reinforced effect of nanometer reinforcement；Together
When one layer of carbon of offer is provided on whisker surface, inhibit the chemical bonding of whisker and ceramic composite, further increase and receive
The toughened and reinforced effect of rice reinforcement.
Simultaneously in order to improve the anti-oxidant of ceramic matric composite, hinder oxidation component by being formed during applied at elevated temperature
The channels such as crackle, hole fiber is damaged, pass through in the research of part and introduce SiBCN, boron in ceramic matric composite
Powder etc. forms B, N component in SiC matrix in the high temperature environment, and fine and close oxidation film is formed in composite material surface, inhibits oxygen
Impervious and oxidation reaction improve the high-temperature oxidation resistant energy of ceramic matric composite.
Summary of the invention:
The invention proposes a kind of preparation methods of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites, by drawing
Enter the toughness that multistage reinforcement improves ceramic matric composite, and improves ceramic matric composite by introducing antioxidant composition
It is anti-oxidant, the protection to nanometer reinforcement is introduced is realized by the design of technical process, and realize by different dipping process
The introducing of one or more antioxidant compositions realizes quick densifying finally by infiltration process.
The purpose of the present invention is what is realized by following technological approaches:
The step of preparation method of this kind multistage fiber coordination plasticizing oxidation-resistant ceramic based composites, is as follows:
Step 1: preparing mixed slurry
High carbon residue resin, micro/nano-scale reinforcement and dehydrated alcohol are uniformly mixed according to 5~10: 1: 10~20 mass ratio
Close, using ultrasound+churned mechanically method it is uniform after obtain mixed slurry, 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: the preparation of prepreg
After the mixed slurry prepared in step 1 is introduced into completion step 2 by wet process prepreg preparation process
In continuous-filament woven fabric, prepreg is obtained；
Step 4: the preparation of multistage fiber coordination plasticizing precast body
Prepreg in step 3 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 the precast body of multistage fiber coordination plasticizing is obtained after pressure maintaining；
Step 5: the preparation of multistage fiber coordination plasticizing porous body
The precast body for the multistage fiber coordination plasticizing that step 4 obtains is put into high temperature furnace and is heated to 1000 DEG C or more, is obtained
To multistage fiber coordination plasticizing porous body；
Step 6: precursor resin impregnates
Multistage fiber coordination plasticizing porous body is put into vacuum impregnation case, using vacuum pump to being vacuumized in dipping box,
Precursor resin is then injected into dipping box, after multistage fiber coordination plasticizing porous body is totally submerged by precursor solution, leaching
Steep 3~5h；
1000 DEG C or more are heated to Step 7: the multistage fiber coordination plasticizing porous body after immersion is put into high temperature furnace,
Obtain the multistage fiber coordination plasticizing porous body of initial densification；
Step 8: infiltration densifies
The multistage fiber coordination plasticizing porous body of initial densification is put into graphite crucible, by the way of melting siliconising
Multistage fiber coordination plasticizing oxidation-resistant ceramic based composites are prepared.
In a kind of implementation, ultrasound described in step 1+churned mechanically incorporation time 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, introducing described in step 3 is using the method repeatedly brushed, then by prepreg in room
5~30h is dried under temperature.
In a kind of implementation, the fiber for forming continuous-filament woven fabric is carbon fiber or silicon carbide fibre.
In a kind of implementation, the high carbon residue resin is one of phenolic resin, furane resins or polyimide resin
Or several mixture.
In a kind of implementation, the micro/nano-scale reinforcement is nanometer silicon carbide fiber, nanometer silicon carbide whiskers, is chopped
The mixture of one or more of carbon fiber.
In a kind of implementation, the precursor resin is Si-B-C-N precursor, one or two kinds of in boron nitride precursor body
Mixture.
In a kind of implementation, before carrying out step 8, the operation Step 6: step 7 is repeated.
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 disperses nanometer reinforcement in high carbon residue resin, prepares mixed slurry, and use mixed slurry
Prepreg is prepared, high carbon residue resin employed in this method facilitates the dispersion of nanometer reinforcement, and enhances body surface in nanometer
Face forms resin package, forms pyrolytic carbon layer after charing, is conducive to the toughening effect for improving nanometer reinforcement；
2, the present invention is by introducing precursor dipping in the porous body after hot pressing charing, in the pyrolytic carbon of nanometer reinforcement
Layer surface re-forms anti-oxidant base, forms the protection to multistage reinforcement, and anti-oxidant base cracks to form self-healing after high temperature
Phase improves the anti-oxidant of ceramic matric composite；
3, the present invention can be introduced by the method for precursor infiltration and pyrolysis after hot pressing charing by different step respectively
One or more precursor components can effectively control every kind of component and introduce content；
4, densification process last in the present invention reduces the porosity of final molding material using melting siliconizing treatment processes,
Effectively improve efficiency of densification.
Specific embodiment
Embodiment 1
The step of preparation method of this kind multistage fiber coordination plasticizing oxidation-resistant ceramic based composites, is as follows:
Step 1: by phenolic resin, silicon carbide whisker and dehydrated alcohol according to 5:1:15 mass fraction than uniformly mixing, and
It mixes 2 hours using ultrasound+churned mechanically mode and obtains slurry, for use；
Step 2: a combination thereof mode is pyrolytic carbon (PyC)/boron nitride (BN)/carbon in continuous fiber surface deposited interfacial layer
The compound interface layer of SiClx (SiC), the wherein interface pyrolytic carbon (PyC) thickness about 100nm, wherein the interface boron nitride (BN) is thick
Degree is in 400nm, and wherein the interface silicon carbide (SiC) thickness is in 500nm；
Step 3: will be introduced into the fiber prepared in step 2 with the slurry got ready by wet method preparation process, prepare
Prepreg.It needs strict control to introduce the amount of slurry in brushing process, using the method repeatedly brushed, guarantees slurry in prepreg
The uniformity of distribution, then dries 12h for prepreg at room temperature, obtains multistage fiber prepreg material；
Step 4: the multistage fiber prepreg material prepared in step 3 is cut according to target size, paving；And it is paving is good
Prepreg be placed in it is hot-forming in heat pressing and molding mold.Hot-forming temperature is 160 DEG C, and briquetting pressure is about 3MPa, is protected
Pressing the time is about 3h, and multistage fiber coordination plasticizing precast body is prepared into after pressure maintaining；
It is heat-treated to obtain multistage fiber Step 5: the resin base precast body prepared in step 4 is put into high temperature furnace high temperature
The porous body of coordination plasticizing, the maximum temperature of porous body preparation are 1000 DEG C.
Step 6: the porous body prepared in step 5 is put into vacuum impregnation case, using vacuum pump to being taken out in dipping box
Si-B-C-N precursor is then injected dipping box by vacuum, after precursor solution is totally submerged sample, impregnates 4h；
It is heat-treated to obtain porous body, porous system Step 7: the sample after step 6 is impregnated is put into high temperature furnace high temperature
Standby maximum temperature is about 1200 DEG C.
Step 8: repeating Step 6: 71 times, initial densification is carried out to prepared sample；
It is put into graphite crucible Step 9: step 8 is prepared resulting half densification sample, using the side of melting siliconising
Formula obtains the oxidation-resistant ceramic based composites of multistage fiber coordination plasticizing, and high-temperature fusion siliconizing treatment processes temperature is about 1460 DEG C.
The oxidation-resistant ceramic based composites of multistage fiber coordination plasticizing, preparation can be effectivelyed prepared out by above-mentioned technique
Efficiency is apparently higher than first body impregnating cracking technology, and density of material is up to 2.7g/cm3, bending strength, tensile strength, fracture
Toughness and inoxidizability significantly improve.
Embodiment 2
The step of preparation method of this kind multistage fiber coordination plasticizing oxidation-resistant ceramic based composites, is as follows:
Step 1: by furane resins, silicon carbide whisker and dehydrated alcohol according to 10:1:20 mass fraction than uniformly mixing,
And mix 5 hours using ultrasound+churned mechanically mode and obtain slurry, for use；
Step 2: in continuous fiber surface deposited interfacial layer, a combination thereof mode include pyrolytic carbon (PyC)/boron nitride (BN)/
The combination of the compound interfaces layers such as silicon carbide (SiC)/pyrolytic carbon (PyC), single layer interfacial layer thickness is about 300nm, boundary layer overall thickness
About 1.2 μm；
Step 3: by wet process prepreg preparation process the fiber prepared in step 2 will be introduced into the slurry got ready
In, prepare prepreg.It needs strict control to introduce the amount of slurry in brushing process, using the method repeatedly brushed, guarantees preimpregnation
The uniformity that slurry is distributed in material, then dries 20h for prepreg at room temperature, obtains multistage fiber prepreg material；
Step 4: the multistage fiber prepreg material prepared in step 3 is cut according to target size, paving；And it is paving is good
Prepreg be placed in it is hot-forming in heat pressing and molding mold.Hot-forming temperature is 200 DEG C, and briquetting pressure is about 3MPa, is protected
Pressing the time is about 3h, and the precast body of multistage fiber coordination plasticizing is prepared into after pressure maintaining；
It is heat-treated to obtain multistage fiber Step 5: the resin base precast body prepared in step 4 is put into high temperature furnace high temperature
The porous body of coordination plasticizing, the maximum temperature of porous body preparation are 1000 DEG C.
Step 6: the porous body prepared in step 5 is put into vacuum impregnation case, using vacuum pump to being taken out in dipping box
Boron nitride precursor body is then injected dipping box by vacuum, after precursor solution is totally submerged sample, impregnates 5h；
Step 7: the sample after step 6 is impregnated is put into high temperature furnace and carbonizes, it is put into high temperature furnace high temperature and is heat-treated
To porous body；The maximum temperature of porous body preparation is about 1200 DEG C.
Step 8: repeating Step 6: 72 times, initial densification is carried out to prepared sample；
It is put into graphite crucible Step 9: step 8 is prepared resulting half densification sample, using high-temperature fusion siliconising
Mode obtain the oxidation-resistant ceramic based composites of multistage fiber coordination plasticizing, high-temperature fusion siliconizing treatment processes temperature is about 1460
℃。
Claims (10)
1. a kind of preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites, it is characterised in that: this method
Steps are as follows:
Step 1: preparing mixed slurry
High carbon residue resin, micro/nano-scale reinforcement and dehydrated alcohol are uniformly mixed according to 5~10: 1: 10~20 mass ratio,
Using ultrasound+churned mechanically method it is uniform after obtain mixed 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: the preparation of prepreg
By wet process prepreg preparation process by the mixed slurry prepared in step 1 be introduced into complete step 2 after it is continuous
In fabric, prepreg is obtained；
Step 4: the preparation of multistage fiber coordination plasticizing precast body
Prepreg in step 3 is placed in heat pressing and molding mold and is formed, hot-forming temperature is 150~400 DEG C, molding
Pressure is about 1~5MPa, and the dwell time is about 1~5h, and the precast body of multistage fiber coordination plasticizing is obtained after pressure maintaining；
Step 5: the preparation of multistage fiber coordination plasticizing porous body
The precast body for the multistage fiber coordination plasticizing that step 4 obtains is put into high temperature furnace and is heated to 1000 DEG C or more, is obtained more
Grade fiber coordination plasticizing porous body；
Step 6: precursor resin impregnates
Multistage fiber coordination plasticizing porous body is put into vacuum impregnation case, using vacuum pump to being vacuumized in dipping box, then
Precursor resin is injected into dipping box, after multistage fiber coordination plasticizing porous body is totally submerged by precursor solution, immersion 3~
5h；
1000 DEG C or more are heated to Step 7: the multistage fiber coordination plasticizing porous body after immersion is put into high temperature furnace, is obtained
The multistage fiber coordination plasticizing porous body of initial densification；
Step 8: infiltration densifies
The multistage fiber coordination plasticizing porous body of initial densification is put into graphite crucible, is prepared by the way of melting siliconising
Obtain multistage fiber coordination plasticizing oxidation-resistant ceramic based composites.
2. the preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites according to claim 1, special
Sign is: ultrasound described in step 1+churned mechanically incorporation time is 1~5 hour.
3. the preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites according to claim 1, special
Sign is: single layer interfacial layer thickness described in step 2 is 100~500nm, and boundary layer overall thickness is about 1~2 μm.
4. the preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites according to claim 1, special
Sign is: introducing described in step 3 is that prepreg is then dried 5~30h at room temperature using the method repeatedly brushed.
5. the preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites according to claim 1, special
Sign is: the fiber for forming continuous-filament woven fabric is carbon fiber or silicon carbide fibre.
6. the preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites according to claim 1, special
Sign is: the high carbon residue resin is the mixture of one or more of phenolic resin, furane resins or polyimide resin.
7. the preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites according to claim 1, special
Sign is: the micro/nano-scale reinforcement is one of nanometer silicon carbide fiber, nanometer silicon carbide whiskers, chopped carbon fiber
Or several mixture.
8. the preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites according to claim 1, special
Sign is: the precursor resin is Si-B-C-N precursor, mixture one or two kinds of in boron nitride precursor body.
9. the preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites according to claim 1, special
Sign is: before carrying out step 8, repeating the operation Step 6: step 7.
10. the preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites according to claim 1, special
Sign is: the technological temperature for melting siliconising is 1400~1800 DEG C.
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| CN111393178A (en) * | 2020-02-27 | 2020-07-10 | 哈尔滨工业大学 | SiCfPreparation method of @ BN core-shell structure chopped fiber |
| CN111892405A (en) * | 2020-07-08 | 2020-11-06 | 中国航发北京航空材料研究院 | Preparation method for preparing ceramic matrix composite material by interface-layer-free process |
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