CN106957180A - A kind of Cf/ C SiC ceramic matrix composite materials and its preparation method and application - Google Patents

A kind of Cf/ C SiC ceramic matrix composite materials and its preparation method and application Download PDF

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CN106957180A
CN106957180A CN201710141633.8A CN201710141633A CN106957180A CN 106957180 A CN106957180 A CN 106957180A CN 201710141633 A CN201710141633 A CN 201710141633A CN 106957180 A CN106957180 A CN 106957180A
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carbon
precast body
carbon fiber
finished product
titanium
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CN106957180B (en
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孙少伟
欧阳晓平
齐福刚
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Xiangtan University
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    • F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
    • F02F—CYLINDERS, PISTONS OR CASINGS, FOR COMBUSTION ENGINES; ARRANGEMENTS OF SEALINGS IN COMBUSTION ENGINES
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Abstract

Composite designed by the present invention includes carbon fiber precast body, matrix carbon, filler and DLC；Described matrix carbon is evenly affixed on the carbon fiber of precast body, constitutes the carbon fiber precast body with matrix carbon；The filler is filled in the prefabricated carbon fiber body with matrix carbon and is coated on the prefabricated carbon fiber with matrix carbon in vitro, constitutes semi-finished product, and the DLC is coated on formation diamond-like rock layers on semi-finished product；Contain Ti elements, Si elements, C element, Mo elements in the filler.The method that the present invention uses tetra- kinds of process combinations of CVI+SI+RMI+PECVD, be made have the advantages that consistency is high, thermal coefficient of expansion is small, coefficient of friction is small, self lubricity is high, thermal conductivity is high, anti-oxidant anti-thermal shock, resistance to ablation is wear-resistant, high-intensity high-tenacity finished product, present invention process is simple simultaneously, short preparation period, low equipment requirement, low cost and being realized be molded only, is easy to heavy industrialization application.

Description

A kind of Cf/ C-SiC composites and its preparation method and application
Technical field
The invention belongs to mechanical material field, relate more specifically to a kind of Cf/ C-SiC composites and preparation method thereof And application.
Background technology
Piston is automobile engine " heart ", bears the mechanical load and thermic load of alternation, is the bar that works in engine One of worst key components and parts of part.The function of piston is subject to gas pressure, and is transmitted to connecting rod by piston pin and drives song Axle rotates, the part of top land or combustion chamber.With developing rapidly for automobile industry, as Ferrari, Lamborghini Requirement etc. high-end sport car to " heart " is more and more harsher.In order to extend the service life of piston and improve its safety in utilization, Design of having to is various abnormally-structured and uses advanced coating treatment technology.In fact in actual applications, irregular excircle is designed The structures such as compound face, special pinhole, often make modular construction design complication, increase the difficulty of processing, and increase Development and cost of use.Even if cast-iron piston and all-aluminium piston before used have developed the place of various advanced coatings Reason technology, it is also apparent that can not meet its high rotating speed, high pressure, the operating mode of high thermal shock, this long period, Gao Cheng on the contrary The expense of this development ＆ production coating makes manufacturers suffer untold misery.In the recent period, relevant unit and enterprise propose a kind of carbon fiber It is prepared by the piston of piston, i.e. carbon fiber reinforced carbon matrix composite manufacture, including head, skirt section and key seat, this composite Piston have the advantages that certain high-temp and high-strength, density be small, coefficient of friction is small really.But so far, this piston Production is had not been put to, still loses its marketization, is primarily due to currently without a complete specific carbon fiber piston production system Standby process route, along with simple carbon/carbon compound material inherently has, mechanical behavior under high temperature is poor, the capacity of heat transmission is poor, easily soft change Birth defects such as shape, and manufacturing cycle is longer, so wanting large-scale production and being difficult, so this is just to carbon/carbon compound material Modified prepare and process proposes very high request.
Therefore unique, low cost a, short-period C is exploredfThe preparation technology of/C-SiC composites, passes through Adulterate filler modified simple carbon/carbon compound material, so that carbon fiber piston best in quality is prepared, in addition along with reality With effective and inexpensive coating, the large-scale production and the marketization of carbon fiber piston can be accelerated to expand.
The content of the invention
There is provided a kind of C for part in view of the shortcomings of the prior art of the inventionf/ C-SiC composites and its preparation side Method and application.
A kind of C of the present inventionf/ C-SiC composites, including carbon fiber precast body, matrix carbon, filler and diamond-like Stone；Described matrix carbon is evenly affixed on the carbon fiber of precast body, constitutes the carbon fiber precast body with matrix carbon；It is described to fill out Fill thing and be filled in the prefabricated carbon fiber body with matrix carbon and be coated on the prefabricated carbon fiber with matrix carbon in vitro, constitute Semi-finished product, the DLC is coated on formation diamond-like rock layers on semi-finished product；Contain Ti elements, Si members in the filler Element, C element, Mo elements；Ti elements in filler exist with any one in titanium carbide, silicon-carbon titanium or two ways；Filling Si elements in thing exist with least one of SiC, simple substance Si, silicon-carbon titanium, molybdenum silicide mode；C element in filler with At least one of SiC, silicon-carbon titanium, silicon-carbon titanium mode is present；Mo elements in filler are with zeroth order molybdenum, molybdenum silicide, molybdenum carbide At least one of mode exist.
Preferably, a kind of C of the inventionfSi elements in/C-SiC composites, filler are with silicon-carbon titanium, silicon Change at least one of molybdenum with SiC, simple substance the Si mode being blended to exist.
A kind of C of the present inventionf/ C-SiC composites, the Cf/ C-SiC composites contain silicon-carbon titanium (Ti3SiC2) phase, Molybdenum silicide (MoSi2) phase, molybdenum carbide (Mo2C) phase.
A kind of C of the present inventionf/ C-SiC composites, choose the semi-finished product that quality is B, and measurement takes Ti members in semi-finished product Element and the quality sums of Mo elements, and be defined as A, then A/B=0.04-0.08.Preferably A/B=0.04-0.075.Further Preferably A/B=0.045-0.075.
A kind of C of the present inventionf/ C-SiC composites, titanium and Mo mass ratio are 0.6-1.04:1.Preferably 0.65- 0.68:1。
A kind of C of the present inventionf/ C-SiC composites, the density of carbon fiber precast body is 0.5-0.6g/cm3。
A kind of C of the present inventionf/ C-SiC composites, the density of the carbon fiber precast body with matrix carbon for 1.3~ 1.4g/cm3。
A kind of C of the present inventionf/ C-SiC composites, the density of semi-finished product is 1.8~1.9g/cm3。
A kind of C of the present inventionf/ C-SiC composites, the CfThe density of/C-SiC composites is 1.82~1.92g/ cm3.In the present invention, the CfThe density of/C-SiC composites is more than the density of semi-finished product.
A kind of C of the present inventionfThe preparation method of/C-SiC composites, comprises the steps：
Step one
Carbon fiber is woven into precast body, chemical vapor infiltration depositing base carbon is then carried out；Obtain density for 1.3~ 1.4g/cm3The carbon fiber precast body with matrix carbon；The density of the precast body is 0.5~0.6g/cm3；
Step 2
Carbon fiber precast body with matrix carbon obtained by step one is placed in the maceration extract containing Ti, Mo and impregnated, is contained There are Ti, Mo precast body；
Step 3
Precast body containing Ti, Mo obtained by step 2 is placed on Si powder or is embedded in Si powder, under vacuum atmosphere, Siliconising processing is carried out in 1500-1750 DEG C；Density is obtained for 1.8~1.9g/cm3Semi-finished product；
Step 4
One layer of diamond-like rock layers are coated in surface of semi-finished obtained by step 3；Obtain finished product.
A kind of C of the present inventionfIn the preparation method of/C-SiC composites, step one, the carbon fiber is mesophase pitch Base carbon fibre.Mesophase pitch-based carbon fibers compare polyacrylonitrile-based carbon fibre, cheap and easy to get；Compared to viscose-based carbon fiber, power Learn excellent performance, it is easy to weave；More importantly the heat conductivility of mesophase pitch-based carbon fibers is better than polyacrylonitrile-based carbon Fiber and viscose-based carbon fiber.
A kind of C of the present inventionfIn the preparation method of/C-SiC composites, step one, the precast body be three-dimensional four-way or Three-dimensional five to acupuncture carbon felt porous preform.Compared to the weaving of one-dimensional, two-dimentional 2.5 dimensions, three-dimensional four-way or three-dimensional Five to the globality of acupuncture braid significantly improve the volume fraction of thickness direction fiber, material can be effectively improved The interlaminar shear strength of material and the strength and stiffness of thickness direction.And be not layered from weaving, being compound to finished product, it is inorganic Tool is processed or only does a small amount of processing for not injuring carbon fiber piston porous preform, maintains the globality of material.
A kind of C of the present inventionfIn the preparation method of/C-SiC composites, step one, chemical vapor infiltration depositing base carbon When, at least one of the carbon-source gas used in propane, ethene, acetylene.Preferably propane.Using propane as carbon precursor, material Material is easy to get, technical maturity, easy to operate, and preparation cost is relatively low, can prepare the excellent carbon base body of mechanical behavior under high temperature, and ooze product Carbon base body dense uniform, crackle it is few.
A kind of C of the present inventionfIn the preparation method of/C-SiC composites, step one, chemical vapor infiltration depositing base carbon When, diluent gas used selected from argon gas, nitrogen, at least one.Preferably argon gas.
A kind of C of the present inventionfIn the preparation method of/C-SiC composites, step one, chemical vapor infiltration depositing base carbon When, the intake velocity of carbon-source gas is 0.5-0.9L/min, is preferably 0.7L/min；The intake velocity of diluent gas is 2.5- 3.3L/min, preferably 3L/min.
A kind of C of the present inventionfIn the preparation method of/C-SiC composites, step one, chemical vapor infiltration depositing base carbon When, it is 5-6 DEG C/min to control heating rate；It is 1000-1100 DEG C, preferably 1000 DEG C to control depositing temperature；In depositing temperature Under, it is 450~600h hours to control soaking time.
The present invention only needs about 500 hours, deposits comparatively dense uniform part carbon base body, its density is in 1.3 ~1.4g/cm3Between, to still leaving appropriate space among carbon/carbon precast body.This process can both shorten preparation It is cycle, cost-effective, it is also beneficial to the infiltration of slurry below.It can disperse uneven when carbon base body too high levels, cause performance Decline, and space is filled, and also make it that slurry is difficult that infiltration is entered, and then be difficult to filler modified purpose of adulterating；When The too low effect for causing carbon fiber of content is from giving full play to, it is impossible to be obviously improved material property.So, by lot of experiments Checking, is preferably 500h~600h to carbon fiber piston porous preform carburizing time, make the density of carbon/carbon precast body 1.3~ 1.4g/cm3Between.
A kind of C of the present inventionfIn the preparation method of/C-SiC composites, step 2,
Carbon fiber precast body with matrix carbon obtained by step one is placed in the maceration extract containing Ti, Mo and carries out Vaccum Permeating Stain, after vacuum impregnation, dries, obtains the precast body containing Ti, Mo；The maceration extract containing Ti, Mo is by water, micrometer silicon carbide titanium (TiC), micron molybdenum (Mo), CMC (sodium carboxymethylcellulose) in mass ratio, water：Micrometer silicon carbide titanium (TiC)：Micron molybdenum (Mo)： CMC (sodium carboxymethylcellulose)=100-90:50-55:60-65:0.5-0.8, preferably 100：50：60：0.8 composition；It is described During vacuum impregnation, the air pressure in equipment is less than or equal to 13.33Pa.
In industrial applications, 25h~30h is fully ground using electric slurry machine after dispensing, is reached fully dispersed Uniform state.It is sent to again during vacuum impregnation fills, and vacuum impregnation is filled vacuumizes and be less than limit residual voltage 13.33Pa. During vacuum impregnation, moisture content can largely depart from.Moisture content plays translocation in dipping process, when it is by micrometer silicon carbide titanium (TiC) after, micron molybdenum (Mo) is transported in precast body, precast body can be rapidly separated.So after the present invention is impregnated, can be with Selection is dried in the shade or low-temperature bake, the carbon after being infiltrated/carbon precast body.
The granularity of the micrometer silicon carbide titanium is 20-50 microns；The granularity of the micron molybdenum is 20-50 microns.
In order to ensure that micrometer silicon carbide titanium (TiC) and micron molybdenum (Mo) can be fully infiltrated up among carbon/carbon porous preform, The vacuum impregnation time is preferably 25-32h, and overlong time then influences preparation efficiency, wastes the energy, and to improving material property simultaneously Without large effect.Verified through lot of experiments, carbon/carbon that the micrometer silicon carbide titanium and micron molybdenum of introducing are accounted for after whole infiltration is prefabricated The 6%~9% of weight is advisable.
It is preferred that, the Infiltration Technics are vacuum infiltration.Added with distilled water, micrometer silicon carbide titanium (TiC), micron molybdenum (Mo) The dipping sizing agent prepared with CMC (sodium carboxymethylcellulose) mixture has good wetability, contact angle with carbon base body Small, infiltration pressure is big, can also infiltrate at ambient pressure, it is clear that can accelerate impregnation rate using vacuum infiltration, shortens and prepares week Phase.Without using vacuum pressed infiltration, because can be damaged during pressurization to the carbon/carbon precast body being not yet molded completely, making it The faint deformation of generation.
A kind of C of the present inventionfIn the preparation method of/C-SiC composites, step 3,
Precast body containing Ti, Mo obtained by step 2 is placed on Si powder or is embedded in Si powder, under vacuum atmosphere, Siliconising processing is carried out in 1500-1750 DEG C；Density is obtained for 1.8~1.9g/cm3Semi-finished product.
Preferably, under vacuum atmosphere, the pressure in stove is 3~6Pa.
Preferably, first to vacuum reaction stove evacuation in step 3, it is 3~6Pa to be still less than furnace pressure；Then Furnace temperature is raised to 1500 DEG C in 7~8h, 5h is incubated；Then furnace temperature is raised to 1750 DEG C using 1h again, is incubated 0.5h；It is last with Argon gas does protection gas, and it is 2.5KPa, furnace cooling to control argon pressure.
When siliconising is handled in the present invention, step 3, there is good wetability between molten silicon and carbon, titanium carbide, molybdenum, compared with Small contact angle, high vacuum process advan is accelerated and the reaction between carbon base body and filler in the seepage velocity of increase molten silicon Speed, beneficial to silicon carbide ceramics, silicon-carbon titanium and the equal generation of molybdenum silicide.Pressurization siliconising is not used also to allow for siliconising Initial stage can damage to carbon/carbon piston precast body, cause it to occur ess-strain.Precursor infiltration and pyrolysis is not used equally Method prepares silicon carbide substrate, is to substantially shorten manufacturing cycle, saved cost.Meanwhile, using designed by the present invention Vacuum reaction melting siliconizing treatment processes, its prepare silicon carbide ceramics matrix comply fully with product special dimension application (such as The required anti-high pressure of piston, high temperature resistance, heat shock resistance).
A kind of C of the present inventionfIn the preparation method of/C-SiC composites, step 4,
Semi-finished product obtained by step 3 are placed in cvd furnace, using plasma deposition technique deposition cladding diamond-like rock layers； During plasma deposition technique depositing diamond-like layer, control furnace pressure for 3-13.33Pa, be preferably 5Pa, control deposition temperature Degree is 60 DEG C~80 DEG C, deposition power is 600-620W, to deposit gases used be CH4And H2, the two flow is respectively 2.1- 2.4mL/min and 6.4-6.9mL/min, sedimentation time is 15h~16h.
It is preferred that, diamond-like coating thickness is 8~10 μm.Sedimentation time is long, causes coating layer thickness excessive, unfavorable In heat conduction, when it is used as piston, easily there is ablation in piston aditus laryngis, causes coating sheet to come off.Sedimentation time is too short, applies Layer is excessively thin, does not also have the effect of resistance to thermal ablation.
It is upper in application, the density of the carbon fiber precast body with matrix carbon, rate-determining steps two as obtained by rate-determining steps one Si temperature is soaked in melting in micrometer silicon carbide titanium (TiC), the consumption of micron molybdenum (Mo) and immersion condition matching step three in middle slurry Degree and the condition such as time control the value of the A/B in resulting materials.
Why the present invention, plate DLC, because the carbon fiber piston face prepared must have Si remaining, and Si can press down The graphitization of DLC coatings processed, the oxide thin layer silicon of coating surface serves the effect for hindering oxidation or quick conductive, and its heat is steady Qualitative and wearability can be greatly enhanced, and DLC coatings have the unique in effect of antifriction antiwear, extremely meet piston Working condition requirement.In addition, using methane as DLC coating precursors, material is easy to get, easy to operate, preparation cost is relatively low, can prepare height The DLC coatings of warm good mechanical performance, and the coating prepared and the inner surface adhesion of preparation are strong, even compact is difficult for drop-off, Excellent effect.
A kind of C of the present inventionfThe application of/C-SiC composites, including it is used as piston.During as piston, only need by Carbon fiber is woven into piston-shaped precast body；Other operations are carried out according to the scheme described in the present invention.
A kind of C of the present inventionfThe application of/C-SiC composites, is additionally included in the field such as space flight, military industry field, civilian Using.
Principle and advantage
The present invention is using chemical vapor infiltration (CVI)+slurry method of impregnation (SI)+vacuum reaction molten liquid forming (RMI) The method of+plasma enhanced chemical vapor deposition method (PECVD) four kinds of process combinations, and it is micro- by adulterating in the slurry Rice titanium carbide (TiC) and two kinds of fillers of micron molybdenum (Mo), prepare finished product.The present invention is fine using intermediate phase pitch-based carbon first Dimension knit out three-dimensional four-way or three-dimensional five to acupuncture carbon felt porous preform, then using CVI methods deposition carbon, fill many Fine pore in the fibre bundle of hole precast body, forms carbon/carbon precast body.Added with water, micrometer silicon carbide titanium (TiC), micron molybdenum (Mo) Mixture using CMC (sodium carboxymethylcellulose) is dipping sizing agent, using SI methods vacuum impregnation carbon/carbon piston precast body, so that Micrometer silicon carbide titanium (TiC) and two kinds of fillers of micron molybdenum (Mo) are introduced in carbon/carbon precast body.Again with RMI methods to carbon/carbon piston Precast body melts siliconising, so as to prepare the carbon fiber piston containing carbon-silicon carbide double substrate.It is finally fine in carbon using PECVD Dimension piston face deposits DLC coatings.The present invention passes through from former material of the mesophase pitch-based carbon fibers as braiding precast body Material, reason is that it has high heat conduction, high-modulus, is easy to graphitization, prior low cost.And be woven into three-dimensional four-way or Person's three-dimensional five to acupuncture carbon felt precast body be because this braiding structure more easily to have given play to carbon fiber each to excellent power Learn performance.Firm basis is laid to the high heat conduction after shaping, high intensity at this 2 points above.Then sunk using CVI methods When carbon distribution matrix, not easy damaged carbon fiber, it is ensured that the later stage of composite property is perfect.Again by being infiltrated in slurry Titanium carbide (TiC) and micron molybdenum (Mo) are added in the dipping sizing agent of method as filler, because their volume and quality is not sent out Changing, can suppress the contraction of carbon base body to a certain extent so that material quick densifying, shorten manufacturing cycle.With that It is that, to siliconising in micron TiC and micron Mo carbon/carbon piston precast body is doped with, substantial amounts of carborundum can be generated using RMI methods Ceramic hard matrix, piston prepared by this carbon-fiber reinforced carbon and silicon carbide double matrix composite has that density is low, antioxygen The advantages of changing performance good, corrosion-resistant, wear-resistant, excellent mechanical property and thermophysical property.Meanwhile, when a small amount of silicon of generation Carbon titanium (Ti3SiC2), molybdenum silicide (MoSi2) molybdenum carbide (Mo2) etc. C during phase, phases of these generations in the base can by Grain dispersion-strengtherning and bending strength and fracture toughness prepared by whole composite are improved to cooperate with matrix, along with life Into mutually also having self-healing micromechanism of damage, self lubricity and the low good feature of coefficient of friction, extremely suit the operating mode of piston. The material developed simultaneously has preferable plasticity, and this is conducive to the machine-shaping of piston.PECVD is finally used again, to work Plug plates DLC coatings.Why DLC is plated, because the carbon fiber piston face prepared there must be Si remaining, and Si can press down The graphitization of DLC coatings processed, the oxide thin layer silicon of coating surface serves the effect for hindering oxidation or quick conductive, and its heat is steady Qualitative and wearability can be greatly enhanced, and DLC coatings have the unique in effect of antifriction antiwear, extremely meet piston Working condition requirement.
In a word, the present invention, which have devised a kind of material of superior performance and explore a complete doping filler, changes Property prepares the process route of carbon fiber.The technique that especially entirely prepares piston is simple, the cycle is short, equipment requirement is simple, cost It is low, can realize that piston is molded only, and the piston prepared can meet high pressure, high rotating speed, the harsh operating mode of high thermal shock, Its service life is longer much than common piston service life under continuously circulation work.
The additional aspect and advantage of the present invention will be set forth in part in the description, partly will from the following description Become obvious, or recognized by the practice of the present invention.
Brief description of the drawings
In order to illustrate more clearly of the technical scheme of the specific embodiment of the invention, embodiment will be retouched below The accompanying drawing to be used needed for stating is briefly described.
Fig. 1 is the flow chart for the process of preparing that the embodiment of the present invention one is provided.
Embodiment
The embodiment of technical solution of the present invention is described in detail below in conjunction with accompanying drawing.Following examples are only used In clearly illustrating technical scheme, therefore example is only used as, and the protection of the present invention can not be limited with this Scope.It should be noted that unless otherwise indicated, technical term or scientific terminology used in this application should be the present invention The ordinary meaning that one of ordinary skill in the art are understood.
Embodiment 1
As shown in figure 1, the preparation of silicon carbide fiber reinforced silicon carbide ceramic matric composite provided in an embodiment of the present invention Method, comprises the following steps：
Step 1, prepare carbon fiber piston porous preform：
Carbon fiber is woven into by piston-shaped precast body using knitting；In the carbon fiber piston porous preform Carbon fiber be mesophase pitch-based carbon fibers.The density of the piston-shaped precast body is 0.58g/cm3；Precast body is choosing Three-dimensional five to acupuncture carbon felt porous preform；
Step 2, prepare carbon/carbon piston precast body：
Using chemical vapor infiltration, carbon fiber piston porous preform is placed in moulds of industrial equipment, then put together again In theory of evolution gaseous phase deposition stove.Product is oozed on the carbon fiber piston precast body that step 1 is obtained by carbon organic matter precursor Carbon, prepares density for 1.34g/cm3Carbon/carbon piston precast body；During chemical vapor infiltration depositing base carbon, carbon used When source gas is that propane, diluent gas used are argon gas, chemical vapor infiltration depositing base carbon, the intake velocity of carbon-source gas For 0.7L/min；The intake velocity of diluent gas is 0.18Nm3/ h (i.e. 3L/min).During chemical vapor infiltration depositing base carbon, It is 5.6 DEG C/min to control heating rate；It is 1000 DEG C to control depositing temperature；Under depositing temperature, it is 560h to control soaking time Hour.
Step 3, prepare slurry infiltration carbon/carbon piston precast body：
Step 2 gained carbon/carbon piston precast body is placed in the maceration extract containing Ti, Mo and carries out vacuum impregnation, is contained Ti, Mo precast body；The maceration extract containing Ti, Mo is by water, micrometer silicon carbide titanium (TiC), micron molybdenum (Mo), CMC (carboxymethyls Sodium cellulosate) in mass ratio, water：Micrometer silicon carbide titanium (TiC)：Micron molybdenum (Mo)：CMC (sodium carboxymethylcellulose)=100：50： 60：0.8 composition；During the vacuum impregnation, the air pressure in equipment is less than or equal to 13.33Pa.The granularity of the micrometer silicon carbide titanium is 30 microns；The granularity of the micron molybdenum is 30 microns.The vacuum impregnation time is 27h.After the completion of vacuum impregnation, dry；Contained There are Ti, Mo precast body；The micrometer silicon carbide titanium and micron molybdenum introduced after the completion of vacuum impregnation accounts for whole containing the prefabricated of Ti, Mo The 7% of body dry weight.
The preparation method of the maceration extract is：
25h~30h is fully ground using electric slurry machine after dispensing, fully dispersed uniform state is reached.Again will It is sent into during vacuum impregnation fills, and vacuum impregnation is filled vacuumizes and be less than limit residual voltage 13.33Pa.
Step 4, carbon fiber piston of the preparation containing carbon-silicon carbide matrix：
Precast body containing Ti, Mo obtained by step 3 is placed on Si powder or is embedded in Si powder, under vacuum atmosphere, in 1500 DEG C of progress siliconising processing；Density is obtained for 1.89g/cm3Semi-finished product.
Before siliconising, first to vacuum reaction stove evacuation, it is 3~6Pa to be still less than furnace pressure；Then furnace temperature is raised in 7h 1500 DEG C, it is incubated 5h；Then furnace temperature is raised to 1750 DEG C using 1h again, is incubated 0.5h；Protection gas is finally done with argon gas, controlled Argon pressure is 2.5KPa, furnace cooling.
Step 5, prepare carbon fiber piston face coating：
Using plasma strengthens chemical vapour deposition technique, and semi-finished product will be obtained in step 4 and put plasma chemistry gas into Mutually deposition equipment in, by ionize carbon organic matter precursor its surface deposition obtain DLC (DLC) coating.Deng from During sub- techniques of deposition diamond-like rock layers, it is 5Pa to control furnace pressure, and it is 60 DEG C~80 DEG C, deposition work(to control depositing temperature Rate be 600W, deposit it is gases used be CH4And H2, the two flow is respectively 2.1mL/min and 6.4mL/min, and sedimentation time is 15h~16h；Obtain the finished product that diamond-like coating thickness is 9 μm.Gained end properties is shown in Table 1
Table 1 uses the performance parameter of the prepared carbon fiber piston of the present invention
Embodiment 2
Step 1, prepare carbon fiber piston porous preform：
Carbon fiber is woven into by piston-shaped precast body using knitting；In the carbon fiber piston porous preform Carbon fiber be mesophase pitch-based carbon fibers.The density of the piston-shaped precast body is 0.6g/cm3；Precast body is three-dimensional Five to acupuncture carbon felt porous preform；
Step 2, prepare carbon/carbon piston precast body：
Using chemical vapor infiltration, carbon fiber piston porous preform is placed in moulds of industrial equipment, then put together again In theory of evolution gaseous phase deposition stove.Product is oozed on the carbon fiber piston precast body that step 1 is obtained by carbon organic matter precursor Carbon, prepares density for 1.38g/cm3Carbon/carbon piston precast body；During chemical vapor infiltration depositing base carbon, carbon used When source gas is that propane, diluent gas used are argon gas, chemical vapor infiltration depositing base carbon, the intake velocity of carbon-source gas For 0.8L/min；The intake velocity of diluent gas is 3.3 L/min.During chemical vapor infiltration depositing base carbon, control heating speed Rate is 5.5 DEG C/min；It is 1000 DEG C to control depositing temperature；Under depositing temperature, it is 550h hours to control soaking time.
Step 3, prepare slurry infiltration carbon/carbon piston precast body：
Step 2 gained carbon/carbon piston precast body is placed in the maceration extract containing Ti, Mo and carries out vacuum impregnation, is contained Ti, Mo precast body；The maceration extract containing Ti, Mo is by water, micrometer silicon carbide titanium (TiC), micron molybdenum (Mo), CMC (carboxymethyls Sodium cellulosate) in mass ratio, water：Micrometer silicon carbide titanium (TiC)：Micron molybdenum (Mo)：CMC (sodium carboxymethylcellulose)=100：50： 60：0.8 composition；During the vacuum impregnation, the air pressure in equipment is less than or equal to 13.33Pa.The granularity of the micrometer silicon carbide titanium is 50 microns；The granularity of the micron molybdenum is 50 microns.The vacuum impregnation time is 24h, 25h, 27h, 29h, 32h, 36h.Vaccum Permeating After the completion of stain, the precast body containing Ti, Mo is obtained；The micrometer silicon carbide titanium and micron molybdenum introduced after the completion of vacuum impregnation is accounted for entirely The a series of samples such as 5%, 6%, 7%, 8%, 9%, 10% of the prefabricated weight containing Ti, Mo.
The preparation method of the maceration extract is：
25h~30h is fully ground using electric slurry machine after dispensing, fully dispersed uniform state is reached.Again will It is sent into during vacuum impregnation fills, and vacuum impregnation is filled vacuumizes and be less than limit residual voltage 13.33Pa.
Step 4, carbon fiber piston of the preparation containing carbon-silicon carbide matrix：
Precast body containing Ti, Mo obtained by step 3 is placed on Si powder or is embedded in Si powder, under vacuum atmosphere, in 1750 DEG C of progress siliconising processing；Density is obtained for 1.88g/cm3Semi-finished product.
Before siliconising, first to vacuum reaction stove evacuation, it is 3~6Pa to be still less than furnace pressure；Then furnace temperature is raised in 7h 1500 DEG C, it is incubated 5h；Then furnace temperature is raised to 1750 DEG C using 1h again, is incubated 0.5h；Protection gas is finally done with argon gas, controlled Argon pressure is 2.5KPa, furnace cooling.
Step 5, prepare carbon fiber piston face coating：
Using plasma strengthens chemical vapour deposition technique, and semi-finished product will be obtained in step 4 and put plasma chemistry gas into Mutually deposition equipment in, by ionize carbon organic matter precursor its surface deposition obtain DLC (DLC) coating.Deng from During sub- techniques of deposition diamond-like rock layers, it is 5Pa to control furnace pressure, and it is 60 DEG C~80 DEG C, deposition to control depositing temperature Power be 600W, deposit it is gases used be CH4And H2, the two flow is respectively 2.1mL/min and 6.4mL/min, sedimentation time For 15h~16h；Obtain the finished product that diamond-like coating thickness is 10 μm.Gained end properties is shown in Table 2
Verified by lot of experiments, obtained four the most key to piston performance impact of packing quality fraction that adulterate Performance parameter, as described in Table 2：
Influence of the doping packing quality fraction of table 2 to piston performance parameter
Embodiment 3
Step 1, prepare carbon fiber piston porous preform：
Carbon fiber is woven into by piston-shaped precast body using knitting；In the carbon fiber piston porous preform Carbon fiber be mesophase pitch-based carbon fibers.The density of the piston-shaped precast body is 0.58g/cm3；Precast body is three Dimension five to acupuncture carbon felt porous preform；
Step 2, prepare carbon/carbon piston precast body：
Using chemical vapor infiltration, carbon fiber piston porous preform is placed in moulds of industrial equipment, then put together again In theory of evolution gaseous phase deposition stove.Product is oozed on the carbon fiber piston precast body that step 1 is obtained by carbon organic matter precursor Carbon, prepares carbon/carbon piston precast body；During chemical vapor infiltration depositing base carbon, carbon-source gas used are propane, used When diluent gas is argon gas, chemical vapor infiltration depositing base carbon, the intake velocity of carbon-source gas is 0.8L/min；Carrier gas The intake velocity of body is 3L/min.During chemical vapor infiltration depositing base carbon, it is 5.6 DEG C/min to control heating rate；Control is heavy Accumulated temperature degree is 1100 DEG C；Under depositing temperature, it is 550h hours to control soaking time.
Step 3, prepare slurry infiltration carbon/carbon piston precast body：
Step 2 gained carbon/carbon piston precast body is placed in the maceration extract containing Ti, Mo and carries out vacuum impregnation, is contained Ti, Mo precast body；The maceration extract containing Ti, Mo is by water, micrometer silicon carbide titanium (TiC), micron molybdenum (Mo), CMC (carboxymethyls Sodium cellulosate) in mass ratio, water：Micrometer silicon carbide titanium (TiC)：Micron molybdenum (Mo)：CMC (sodium carboxymethylcellulose)=100：50： 60：0.8 composition；During the vacuum impregnation, the air pressure in equipment is less than or equal to 13.33Pa.The granularity of the micrometer silicon carbide titanium is 20 microns；The granularity of the micron molybdenum is 20 microns.The vacuum impregnation time is 27h.After the completion of vacuum impregnation, obtain containing Ti, Mo precast body；The micrometer silicon carbide titanium and micron molybdenum introduced after the completion of vacuum impregnation accounts for the whole prefabricated constitution containing Ti, Mo The a series of samples such as 5%, 6%, 7%, 8%, 9%, 10% of amount.
The preparation method of the maceration extract is：
30h is fully ground using electric slurry machine after dispensing, fully dispersed uniform state is reached.Sent again Enter during vacuum impregnation fills, and vacuum impregnation is filled vacuumize and be less than limit residual voltage 13.33Pa.
Step 4, carbon fiber piston of the preparation containing carbon-silicon carbide matrix：
Precast body containing Ti, Mo obtained by step 3 is placed on Si powder or is embedded in Si powder, under vacuum atmosphere, in 1500 DEG C of progress siliconising processing；Density is obtained for 1.89g/cm3Semi-finished product.
Preferably, under vacuum atmosphere, the pressure in stove is 3~6Pa.
Siliconising money, first to vacuum reaction stove evacuation, it is 3~6Pa to be still less than furnace pressure；Then furnace temperature is raised in 7h 1500 DEG C, it is incubated 5h；Then furnace temperature is raised to 1750 DEG C using 1h again, is incubated 0.5h；Protection gas is finally done with argon gas, controlled Argon pressure is 2.5KPa, furnace cooling.
Step 5, prepare carbon fiber piston face coating：
Using plasma strengthens chemical vapour deposition technique, and semi-finished product will be obtained in step 4 and put plasma chemistry gas into Mutually deposition equipment in, by ionize carbon organic matter precursor its surface deposition obtain DLC (DLC) coating.Deng from During sub- techniques of deposition diamond-like rock layers, control furnace pressure for 10Pa, control depositing temperature for 60 DEG C~80 DEG C, deposit Power be 600W, deposit it is gases used be CH4And H2, the two flow is respectively 2.1mL/min and 6.4mL/min, sedimentation time For 15h~16h；Obtain the finished product that diamond-like coating thickness is 10 μm.
From the selection of piston, braiding, heavy carbon, dipping filler, siliconising to coating, this preparation explored of the invention The piston (finished product obtained by embodiment 1-3) that process is prepared is by piston machine fatigue test, and pin-and-hole is followed 30MPa's Under ring compression, operation 107Circulation flawless.Tested by piston fatigue, top land is by 3000 circulation thermal shock examinations Test rear flawless.Meet the durable examination of installation in 1100 hours under the conditions of engine speed 4300rpm, detonation pressure 30MPa.And have Self-lubricating and high temperature self-healing micromechanism of damage, fully meet the severe operating mode of piston, and service life is closed compared to cast-iron piston and aluminium Golden piston can double many.
In the specification of the present invention, numerous specific details are set forth.It is to be appreciated, however, that embodiments of the invention can be with Put into practice in the case of these no details.In some instances, known method, structure and skill is not been shown in detail Art, so as not to obscure the understanding of this description.
Finally it should be noted that：Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations； Although the present invention is described in detail with reference to foregoing embodiments, it will be understood by those within the art that：Its The technical scheme described in foregoing embodiments can still be modified, or it is special to which part or whole technologies Levy carry out equivalent；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention The scope of technical scheme, it all should cover among the claim of the present invention and the scope of specification.

Claims (10)

1. a kind of Cf/ C-SiC composites, it is characterised in that：The Cf/ C-SiC composites include carbon fiber precast body, base Body carbon, filler and DLC；Described matrix carbon is evenly affixed on the carbon fiber of precast body, is constituted with matrix carbon Carbon fiber precast body；The filler is filled in the prefabricated carbon fiber body with matrix carbon and is coated on the carbon with matrix carbon Fibre preforms are external, constitute semi-finished product, and the DLC is coated on formation diamond-like rock layers on semi-finished product；In the filler Contain Ti elements, Si elements, C element, Mo elements；Ti elements in filler are with any one in titanium carbide, silicon-carbon titanium or two The mode of kind is present；Si elements in filler exist with least one of SiC, simple substance Si, silicon-carbon titanium, molybdenum silicide mode；Filling C element in thing exists with least one of SiC, silicon-carbon titanium, silicon-carbon titanium mode；Mo elements in filler are with zeroth order molybdenum, silicon Change at least one of molybdenum, molybdenum carbide mode to exist.
2. a kind of C according to claims 1f/ C-SiC composites, it is characterised in that：
The Cf/ C-SiC composites contain silicon-carbon titanium phase, molybdenum silicide phase, molybdenum carbide phase.
3. a kind of C according to claims 1f/ C-SiC composites, it is characterised in that：
The semi-finished product that quality is B are chosen, measurement takes the quality sum of Ti elements and Mo elements in semi-finished product, and is defined as A, then A/B=0.04-0.08.
4. a kind of C according to claims 1f/ C-SiC composites, it is characterised in that：
Titanium and Mo mass ratio are 0.6-1.04:1.
5. a kind of C according to claims 1f/ C-SiC composites, it is characterised in that：
The density of carbon fiber precast body is 0.5-0.6g/cm3；
The density of carbon fiber precast body with matrix carbon is 1.3~1.4g/cm3；
The density of semi-finished product is 1.8~1.9g/cm3；
The CfThe density of/C-SiC composites is 1.82~1.92g/cm3。
6. one kind prepares the C as described in claim 1-5 any onefThe method of/C-SiC composites, it is characterised in that including under State step：
Step one
Carbon fiber is woven into precast body, chemical vapor infiltration depositing base carbon is then carried out；Density is obtained for 1.3~1.4g/ cm3The carbon fiber precast body with matrix carbon；The density of the precast body is 0.5~0.6g/cm3；
Step 2
Carbon fiber precast body with matrix carbon obtained by step one is placed in the maceration extract containing Ti, Mo and impregnated, after dipping, is done It is dry, obtain the precast body containing Ti, Mo；
Step 3
Precast body containing Ti, Mo obtained by step 2 is embedded in Si powder, under vacuum atmosphere, in 1500-1750 DEG C of progress Siliconising is handled；Density is obtained for 1.8~1.9g/cm3Semi-finished product；
Step 4
One layer of diamond-like rock layers are coated in surface of semi-finished obtained by step 3；Obtain finished product.
7. a kind of C according to claim 6fThe preparation method of/C-SiC composites, it is characterised in that：
In step one, the carbon fiber is mesophase pitch-based carbon fibers；
In step one, the precast body be three-dimensional four-way or three-dimensional five to acupuncture carbon felt porous preform；
In step one, during chemical vapor infiltration depositing base carbon, carbon-source gas used in propane, ethylene acetylene at least one Kind；
In step one, during chemical vapor infiltration depositing base carbon, at least one of the diluent gas used in argon gas, nitrogen；
In step one, during chemical vapor infiltration depositing base carbon, the intake velocity of carbon-source gas is 0.5-0.9L/min；Carrier gas The intake velocity of body is 2.5-3.3L/min；
In step one, during chemical vapor infiltration depositing base carbon, it is 5-6 DEG C/min to control heating rate；The depositing temperature is controlled to be 1000-1100℃、；Under depositing temperature, it is 450~600h hours to control soaking time.
8. a kind of C according to claim 6fThe preparation method of/C-SiC composites, it is characterised in that：
In step 2,
Carbon fiber precast body with matrix carbon obtained by step one is placed in the maceration extract containing Ti, Mo and carries out vacuum impregnation, is obtained To the precast body containing Ti, Mo；The maceration extract containing Ti, Mo by water, micrometer silicon carbide titanium, micron molybdenum, CMC in mass ratio, water： Micrometer silicon carbide titanium：Micron molybdenum：CMC=100-90:50-55:60-65:0.5-0.8 is constituted；During the vacuum impregnation, in equipment Air pressure is less than or equal to 13.33Pa；The vacuum impregnation time is 25h~32h；The granularity of the micrometer silicon carbide titanium is 20-50 microns；Institute The granularity for stating micron molybdenum is 20-50 microns；After the completion of vacuum impregnation, dry, obtain the precast body containing Ti, Mo；
In step 3, the precast body containing Ti, Mo obtained by step 2 is placed on Si powder or is embedded in Si powder, in vacuum atmosphere Under, carry out siliconising processing in 1500-1750 DEG C；Density is obtained for 1.8~1.9g/cm3Semi-finished product；
In step 4, semi-finished product obtained by step 3 are placed in cvd furnace, using plasma deposition technique deposition cladding diamond-like Rock layers；During plasma deposition technique depositing diamond-like layer, control furnace pressure for 3-13.33Pa, be preferably 5Pa, control is heavy Accumulated temperature degree is 60 DEG C~80 DEG C, deposition power is 600-620W, to deposit gases used be CH4And H2, the two flow is respectively 2.1- 2.4mL/min and 6.4-6.9mL/min, sedimentation time is 15h~16h；The diamond-like coating thickness is 8~10 μm.
9. a kind of C according to claim 8fThe preparation method of/C-SiC composites, it is characterised in that：
First to vacuum reaction stove evacuation in step 3, it is 3~6Pa to be less than furnace pressure；Then furnace temperature is raised to 1500 in 7~8h DEG C, it is incubated 5h；Then furnace temperature is raised to 1750 DEG C using 1h again, is incubated 0.5h；It is last that protection gas is done with argon gas, control Ar Pressure Power is 2.5KPa, furnace cooling.
10. one kind C as described in claim 1-5 any onefThe application of/C-SiC composites, it is characterised in that：Including by its As piston.
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CN116332663B (en) * 2023-03-02 2024-06-28 中南大学 Preparation method of carbon/carbon-silicon carbide composite material

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