CN102352472A - Silicon nitride and aluminum double continuous phase composite material and preparation method thereof - Google Patents
Silicon nitride and aluminum double continuous phase composite material and preparation method thereof Download PDFInfo
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- CN102352472A CN102352472A CN2011102010220A CN201110201022A CN102352472A CN 102352472 A CN102352472 A CN 102352472A CN 2011102010220 A CN2011102010220 A CN 2011102010220A CN 201110201022 A CN201110201022 A CN 201110201022A CN 102352472 A CN102352472 A CN 102352472A
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Abstract
Provided is a silicon nitride and aluminum double continuous phase composite material, wherein, an aluminum phase is cast aluminum alloy with copper, the volume of the aluminum phase is 30% to 60% of the total volume of the composite material, an silicon nitride phase is a beta phase, and the beta-Si3N4 phase and the aluminum phase are distributed in the way of a bicontinuous phase; that is, the beta-Si3N4 phase and the aluminum phase form an interprepenetrating polymer network. A preparation method for the composite material is as follows: a green body and a preformed body of silicon nitride are prepared; the preformed body of silicon nitride and aluminum alloy are placed in a high temperature crucible which is subjected to pressureless infiltration in a vacuum furnace; after cooled, the high temperature crucible is placed in a muffle furnace for heating; after aluminum liquid is totally fused, an infiltrated sample of the composite material is taken out and placed in the muffle furnace for T6 heat treatment; newly-prepared preformed bodies of silicon nitride are continued to be infiltrated in fused aluminum liquid, and above-mentioned procedures are repeated so as to realize continuous preparation. The preparation method provided in the invention has the advantages of a simple process and low cost and can be used for preparing composite materials of a variety of complex shapes; and the silicon nitride and aluminum double continuous phase composite material prepared by the method has excellent mechanical performance.
Description
Technical field
The present invention relates to a kind of matrix material, be specifically related to a kind of silicon nitride and aluminium co-continuous phase composite materials and preparation method thereof.
Background technology
The fiber reinforcement aluminum matrix composite is with its high specific tenacity, specific rigidity, axial tensile strength and wear resistance; Outstanding high temperature resistance and low thermal expansivity; Good advantages such as dimensional stability under favorable conductive, thermal conductivity, fatigue resistence and humidity or the radiation environment; In fields such as space flight and aviation, automobile, mechano-electronics as the high-strength high temperature-resistant material, demonstrate huge application potential.The method of manufacture of fiber reinforcement aluminum matrix composite mainly contains infiltrated with molten metal method, pressure casting method, diffusion bonding method and powder metallurgic method etc.
(1) infiltrated with molten metal method
The infiltrated with molten metal method is to soak into fibrous bundle with liquid aluminium and duraluminum, or with fibrous bundle through liquid aluminium and duraluminum molten bath, every fiber is melted remove unnecessary metal covering behind the wetting metal to obtain composite filament, make matrix material through extruding again.Its shortcoming is when fiber is easy to soaked into, and molten aluminum and duraluminum may cause damage to fibre property.Referring to Tanaka Lang Ping, " fiber-reinforced metal matrix composite ", metallurgical industry press, 1986.
(2) diffusion bonding method
The diffusion bonding method mainly is meant aluminium foil and the fiber yarn that after surface treatment, soaks into aluminium liquid or composite filament or single plate by the order specified lamination, under vacuum or inert gas conditions through high-temperature pressurizing diffusion bonding moulding to obtain the method for manufacture of aluminum matrix composite.In addition, diffusion bonding method also comprises normal pressure-sintered method, pressure sintering, high temperature ironing.Being illustrated in is suitable, " metal-base composites and technology of preparing thereof ", Chemical Industry Press, ISBN number: 7502592571.
(3) powder metallurgic method
Powder metallurgic method is the traditional development of powder metallurgical technique in new engineering materials preparation.Perfect along with the development of flouring technology and dispersing technology method, people have utilized powder metallurgic method successfully to prepare the aluminum matrix composite of a large amount of excellent performances.They have not only that height ratio is strong, height ratio mould, low bulk, high wear-resistant characteristics, and random adjusting process route.Wild phase is evenly distributed in the aluminum matrix composite of this method preparation, and surface reaction is easy to control, on performance and stability, is superior to the material of other process method preparation greatly.Referring to Chinese patent CN1487109 " powder metallurgy self-generating ceramic particle reinforced aluminium base composite material and preparation method thereof ".
(4) pressure casting method
Pressure casting method is to make molten aluminum and duraluminum force to be pressed into the fixedly die cavity of built-in fabric prefab, and pressure is applied to always and solidifies end.Pressure casting method has improved the wellability of metal melt because of high pressure, and the reaction between the fortifying fibre of obtained matrix material and aluminium and duraluminum is minimum, and routine casting defectives such as hole and shrinkage cavity are less.Casting pressure and reinforced fiber content have considerable influence to the performance of aluminum matrix composite.Referring to Peng L M.Mechanical properties of ceramic-metal composites by pressure infiltration of metal into porous ceramics; Materials Science and Engineering A; 2004,374:1-9.
(5) pressure-free impregnation method
The pressure-free impregnation method is belong to liquid phase process a kind of, because the singularity of its technology is listed separately.The pressure-free impregnation method refers under vacuum or condition of normal pressure, precast body contacted with molten metal or macromolecular material, and be motivating force with the capillary force, make liquid metal or polymer spontaneous infiltration go into precast body, form the technology of densified composite.Propose by U.S. Rand Corporation at first, and be successfully applied to some ceramic/metal composite materials system.The system of existing report mainly is aluminum oxide/aluminium and silit/aluminum composite system at present.On a small quantity about the spherical α-Si of the pressure-free impregnation process using of silicon nitride/aluminum composite
3N
4Preparation ceramics preparative body, duraluminum adopt and contain higher ZL301 or the 6061Al of Mg amount.But because in the infiltration process, Mg and Si
3N
4Serious etc. surface reaction, be unfavorable for performance of composites.In addition, the precast body performance of spheroidal particle preparation is not high, and corresponding matrix material can not be extracted the mechanism of grade through fiber and matrix material strengthened toughness reinforcing when fracture, and its performance has bar-shaped β-Si not as utilization
3N
4Matrix material as the precast body preparation.Referring to [1] Akhtar Farid, Guo Shi ju.Development of Si
3N
4/ A1 composite by pressureless melt infiltration.Trans.Nonferrous Met.SOC.China16 (2006) 629-632. [2]. Wang Yangwei, Yu Xiaodong etc.Pressure-free impregnation prepares Si
3N
4The mechanical property of/AlN-Al matrix material.Special Processes of Metal Castings and non-ferrous alloy.2008 the 28th the 5th phases of volume.
At present aspect the preparation of fiber reinforcement aluminum matrix composite, also have some problems: fiber is discontinuous mutually in (1) most of matrix material.Current research shows, when the wild phase in the matrix material and matrix are the interpenetrating(polymer)networks distributed architecture, just can show excellent mechanical property.(2) fibre-reinforced Al alloy composite has very good mechanical property, but because costing an arm and a leg of fiber has toxicity again to human body, fails normally to use on component.(3) ceramics preparative body and molten metal bath wettability are poor.Do not have impressed pressure, molten metal bath is difficult to infiltrate in the ceramics preparative body.(4) adopt the pressure impregnation technology, need expensive molding apparatus and specific mould, increased preparation cost greatly, and the pressure infiltration process is introduced subsurface defect easily.(5) existing pressure-free impregnation technology only is applicable to the porous silicon nitride with the spheroidal particle preparation, rather than is fibrous β-Si
3N
4And Infiltration Technics requires high to al alloy component, the interface side reaction is serious.
Summary of the invention
In order to overcome the deficiency of above-mentioned prior art; The object of the present invention is to provide a kind of silicon nitride and aluminium co-continuous phase composite materials and preparation method thereof; Preparing method's technology of the present invention is simple, with low cost and can be used for preparing the matrix material with various complicated shapes, adopts the silicon nitride of preparing method's preparation of the present invention and aluminium co-continuous phase composite materials to have excellent mechanical property.
To achieve these goals, the technical scheme of the present invention's employing is:
A kind of silicon nitride and aluminium co-continuous phase composite materials, it is characterized in that: aluminium is mutually for to have added the y alloy y of copper and the 30%-60% that the aluminium phase volume accounts for total composite volume in the said matrix material, and silicon nitride is the β phase mutually, β-Si
3N
4Be co-continuous mutually with aluminium and distribute mutually, be IPN pore network structure.
A kind of method for preparing said silicon nitride and aluminium co-continuous phase composite materials comprises the steps:
Step 1: take by weighing at first by weight percentage: α-Si
3N
4Powder 90%～99%, Y
2O
3Sintering aid 1%～10%; Wet ball grinding is prepared into mixed powder then; Subsequently mixed powder is crossed 60 mesh sieves, will cross subsequently mixed powder behind 60 mesh sieves after 50-70 ℃ of dry 4-12 hour after 200 mesh sieves, the compression molding in the mold cavity of packing into of the mixed powder behind 200 orders that will sieve at last; Forming pressure is 5-10MPa, processes green compact;
Step 2: the green compact of at first step 1 being processed place vacuum oven; Make vacuum tightness below 5Pa, in 0.5 hour, furnace temperature is risen to 1150-1250 ℃, feed nitrogen then; Making nitrogen pressure is 0.2-0.3MPa; With the heat-up rate of 5 ℃/min furnace temperature is risen to 1650-1850 ℃ more subsequently, be incubated 0.5-2 hour, obtain the silicon nitride precast body at last;
Step 3: at first silicon nitride precast body of processing in the step 2 and duraluminum are placed in the high-temperature crucible; And be fixed on the silicon nitride precast body in the high-temperature crucible; After the add-on of duraluminum will guarantee aluminum alloy melting, the aluminium fluid power soaked the silicon nitride precast body and the silicon nitride precast body needs to expose outside preset big or small part at aluminium liquid;
Step 4: begin to be evacuated to below the 100Pa after high-temperature crucible placed vacuum oven; Then vacuum oven is risen to 900-1300 ℃ with the speed of 5-10 ℃/min; And insulation completion in 0.5-4 hour pressure-free impregnation, the high-temperature crucible furnace cooling perhaps charges into rare gas element and quickens cooling subsequently;
Step 5: high-temperature crucible is taken out from vacuum oven, places retort furnace to be heated to 700-800 ℃ then, treat aluminium liquid fusing after, from crucible, take out the matrix material sample of accomplishing infiltration;
Step 6: after the sample that at first step 5 is taken out is put into retort furnace; Carry out T6 thermal treatment then: the furnace temperature with retort furnace in 0.5 hour rises to 450-550 ℃ from room temperature, and is incubated 4-6 hour, subsequently sample is taken out shrend; When temperature in the retort furnace is reduced to 150-200 ℃; Put into the sample after the shrend retort furnace and be incubated 4-6 hour, obtain matrix material at last, and from retort furnace, take out;
Step 7: continue in the aluminium liquid of step 5 fusing, to immerse the silicon nitride precast body of new step 2 preparation, preparation is continuously realized in repeating step (3)～(8).
The void content of the silicon nitride precast body that said step 2 obtains is 30%～60%, α-Si behind the sintering
3N
4Being converted into crystal grain is bar-shaped β phase.
Used duraluminum is the y alloy y that contains copper in the said step 3, and copper content accounts for the 1-10% of duraluminum weight percent.
Compared with prior art, the invention has the beneficial effects as follows:
This patent utilizes the precast body of normal pressure-sintered technology preparation porous silicon nitride as matrix material, and the silicon nitride and the aluminium co-continuous phase composite materials that adopt the preparation of pressure-free impregnation technology to have excellent mechanical property compared with prior art, the invention has the beneficial effects as follows:
(1) through regulating Y
2O
3The content of sintering aid can be regulated the void content of precast body, thereby obtains to have the precast body and corresponding matrix material of different performance;
(2) adopt the porous silicon nitride of this patent sintering process preparation to have bar-shaped β-Si
3N
4Crystal grain overlaps the unique microstructures that forms each other, bar-like grains extract the mechanical property that can improve porous silicon nitride with bridge joint, so the porous preform of this law preparation has excellent mechanical property;
(3) because the bar-shaped β-Si of porous silicon nitride
3N
4Tissue is in close proximity to silicon nitride fiber, and is theoretical according to fiber reinforcement technology, has the β-Si of high length-diameter ratio
3N
4Bridge joint that crystal grain produced and the expansion of extracting effect prevention crackle, so the structure of matrix material is also close with fibre-reinforced Al alloy composite with performance, has excellent mechanical property;
(4) because the inner pore of porous silicon nitride precast body of normal pressure-sintered method preparation is the communicating aperture that is evenly distributed in this patent method; So the matrix material of preparation is IPN pore network tissue; Its microtexture is superior to fibre-reinforced Al alloy composite, and performance of composites is highly beneficial for improving;
(5) this experiment adopts not magniferous duraluminum to carry out pressure-free impregnation, has avoided the generation of a large amount of side reactions in infiltration process, has improved performance of composites.Simultaneously, also widened the kind of the optional duraluminum of pressure-free impregnation;
(6) through attemperation and time, can obtain to have the very matrix material of high-compactness, so this method does not need special die casting equipment and specific mould, preparation technology is simple, can reduce preparation cost greatly; Owing to do not need die casting equipment and particular mold, this method can be used for preparing the matrix material with various complicated shapes, has expanded the scope of application of silicon nitride and aluminium co-continuous phase composite materials greatly.
Embodiment
With specific embodiment the present invention is explained further details below.
Embodiment one:
A kind of silicon nitride of present embodiment/aluminium co-continuous phase composite materials, the aluminium phase volume accounts for 59% of total composite volume, and silicon nitride is the β phase mutually, β-Si
3N
4Be co-continuous mutually with aluminium and distribute mutually, be IPN pore network structure.
The preparation method of a kind of silicon nitride of present embodiment/aluminium co-continuous phase composite materials comprises the steps:
Step 1: take by weighing at first by weight percentage: α-Si
3N
4Powder 99%, Y
2O
3Sintering aid 1%; Wet ball grinding is prepared into mixed powder then; Subsequently mixed powder is crossed 60 mesh sieves, will cross subsequently behind 60 mesh sieves mixed powder 50 ℃ of dryings after 12 hours after 200 mesh sieves, the compression molding in the mold cavity of packing into of the mixed powder behind 200 orders that will sieve at last; Forming pressure is 5MPa, processes green compact;
Step 2: the green compact of at first step 1 being processed place vacuum oven; Making vacuum tightness is 5Pa, with 0.3 hour furnace temperature is risen to 1150 ℃, feeds nitrogen then; Making nitrogen pressure is 0.2MPa; With the heat-up rate of 5 ℃/min furnace temperature is risen to 1650 ℃ more subsequently, be incubated 0.5 hour, obtain void content at last and be 59%, crystal grain is bar-shaped beta phase silicon nitride precast body;
Step 3: at first silicon nitride precast body of processing in the step 2 and the y alloy y that contains copper are placed in the high-temperature crucible; Copper content accounts for 4% of duraluminum weight percent; And be fixed on the silicon nitride precast body in the high-temperature crucible; After the add-on of duraluminum will guarantee aluminum alloy melting, the aluminium fluid power soaked the silicon nitride precast body and the silicon nitride precast body needs to expose outside preset big or small part at aluminium liquid;
Step 4: begin to be evacuated to 95Pa after high-temperature crucible placed vacuum oven, then vacuum oven is risen to 1100 ℃ with the speed of 5 ℃/min, and be incubated 1 hour and accomplish pressure-free impregnation, subsequently high-temperature crucible furnace cooling or charge into rare gas element and quicken cooling;
Step 5: high-temperature crucible is taken out from vacuum oven, places retort furnace to be heated to 700 ℃ then, treat aluminium liquid fusing after, from crucible, take out the matrix material sample of accomplishing infiltration;
Step 6: after the sample that at first step 5 is taken out is put into retort furnace; Carry out T6 thermal treatment then: rise to 450 ℃ with 0.3 hour furnace temperature from room temperature, and be incubated 6 hours, subsequently sample is taken out shrend with retort furnace; When temperature in the retort furnace is reduced to 150 ℃; Put into the sample after the shrend retort furnace and be incubated 6 hours, obtain matrix material at last, and from retort furnace, take out;
Step 7: continue in the aluminium liquid of step 5 fusing, to immerse the silicon nitride precast body of new step 2 preparation, preparation is continuously realized in repeating step (3)～(8).
Present embodiment is through measuring, and the density of infiltration back matrix material is 2.89g/cm
3, flexural strength is 481MPa, fracture toughness property is 12.3MPa.m
1/2, mainly be Si mutually
3N
4, Al.
Embodiment two:
A kind of silicon nitride of present embodiment/aluminium co-continuous phase composite materials, the aluminium phase volume accounts for 42% of total composite volume, and silicon nitride is the β phase mutually, β-Si
3N
4Be co-continuous mutually with aluminium and distribute mutually, be IPN pore network structure.
The preparation method of a kind of silicon nitride of present embodiment/aluminium co-continuous phase composite materials comprises the steps:
Step 1: take by weighing at first by weight percentage: α-Si
3N
4Powder 95%, Y
2O
3Sintering aid 5%; Wet ball grinding is prepared into mixed powder then; Subsequently mixed powder is crossed 60 mesh sieves, will cross subsequently behind 60 mesh sieves mixed powder 55 ℃ of dryings after 12 hours after 200 mesh sieves, the compression molding in the mold cavity of packing into of the mixed powder behind 200 orders that will sieve at last; Forming pressure is 5MPa, processes green compact;
Step 2: the green compact of at first step 1 being processed place vacuum oven; Making the vacuum bar is 4Pa, with 0.4 hour furnace temperature is risen to 1200 ℃, feeds nitrogen then; Making nitrogen pressure is 0.225MPa; With the heat-up rate of 5 ℃/min furnace temperature is risen to 1750 ℃ more subsequently, be incubated 2 hours, obtain void content at last and be 42%, crystal grain is bar-shaped beta phase silicon nitride precast body;
Step 3: at first silicon nitride precast body of processing in the step 2 and the y alloy y that contains copper are placed in the high-temperature crucible; Copper content accounts for 4% of duraluminum weight percent; And be fixed on the silicon nitride precast body in the high-temperature crucible; After the add-on of duraluminum will guarantee aluminum alloy melting, the aluminium fluid power soaked the silicon nitride precast body and the silicon nitride precast body needs to expose outside preset big or small part at aluminium liquid;
Step 4: begin to be evacuated to 100Pa after high-temperature crucible placed vacuum oven, then vacuum oven is risen to 1100 ℃ with the speed of 5 ℃/min, and be incubated 1 hour and accomplish pressure-free impregnation, subsequently high-temperature crucible furnace cooling or charge into rare gas element and quicken cooling;
Step 5: high-temperature crucible is taken out from vacuum oven, places retort furnace to be heated to 800 ℃ then, treat aluminium liquid fusing after, from crucible, take out the matrix material sample of accomplishing infiltration;
Step 6: after the sample that at first step 5 is taken out is put into retort furnace; Carry out T6 thermal treatment then: rise to 500 ℃ with 0.4 hour furnace temperature from room temperature, and be incubated 6 hours, subsequently sample is taken out shrend with retort furnace; When temperature in the retort furnace is reduced to 180 ℃; Put into the sample after the shrend retort furnace and be incubated 6 hours, obtain matrix material at last, and from retort furnace, take out;
Step 7: continue in the aluminium liquid of step 5 fusing, to immerse the silicon nitride precast body of new step 2 preparation, preparation is continuously realized in repeating step (3)～(8).
Present embodiment is through measuring, and the density of infiltration back matrix material is 2.95g/cm
3, flexural strength is 497MPa, fracture toughness property is 9.8MPa.m
1/2, mainly be Si mutually
3N
4, Al.
Embodiment three:
A kind of silicon nitride of present embodiment/aluminium co-continuous phase composite materials, the aluminium phase volume accounts for 31% of total composite volume, and silicon nitride is the β phase mutually, β-Si
3N
4Be co-continuous mutually with aluminium and distribute mutually, be IPN pore network structure.
The preparation method of a kind of silicon nitride of present embodiment/aluminium co-continuous phase composite materials comprises the steps:
Step 1: take by weighing at first by weight percentage: α-Si
3N
4Powder 90%, Y
2O
3Sintering aid 10%; Wet ball grinding is prepared into mixed powder then; Subsequently mixed powder is crossed 60 mesh sieves, will cross subsequently behind 60 mesh sieves mixed powder 70 ℃ of dryings after 4 hours after 200 mesh sieves, the compression molding in the mold cavity of packing into of the mixed powder behind 200 orders that will sieve at last; Forming pressure is 10MPa, processes green compact;
Step 2: the green compact of at first step 1 being processed place vacuum oven; Making vacuum is 3Pa, with 0.5 hour furnace temperature is risen to 1250 ℃, feeds nitrogen then; Making nitrogen pressure is 0.3MPa; With the heat-up rate of 5 ℃/min furnace temperature is risen to 1850 ℃ more subsequently, be incubated 0.5 hour, obtain void content at last and be 31%, crystal grain is bar-shaped beta phase silicon nitride precast body;
Step 3: at first silicon nitride precast body of processing in the step 2 and the y alloy y that contains copper are placed in the high-temperature crucible; Copper content accounts for 4% of duraluminum weight percent; And be fixed on the silicon nitride precast body in the high-temperature crucible; After the add-on of duraluminum will guarantee aluminum alloy melting, the aluminium fluid power soaked the silicon nitride precast body and the silicon nitride precast body needs to expose outside preset big or small part at aluminium liquid;
Step 4: begin to be evacuated to 90Pa after high-temperature crucible placed vacuum oven, then vacuum oven is risen to 1100 ℃ with the speed of 10 ℃/min, and be incubated 1 hour and accomplish pressure-free impregnation, subsequently high-temperature crucible furnace cooling or charge into rare gas element and quicken cooling;
Step 5: high-temperature crucible is taken out from vacuum oven, places retort furnace to be heated to 700 ℃ then, treat aluminium liquid fusing after, from crucible, take out the matrix material sample of accomplishing infiltration;
Step 6: after the sample that at first step 5 is taken out is put into retort furnace; Carry out T6 thermal treatment then: rise to 550 ℃ with 0.5 hour furnace temperature from room temperature, and be incubated 4 hours, subsequently sample is taken out shrend with retort furnace; When temperature in the retort furnace is reduced to 200 ℃; Put into the sample after the shrend retort furnace and be incubated 4 hours, obtain matrix material at last, and from retort furnace, take out;
Step 7: continue in the aluminium liquid of step 5 fusing, to immerse the silicon nitride precast body of new step 2 preparation, preparation is continuously realized in repeating step (3)～(8).
Present embodiment is through measuring, and the density of infiltration back matrix material is 3.02g/cm
3, flexural strength is 469MPa, fracture toughness property is 8.6MPa.m
1/2, mainly be Si mutually
3N
4, Al.
Embodiment four:
A kind of silicon nitride of present embodiment/aluminium co-continuous phase composite materials, the aluminium phase volume accounts for 42% of total composite volume, and silicon nitride is the β phase mutually, β-Si
3N
4Be co-continuous mutually with aluminium and distribute mutually, be IPN pore network structure.
The preparation method of a kind of silicon nitride of present embodiment/aluminium co-continuous phase composite materials comprises the steps:
Step 1: take by weighing at first by weight percentage: α-Si
3N
4Powder 95%, Y
2O
3Sintering aid 5%; Wet ball grinding is prepared into mixed powder then; Subsequently mixed powder is crossed 60 mesh sieves, will cross subsequently behind 60 mesh sieves mixed powder 55 ℃ of dryings after 12 hours after 200 mesh sieves, the compression molding in the mold cavity of packing into of the mixed powder behind 200 orders that will sieve at last; Forming pressure is 5MPa, processes green compact;
Step 2: the green compact of at first step 1 being processed place vacuum oven; Making vacuum tightness is 3Pa, with 0.4 hour furnace temperature is risen to 1200 ℃, feeds nitrogen then; Making nitrogen pressure is 0.225MPa; With the heat-up rate of 5 ℃/min furnace temperature is risen to 1750 ℃ more subsequently, be incubated 2 hours, obtain void content at last and be 42%, crystal grain is bar-shaped beta phase silicon nitride precast body;
Step 3: at first silicon nitride precast body of processing in the step 2 and the y alloy y that contains copper are placed in the high-temperature crucible; Copper content accounts for 10% of duraluminum weight percent; And be fixed on the silicon nitride precast body in the high-temperature crucible; After the add-on of duraluminum will guarantee aluminum alloy melting, the aluminium fluid power soaked the silicon nitride precast body and the silicon nitride precast body needs to expose outside preset big or small part at aluminium liquid;
Step 4: begin to be evacuated to 90Pa after high-temperature crucible placed vacuum oven, then vacuum oven is risen to 900 ℃ with the speed of 5 ℃/min, and be incubated 4 hours and accomplish pressure-free impregnation, subsequently high-temperature crucible furnace cooling or charge into rare gas element and quicken cooling;
Step 5: high-temperature crucible is taken out from vacuum oven, places retort furnace to be heated to 800 ℃ then, treat aluminium liquid fusing after, from crucible, take out the matrix material sample of accomplishing infiltration;
Step 6: after the sample that at first step 5 is taken out is put into retort furnace; Carry out T6 thermal treatment then: rise to 500 ℃ with 0.4 hour furnace temperature from room temperature, and be incubated 6 hours, subsequently sample is taken out shrend with retort furnace; When temperature in the retort furnace is reduced to 180 ℃; Put into the sample after the shrend retort furnace and be incubated 6 hours, obtain matrix material at last, and from retort furnace, take out;
Step 7: continue in the aluminium liquid of step 5 fusing, to immerse the silicon nitride precast body of new step 2 preparation, preparation is continuously realized in repeating step (3)～(8).
Present embodiment is through measuring, and the density of infiltration back matrix material is 2.77g/cm
3, flexural strength is 288MPa, fracture toughness property is 6.7MPa.m
1/2, mainly be Si mutually
3N
4, Al.
Embodiment five:
A kind of silicon nitride of present embodiment/aluminium co-continuous phase composite materials, the aluminium phase volume accounts for 42% of total composite volume, and silicon nitride is the β phase mutually, β-Si
3N
4Be co-continuous mutually with aluminium and distribute mutually, be IPN pore network structure.
The preparation method of a kind of silicon nitride of present embodiment/aluminium co-continuous phase composite materials comprises the steps:
Step 1: take by weighing at first by weight percentage: α-Si
3N
4Powder 95%, Y
2O
3Sintering aid 5%; Wet ball grinding is prepared into mixed powder then; Subsequently mixed powder is crossed 60 mesh sieves, will cross subsequently behind 60 mesh sieves mixed powder 55 ℃ of dryings after 12 hours after 200 mesh sieves, the compression molding in the mold cavity of packing into of the mixed powder behind 200 orders that will sieve at last; Forming pressure is 5MPa, processes green compact;
Step 2: the green compact of at first step 1 being processed place vacuum oven; Making vacuum tightness is 3Pa, with 0.4 hour furnace temperature is risen to 1200 ℃, feeds nitrogen then; Making nitrogen pressure is 0.225MPa; With the heat-up rate of 5 ℃/min furnace temperature is risen to 1750 ℃ more subsequently, be incubated 2 hours, obtain void content at last and be 42%, crystal grain is bar-shaped beta phase silicon nitride precast body;
Step 3: at first silicon nitride precast body of processing in the step 2 and the y alloy y that contains copper are placed in the high-temperature crucible; Copper content accounts for 4% of duraluminum weight percent; And be fixed on the silicon nitride precast body in the high-temperature crucible; After the add-on of duraluminum will guarantee aluminum alloy melting, the aluminium fluid power soaked the silicon nitride precast body and the silicon nitride precast body needs to expose outside preset big or small part at aluminium liquid;
Step 4: begin to be evacuated to 85Pa after high-temperature crucible placed vacuum oven, then vacuum oven is risen to 1300 ℃ with the speed of 10 ℃/min, and be incubated 1 hour and accomplish pressure-free impregnation, subsequently high-temperature crucible furnace cooling or charge into rare gas element and quicken cooling;
Step 5: high-temperature crucible is taken out from vacuum oven, places retort furnace to be heated to 800 ℃ then, treat aluminium liquid fusing after, from crucible, take out the matrix material sample of accomplishing infiltration;
Step 6: after the sample that at first step 5 is taken out is put into retort furnace; Carry out T6 thermal treatment then: rise to 500 ℃ with 0.5 hour furnace temperature from room temperature, and be incubated 6 hours, subsequently sample is taken out shrend with retort furnace; When temperature in the retort furnace is reduced to 180 ℃; Put into the sample after the shrend retort furnace and be incubated 6 hours, obtain matrix material at last, and from retort furnace, take out;
Step 7: continue in the aluminium liquid of step 5 fusing, to immerse the silicon nitride precast body of new step 2 preparation, preparation is continuously realized in repeating step (3)～(8).
Present embodiment is through measuring, and the density of infiltration back matrix material is 2.85g/cm
3, flexural strength is 427MPa, fracture toughness property is 7.8MPa.m
1/2, mainly be Si mutually
3N
4, Al.
Embodiment six:
A kind of silicon nitride of present embodiment/aluminium co-continuous phase composite materials, the aluminium phase volume accounts for 40% of total composite volume, and silicon nitride is the β phase mutually, β-Si
3N
4Be co-continuous mutually with aluminium and distribute mutually, be IPN pore network structure.
The preparation method of a kind of silicon nitride of present embodiment/aluminium co-continuous phase composite materials comprises the steps:
Step 1: take by weighing at first by weight percentage: α-Si
3N
4Powder 95%, Y
2O
3Sintering aid 5%; Wet ball grinding is prepared into mixed powder then; Subsequently mixed powder is crossed 60 mesh sieves, will cross subsequently behind 60 mesh sieves mixed powder 55 ℃ of dryings after 12 hours after 200 mesh sieves, the compression molding in the mold cavity of packing into of the mixed powder behind 200 orders that will sieve at last; Forming pressure is 5MPa, processes green compact;
Step 2: the green compact of at first step 1 being processed place vacuum oven; Making vacuum tightness is 3Pa, with 0.4 hour furnace temperature is risen to 1200 ℃, feeds nitrogen then; Making nitrogen pressure is 0.225MPa; With the heat-up rate of 5 ℃/min furnace temperature is risen to 1750 ℃ more subsequently, be incubated 2 hours, obtain void content at last and be 40%, crystal grain is bar-shaped beta phase silicon nitride precast body;
Step 3: at first silicon nitride precast body of processing in the step 2 and the y alloy y that contains copper are placed in the high-temperature crucible; Copper content accounts for 1% of duraluminum weight percent; And be fixed on the silicon nitride precast body in the high-temperature crucible; After the add-on of duraluminum will guarantee aluminum alloy melting, the aluminium fluid power soaked the silicon nitride precast body and the silicon nitride precast body needs to expose outside preset big or small part at aluminium liquid;
Step 4: begin to be evacuated to 90Pa after high-temperature crucible placed vacuum oven; Then vacuum oven is risen to 1300 ℃ with the speed of 5 ℃/min; And being incubated 0.5 hour completion pressure-free impregnation, the high-temperature crucible furnace cooling perhaps charges into rare gas element and quickens cooling subsequently;
Step 5: high-temperature crucible is taken out from vacuum oven, places retort furnace to be heated to 800 ℃ then, treat aluminium liquid fusing after, from crucible, take out the matrix material sample of accomplishing infiltration;
Step 6: after the sample that at first step 5 is taken out is put into retort furnace; Carry out T6 thermal treatment then: rise to 500 ℃ with 0.4 hour furnace temperature from room temperature, and be incubated 6 hours, subsequently sample is taken out shrend with retort furnace; When temperature in the retort furnace is reduced to 180 ℃; Put into the sample after the shrend retort furnace and be incubated 6 hours, obtain matrix material at last, and from retort furnace, take out;
Step 7: continue in the aluminium liquid of step 5 fusing, to immerse the silicon nitride precast body of new step 2 preparation, preparation is continuously realized in repeating step (3)～(8).
Present embodiment is through measuring, and the density of infiltration back matrix material is 2.92g/cm
3, flexural strength is 434MPa, fracture toughness property is 8.8MPa.m
1/2, mainly be Si mutually
3N
4, Al.
Claims (4)
1. silicon nitride and aluminium co-continuous phase composite materials, it is characterized in that: aluminium is mutually for to have added the y alloy y of copper and the 30%-60% that the aluminium phase volume accounts for total composite volume in the said matrix material, and silicon nitride is the β phase mutually, β-Si
3N
4Be co-continuous mutually with aluminium and distribute mutually, be IPN pore network structure.
2. a method for preparing the said matrix material of claim 1 is characterized in that: comprise the steps:
Step 1: take by weighing at first by weight percentage: α-Si
3N
4Powder 90%～99%, Y
2O
3Sintering aid 1%～10%; Wet ball grinding is prepared into mixed powder then; Subsequently mixed powder is crossed 60 mesh sieves, will cross subsequently mixed powder behind 60 mesh sieves after 50-70 ℃ of dry 4-12 hour after 200 mesh sieves, the compression molding in the mold cavity of packing into of the mixed powder behind 200 orders that will sieve at last; Forming pressure is 5-10MPa, processes green compact;
Step 2: the green compact of at first step 1 being processed place vacuum oven; Make vacuum tightness below 5Pa, in 0.5 hour, furnace temperature is risen to 1150-1250 ℃, feed nitrogen then; Making nitrogen pressure is 0.2-0.3MPa; With the heat-up rate of 5 ℃/min furnace temperature is risen to 1650-1850 ℃ more subsequently, be incubated 0.5-2 hour, obtain the silicon nitride precast body at last;
Step 3: at first silicon nitride precast body of processing in the step 2 and duraluminum are placed in the high-temperature crucible; And be fixed on the silicon nitride precast body in the high-temperature crucible; After the add-on of duraluminum will guarantee aluminum alloy melting, the aluminium fluid power soaked the silicon nitride precast body and the silicon nitride precast body needs to expose outside preset big or small part at aluminium liquid;
Step 4: begin to be evacuated to below the 100Pa after high-temperature crucible placed vacuum oven; Then vacuum oven is risen to 900-1300 ℃ with the speed of 5-10 ℃/min; And insulation completion in 0.5-4 hour pressure-free impregnation, the high-temperature crucible furnace cooling perhaps charges into rare gas element and quickens cooling subsequently;
Step 5: high-temperature crucible is taken out from vacuum oven, places retort furnace to be heated to 700-800 ℃ then, treat aluminium liquid fusing after, from crucible, take out the matrix material sample of accomplishing infiltration;
Step 6: after the sample that at first step 5 is taken out is put into retort furnace; Carry out T6 thermal treatment then: the furnace temperature with retort furnace in 0.5 hour rises to 450-550 ℃ from room temperature, and is incubated 4-6 hour, subsequently sample is taken out shrend; When temperature in the retort furnace is reduced to 150-200 ℃; Put into the sample after the shrend retort furnace and be incubated 4-6 hour, obtain matrix material at last, and from retort furnace, take out;
Step 7: continue in the aluminium liquid of step 5 fusing, to immerse the silicon nitride precast body of new step 2 preparation, preparation is continuously realized in repeating step (3)～(8).
3. the method for preparing matrix material according to claim 2 is characterized in that: the void content of the silicon nitride precast body that said step 2 obtains is 30%～60%, α-Si behind the sintering
3N
4Being converted into crystal grain is bar-shaped β phase.
4. the method for preparing matrix material according to claim 2 is characterized in that: used duraluminum is the y alloy y that contains copper in the said step 3, and copper content accounts for the 1-10% of duraluminum weight percent.
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| CN114645796A (en) * | 2022-01-13 | 2022-06-21 | 爱柯迪股份有限公司 | Silicon nitride fiber reinforced aluminum alloy engine cylinder sleeve and preparation method thereof |
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