CN103288468A - Preparation method for fiber reinforced carbon-silicon carbide-zirconium carbide-based composite material - Google Patents
Preparation method for fiber reinforced carbon-silicon carbide-zirconium carbide-based composite material Download PDFInfo
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Abstract
The invention discloses a preparation method for a fiber reinforced carbon-silicon carbide-zirconium carbide-based (C/C-SiC-ZrC) composite material. The preparation method comprises the following steps of: (a) evenly dispersing ZrC nanopowder in absolute ethyl alcohol; (b) mixing phenolic resin and ZrC dispersion liquid to form slurry; (c) immersing a two-dimensional carbon fiber sheet into the slurry for dipping and drying, then carrying out continuous superposition paving on the two-dimensional carbon fiber sheet, and carrying out curing and post-curing treatment to prepare a fiber-reinforced sintered body; (d) cracking the fiber-reinforced sintered body to obtain a porous C/C prefabricate; (e) placing silicon powder into a graphite crucible, burying the porous C/C prefabricate into the silicon powder, heating to 1,500-1,650 DEG C, and preserving heat for preset time so as to carry out liquid silicon permeation. The method can be used for improving the high-temperature oxidizing property and ablation property of the carbon fiber reinforced ceramic (C/C-SiC) composite material.
Description
Technical field
The present invention relates to the technology of preparing of fiber reinforcement multiphase ceramic based composites, particularly adopt the insoluble metal carbide matrices of composite material to be carried out the Technology of modification.
Background technology
Carbon-fiber reinforced carbon Tao Ji (C/C-SiC) matrix material is a kind of novel high-performance thermal structure material, has highly than excellent properties such as strong, Gao Bimo, corrosion-resistant, anti-thermal shocks, has very large application potential at high-technology fields such as aerospace.But complicated along with Service Environment had higher requirement to material system, and requires material system to have stronger designability.The C/C-SiC matrix material is being difficult to satisfy performance requirement anti-oxidant, anti-ablation more than 1600 ℃.In order further to improve oxidation-resistance and the ablation property of C/C-SiC matrix material, introducing ultrahigh-temperature ceramic phase (being mainly refractory carbide) in material is a kind of effective ways.This mainly has characteristics such as high-melting-point, excellent mechanical behavior under high temperature, anti-oxidant and anti-ablation owing to the ultrahigh-temperature pottery.
Zirconium carbide (ZrC) belongs to typical insoluble metal carbide, and its fusing point can generate the zone of oxidation of thickness up to 3420 ℃ under high-temperature oxidation environment, and protecting materials is further oxided and degrades, and makes material have excellent high-temperature stability.The method that at present ZrC is incorporated in the C/C-SiC matrix material mainly contains solution impregnation cracking process and zirconium alloy permeable reactive method etc.Not only preparation cycle is long and cost is high for these Technologies, is unfavorable for suitability for industrialized production.
Summary of the invention
The object of the present invention is to provide a kind of technological process simple, can realize that the dead size shaping fiber strengthens the preparation method of carbon-silicon carbide-zirconium carbide base (C/C-SiC-ZrC) matrix material.
Specific embodiments is as follows:
The preparation method of a kind of fiber reinforcement carbon-silicon carbide-zirconium carbide based composites is characterized in that, comprises the steps:
(a) a certain proportion of ZrC nanometer powder is joined in a certain amount of dehydrated alcohol, through fully behind stirring and the sonic oscillation ZrC nanometer powder evenly being disperseed in dehydrated alcohol;
(b) the ZrC dispersion liquid that resol and step (a) are obtained, makes resol be dissolved in the dehydrated alcohol and adopts ultra-sonic oscillation to make the ZrC nanometer powder evenly disperse to form slurry than mixing according to certain mass;
(c) two-dimentional carbon cloth is immersed in the slurry that step (b) obtains and fully floods, dry two-dimentional carbon cloth through dipping, in mould, this two dimension carbon cloth is folded overlay continuously then, and behind folded overlay, be cured and post curing treatment preparation fiber reinforcement biscuit body;
(d) the fiber reinforcement biscuit body that step (c) is obtained places in the pyrographite stove, is warmed up to default temperature rise rate and carries out cracking more than 900 ℃, obtains the porous C/C precast body of even dispersion ZrC particle;
(e) silica flour is positioned in the plumbago crucible, and porous C/C precast body that step (d) is obtained is embedded in the silica flour, plumbago crucible is placed in the pyrographite stove, be heated to 1500-1650 ℃ and be incubated the scheduled time and carry out the liquid silicon infiltration with default temperature rise rate, obtain fiber reinforcement carbon-silicon carbide-zirconium carbide based composites.
In step (a), preferably more than 99.0%, granularity is preferably 10-60nm to the purity of ZrC nanometer powder, when big as if powder size, need reduce granularity through high-energy ball milling.In addition, the mass ratio of ZrC nanometer powder and dehydrated alcohol is preferably 0.025-0.125:1.
In step (b), the resol kind of using is not particularly limited.ZrC nanometer powder in the ZrC dispersion liquid and the mass ratio of resol are preferably 0.02-0.1:1, by adopting ultrasonic oscillation, can obtain the resin adhesive liquid of even dispersion ZrC nanometer powder.In addition, in order to promote the dissolving of resol in dehydrated alcohol, before preferably mixing with the ZrC dispersion liquid resol is carried out fragmentation and handle, and the preferred mixed solution that heats between 30-50 ℃ is finished up to the dissolution process of resol in dehydrated alcohol.
In step (c), two-dimentional carbon cloth is T300, T700 or other product.Two-dimentional carbon cloth is fully flooded in the slurry that step (b) obtains, fully dipping is by the super-dry process, absolute ethanol volatilizes, even dispersion resin and ZrC nanometer powder in the fibrous bundle of two dimension carbon cloth, the mass ratio of its disperse quality and two-dimentional carbon cloth is preferably 1:1.4-2.6.Two-dimentional carbon cloth behind the folded overlay is preferably applied the pressure of 2-5MPa, can make the gas that discharges in the resin solidification cross-linking process be extruded eliminating like this, thereby prepare the fiber reinforcement biscuit body of tight shop layer.Condition of cure is preferably 130-150 ℃, 6-10 hour, and the after fixing condition is 180-230 ℃, 20-30 hour.In addition, the shop number of plies is not particularly limited, can requires suitably to adjust according to material thickness.
In step (d), default temperature rise rate is generally 1-3 ℃/minute, and the cracking time was generally 30-60 minute.Under the Pintsch process condition, resol generation polycondensation in the fiber reinforcement biscuit body, thereby the volumetric shrinkage that 50%-60% occurs, owing to contain fortifying fibre in the biscuit body, resin matrix tension stress occurs owing to being subjected to the different resistance of fiber both direction in contraction process, this makes and produces tiny crack in the matrix.Simultaneously, resin also can produce a large amount of gases in cracking process, along with the rising of cracking temperature, gas yield accumulates and forms air pressure gradually in base cavity, air pressure progressively raises and finally causes pore to break, and produces micropore, forms the C/C precast body of porous/crackle.In order there to be more cracking carbon to generate in the precast body, the preferred higher resin system of carbon residue rate, the present invention selects resol for use.In addition, cracking environmental optimization nitrogen environment, this is because two-dimentional carbon cloth can not cause the fibre strength degradation under nitrogen environment, can keep the wild phase fibre shape.
In step (e), the mass ratio of C/C precast body and silica flour is preferably 0.4-0.5:1, by adopting this mass ratio, can make matrix carbon and liquid silicon that fully reaction takes place, and does not have too much liquid silicon infiltration simultaneously and forms the residual silicon phase.Silicon particle size is generally the 10-40 order.In addition, default temperature rise rate is generally 3-5 ℃/minute, and the insulation Preset Time was generally 30-60 minute.
The beneficial effect of the invention is:
(1) can prepare comparatively fine and close C/C-SiC-ZrC matrix material by the present invention, and this C/C-SiC-ZrC matrix material effectively improves its oxidation-resistance and ablation resistance with respect to the C/C-SiC matrix material, therefore had excellent high-temperature stability.
(2) because the present invention directly is incorporated into ZrC ultrahigh-temperature ceramic phase in the C/C-SiC matrix material, make that whole prepared cycle shortening and operating process are simple, be conducive to suitability for industrialized production more.
(3) the matrix modification method that adopts among the present invention is conducive to carbon-fiber reinforced carbon pottery based composites is carried out heterogeneous matrix component optimization, to satisfy the different requirements under the complicated Service Environment.
Embodiment
Describe the present invention in detail below in conjunction with embodiment; but the following examples only are preferred implementation of the present invention; protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to replacement or change according to technical scheme of the present invention and inventive concept thereof, all should be encompassed within protection scope of the present invention.
Material therefor is the commercially available material among the following embodiment.
Embodiment 1
In the present embodiment, ZrC nanometer powder and resol mass ratio are 0.02:1, and selected two-dimentional carbon cloth is two-dimentional T300 carbon cloth.Its implementation method is carried out according to following step:
1. be that 0.1 milligram analytical balance takes by weighing 2 gram ZrC nanometer powder (purity 99.0% in precision, median size 50nm), take by weighing 80 gram dehydrated alcohols at general utility balance, both mix, stir, being placed on vibrates in the ultrasonic bath is uniformly dispersed the ZrC nanometer powder.
2. after solid phenolic resin being carried out fragmentation (the bulk resin is suitably broken), taking by weighing 100 gram resins joins in the dispersion liquid of step 1 preparation, mixed solution is placed on is heated to resin in 50 ℃ of baking ovens and dissolves fully, adopt ultra-sonic oscillation to make the ZrC nanometer powder evenly disperse to form slurry then.
3. (size: 100 * 70 * 60mm) in the slurry that step 2 obtains fully behind the dipping with the two-dimentional T300 carbon cloth of about 25 grams after the cuttings, in air, dry, take by weighing cloth after drying at general utility balance, quality is about 43g, (from molding jig, size: continuous shop layer is to 20 layers in 100 * 70 * 60mm) at mould then.Shop layer is finished the back mould and is added 2MPa pressure, is positioned over that 130 ℃ of heating were cured in 10 hours in the baking oven, puts into retort furnace again and continues to heat with 180 ℃ and finished after fixing in 20 hours.
4. the material that step 3 is obtained is placed in the pyrographite stove, vacuumize and inflated with nitrogen after, be warmed up to 1200 ℃ and be incubated 60 minutes with 2 ℃/minute speed, insulation finishes the back powered-down, naturally cooling returns to room temperature, obtains about 27 gram porous C/C-ZrC precast bodies.
5. the silica flour (purity 〉=98%) that 60 grams, 40 mesh sieves sieve is got is positioned in the plumbago crucible, and porous C/C-ZrC precast body that step 4 is obtained is embedded in the silica flour, crucible is placed the pyrographite stove, be heated to 1650 ℃ and be incubated 60 minutes and carry out the liquid silicon infiltration with 5 ℃/minute temperature rise rates, insulation finishes the back powered-down, naturally cooling returns to room temperature, obtains the C/C-SiC-ZrC matrix material.
Embodiment 2
The present embodiment mass ratio of ZrC nanometer powder and resol as different from Example 1 is 0.05:1(ZrC nanometer powder 5 grams), other are identical with embodiment 1.
Embodiment 3
The present embodiment mass ratio of ZrC nanometer powder and resol as different from Example 1 is 0.08:1(ZrC nanometer powder 8 grams), other are identical with embodiment 1.
Embodiment 4
The present embodiment mass ratio of ZrC nanometer powder and resol as different from Example 1 is 0.1:1(ZrC nanometer powder 10 grams), other are identical with embodiment 1.
Embodiment 5
Present embodiment selected two-dimentional carbon cloth as different from Example 1 is two-dimentional T700 carbon cloth, and other are identical with embodiment 1.
Embodiment 6
The present embodiment mass ratio of ZrC nanometer powder and resol as different from Example 1 is 0.05:1(ZrC nanometer powder 5 grams), selected two-dimentional carbon cloth is two-dimentional T700 carbon cloth, other are identical with embodiment 1.
Embodiment 7
The present embodiment mass ratio of ZrC nanometer powder and resol as different from Example 1 is 0.08:1(ZrC nanometer powder 8 grams), selected two-dimentional carbon cloth is two-dimentional T700 carbon cloth, other are identical with embodiment 1.
Embodiment 8
The present embodiment mass ratio of ZrC nanometer powder and resol as different from Example 1 is 0.1:1(ZrC nanometer powder 10 grams), selected two-dimentional carbon cloth is two-dimentional T700 carbon cloth, other are identical with embodiment 1.
At first, adopt sem observation sample microscopic appearance.Used sample and observed result are as follows: gained C/C-SiC-ZrC matrix material and the sample section after the cutting carried out polished finish among (1) cutting embodiment 1-8, observe the sample section after the polishing, and find that the matrix material that obtains is comparatively fine and close.(2) gained C/C-SiC-ZrC matrix material among the embodiment 1-8 is carried out three-point bending mechanical property test (implementing according to the ASTMC1341-06 testing standard), find that the material fracture is non-brittle rupture, fracture surface of sample has tangible fiber bridging and fiber to extract, and fiber has played good toughening effect.(3) surface topography of sample is observed in (implementing according to the ASTM E458-2008 testing standard) back of ablating of gained C/C-SiC-ZrC matrix material among the embodiment 1-8, discovery has glassy oxides to generate, and this is the SiO that matrix (SiC, ZrC) high temperature oxidation generates
2And ZrO
2, its formation has protected material inside to be further oxided well, has improved the anti-oxidant and ablation resistance of material.
Among the cutting embodiment 1-8 gained C/C-SiC-ZrC matrix material and the specimen surface after the cutting carried out polished finish after, carry out Mechanics Performance Testing.Table 1 has been listed Mechanics Performance Testing result (flexural strength is implemented according to ASTM C1341-06 testing standard, and fracture toughness property is implemented according to ASTM C1421-10 testing standard).
Table 1
As can be seen from Table 1, the flexural strength of T700 fiber reinforcement C/C-SiC-ZrC matrix material and fracture toughness property all are higher than T300 fiber reinforcement C/C-SiC-ZrC matrix material.This is that T700 tensile strength of fiber (4.9GPa) is higher than due to the T300 tensile strength of fiber (3.5GPa) simultaneously because the C/C-SiC-ZrC matrix material of T700 fiber production contains higher fiber volume fraction.In addition, the present invention finds, the ZrC nanometer powder of interpolation different mass mark has tangible influence to the mechanical property of final C/C-SiC-ZrC matrix material, when the content of ZrC nanometer powder in resin is that the mass ratio of 5%(ZrC nanometer powder and resol is 0.05:1) time, it is optimum that the flexural strength of matrix material and fracture toughness property all reach, and add too much ZrC nanometer powder slurry viscosity is increased, easily form thicker ZrC nano powder reunion layer at the carbon cloth interlayer, thereby cause the arch formation of micro mist, cause mechanical property to reduce.
Simultaneously, among the cutting embodiment 1-8 gained C/C-SiC-ZrC matrix material and the specimen surface after the cutting carried out polished finish after, investigate its antioxidant property (natural air atmosphere in the tube furnace, oxidizing temperature is selected 500,700,900,1200,1400,1500 degrees centigrade, oxidization time was respectively 2,5 hours), discovery is under the high temperature atmosphere well-oxygenated environment, and the mass loss of the C/C-SiC-ZrC matrix material of the present invention's preparation is lower than the C/C-SiC matrix material.This is because under well-oxygenated environment, the oxidation of SiC and ZrC causes SiO
2And ZrO
2Formation, these oxidation productss are overlying on material surface and stop oxygen further to the material internal diffusion, thereby improve the material resistance of oxidation.
Claims (9)
1. the preparation method of fiber reinforcement carbon-silicon carbide-zirconium carbide based composites is characterized in that, comprises the steps:
(a) a certain proportion of ZrC nanometer powder is joined in a certain amount of dehydrated alcohol, through fully behind stirring and the sonic oscillation ZrC nanometer powder evenly being disperseed in dehydrated alcohol;
(b) the ZrC dispersion liquid that resol and step (a) are obtained, makes resol be dissolved in the dehydrated alcohol and adopts ultra-sonic oscillation to make the ZrC nanometer powder evenly disperse to form slurry than mixing according to certain mass;
(c) two-dimentional carbon cloth is immersed in the slurry that step (b) obtains and fully floods, dry two-dimentional carbon cloth through dipping, in mould, this two dimension carbon cloth is folded overlay continuously then, and behind folded overlay, be cured and post curing treatment preparation fiber reinforcement biscuit body;
(d) the fiber reinforcement biscuit body that step (c) is obtained places in the pyrographite stove, is warmed up to default temperature rise rate and carries out cracking more than 900 ℃, obtains the porous C/C precast body of even dispersion ZrC particle;
(e) silica flour is positioned in the plumbago crucible, and porous C/C precast body that step (d) is obtained is embedded in the silica flour, plumbago crucible is placed in the pyrographite stove, be heated to 1500-1650 ℃ and be incubated the scheduled time and carry out the liquid silicon infiltration with default temperature rise rate, obtain fiber reinforcement carbon-silicon carbide-zirconium carbide based composites.
2. method according to claim 1 is characterized in that, in step (a), the purity of described ZrC nanometer powder is more than 99.0%, and granularity is 10-60nm, and the mass ratio of ZrC nanometer powder and dehydrated alcohol is 0.025-0.125:1.
3. method according to claim 1 is characterized in that, in step (b), the ZrC nanometer powder in the ZrC dispersion liquid and the mass ratio of resol are 0.02-0.1:1.
4. method according to claim 1 is characterized in that, in step (b), before mixing with the ZrC dispersion liquid resol is carried out fragmentation and handle, and the heating mixed solution is finished up to the dissolution process of resol in dehydrated alcohol between 30-50 ℃.
5. method according to claim 1, it is characterized in that, in step (c), fully dipping is by the super-dry process, absolute ethanol volatilizes, even dispersion resin and ZrC nanometer powder in the fibrous bundle of two dimension carbon cloth, the mass ratio of its disperse quality and two-dimentional carbon cloth is 1:1.4-2.6.
6. method according to claim 1 is characterized in that, in step (c), the two-dimentional carbon cloth behind the folded overlay is applied the pressure of 2-5MPa, and condition of cure is 130-150 ℃, 6-10 hour, and the after fixing condition is 180-230 ℃, 20-30 hour.
7. method according to claim 1 is characterized in that, in step (d), default temperature rise rate is 1-3 ℃/minute, and the cracking environment is nitrogen environment.
8. method according to claim 1 is characterized in that, in step (e), the mass ratio of porous C/C precast body and silica flour is 0.4-0.5:1, and silicon particle size is the 10-40 order.
9. according to any described method of claim 1-8, it is characterized in that in step (e), default temperature rise rate is 3-5 ℃/minute, the insulation Preset Time is 30-60 minute.
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