CN1850730A - Method for preparing carbon-fiber reinforced silicon carbonate base composite by gas-phase siliconizing technology - Google Patents
Method for preparing carbon-fiber reinforced silicon carbonate base composite by gas-phase siliconizing technology Download PDFInfo
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Abstract
This invention relates to preparation method gas phase siliconizing technique preparing high compact fiber reinforcement SiC group composite material. Protection layer interface is formed on fiber surface through gas phase or liquid phase, then they are dipped and cracked through nm SiC slime to make certain density precast body of fiber reinforcement SiC group. Carbon is added into the body through dipping and cracking way to form group body with certain pore, the group body penetrates inner part of the multi-hole body through gas phase silicon after it is high temperature treated, then it reacts with carbon and fills the pore to get compact basal body. The density of the material can reach 2.25-2.30g/cm3, open porosity is 3-6 percent; it is large more higher than traditional method of getting Cf/SiC material.
Description
Technical field
The present invention relates to the preparation method that a kind of feltwork strengthens ceramic matric composite, or rather, relate to a kind of method of gas phase siliconising prepared dense carbon fiber reinforcement SiC based composites, promptly belong to the reaction sintering technology field.
Background technology
Fiber reinforcement SiC based composites has excellent high-temperature mechanical property, antioxidant property, and improved the shortcoming of the easy sudden failure of stupalith, has strong survivability, thereby the application prospects that has, particularly, have more the potential practical value in fields such as aerospace, national defense and military and new forms of energy.
At present, the preparation method of fiber reinforcement SiC based composites mainly contains chemical vapor infiltration (CVI) method, organic precursors infiltration pyrolysis (PIP) method, hot pressed sintering (HP) and reaction sintering (RS) method.Wherein CVI is relative with the PIP cost higher, and because technology self, the fiber reinforcement SiC based composites that obtains has higher porosity, generally at 10-15%.The existence of these holes for the diffusion of oxygen under the high temperature provides approach, causes the high-temperature behavior of material to be subjected to restricting significantly.Adopt the fiber reinforcement SiC based composites of HP preparation to have higher density, every performance is also better, but is subjected to the restriction of hot pressing form, has strong advantage for the relatively simple material of shape.Yet on large size or complicated shape preparation of devices, the hot pressed sintering practicality is not enough.It is a kind of technology of practicality that reaction sintering prepares fiber reinforcement SiC based composites, and cheap, but nearly all is to concentrate in the mode of liquid-phase silicone to permeate at present.Normally make the silicon fusion under the hot conditions, under wicking action, in porous insert, permeate, form SiC with the C reaction.Thereby in the whole technological process, the infiltration of liquid-phase silicone is very big to the final performance impact of material.People have carried out a large amount of research on the permeable reactive of liquid-phase silicone for a long time, find that its technology controlling and process is difficult, too fast with respect to liquid infiltration speed in the liquid-phase silicone process of osmosis owing to speed of response, it is controlled to make that technology is difficult for, thereby easily stops up preparation and performance thereof that duct, generation defective etc. influence material.For this reason, improve the performance of reaction sintering SiC, effectively reduce reacting phase and be very important for the speed of permeating.
Summary of the invention
The object of the present invention is to provide a kind of gas phase siliconising prepared feltwork to strengthen the method for carborundum based material, its basic ideas are the modes that change traditional siliconising, take place when avoiding entering the duct to stop up to cause defective, make the silicon infiltration process easily controlled.Adopt hot conditions to make the silicon fusing, produce a certain amount of silicon vapor, change the vapor volume size by controlled temperature, thereby control whole siliconising and reaction process.Because molten silicon has certain saturation vapour pressure under the high temperature, by controlled temperature, can form a certain amount of Si steam.Because the silicon vapor amount is less, can control by temperature, whole infiltration and reaction process can be realized by temperature control.And the Si steam enters the duct easily, and liquid-phase silicone is difficult for stopping up the duct relatively, helps the uniform contact of silicon and carbon in the porous insert and reacts, and obtains the dense material of uniformity.
The invention is characterized in the mode that adopts gas phase, elemental silicon is penetrated in the carbonaceous porous matrix with the gas phase form, and reacts with carbon, generate SiC, obtain dense substrate, its technical process as shown in Figure 1.At first, adopt CVI or alternate manner to apply the interface at employed enhancing body fiber surface, its thickness can be determined according to actual needs.Its effect both can be used as protective layer and has avoided fiber corroded by silicon, also can improve fiber and substrate combinating strength, regulated the mismatch degree between fiber and matrix.To be coated with the fiber or the fiber preform at interface then, successively the precursor pulp of the carbon of forming at nano SiC and resin infiltration pyrolysis repeatedly forms the carbon containing porous insert with certain hole.At last, through gas-phase silicon infiltration (as Fig. 2), reaction generates SiC, and and matrix bond, thereby realize that feltwork strengthens the preparation of SiC based composites.
1, the interface applies
Because elemental silicon has stronger erosion action to fiber (as carbon fiber), fibre property is degenerated, finally cause material property to reduce.Facts have proved that the SiC layer has barrier effect preferably to Si, be often used as the interface protective layer of fiber.In order further to improve material property, (pyrolysis C/SiC) n or (BN/SiC) n bilayer or MULTILAYER COMPOSITE interface be used as the interface, with the protection fiber, improve interface bonding state simultaneously.Usually, adopt pulse chemical gas phase permeating technology (CVI) or apply the interface of fortifying fibre through improved pressure pulse chemical vapor deposition method (separate case application), it adopts hydrocarbon compound, trichloromethyl silane (MTS) and BCl
3-NH
3As precursor, obtain PyC (RESEARCH OF PYROCARBON), SiC or BN etc. system in hot conditions and fiber surface uniform deposition.In deposition process, can realize the deposition at multilayer interface by alternately changing gas precursor (as pulse CV I).In addition, or by in resin, Polycarbosilane liquid phase forerunner articles such as (PCS) dipping after cracking obtains the interface.Adopt pulse CV I or force pulse CV I to generate (C-SiC) n or (BN-SiC) temperature 900-1200 ℃ of n MULTILAYER COMPOSITE interface, several kPas to tens kPas of pressure.
2, the preparation of carbon containing porous insert
With the nano SiC powder (～60nm) mix with PCS or resol, pitch etc., wherein SiC content is at 0-70vol.%, PCS resol or pitch are both as the precursor of matrix, simultaneously also as dispersion agent in the slurry and binding agent, its content can be according to the needs of size performance and final required porous structure, in 0-100vol.%, change, make homodisperse nano SiC slurry through ball milling again.
Then, place slurry to flood the bilayer of step (1) coating or the continuous fibre at MULTILAYER COMPOSITE interface, be wound in the synusia of unidirectional array, dry, and with 0 °, 30 °, 45 °, 90 ° or angle changing stacking synusia as required, acquisition has the base substrate that certain orientation is arranged, extrusion forming under the 200-300 ℃ of cold condition, and acquisition has the precast body of certain fibre content.Then, infiltration pyrolysis repeatedly in SiC or resol slurry, final high temperature is handled, the carbon containing porous insert that obtains having certain voidage and void distribution, about 1100 ℃ of cracking temperatures, the pyroprocessing temperature is 1750-1850 ℃ and forms porous insert.
For two-dimensional fiber cloth, directly dipping back stacking in slurry, and low temperature 200-300 ℃ extrusion forming, then, and infiltration pyrolysis repeatedly in SiC or resol slurry, final high temperature is handled, and obtains required carbon containing porous insert; For staple fibre, directly a certain amount of staple fibre is distributed in the slurry, drying and moulding can obtain carbonaceous porous insert; For fibrage bodies such as staple fibre plate or 3D, direct infiltration pyrolysis repeatedly in SiC or resol slurry after interface deposition applies, final high temperature is handled, and obtains having certain voidage carbon containing porous insert.The volume density of carbon containing porous insert is controlled at 1.40-1.55g/cm
3Between, the too low close property of changing of final matrix material that is unfavorable for of density, the too high infiltration that then is unfavorable for gas-phase silicon of density.
3, gas phase siliconising
Silica flour is placed in the plumbago crucible bottom that scribbles BN at inwall one, places the carbon containing porous matrix according to step 2 preparation above silica flour, as Fig. 2.Make the silica flour fusing then under high temperature (1600-1800 ℃) inert atmosphere or the vacuum condition, molten silicon produces certain silicon vapor, is penetrated into the inside of porous matrix, and carbon and silicon react and generates SiC, and volume increases, filling pore.The Si steam becomes elemental silicon in temperature-fall period, remain in the hole dense substrate.Thereby by the control level of response, final matrix mutually can C, Si or the existence of SiC form.
4, the adjustment optimization of performance
Because form difference in the final matrix material, its performance also will have bigger variation.When final residue had C, C became gas under the oxidizing atmosphere, stayed the space, and the diffusion of oxygen supply provides approach, made material property descend.When Si content was higher, material fragility increased, and the material use temperature generally is limited in below 1400 ℃.When existing with the SiC substrate forms, matrix material has the excellent high-temperature performance, and the toughness height.Because the matrix density improves, and has reduced the diffusion of oxygen, makes oxidation-resistance that bigger improvement arranged.So, for obtaining high performance fiber reinforcement SiC based composites, should control content and the voidage of C in the porous insert 1, make that carbon fully reacts, its volume increase is advisable with filling pore.
The present invention's superiority compared to existing technology is:
This process reform in traditional reaction sintering technology liquid-phase silicone infiltration easily stop up the duct, generate shortcoming such as defective because speed of response is too fast with respect to liquid infiltration speed, and technology is difficult for controlled.It produces certain saturation vapour pressure with molten state liquid, at high temperature makes silicon fusing and produce silicon vapor, and uniformly penetrating is to porous insert inside, and generates SiC with the carbon reaction, effectively forms dense material, to reduce hole, the raising material property.
By processing method provided by the invention, make carbon fiber enhancing SiC composite density and reach 2.25-2.30g/cm
3, the clearance gap rate is 3-6% only, is much higher than the C of traditional chemical vapor infiltration method or organic precursors infiltration pyrolysis method gained
f/ SiC matrix material.
Description of drawings
Fig. 1 gas-phase silicon permeable reactive agglomerating process flow sheet;
Fig. 2 gas-phase silicon permeator synoptic diagram; 1-carbon containing porous insert among the figure; The 2-silicon vapor; The 3-molten silicon; The 4-crucible;
The PyC-SiC layer of Fig. 3 fiber surface;
Fig. 4 C
fThe density of/SiC and open porosity are with variation of temperature;
The 3DC of gas phase siliconising preparation during 1700 ℃ of Fig. 5
fThe damage curve of/SiC;
The unidirectional C of gas phase siliconising preparation during 1700 ℃ of Fig. 6
fThe damage curve of/SiC.
Embodiment
The present invention will be further described in conjunction with the embodiments:
Carbon fiber knit is become the 3D knitted body, and the mode (separate case application) that adopts pulse CV I or force pulse CV I is respectively with methane (CH
4) and MTS be the gas phase precursor, at the double-deck interface of C fiber surface deposition pyrolysis C/SiC, its thickness is respectively～150 and～250nm (as Fig. 3).Pyrolysis temperature be 900-1200 ℃ of pressure be several kPas to tens kPas through several seconds to tens seconds.The 3D knitted body with pyrolysis C and double-deck interface with gained is 50vol.% at SiC content successively then, flood in the SiC/PCS slurry of 30vol.% and 0vol.%, and, adopt resin impregnating at last again in 1100 ℃ of cracking, 1800 ℃ of pyroprocessing form porous matrix.Its density is about 1.50g/cm
3, clearance gap rate about 20%.By in placement sample shown in Figure 2 and the graphite carbon pipe furnace, vacuum condition (～1Pa) under, 1600-1750 ℃ of gas phase siliconising sintering 3 hours obtains C
f/ SiC, its density and perforate space are as shown in Figure 4.Can find that in the time of 1700 ℃ behind the gas phase siliconising reaction sintering, its density reaches 2.25g/cm
3, voidage is 6%, is much higher than traditional chemical gas-phase permeation (CVI) or organic precursors infiltration pyrolysis (PIP) method.Zhi Bei C with this understanding
f/ SiC, three-point bending strength reaches 300MPa, shows as non-brittle destruction (as Fig. 5), and remaining silicone content is about 14.5vol.%.
With methane (CH
4) and MTS be the gas phase precursor, the mode that adopts pulse CV I or force pulse CV I is in C fiber surface deposition (C-SiC)
6The multilayer interface, its thickness is about 100nm.Fibrous bundle is put in the nano SiC that SiC content is 50vol.%/PCS slurry floods, be wound in the thin slice of unidirectional array, with 0 ° of stacking, 200-300 ℃ of extrusion forming is then with resol slurry dipping, 1800 ℃ of cracking, obtain porous insert, density is about 1.47g/cm
3, clearance gap rate about 21.6%.Behind gas phase siliconising reaction sintering under 1700 ℃ of vacuum conditions, its density is at 2.31g/cm
3, porosity is 3.1%, three-point bending resistance intensity is 220MPa, shows as non-brittle fracture (as Fig. 6).
Contain two-dimentional carbon cloth and prepare the SiC based composites.
At carbon cloth surface deposition BN/SiC multilayer interface, use BCl
3-NH
3Make presoma with MTS,, adopt pulse CV I or force pulse CV I technology, make coated with multiple layer on the carbon cloth (BN-SiC) interface at 900-1200 ℃.Undertaken by the mode of embodiment 1 then.Obtain similar performance SiC based composites.
The pressure pulse CV I technology that relates in the various embodiments described above is based on pulse CV I technology, it is characterized in that introducing the method for forcing effect of Fluid Pulsation, improves the interface sedimentation rate when remaining on the interface uniform deposition; Concrete technology is the graphite jig upper opening, gas duct is positioned at the graphite jig bottom, in the deposition process of interface, with fiber, fibrage or prefabricated component are placed on graphite jig top, charge into the gas that contains pre-reaction material in the vacuum state downhill reaction device, by the gas deferent gas transport is arrived in the graphite jig of preheating, forced gas is upward through through fiber, fibrage body or prefabricated component, the process several seconds reaches the required pressure of reaction, and maintenance gas residence time in pyroreaction, by vacuum pump gas in the reaction vessel is extracted then, gaseous tension is lower than tens to the hundreds of handkerchief in reaction vessel, in reaction vessel, charge into the gas cycle pulse like this of pre-reaction material once more, reach quick interface deposition.
Claims (8)
1, a kind of method of gas phase siliconising prepared carbon fibre reinforced silicon carbide based composites, it is characterized in that elemental silicon under 1600-1800 ℃ of high temperature, be penetrated in the carbonaceous porous matrix with the gas phase form, obtain the carbon fiber reinforced carborundum based material with carbon reaction in the porous matrix, concrete processing step is:
(a) the carbon fiber interface applies
Adopt pulse chemical gas phase permeating or force pulse gas-phase permeation technology, with hydrocarbon compound, trichloromethyl silane or BCl
3-NH
3Make presoma,, make the interface of C fiber or fibrage body apply bilayer or multiwalled under several kPas to the tens kPas pressure at 900-1200 ℃; RESEARCH OF PYROCARBON/SiC or BN/SiC;
(b) carbon containing porous insert preparation
The interface coated carbon fibers or the fibrage body of step (a) preparation are immersed in nano SiC powder and the Polycarbosilane slurry, and dipping is after 1100 ℃ of cracking again with resol or bituminizing pyroprocessing, repeat repeatedly to form the carbon containing porous matrix at last;
(c) place silica flour in the plumbago crucible bottom, on silica flour, place carbon containing porous matrix according to step (b) preparation, then under 1600-1800 ℃ of temperature, under inert atmosphere or the vacuum condition, molten silicon is penetrated in the porous insert matrix with the gas phase form, carbon and pasc reaction generate SiC, form the carbon fiber reinforced composite material of silicon carbide.
2,, it is characterized in that the volumn concentration 0-70% of carborundum powder in the slurry of nano carborundum powder and Polycarbosilane composition by the method for the described gas phase siliconising of claim 1 prepared carbon fibre reinforced silicon carbide based composites.
3,, it is characterized in that being respectively 150nm and 250nm in C fiber surface deposition RESEARCH OF PYROCARBON and the double-deck interfacial thickness of silicon carbide by the method for the described gas phase siliconising of claim 1 prepared carbon fibre reinforced silicon carbide based composites.
4, press the method for the described gas phase siliconising of claim 1 prepared carbon fibre reinforced silicon carbide based composites, it is characterized in that the bilayer or the multiwalled carbon fiber that are applied by step (a) are the method for continuous fibre material, when it is characterized in that the bilayer that applied by step (a) or multiwalled carbon fiber are continuous fibre, be wound in unidirectional array synusia, dry, and with 0 °, 30 °, 45 °, 90 ° angles or arbitrarily angled stacking synusia, 200-300 ℃ of extrusion forming obtains the carbon containing precast body; Through cracking and pyroprocessing, make the carbon containing porous insert again.
5, press the method for the described gas phase siliconising of claim 1 prepared carbon fibre reinforced silicon carbide based composites, when it is characterized in that the bilayer that applied by step (a) or multiwalled carbon fiber are two-dimensional fiber cloth, then directly in slurry, flood the back stacking, and 200-300 ℃ of extrusion forming, infiltration pyrolysis repeatedly in SiC or resol, pyroprocessing obtains the carbon containing porous matrix.
6, press the method for the described gas phase siliconising of claim 1 prepared carbon fibre reinforced silicon carbide based composites, it is characterized in that: to staple fibre plate or three-dimensional fiber knitted body, direct infiltration pyrolysis repeatedly in SiC/ Polycarbosilane or resol or pitch after the knot face applies, final high temperature is handled and is obtained porous matrix.
7, by claim 1,4,5 or the method for described gas phase siliconising prepared carbon fibre reinforced silicon carbide based composites, it is characterized in that carbon containing porous insert volume density is controlled at 1.40-1.55g/cm
3Between.
8, by the method for the described gas phase siliconising of claim 1 prepared carbon fibre reinforced silicon carbide based composites, it is characterized in that scribbling on the plumbago crucible inwall i layer.
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| CN116143535A (en) * | 2023-03-02 | 2023-05-23 | 中南大学 | Preparation method of carbon/ceramic composite material |
| CN116143535B (en) * | 2023-03-02 | 2024-05-31 | 中南大学 | Preparation method of carbon/ceramic composite material |
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