CN1986490A - High strength and high toughness foamed SiC/Al material and its preparing method - Google Patents
High strength and high toughness foamed SiC/Al material and its preparing method Download PDFInfo
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Abstract
The present invention relates to heterogeneous foamed ceramic/metal material, and is especially one kind of high strength and high toughness foamed SiC/Al material and its preparation process. The foamed SiC/Al material has basic units of closed polygonal ring to form connected 3D network structure, and each of the closed polygonal ring units is heterogeneous foamed ribs comprising SiC in 50-95 vol% and metal Al in 5-50 vol% and with the relative density not lower than 99 %. The foamed SiC/Al material is prepared through organic foam soaking, hot pressing to densify, pressure injection filling, thermal decomposition and reaction sintering. The preparation process is simple and low in cost.
Description
Technical field
The invention belongs to ceramic/metal complex phase mesh perforated foams and technology of preparing thereof, a kind of high-strength and high ductility SiC/Al foam materials and preparation method thereof is provided especially.
Background technology
The mesh perforated foams by the body material skeleton, can change the aperture, higher porosity is formed, such material has the three-dimensional network skeleton structure and pore is interconnected, and is a kind of important multifunctional material.Such foam materials mainly contains foamed metal and foamed ceramics two big classes at present.Foamed metal has multiple functions such as damping, sound, heat, electromagnetic shielding, and its appearance meets this material new development trend of structured material multifunction, thereby nearly ten years are developed rapidly.Foamed ceramics is except the general characteristic that has porous ceramics and have, it also has high permeability, high-ratio surface and complicated characteristics such as pore passage structure, these characteristics make it can be used as high temperature filtration, purification, absorption, separation, mixing, heat insulation and heat exchange device in industries such as metallurgy, chemical industry, machinery, environmental protection, the energy, use very extensive.
The preparation method of foam metal material mainly contains metal deposition, powder metallurgy (PM) method, casting etc.Metal deposition be by the atomic state metal after organic porous matrix internal surface deposition, removing organism and sintering forms, this class porous metal porosity communication, porosity height (＞80%), has three-dimensional net structure, say it is a kind of type material of excellent performance in a sense, but its characteristic has determined its strength property to be very restricted, and production efficiency is not high; Powder metallurgy (PM) method is development a kind of method early, and this method is as raw material, through the process of moulding and sintering manufacturing porous metal with metal-powder (or powder mix of metal-powder and non-metal powder).But such porous metal aperture is mostly less than 0.3mm, and porosity generally is not higher than 30%, and article shape, size are very restricted; Casting prepares porous metal and is mostly to be formed after the foam process cooled and solidified by molten metal or alloy; Or rare gas element is blown into molten metal forms a large amount of bubble postcooling and solidify formation; Or make model with the organic foam of three-dimensional net structure, molten metal is flowed into remove organism in the model hole after the cooled and solidified and obtain, but goods mostly are the porous material of closed pore crack or half through hole greatly, and the material preparation cost is very high.
The foam silicon carbon pottery has following four kinds of methods preparation: powder sintering, solid state reaction sintering process, contain silicone resin pyrolysis method and vapour deposition process.Powder sintering is divided into two kinds of different processes again.After the first will contain the slip of the carborundum powder of a certain amount of sintering aid and linking agent (as ethyl silicate hydrolyzed solution, silicon sol etc.) furnishing suitable concn, soak and hang on the polyurethane foam, after solidifying drying, deviate from linking agent and polyurethane foam 200～600 ℃ of scopes.Then, temperature is elevated to carries out sintering between 1500～2200 ℃ and just obtain foamed silicon carbide ceramics; Another kind method is with after containing the carborundum powder and strain shape whipping agent uniform mixing of sintering aid, with mold pressing or pouring procedure moulding.Deviate from whipping agent by fusing or gasification, carry out high temperature sintering then to obtain the spumescence silicon carbide ceramics; The solid state reaction sintering process is with strain shape whipping agent and silica flour and the moulding of carbon dust uniform mixing.Deviate from whipping agent by fusing or gasification, through promptly obtaining the spumescence silicon carbide ceramics behind the pyroreaction sintering; Containing the silicone resin pyrolysis method is that the organosilicon presoma is made high-molecular gel, obtains the foamed silicone resin that contains after deviating from the organic solvent in the gel, carries out pyrolysis and promptly obtain the spumescence silicon carbide ceramics after fully giving oxidation; To be the method for utilizing chemical vapour deposition with silicon carbide deposit on the netlike carbon fiber knitted body vapour deposition process and obtain the spumescence silicon carbide ceramics.Above-mentioned four kinds of methods all have deficiency separately.First three methods is not owing to there is hot pressing, and initial density is not high, and the spumescence silicon carbide ceramics of preparation is not fine and close, thereby intensity is low, and solid state reaction sintering process and contain silicone resin pyrolysis method volume of voids and size is difficult to control; And vapour deposition process faces the cost of manufacture height, and speed waits problem slowly.These problems make the application of spumescence silicon carbide ceramics, and particularly new application is subjected to restriction in various degree.
Tradition mesh porous foam is because the unicity that the matrix framework material is formed, or be metal or for ceramic, and makes its performance have limitation, and then limits the multifunctionality of its use.Metal foam is easily oxidation in high temperature, and intensity is reduced greatly, and hardness generally is not very high, and wear resisting property is poor, especially under the washing away of high temperature even high pressure fluid the mis-behave embodiment still be remarkable.Ceramic foam is high temperature resistant, corrosion-resistant but heat conductivility is not high, poor high temperature stability, especially the intrinsic fragility of ceramic intrinsic become its as structural element biggest obstacle, and processing and install and all to have a technical difficult problem that is difficult to overcome, adopt ZrO at present
2The Research on Toughening of particle or fiber grade in an imperial examination two relative stupaliths is a lot, also have to adopt and prepare the method that ceramic matric composite comes the reinforcing structure pottery, it is very difficult that but these methods are applied in the preparation of porous ceramics, and effect is also not obvious, if in the mesh porous foam, metal and ceramic fusion are got up, form a kind of base material and strengthening phase and be continuous state, and make the two become three-dimensional successive structure separately at micro-scale, the high tenacity that just can utilize metal is to the three-dimensional toughness that increases the mesh porous foam ceramic that connects of ceramic phase base material, improve anti-brittle failure ability of foamed ceramics and thermostability, the lot of advantages of metallic substance is (as Cu simultaneously, Al etc. have high heat conduction, high electricity is led) also can in pottery, play a role and improve the relevant characteristic of foamed ceramics, it is high tough to make foamed ceramics obtain under dystectic situation like this, hardness is big, strong anti-oxidant and wear resistance, and have certain ductility and good thermal stability.
Summary of the invention
The object of the present invention is to provide a kind of high-strength and high ductility SiC/Al foam materials and preparation method thereof, that the SiC/Al foam materials of the present invention preparation has is high-strength, the characteristics of high-ductility, high thermal conductivity, high conductivity, porous, high-ratio surface and high through-hole rate, and pore structure (aperture and void content) can be regulated and control.Preparation method's technology provided by the invention is simple, easy to operate, need not complex apparatus, low cost of manufacture.
Technical scheme of the present invention is:
The invention provides a kind of high-strength and high ductility SiC/Al foam materials, wherein said SiC/Al foam materials is an elementary cell with polygonal Closed loop, and each elementary cell is interconnected to form three-dimensional networks; Constitute the unitary complex phase foam of Polygons Closed loop muscle and comprise that silicon carbide and aluminum metallic matrix form, and form to regulate and control, percentage ratio meter by volume, silicon carbide can change 95～50%, and the Al metallographic phase can change 5～50%; The relative density of muscle 〉=99%.
The present invention also provides the preparation method of above-mentioned high-strength and high ductility SiC/Al foam materials, with carborundum powder, silica flour (or mixed powder of carborundum powder and silica flour) and the resin that has than high carbon output rate is raw material, with the polyurethane foamed plastic is template, and preparation process is as follows:
(1) slip preparation
Powder of solid particles, macromolecular material, solidifying agent and organic solvent are mixed in proportion, mass percent example between powder of solid particles, macromolecular material, the solidifying agent is 70wt%～20wt%: 20wt%～70wt%: 1wt%～10wt%, ball milling after mechanical stirring, filter, get slip, described slurry solution solute is 5～70% of a total mass;
(2) soak extension
Polyurethane foamed plastic is cut into desired shape and size, immerse in the slip equably, take out afterwards to squeeze and go unnecessary slip, employing air-blowing or air-blowing to remove unnecessary slip in conjunction with the centrifugal mode, the heating semicure, under 50～80 ℃ of temperature, solidify, 5～60 minutes time, the above-mentioned material, material extrusion, solidification process of soaking repeats repeatedly, reaches needed percent by volume 5-85%, obtains the organic compound prefabricated skeleton body of foam;
(3) hot-pressing densification
The compound precast body of foam organic backbone is put into high pressure vessel, charge into nitrogen or argon gas and carry out high temperature, high pressure curing, obtain the fine and close organic compound precast body of foam (abbreviating foam preform as).
(4) pyrolysis
The organic compound prefabricated skeleton body of the foam of densification under the protection of argon gas, nitrogen or other rare gas element or pyrolysis under vacuum condition, is generated carbonaceous foam framework; Wherein the temperature rise rate per minute is 1～10 ℃, is warming up to 600～1200 ℃, is incubated 0.5～2 hour;
(5) fill the carbon skeleton centre hole
Because polyamine fat vacuole foam is burnt after the pyrolysis, stays centre hole in foamy carbon skeleton muscle.Under the situation of the high ceramic volumetric percentage ratio of needs, be necessary centre hole ground paste filling in the muscle, thus the density of raising skeleton.Specific practice is: after the centre hole mill on carbon skeleton surface is opened, utilize the vacuum suction will fill slip in conjunction with the method for high pressure pressure injection and be pressed in the centre hole.Again through obtaining the higher foamy carbon skeleton of density after curing in the above-mentioned steps 3 and the pyrolysis in the step 4.The number of times of this step can be selected according to the height of the ceramic volumetric percentage ratio in the foam materials of final acquisition.
(6) liquid phase reaction infiltration
Foamy carbon skeleton fine and close after the pyrolysis is desired shape and size through being machined to; carry out the reaction sintering infiltration then; infiltration carries out under protection of inert gas atmosphere or vacuum condition; temperature rise rate is 1～50 ℃ of per minute (being preferably 5～20 ℃); melt temperature is: 1300～1900 ℃; be incubated 0.5～5 hour, get the SiC/Al foam materials.
Macromolecular material of the present invention can be selected from one or more of Resins, epoxy, resol, furfuryl resin; Organic solvent can be acetone, ethanol etc., the powder of solid particles that can also sneak in described macromolecular material can be carborundum powder, silica flour or the mixed powder of the two, the mean particle size of powder can be between 10nm～25 μ m, add-on is 5～90% percent by volumes, is good with 40～60% percent by volumes.When adopting carborundum powder and silica flour mixed powder, the two mass ratio is 20～80%: 80～20%.
Solidifying agent of the present invention is: product, oxalic acid or citric acid etc. are taken off in tosic acid, five Lip rivers, and content is 1～40% of weight resin, is good with 2～8%, heat curing temperature between 100～250 ℃, 10 minutes～2 hours time.
In hot-pressing densification process of the present invention, pressure is that 5～22MPa, temperature are that heat-up rate is 1～5 ℃/min, is incubated 10 minutes～3 hours at 100～300 ℃.
In pyrolytic process of the present invention, 1～10 ℃ of temperature rise rate per minute is warming up to 600～1200 ℃, is incubated 0.5～2 hour; Best 600～1200 ℃ of pyrolysis temperature, best 2～4 ℃/min of temperature rise rate.
Fill carbon skeleton centre hole process in the present invention and be the method for utilizing the high pressure pressure injection and will fill slip and be pressed in the centre hole, pressure is 5～22MPa, pressurize 10 minutes～2 hours.
The raw material of selecting for use in the reaction sintering infiltration of the present invention is an aluminum silicon alloy, and the content of Si can also add other useful metallic elements at 90～5% (by weight percentage) in the alloy, as: Cu, Fe, Ni, Co, Ti, Zr, Cr, Mg, Ce etc.Sintering stove of the present invention can be vacuum induction process furnace, vacuum carbon tube furnace and vacuum resistance furnace etc.
In a word, process of the present invention is: the polymer of powder of solid particles (carborundum powder, silica flour or the two mixed powder) and high carbon output rate is mixed and made into slip.Select the polyurethane foam plastic in suitable aperture, and be cut into needed shape and size, then it is immersed in the slip, after the taking-up, remove unnecessary slip with extruding, wind, mode such as centrifugal, semicure repeats repeatedly, to reaching needed percent by volume, obtain the organic compound prefabricated skeleton body of foam.High temperature, high pressure solidify in high pressure vessel, to improve the initial density of the organic compound prefabricated skeleton body of foam.Foams after solidifying are carried out Polyurethane remove and the resin pyrolysis in vacuum or inert atmosphere furnace, obtain and the equiform foamy carbon skeleton of forming by solid powder particle and RESEARCH OF PYROCARBON of original foam polyurethane.On this basis, carry out the reaction sintering infiltration.Used alloy is an aluminum silicon alloy.Aluminum silicon alloy is heat fused under vacuum or protective atmosphere, forms superheated melt.Silicon in the melt and the reaction of the carbon in the carbon skeleton generate silicon carbide, and combine closely with the original silicon-carbide particle in the foam framework, wherein the space that produces after the organic polymer pyrolysis is then filled by aluminium alloy melt, thereby obtains high-strength, high-ductility, high fine and close SiC/Al foam materials.
The present invention has developed a kind of method for preparing high strength, high tenacity, high fine and close SiC/Al foam materials on organic foam body impregnation technology prepares the technology basis of foamed ceramics, have following advantage:
1, the SiC/Al foam materials has characteristics such as the easy control of porous, high-ratio surface, high through-hole rate, aperture and voidage.
Polyurethane foam plastic is the primary template that obtains final SiC/Al foam materials, thereby by selecting different templates just can control pore size in the three-dimensional net structure; For same template, can hang number of times and pulp density by selecting to soak to soak in the extension process, realize control, and eliminate closed pores the thickness of ceramic volumetric percentage ratio in the foam preform and prefabricated skeleton body muscle.Fig. 1 is the SiC/Al foam materials photo in kind that is made by the present invention.
2, high strength, high tenacity, high-compactness, good mechanical performance
The present invention adopts the method for the organic compound prefabricated skeleton body of hot-press solidifying foam, can significantly improve its initial density and homogeneity of structure, eliminates demixing phenomenon, and then avoids " dead skin is hollow " problem of causing because of layering; Adopt the liquid phase reaction infiltration that the network muscle of SiC/Al foam materials is had near 100% relative density and the even fine and closely woven microstructure of 0.5-15 μ m, can also make simultaneously silicon and the reaction of the carbon in the carbon skeleton in the metal solution generate silicon carbide, and the original silicon-carbide particle in the foam framework is firmly bonded to together in chemically combined mode, have very high bonding strength in the network muscle between ceramic phase thereby make.Meanwhile, the Al silicon alloy is filled in the space that stays after the prefabricated skeleton body heat is separated, and forms the three-dimensional net structure of mutual perforation on micro-meter scale with silicon carbide.Above factor makes the SiC/Al foam materials possess high intensity and high toughness simultaneously.(seeing accompanying drawing 2,3).
3, pottery, metallographic phase adjustable ratio, the metallographic phase composition is adjustable
In the slip layoutprocedure, the ratio of SiC powder and organic polymer resin can be produced the even hole of different volumes ratio in the adjusting powder of solid particles in the carbon skeleton precast body, these uniform holes are filled by the infiltrated metal raw material in the liquid phase reaction infiltration, and then can obtain the metallographic phase of different volumes ratio; The infiltrated metal raw material is selected the Al-Si alloy for use, the content of Si can be at 90～5% (by weight percentage) in the alloy, can also add other useful metallic elements, as: Cu, Fe, Ni, Co, Ti, Zr, Cr, Mg, Ce etc., it is adjustable that the metallographic phase composition is realized.
4, rigidity, intensity and high-temperature behavior significantly are better than foam Al; Heat conductivility and conductivity all are better than the SiC foamed ceramics
The restriction that traditional foam Al is made up of its starting material, rigidity and intensity are low and be difficult to use as structural part, and the high-temperature behavior difference limits its use temperature and is difficult to above 200 ℃.And the SiC/Al foam materials that the present invention makes can SiC ceramic main phase, and the high temperature use properties is good; It consists of SiC and remaining Si traditional foam silicon carbon stupalith, this kind phase composite determines its heat conductivility and conductivity not high, and the foam SiC/Al metal composite that the present invention makes consists of SiC and Al phase, thereby high heat-conducting property and conductivity are arranged.
5, good formability and processibility
First, as the primary template of composite material of foamed metal, polyurethane foam plastic very easily is processed into arbitrary shape; Second, precast body has favorable mechanical and electromachining performance through the carbon skeleton that contains ceramic raw material of pyrolysis or acquisition, the very easy part body that is processed into different shape and dimensional requirement; Three, the liquid phase reaction infiltration almost is a process of not having distortion, and the SiC/Al foam materials that obtains needn't carry out post-treatment.Above-mentioned 3 factors make the SiC/Al foam materials possess good formability and processing characteristics, make tooling cost thereby reduce it greatly.
In sum, the invention provides a kind of new, cheap high-strength and high ductility SiC/Al foam materials and preparation method thereof.In the method, organic foam body dipping, hot-press solidifying, pressure injection are filled centre hole, polymer pyrolysis and reaction sintering and are combined, make the foam SiC/Al metal composite of preparing have porous, high-ratio surface and high through-hole rate, and pore structure can be regulated and control, the characteristics that aperture, voidage are easy to control; Three-dimensional network muscle density height (can reach nearly 100%), pottery, metallographic phase adjustable ratio, the metallographic phase composition is adjustable; Three-dimensional network muscle condition of surface can arbitrarily design; Material heat conduction is good, foams high strength, characteristics such as high tenacity.
Description of drawings
Fig. 1 is the photo in kind of SiC/Al foam materials.
Fig. 2 is the tough break pattern of SiC/Al foam materials muscle.
Fig. 3 is the tough break microstructure of SiC/Al foam materials muscle inside.
Embodiment
Below by embodiment in detail the present invention is described in detail.
Embodiment 1
The mean particle size 5 μ m carborundum powders, ammonia resol, the tosic acid that weight ratio are respectively 55%: 40%: 5% are dissolved in the dehydrated alcohol altogether, make slip, and described slurry solution solute is 50% of a gross weight; The polyamine fat vacuole foam of aperture 2mm cut into require to immerse equably in the described slip after the size, soaked 1 minute, squeeze after taking out and remove unnecessary slip, air-dry back 50 ℃ of semicures 15 minutes, the said process repeated multiple times is up to the pre-determined volume percentage ratio (percent by volume of complex phase foam muscle in the finished product) that reaches 30%.Then, put into high pressure vessel, charge into nitrogen and make air pressure reach 15MPa, 1 ℃ of temperature rise rate per minute is warming up to 230 ℃, is incubated curing in 1.5 hours.Pyrolysis under argon shield generates carbon skeleton; Wherein the temperature rise rate per minute is 2 ℃, is warming up to 800 ℃, is incubated 0.5 hour.After the pyrolysis, the centre hole mill on carbon skeleton surface is opened, in high pressure vessel, with viscosity is that the slip of 200mPa.s is pressed in the centre hole, pressure 5MPa, pressurize 20 minutes is pressed that above-mentioned parameter solidifies again, after the pyrolysis, is carried out the vacuum reaction infiltration, 1450 ℃ of temperature of reaction, temperature rise rate is 15 ℃/minute, is incubated 1 hour, and the infiltration raw material is Al77.5Si20Cu2Mg0.5 (Wt%) alloy, obtain the SiC/Al foam materials, complex phase foam muscle relative density is 99%, and silicon carbide average crystal grain granularity is 2 μ m, and the metallographic phase mean sizes is 3 μ m; Complex phase foam muscle consist of SiC and Al alloy phase, percentage ratio meter by volume, in the complex phase foam muscle, silicon carbide accounts for 85%, aluminium alloy accounts for 15% mutually, gained SiC/Al foam materials ultimate compression strength is 31MPa.
Embodiment 2
Weight ratio was respectively 40%: 20%: 35%: 5% mean particle size 2 μ m carborundum powders, silica flour, ammonia resol, tosic acid are dissolved in the dehydrated alcohol altogether, make slip, and described slurry solution solute is 60% of a gross weight; The polyamine fat vacuole foam of aperture 1mm cut into require to immerse equably in the described slip after the size, soaked 1 minute, squeeze after taking out and remove unnecessary slip, air-dry back 50 ℃ of semicures 30 minutes, the said process repeated multiple times is up to the pre-determined volume percentage ratio (percent by volume of complex phase foam muscle in the finished product) that reaches 45%.Then, put into high pressure vessel, charge into nitrogen and make air pressure reach 12MPa, 2 ℃ of temperature rise rate per minutes are warming up to 250 ℃, are incubated curing in 1 hour.Pyrolysis under argon shield generates carbon skeleton; Wherein the temperature rise rate per minute is 2 ℃, is warming up to 800 ℃, is incubated 0.5 hour.After the pyrolysis, the centre hole mill on carbon skeleton surface is opened, in high pressure vessel, with viscosity is that the slip of 200mPa.s is pressed in the centre hole, pressure 10MPa, pressurize 40 minutes is pressed above-mentioned parameter again and is solidified, after the pyrolysis, carry out the vacuum reaction infiltration, 1500 ℃ of temperature of reaction, temperature rise rate are 10 ℃/minute, are incubated 1.2 hours, the infiltration raw material is Al70Si30 (Wt%) alloy, obtain the SiC/Al foam materials, complex phase foam muscle relative density is 99%, and silicon carbide average crystal grain granularity is 5 μ m, the metallographic phase mean sizes is 7 μ m, complex phase foam muscle consist of SiC and Al-Si alloy phase, percentage ratio meter by volume is in the complex phase foam muscle, silicon carbide accounts for 75%, and the Al-Si alloy phase accounts for 25%; Gained SiC/Al foam materials ultimate compression strength is 43MPa.
Weight ratio was respectively 35%: 15%: 40%: 10% mean particle size 3.5 μ m carborundum powders, silica flour, Resins, epoxy (trade mark is EP0141-310), tosic acid are dissolved in the dehydrated alcohol altogether, make slip, described slurry solution solute is 45% of a gross weight; The polyamine fat vacuole foam of aperture 4mm cut into require to immerse equably in the described slip after the size, soaked 1 minute, squeeze after taking out and remove unnecessary slip, air-dry back 50 ℃ of semicures 10 minutes, the said process repeated multiple times is up to the pre-determined volume percentage ratio (percent by volume of complex phase foam muscle in the finished product) that reaches 25%.Then, put into high pressure vessel, charge into nitrogen and make air pressure reach 10MPa, 5 ℃ of temperature rise rate per minutes are warming up to 200 ℃, are incubated curing in 1.5 hours.Pyrolysis under argon shield generates carbon skeleton; Wherein the temperature rise rate per minute is 2 ℃, is warming up to 900 ℃, is incubated 0.5 hour.After the pyrolysis, the centre hole mill on carbon skeleton surface is opened, in high pressure vessel, with viscosity is that the slip of 200mPa.s is pressed in the centre hole, pressure 15MPa, pressurize 1 hour is pressed above-mentioned parameter again and is solidified, after the pyrolysis, carry out the vacuum reaction infiltration, 1650 ℃ of temperature of reaction, temperature rise rate are 20 ℃/minute, are incubated 1 hour, the infiltration raw material is Al73Si15Fe8Ce4 (Wt%) alloy, obtain the SiC/Al foam materials, complex phase foam muscle relative density is 99%, and silicon carbide average crystal grain granularity is 2.5 μ m, the metallographic phase mean sizes is 4.5 μ m, complex phase foam muscle consist of SiC and Al alloy phase, percentage ratio meter by volume is in the complex phase foam muscle, silicon carbide accounts for 80%, and aluminium alloy accounts for 20% mutually; Gained SiC/Al foam materials ultimate compression strength is 21MPa.
Embodiment 4
Weight ratio is respectively 54% and 40% heat-reactive phenolic resin and furfuryl resin (wherein, heat-reactive phenolic resin weight ratio 60%, furfuryl resin weight ratio 40%) be dissolved in the dehydrated alcohol altogether with 6% citric acid, make slurry solution, the carborundum powder and the silica flour (mass ratio is 30: 80) that with mean particle size are 10 μ m again evenly add in the above-mentioned solution, forming resin/powder volume ratio is 5: 5 slip, and described slurry solution solute is 50% of a gross weight; The polyamine fat vacuole foam of aperture 2.5mm cut into require to immerse equably in the described slip after the size, soaked 1 minute, squeeze after taking out and remove unnecessary slip, air-dry back 50 ℃ of semicures 10 minutes, the said process repeated multiple times is up to the pre-determined volume percentage ratio (percent by volume of complex phase foam muscle in the finished product) that reaches 60%.Then, put into high pressure vessel, charge into nitrogen and make air pressure reach 10MPa, 2.5 ℃ of temperature rise rate per minutes are warming up to 200 ℃, are incubated curing in 1 hour.Pyrolysis under argon shield generates carbon skeleton; Wherein the temperature rise rate per minute is 2 ℃, is warming up to 1000 ℃, is incubated 0.5 hour.After the pyrolysis, the centre hole mill on carbon skeleton surface is opened, in high pressure vessel, with viscosity is that the slip of 200mPa.s is pressed in the centre hole, pressure 22MPa, pressurize 2 hours is pressed above-mentioned parameter again and is solidified, after the pyrolysis, infiltration under argon shield atmosphere, 1700 ℃ of temperature of reaction, temperature rise rate are 10 ℃/minute, are incubated 1 hour, the infiltration raw material is Al88.5Si10ColZr0.5 (Wt%) alloy, obtain the SiC/Al foam materials, complex phase foam muscle relative density is 99%, and silicon carbide average crystal grain granularity is 4.5 μ m, the metallographic phase mean sizes is 11 μ m, complex phase foam muscle consist of SiC and Al alloy phase, percentage ratio meter by volume is in the complex phase foam muscle, silicon carbide accounts for 76%, and aluminium alloy accounts for 24% mutually; Gained SiC/Al foam materials ultimate compression strength is 54MPa.
Embodiment 5
Weight ratio is respectively 35% and 60% heat-reactive phenolic resin and furfuryl resin (wherein, heat-reactive phenolic resin weight ratio 50%, furfuryl resin weight ratio 50%) taking off product with 5% 5 Lip river is dissolved in the dehydrated alcohol altogether, make slurry solution, the carborundum powder and the silica flour (weight ratio is 60: 40) that with mean particle size are 6.5 μ m again evenly add in the above-mentioned solution, forming resin/powder volume ratio is 6/4 slip, and described slurry solution solute is 65% of a gross weight; The polyamine fat vacuole foam of aperture 3.5mm cut into require to immerse equably in the described slip after the size, soaked 1 minute, squeeze after taking out and remove unnecessary slip, air-dry back 50 ℃ of semicures 30 minutes, the said process repeated multiple times is up to the pre-determined volume percentage ratio (percent by volume of complex phase foam muscle in the finished product) that reaches 50%.Then, put into high pressure vessel, charge into nitrogen and make air pressure reach 15MPa, 3.5 ℃ of temperature rise rate per minutes are warming up to 240 ℃, are incubated curing in 1 hour.Pyrolysis under argon shield generates carbon skeleton; Wherein the temperature rise rate per minute is 2 ℃, is warming up to 1200 ℃, is incubated 0.5 hour.After the pyrolysis, the centre hole mill on carbon skeleton surface is opened, in high pressure vessel, with viscosity is that the slip of 200mPa.s is pressed in the centre hole, pressure 18MPa, pressurize 100 minutes is pressed above-mentioned parameter again and is solidified, after the pyrolysis, infiltration under argon shield atmosphere, 1450 ℃ of temperature of reaction, temperature rise rate are 20 ℃/minute, are incubated 1 hour, the infiltration raw material is Al50Si50 (Wt%) alloy, obtain the SiC/Al foam materials, complex phase foam muscle relative density is 99%, and silicon carbide average crystal grain granularity is 4 μ m, the metallographic phase mean sizes is 14 μ m, complex phase foam muscle consist of SiC and Al-Si alloy phase, percentage ratio meter by volume is in the complex phase foam muscle, silicon carbide accounts for 79%, and the Al-Si alloy phase accounts for 21%; Gained SiC/Al foam materials ultimate compression strength is 49MPa.
Claims (10)
1. high-strength and high ductility SiC/Al foam materials, it is characterized in that: described foam materials is an elementary cell with polygonal Closed loop, and each elementary cell is interconnected to form three-dimensional networks; The complex phase foam muscle that constitutes three-dimensional networks comprises silicon carbide and Al metallographic phase, and two phase composites can be regulated and control within the specific limits, percentage ratio meter by volume, and silicon carbide is in 95～50% scopes, and the Al metallographic phase is in 5～50% scopes; Relative density 〉=99% of complex phase foam muscle, average grain size is at 1/ μ m-15 μ m.
2. preparation method by the described high-strength and high ductility SiC/Al of claim 1 foam materials, it is characterized in that: is raw material with powder of solid particles with the macromolecular material that has than high carbon output rate, with the polyurethane foamed plastic is template, wherein, powder of solid particles is carborundum powder, silica flour or the two powder mix, and concrete preparation process is as follows:
(1) slip preparation
Powder of solid particles, macromolecular material, solidifying agent and organic solvent are mixed in proportion, weight percent between powder of solid particles, macromolecular material, the solidifying agent is 70wt%～20wt%:20wt%～70wt%:1wt%～10wt%, ball milling after mechanical stirring, filter, get slip, described slurry solution solute is 5～70% of a total mass;
(2) soak extension
Polyurethane foamed plastic is cut into desired shape and size, immerse in the slip equably, take out afterwards to squeeze and go unnecessary slip, employing air-blowing or air-blowing to remove unnecessary slip in conjunction with the centrifugal mode, the heating semicure, under 50～80 ℃ of temperature, solidify, time 5-60 minute, the above-mentioned material, material extrusion, solidification process of soaking repeats repeatedly, reaches needed percent by volume 5-85%, obtains the organic compound prefabricated skeleton body of foam;
(3) hot-pressing densification
The organic compound prefabricated skeleton body of foam is put into high pressure vessel, charge into nitrogen or argon gas, high temperature, high pressure solidify, pressure is that 5～22MPa, temperature are at 100～300 ℃, 1～5 ℃ of heat-up rate is incubated 10 minutes～3 hours, obtains the organic compound prefabricated skeleton body of foam of homogeneous microstructure, densification;
(4) pyrolysis
The organic compound prefabricated skeleton body of the foam of densification under the protection of nitrogen, argon gas or other rare gas element or pyrolysis under vacuum condition, is generated carbonaceous foam framework; Wherein the temperature rise rate per minute is 1～10 ℃, is warming up to 600～1200 ℃, is incubated 0.5～2 hour;
(5) filled and process carbon skeleton centre hole
After the centre hole on carbon skeleton surface mill opened, will fill slip and be pressed in the centre hole; Again through obtaining the higher foamy carbon skeleton of density after curing in the step 3 and the pyrolysis in the step 4; The number of times of this step is selected according to the height of the ceramic volumetric percentage ratio in the final foam materials that obtains;
(6) liquid phase reaction infiltration
Foamy carbon skeleton fine and close after the pyrolysis is desired shape and size through being machined to; carry out the reaction sintering infiltration then; infiltration carries out under protection of inert gas atmosphere or vacuum condition; temperature rise rate is 1～50 ℃ of a per minute; melt temperature is: 1300～1900 ℃; be incubated 0.5～5 hour, get the SiC/Al foam materials.
3. according to the preparation method of the described high-strength and high ductility SiC/Al of claim 2 foam materials, it is characterized in that: described macromolecular material is selected from one or more of Resins, epoxy, resol and furfuryl resin.
4. according to the preparation method of the described high-strength and high ductility SiC/Al of claim 2 foam materials, it is characterized in that: described organic solvent is ethanol or formaldehyde, solvent volume concentration 〉=75%.
5. according to the preparation method of the described high-strength and high ductility SiC/Al of claim 2 foam materials, it is characterized in that: the mean particle size of described carborundum powder and silica flour is 10nm～25 μ m, and silica flour and carborundum powder purity are more than 95%.
6. according to the preparation method of the described high-strength and high ductility SiC/Al of claim 2 foam materials, it is characterized in that: when adopting carborundum powder and silica flour mixed powder, the two part by weight is 20～80%: 80～20%.
7. according to the preparation method of the described high-strength and high ductility SiC/Al of claim 2 foam materials, it is characterized in that: described solidifying agent is that product, oxalic acid or citric acid are taken off in tosic acid, five Lip rivers, content is 1～40% of resin quality, solidifies 10 minutes～2 hours time under 100～250 ℃ of temperature.
8. according to the preparation method of the described high-strength and high ductility SiC/Al of claim 2 foam materials, it is characterized in that: in the described step (5), filled and process carbon skeleton centre hole process is utilized the method for high pressure pressure injection will fill slip and is pressed in the centre hole, and pressure is 5～22MPa, pressurize 10 minutes～2 hours.
9. according to the preparation method of the described high-strength and high ductility SiC/Al of claim 2 foam materials, it is characterized in that: a conventional oven or shrinking machine are adopted in the curing in the sluny impregnation process; The high pressure vessel that foam framework precast body hot-pressing densification adopts is reactor or hot isostatic press; The pyrolysis stove is carbon tube furnace or vacuum induction process furnace; The sintering stove is vacuum induction sintering oven, vacuum carbon tube furnace or vacuum resistance furnace.
10. according to the preparation method of the described high-strength and high ductility SiC/Al of claim 3 foam materials, it is characterized in that: in the described step (6), the raw material of selecting for use in the reaction sintering infiltration is an aluminum silicon alloy, and by weight percentage, the content of Si is 90～5% in the alloy; Perhaps, add one or more of other useful metallic element: Cu, Fe, Ni, Co, Ti, Zr, Cr, Mg, Ce in the aluminum silicon alloy.
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