CN105859318A - Staple fiber-silicon carbide nanofiber reinforced silicon carbide porous ceramic material and preparation method thereof - Google Patents

Staple fiber-silicon carbide nanofiber reinforced silicon carbide porous ceramic material and preparation method thereof Download PDF

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CN105859318A
CN105859318A CN201610231795.6A CN201610231795A CN105859318A CN 105859318 A CN105859318 A CN 105859318A CN 201610231795 A CN201610231795 A CN 201610231795A CN 105859318 A CN105859318 A CN 105859318A
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fiber
carbon fiber
silicon carbide
phenolic resin
chopped
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CN105859318B (en
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代吉祥
沙建军
吕钊钊
邵俊琦
张兆甫
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Dalian University of Technology
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Abstract

The invention discloses a preparation method of a staple fiber-silicon carbide nanofiber reinforced silicon carbide porous ceramic material. Staple carbon fibers serve as a three-dimensional reinforcement skeleton, active carbon and phenolic resin serve as a carbon source, and the materials are heated in an argon atmosphere to a silicon melting point and then reacted with silicon powder. Carbon fibers and silicon carbide nanofibers are adopted for toughening and reinforcing porous silicon carbide ceramic, so that porous ceramic has high bending strength and also has certain fracture toughness.

Description

Chopped fiber-SiC nano fiber strengthens carborundum porous ceramics material and preparation method thereof
Technical field
The present invention relates to technology field of ceramic matrix composite material, particularly chopped fiber-SiC nano fiber strengthens carborundum porous ceramics material and preparation method thereof.
Background technology
Porous ceramics is used as the filter of motlten metal owing to having the advantages such as thermal shock resistance, chemical stability and anti-metal erosion.Simultaneously due also to it has, the pressure loss is low, thermostability, resistance to sudden heating and oil smoke collect the characteristics such as efficiency is high so that it is be widely used in a variety of applications in terms of Diesel soot collects filtration;Additionally, owing to its surface is the most uneven, there is a large amount of micropore, when as catalyst carrier, this special microstructure significantly increases biphase contact area, and the time that the highest thermal conductivity can make catalyst reach to react required activation temperature is greatly shortened.Therefore, carborundum porous ceramics also has broad prospects as catalyst carrier;On the other hand can adjust as required due to porosity, the aperture parameters of porous ceramic film material, even obtain the pore structure being interconnected, this makes it become preferable skeletal tissue substitute.
At present, traditional porous ceramics preparation technology mainly has interpolation pore creating material, foam impregnation, foaming and sol-gal process.From complex technical process and prepare product aspect of performance for, it is poor that these methods also exist even air hole distribution, and porosity is low, article shape is restricted, and composition and density are wayward, high simultaneously for ingredient requirement, the shortcomings such as productivity ratio is low, processing performance difference.Therefore, some special preparation methoies are suggested, and mainly have cracking process, solid state reaction sintering process and gas phase reaction infiltration method etc..Wherein containing silicone resin cracking process refers to make organosilane precursor high-molecular gel, obtains the containing silicone resin of cystose after the organic solvent in abjection gel, carries out cracking the silicon carbide ceramics obtaining cystose after fully pre-oxidation;Solid state reaction sintering process is that with Si powder and C powder, foaming agent is uniformly mixed aftershaping, by fusing or vaporization abjection foaming agent, i.e. obtains cystose pottery after pyroreaction sinters;Gas phase reaction infiltration method refers to that silicon gas and porous carbon react preparation perforate SiC material.
No matter taking any technique, the character of porous ceramics is closely related with its pore structure, and Recent study person all concentrate on the functional aspects such as pore-size distribution, porosity and liquid permeation rate to the research of porous ceramics.But, if wanting so that porous ceramics possesses higher combination property, in addition to possessing the functional performance of excellence, in addition it is also necessary to possess preferable structural behaviour.The abatvoix that chemical industry system of Qinhua Univ., Beijing develops can reach the average attraction coefficient of 25%, but its bending strength only has 1.47MPa, this also makes this porous ceramics there is the problem that fragility is bigger, therefore improves the key that its mechanical property is development high-performance porous ceramics under assurance function premise.
Summary of the invention
The present invention needs the technical problem underlying solved to be the structural behaviour significantly improving carborundum porous ceramics so that such material has stronger combination property.For solving this technical problem, the present invention proposes and strengthens carborundum porous ceramics material by carbon fiber and SiC nano fiber, wherein matrix silicon carbide ceramics obtains mainly by silicon-carbon solid state reaction in situ, and SiC nano fiber is then that the reaction of silicon-carbon gas phase generates.
Chopped fiber of the present invention-SiC nano fiber strengthens the preparation method of carborundum porous ceramics material, strengthens skeleton using chopped carbon fiber as three-dimensional, with activated carbon and phenolic resin as carbon source, is heated to more than silicon fusing point and reacts with silica flour in argon gas atmosphere.
In reaction, carbon source is mainly derived from activated carbon powder and cracking carbon, and cracking carbon is obtained by phenolic resin Pintsch process, during Pintsch process, phenolic resin will occur polycondensation reaction, tensile stress can be produced inside it, have a large amount of low-molecular material to release, so that material occurs hole.
Being heated to more than silicon fusing point and silicon in argon gas atmosphere carry out reaction and include the gentle phase reaction of solid state reaction, wherein solid state reaction generates silicon carbide ceramics matrix, and this reaction is the process of a volume contraction.Volume contraction in course of reaction can cause the appearance of material mesopore, thus improves the porosity of material further.Gas phase reaction then generates SiC nano fiber, and the SiC nano fiber of generation is by collaborative chopped carbon fiber, in crackle transmittance process, will by micro-/receive the absorption energy such as spike protein gene, bridge joint, nano net strengthening, improve the architectural characteristic of porous ceramics with this.
As preferred technical scheme, described preparation method, comprise the following steps:
(1) silica flour and activated carbon powder mixing and ball milling are uniformly dispersed, as compound;
(2) dehydrated alcohol and phenolic resin are prepared solution according to mass ratio 1: 0.8, adding chopped carbon fiber and dispersant, being uniformly dispersed adds described compound afterwards and is prepared into suspension, and described suspension shakes in ultrasound wave dispersion, it is dried, is prepared into raw material crude green body;
(3) described raw material crude green body is carried out cured, the compressing rear demoulding for the first time, the crude green body after the demoulding is carried out second time cured and obtains precast body;
(4) described precast body is placed in Vacuum graphite oven, within being evacuated to 10Pa, is warming up to more than silicon fusing point, cools down after insulation 30min.
As preferred technical scheme, in step (1), silica flour is 3~7: 1 with the mass ratio of activated carbon powder, most preferably 5: 1.In silicon-carbon course of reaction, have more remaining C, Si in most cases and exist.At high temperature, remaining C directly affects the intensity of material, does not has the porous ceramics of remaining C to remain to keep the bending under room temperature and compressive strength at 1350 DEG C, has the elevated temperature strength of the porous ceramics of remaining C to be then decreased obviously.The existence of the most remaining Si phase also can make the high temperature microstructure hydraulic performance decline of material, and therefore silicon phase is extremely important with the mass ratio of carbon phase.In the reaction, if silica flour to be allowed (Si) and activated carbon powder (C) occur reaction (Si+C=SiC) completely, then mass ratio is 2.33: 1.But the mass ratio choosing silica flour and activated carbon in the present invention is 3~7: 1.Wherein the purpose of silica flour excess is mainly based upon following 2 points: first is that phenolic resin can be converted into carbon base body in cracking process, and therefore the silicon of excess can react with carbon base body thus generate silicon carbide substrate;On the other hand it is that silicon can evaporate in high temperature environments, silicon steam will react generation SiC nano fiber with carbon generation gas phase during flowing out, therefore the silicon of excess can ensure the generation that gas phase is reacted, thus generates SiC nano fiber, is 5: 1 through being calculated optimal proportion.
As preferred technical scheme, in step (2), at least one in methylcellulose, hydroxyethyl cellulose or sodium carboxymethyl cellulose of dispersant.Three kinds of dispersants are respectively provided with good peptizaiton to chopped carbon fiber.Wherein containing more hydroxyl polar group in its structure of hydroxy ethyl fiber procatarxis, the polar group being more soluble in water and chopped carbon fiber surface forms hydrogen bond or bridging, thus chopped carbon fiber cladding is wherein formed " Nang Bao ", between these " Nang Bao " the most attractive, have again repulsion, under ultrasound wave or External Force Acting, gravitation and repulsion interact, when both reach balance, form metastable class colloidal dispersion system, now chopped carbon fiber in dispersant in ideal dispersion state.As preferred technical scheme, in step (2), compound is 0.5~2: 1 with the mass ratio of phenolic resin;The volume (ml) of dispersant and phenolic resin quality (g) ratio are 2: 1.In order to protect the integrity of chopped carbon fiber in the present invention, use phenolic resin cracking carbon to serve as exhaustion layer, prevent the liquid silicon damage to carbon fiber in high-temperature reaction process with this as far as possible, improve the carbon fiber strengthening and toughening effect for carborundum porous ceramics material.And reaction completely can be occurred (to calculate with the carbon yield of phenolic resin 50% with the silicon of excess so that obtain carbon base body after phenolic resin cracking, optimal proportion is to calculate acquisition according to Si and C with a mole reaction completely), the mass ratio obtaining compound and phenolic resin is 0.5~2: 1, and optimum is 1: 1.
Structural and the functional and chopped carbon fiber distribution of fiber reinforcement porous ceramics has direct affects relation.It is uniformly distributed to obtain aperture size, the equally distributed porous ceramics of chopped carbon fiber.In technical solution of the present invention, add dispersant and prepare suspension, this makes chopped carbon fiber in raw material crude green body in three-dimensional support frame, occur without lamination and dispersion is very uniform, and this dispersing mode improves the technological deficiency of chopped carbon fiber poor dispersion in general open report document.
As preferred technical scheme, in step (2), a length of the 1 of described chopped carbon fiber~2mm;In described suspension, chopped carbon fiber volume content is 5-20%.Wherein chopped carbon fiber optimization polypropylene nitrile carbon fiber, does not has particular/special requirement for its modulus and intensity, can use general purpose grade, high mould level or high intensity level.A length of 1~2mm, if fibre length is the shortest, then fiber is more weak for the toughness reinforcing reinforced effects of ceramic material;If length is oversize, then its dispersibility it is impossible to ensure that, the less stable of structural behaviour.In suspension, the volume content of chopped carbon fiber is 5-20%, if carbon fiber volume content is relatively low, then fiber is for the activeness and quietness DeGrain of ceramic material;And carbon fiber volume content is higher, then carbon fiber disperses uneven in suspension, can reduce the combination property of final material equally.Chopped carbon fiber volume content in the present invention is with 12% for optimum.
As preferred technical scheme, in step (3), condition of cure is 150 DEG C of insulation 5h for the first time, and pressure is 0.5-3MPa, and condition of cure is 200 DEG C of insulation 24h for the second time.In technical solution of the present invention, raw material crude green body is carried out solidification pressurization, with this, pore-size distribution and the density of porous ceramics is regulated and controled.To take different pressure in the present invention, its pressurization scope is 0.5-3MPa.If pressure is the least, then porosity is the highest, and bending strength and fracture toughness are the least;If pressure is excessive, porosity reduces, and its bending strength is higher, but fracture toughness is the least, with 2MPa as optimum.The demoulding after solidification terminates for the first time, carries out second time cured, and solidification process is on the one hand so that the further crosslinking curing of base substrate for the second time, on the other hand can improve the carbon yield of phenolic resin.
As preferred technical scheme, in step (4), heating rate is not more than 5 DEG C/min in 900 DEG C, higher than 5 DEG C/min during higher than 900 DEG C.In technical solution of the present invention, phenolic resin fragmentation pathways and high-temperature reaction process are that a step completes, and this makes the manufacturing cycle of such material be greatly shortened, but want to obtain high performance carborundum porous ceramics, need to control well the rate of heat addition.Within being 900 DEG C due to the major cleavage interval of phenolic resin, in this warm area, phenolic resin generation polycondensation reaction, the internal tensile stress that produces, the releasing of a large amount of low-molecular materials causes hole occur.If heating rate is too fast, internal tensile stress will be caused to discharge in time, so that the phenomenon such as bulge, fragmentation occurs in base substrate, destroy the pore-size distribution of material, reduce the mechanical property of material.If heating rate is the slowest, then can lengthen manufacturing cycle.It is highly preferred that be warming up to 200 DEG C with 5 DEG C/min in described step (4), 2 DEG C/min is warming up to 900 DEG C, is warming up to 1500 DEG C with 10 DEG C/min.
It is 5-10MPa that the present invention also provides for the bending strength of chopped fiber-SiC nano fiber enhancing carborundum porous ceramics prepared by said method, and fracture toughness is 250-500Pa m1/2, porosity is 50-70%.The present invention prepares the enhancing of porous ceramics and strengthens skeleton for chopped carbon fiber and the three-dimensional of SiC nano fiber mutually, use micro-nano multi-scale technology activeness and quietness carborundum porous ceramics, this receives micro-meter scale and nanoscale to strengthen the different advantages of phase to a certain extent, and compensate its defect so that the performance of porous material is more superior and stable.In the present invention, the bending strength of carborundum porous ceramics material is 5-10MPa, and this is higher than general open report.It is about 250-500Pa m simultaneously also by SEN beam method test fracture toughness1/2, and for the fracture toughness of porous ceramic film material, current rarely found open report.
Invention effect
The present invention uses carbon fiber-SiC nano fiber to carry out toughened and reinforced to porous silicon carbide ceramic so that porous ceramics has higher bending strength (5-10MPa), the most also has certain fracture toughness (250-500Pa m1/2)。
The present invention is by controlling the heating rate of different warm area so that cracking and silicon-carbon reaction in-situ one step of phenolic resin complete, and greatly reduce the manufacturing cycle of such material.
The present invention, to there is tensile stress in phenolic resin cracking process, produces loose structure with the release of little molecule, and under high temperature, silicon-carbon reaction is reacted for volume contraction simultaneously, and this makes the porosity of porous ceramics increase further.
The present invention utilize cracking carbon base body and activated carbon provide carbon source; wherein carbon base body can reduce liquid silicon for strengthening the corrosion damage of phase carbon fiber; protect the integrity of carbon fiber so that it is given full play to the carbon fiber toughened and reinforced effect for porous silicon carbide ceramic.
Carbon pasc reaction of the present invention is the gentle phase reaction of solid state reaction, also generates SiC nano fiber while generating silicon carbide ceramics matrix, and the strengthening and toughening of porous ceramic film material will be played certain effect in nano-scale by the generation of nanofiber.
The present invention utilizes dispersant, and prepared by carbon fiber and reaction powder body suspension, and this makes the most scattered three-dimensional enhancing skeleton of carbon fiber, thus avoids the occurrence of lamination, solves the technological deficiency that the fiber dispersion occurred in common technology means is bad.
Accompanying drawing explanation
Fig. 1 is the optics Electronic Speculum figure of raw material crude green body in embodiment 1;
Fig. 2 is the scanning electron microscope (SEM) photograph of prepared carborundum porous ceramics material in embodiment 1;
Fig. 3 is the load-displacement curves figure preparing carborundum porous ceramics material in embodiment 1.
Detailed description of the invention
The present invention is described in detail below in conjunction with embodiment; but the following examples are only the present invention preferably embodiment; protection scope of the present invention is not limited thereto; any those familiar with the art is in the technical scope of present disclosure; according to technical scheme and inventive concept equivalent or change in addition thereof, all should contain within protection scope of the present invention.
Embodiment 1: chopped fiber-SiC nano fiber strengthens the preparation method of carborundum porous ceramics material, comprises the steps:
(1) by 7g silica flour and 2g activated carbon powder (Aladdin reagent) mixing and ball milling, ball milling parameter is 150r/min, and Ball-milling Time is 24 hours, is uniformly dispersed after ball milling after crucible grinds.(2) phenolic resin of about 5g is weighed, the dehydrated alcohol adding about 6.25g is configured to solution, the hydroxyethyl cellulose (mixing speed and the mixing time of dispersant are not construed as limiting by the present invention) of 10ml is added in this liquation, adding the chopped carbon fiber of 0.6g, the length of chopped carbon fiber is about 1mm.Adding the compound obtained in 2.5g step (1) afterwards, be prepared into suspension, in described suspension, chopped carbon fiber volume content is 6%.Said apparatus is shaken in ultrasound wave dispersion, in room temperature environment, is then dried about 24h, prepares raw material crude green body.
(3) being placed in graphite jig by raw material crude green body, be placed on temperature and pressure machine by this graphite jig, be heated to 150 DEG C with the heating rate of 5 DEG C/min, insulation 5h carries out cured for the first time, and the pressure in solidification process is 0.5MPa.Solidification terminates the rear demoulding and processes, and is placed in Muffle furnace by this base substrate, carries out second time cured at 200 DEG C of insulation 24h.
(4) sample that second time solidification terminates is positioned in graphite crucible, this graphite crucible is placed in Vacuum graphite oven, within being first evacuated to 10Pa, heat again, heating process is: with 5 DEG C/min to 200 DEG C, then it is warming up to 900 DEG C with 2 DEG C/min, then is warming up to 1500 DEG C with 5 DEG C/min, furnace cooling after insulation 30min.
Embodiment 2:
The present embodiment is compared with Example 1, the addition of silica flour, activated carbon powder, phenolic resin and dispersant is constant, uniquely change is the addition of chopped carbon fiber, and chopped carbon fiber quality is 1.2g (volume fraction is 12% in suspension) in this embodiment.
Embodiment 3:
Compared with Example 1, the addition of silica flour, activated carbon powder, phenolic resin and dispersant is constant for the present embodiment, and uniquely change is the addition of chopped carbon fiber, and carbon fiber quality is 2g (volume fraction in suspension is 18%) in this embodiment.
Embodiment 4:
Compared with Example 1, the addition of chopped carbon fiber, activated carbon powder, phenolic resin and dispersant is constant for the present embodiment, and the silica flour quality of unique change, silica flour quality is 10g in this embodiment.
Embodiment 5:
Compared with Example 1, the addition of chopped carbon fiber, activated carbon powder, phenolic resin and dispersant is constant for the present embodiment, and the silica flour quality of unique change, silica flour quality is 13g in this embodiment.
Embodiment 6:
Compared with Example 1, the addition of chopped carbon fiber, silica flour, activated carbon powder, phenolic resin and dispersant is constant for the present embodiment, the pressure when first time of unique change solidifies.In the present embodiment, pressure is 1MPa.
Embodiment 7:
Compared with Example 1, the addition of chopped carbon fiber, silica flour, activated carbon powder, phenolic resin and dispersant is constant for the present embodiment, the pressure when first time of unique change solidifies.In the present embodiment, pressure is 2MPa.
Embodiment 8:
Compared with Example 1, the addition of chopped carbon fiber, silica flour, activated carbon powder, phenolic resin and dispersant is constant for the present embodiment, the pressure when first time of unique change solidifies.In the present embodiment, pressure is 4MPa.
Embodiment 9:
Compared with Example 1, uniquely change is the kind of dispersant to the present embodiment, and the dispersant used in the present embodiment is methylcellulose
Embodiment 10:
Compared with Example 1, uniquely change is the kind of dispersant to the present embodiment, and the dispersant used in the present embodiment is sodium carboxymethyl cellulose
With optical microscope, the dispersing uniformity of the chopped carbon fiber in crude green body in embodiment 1 is observed, as shown in Figure 1, can be seen that and prepare suspension through dispersant, in the dried crude green body obtained of concussion dispersion, there is not layering in chopped carbon fiber, disperses the most uniform.
With scanning microscope, the microscopic appearance of the ceramic porous material of preparation in embodiment 1 is observed (as shown in Figure 2), by Fig. 2 (a) can be seen that in material containing more hole, can significantly find out that carbon fiber act as three-dimensional enhancing skeleton simultaneously, dispersion is more uniform, also fills up silicon carbide ceramics matrix between the fibers simultaneously.Amplify this picture further, as shown in Fig. 2 (b), the integrity finding out carbon fiber surface that can become apparent from is preferable, this shows in silicon-carbon course of reaction, liquid silicon is less for the corrosion damage of carbon fiber surface, and fiber maintains a preferable integrity, simultaneously it is also seen that fiber is combined more weak with basal body interface, this also makes this porous ceramics have higher bending strength and fracture toughness, simultaneously the aperture not of uniform size it is also seen that material internal is scattered here and there.Amplify this picture further, as shown in Fig. 2 (c), can be seen that micro-meter scale carbon fiber surface grows a lot of SiC nano fiber, these SiC nano fibers can by extracting, bridge joint etc. carry out energy absorption, so that this porous ceramic film material has higher mechanical property.
Fig. 2 (c) is the displacement-load curves of the ceramic porous material of embodiment 1 preparation, can be seen that this porous ceramics is not brittle fracture when fracture, but become pseudoplastic behavior fracture mode, this should be to there occurs in crackle transmittance process that fiber-bridged, the process such as extract absorb energy to failure, thus cause porous material to present plastic behavior.
Percent opening and mechanical property to embodiments all in the present invention are tested, as shown in table 1.
From embodiment 1-10 it can be seen that in the present invention, the chopped fiber of preparation-SiC nano fiber strengthens the density of carborundum porous ceramics material at 1.7-2.1g/cm3, its porosity is between 50-70%, and bending strength is 5-10MPa;Fracture toughness is 250-500Pa m1/2
Knowable to embodiment 1-3, improve the percent by volume of carbon fiber in carborundum porous ceramics material, its composite density is basically unchanged, and the porosity has and somewhat rises, bending strength reduces simultaneously, the reason that the reduction of bending strength increases mainly due to the porosity, and along with the increase of fiber volume fraction, the fracture toughness of material also improves.
Knowable to embodiment 1,4,5, keeping the content of fiber C, improve the quality of silica flour, its density rises, and percent opening is held essentially constant simultaneously, and bending strength has significantly rising, and fracture toughness is then decreased obviously.In example 4, silicon-carbon mass ratio is complete reaction ratio, and in final composite, remaining silicon is compared little, for not finding in the observation of microscopic appearance that the most remaining silicon is distributed mutually.But room temperature flexural intensity and fracture toughness do not show obvious advantage in this embodiment.This is due under room temperature state, the existence of remaining silicon phase is not clearly for the impact of material mechanical performance, and report according to open source literature, remaining silicon mainly affects high-temperature hot structure and the structure stability of porous ceramics, therefore, the mechanical behavior under high temperature in this embodiment is better than other embodiments.
Knowable to embodiment 1,6,7,8, the inventive method is beneficial to the porosity of porous ceramics, and along with the continuous increase to raw material crude green body pressure, the porosity of porous body reduces, and the bending strength of porous ceramic film material increases simultaneously, and fracture toughness is then decreased obviously.
Knowable to embodiment 1,9,10, the three kinds of dispersants (methylcellulose, hydroxyethyl cellulose or sodium carboxymethyl cellulose) used in the present invention are respectively provided with preferable dispersion effect for chopped carbon fiber, therefore for the physical property (density and percent opening) of porous material and the impact of mechanical property (bending strength and fracture toughness) inconspicuous.Therefore at least one in methylcellulose, hydroxyethyl cellulose or sodium carboxymethyl cellulose of dispersant in the present invention.

Claims (10)

1. chopped fiber-SiC nano fiber strengthens the preparation method of carborundum porous ceramics material, it is characterised in that Strengthen skeleton using chopped carbon fiber as three-dimensional, with activated carbon and phenolic resin as carbon source, be heated in argon gas atmosphere More than silicon fusing point react with silica flour.
Preparation method the most according to claim 1, it is characterised in that comprise the following steps:
(1) silica flour and activated carbon powder mixing and ball milling are uniformly dispersed, as compound;
(2) dehydrated alcohol and phenolic resin are prepared solution according to mass ratio 1: 0.8, add chopped carbon fiber and dispersant, It is uniformly dispersed and adds described compound afterwards and be prepared into suspension, described suspension is shaken in ultrasound wave dispersion, dry Dry, it is prepared into raw material crude green body;
(3) described raw material crude green body is carried out cured, the compressing rear demoulding for the first time, the crude green body after the demoulding is carried out Cured obtains precast body for the second time;
(4) described precast body is placed in Vacuum graphite oven, within being evacuated to 10Pa, is warming up to more than silicon fusing point, protect Cool down after temperature 30min.
Method the most according to claim 1, it is characterised in that in described step (1), silica flour and activated carbon powder Mass ratio is 3~7: 1.
Method the most according to claim 1, it is characterised in that in described step (2), dispersant is fine selected from methyl At least one in dimension element, hydroxyethyl cellulose or sodium carboxymethyl cellulose.
Method the most according to claim 1, it is characterised in that in described step (2), compound and phenolic resin Mass ratio be 0.5~2: 1;The volume of dispersant and phenolic resin mass ratio are 2: 1.
Method the most according to claim 1, it is characterised in that in described step (2), described chopped carbon fiber A length of 1~2mm;In described suspension, chopped carbon fiber volume content is 5-20%.
Method the most according to claim 1, it is characterised in that in described step (3), condition of cure is for the first time 150 DEG C of insulation 5h, pressure is 0.5-3MPa;Condition of cure is 200 DEG C of insulation 24h for the second time.
Method the most according to claim 1, it is characterised in that in described step (4), heating rate is at 900 DEG C Interior no more than 5 DEG C/min, higher than 5 DEG C/min during higher than 900 DEG C.
Method the most according to claim 1, it is characterised in that in described step (4), described intensification is with 5 DEG C / min is warming up to 200 DEG C, and 2 DEG C/min is warming up to 900 DEG C, and 10 DEG C/min is warming up to 1500 DEG C.
10. it is many that the chopped fiber that prepared by method described in claim 1-9 any one-SiC nano fiber strengthens carborundum Hole pottery, it is characterised in that the bending strength of described porous ceramics is 5-10MPa;Fracture toughness is 250-500Pa·m1/2;Porosity is 50-70%.
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CN107010979B (en) * 2017-04-25 2020-08-04 宁波欧翔精细陶瓷技术有限公司 Preparation method of novel carbon fiber reinforced silicon carbide composite material
CN107935614A (en) * 2017-11-30 2018-04-20 北京天宜上佳新材料股份有限公司 Carbon ceramic composite material and preparation method thereof
CN112010654A (en) * 2020-09-11 2020-12-01 航天特种材料及工艺技术研究所 Fiber-reinforced silicon nitride composite material and preparation method thereof
CN113158491B (en) * 2021-05-14 2023-09-12 南京工程学院 Method and device for judging breaking strength limit of ceramic special-shaped micropore, computer equipment and storage medium
CN113158491A (en) * 2021-05-14 2021-07-23 南京工程学院 Ceramic special-shaped micropore damage strength limit judging method and device, computer equipment and storage medium
CN113773094A (en) * 2021-09-30 2021-12-10 中国航发北京航空材料研究院 Method for treating silicon powder for melt siliconizing
CN113773094B (en) * 2021-09-30 2023-12-22 中国航发北京航空材料研究院 Treatment method of silicon powder for melt siliconizing
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CN115493455A (en) * 2022-09-27 2022-12-20 江苏领瑞新材料科技有限公司 High-strength fiber material with bulletproof function and preparation method thereof
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CN115872758A (en) * 2022-12-16 2023-03-31 西安交通大学 BJ3DP printed reaction sintered silicon carbide ceramic and preparation method thereof
CN115872758B (en) * 2022-12-16 2024-03-29 西安交通大学 BJ3DP printed reaction sintering silicon carbide ceramic and preparation method thereof
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