CN102659441B - Composite structure prestressed tendon reinforced ceramic matrix composite and producing method thereof - Google Patents
Composite structure prestressed tendon reinforced ceramic matrix composite and producing method thereof Download PDFInfo
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Abstract
The invention discloses a composite structure prestressed tendon reinforced ceramic matrix composite and a producing method thereof. The producing method includes weaving fiber bundle tendons and fibers into a prefabricated body or using the fiber bundle tendons alone for producing a rough blank of the fiber reinforced ceramic matrix composite through a chemical vapor infiltration (CVI) method; eliminating end anchorage of the fiber tendons by subjecting the rough blank to grinding or drilling so as to exert prestress on a ceramic matrix; performing molten silicon infiltration under a negative pressure and a high temperature of 1500 DEG C-1600 DEG C to fill a gap between an outer tube and a core rod; enabling the core rod to be stressed; and finally obtaining an end product. According to the composite structure prestressed tendon reinforced ceramic matrix composite and the producing method thereof, flexibility and simplicity of tendon distribution of the fiber bundle tendons are used, the tendons are distributed according to a principle tensile stress trace, stress performance of structural ceramics is improved, toughness and intensity of the ceramic composite are improved, and the problem of early cracking of the matrix of the continuous fiber reinforced ceramic matrix composite is solved. The fiber bundle tendon is characterized by being suitable for a plurality of ceramic producing processes.
Description
Technical field
The present invention relates to a kind of composite structure stress rib that prestores and strengthen ceramic matric composite, the invention still further relates to this composite structure stress rib that prestores and strengthen the manufacture method of ceramic matric composite, remove by the prestore anchoring of stress rib self of composite structure, to ceramic matrix, provide prestress.
Background technology
Stupalith is just because of its high temperature resistant, anti-oxidant, high abrasion, numerous excellent properties such as hardness is large, corrosion-resistant, ultimate compression strength is high, it is ubiquitous making pottery in the world today, it has its irreplaceable contribution and effect in military affairs, civilian industries such as aerospace, machinery, electronics, the energy, yet, the deadly defect of pottery is exactly that fragility is very large, tensile strength is very low, it is responsive especially to defects such as crackle, pore, impurity, has greatly limited its application in various fields.Therefore numerous experts and scholars no sooner has one fallen than another steps into the breach, go to unremitting effort the ceramic fragility of research improvement, improve its tensile strength, the reliability that increases its use extends its length of service, such as by control ceramic grain size, the application phase-change mechanism improve its toughness, at ceramic matrix, add the things such as whisker, enhanced granule toughness reinforcing in addition, but toughening effect is not good, the ceramic matric composite fracture toughness K after toughness reinforcing
iCgenerally be no more than 12MPam1
/ 2and the fracture toughness K of the FRCMC of employing high strength, high tenacity
iCat 20MPam
1/2left and right, the fracture toughness K of the ceramic composite that some continuous fibre is toughness reinforcing
iCcan surpass 30MPam
1/2, so its fracture toughness is compared with proportionality limit stress foregoing toughness reinforcing approach and really is greatly improved
[1].Although as continuous fibre as reinforcement In the view of toughening effect is best at present, but can't resolve its ceramic base strengthened this problem that ftractures too early.
When this material members is stressed, along with load increases, at first ceramic matrix ftractures, and now the stress of fibre reinforcement is very little, and it does not also far reach the intensity of oneself, and not high enough fibre reinforcement is more obvious to those Young's modulus.Have a strong impact on weather resistance, the security of member after the ceramic matrix cracking, so stress performance thereafter is greatly affected.Because its fragility in essence of pottery has still limited the toughening effect of this kind of toughness reinforcing approach greatly, use exactly the fortifying fibre of suitable high elastic coefficient, be also to be difficult to change this kind of inferior position.Do therefore how we change this inferior position? can utilize electrothermal prestressing?
At continuous fibre in toughness reinforcing ceramic composite toughening mechanism, the purpose that reinforcement is introduced is exactly its superior tensile property of performance, bear main tensile stress in member, in order to prevent that matrix from ftractureing too early, why not at composite element, adopt prestressing effect, make in advance ceramic matrix be compressed stress, in composite material shaping process, allow reinforcement to the ceramic matrix precompressed, when ceramic matrix is subject to tension force, must be first surpass the stress under compression added in advance, thereby increased that ceramic matrix is subject to tension force and the dependent variable that ftractures.Utilize like this ultimate compression strength of ceramic super large, made up the fragility of ceramic matrix, well increased toughness, globality, the weather resistance of composite element.
Document
[2]show, in the middle of the design to fibre reinforcement or toughening ceramic, reinforcement and matrix are except chemically having consistency, also compatible physically.Flexible modulus and coefficient of linear expansion aspect physical compatibility, the Young's modulus of reinforcement and matrix will mate, and makes the bullet mould of reinforcement be greater than the bullet mould of matrix as far as possible, and its purpose makes reinforcement stressed exactly.And for the coefficient of linear expansion aspect, the coefficient of linear expansion of reinforcement is greater than the coefficient of linear expansion of ceramic matrix, its purpose is exactly that reinforcement can be brought compressive pre-stress to matrix when the composite material forming temperature is following, is conducive to like this performance of selected whole matrix material.The prestressed method obtained by the swollen coefficient difference of line of material, be called the poor method of coefficient of linear expansion here for the time being.Therefore composite temperature is lower, and reinforcement is just larger to the prestress of ceramic matrix.Continuous Fiber Reinforced Ceramic Matrix Composites mainly adopts carbon fiber at present, and the coefficient of linear expansion of carbon fiber is generally less than 1.1 * 10
-6k
-1below, and the coefficient of linear expansion of pottery is greater than 2.0 * 10
-6k
-1the forming temperature of this matrix material is general over 1000 ℃, this just mean both compound under forming temperature after, when composite temperature during lower than this temperature, carbon fiber will apply tensile stress to ceramic matrix, as long as after temperature drops to a certain degree, the poor thermal stress caused of coefficient of linear expansion surpasses the ultimate tensile stress of ceramic matrix, this matrix material will ftracture, and causes a series of performance reductions such as reliability of material.Such as toray company's T 300 carbon fibers, its axis coefficient of linear expansion is 1 * 10
-6k
-1, intensity is 3.53GPa, Young's modulus is 230GPa
[3].In matrix material, the volume fraction of ceramic matrix and carbon fiber is 1: 1, suppose that ceramic coefficient of linear expansion is 0, when the temperature of matrix material descends 1000 ℃, it is exactly the ceramic matrix compressive deformation not of pressurized, its thermal stress is about 230MPa, only has 6.5% left and right of its intensity, and the precompression therefore applied to ceramic matrix by the poor method of coefficient of linear expansion is too small, the coefficient of linear expansion of ceramic matrix all is greater than 0 still more, and compressive pre-stress is just less like this.Moreover, with the poor prestress that provides of coefficient of linear expansion, this approach be difficult to be controlled, when temperature approaches the composite material forming temperature, its prestress will slowly disappear still more, and the toughness reinforcing or effect of gaining in strength of prestress disappears thereupon.When temperature surpasses the composite material forming temperature, reinforcement will allow ceramic matrix tensile stress occur, accelerates the cracking of matrix, causes composite property to descend.
Have to stupalith other electrothermal prestressing toughness reinforcing and that strengthen: 1, prestress, manufacture one deck compressive stress layer at material surface artificially, in this materials'use process, before ceramic material surfaces is subject to fail in tension, at first must overcome lip-deep residual compressive stress, as toughened glass adopts this method toughness reinforcing, by certain heating, cooling system, introduce artificially residual compressive stress on surface toughness reinforcing, but this method toughening effect is limited; 2, chemical enhanced, as the ion exchange method, when matrix heats up, the small ion in material is replaced to heavy ion, after material cooled, heavy ion is squeezed, and to material, provides precompression, but the residual prestress size in this method is difficult to be controlled
[4]; 3, ceramic/metal is compound, and the method for its prestress constraint stupalith has the metal thermal spraying sedimentation
[5], metal cladding method
[6]deng, by the metallic cover pottery, utilize the coefficient of linear expansion of metal to be greater than good tension and the toughness of ceramic coefficient of linear expansion and metal thereof, provide compressive pre-stress to pottery
[7].Although the method for metallic cover pottery is than being easier to the pottery stress that imposes restriction, the level of its restraint stress is difficult to be controlled.And metal can't bear hot environment.
Method-pretensioning method of and for example applying at prestressed concrete, before the FRCMC moulding, in advance fiber is carried out to stretch-draw, then build the ceramic matrix that structure is combined with fiber, after ceramic matrix solidifies, cancel the stretch-draw to fiber, and then fiber bounces back and gives stress under compression to ceramic matrix.But realize this method and be not easy, again let alone in the environment of high-temperature molding.
Yet, no matter use above-mentioned which kind of method all to be difficult to, according to controlling the required prestress value level of material, can't meet the stressed demand of stupalith.
Along with the development of material science and technology and the improvement of technique, filamentary material intensity and Young's modulus are more and more higher, more than the PAN base carbon fibre tensile strength of producing as toray company has reached 8GPa, the PAN-CF carbon fiber that the trade mark that Hercules company produces is MagnamiteIM7, its ultimate compression strength has reached 8.8GPa
[3].So high-intensity reinforcement like this and Ceramic Composite, if the fiber in matrix material and matrix are in the low or unstress state of stress, ceramic matrix is before cracking so, the fiber of these superstrengths does not basically play a role aspect cracking resistance, thereby, because the ceramic matrix serious cracking affects security, reliability, the weather resistance of member, also cause the very large surplus of fibre strength.Even therefore the fiber of ultra high modulus can not solve this kind of thorny problem, Young's modulus is higher still more, and the toughness of matrix material is poorer, and this problem of ceramic fragility is not still solved.
Summary of the invention
It is large from the stressed dependent variable to destroying that first technical problem to be solved by this invention is to provide a kind of matrix, the appearance of matrix crack is postponed greatly, and the composite structure that the toughness of material, globality, reliability the increase stress rib that prestores strengthens ceramic matric composite.
This second technical problem to be solved is to provide a kind of this composite structure stress rib that prestores of manufacturing and strengthens the method for ceramic matric composite.
In order to solve above-mentioned first technical problem, the composite structure provided by the invention stress rib that prestores strengthens ceramic matric composite, adopt following method to make: become precast body by the fibrous bundle muscle with fibrage or acupuncture or use separately the fibrous bundle muscle to be woven into precast body, during the braiding of precast body, make an end at least wherein of fibrous bundle muscle be in the position of being convenient to cutting and prestress release, by chemical vapor infiltration (CVI), make the thick embryo of ceramic matric composite, or employing precursor conversion process, hot-pressing sintering technique, chemical vapor infiltration, perhaps these three kinds of process integrations are used, then by the method that the thick embryo of ceramic matric composite is carried out to grinding or boring, remove the end anchorage of fibrous bundle muscle self, the interface cohesive action of fibrous bundle muscle and matrix applies compressive pre-stress to ceramic matrix, carry out subsequently 1500 ℃～1600 ℃ negative pressure high-temperature fusion and soak the gap that silicon is filled outer tube and plug, but or the gap of the thermosetting resin of employing carbonization filling outer tube and plug, plug is participated in stressed, finally make finished product, perhaps plug is taken out, then adopt chemical Vapor deposition process or negative pressure high-temperature fusion to soak silicon plug-hole, then moulding.
In order to solve above-mentioned second technical problem, the manufacture composite structure provided by the invention stress rib that prestores strengthens the method for ceramic matric composite, the fibrous bundle muscle become to precast body with fibrage or acupuncture or use separately the fibrous bundle muscle to be woven into precast body, during the braiding of precast body, make an end at least wherein of fibrous bundle muscle be in the position of being convenient to cutting and prestress release, the volume fraction of fibrous bundle muscle is made in the required calculation of Prestress of matrix material, the volume fraction scope of fibrous bundle muscle is 3～60%, above-mentioned precast body is put into to chemical vapour infiltration/cvd furnace, manufacture the SiC based composites, depositing temperature is 1000 ℃～1100 ℃, vacuum keep is at 50～500Pa, the gas flow of unstripped gas is 180～220L/min, shielding gas adopts Ar gas, flow is got 180～220L/mi n, depositing time is 8～12 days for the first time, the time of the reaching component surface of taking out and polish, open its hole and continue deposition for the second time, within 8～12 days, take out afterwards, complete the thick embryo of ceramic matric composite manufacturing process, then the thick embryo of ceramic matric composite is carried out to prestress release type manufacturing procedure, if plug does not need to take out, this operation can beginning from having deposited for the first time, complete after prestress release type manufacturing procedure by 1.2～1.5 times of the required Si amount of theory, adding the Si micro mists, its Powder Particle Size is 10～100 μ m, the thick embryo of Si powder and ceramic matric composite is placed in plumbago crucible grinding line face is contacted with Si, it is to carry out melting in 1500～1600 ℃ of negative pressure High Temperature Furnaces Heating Apparatuss (being filled with the pressure-fired of 0～500Pa of Ar gas) to soak the gap that silicon carries out outer tube 3 and the plug 4 of fiberfill fibers bundle muscle that plumbago crucible is placed in to temperature, be incubated 1.5～2.5 hours, perhaps at the outer tube 3 of fibrous bundle muscle and the gap of plug 4, add the presoma material Pintsch process of carbon to fill gap, perhaps plug is taken out, adopt again chemical Vapor deposition process or negative pressure high-temperature fusion to soak the silicon plug-hole, to obtain subsequently the C/SiC matrix material and carry out mechanical workout, finally obtain finished product.For take the unstripped gas that SiC uses as matrix CVI, be CH
3siCl
3+ H
2, for take the unstripped gas BCl/BF+NH that BN uses as matrix CVI
3+ H
2, with Al
2o
3the unstripped gas AlCl used for matrix CVI
4+ CO
2+ H
2, with TiB
2the unstripped gas TiCl used for matrix CVI
4+ BCl
3+ H
2.
Described prestress release type manufacturing procedure refers to along the grinding line of the thick embryo of ceramic matric composite carries out grinding, and the cutting zone of worn fibrous bundle muscle discharges the prestress of fibrous bundle muscle, or takes boring method to discharge prestress to the thick embryo of ceramic matric composite.
The manufacture method of described fibrous bundle muscle is:
The first step, manufacture plug, plug adopts the pultrusion production technique, fiber adopts at the PAN of 2000 ℃ of left and right carbonizing treatment base carbon fibre, or employing asphalt series or cellulose-based carbon fiber, shaping medium precursor substance in the glue groove adopts resol and ethanol to press the weight ratio mixing solutions of 1: 1, or the polymkeric substance of the high carbon residue rate of employing polyether-ether-ketone, perhaps adopt Polycarbosilane (PCS) solution, or the solution that adopts polyvinyl alcohol and warm water to mix by the weight ratio of 1: 5, fiber is curing molding in mould, then in a vacuum, under 1500～2100 ℃, 1 hour high temperature graphitization of heating is processed,
Second step, fibrous bundle muscle precursor is by the pultrusion production technique, fiber adopts at the PAN of 1500 ℃ of left and right carbonizing treatment base carbon fibre, shaping medium precursor substance in the glue groove adopts resol and ethanol by 1: the weight ratio mixing solutions, at first be wound around polytetrafluoroethylene film on the plug finished product, then hoop is wound around fiber by winding wheel, the fiber that another group is soaked into glue enters the mold cured moulding through preformed board with plug, make the fiber bar precursor, and fiber enters, the mode of mould is braiding, canoe enters; Be wound around fiber at the place, two ends of fiber bar precursor if necessary, form termination and increase, be convenient to the stretch-draw of follow-up outer tube.Then by forming material in a vacuum, first be heated to 300 ℃ of heating and make the preliminary carbonization of resol, then under 1000 ℃～1500 ℃, heat 1 hour, make the further carbonization of resol, in being heated to 400 above temperature courses, polytetrafluoroethylene film cracking gradually disappears, thus the outer tube moulding, and have gap with the plug in it;
The 3rd step, by to fibrous bundle muscle precursor outer tube, stretch-draw enters, clamp the outer tube end with the anchoring ring, the stretch-draw outer tube, outer tube extends, and then keeps the tension stress of outer tube, and between the outer tube mouth of pipe and plug end face the filling binding agent, the hot setting binding agent, the stretch-draw of then unclamping outer tube, this fibrous bundle muscle end anchorage adopts resol (PF)/norbide (B with binding agent
4c) hot setting adhesive, but or the thermosetting resin of employing carbonization, at 300 ℃～1000 ℃, be heating and curing, then unclamp stretch-draw and make the fibrous bundle muscle.
In above-mentioned second step, in film, add in advance graphite microparticles as lubricant.
In above-mentioned second step, excessive too much and prevent that the gas of follow-up CVI method from entering the gap of outer tube and plug for the carbonization space that prevents outer tube, add ceramic in the glue groove, as the SiC micro mist, contraction and the space of minimizing carbonization process.
In above-mentioned second step, outside surface painting resol carbonization at outer tube, repeat this process, prevents that the gas of follow-up CVI method from entering the gap of outer tube and plug.
Adopt the composite structure of the technique scheme stress rib that prestores to strengthen ceramic matric composite and manufacture method thereof, the composite structure stress fiber bundle muscle that prestores is under the jurisdiction of prestore a kind of in stress rib of composite structure, for convenience of description, be called for the time being the fibrous bundle muscle below.The structure of fibrous bundle muscle of the present invention is that by resistant to elevated temperatures binding agent, at two ends, anchoring forms by the fibrous bundle outer tube of high-temperature molding, fibrous bundle plug, and the plug that wherein bears pressurized in the outer tube of stretching force and its abdomen forms the tension and compression balanced body.Detailed explanation is arranged in the file that the structure formation of fibrous bundle muscle is 201110383561.0 at application number, repeat no more.The application of fibrous bundle muscle has increased the property easy to control of handiness, simplicity and the prestress release thereof of prestressed layout, and considerable prestress value can be provided.For example, the outer tube that adopts T300S carbon fiber (tensile strength is 4.8GPa) and the fibrous bundle muscle that adopts T300S carbon fiber (ultimate compression strength is 6.1GPa) be the above stress of exportable 1.5GPa roughly.Owing to can manufacturing the fibrous bundle muscle that diameter is less (diameter can be less than 1mm), soft and flexible, can be according to the ceramic composite stressing conditions, carry out the cloth muscle by the principal tensile stress trace, improve so better the stress performance of structural ceramics, increase toughness and the intensity of ceramic composite.Again because this prestress is subject to influence of temperature change very little in the materials'use temperature range, thereby well solve in the past prestressing technique in the insoluble problem of porcelain based composites.Mainly illustrate about being applied to the manufacture method of the fibrous bundle muscle in the high-temperature-resistant structure pottery in literary composition of the present invention, adopt some ceramic matric composite moulding process, make this muscle and Ceramic Composite, then by prestress method for releasing and follow-up moulding process thereof.
During due to the ceramic matric composite moulding, temperature generally reaches more than 1000 ℃, at so high temperature, must select can anti-this high temperature filamentary material, and the fibrous bundle muscle that contains this fiber is under high temperature and high-stress state, can not cause prestressed loss, thereby just have enough prestress to be transferred to ceramic matrix after self anchoring of removing the fibrous bundle muscle.Therefore at high temperature must meet mechanical property requirements at the medium of selecting outer tube and plug filamentary material used and their moulding, with matrix chemically and also all compatible physically.Filamentary material in outer tube and plug can be selected carbon fiber on selecting at present, more than its intensity reaches as high as 8GPa, in inert atmosphere, is exactly under high temperature more than 2000 ℃, still has the intensity in the room temperature situation; Can select the SiC fiber, its intensity reaches as high as 3.5GPa, and use temperature can reach 1300 ℃, and maximum operation (service) temperature is at 1400 ℃; Can select Al
2o
3fiber, its intensity reaches as high as 3GPa, its intensity in air, be heated to 1000 ℃～1100 ℃ basically constant; Can select the B fiber, its intensity reaches as high as 3.5GPa, and its high temperature resistant property is also fine; Also have the ceramic fiber of other a lot of high temperature resistance and high strengths available.The method that fiber and medium are made outer tube and plug in the present invention adopts soaks into the method that then precursor substance heats---precursor conversion method.But, in the combination of fiber and bunchy medium, preferably adopt the matched combined of oxide compound and oxide compound, or non-oxidized substance and non-oxidized substance matched combined.If oxide compound becomes outer tube or plug with the non-oxidized substance matched combined, because the temperature of reaction of the Composite processes such as the cracking follow-up or sintering is very high, react very strong between oxide compound and non-oxidized substance, very likely cause fibrous bundle characteristic variation, thereby its stress performance descends.If really need such combination, the little composition of coating BN isoreactivity on fiber surface, can prevent the reaction of this fierceness to a certain extent in advance.Except aforesaid method, outer tube and plug can also adopt slurry or the chemical gas phase impregnating manufacture method of steeping medium composition
[9].
The outer tube of making for fiber and medium is except high temperature resistant, and it should have higher tensile strength and certain Young's modulus, and the stress rib that prestores of unit volume can store more energy of deformation like this, and base material just can obtain larger prestress.The intensity of outer tube and Young's modulus are heated rear impact need be little, and the intensity of the temperature section when room temperature and forming materials and elastic modulus change need less.In the mandrel material consisted of fiber and medium is selected, plug is except high temperature resistant, intensity and the elastic modulus change of the temperature section when room temperature and forming materials should be less, also need higher ultimate compression strength, the Young's modulus of its material is also high than the Young's modulus of outer tube material, the reduction of stress when the tension and compression deformation that can reduce like this outer tube and plug shrinks, thus prestressed reserves increased.In anchoring is selected with binder material, the high temperature while at first wanting anti-composite material forming, should have higher intensity and Young's modulus after solidifying, and its intensity is enough to resist the shearing of tension and compression body when normal operation, and can be with outer tube and plug reaction.Therefore, anchoring can be selected high-temperature inorganic adhesive, resol (PF)/norbide (B with binding agent
4c) hot setting adhesive
[10]but and the resin material of high temperature cabonization.The outer tube filamentary material can be chosen at carbon fiber after 1500 ℃ of left and right carbonizing treatment, and its tensile strength can reach maximum value.Along with carbonization temperature raises, intensity can reduce, but Young's modulus increases, and more than 2000 ℃, thermal treatment can obtain higher Young's modulus, so plug can be taken at the carbon fiber of temperature carbonization more than 2000 ℃
[11].The medium that forms outer tube and plug can adopt resol or Polycarbosilane to carry out Pintsch process, by the continuous fibre bunchy that bonds.
In selection, prepare on the method for FRCMC equally, if select the too high method of mold temperature, the strength and stiffness of fibrous bundle muscle and anchoring bond agent cohesive strength all can descend, certainly will affect the fibrous bundle muscle to the prestressed release of ceramic matrix, cause the excessive loss of prestress, and affect the performance of matrix material.Therefore the present invention considers to adopt the CVI method, and it can, under the temperature environment of 900～1100 ℃, make high-compactness and highly purified SiC pottery, chemical equation
[12]:
The carbon fiber of making due to the CVI method strengthens the SiC based composites under 1000 ℃ of hot environments, with the normal temperature state, compares, and its strength and stiffness remain unchanged
[13]thick embryo is carried out to grinding or boring, destroy the anchoring in the end anchorage district of fibrous bundle muscle self, after applying compressive pre-stress to ceramic matrix, carry out under 1000 ℃ of left and right high temperature again that chemical vapor infiltration is long-pending, high temperature negative pressure infiltration or infiltration resin high temperature cabonization fill outer tube and plug gap operation, the prestress that this operation can not apply to the SiC base outer tube causes damage, and then can be to carbon fiber exposed area and outer tube and bold being covered and filling of plug gap location.Equally, the SiC/SiC based composites that the CVI method is made is under 1000 ℃ of hot environments, and strength and stiffness change less, therefore in the long-pending filling work procedure of chemical vapor infiltration, little on the impact of loss of prestress aspect.
Consider that the fibrous bundle muscle belongs to the structure that slenderness ratio is very large, strut buckling destruction problem needs demonstration.For the tension and compression structure of fibrous bundle muscle, outer tube is pull bar, and plug is depression bar, although outer tube and plug slenderness ratio are very large, i.e. whether large flexibility rod member, can this problem of unstable failure, below does simple answer.Because the prerequisite of strut and tie unstable failure is under the critical load of unstability, pull bar will start to separate with depression bar stressed axis separately, and when load surpasses critical load, both stressed axis distance of separations are just increasing, until strut and tie destroys.And, in fibrous bundle muscle tension and compression structure of the present invention, due to plug, just at the intraperitoneal of outer tube, after both are stressed, be exactly while approaching their ultimate value of intensity, as long as both stressed axis can not separate, the tension and compression structure just not there will be unstable failure.Unless outer tube generation explosion, the plug pressurized is extruded, and causes unstable failure; Perhaps outer tube causes unstable failure with plug de-glutinous the separation.As long as therefore allow outer tube, in the body circumferential direction, sufficient intensity is arranged, just not there will be because of the unstable failure situation; Perhaps outer tube enough separates by force and not with the cohesive force of plug, also not there will be because of the unstable failure situation.Although fibrous bundle muscle structure can unstable failure, if but the excessive clearance on outer pipe internal surface and mandrel outer surface, when both pressure axis spaces are excessive, causes the eccentricity of outer tube and plug excessive, certainly will cause certain eccentric force to make the outer tube bending, unfavorable to some extent to the cloth muscle like this.Therefore when manufacturing the fibrous bundle muscle, the diameter of outer tube diameter and plug will match.If the excessive clearance of outer tube and plug, cause the excessive bending of fibrous bundle muscle, and affect its use properties.If gap is too small, at outer tube, be subject in stretching process, internal diameter diminishes, cause outer pipe internal surface to contact or push with mandrel surface, frictional force increases, thereby drive plug, is subject to stretch-draw, cause the specific elongation between outer tube and plug poor not, do not reach the prestressed set(ting)value of fibrous bundle muscle.Therefore the internal-and external diameter of outer tube and the diameter of plug must calculate in advance and set, and avoid the appearance of the problems referred to above.
In the file that the manufacture method of fibrous bundle muscle is 201110383561.0 at application number, had illustrated, such as penetrate method: " a kind of manufacture method in the stress rib that prestores that the 3rd class formation forms: plug is penetrated to outer tube; to the gap of outer tube and core rod end, inject a certain amount of binding agent; the stretch-draw outer tube; reach default stress value, and keep this stress value.To be bonded dose solidify after, the stretch-draw of unclamping outer tube, complete manufacture." its outer pipe manufacturer is to become pipe by sloughing core after pultrusion, is applicable to the smaller outer pipe manufacturer of major diameter, but when outer tube diameter less with and length when longer, the method that penetrates that plug is penetrated to outer tube is just pretty troublesome.Therefore the present invention adopts new manufacture, at first manufactures plug, and by the fibrous bundle by the dip-coating resin medium, through the forming hole pultrusion, then Pintsch process becomes the fibrous bundle plug.Be coated with or be wound around the volatilizable resin of one deck high temperature and solidify at mandrel surface, then directly take it as core, by winding and pultrude process, manufacturing outer tube, being placed on subsequently cracking moulding under high temperature.Because plug is in pipe, without poling, available tensioning equipment stretch-draw outer tube, reach default stress value, and keep this stress value, and the tube end place, squeeze and fill out binding agent outside, heats up and solidify, and after reaching intensity, unclamps the stretch-draw of outer tube, completes manufacture.
Aspect the outer tube control stress for prestressing, as described in Example 1, control the control stress for prestressing σ of outer tube
con≤ 0.65f
pk(f
pkstandard tensile strength for the carbon fiber outer tube), plug pressurized proof stress σ
con≤ 0.7f
pk(f
pkstandard ultimate compression strength for the carbon fiber outer tube).Outer tube should equate with the section area of plug as far as possible, and its end anchorage length is determined according to the required stress calculation of anchoring.At the diametrically of fibrous bundle muscle, its diameter range is generally at 0.1～5mm, if the too small difficulty of manufacturing that increases of diameter, the excessive unsuitable cloth muscle of diameter, so the diameter of fibrous bundle muscle is wanted suitably.
Compared with prior art, the invention has the advantages that: the present invention can increase matrix from the stressed dependent variable to destroying by matrix, applying compressive pre-stress, has greatly postponed the appearance of matrix crack, thereby has increased toughness, globality, the reliability of material.The fibrous bundle muscle of making in the present invention is self-balancing system because of it, therefore crooked in its elastic range, its sinuousness is relevant with himself diameter and rigidity, and diameter and rigidity are less, flexible is just better, therefore greatly facilitates prestressed control, enforcement and layout.Due to prestressed existence, the toughness reinforcing method with strengthening of prestress of the present invention unrelieved stress toughness reinforcing and that Enhancement Method is different from the past, present method obviously is better than the latter, and its stress value is not subject to the impact of temperature rise, it can be by increasing the first toughness of CMC (FRCMC) than the high-intensity fibrous bundle muscle of low modulus, prevent the too early cracking destruction of matrix, thereby increase greatly globality, the safety and reliability of material.
The present invention is applicable to the structure unit that aerospacecraft, nuclear reactor wall, combustion gas turbine burner etc. require high strength, high rigidity, high temperature resistant and high temperature resistance thermal shock, is applicable to gun barrel, panzer, spacecraft, cylinder of internal-combustion engine, braking equipment etc. and requires high strength, high rigidity, high temperature resistant and shock proof structure unit.
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[12] beneficial little Su, Du Shanyi, Zhang Litong. Chinese material engineering grand ceremony: the 10th volume composite material engineering, 2006:610
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[15] Yang Mingbo, Tang Zhiyu. the grand ceremony of Chinese material engineering: the 7th volume macromolecular material engineering (under), 2006
The accompanying drawing explanation
Fig. 1 is that the plug pultrusion is produced schematic diagram;
Fig. 2 is that fibrous bundle muscle precursor pultrusion is produced schematic diagram;
Fig. 3 is that the fibrous bundle muscle is manufactured schematic diagram;
Fig. 4 is fibrous bundle muscle three-dimensional preformed body schematic diagram;
Fig. 5 is turbine ceramic blade fibrous bundle muscle cloth muscle schematic diagram;
Fig. 6 is turbine ceramic blade schematic diagram;
Fig. 7 is Nozzle of Liquid Rocket Motor cloth muscle schematic diagram;
Fig. 8 is the Nozzle of Liquid Rocket Motor schematic diagram;
Fig. 9 is without latitude fibrous bundle muscle layer schematic diagram;
Figure 10 is engine jet pipe adjustment sheet schematic diagram.
In the drawings:
The 1-high modulus fibre; The 2-high strength fibre; The 3-outer tube; The 4-plug; The 5-binding agent; 6-fibrous bundle muscle; The 7-space of stretching; 8-wavy fiber bundle muscle; 9-straight line fibrous bundle muscle; 10-grinding line; The 11-grinding area; The 12-blade; 13-dovetail attachment portion; The 14-root of blade; 15-derotation spiral fiber bundle muscle; 16-dextrorotation spiral fiber bundle muscle; The 17-jet pipe, creel 18, preforming mould 19, the first moulds 20, reciprocating traction device 21, the first glue grooves 22, polytetrafluoroethylene film 23, the second glue groove 24, the second moulds 25, cutting machine 26, preformed board 27, winding wheel 28, fiber bar precursor 29.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further elaborated.
Embodiment 1:
At first the manufacture method of plug 4 is described.The manufacture of plug 4 adopts pultrusion production technique as shown in Figure 1, Fig. 1 is: creel 18, preforming mould 19, the first mould 20, reciprocating traction device 21, the first glue groove 22, high modulus fibre 1 adopts at the PAN of 2000 ℃ of left and right carbonizing treatment base carbon fibre, shaping medium precursor substance in the first glue groove 22 adopts resol and ethanol to press the weight ratio mixing solutions of 1: 1, curing molding in the first mould 20, then in a vacuum, 1 hour high temperature graphitization of heating is processed under 1800～2100 ℃.In this course, the radical of the carbon fiber used by change, change the diameter of plug 4.The content of the carbon medium of the plug 4 obtained in this way, no matter the size of diameter is all approximately about 60% (volume).Shaping medium precursor substance in the first glue groove 22 can also adopt the polymkeric substance of the contour carbon residue rate of polyether-ether-ketone, or adopts Polycarbosilane (PCS) solution, and both are equally applicable to the medium of outer tube 3 described below.
As shown in Figure 2, fibrous bundle muscle precursor is by the pultrusion production technique, Fig. 2 is: the second glue groove 24, polytetrafluoroethylene film 23, the second moulds 25, cutting machine 26, preformed board 27, winding wheel 28, fiber bar precursor 29, fiber adopts at the PAN of 1500 ℃ of left and right carbonizing treatment base carbon fibre, and the shaping medium precursor substance in the second glue groove 24 adopts resol and ethanol to press the weight ratio mixing solutions of 1: 1.At first be wound around polytetrafluoroethylene film 23 on plug 4 finished products, the internal diameter varies amount of the thickness of polytetrafluoroethylene film 23 after by outer tube 3 stretch-draw and the shrinkage of outer tube 3 cracking are carried out calculative determination.Then hoop is wound around high strength fibre 2 by winding wheel 28, the high strength fibre 2 that another group is soaked into glue enters the second mould 25 curing moldings through preformed board 27 with plug 4, making fiber bar precursor 29, can be that the modes such as braiding, winding enter and high strength fibre 2 enters the mode of mould.If necessary can be before fiber bar, 29 place, two ends is wound around fiber, forms termination and increases, and is convenient to the stretch-draw of follow-up outer tube.Then by forming material in a vacuum, first be heated to 300 ℃ of heating and make the preliminary carbonization of resol, then under 1000 ℃～1500 ℃, heat 1 hour, make the further carbonization of resol, be heated to more than 400 ℃ in temperature course, polytetrafluoroethylene film 23 cracking gradually disappears, thus outer tube 3 moulding, and have gap with the plug 4 in it.Stretch-draw and the prestressed release of fibrous bundle muscle 6 for the ease of follow-up outer tube 3, can add graphite microparticles as lubricant 23 li of polytetrafluoroethylene films in advance.For the carbonization space that prevents outer tube 3 excessive too much and the gas that prevents follow-up CVI method enter the gap of outer tube 3 and plug 4, can in the second glue groove 24, add ceramic, as the SiC micro mist, reduce contraction and the space of carbonization process.Can also be coated with resol carbonization at the outside surface of outer tube 3 if necessary, repeat this process, the gas that prevents follow-up CVI method enters the gap of outer tube 3 and plug 4, avoids both fixed of outer tube 3 and plug 4, thereby increases the reliability that fibrous bundle muscle 6 prestress discharge.
As shown in Figure 3, by to fibrous bundle muscle precursor outer tube, stretch-draw enters as the manufacturing process in Fig. 3, by to fibrous bundle muscle precursor outer tube, 3 stretch-draw enter, clamp outer tube 3 ends with the anchoring ring, stretch-draw outer tube 3, be outer tube 3 elongations, then the tension stress that keeps outer tube 3, and between outer tube 3 mouths of pipe and plug 4 end faces the filling binding agent, the hot setting binding agent, then unclamp the stretch-draw of outer tube, form flexible space 7 between outer tube 3 and plug 4, this fibrous bundle muscle end anchorage adopts resol (PF)/norbide (B with binding agent 5
4c) hot setting adhesive, be heating and curing at 300 ℃～1000 ℃, then unclamps stretch-draw and make fibrous bundle muscle 6.The control stress for prestressing σ of outer tube 3
con≤ 0.65f
pk(f
pkstandard tensile strength for the carbon fiber outer tube), plug 4 pressurized proof stress σ
con≤ 0.7f
pk(f
pkstandard ultimate compression strength for the carbon fiber outer tube).Outer tube 3 should equate with the section area of plug 4 as far as possible.This fibrous bundle muscle end anchorage length is determined according to the required stress calculation of anchoring.
Wherein H2 is carrier gas and diluent gas, approximately 24 ℃ of raw material gas tank temperature, and gas flow is made as 200L/min, and shielding gas adopts Ar gas, and flow is got 200L/min, and depositing time is 10 days for the first time.The time of the reaching component surface of taking out and polish, open its hole and continue deposition for the second time, within 10 days, takes out afterwards, complete coarse-blank manufacturing process.If the density of not meeting the requirements of, can repeat the density of CVI method and reach design requirements.Then need thick embryo member is carried out to prestress release type manufacturing procedure.If plug does not need to take out, this operation can beginning from having deposited for the first time.The thick embryo that precast body shown in Fig. 4 is made, carry out grinding to its any non-parallel three faces, the cutting zone of worn fibrous bundle muscle, the prestress of release fibrous bundle muscle.Then to 1.2 times of interpolation Si micro mists by theoretical required Si amount, its Powder Particle Size is 10～100 μ m, and Si powder and thick embryo are placed in plumbago crucible.It is to carry out melting in 1500～1600 ℃ of negative pressure High Temperature Furnaces Heating Apparatuss to soak the gap that silicon is filled outer tube 3 and plug 4 that plumbago crucible is placed in to temperature, or molten silicon infiltration in the pressure-fired High Temperature Furnaces Heating Apparatus of the 100Pa left and right that is filled with Ar gas, is incubated 2 hours.To obtain subsequently the C/SiC matrix material and carry out mechanical workout, finally obtain finished product.If the matrix material of demand heat-proof quality, can take out all plugs 4, two stomidiums that then carry out the stifled outer tube 3 of upper method get final product, and form hollow composite.For one dimension or the thick embryo of two-dimentional precast body, can also take boring to discharge prestressed method.
For take the unstripped gas BCl/BF+NH that BN uses as matrix CVI
3+ H
2, with Al
2o
3the unstripped gas AlCl used for matrix CVI
4+ CO
2+ H
2, with TiB
2the unstripped gas TiCl used for matrix CVI
4+ BCl
3+ H
2can adopt method as above.The one dimension be compiled into fibrous bundle muscle 6 or two-dimentional precast body, can carry out equally above-mentioned CVI legal system and make composite wood.
Be illustrated in figure 5 fiber bar brake facing precast body longitudinal section view, Fig. 5 is: blade 12; Dovetail attachment portion 13; Root of blade 14; Be also by above-mentioned CVI method, after making the thick embryo of ceramic base, to it, take boring method to discharge prestress, contribute to the heat radiation of brake facing simultaneously, as shown in Figure 6, boring can be described as louvre simultaneously.Then to outer tube 3 and the gap of plug 4, taking high-temperature fusion described above to soak the silicon method fills or plug-hole, finally obtains finished product.
Embodiment 2:
In embodiment 1, the manufacture of described fibrous bundle muscle, all fibers of outer tube 3 and plug 4 adopt the PAN based carbon fiber, in addition can also adopt asphalt series or cellulose-based carbon fiber, and the three also can be optimized combination according to the stressing conditions of material.Other fiber selection principle of each germline adopts roughly the same described above, and outer tube 3 adopts the carbon fiber of maximum intensity mold temperature, and plug 4 adopts the carbon fiber of ultra high modulus.
As shown in Figure 2, fibrous bundle muscle precursor is by the pultrusion production technique, and fiber adopts at the PAN of 1500 ℃ of left and right carbonizing treatment base carbon fibre, the solution that the shaping medium precursor substance employing polyvinyl alcohol in the glue groove and warm water mix by the weight ratio of 1: 5.At first be wound around polytetrafluoroethylene film on plug 4 finished products, the internal diameter varies amount of the thickness of film after by outer tube stretch-draw and the shrinkage of outer tube cracking are carried out calculative determination.Then hoop is wound around high strength fibre 2 by winding wheel, the high strength fibre 2 that another group is soaked into glue enters the mold cured moulding through preformed board with plug 4, make the fiber bar precursor, can be wound around fiber at the place, two ends of fiber bar precursor if necessary, the formation termination increases, and is convenient to the stretch-draw of follow-up outer tube.Then by forming material in a vacuum, first be heated to 300 ℃ of heating and make the preliminary carbonization of polyvinyl alcohol, then heat 1 hour under 1000 ℃～1500 ℃, make the further carbonization of polyvinyl alcohol, obtain fibrous bundle muscle precursor, then carry out making matrix material as embodiment 1 following operation.
The following describes and take plug 4 and the fibrous bundle muscle precursor molding production process that SiC is medium, the medium precursor material of glue groove is Polycarbosilane, and ensuing plug 4 moulding processs are with upper identical.In fibrous bundle muscle precursor production technique, the temperature of preliminary carbonization is 350 ℃, and other step is the same.The volume content of the outer tube 3 obtained by this method and the SiC medium of plug 4 is in 50% left and right.The content of this medium can be adjusted by the concentration or the dipping number of times that change precursor solution.
The more than C of fiber bunchy medium and SiC, also have TiC, BN, Si
3n
4, SiO
2, Al
2o
3, TiO
2and TaO
5deng precursor substance, by being heating and curing, its technique and the above roughly the same, do not describe in detail one by one.For in the glue groove in Fig. 1 and Fig. 2, adopting respectively medium precursor material described above.Fiber, except C, also can adopt the fibers such as SiC, BN, B, Al2O3, and the compound inorganic fibre bundle of the medium composition of corresponding compound separately that obtains of fiber and various medium precursor combined heated, can also form bundle by a branch of multiple fiber.In the combination of fiber and bunchy medium, adopt the matched combined of oxide compound and oxide compound as far as possible, non-oxidized substance and non-oxidized substance matched combined, can apply in advance the little composition of BN isoreactivity if necessary on fiber surface, can prevent pyroreaction to a certain extent, avoid causing the damage of fiber.
For with top, describedly having other to penetrate the method manufacturing process, its fiber and bunchy medium precursor material use and combination and above-mentioned can be basically identical.
Embodiment 3:
The preparation method of the turbine ceramic blade that the fibrous bundle muscle strengthens, its preparation process is as follows:
The fibrous bundle muscle adopts the described fibrous bundle muscle of embodiment 1, and fibrous bundle muscle and carbon fiber are compiled into to precast body with turbine ceramic blade shape, and wherein the fibrous bundle muscle is main strength bar.The braiding of precast body must be noted that the position of the cutting zone of fibrous bundle muscle, and an end wherein should be in the position of being convenient to cutting and prestress release.As shown in Figure 5, wavy fiber bundle muscle 8 and straight line fibrous bundle muscle 9 are according to the suffered cloth muscle that carries out of blade, in this figure, carbon fiber does not show, wavy fiber bundle muscle 8 and straight line fibrous bundle muscle 9 be just signal in this figure, one end cutting zone of fibrous bundle muscle will be in 11 li of the end grinding area of blade, and the other end gos deep into turbine ceramic blade afterbody (also can set up grinding area at afterbody).The volume fraction of fibrous bundle muscle is made in the required calculation of Prestress of matrix material.The volume fraction scope of fibrous bundle muscle is generally 3～60%.Above-mentioned three-dimensional preformed body is put into to chemical vapour infiltration/cvd furnace, manufacture the SiC based composites, depositing temperature is 1100 ℃, and vacuum keep is at 120Pa, and unstripped gas is CH
3siCl
3+ H
2, its chemical equation has:
Wherein H2 is carrier gas and diluent gas, and gas flow is made as 220L/min, and shielding gas adopts Ar gas, and flow is got 220L/min, and depositing time is 8 days for the first time.The time of the reaching component surface of taking out and polish, open its hole and continue deposition for the second time, within 8 days, takes out afterwards, complete coarse-blank manufacturing process.If the density of not meeting the requirements of, can repeat the density of CVI method and reach design requirements.Then need thick embryo member is carried out to prestress release type manufacturing procedure.As shown in Figure 5, along the grinding line 10 of blade tip, carry out grinding, thereby the cutting zone of worn fibrous bundle muscle discharges the prestress of fibrous bundle muscle.Then to 1.5 times of interpolation Si micro mists by theoretical required Si amount, its Powder Particle Size is 10～100 μ m, and the blade idiosome after Si powder and grinding is placed in plumbago crucible, and the blade idiosome stands upside down on the plumbago crucible bottom surface, 10, grinding line is contacted with Si, be convenient to the infiltration of Si powder.Then plumbago crucible being placed in to temperature is to carry out melting in 1500 ℃～1600 ℃ negative pressure High Temperature Furnaces Heating Apparatuss to soak the gap that silicon is filled outer tube 3 and plug 4, or molten silicon infiltration in the pressure-fired High Temperature Furnaces Heating Apparatus of the 100Pa left and right that is filled with Ar gas, is incubated 1.5 hours.To obtain subsequently the C/SiC matrix material and carry out mechanical workout, finally obtain finished product, as shown in Figure 6.
Embodiment 4:
The preparation method of the Nozzle of Liquid Rocket Motor that the fibrous bundle muscle strengthens, its preparation process is as follows:
The fibrous bundle muscle adopts the described fibrous bundle muscle of embodiment 1, and the fibrous bundle muscle is become to precast body with carbon fiber with Nozzle of Liquid Rocket Motor 17 shape establishments or acupuncture.The braiding of precast body must be noted that the position of the cutting zone of fibrous bundle muscle, and an end wherein should be in the position of being convenient to cutting and prestress release.As shown in Figure 7, (forward of Z axis of take is working direction for derotation spiral fiber bundle muscle 15 and dextrorotation spiral fiber bundle muscle 16, clockwise turn to dextrorotation) be main strength bar, with the carbon fiber of its braiding, in this figure, do not show, each is positive and negative revolve muscle jet pipe 17 circumferential directions take respectively central shaft as symmetry axis evenly equally spaced in jet pipe 17 walls the cloth muscle, a positive and negative end cutting zone of revolving muscle must be in the grinding area 11 of the same upper end of jet pipe 17 or lower end.The volume fraction of fibrous bundle muscle is made in the required calculation of Prestress of matrix material.The volume fraction scope of fibrous bundle muscle is generally 3～60%, and for the ease of bending, the diameter of fibrous bundle muscle is preferably in below 1mm.Aspect the spiral cloth muscle, the excessive loss of prestress that frictional force for fear of outer tube 3 and plug 4 when the bending causes, the length of fibrous bundle muscle should be less than critical length (when prestress, when loss of prestress equals fibrous bundle prestress value 5% that muscle is stored, the length of fibrous bundle muscle now).Above-mentioned three-dimensional preformed body is put into to chemical vapour infiltration/cvd furnace, manufacture the SiC based composites, depositing temperature is 1100 ℃, and vacuum keep is at 80Pa, and unstripped gas is CH
3siCl
3+ H
2, its chemical equation has:
Wherein H2 is carrier gas and diluent gas, and gas flow is made as 180L/min, and shielding gas adopts Ar gas, and flow is got 180L/min, and depositing time is 12 days for the first time.The time of the reaching component surface of taking out and polish, open its hole and continue deposition for the second time, within 12 days, takes out afterwards, complete coarse-blank manufacturing process.If the density of not meeting the requirements of, can repeat the density of CVI method and reach design requirements.Then need thick embryo member is carried out to prestress release type manufacturing procedure.As shown in Figure 7, along the grinding line 10 of jet pipe 17 upper ends or lower end, carry out grinding, thereby the cutting zone of worn fibrous bundle muscle discharges the prestress of fibrous bundle muscle.Then to 1.2 times of interpolation Si micro mists by theoretical required Si amount, its Powder Particle Size is 10～100 μ m, and the jet pipe idiosome after Si powder and grinding is placed in plumbago crucible, and the jet pipe idiosome stands upside down on the plumbago crucible bottom surface, 10, grinding line is contacted with Si, be convenient to the infiltration of Si powder.Then plumbago crucible being placed in to temperature is to carry out melting in 1500 ℃～1600 ℃ negative pressure High Temperature Furnaces Heating Apparatuss to soak the gap that silicon is filled outer tube 3 and plug 4, or molten silicon infiltration in the pressure-fired High Temperature Furnaces Heating Apparatus of the 100Pa left and right that is filled with Ar gas, is incubated 2.5 hours.To obtain subsequently the C/SiC matrix material and carry out mechanical workout, finally obtain finished product, as shown in Figure 8.
Embodiment 5:
The preparation method of the engine jet pipe adjustment sheet that the fibrous bundle muscle strengthens, its preparation process is as follows:
The fibrous bundle muscle adopts the described fibrous bundle muscle of embodiment 2, by as shown in Figure 9 become whole charcoal felt without latitude fibrous bundle muscle layer with the acupuncture of net tire, need exchange the tensile stress that nodal plate produces according to thermal shock and air-flow without the spacing of the fibrous bundle muscle 6 of latitude fibrous bundle muscle layer and interlamellar spacing thereof and carry out calculative determination.The volume fraction of fibrous bundle muscle is made in the required calculation of Prestress of matrix material, and the volume fraction scope of fibrous bundle muscle is generally 3～60%, and the diameter of fibrous bundle muscle is 0.6mm.Above-mentioned charcoal felt is put into to cvd furnace, and depositing temperature is 1100 ℃, and vacuum keep is in the 100Pa left and right, and unstripped gas is CH
3siCl
3+ H
2, its chemical equation has:
Wherein H2 is carrier gas and diluent gas, and gas flow is made as 200L/min, and shielding gas adopts Ar gas, and flow is got 200L/min, and depositing time is 10 days for the first time.The time of the reaching component surface of taking out and polish, open its hole and continue deposition for the second time, within 10 days, takes out afterwards, complete coarse-blank manufacturing process.If the density of not meeting the requirements of, can repeat the density of CVI method and reach design requirements.Then need thick embryo member is carried out to prestress release type manufacturing procedure.As shown in figure 10, along the grinding line 10 at adjustment sheet both ends, carry out grinding, thereby the cutting zone of worn fibrous bundle muscle discharges the prestress of fibrous bundle muscle.Then to 1.3 times of interpolation Si micro mists by theoretical required Si amount, its Powder Particle Size is 10～100 μ m, the Si powder is contacted with the Si on the plumbago crucible bottom surface with the grinding surface after the adjustment sheet grinding, then plumbago crucible being placed in to temperature is to carry out melting in 1500 ℃～1600 ℃ negative pressure High Temperature Furnaces Heating Apparatuss to soak the gap that silicon is filled outer tube 3 and plug 4, or molten silicon infiltration in the pressure-fired High Temperature Furnaces Heating Apparatus of the 0～500Pa left and right that is filled with Ar gas, be incubated 1～2 hour.Carry out again the infiltration of the Si powder of another side after infiltration is complete.To obtain subsequently the C/SiC matrix material and carry out mechanical workout, finally obtain finished product.
Claims (8)
1. the composite structure stress rib that prestores strengthens ceramic matric composite, it is characterized in that: adopt following method to make: become precast body by the fibrous bundle muscle with fibrage or acupuncture or use separately the fibrous bundle muscle to be woven into precast body, during the braiding of precast body, make an end at least wherein of fibrous bundle muscle be in the position of being convenient to cutting and prestress release, by the CVI method, make the thick embryo of ceramic matric composite, then by the method that the thick embryo of ceramic matric composite is carried out to grinding or boring, remove the end anchorage of fibrous bundle muscle self, the interface cohesive action of fibrous bundle muscle and matrix applies compressive pre-stress to ceramic matrix, carry out subsequently 1500 ℃～1600 ℃ negative pressure high-temperature fusion and soak the gap that silicon is filled outer tube and plug, but or the gap of the thermosetting resin of employing carbonization filling outer tube and plug, plug is participated in stressed, finally make finished product, perhaps plug is taken out, then adopt chemical Vapor deposition process or negative pressure high-temperature fusion to soak silicon plug-hole, then moulding, described fibrous bundle muscle adopts following method manufacture:
The first step, manufacture plug, plug adopts the pultrusion production technique, fiber adopts at the PAN of 2000 ℃ of carbonizing treatment base carbon fibre, or employing asphalt series or cellulose-based carbon fiber, shaping medium precursor substance in the glue groove adopts resol and ethanol to press the weight ratio mixing solutions of 1:1, or the polymkeric substance of the high carbon residue rate of employing polyether-ether-ketone, perhaps adopt Polycarbosilane (PCS) solution, or the solution that adopts polyvinyl alcohol and warm water to mix by the weight ratio of 1:5, fiber is curing molding in mould, then in a vacuum, under 1500～2100 ℃, l hour high temperature graphitization of heating processed,
Second step, fibrous bundle muscle precursor is by the pultrusion production technique, fiber adopts at the PAN of 1500 ℃ of carbonizing treatment base carbon fibre, shaping medium precursor substance in the glue groove adopts resol and ethanol to press the weight ratio mixing solutions of 1:1, at first be wound around polytetrafluoroethylene film on the plug finished product, then hoop is wound around fiber by winding wheel, the fiber that another group is soaked into glue enters the mold cured moulding through preformed board with plug, make the fiber bar precursor, and fiber enters, the mode of mould is braiding, canoe enters; Place, two ends at the fiber bar precursor is wound around fiber, forms termination and increases, and is convenient to the stretch-draw of follow-up outer tube; Then by forming material in a vacuum, first be heated to 300 ℃ of heating and make the preliminary carbonization of resol, then heat l hour under 1000 ℃～1500 ℃, make the further carbonization of resol, be heated to more than 400 ℃ in temperature course, polytetrafluoroethylene film cracking gradually disappears, thus the outer tube moulding, and have gap with the plug in it;
The 3rd step, by to fibrous bundle muscle precursor outer tube, stretch-draw enters, clamp the outer tube end with the anchoring ring, the stretch-draw outer tube, it is the outer tube elongation, then the tension stress that keeps outer tube, and between the outer tube mouth of pipe and plug end face the filling binding agent, the hot setting binding agent, then unclamp the stretch-draw of outer tube, this fibrous bundle muscle end anchorage adopts resol/norbide hot setting adhesive with binding agent, but or the thermosetting resin of employing carbonization, be heating and curing at 300 ℃～1000 ℃, then unclamp stretch-draw and make the fibrous bundle muscle.
2. manufacture the composite structure claimed in claim 1 stress rib that prestores and strengthen the method for ceramic matric composite, it is characterized in that: the fibrous bundle muscle become to precast body with fibrage or acupuncture or use separately the fibrous bundle muscle to be woven into precast body, during the braiding of precast body, make an end at least wherein of fibrous bundle muscle be in the position of being convenient to cutting and prestress release, the volume fraction of fibrous bundle muscle is made in the required calculation of Prestress of matrix material, the volume fraction scope of fibrous bundle muscle is 3～60%, above-mentioned precast body is put into to the CVI/ cvd furnace, manufacture the SiC based composites, depositing temperature is 1000 ℃～1100 ℃, vacuum keep is at 50～500Pa, the gas flow of unstripped gas is 180～220L/min, shielding gas adopts Ar gas, flow is got 180～220L/min, depositing time is 8～12 days for the first time, the time of the reaching component surface of taking out and polish, open its hole and continue deposition for the second time, within 8～12 days, take out afterwards, complete the thick embryo of ceramic matric composite manufacturing process, then the thick embryo of ceramic matric composite is carried out to prestress release type manufacturing procedure, if plug does not need to take out, the beginning from having deposited for the first time of this operation, complete after prestress release type manufacturing procedure by 1.2～1.5 times of the required Si amount of theory, adding the Si micro mists, its Powder Particle Size is 10～100 μ m, the thick embryo of Si powder and ceramic matric composite is placed in plumbago crucible grinding line face is contacted with Si, it is to carry out melting in 1500 ℃～1600 ℃ negative pressure High Temperature Furnaces Heating Apparatuss to soak the gap that silicon is filled outer tube (3) and plug (4) that plumbago crucible is placed in to temperature, or molten silicon infiltration in the pressure-fired High Temperature Furnaces Heating Apparatus of the 100Pa that is filled with Ar gas, be incubated 1.5～2.5 hours, perhaps at the outer tube (3) of fibrous bundle muscle and the gap of plug (4), add the presoma material Pintsch process of carbon to fill gap, perhaps plug is taken out, adopt again chemical Vapor deposition process or negative pressure high-temperature fusion to soak the silicon plug-hole, to obtain subsequently the C/SiC matrix material and carry out mechanical workout, finally obtain finished product.
3. the manufacture composite structure according to claim 2 stress rib that prestores strengthens the method for ceramic matric composite, it is characterized in that: for take the unstripped gas that SiC uses as matrix CVI, be CH3SiCl3+H2.
4. strengthen the method for ceramic matric composite according to the described manufacture composite structure of claim 2 or 3 stress rib that prestores, it is characterized in that: described prestress release type manufacturing procedure refers to along the grinding line of the thick embryo of ceramic matric composite carries out grinding, the cutting zone of worn fibrous bundle muscle, discharge the prestress of fibrous bundle muscle, or take boring method to discharge prestress to the thick embryo of ceramic matric composite.
5. strengthen the method for ceramic matric composite according to the described manufacture composite structure of claim 2 or 3 stress rib that prestores, it is characterized in that: described fibrous bundle muscle adopts following method manufacture:
The first step, manufacture plug, plug adopts the pultrusion production technique, fiber adopts at the PAN of 2000 ℃ of carbonizing treatment base carbon fibre, or employing asphalt series or cellulose-based carbon fiber, shaping medium precursor substance in the glue groove adopts resol and ethanol to press the weight ratio mixing solutions of 1:1, or the polymkeric substance of the high carbon residue rate of employing polyether-ether-ketone, perhaps adopt Polycarbosilane (PCS) solution, or the solution that adopts polyvinyl alcohol and warm water to mix by the weight ratio of 1:5, fiber is curing molding in mould, then in a vacuum, under 1500～2100 ℃, l hour high temperature graphitization of heating processed,
Second step, fibrous bundle muscle precursor is by the pultrusion production technique, fiber adopts at the PAN of 1500 ℃ of carbonizing treatment base carbon fibre, shaping medium precursor substance in the glue groove adopts resol and ethanol to press the weight ratio mixing solutions of 1:1, at first be wound around polytetrafluoroethylene film on the plug finished product, then hoop is wound around fiber by winding wheel, the fiber that another group is soaked into glue enters the mold cured moulding through preformed board with plug, make the fiber bar precursor, and fiber enters, the mode of mould is braiding, canoe enters; Be wound around fiber at the place, two ends of fiber bar precursor if necessary, form termination and increase, be convenient to the stretch-draw of follow-up outer tube; Then by forming material in a vacuum, first be heated to 300 ℃ of heating and make the preliminary carbonization of resol, then heat l hour under 1000 ℃～1500 ℃, make the further carbonization of resol, be heated to more than 400 ℃ in temperature course, polytetrafluoroethylene film cracking gradually disappears, thus the outer tube moulding, and have gap with the plug in it;
The 3rd step, by to fibrous bundle muscle precursor outer tube, stretch-draw enters, clamp the outer tube end with the anchoring ring, the stretch-draw outer tube, it is the outer tube elongation, then the tension stress that keeps outer tube, and between the outer tube mouth of pipe and plug end face the filling binding agent, the hot setting binding agent, then unclamp the stretch-draw of outer tube, this fibrous bundle muscle end anchorage adopts resol (PF)/norbide (B4C) hot setting adhesive with binding agent, but or the thermosetting resin of employing carbonization, be heating and curing at 300 ℃～1000 ℃, then unclamp stretch-draw and make the fibrous bundle muscle.
6. the manufacture composite structure according to claim 5 stress rib that prestores strengthens the method for ceramic matric composite, it is characterized in that: in above-mentioned second step, in film, add in advance graphite microparticles as lubricant.
7. the manufacture composite structure according to claim 5 stress rib that prestores strengthens the method for ceramic matric composite, it is characterized in that: in above-mentioned second step, for space after the carbonization that prevents outer tube excessive too much and prevent that the gas of follow-up CVI method from entering the gap of outer tube and plug, add the SiC micro mist in the glue groove, reduce contraction and the space of carbonization process.
8. the manufacture composite structure according to claim 5 stress rib that prestores strengthens the method for ceramic matric composite, it is characterized in that: in above-mentioned second step, outside surface at outer tube is coated with resol or other thermosetting resin carbonization, repeat this process, prevent that the gas of follow-up CVI method from entering the gap of outer tube and plug.
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| RU2620810C1 (en) * | 2016-05-06 | 2017-05-29 | Открытое акционерное общество "Композит" | Method of manufacturing porous base scaffold of composite material |
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| CN113461433B (en) * | 2021-08-05 | 2022-05-27 | 上海大学 | Prestressed fiber reinforced C/SiBCN ceramic composite material and preparation method thereof |
| CN113563097B (en) * | 2021-08-25 | 2022-04-22 | 上海大学 | Carbon fiber preform, preparation method thereof and preparation method of carbon/carbon composite material |
| CN116023161B (en) * | 2023-01-31 | 2023-07-11 | 北京理工大学 | Large-size high Jiang Taoci-matrix composite special-shaped lattice structure and preparation method thereof |
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| JPH1120025A (en) * | 1997-07-08 | 1999-01-26 | Ohbayashi Corp | Connecting structure of fiber reinforced plastic wire rod |
| ITTV20010081A1 (en) * | 2001-06-18 | 2002-12-18 | Marcello Toncelli | PANEL COMPOSED OF A STRUCTURAL SHEET OF FIBER RESIN AND A DECORATIVE SHEET OF STONE OR CERAMIC MATERIAL |
| US20060163773A1 (en) * | 2005-01-24 | 2006-07-27 | General Electric Company | Method for performing silicon melt infiltration of ceramic matrix composites |
| CN101343870A (en) * | 2008-08-22 | 2009-01-14 | 北京航空航天大学 | Fiber-reinforced composite material rib concrete pile and its production and construction method |
| CN101913896A (en) * | 2010-08-13 | 2010-12-15 | 中南大学 | Method for rapidly densifying high-density full-gaseous phase pyrolytic carbon-based carbon/carbon composite materials |
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| RU2620810C1 (en) * | 2016-05-06 | 2017-05-29 | Открытое акционерное общество "Композит" | Method of manufacturing porous base scaffold of composite material |
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