CN109467450A - One kind containing Ti3SiC2The SiC of boundary layerfThe preparation method of/SiC ceramic matrix composite material - Google Patents

One kind containing Ti3SiC2The SiC of boundary layerfThe preparation method of/SiC ceramic matrix composite material Download PDF

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CN109467450A
CN109467450A CN201811524818.8A CN201811524818A CN109467450A CN 109467450 A CN109467450 A CN 109467450A CN 201811524818 A CN201811524818 A CN 201811524818A CN 109467450 A CN109467450 A CN 109467450A
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sic
composite material
boundary layer
target
matrix composite
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CN109467450B (en
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黄小忠
王春齐
唐云
彭立华
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Hunan Zerui New Material Co., Ltd
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HUNAN BOOM NEW MATERIALS CO Ltd
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Abstract

The invention discloses one kind to contain Ti3SiC2The SiC of boundary layerfThe preparation method of/SiC ceramic matrix composite material carries out depositing Ti to SiC fiber braid using the method for magnetron sputtering3SiC2, obtain and contain Ti3SiC2Then the SiC fiber braid of boundary layer obtains SiC by resin impregnation carbonizationf/ C porous body, then SiC is obtained by gas phase siliconisingf/ SiC ceramic matrix composite material；The magnetron sputtering is first to carry out magnetron sputtering using TiC target, crosses coating in the TiC that SiC fibre bundle or SiC fiber braid surface obtain 0.1~0.2 μm, then obtains Ti using TiC target and Si target double target co-sputtering again3SiC2, the Ti3SiC2Thickness control be 0.6~1.0 μm；What the present invention initiated is obtained using the method for magnetron sputtering containing Ti3SiC2The SiC of boundary layerf/ SiC ceramic matrix composite material, effectively reduces depositing temperature, avoids the damage of fiber, gained boundary layer is in terms of antioxygenic property better than boundary layers such as the prior art common C, BN.The present invention carries out ceramic using contactless gas phase siliconising method simultaneously, effectively reduces density gradient, and can guarantee 100% qualification rate.

Description

One kind containing Ti3SiC2The SiC of boundary layerfThe preparation method of/SiC ceramic matrix composite material
Technical field
The present invention relates to ceramic matric composite fields, more particularly to one kind to contain Ti3SiC2The SiCf/SiC of boundary layer is compound The preparation method of material.
Background technique
Continuous carbofrax fibre enhances ceramic matric composite (SiCf/ SiC) it is to grow up this beginning of the century by weight Depending on a kind of high-temperature structural material, compared with other materials, it have low-density, high temperature resistant, anticorrosive, high-intensitive, high-modulus The advantages that, with the continuous improvement of technology of preparing, development is very rapid, is mainly used in hypersonic aircraft, aviation hair Motivation, fusion reactor and high temperature inhale numerous high-grade, precision and advanced fields such as wave.
In SiCfIn/SiC ceramic matrix composite material, boundary layer is the bridge that load is transmitted between knitted body fiber and basis material, It is the key factor of the excellent continuous SiC fiber enhancing composite material of processability.In SiCfIn/SiC ceramic matrix composite material, preferably Boundary layer mainly has the following aspects effect.(1) SiC fiber is protected, inhibits to cause fiber in composite material preparation process Damage.(2) bond strength between SiC fiber and SiC matrix is adjusted, so that SiCfFiber in/SiC ceramic matrix composite material fracture process The energy dissipation mechanisms such as extraction, crack deflection play a role, and enhance the toughness of composite material.
Most common SiCfBoundary layer in/SiC ceramic matrix composite material is pyrolytic carbon (Pyrolytic Carbon, PyC) With hexagonal boron nitride (Hexagonal-BN), but in use discovery, be oxidized easily, and then composite material is caused to irradiate It is insufficient with the military service stability under oxidation environment.
In recent years, one kind is with Ti3SiC2(M: transition is received significant attention for the ternary transition metal compound MAX phase of representative Race's metallic element；A: major element；X is C or N；N=1~3).The crystal structure of MAX phase is six side's layer structures, MX lamella It is alternately stacked on c-axis direction with A atomic layer, unique crystal structure imparts its special chemical bond feature, to make Obtain the excellent characteristics that this kind of ceramic materials have taken into account metal material and ceramic material, on the one hand, have good as metal Good thermally conductive/electrical property and thermal shock resistance excellent at high temperature and plasticity.On the other hand, the Gao Rong of ceramics has also been assembled The features such as point, high rigidity.Different from general carbide, machinability is conducive to high volume applications in engineering, this is allowed for MAX phase ceramics, which are gathered around, to have broad application prospects.It not only can be used alone, also have as activeness and quietness body in the composite Highly important influence.But it is there is no at present in fiber surface Ti3SiC2The relevant report of boundary layer.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of containing Ti3SiC2The SiC of boundary layerfThe system of/SiC ceramic matrix composite material Preparation Method.
It is of the invention a kind of containing Ti3SiC2The SiC of boundary layerfThe preparation method of/SiC ceramic matrix composite material includes the following steps: to adopt Depositing Ti is carried out to SiC fiber braid with the method for magnetron sputtering3SiC2, obtain and contain Ti3SiC2The SiC fiber of boundary layer is compiled Part is knitted, SiC is then obtained by resin impregnation carbonizationf/ C porous body, then SiC is obtained by gas phase siliconisingf/ SiC ceramic matrix composite material.
Preferred scheme, the method for the magnetron sputtering are double target magnetic control sputtering methods, and double targets are respectively TiC Target, Si target.
Preferred scheme, the magnetron sputtering is first to carry out magnetron sputtering using TiC target, in SiC fibre bundle or SiC fiber The TiC that braided part surface obtains 0.1~0.2 μm crosses coating, is then obtained again using TiC target and Si target double target co-sputtering Ti3SiC2, the Ti3SiC2Thickness control be 0.6~1.0 μm.
Inventors have found that first one layer of TiC of deposition is on the one hand more preferable to the covering property of SiC fiber, associativity, while can be complete Si gas is avoided to erode SiC fiber braid entirely.
Further preferred, TiC crosses the deposition process of coating are as follows: SiC fiber braid is placed in magnetron sputtering vacuum chamber In, first sputtered using TiC target, sputtering initial vacuum degree is 1~5 × 10-3Pa, the distance between target and fiber for 80~ 120mm, argon flow are 30~50sccm, and sputter temperature is room temperature, and sputtering power is 2200~2800W, deposition rate 10 ~20nm/min, sputtering time are 5~20mim.
It is further preferred, the Ti3SiC2Deposition process are as follows: use TiC target and Si target co-sputtering, it is true before sputtering Reciprocal of duty cycle is 1~5 × 10-3Pa, the distance between target and fiber are 80~120mm, argon flow is 30~50sccm, sputter temperature For room temperature, sputtering power is 1500~2000W, and deposition rate is 5~10nm/min, and sputtering time is 80~200mim.
Preferred scheme, the process of the resin impregnation carbonization are as follows: Ti will be contained3SiC2The SiC fiber braid of boundary layer is set In maceration extract, vacuum impregnation is carried out, after the completion of dipping, solidification, cracking repeat above-mentioned dipping-solidification-cracking process 3~5 Secondary, finally preparing density is 1.6~1.8g/cm3SiCf/ C porous materials, it includes such as that the maceration extract is counted in mass ratio Lower composition: resorcinol, formaldehyde, dehydrated alcohol are according to mass ratio (4~6): (8~10): (20~26).
Preferred scheme, the vacuum-impregnated vacuum degree≤0.001MPa, the vacuum-impregnated time are 1~3h.
Preferred scheme, the cured temperature are 160 DEG C~220 DEG C, and the cured time is 2~3h.
Preferred scheme, the temperature of the cracking are 800 DEG C~1000 DEG C, and the time of the cracking is 1~2h.
Preferred scheme, the process of the gas phase siliconising are as follows: by SiCf/ C porous materials are placed in the stone for being equipped with silicon powder In black mold, the SiCfIt is lined with graphite block body below/C porous materials, so that SiCf/ C porous materials and silicon powder be not direct Contact is warming up to 1900~2000 DEG C under vacuum conditions, keeps the temperature 30~60min, i.e. acquisition SiCf/ SiC ceramic matrix composite material.
Preferred scheme, the graphite block body are hollow graphite block.
Preferred scheme, the vacuum degree are 800~1200pa.
Preferred scheme, the heating rate are 5~20 DEG C/min.
In the present invention, silicon steam and SiC are obtained using contactless gas phase siliconising methodfC in/C porous materials is anti- Answer, form the silicon carbide substrate of dense uniform, during contactless, silicon powder in mold by siphonage with SiCfThe reaction of/C porous materials can obtain better siphon effect, institute during preferably using hollow graphite block State SiCfThe case where/SiC ceramic matrix composite material surface is clean, is not in the silicon powder incrustation for melting and often having during silicon, so that product Qualification rate is 100%, while significantly reducing the density gradient due to melting silicon process formation in the prior art.
Preferred scheme, the mesh number of the silicon powder are 80~120 mesh.
Inventors have found that extremely important to reaction effect, silicon powder partial size is excessive too small, instead during gas phase siliconising It is unfavorable for forming gas-phase silicon.
The utility model has the advantages that
1) the double target magnetic control sputterings of the pioneering use of the present invention obtain MAX phase boundary surface layer in SiC fiber surface, using magnetic control Sputtering effectively reduces depositing temperature, avoids the damage of fiber, and gained boundary layer is better than existing skill in terms of antioxygenic property The boundary layers such as art common C, BN.The boundary layer also has the characteristics that anti-neutron radiation simultaneously, can be used for nuclear radiation field.
2) present invention is using in preparation SiCfDuring/C porous materials, polycondensation is carried out using resorcinol and formaldehyde Reaction generates phenolic resin, while joined dehydrated alcohol as solvent, in solution system, can obtain preferably dipping effect Fruit forms many holes simultaneously because volatilizing in dehydrated alcohol solidification process, and high-specific surface area, high hole are obtained after cracking Porous C/C composite of rate, and conventional resins compactness extent is higher, it is difficult to obtain biggish specific surface area.
3) silicon steam and SiC in the present invention, are obtained using contactless gas phase siliconising methodfC in/C porous materials Reaction, forms the silicon carbide substrate of dense uniform, during contactless, silicon powder in mold by siphonage with SiCfThe reaction of/C porous materials, can obtain better siphon effect, the SiCf/ SiC ceramic matrix composite material surface is clean, product Qualification rate is 100%, significantly reduces the density gradient in the prior art due to melting silicon process formation.
Specific embodiment
Following embodiment is intended to further illustrate the content of present invention, rather than limits the protection model of the claims in the present invention It encloses.
Embodiment 1
SiC fiber braid is placed in magnetron sputtering vacuum chamber, is first sputtered using TiC target, initial vacuum degree is sputtered For 2 × 10-3Pa, the distance between target and fiber are 80mm, argon flow 30sccm, and sputter temperature is room temperature, sputtering power For 2200W, deposition rate 10nm/min, sputtering time 10mim.Silicon carbide fibre braided part in transition zone containing TiC is obtained, Then use TiC target and Si target co-sputtering, sputtering initial vacuum degree be 1 × 10-3Pa, the distance between target and fiber be 90mm, Argon flow is 40sccm, and sputter temperature is room temperature, sputtering power 1500W, deposition rate 5nm/min, and sputtering time is 100mim.It obtains and contains Ti3SiC2The silicon carbide fibre braided part of boundary layer,
Then contain Ti3SiC2The SiC fiber of boundary layer is placed in maceration extract, carries out vacuum impregnation, is controlled vacuum-impregnated true Reciprocal of duty cycle≤0.001MPa impregnates 2h, is then solidified in 160 DEG C, and curing time 3h, right thing is cracked then at 800 DEG C, Pyrolysis time is 2h, repeats the dipping-solidification-cracking process 4 times, and acquisition density is 1.68g/cm3SiCf/ C porous body material Material, it includes following composition that the maceration extract is counted in mass ratio: resorcinol, formaldehyde, dehydrated alcohol are according to mass ratio 4:8:26.
By above-mentioned SiCf/ C porous materials are placed in the graphite jig for being equipped with 80 mesh silicon powders, the SiCf/ C porous body It is lined with hollow graphite block body below material, so that SiCf/ C porous materials are not directly contacted with, and under vacuum conditions, are warming up to 1900 DEG C, vacuum degree 800Pa, 60min is kept the temperature, i.e. acquisition SiCf/ SiC ceramic matrix composite material.
Embodiment 2
SiC fiber braid is placed in magnetron sputtering vacuum chamber, is first sputtered using TiC target, initial vacuum degree is sputtered It is 3 × 10-3Pa, the distance between target and fiber are 100mm, argon flow 40sccm, and sputter temperature is room temperature, sputtering power For 2400W, deposition rate 15nm/min, sputtering time 15mim.Silicon carbide fibre braided part in the journey of transition containing TiC is obtained, Then TiC target and Si target co-sputtering are used, sputtering initial vacuum degree is 3 × 10-3Pa, the distance between target and fiber be 80mm, Argon flow is 30sccm, and sputter temperature is room temperature, sputtering power 1700W, deposition rate 7nm/min, and sputtering time is 90mim.It obtains and contains Ti3SiC2The silicon carbide fibre braided part of boundary layer.
Then contain Ti3SiC2The SiC fiber of boundary layer is placed in maceration extract, carries out vacuum impregnation, is controlled vacuum-impregnated true Reciprocal of duty cycle≤0.001MPa impregnates 2h, is then solidified in 200 DEG C, curing time 2.5h, right thing is split then at 900 DEG C Solution, pyrolysis time 1.5h repeat the dipping-solidification-cracking process 5 times, and acquisition density is 1.79g/cm3SiCf/ C is porous Body material, it includes following composition that the maceration extract is counted in mass ratio: resorcinol, formaldehyde, dehydrated alcohol are according to mass ratio 5:9: 26。
By above-mentioned SiCf/ C porous materials are placed in the graphite jig for being equipped with 90 mesh silicon powders, the SiCf/ C porous body It is lined with hollow graphite block body below material, so that SiCf/ C porous materials are not directly contacted with, and under vacuum conditions, are warming up to 2000 DEG C, vacuum degree 800Pa, 40min is kept the temperature, i.e. acquisition SiCf/ SiC ceramic matrix composite material.
Embodiment 3
SiC fiber braid is placed in magnetron sputtering vacuum chamber, is first sputtered using TiC target, initial vacuum degree is sputtered For 5 × 10-3Pa, the distance between target and fiber are 120mm, argon flow 40sccm, and sputter temperature is room temperature, sputter function Rate is 2600W, deposition rate 10nm/min, sputtering time 20mim.Obtain silicon carbide fibre braiding in the journey of transition containing TiC Then part uses TiC target and Si target co-sputtering, sputtering initial vacuum degree is 2 × 10-3Pa, and the distance between target and fiber are 110mm, argon flow 50sccm, sputter temperature are room temperature, sputtering power 1800W, deposition rate 10nm/min, sputtering Time is 150mim.It obtains and contains Ti3SiC2The silicon carbide fibre braided part of boundary layer.
Then contain Ti3SiC2The SiC fiber of boundary layer is placed in maceration extract, carries out vacuum impregnation, is controlled vacuum-impregnated true Reciprocal of duty cycle≤0.001MPa impregnates 2h, is then solidified in 200 DEG C, curing time 2h, right thing is split then at 1000 DEG C Solution, pyrolysis time 1h repeat the dipping-solidification-cracking process 3 times, and acquisition density is 1.64g/cm3SiCf/ C porous body Material, it includes following composition that the maceration extract is counted in mass ratio: resorcinol, formaldehyde, dehydrated alcohol are according to mass ratio 6:10: 20。
By above-mentioned SiCf/ C porous materials are placed in the graphite jig for being equipped with 80 mesh silicon powders, the SiCf/ C porous body It is lined with hollow graphite block body below material, so that SiCf/ C porous materials are not directly contacted with, and under vacuum conditions, are warming up to 1950 DEG C, vacuum degree 1000Pa, 50min is kept the temperature, i.e. acquisition SiCf/ SiC ceramic matrix composite material.
Comparative example 1
Other conditions are same as Example 1, only not first depositing Ti C transition zone, obtain SiCf/ SiC ceramic matrix composite material.
Comparative example 2
Other conditions are same as Example 2, and maceration extract is phenolic resin, obtain SiCf/ SiC ceramic matrix composite material.Porous performance Poor, density gradient is big after later period siliconising.
Comparative example 3
Other conditions are same as Example 2, using the silicon powder of 800 mesh, obtain SiCf/ SiC ceramic matrix composite material.
Comparative example 4
Ceramming process and embodiment 3 are consistent, only first obtain C boundary layer using CVI method, then obtain through ceramic SiCf/ SiC ceramic matrix composite material
Performance test
SiC prepared by above-described embodiment and comparative examplefIt is tested for the property after/SiC ceramic matrix composite material is processed, it is resulting Results of property is as shown in table 1.
1 SiC of tablef/ SiC ceramic matrix composite material performance test table
By prepared by above-described embodiment and comparative example in air 1200 DEG C oxidation after carry out Mechanics Performance Testing, tie Fruit such as table 2.
2 SiC of tablefMechanical property in/SiC ceramic matrix composite material air after 1200 DEG C of oxidations

Claims (10)

1. one kind contains Ti3SiC2The SiC of boundary layerfThe preparation method of/SiC ceramic matrix composite material, which comprises the steps of: Depositing Ti is carried out to SiC fiber braid using the method for magnetron sputtering3SiC2, obtain and contain Ti3SiC2The SiC fiber of boundary layer Then braided part obtains SiC by resin impregnation carbonizationf/ C porous body, then SiC is obtained by gas phase siliconisingf/ SiC composite wood Material.
2. according to claim 1 a kind of containing Ti3SiC2The SiC of boundary layerfThe preparation method of/SiC ceramic matrix composite material, it is special Sign is: the method for magnetron sputtering is double target magnetic control sputtering methods, and double targets are respectively TiC target, Si target.
3. according to claim 2 a kind of containing Ti3SiC2The SiC of boundary layerfThe preparation method of/SiC ceramic matrix composite material, it is special Sign is: the method for the magnetron sputtering is first to carry out magnetron sputtering using TiC target, in SiC fibre bundle or SiC fiber braid The TiC that surface obtains 0.1~0.2 μm crosses coating, then obtains Ti using TiC target and Si target double target co-sputtering again3SiC2, institute State Ti3SiC2Thickness control be 0.6~1.0 μm.
4. according to claim 3 a kind of containing Ti3SiC2The SiC of boundary layerfThe preparation method of/SiC ceramic matrix composite material, it is special Sign is: the deposition process that TiC crosses coating is that SiC fiber braid is placed in magnetron sputtering vacuum chamber, first uses TiC target It is sputtered, sputtering initial vacuum degree is 1~5 × 10-3Pa, the distance between target and fiber are 80~120mm, argon flow 30 ~50sccm, sputter temperature are room temperature, and sputtering power is 2200~2800W, and deposition rate is 10~20nm/min, sputtering time For 5~20mim.
5. according to claim 3 a kind of containing Ti3SiC2The SiC of boundary layerfThe preparation method of/SiC ceramic matrix composite material, it is special Sign is: the Ti3SiC2Deposition process be that using TiC target and Si target co-sputtering, sputtering initial vacuum degree is 1~5 × 10-3Pa, the distance between target and fiber are 80~120mm, argon flow is 30~50sccm, and sputter temperature is room temperature, sputter function Rate is 1500~2000W, and deposition rate is 5~10nm/min, and sputtering time is 80~200min.
6. according to claim 1 a kind of containing Ti3SiC2The SiC of boundary layerfThe preparation method of/SiC ceramic matrix composite material, it is special Sign is: the process of the resin impregnation carbonization are as follows: will contain Ti3SiC2The SiC fiber braid of boundary layer is placed in maceration extract, Vacuum impregnation is carried out, after the completion of dipping, solidification, cracking repeat above-mentioned dipping-solidification-cracking process 3~5 times, finally prepare Density is 1.6~1.8g/cm3SiCf/ C porous materials, it includes following composition: isophthalic two that the maceration extract is counted in mass ratio Phenol, formaldehyde, dehydrated alcohol are according to mass ratio (4~6): (8~10): (20~26).
7. according to claim 6 a kind of containing Ti3SiC2The SiC of boundary layerfThe preparation method of/SiC ceramic matrix composite material, it is special Sign is: the vacuum-impregnated vacuum degree≤0.001MPa, and the vacuum-impregnated time is 1~3h；The cured temperature Degree is 160 DEG C~220 DEG C, and the cured time is 2~3h；The temperature of the cracking is 800 DEG C~100 DEG C, the solidification Time be 1~2h.
8. according to claim 1 a kind of containing Ti3SiC2The SiC of boundary layerfThe preparation method of/SiC ceramic matrix composite material, it is special Sign is: the process of the gas phase siliconising is, by SiCf/ C porous materials are placed in the graphite jig for being equipped with silicon powder, described SiCfIt is lined with graphite block body below/C porous materials, so that SiCf/ C porous materials are not directly contacted with silicon powder, in vacuum item Under part, 1900~2000 DEG C are warming up to, keeps the temperature 30~60min, is i.e. acquisition SiCf/ SiC ceramic matrix composite material.
9. according to claim 8 a kind of containing Ti3SiC2The SiC of boundary layerfThe preparation method of/SiC ceramic matrix composite material, it is special Sign is: the graphite block body is hollow graphite block.
10. according to claim 8 a kind of containing Ti3SiC2The SiC of boundary layerfThe preparation method of/SiC ceramic matrix composite material, it is special Sign is: the mesh number of the silicon powder is 80~120 mesh.
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CN116836002B (en) * 2023-05-26 2024-04-30 西北工业大学 Be used for SiCfTi-Si-C composite coating on SiC surface and preparation method thereof

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