CN1267380C - Preparation method of enhanced silicon carbide based composite material in short fiber - Google Patents
Preparation method of enhanced silicon carbide based composite material in short fiber Download PDFInfo
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- CN1267380C CN1267380C CN 200410067103 CN200410067103A CN1267380C CN 1267380 C CN1267380 C CN 1267380C CN 200410067103 CN200410067103 CN 200410067103 CN 200410067103 A CN200410067103 A CN 200410067103A CN 1267380 C CN1267380 C CN 1267380C
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Abstract
The present invention provides a preparation method of an enhanced SiC composite material in short fiber, which belongs to the field of ceramic-based composite materials. The preparation method of an enhanced SiC composite material in short fiber is characterized in that SiC powder is prepared into material slurry and short fiber; fiber is sufficiently dispersed in the base body in an ultrasonic dispersion mode; the adhesiveness of SiC powder is removed after drying; finally, the enhanced SiC composite material in short fiber is prepared by a discharging plasma rapid sintering method. The composite material with uniform fiber dispersion can be prepared by the technology; simultaneously, the fiber damage in the process of preparation can be reduced by discharging plasma sintering. The fiber content of the enhanced SiC composite material in short fiber, which is prepared by the technology provided by the present invention, reaches 45 vol%; when 45 vol% SiC fiber is reinforced, the preparation method provided by the present invention is adopted; the intensity of a prepared SiC/SiC composite material reaches 350MPa. The maximum strain is 0.15%, which is remarkably larger than the strain of monomer SiC.
Description
Technical field
The invention relates to the preparation method of enhanced silicon carbide based composite material in short fiber, belong to the ceramic matric composite field.
Background technology
High temperature resistant, the low density of stupalith, oxidation-resistance and good characteristic such as anticorrosive make it have the potentiality of part alternative metals as high-temperature structural material of new generation.But because the weakness of stupalith itself: fragility, seriously hindered the widespread use of stupalith.FRCMC is the most noticeable, has the fracture behaviour of metalloid, to the not clear sense of crackle, does not produce catastrophic failure.In order to improve the intensity and the fracture toughness property of pottery, the unremitting effort that many material supplier authors carry out.At the beginning of the seventies, FRCMC is to strengthen on the basis of polymkeric substance and fiber-reinforced metal matrix composite at fiberoptic fiber, proposes the notion of FRCMC first.Fiber is introduced and to be made pottery mechanism such as extract at breaking-down process by crack deflection, fibre breakage and fiber in the ceramic matrix to absorb energy, both improved the fracture toughness property of material, kept original performance of ceramic matrix again.Enlarged the range of application of stupalith greatly.
The SiC pottery has very high hot strength, thermal conduction capability and good high temperature resistant, anti-oxidant, corrosion-resistant and creep resistance, so fiber reinforcement SiC matrix material is one of most important material in the ceramic matric composite, has been widely used in military affairs and aviation field.The main method of the SiC of preparation fiber reinforcement at present matrix material has: chemical vapor infiltration (CVI), organic precursor dipping and cracking (PIP), reaction sintering (RS) and hot pressed sintering (HP), these methods respectively have relative merits, and all be used to prepare Continuous Fiber Reinforced Ceramic Matrix Composites, mainly be because the enhancing body of continuous fibre enhancing SiC matrix material weaves in advance, matrix is that original position generates or dipping enters inside and outside the fibrous bundle, finally be prepared into required material, what need solution mainly is the voidage that how to reduce fibrous inside, improve the compactness of material, thereby improve the intensity of material.Should manage how to make the material densification on the one hand and strengthen the SiC matrix material for staple fibre, what also need simultaneously to consider is how to make fiber uniform distribution in matrix.Up to now, still do not have in advance fiber reinforcement is positioned the fixed method, so requiring of preparation process and continuous fibre enhancing SiC is different, and staple fibre strengthens very difficult raising of SiC Composite Preparation process fibre content, and toughening effect do not have continuous fibre obvious, so no matter be that domestic or international research report to this respect is considerably less.
At present, the preparation that strengthens the SiC based composites of preparation staple fibre mainly is mixed with the slurry that is fit to flow casting molding to SiC particle and staple fibre at present and is prepared from conjunction with hot pressing agglomerating mode.By the curtain coating mode for the casting slurry performance requriements than higher, long owing to the hot pressed sintering time simultaneously, make fiber long in the pyritous time, damage to fiber is bigger, so can influence the particularly reinforced effects of the higher fiber of performance specific activity of fiber, hot pressed sintering process grain growth simultaneously influence the thermal shock resistance of material, and technology is more loaded down with trivial details.Plasma discharging (spark plasma sintering is called for short SPS) is the flash sintering method that development in recent years is got up, and has homogeneous heating, heat-up rate is fast, and sintering temperature is low, and the time is short, production efficiency height, product are organized tiny even, can keep raw-material state of nature; Can obtain the material of high-compactness; Can the sintering gradient material and material with complex such as large-scale workpiece.In sintering process, can overcome damage preferably to fiber.
Summary of the invention
The object of the present invention is to provide that a kind of fast simple and easy cheap preparation staple fibre strengthens the SiC based composites, respectively with SiC, C fiber and B fiber as strengthening body, it is even to obtain fiber dispersion by special process, the material of better performances.
At preparation fiber reinforcement SiC based composites high performance fiber must be arranged, this is because high-performance fiber is to make fiber owing to certain micritization, reduces the activity of fiber, improves the resistance of oxidation of fiber; Also can weaken the simultaneously Chemical bond of fiber and matrix is given full play to the enhancement of fiber.The present invention relates to a kind of quick preparation fiber reinforcement SiC based composites, make fiber be difficult to react, reduce the Chemical bond of fiber and matrix with matrix in the process of preparation.
The invention provides the preparation method that a kind of preparation staple fibre (C fiber, SiC fiber and B fiber etc.) strengthens ceramic matric composites such as SiC base, its step is as follows:
(a) nanometer or submicron SiC powder and a certain amount of sintering aid are carried out the ball milling wet-mixed, dry under the vacuum drying oven certain temperature then, sieve with 200 mesh sieve at last; Also be that particle diameter is less than 75 μ m; The sintering aid that is adopted is Al
2O
3, Y
2O
3Or a kind of or two kinds among the AlN, its add-on is 3～10wt% of SiC powder;
(b) nanometer that contains sintering aid that step (a) is made or submicron SiC and a certain amount of binding agent (simultaneously also as dispersion agent) mixture ball milling in organic solvent is mixed into slurry usefulness Polycarbosilane as binding agent, its content is 5%～50%, and dispersion medium is gasoline or dimethylbenzene; During as binding agent, its content is 2%～5% with resol, and dispersion medium is an alcohol;
(c) with certain volume content (10%-45%), staple fibre from several centimetre-sized to micron order length, at first with agitator with staple fibre stirred 30 minutes to 1 hour in the dispersion medium of corresponding SiC slip; Staple length is the most frequently used for the 0.5-5 millimeter;
(d) in the fiber that stirs in advance, add a certain amount of slurry, make fiber be dispersed in fully in the SiC slip with 30 minutes～1 hour method of ultra-sonic dispersion simultaneously;
(e) rapid drying under the high wind condition with scattered fiber and pulp solution obtains certain thickness fiber reinforcement SiC matrix material biscuit at last, and unsticking cracking binding agent is carried out in dry back under 750～800 ℃ of certain temperature conditions under vacuum or argon gas condition;
(f) in 1550 ℃～1650 ℃ scopes, heat-up rate with 100 ℃/min～300 ℃/min, insulation 2～10min, pressure is the fiber reinforcement SiC based composites of preparing different content under the condition of 15MPa～45MPa (press the SPS routine, pressure and electric current are all vertical direction) with the plasma discharging flash sintering method.
This shows that advantage of the present invention is:
(1) utilizes fiber and matrix dispersive mode in organic dispersing agent to prepare staple fibre and strengthen the SiC matrix material, overcome in the past and prepared the dependent form of staple fibre enhancing SiC based composites the SiC size performance with casting method, the material fiber of preparation is evenly distributed and content can be up to 45%, make preparation technology simplify, do not need casting apparatus, reduced cost.
(2) determine SPS Fast Sintering technology, to the damage of fiber, be particularly suitable for that the higher fibre reinforcement of activity is had good practical value in the reduction sintering preparation process; Fiber surface is more smooth, and basic not degraded becomes spongy unformed material to form sharp contrast (Fig. 1) with fiber degradation in the SiC based composites of hot pressed sintering.
(3) technology is simpler, and preparation cycle is short, is fit to produce in batches; Also be fit to the preparation fiber reinforcement
Other ceramic matric composite and Continuous Fiber Reinforced Ceramic Matrix Composites.
Description of drawings
Fig. 1 hot pressed sintering (a) compares with the fracture pattern of SPS sintering (b) C/SiC matrix material
The glazed surface microstructure of Figure 22 5V%C/SiC matrix material (300 times)
The glazed surface microstructure of Figure 32 5V%C/SiC matrix material (5000 times)
The section microstructure of Figure 42 5V%C/SiC matrix material (300 times)
The section microstructure of Figure 52 5V%C/SiC matrix material (3000 times)
The glazed surface microstructure of Figure 64 5V%SiC/SiC matrix material (1000 times)
The glazed surface microstructure of Figure 74 5V%SiC/SiC matrix material (5000 times)
The glazed surface section structure of Figure 84 5V%SiC/SiC matrix material (300 times)
The glazed surface section structure of Figure 94 5V%SiC/SiC matrix material (5000 times)
Figure 10 staple fibre provided by the invention strengthens preparation technology's flow process of SiC based composites
Embodiment:
Further specify the method provided by the invention of utilizing below by example, availability staple fibre preferably strengthens the SiC matrix material, but limits the present invention absolutely not.
Embodiment 1
Weighing is 1～2 centimetre fiber 25% volume content C fiber by the length that calculating is good in advance, in alcohol, disperseed 30 minutes with stirring method in advance, the back made it fully disperse in alcohol in 60 minutes with ultra-sonic dispersion, and the nano SiC that adds simultaneously in the dispersion process (contains 5wt%Al
2O
3And Y
2O
3) slip (slip is made dispersion agent with resol, and content is 4%), it is disperseed between fiber fully.After scattered fiber and SiC slip drying, under being 800 ℃, vacuum condition, temperature carries out unsticking, be cut into required shape with scalpel, utilize the required matrix material of plasma discharging Fast Sintering at last, sintering condition is: 1650 ℃ of temperature, soaking time 3 minutes, temperature rise rate are 200 ℃/min, and pressure is 15MPa.Its microtexture of C/SiC matrix material such as Fig. 2, Fig. 3 of preparing at last, fiber dispersive in matrix is more even, and Fig. 4,5 shows that fiber extracts the fiber surface smoother from matrix.Its intensity reaches 270MPa, maximum strain is 0.2%, strain much larger than the SiC one-component ceramic, illustrate that fiber plays toughness reinforcing effect to the SiC pottery, and the C/SiC matrix material by hot pressed sintering preparation is because fiber degradation serious, intensity is reduced, have only 180Mpa (Fig. 1), its technical process as shown in figure 10.
Embodiment 2
Weighing is the fiber 45% content volume content SiC fiber of 2～3mm by calculating good length in advance.Disperseed in alcohol 60 minutes with stirring method earlier, the back made it fully disperse in gasoline in 30 minutes with ultra-sonic dispersion, and the nano SiC that adds simultaneously in the dispersion process (contains AlN and Y
2O
3) slip (the SiC slip is made dispersion agent with Polycarbosilane, and content is 10%), it is disperseed between fiber fully.After scattered fiber and SiC slip drying; under being 800 ℃, argon shield condition, temperature carries out unsticking; be cut into required shape with scalpel; utilize the required matrix material of plasma discharging Fast Sintering at last; sintering condition is: 1600 ℃ of temperature; soaking time 6 minutes, pressure is 300 ℃/min for the 30MPa temperature rise rate.Its microtexture of SiC/SiC matrix material such as Fig. 6,7 of preparing at last; fiber dispersive in matrix is more even; in order to reduce the bonding force of fiber and matrix; the SiC fiber surface scribbles one deck carbon; extract of the protection of fiber surface carbon as can be seen from Fig. 8,9 to fiber; the intensity of last SiC/SiC matrix material is 350MPa, and maximum strain is 0.15%, also greater than the monomeric strain of SiC.
Embodiment 3
Weighing is the fiber 10% content volume content B fiber of 0.5～0.8mm by calculating good length in advance.Disperseed in alcohol 40 minutes with stirring method earlier, the back made it fully disperse in alcohol in 40 minutes with ultra-sonic dispersion, and the micron SiC that adds simultaneously in the dispersion process (contains AlN and Y
2O
3) slip (slip resol is dispersion agent, and its content is 5%), it is disperseed between fiber fully.After scattered fiber and SiC slip drying, under being 800 ℃, vacuum condition, temperature carries out unsticking, be cut into required shape with scalpel, utilize the required matrix material of plasma discharging Fast Sintering at last, sintering condition is: 1550 ℃ of temperature, soaking time 10 minutes, temperature rise rate are 250 ℃/min, and pressure is 45MPa.The B/SiC matrix material for preparing at last.The gained material intensity be 220MPa, maximum strain is 0.3%.
Claims (8)
1. the preparation method of an enhanced silicon carbide based composite material in short fiber comprises that staple fibre disperses, and the preparation of SiC slip and both uniform mixing, drying, sintering process process is characterized in that comprising following processing step:
(a) nanometer or submicron SiC powder and sintering aid are carried out ball milling wet-mixed, vacuum-drying then;
(b) nanometer that contains sintering aid that step (a) is made or submicron SiC and binder mixtures ball milling in organic solvent are mixed into slurry;
(c) with the staple fibre from several centimetre-sized to micron order length of 10%-45% volume content, at first with agitator with staple fibre stir in the dispersion medium of corresponding SiC slip;
(d) with ultra-sonic dispersion method fiber is dispersed in the SiC slip fully when in the staple fibre that stirs in advance, adding the slurry of step (b) preparation;
(e) with scattered fiber and pulp solution rapid drying, obtain certain thickness fiber reinforcement SiC matrix material biscuit at last, unsticking cracking binding agent is carried out in dry back under 750～800 ℃ of conditions under vacuum or argon gas condition;
(f) at last in 1550 ℃～1650 ℃ scopes, heat-up rate with 100 ℃/min～300 ℃/min, insulation 2～10min, pressure is 15MPa～45Mpa, and pressure and electric current are all the fiber reinforcement SiC based composites of preparing different content under the condition of vertical direction with the plasma discharging flash sintering method.
2. by the preparation method of the described enhanced silicon carbide based composite material in short fiber of claim 1, it is characterized in that described sintering aid is Al
2O
3, Y
2O
3Or a kind of or two kinds among the AlN, its add-on is 3～10wt% of SiC powder.
3. by the preparation method of the described enhanced silicon carbide based composite material in short fiber of claim 1, add-on is 5～10wt% when it is characterized in that Polycarbosilane is made binding agent; Add-on is 2%～5% during as binding agent with resol.
4. by the preparation method of the described enhanced silicon carbide based composite material in short fiber of claim 1, it is characterized in that described staple fibre is a kind of in SiC, C or the B fiber.
5. by the preparation method of claim 1 or 4 described enhanced silicon carbide based composite material in short fiber, it is characterized in that described staple length is 0.5～5 millimeter.
6. by the preparation method of claim 1 or 4 described enhanced silicon carbide based composite material in short fiber, it is characterized in that described staple fibre to carry out churning time in the dispersion medium of corresponding SiC slip be 30～60 minutes.
7. by the preparation method of claim 1 or 4 described enhanced silicon carbide based composite material in short fiber, it is characterized in that adding the SiC slurry in the described staple fibre that stirs in advance is 30～60 minutes with the ultra-sonic dispersion time simultaneously.
8. by the preparation method of the described enhanced silicon carbide based composite material in short fiber of claim 1, it is characterized in that containing the nanometer of sintering aid or submicron SiC dried bean noodles dry after, sieve, make particle diameter less than 75 μ m.
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