CN102795871A - Method for quickly preparing C/SiC ceramic matrix composite material - Google Patents
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Abstract
The invention belongs to the technical field of preparation of C/SiC ceramic matrix composite materials, and relates to a method for quickly preparing a C/SiC ceramic matrix composite material. By using low-molecular liquid polycarbosilane as a precursor and a carbon fiber prefabricated part as a frame, a pulse-heating chemical solution vapor deposition technique is utilized to quickly prepare the C/SiC ceramic matrix composite material. By adopting the pulse heating mode, the invention can effectively improve the permeation process of the precursor in the chemical solution vapor deposition technique, so that the prepared C/SiC ceramic matrix composite material has uniform density distribution and high density; and meanwhile, the method provided by the invention has the advantages of short production cycle, high utilization ratio of raw materials, low production cost and the like. The process and equipment for preparing the C/SiC ceramic matrix composite material are simple and do not pollute the environment.
Description
Technical field:
The invention belongs to the technical field of C/SiC ceramic matric composite preparation.Being particularly related to a kind of is precursor with the liquid Polycarbosilane of low molecule, and prefabricated carbon fiber spare is a skeleton, and the chemical liquids gas-phase deposition that adopts pulsed to heat prepares the method for C/SiC ceramic matric composite fast.
Background technology:
The C/SiC ceramic matric composite has good characteristics such as low density, HS, H.T., high temperature resistant, anti-thermal shock, high abrasion, resistance to chemical attack, thermal expansivity be low, can be used as high-temperature structural material, thermally protective materials, brake material and is applied to fields such as aerospace, the energy, traffic.Like C/SiC larynx lining, jet pipe and combustion chamber, C/SiC heat exchanger, C/SiC brake flange and brake facing etc.
Traditional C/SiC ceramic matric composite preparation technology mainly is chemical vapor infiltration (CVI) and precursor infiltration and pyrolysis (PIP).CVI technology is the gaseous state precursor that contains Si to be heated to certain temperature and in prefabricated carbon fiber spare, to decompose generate the SiC matrix; PIP technology then is through organic polymer solution or molten mass impregnation of carbon fibers prefab with Si; Behind the dry solidification under inert atmosphere protection Pintsch process, obtain the SiC matrix.In the CVI technological process; Because the gas concentration height that prefab is outside; The outside sedimentation rate of prefab is greater than the sedimentation rate of its inside, causes easily that prefab is outside incrustive phenomenon to occur, need repeatedly process preform surfaces and just can proceed to deposit after its external pores opened; To increase production process like this, and prolong preparation cycle and improve production cost.And PIP technology needs to flood repeatedly because the cracking productive rate of precursor is lower usually---cracking could realize densification more than 10 times, its preparation cycle reached more than 1 month, has greatly increased production cost.
Above-mentioned traditional method for preparing the C/SiC ceramic matric composite receives its process technology limit, is difficult to prepare at short notice the C/SiC ceramic matric composite that cost is low and performance is good.Recently, the method that a kind of chemical liquids vapour deposition/infiltration (CLVD/CLVI) prepared carbon back or ceramic matric composite have occurred.The chemical liquids gas-phase deposition is that prefabricated carbon fiber spare is immersed in the cvd furnace that fills liquid precursor; Adopt the mode of induction heating or resistive heating; Make liquid precursor gasification, cracking generate ceramic matrix and be deposited on prefab inside; Accomplish densification from inside to outside, thereby obtain carbon back or ceramic matric composite.This technology has effectively combined the advantage of successive sedimentation of efficient dipping and the CVI technology of PIP technology; Only need primary depositing just can accomplish the densification of prefab; Therefore, adopt this prepared carbon back or ceramic matric composite can greatly shorten preparation cycle, thereby reduce production costs.But because the existence of prefab internal temperature gradient, the material that finally obtains has certain density gradient from inside to outside, and this will influence performance of composites, thereby limits the application of this technology.Density distribution is even in order to obtain, the better carbon back of performance or ceramic matric composite, and the researchist improves this technology.Be employed in the method for the outer felt of cylindrical preform like (U.S. Pat 5981002) such as Connors,, thereby improve the density in the prefab outside with the thermograde outside reducing in the prefab around lagging material (carbon felt).But because the joule effect of induction heating, carbon felt self also can produce heat and portion's deposition matrix within it, and to get into prefab inner thereby hinder precursor, makes prefab densification fully, and its inboard density is lower than the outside.(Improvement of film boiling chemical vapor infiltration process for fabrication of large size C/C composite such as Wang Jiping; Materials Letters; 2006; 60:1269-1272) the mode through respectively placing a heating element in the top and the bottom of discoid prefab changes the prefab temperature inside and distributes, and makes deposition carry out to middle portion from the two ends up and down of prefab.But; Because the surface action of induction heating, along heating element radially, the temperature in the outside will be higher than inboard temperature; Therefore; Prefab near the heating element Outboard Sections can preferentially deposit, and then hinders the carrying out of prefab top and bottom center portion densification, causes density regions occurring at these positions.(1250 ℃ of Densification behavior and microstructure of carbon/carbon composites prepared by chemical vapor infiltration from xylene at temperatures between 900 and such as Deng Hailiang; Carbon; 2011; 49:2561-2570) then adopt the mode of major and minor heating element that discoid prefab is heated, thereby in thermograde from top to bottom of the inner formation of prefab.But this method can greatly reduce prefab temperature inside gradient on the one hand, makes sedimentation rate slack-off, and sedimentation effect reduces; Owing to temperature distributing disproportionation on the heating element, make the bottom centre of prefab and top edge portion density regions occur on the other hand.
The improvement technology of above-mentioned CLVD all is the improvement to thermograde, improves deposition effect with the mode that reduces thermograde, but will cause prefab inside density regions to occur like this.People such as David (U.S. Pat 6994886) are then improving CLVD technology aspect the infiltration of control precursor in prefab; They are the modes of twining the polytetrafluoroethylene (PTFE) cloth through in the cylindrical preform outside; Restriction gets in the prefab and the precursor liquid of gasification, to reduce energy expenditure and to realize uniform deposition.But when prefab is thicker, reduce to get into the precursor gas concentration that the inner precursor of prefab can reduce its inside part, make its inside part form a unsound zone (sometimes even can form a hollow nuclear) owing to lacking precursor.For avoiding the formation of hollow core, need to reduce densification rate, but will greatly increase preparation time like this.
The problems such as density gradient that occur during to CLVD prepared carbon back or ceramic matric composite; People (Rapid densification of C/SiC composites by joint processes of CLVD and PIP such as Chen Si ' an; Materials Letters, 2011,65:3137-3139) this technology is improved; The mode that the employing staged heats up is improved the process of osmosis of precursor, prepares density distribution C/SiC ceramic matric composite relatively uniformly.But; Because sedimentary at low temperatures speed is lower, sedimentation products can't the inboard fibrous bundle of completely filled prefab between and the hole of carbon cloth interlayer, and at low temperatures the product that obtains of deposition density than deposition at high temperature obtain low; After depositing temperature raises; Sedimentation rate is also accelerated, and prefab inner distance heating element part far away also begins deposition, thereby hinders the inboard further densification of prefab.Therefore, the C/SiC ceramic matric composite that adopts CLVD technology that staged heats up to make, its inboard still exists density regions, and residual porosity is high in the material.
Therefore, need further improve, enable to prepare fast the C/SiC ceramic matric composite that density distribution is even and density is high CLVD technology.
Summary of the invention:
The objective of the invention is to overcome the C/SiC ceramic matric composite that adopts CLVD technology that staged heats up to make; Its inboard still exists density regions; And the residual high defective of porosity in the material provides a kind of densification technology of quick preparation C/SiC ceramic matric composite.It is to be precursor with the liquid Polycarbosilane of low molecule; The prefab of processing with thomel is a skeleton; It is even and density is high to adopt chemical liquids vapour deposition (pulse CLVD) prepared of pulsed heating to go out density distribution; With short production cycle, raw material availability is high, the C/SiC ceramic matric composite that cost is low.
For achieving the above object, the present invention takes following technical scheme to be achieved:
(1) preparation of prefabricated carbon fiber spare: thomel is arranged or weaving manner is processed the unidirectional or three-dimensional prefabricated carbon fiber spare of one dimension with unidirectional, in addition, also can two-dimentional carbon cloth successively be arranged or lamination is arranged+punctured and makes prefabricated carbon fiber spare.The volume integral number average of thomel is controlled at 30～55% in the prefabricated carbon fiber spare.
(2) pulse CLVD prepared C/SiC ceramic matric composite: prefabricated carbon fiber spare placed in the chemical liquids gaseous phase deposition stove that fills liquid low molecular weight polycaprolactone carbon silane precursor solution fully dipping; Then under the protection of rare gas element; Adopt pulse CLVD technology that prefabricated carbon fiber spare is carried out densification, finally make the uniform C/SiC ceramic matric composite of density distribution.Wherein, temperature rise rate is 500～1000 ℃/h, and the time of recurrence interval internal heating is 3～10min, and the time that stops to heat is 10s～3min, and depositing time is 1～8h, and depositing temperature is 1000～1600 ℃.
(3) test specimen mechanical workout: after the process of accomplishing pulse CLVD, the C/SiC ceramic matric composite that obtains is dried by the fire 1～3h down at 150～200 ℃, then base substrate is carried out surface working, obtain ganoid test specimen; After surface working is accomplished,, finally obtain required C/SiC ceramic matric composite if prefab band graphite core is then deviate from core from test specimen.
Compared with prior art; The invention has the advantages that: at first; The present invention adopts the mode of pulse heating to come heating deposition; Can effectively improve the process of osmosis of precursor, make precursor penetrate into the inside part of prefab easily and by product is discharged easily, thereby obtain inside part densification and the uniform material of density distribution; Secondly, the present invention adopts pulse CLVD prepared C/SiC ceramic matric composite can greatly shorten preparation cycle, improves raw material availability, reduces production costs; Once more, the Processes and apparatus of the present invention's technology preparation C/SiC ceramic matric composite is simple, environmentally safe.
Description of drawings
Fig. 1 is the SEM photo of the C/SiC ceramic matric composite for preparing among the embodiment 1;
Fig. 2 is the SEM photo of the C/SiC ceramic matric composite for preparing among the comparative example 1.
Embodiment:
Embodiment 1:
Adopt the C/SiC ceramic matric composite of the present invention's preparation may further comprise the steps:
1, with graphite be core, the two-dimentional carbon cloth that forms with toray product T300 type carbon fiber knit serves as to strengthen body, carbon cloth is wrapped on the cylindrical core processes prefab, and the prefab fiber volume fraction is 30%.
2, be precursor solution with liquid low molecular weight polycaprolactone carbon silane, prefab is flooded in the chemical liquids gaseous phase deposition stove, under argon shield, adopt pulse CLVD technology to carry out densification then, obtain the C/SiC ceramic matric composite.Wherein temperature rise rate is 500 ℃/h, and the pulse heating mode is that every heating 10min stops to heat 3min, and depositing temperature is 1000 ℃, and soaking time is 8h;
3, the C/SiC ceramic matric composite base substrate that makes is incubated 2h down in 180 ℃ and carries out drying, afterwards its outside surface is processed, then the graphite core is deviate from.
Finally making density is 1.91g/cm
3, the uniform C/SiC ceramic matric composite of density distribution.
The comparative example 1:
Adopt the C/SiC ceramic matric composite of the chemical liquids gas-phase deposition preparation of heating continuously may further comprise the steps:
1, with graphite be core, the two-dimentional carbon cloth that forms with toray product T300 type carbon fiber knit serves as to strengthen body, carbon cloth is wrapped on the cylindrical core processes prefab, and the prefab fiber volume fraction is 30%.
2, be precursor solution with liquid low molecular weight polycaprolactone carbon silane, prefab is flooded in the chemical liquids gaseous phase deposition stove, under argon shield, adopt the CLVD technology of heating continuously to carry out densification then, obtain the C/SiC ceramic matric composite.Wherein temperature rise rate is 500 ℃/h, and depositing temperature is 1000 ℃, and soaking time is 8h;
3, the C/SiC ceramic matric composite base substrate that makes is incubated 2h down in 180 ℃ and carries out drying, afterwards its outside surface is processed, then the graphite core is deviate from.
Finally making density is 1.71g/cm
3, the unsound C/SiC ceramic matric composite of inside part.
Therefore, to compare with the comparative example, the density and the homogeneity of the C/SiC ceramic matric composite of the embodiment of the invention 1 preparation have had great improvement.
Embodiment 2:
Adopt the C/SiC ceramic matric composite of the present invention's preparation may further comprise the steps:
1, toray is produced T300 type thomel and be wrapped on the graphite core with unidirectional mode of arranging, make one dimension unidirectional carbon fiber dimension prefab, the prefab fiber volume fraction is 55%.
2, be precursor solution with liquid low molecular weight polycaprolactone carbon silane, prefab is flooded in the chemical liquids gaseous phase deposition stove, under argon shield, adopt pulse CLVD technology to carry out densification then, obtain the C/SiC ceramic matric composite.Wherein temperature rise rate is 1000 ℃/h, and the pulse heating mode is that every heating 3min stops to heat 10s, and depositing temperature is 1600 ℃, and soaking time is 1h.
3, the C/SiC ceramic matric composite base substrate that makes is incubated 1h down in 200 ℃ and carries out drying, afterwards its outside surface is processed.
Finally making density is 1.85g/cm
3, the uniform C/SiC ceramic matric composite of density distribution.
Embodiment 3:
Adopt the C/SiC ceramic matric composite of the present invention's preparation may further comprise the steps:
1, producing T300 type thomel with toray is starting material, adopts the mode of 3 D weaving to make three-dimensional prefabricated carbon fiber spare, and the prefab fiber volume fraction is 45%.
2, be precursor solution with liquid low molecular weight polycaprolactone carbon silane, prefab is flooded in the chemical liquids gaseous phase deposition stove, under argon shield, adopt pulse CLVD technology to carry out densification then, obtain the C/SiC ceramic matric composite.Wherein temperature rise rate is 1000 ℃/h, and the pulse heating mode is that every heating 5min stops to heat 1min, and depositing temperature is 1400 ℃, and soaking time is 3h.
3, the C/SiC ceramic matric composite that makes is incubated 3h down in 150 ℃ and carries out drying, afterwards its outside surface is processed.
Finally making density is 1.89g/cm
3, the uniform C/SiC ceramic matric composite of density distribution.
Claims (1)
1. method for preparing fast the C/SiC ceramic matric composite is characterized in that:
(1) preparation of prefabricated carbon fiber spare: thomel is arranged or weaving manner is processed the unidirectional or three-dimensional prefabricated carbon fiber spare of one dimension with unidirectional, or two-dimentional carbon cloth is successively arranged or lamination is arranged+punctured and makes prefabricated carbon fiber spare;
The volume integral number average of thomel is controlled at 30～55% in the prefabricated carbon fiber spare;
(2) pulse CLVD prepared C/SiC ceramic matric composite: prefabricated carbon fiber spare placed in the chemical liquids gaseous phase deposition stove that fills liquid low molecular weight polycaprolactone carbon silane precursor solution fully dipping; Then under the protection of rare gas element; Adopt the CLVD technology of pulsed heating that prefabricated carbon fiber spare is carried out densification, finally make the uniform C/SiC ceramic matric composite of density distribution; Wherein, temperature rise rate is 500～1000 ℃/h, and the time of recurrence interval internal heating is 3～10min, and the time that stops to heat is 10s～3min, and depositing time is 1～8h, and depositing temperature is 1000～1600 ℃;
(3) test specimen mechanical workout: after the process of accomplishing pulse CLVD, the C/SiC ceramic matric composite that obtains is dried by the fire 1～3h down at 150～200 ℃, then base substrate is carried out surface working, obtain ganoid test specimen; After surface working is accomplished,, finally obtain required C/SiC ceramic matric composite if prefab band graphite core is then deviate from core from test specimen.
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| CN103113123A (en) * | 2013-02-04 | 2013-05-22 | 西安交通大学 | Preparation method of SiCf/SiC ceramic matrix composite turbine blades |
| CN104880351A (en) * | 2015-05-27 | 2015-09-02 | 南京航空航天大学 | One-way ceramic matrix composite plate test piece and preparation method thereof |
| CN106830970A (en) * | 2016-12-20 | 2017-06-13 | 中国人民解放军国防科学技术大学 | SiC ceramic based composite material component and preparation method thereof |
| CN107042661A (en) * | 2016-12-06 | 2017-08-15 | 航天特种材料及工艺技术研究所 | A kind of high temperature heat-resistant protective materials and preparation method thereof |
| CN107602142A (en) * | 2017-08-09 | 2018-01-19 | 湖北航天技术研究院总体设计所 | Integrated integral composite airvane preparation method |
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| CN110066186A (en) * | 2018-01-23 | 2019-07-30 | 航天特种材料及工艺技术研究所 | A kind of C/SiC composite material and preparation method |
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| CN115417684A (en) * | 2022-08-23 | 2022-12-02 | 湖南远辉复合材料有限公司 | Method for preparing SiC-based composite material by melting, impregnating, pressurizing and crosslinking polycarbosilane |
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Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103113123A (en) * | 2013-02-04 | 2013-05-22 | 西安交通大学 | Preparation method of SiCf/SiC ceramic matrix composite turbine blades |
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