CN108585907A - A kind of Cr2The self-sealing silicon carbide ceramic based composite material and preparation method thereof that AlC is modified - Google Patents

A kind of Cr2The self-sealing silicon carbide ceramic based composite material and preparation method thereof that AlC is modified Download PDF

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CN108585907A
CN108585907A CN201810413978.9A CN201810413978A CN108585907A CN 108585907 A CN108585907 A CN 108585907A CN 201810413978 A CN201810413978 A CN 201810413978A CN 108585907 A CN108585907 A CN 108585907A
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silicon carbide
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周怡然
焦健
刘虎
杨金华
姜卓钰
吕晓旭
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AECC Beijing Institute of Aeronautical Materials
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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Abstract

The invention belongs to ceramic matric composite preparing technical fields, and in particular to a kind of Cr2The self-sealing silicon carbide ceramic based composite material and preparation method thereof that AlC is modified.By Cr2AlC particles are mixed into the matrix slurry for preparing ceramic matric composite, after being prepared into prepreg with fiber, by hot pressing, charing, melting silicon infiltration up to Cr2The self-sealing silicon carbide ceramic based composite material that AlC is modified.Under hot environment, when crack propagation to self-healing phase Cr2At AlC particles, Cr2AlC, which can be aoxidized, generates glass phase packing hole and crackle, the further diffusion of the surrounding mediums such as blocking oxygen, the effect of to play self-healing.In addition, the unique layer structures of Cr2AlC itself are conducive to increase the toughness of matrices of composite material.

Description

A kind of Cr2The self-sealing silicon carbide ceramic based composite material and its preparation that AlC is modified Method
Technical field
The invention belongs to ceramic matric composite preparing technical fields, and in particular to a kind of Cr2The self-healing carbon that AlC is modified SiClx ceramic matric composite and preparation method thereof.
Background technology
As novel high thrust-weight ratio aero-engine high-temperature structural material, ceramic matric composite is overcoming ceramic material While brittleness, also there are the feature performance benefits such as specific strength height, high temperature resistant.Due to the shadow by factors such as moulding process and internal structures It rings, ceramic matric composite is inevitably present the faults of construction such as hole and micro-crack, these defects can be the rings such as oxygen Border medium provides transmission channel, at high temperature so that material internal suffers erosion, to seriously affect the service life of material.Cause This, studies the ceramic matric composite with self-healing capability and is of great significance.
Self-healing ceramic matric composite is a kind of high-tech composite material to be got up based on bionics concept development, its energy Enough crackles (or in the case where imposing environmental stimuli) invisible caused by the external world are repaired automatically, and crackle is made to be cured substantially It closes, to achieve the purpose that performance can continue to, a kind of new method is provided for prevention is potentially hazardous.
In recent years, (ternary transition metal compound, wherein M are transition metal element to MAX phase ceramics；A is major element；X For C or N) determine that it takes into account the excellent specific property of metal and ceramic material and by extensive due to its own unique structure Concern.Some researches show that MAX phase ceramics, and significant self-healing capability can be shown under high-temperature oxygen atmosphere, most common to have Ti3AlC2、Ti2AlC and Cr2AlC, self-healing mechanism are all by generating firm glass phase α-Al in crack surfaces2O3, from And the further diffusion of oxide isolation is prevented, to achieve the purpose that the self-healing of material, prolong the service life.And for Ti-Al- The MAX phases of C ternary systems generate α-Al after oxidation2O3While will additionally generate the porous TiO for easily causing matrix defect2, instead Material mechanical performance is restricted to improve.Cr2AlC is as novel self-healing MAX phases in recent years, at high temperature prior to crack surfaces Generate fine and close oxidation product α-Al2O3, it is conducive to the healing of crackle in ceramic matrix, still, since the ceramic hardness is low and is used for Judge its can temperature limit ductile-brittle transition temperature (BDTT)≤1050 DEG C, therefore be not particularly suited for as thermal structure material Material is used alone.
The document overwhelming majority for being related to high temperature self-healing ceramics both at home and abroad is to utilize existing boron-containing compound in matrix It is oxidized to glassy state mobile phase packing matrix cracking at high temperature, barrier is provided to material internal diffusion for oxygen, it is final to send out Wave self-healing function.But some researches show that more than 1100 DEG C oxidation product B2O3It will largely volatilize so that self-healing is mutually broken It is bad.
Invention content
The present invention is for insufficient a kind of Cr of proposition in the prior art2The self-sealing silicon carbide ceramic base that AlC is modified is compound Material and preparation method thereof.Technical solution of the invention includes the following steps：
Step 1：By Cr2AlC powders, graphite powder and phenolic resin are added in ethyl alcohol, ball milling 12h~be uniformly mixed for 24 hours.Institute State phenolic resin: Cr2AlC powder: graphite powder: the quality parts ratio of ethyl alcohol is 30~80: 20~60: 10~50: 110~290.
Step 2：Silicon carbide fibre fabric containing interfacial TCO layer is impregnated in the slurry that step 1 obtains, it is pre- that fiber is made Leaching material.
Step 3：The prepreg that step 2 is obtained is clipped, hot-forming, is demoulded after cooling, obtains precast body.The heat It is 120 DEG C~300 DEG C to press temperature, and pressure is 1MPa~10MPa, and hot pressing time is 0.5h~3h.
Step 4：The precast body that step 3 is obtained cracks processing 6h~for 24 hours at 700 DEG C~900 DEG C, and it is porous that charcoal is made Body.
Step 5：It is cube that Si powder, which is cold-pressed at 10MPa~15MPa, is positioned under charcoal porous body, the Si powder with The mass ratio 1.5~6: 1 of charcoal porous body.In the case where temperature is 1400 DEG C~1500 DEG C, 10min~60min is kept the temperature, the anti-of Si is passed through Infiltration should be melted, Cr is obtained2The self-sealing silicon carbide ceramic based composite material that AlC is modified.
The Cr2The grain size of AlC powders is 1 μm~50 μm；The grain size of graphite powder powder is 1~5 μm.
Advantages of the present invention and advantageous effect are：The present invention is modified using MAX with respect to silicon carbide substrate, by Cr2AlC Self-healing feature apply in carbon/silicon carbide ceramic matrix composite.1. there is self-healing capability by being introduced in SiC matrix Cr2AlC particles form polynary self-healing system by self-healing constituent element together with the mutual disperse of SiC constituent elements.SiC matrix sheet Body have certain self-healing capability, and when surrounding medium by crack propagation to self-healing phase when, Cr2AlC and surrounding medium Effect generates glass phase Al2O3Packing crackle further stops that surrounding medium enters, to realize the material after healing 1500 Still there is excellent oxidation resistance under DEG C high temperature；②Cr2The coefficient of thermal expansion of AlC matches with SiC matrix material, the two It can be good at combining.Meanwhile the glass phase Al of generation2O3It is well combined with matrix, no peeling phenomenon so that multiple after self-healing The intensity of condensation material can restore the 75% of green strength；3. due to Cr2AlC has unique stratiform knot as MAX phases itself Structure, crackle, which will be diffused at bed boundary, to deflect, and on the one hand can effectively be weakened the stress concentration of crack tip, be played toughening On the other hand the effect of ceramic matric composite extends crackle approach, equally advantageous to extend the diffusion path of surrounding medium In the service life for improving composite material；4. the melting infiltration that the preparation of this novel self-healing ceramic matric composite uses (MI) technique, it is with short production cycle compared with PIP and CVI techniques, it is at low cost, it is conducive to engineering application.
Specific implementation mode
Illustrate Cr below in conjunction with specific example2The self-sealing silicon carbide ceramic based composite material and its preparation side that AlC is modified Method：
Embodiment 1：
Step 1：By 20gCr2AlC powders (5 μm), 50g graphite powders (1 μm) and 80g phenolic resin are added in 290g ethyl alcohol, Ball milling is uniformly mixed for 24 hours.
Step 2：Silicon carbide fibre fabric containing interfacial TCO layer is impregnated in the slurry that step 1 obtains, it is pre- that fiber is made Leaching material.
Step 3：The prepreg that step 2 is obtained is clipped, hot-forming, and wherein hot pressing temperature is 160 DEG C, pressure 3MPa, hot pressing time 3h demould after cooling, obtain precast body.
Step 4：The precast body that step 3 is obtained cracks processing 6h at 900 DEG C, and charcoal porous body is made.
Step 5：It is that (cubical size, the density etc. do not influence the step to cube that Si powder is cold-pressed at 10MPa Reaction process) be positioned under charcoal porous body, the quality of wherein Si powder is 2 times of charcoal porous body.It is protected at being 1500 DEG C in temperature Cr is obtained by the reaction with porous body using melt of si infiltration in warm 10min2The self-sealing silicon carbide ceramic based composite material that AlC is modified.
Embodiment 2：
Step 1：By 50gCr2150g ethyl alcohol is added in AlC powders (25 μm), 30g graphite powders (3 μm) and 60g phenolic resin In, ball milling 12h is uniformly mixed.
Step 2：Silicon carbide fibre fabric containing interfacial TCO layer is impregnated in the slurry that step 1 obtains, it is pre- that fiber is made Leaching material.
Step 3：The prepreg that step 2 is obtained is clipped, hot-forming, and wherein hot pressing temperature is 200 DEG C, pressure 5MPa, hot pressing time 2h demould after cooling, obtain precast body.
Step 4：The precast body that step 3 is obtained cracks processing 12h at 730 DEG C, and charcoal porous body is made.
Step 5：It is that (cubical size, the density etc. do not influence the step to cube that Si powder is cold-pressed at 12MPa Reaction process) be positioned under charcoal porous body, the quality of wherein Si powder is 2.6 times of charcoal porous body.In the case where temperature is 1480 DEG C 15min is kept the temperature, the self-sealing silicon carbide ceramic base composite wood of Cr2AlC modifications is obtained by the reaction with porous body using melt of si infiltration Material.
Embodiment 3：
Step 1：By 30gCr2150g ethyl alcohol is added in AlC powders (50 μm), 60g graphite powders (5 μm) and 40g phenolic resin In, ball milling 18h is uniformly mixed.
Step 2：Silicon carbide fibre fabric containing interfacial TCO layer is impregnated in the slurry that step 1 obtains, it is pre- that fiber is made Leaching material.
Step 3：The prepreg that step 2 is obtained is clipped, hot-forming, and wherein hot pressing temperature is 260 DEG C, pressure 8MPa, hot pressing time 1.5h demould after cooling, obtain precast body.
Step 4：For 24 hours, charcoal porous body is made in the precast body that step 3 is obtained cracking processing at 850 DEG C.
Step 5：It is that (cubical size, the density etc. do not influence the step to cube that Si powder is cold-pressed at 15MPa Reaction process) be positioned under charcoal porous body, the quality of wherein Si powder is 5.8 times of charcoal porous body.In the case where temperature is 1400 DEG C 60min is kept the temperature, Cr is obtained by the reaction with porous body using melt of si infiltration2The self-sealing silicon carbide ceramic base composite wood that AlC is modified Material.

Claims (2)

1. a kind of Cr2The self-sealing silicon carbide ceramic based composite material and preparation method thereof that AlC is modified, it is characterised in that following step Suddenly：
Step 1：By Cr2AlC powders, graphite powder and phenolic resin are added in ethyl alcohol, ball milling 12h~be uniformly mixed for 24 hours, the phenol Urea formaldehyde: Cr2AlC powder: graphite powder: the quality parts ratio of ethyl alcohol is 30~80: 20~60: 10~50: 110~290；
Step 2：Silicon carbide fibre fabric containing interfacial TCO layer is impregnated in the slurry that step 1 obtains, fiber prepreg material is made；
Step 3：The prepreg that step 2 is obtained is clipped, hot-forming, is demoulded after cooling, obtains precast body, the hot pressing temperature Degree is 120 DEG C~300 DEG C, and pressure is 1MPa~10MPa, and hot pressing time is 0.5h~3h；
Step 4：The precast body that step 3 is obtained cracks processing 6h~for 24 hours at 700 DEG C~900 DEG C, and charcoal porous body is made；
Step 5：It is cube that Si powder is cold-pressed at 10MPa~15MPa, is positioned under charcoal porous body, and the Si powder and charcoal are more The mass ratio of hole body is 1.5~6: 1, in the case where temperature is 1400 DEG C~1500 DEG C, keeps the temperature 10min~60min, passes through the reaction of Si Melting infiltration, obtains Cr2The self-sealing silicon carbide ceramic based composite material that AlC is modified.
2. a kind of Cr according to claim 12The preparation method for the self-sealing silicon carbide ceramic based composite material that AlC is modified, It is characterized in that：The Cr2The grain size of AlC powders is 1 μm~50 μm；The grain size of graphite powder powder is 1~5 μm.
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CN113943160A (en) * 2021-10-15 2022-01-18 中国航发北京航空材料研究院 Preparation method of silicon carbide ceramic matrix composite with self-repairing function
CN115286401A (en) * 2022-06-29 2022-11-04 武汉科技大学 Cr (chromium) 2 AlC combined silicon carbide refractory material and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113943160A (en) * 2021-10-15 2022-01-18 中国航发北京航空材料研究院 Preparation method of silicon carbide ceramic matrix composite with self-repairing function
CN113943160B (en) * 2021-10-15 2022-08-09 中国航发北京航空材料研究院 Preparation method of silicon carbide ceramic matrix composite with self-repairing function
CN115286401A (en) * 2022-06-29 2022-11-04 武汉科技大学 Cr (chromium) 2 AlC combined silicon carbide refractory material and preparation method thereof
CN115286401B (en) * 2022-06-29 2023-03-31 武汉科技大学 Cr (chromium) 2 AlC combined silicon carbide refractory material and preparation method thereof

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