CN110184550A - A kind of cryogenic treating process of continuous filament reinforced metallic matrix composite - Google Patents

A kind of cryogenic treating process of continuous filament reinforced metallic matrix composite Download PDF

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Publication number
CN110184550A
CN110184550A CN201910609328.6A CN201910609328A CN110184550A CN 110184550 A CN110184550 A CN 110184550A CN 201910609328 A CN201910609328 A CN 201910609328A CN 110184550 A CN110184550 A CN 110184550A
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continuous filament
metallic matrix
cryogenic
infiltration
composite
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Inventor
徐志锋
梁祥
单嘉立
余欢
王振军
蔡长春
张守银
汪志太
卢百平
杨伟
熊博文
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Nanchang Hangkong University
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Nanchang Hangkong University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C47/00Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/02Pretreatment of the fibres or filaments
    • C22C47/06Pretreatment of the fibres or filaments by forming the fibres or filaments into a preformed structure, e.g. using a temporary binder to form a mat-like element
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C47/00Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/08Making alloys containing metallic or non-metallic fibres or filaments by contacting the fibres or filaments with molten metal, e.g. by infiltrating the fibres or filaments placed in a mould
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C49/00Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/02Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C49/00Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/02Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
    • C22C49/04Light metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C49/00Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/02Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
    • C22C49/04Light metals
    • C22C49/06Aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/08Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon

Abstract

The invention discloses a kind of cryogenic treating process of continuous filament reinforced metallic matrix composite, belong to advanced composite material technical field.Specific process flow are as follows: continuous filament reinforced metallic matrix composite is first prepared using vacuum gas pressure infiltration method, it is packed into after wire cutting and surface polishing treatment in the low graphite jig of linear expansion coefficient, then -130 DEG C of multiple deep cooling circulations below is carried out to the graphite jig equipped with continuous filament reinforced metallic matrix composite and are handled with the different group technologies risen again.To eliminate or reduce continuous filament reinforced metallic matrix composite internal residual stress, improve the structural homogenity of composite inner infiltration defect and composite material, more importantly, under this cold and hot group technology effect, boundary strength between interface structure and fiber and metal can be regulated and controled, the improvement of interface performance can further promote the comprehensive mechanical property of composite material.It is with a wide range of applications in the fields such as aerospace and automobile.

Description

A kind of cryogenic treating process of continuous filament reinforced metallic matrix composite
Technical field
The present invention relates to technical field of composite materials, more particularly, to a kind of continuous filament reinforced metallic matrix composite Cryogenic treating process.
Background technique
Fiber-reinforced metal matrix composite has light, high specific stiffness and specific strength, more excellent temperature tolerance, corrosion resistant The a series of advantages such as corrosion, shock resistance and damage-resistant are good, special mechanics coupling is good, designability is good, it is especially three-dimensional The composite material of braiding structure avoid traditional unidirectional composite material anisotropy and Two-dimensional Composites it is easy to crack layering, The problem that interlaminar shear strength is low, shock resistance is poor is that nowadays the field of engineering technology such as aerospace and national defence are most sent out Open up one of the structural material of potentiality.But since the wettability between fiber and metallic matrix is poor and matrix alloy and reinforcing fiber Between thermal expansion coefficient (CTE) difference it is huge, using liquid formation method preparation this kind of composite material in there are biggish residual Residue stress, micropore, stomata and the equal forming defects of fiber segregation, interfacial brittle, cause fiber-reinforced metal matrix composite not have Have and reaches expected excellent mechanical property.
And subzero treatment technology is a kind of method handled at -130 DEG C or less material, is that newest material is tough Change one for the treatment of process.Subzero treatment can effectively improve the mechanical property and service life of metal, alloy, and stable dimensions improve Uniformity, Reducing distortion, and also it is easy to operate, workpiece is not destroyed, it is pollution-free, it is at low cost, it is with a wide range of applications and sends out Open up space.However cryogenic treatment process is generally used in the industrial production of steel at present, people are in long-term cold-treating process Middle research finds that certain steels occur transformation of austenite to martensite and can make metal so as to improve the mechanical property of steel Tool abrasive wear resistant weld deposit, corrosion and wear resistance, reduce internal stress and improve material in terms of all obtain certain journey The improvement of degree has at home and abroad obtained largely being widely applied at present.And at the deep coolings such as non-ferrous alloy and its composite material Research and the practical application for managing aspect are then relatively limited, the subzero treatment especially to advanced fiber-reinforced metal matrix composite Technical study is then less.Therefore, it is aobvious to develop a kind of cryogenic treating process for continuous filament reinforced metallic matrix composite It obtains particularly important.
Summary of the invention
The purpose of the present invention is to provide a kind of cryogenic treating process of continuous filament reinforced metallic matrix composite, are adopting It is multiple to continuous filament reinforced metallic matrix on the basis of preparing continuous filament reinforced metallic matrix composite with vacuum gas pressure infiltration method Condensation material carries out liquid nitrogen deep circular treatment, by eliminating or reducing the remnants inside continuous filament reinforced metallic matrix composite Stress improves the variation of composite inner infiltration defect and composite structure and boundary strength under deep cooling repeated action, Further to promote the comprehensive mechanical property of composite material.
The object of the present invention is achieved like this:
A kind of cryogenic treating process of continuous filament reinforced metallic matrix composite, be characterized in: specific step is as follows:
(1), the vacuum gas pressure infiltration preparation of continuous filament reinforced metallic matrix composite: the braiding of fiber preform is carried out first Forming designs mold further according to fiber preform planform, and prepares high purity graphite of the phosphorus content greater than 99.99% and infiltrate Mold, after by stainless steel materials, stainless steel pipe and be embedded with fiber preform high purity graphite infiltration mold carry out welding envelope Dress, only at the top of stalk, there are openings;The high purity graphite of packaged embedded fiber preform is infiltrated into mold, stalk The opening down upper chamber for being placed in vacuum gas pressure infiltration equipment, by melted temperature be 680-1050 DEG C of liquid matrix alloy It is placed in the lower room of vacuum gas pressure infiltration equipment, sealing infiltration upper chamber, lower room then begin to infiltration upper chamber, lower room while taking out Vacuum to vacuum degree is less than 200Pa, stops vacuumizing, and is filled with the argon gas of 99.99% or more purity repeatedly after prepurging 2-4 times;Again Infiltration room is started to vacuumize, until vacuum degree is less than 100Pa, starts to heat fiber preform, when fibre preforms temperature reaches To setting plus 300 DEG C -900 DEG C of pre- temperature after, promoted vacuum gas pressure infiltration equipment lower room;It is filled with argon gas or nitrogen rapidly again It is forced into 1-12MPa, carries out the gas pressure infiltration of composite material, imbibition pressure power is maintained at 1-12MPa, dwell time 1-120min, After the completion of infiltration, the infiltration upper chamber of vacuum gas pressure infiltration equipment, lower room start pressure release, until infiltration upper chamber, under indoor gas Pressure drops to atmospheric pressure, and material to be composite is cooled to 100 DEG C -- and it is taken out after the temperature between room temperature, then carries out demoulding processing;
(2), the continuous filament reinforced metallic matrix composite by step (1) preparation carries out linear cutter, surface polishing treatment And it is clean with acetone or alcohol washes, obtain the clean and tidy composite element in surface;
(3), the composite element for handling step (2) well, is packed into and is fixed in the graphite jig of subzero treatment;
(4), step (3) composite element in the graphite jig of subzero treatment is fixed on to be directly placed into liquid nitrogen container Or in deep freeze refrigeration plant, subzero treatment is carried out after closed container;
It (5), will be at step (4) composite element that treated is fixed in the graphite jig of subzero treatment again deep cooling Reason, process and step (4) unanimously, are repeated the number of above-mentioned steps (4) and recycle for 2-15 times to get to through multiple deep cooling The continuous filament reinforced metallic matrix composite for the group technology processing risen again with difference.
Fiber in the step (1) is one in filament carbon fiber, filament alumina fibre or filament silicon carbide fibre Kind;Matrix alloy is one of aluminium alloy, magnesium alloy or copper alloy.
Cryogenic treatment process in the step (4) be will directly be fixed on it is compound in the graphite jig of subzero treatment Material members are immersed in fast cooling in liquid nitrogen environment, and rate of temperature fall is greater than 40 DEG C/min, reaches requirement to deep cooling soaking time Afterwards, the composite element that taking-up is fixed in the graphite jig of subzero treatment is placed in return in atmosphere and be warmed to room temperature, that is, completes Subzero treatment.
Or, the cryogenic treatment process in the step (4) is will to be directly fixed in the graphite jig of subzero treatment Composite element is immersed in fast cooling in liquid nitrogen environment, and rate of temperature fall is greater than 40 DEG C/min, reaches to deep cooling soaking time After it is required that, the composite element that taking-up is fixed in the graphite jig of subzero treatment is put into fast in 25~100 DEG C of water-bath Speed is risen again, that is, completes a subzero treatment.
Or, the cryogenic treatment process in the step (4) is will to be directly fixed in the graphite jig of subzero treatment Composite element is immersed in fast cooling in liquid nitrogen environment, and rate of temperature fall is greater than 40 DEG C/min, reaches to deep cooling soaking time After it is required that, the composite element that taking-up is fixed in the graphite jig of subzero treatment, which is placed in heat-treatment furnace, to be rapidly heated It to 100-350 DEG C and after keeping 20-1200min, then places and is cooled to room temperature outside furnace, that is, complete a subzero treatment.
Or, the cryogenic treatment process in the step (4) is using the slow cooling under deep freeze refrigeration plant control, cooling rate For 1 DEG C/min-40 DEG C/min, after deep cooling soaking time reaches requirement, taking-up is fixed in the graphite jig of subzero treatment Composite element be placed in atmosphere return be warmed to room temperature, that is, complete a subzero treatment.
Or, the cryogenic treatment process in the step (4) is using the slow cooling under deep freeze refrigeration plant control, cooling rate For 1 DEG C/min-40 DEG C/min, after deep cooling soaking time reaches requirement, taking-up is fixed in the graphite jig of subzero treatment Composite element be put into fast temperature rising in 25~100 DEG C of water-bath, that is, complete a subzero treatment.
Or, the cryogenic treatment process in the step (4) is using the slow cooling under deep freeze refrigeration plant control, cooling rate For 1 DEG C/min-40 DEG C/min, after deep cooling soaking time reaches requirement, taking-up is fixed in the graphite jig of subzero treatment Composite element be placed in heat-treatment furnace and be rapidly heated to 100-350 DEG C and after keeping 20-1200min, then place furnace It is cooled to room temperature outside, that is, completes a subzero treatment.
The design parameter of cryogenic treatment process in the step (4) are as follows: cryogenic temperature is -130 DEG C to -196 DEG C, deep cooling Soaking time is 8-120h, and the time of rising again is 20min-1200min.
The invention has the beneficial effects that:
1, there are apparent volume contractions during subzero treatment for the continuous filament reinforced metallic matrix composite of infiltration preparation Phenomenon, internal capillary and generating the defects of vacancy makes up in the continuous filament reinforced metallic matrix composite for causing infiltration to prepare, Reduce fiber segregation defect in continuous filament reinforced metallic matrix composite, improves continuous filament reinforced metallic matrix composite wood Expect structural homogenity;Meanwhile the remnants of continuous filament reinforced metallic matrix composite can also be eliminated or be reduced to cryogenic treatment process Stress, to be conducive to improve the mechanical property of continuous filament reinforced metallic matrix composite;
2, suitable cryogenic treatment process can regulate and control interface performance between fiber and metal and form new interface phase, interface characteristics The improvement of energy can enable the stress inside continuous filament reinforced metallic matrix composite more evenly transmit, and subzero treatment is conducive to surely The size and shape for determining continuous filament reinforced metallic matrix composite improve the mechanics of continuous filament reinforced metallic matrix composite Performance;
3, extension of the subzero treatment as a kind of normative heat treatment, have it is easy to operate, do not destroy workpiece, be pollution-free, it is at low cost Etc. advantages.
In conclusion the multiple deep cooling of the continuous filament reinforced metallic matrix composite based on vacuum gas pressure infiltration preparation follows Ring and the different group technology high treating effects risen again, stability is strong, is a kind of very ideal continuous filament reinforced metallic matrix The cryogenic treating process of composite material.
Detailed description of the invention
Fig. 1 is vacuum gas pressure infiltration equipment schematic diagram.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.
Embodiment 1:
A kind of cryogenic treating process of three-dimensional orthogonal M40J fiber reinforced aluminum matrix composites, the specific steps are as follows:
(1), the vacuum gas pressure infiltration preparation of three-dimensional orthogonal M40J fiber reinforced aluminum matrix composites: progress three-dimensional orthogonal first The braiding of M40J fiber preform shapes, and designs mold further according to three-dimensional orthogonal M40J fiber preform planform, and prepare High purity graphite of the phosphorus content greater than 99.99% infiltrates mold out, after by stainless plate, stainless tubing and be embedded with three-dimensional orthogonal The infiltration mold of M40J fiber preform carries out welding encapsulation, and only there are openings at the top of stalk;By packaged embedded three The high purity graphite infiltration mold of orthogonal M40J fiber preform is tieed up, the opening down of stalk is placed in vacuum gas pressure infiltration equipment Upper chamber, 720 DEG C of melted liquid ZL301 alloys are placed in the lower room of vacuum gas pressure infiltration equipment, sealing infiltration upper chamber, Lower room then begins to infiltration upper chamber, lower room while being evacuated to vacuum degree 150Pa, stops vacuumizing, be filled with purity 99.99% Above argon gas is repeatedly after prepurging 2 times;Again infiltration upper chamber, lower room are started to vacuumize, until vacuum degree is less than 80Pa, be started pair M40J fiber preform heating, when M40J fibre preforms temperature reaches after adding 500 DEG C of pre- temperature of setting, promotion Impregnation apparatus Lower room;It is filled with nitrogen rapidly again to pressurize to 8MPa, carries out the gas pressure infiltration of composite material, imbibition pressure power is maintained at 8MPa, protects Time 20min is pressed, after the completion of infiltration, infiltrates upper chamber, the pressure release together of lower room, until infiltration upper chamber, lower room pressure drop to greatly Atmospheric pressure, material to be composite take out after being cooled to room temperature, then carry out demoulding processing;
(2), the three-dimensional orthogonal M40J fiber reinforced aluminum matrix composites of step (1) preparation are subjected to linear cutter, surface is thrown It light processing and is cleaned up with acetone, obtains the clean and tidy composite element in surface;
(3), the composite element for handling step (2) well, is packed into and is fixed in the graphite jig of subzero treatment;
(4), the three-dimensional orthogonal M40J fiber reinforcement aluminum-base composite material being fixed on step (3) in the graphite jig of subzero treatment Material component is directly placed into liquid nitrogen container, and subzero treatment, the design parameter of cryogenic treatment process are as follows: deep cooling are carried out after closed container Temperature is -196 DEG C, and deep cooling soaking time is 30h, takes out composite sample and is put into fast temperature rising in 80 DEG C of water-bath, rises again Time is 60min, that is, completes a subzero treatment;
(5), by step (4) treated the subzero treatment again of three-dimensional orthogonal M40J fiber reinforced aluminum matrix composites, process Unanimously with step (4), the number that above-mentioned steps (4) are repeated is 5 times to get the three-dimensional orthogonal M40J for arriving deep cooling circular treatment Fiber reinforced aluminum matrix composites.
After group technology processing by 5 deep cooling circulations and water-bath fast temperature rising, three-dimensional orthogonal M40J fiber reinforcement aluminium The tensile strength and elasticity modulus of based composites improve 15% or more compared with as cast condition.
Embodiment 2:
A kind of cryogenic treating process of three-dimensional orthogonal SiC fiber reinforced magnesium base composite material, the specific steps are as follows:
(1), the vacuum gas pressure infiltration preparation of three-dimensional orthogonal SiC fiber reinforced magnesium base composite material: progress three-dimensional orthogonal SiC first The braiding of fiber preform shapes, and designs mold further according to three-dimensional orthogonal SiC fiber preform planform, and prepare carbon containing High purity graphite of the amount greater than 99.99% infiltrates mold, after by stainless plate, stainless tubing and to be embedded with three-dimensional orthogonal SiC fiber pre- The infiltration mold of body processed carries out welding encapsulation, and only there are openings at the top of stalk;Packaged embedded three-dimensional orthogonal SiC is fine The high purity graphite for tieing up precast body infiltrates mold, and the opening down upper chamber for being placed in vacuum gas pressure infiltration equipment of stalk will melt The 720 DEG C of liquid AZ91D alloys refined are placed in the lower room of vacuum gas pressure infiltration equipment, and sealing infiltration upper chamber, lower room are then opened Begin to be evacuated to vacuum degree 150Pa simultaneously to infiltration upper chamber, lower room, stops vacuumizing, be filled with the argon gas of 99.99% or more purity Repeatedly after prepurging 2 times;Again infiltration upper chamber, lower room are started to vacuumize, until vacuum degree is less than 100Pa, be started pre- to SiC fiber Body processed heating, when SiC fibre preforms temperature reach setting plus after 550 DEG C of pre- temperature, promote the lower room of Impregnation apparatus;It is fast again Speed is filled with argon gas and pressurizes to 10MPa, carries out the gas pressure infiltration of composite material, imbibition pressure power is maintained at 10MPa, dwell time 25min after the completion of infiltration, infiltrates upper chamber, the pressure release together of lower room, until infiltration upper chamber, lower room pressure drop to atmospheric pressure, Material to be composite takes out after being cooled to room temperature, then carries out demoulding processing;
(2), the three-dimensional orthogonal SiC fiber reinforced magnesium base composite material by step (1) preparation carries out linear cutter, surface polishing It handles and clean with alcohol washes, obtains the clean and tidy composite element in surface;
(3), the composite element for handling step (2) well, is packed into and is fixed in the graphite jig of subzero treatment;
(4), the three-dimensional orthogonal SiC fiber reinforced magnesium base composite wood being fixed on step (3) in the graphite jig of subzero treatment Material component is directly placed into liquid nitrogen container, and subzero treatment, the design parameter of cryogenic treatment process are as follows: deep cooling are carried out after closed container Temperature is -196 DEG C, and deep cooling soaking time is for 24 hours that taking-up composite element placement is returned in an atmosphere to be warmed to room temperature, when rising again Between be 120min, that is, complete a subzero treatment;
(5), by step (4) treated three-dimensional orthogonal SiC fiber reinforced aluminum matrix composites subzero treatment again, process with Unanimously, the number that above-mentioned steps (4) are repeated is 7 times fine to get the three-dimensional orthogonal SiC to deep cooling circular treatment to step (4) Dimension enhancing magnesium-based composite material.
After the group technology processing risen again by 7 deep cooling circulations and room temperature, three-dimensional orthogonal SiC fiber reinforced magnesium base is compound The tensile strength and elasticity modulus of material improve 15% or more compared with as cast condition.
Embodiment 3:
A kind of cryogenic treating process of three-dimensional five-way M50J fiber reinforced aluminum matrix composites, the specific steps are as follows:
(1), the vacuum gas pressure infiltration preparation of three-dimensional five-way M50J fiber reinforced aluminum matrix composites: three-dimensional five-way is carried out first The braiding of M50J fiber preform shapes, and designs mold further according to three-dimensional five-way M50J fiber preform planform, and prepare High purity graphite of the phosphorus content greater than 99.99% infiltrates mold out, after by stainless plate, stainless tubing and be embedded with three-dimensional five-way The infiltration mold of M50J fiber preform carries out welding encapsulation, and only there are openings at the top of stalk;By packaged embedded three The high purity graphite for tieing up five-way M50J fiber preform infiltrates mold, and the opening down of stalk is placed in vacuum gas pressure infiltration equipment Upper chamber, 720 DEG C of melted liquid ZL301 alloys are placed in the lower room of vacuum gas pressure infiltration equipment, sealing infiltration upper chamber, Lower room then begins to infiltration upper chamber, lower room while being evacuated to vacuum degree 120Pa, stops vacuumizing, be filled with purity 99.99% Above argon gas is repeatedly after prepurging 3 times;Again infiltration upper chamber, lower room are started to vacuumize, until vacuum degree is less than 40Pa, be started pair M50J fiber preform heating, when M50J fibre preforms temperature reaches after adding 450 DEG C of pre- temperature of setting, promotion Impregnation apparatus Lower room;It being filled with nitrogen rapidly again to pressurize to 12MPa, carries out the gas pressure infiltration of composite material, imbibition pressure power is maintained at 12MPa, Dwell time 50min after the completion of infiltration, infiltrates upper chamber, the pressure release together of lower room, until infiltration upper chamber, lower room pressure drop to Atmospheric pressure, material to be composite take out after being cooled to room temperature, then carry out demoulding processing;
(2), the three-dimensional five-way M50J fiber reinforced aluminum matrix composites of step (1) preparation are subjected to linear cutter, surface is thrown It light processing and is cleaned up with acetone, obtains the clean and tidy composite element in surface;
(3), the composite element for handling step (2) well, is packed into and is fixed in the graphite jig of subzero treatment;
(4), the three-dimensional five-way M50J fiber reinforcement aluminum-base composite material being fixed on step (3) in the graphite jig of subzero treatment Material component is put into deep freeze refrigeration plant, and subzero treatment, the design parameter of cryogenic treatment process are as follows: subzero treatment are carried out after Sealing Arrangement Cooling rate be 10 DEG C/min, cryogenic temperature be -180 DEG C, deep cooling soaking time be 18h, take out composite sample place It returns and is warmed to room temperature in an atmosphere, the time of rising again is 50min, that is, completes a subzero treatment;
(5), by step (4) treated the subzero treatment again of three-dimensional five-way M50J fiber reinforced aluminum matrix composites, process Unanimously with step (4), the number that above-mentioned steps (4) are repeated is 3 times to get the three-dimensional five-way M50J for arriving deep cooling circular treatment Fiber reinforced aluminum matrix composites.
After the group technology processing risen again by 3 deep cooling circulations and room temperature, three-dimensional five-way M50J fiber reinforcement aluminium base is multiple The tensile strength and elasticity modulus of condensation material are significantly improved compared with as cast condition.
Embodiment 4:
A kind of lamination punctures the cryogenic treating process of fabric construction Al2O3 fiber reinforcement Cu-base composites, the specific steps are as follows:
(1), lamination punctures the vacuum gas pressure infiltration preparation of fabric construction Al2O3 fiber reinforcement Cu-base composites: carrying out first Lamination punctures the braiding forming of fabric construction Al2O3 fiber preform, punctures fabric construction Al2O3 fibre preforms further according to lamination Body planform design mold, and prepare phosphorus content greater than 99.99% high purity graphite infiltration mold, after by stainless plate, no Rust tubing and the infiltration mold for being embedded with lamination puncture fabric construction Al2O3 fiber preform carry out welding encapsulation, only in a liter liquid There are openings in tube top portion;The high purity graphite that packaged embedded lamination punctures fabric construction Al2O3 fiber preform is infiltrated into mould Tool, the opening down upper chamber for being placed in vacuum gas pressure infiltration equipment of stalk are green by 1050 DEG C of melted liquid cast berylliums Copper alloy is placed in the lower room of vacuum gas pressure infiltration equipment, and sealing infiltration upper chamber, lower room are then begun to infiltration upper chamber, lower room It is evacuated to vacuum degree 90Pa simultaneously, stops vacuumizing, is filled with the argon gas of 99.99% or more purity repeatedly after prepurging 2 times;Again Infiltration upper chamber, lower room are started to vacuumize, until vacuum degree is less than 30Pa, started pre- to lamination puncture fabric construction Al2O3 fiber Body heating processed reaches after adding 550 DEG C of pre- temperature of setting when lamination punctures fabric construction Al2O3 fibre preforms temperature, is promoted The lower room of Impregnation apparatus;It is filled with nitrogen rapidly again to pressurize to 9MPa, carries out the gas pressure infiltration of composite material, imbibition pressure power is maintained at 9MPa, dwell time 20min after the completion of infiltration, infiltrate upper chamber, the pressure release together of lower room, until under infiltration upper chamber, lower room pressure It is down to atmospheric pressure, material to be composite takes out after being cooled to 50 DEG C, then carries out demoulding processing;
(2), the lamination of step (1) preparation the progress wire cutting of fabric construction Al2O3 fiber reinforcement Cu-base composites is punctured to add It work, surface polishing treatment and is cleaned up with acetone, obtains the clean and tidy composite element in surface;
(3), the composite element for handling step (2) well, is packed into and is fixed in the graphite jig of subzero treatment;
(4), the lamination in the graphite jig of subzero treatment is inlayed and be fixed on to step (3) and puncture fabric construction Al2O3 fibre Dimension enhancing Cu-base composites component is directly placed into deep freeze refrigeration plant, and subzero treatment, cryogenic treatment process are carried out after closed container Design parameter are as follows: cooling rate be 5 DEG C/min, cryogenic temperature be -185 DEG C, deep cooling soaking time be 12h, take out composite wood Material sample is placed in return in atmosphere and be warmed to room temperature, and the time of rising again is 90min, that is, completes a subzero treatment;
(5), step (4) treated lamination is punctured into fabric construction Al2O3 fiber reinforcement Cu-base composites again at deep cooling Reason, unanimously, the number that above-mentioned steps (4) are repeated is 9 times to get folding to deep cooling circular treatment for process and step (4) Layer puncture fabric construction Al2O3 fiber reinforcement Cu-base composites.
After the group technology processing risen again by 9 deep cooling circulations and room temperature, three-dimensional five-way Al2O3 fiber reinforcement aluminium base is multiple The tensile strength and elasticity modulus of condensation material are significantly improved compared with as cast condition.
Embodiment 5
A kind of cryogenic treating process for shallowly handing over direct-connected 2.5D structural carbon fiber enhancing magnesium-based composite material, the specific steps are as follows:
(1), it shallowly hands over the vacuum gas pressure infiltration preparation of direct-connected 2.5D structural carbon fiber enhancing magnesium-based composite material: shallowly being handed over first The braiding of direct-connected 2.5D structural fibers precast body shapes, further according to shallowly handing over direct-connected 2.5D structural carbon fiber precursor structure shape to set Count mold, and prepare high purity graphite infiltration mold of the phosphorus content greater than 99.99%, after by stainless plate, stainless tubing and embedded There is the infiltration mold for shallowly handing over direct-connected 2.5D structural carbon fiber precast body to carry out welding encapsulation, only there are openings at the top of stalk; The packaged embedded high purity graphite for shallowly handing over direct-connected 2.5D structural carbon fiber precast body is infiltrated into mold, stalk it is opening down It is placed in the upper chamber of vacuum gas pressure infiltration equipment, 730 DEG C of melted liquid AZ91D alloys are placed in vacuum gas pressure infiltration and are set Standby lower room, sealing infiltration upper chamber, lower room, then begins to infiltration upper chamber, lower room while being evacuated to vacuum degree 120Pa, stop It only vacuumizes, is filled with the argon gas of 99.99% or more purity repeatedly after prepurging 3 times;Again infiltration upper chamber, lower room are started to vacuumize, It is less than 60Pa to vacuum degree, starts to shallowly handing over direct-connected 2.5D structural carbon fiber precast body to heat, when shallowly hands over direct-connected 2.5D structural carbon After fibre preforms temperature reaches setting plus 530 DEG C of pre- temperature, the lower room of Impregnation apparatus is promoted;It is filled with argon gas rapidly extremely again 10MPa pressurization carries out the gas pressure infiltration of composite material, and imbibition pressure power is maintained at 10MPa, dwell time 15min, and infiltration is completed Afterwards, upper chamber, the pressure release together of lower room are infiltrated, until infiltration upper chamber, lower room pressure drop to atmospheric pressure, material to be composite is cooled to It is taken out after room temperature, then carries out demoulding processing;
The direct-connected 2.5D structural carbon fiber enhancing magnesium-based composite material progress linear cutter of the shallowly friendship for (2), preparing step (1), It surface polishing treatment and is cleaned up with acetone, obtains the clean and tidy composite element in surface;
(3), the composite element for handling step (2) well, is packed into and is fixed in the graphite jig of subzero treatment;
(4), step (3) is fixed on the direct-connected 2.5D structural carbon fiber of the shallowly friendship in the graphite jig of subzero treatment enhances magnesium-based Composite element is directly placed into liquid nitrogen container, and subzero treatment, the design parameter of cryogenic treatment process are carried out after closed container Are as follows: cryogenic temperature is -196 DEG C, and deep cooling soaking time is 30h, and taking-up composite sample, which is placed in heat-treatment furnace, quickly to be risen Temperature after the retention time is 120min, is cooled to room temperature to 230 DEG C outside furnace.Complete a subzero treatment;
(5), by step (4), treated that direct-connected 2.5D structural carbon fiber is shallowly handed over to enhance magnesium-based composite material subzero treatment again, Unanimously, the number that above-mentioned steps (4) are repeated is 7 times straight to get the shallow friendship to deep cooling circular treatment for its process and step (4) Even 2.5D structural carbon fiber enhances magnesium-based composite material.
After the group technology processing risen again by 7 deep cooling circulations and annealing, direct-connected 2.5D graphite fibre enhancing magnesium is shallowly handed over The tensile strength and elasticity modulus of based composites are significantly improved compared with as cast condition.

Claims (9)

1. a kind of cryogenic treating process of continuous filament reinforced metallic matrix composite, it is characterised in that: specific step is as follows:
(1), the vacuum gas pressure infiltration preparation of continuous filament reinforced metallic matrix composite: the braiding of fiber preform is carried out first Forming designs mold further according to fiber preform planform, and prepares high purity graphite of the phosphorus content greater than 99.99% and infiltrate Mold, after by stainless steel materials, stainless steel pipe and be embedded with fiber preform high purity graphite infiltration mold carry out welding envelope Dress, only at the top of stalk, there are openings;The high purity graphite of packaged embedded fiber preform is infiltrated into mold, stalk The opening down upper chamber for being placed in vacuum gas pressure infiltration equipment, by melted temperature be 680-1050 DEG C of liquid matrix alloy It is placed in the lower room of vacuum gas pressure infiltration equipment, sealing infiltration upper chamber, lower room then begin to infiltration upper chamber, lower room while taking out Vacuum to vacuum degree is less than 200Pa, stops vacuumizing, and is filled with the argon gas of 99.99% or more purity repeatedly after prepurging 2-4 times;Again Infiltration room is started to vacuumize, until vacuum degree is less than 100Pa, starts to heat fiber preform, when fibre preforms temperature reaches To setting plus 300 DEG C -900 DEG C of pre- temperature after, promoted vacuum gas pressure infiltration equipment lower room;It is filled with argon gas or nitrogen rapidly again It is forced into 1-12MPa, carries out the gas pressure infiltration of composite material, imbibition pressure power is maintained at 1-12MPa, dwell time 1-120min, After the completion of infiltration, the infiltration upper chamber of vacuum gas pressure infiltration equipment, lower room start pressure release, until infiltration upper chamber, under indoor gas Pressure drops to atmospheric pressure, and material to be composite is cooled to 100 DEG C -- and it is taken out after the temperature between room temperature, then carries out demoulding processing;
(2), the continuous filament reinforced metallic matrix composite by step (1) preparation carries out linear cutter, surface polishing treatment And it is clean with acetone or alcohol washes, obtain the clean and tidy composite element in surface;
(3), the composite element for handling step (2) well, is packed into and is fixed in the graphite jig of subzero treatment;
(4), step (3) composite element in the graphite jig of subzero treatment is fixed on to be directly placed into liquid nitrogen container Or in deep freeze refrigeration plant, subzero treatment is carried out after closed container;
It (5), will be at step (4) composite element that treated is fixed in the graphite jig of subzero treatment again deep cooling Reason, process and step (4) unanimously, are repeated the number of above-mentioned steps (4) and recycle for 2-15 times to get to through multiple deep cooling The continuous filament reinforced metallic matrix composite for the group technology processing risen again with difference.
2. the cryogenic treating process of continuous filament reinforced metallic matrix composite according to claim 1, it is characterised in that: Fiber in the step (1) is one of filament carbon fiber, filament alumina fibre or filament silicon carbide fibre;Matrix closes Gold is one of aluminium alloy, magnesium alloy or copper alloy.
3. the cryogenic treating process of continuous filament reinforced metallic matrix composite according to claim 1, it is characterised in that: Cryogenic treatment process in the step (4) is will to be directly fixed on the composite element in the graphite jig of subzero treatment It is immersed in fast cooling in liquid nitrogen environment, rate of temperature fall is greater than 40 DEG C/min, after deep cooling soaking time reaches requirement, takes out solid The composite element being scheduled in the graphite jig of subzero treatment is placed in return in atmosphere and be warmed to room temperature, that is, completes at a deep cooling Reason.
4. the cryogenic treating process of continuous filament reinforced metallic matrix composite according to claim 1, it is characterised in that: Cryogenic treatment process in the step (4) is will to be directly fixed on the composite element in the graphite jig of subzero treatment It is immersed in fast cooling in liquid nitrogen environment, rate of temperature fall is greater than 40 DEG C/min, after deep cooling soaking time reaches requirement, takes out solid The composite element being scheduled in the graphite jig of subzero treatment is put into fast temperature rising in 25~100 DEG C of water-bath, that is, completes Subzero treatment.
5. the cryogenic treating process of continuous filament reinforced metallic matrix composite according to claim 1, it is characterised in that: Cryogenic treatment process in the step (4) is will to be directly fixed on the composite element in the graphite jig of subzero treatment It is immersed in fast cooling in liquid nitrogen environment, rate of temperature fall is greater than 40 DEG C/min, after deep cooling soaking time reaches requirement, takes out solid The composite element being scheduled in the graphite jig of subzero treatment, which is placed in heat-treatment furnace, to be rapidly heated to 100-350 DEG C simultaneously It after keeping 20-1200min, then places and is cooled to room temperature outside furnace, that is, complete a subzero treatment.
6. the cryogenic treating process of continuous filament reinforced metallic matrix composite according to claim 1, it is characterised in that: Cryogenic treatment process in the step (4) is using the slow cooling under deep freeze refrigeration plant control, and cooling rate is 1 DEG C/min- 40 DEG C/min, after deep cooling soaking time reaches requirement, take out the composite material being fixed in the graphite jig of subzero treatment Component is placed in return in atmosphere and be warmed to room temperature, that is, completes a subzero treatment.
7. the cryogenic treating process of continuous filament reinforced metallic matrix composite according to claim 1, it is characterised in that: Cryogenic treatment process in the step (4) is using the slow cooling under deep freeze refrigeration plant control, and cooling rate is 1 DEG C/min- 40 DEG C/min, after deep cooling soaking time reaches requirement, take out the composite material being fixed in the graphite jig of subzero treatment Component is put into fast temperature rising in 25~100 DEG C of water-bath, that is, completes a subzero treatment.
8. the cryogenic treating process of continuous filament reinforced metallic matrix composite according to claim 1, it is characterised in that: Cryogenic treatment process in the step (4) is using the slow cooling under deep freeze refrigeration plant control, and cooling rate is 1 DEG C/min- 40 DEG C/min, after deep cooling soaking time reaches requirement, take out the composite material being fixed in the graphite jig of subzero treatment Component, which is placed in heat-treatment furnace, to be rapidly heated to 100-350 DEG C and after keeping 20-1200min, then places and be cooled to room outside furnace Temperature completes a subzero treatment.
9. the cryogenic treating process of continuous filament reinforced metallic matrix composite according to claim 1, it is characterised in that: The design parameter of cryogenic treatment process in the step (4) are as follows: cryogenic temperature is -130 DEG C to -196 DEG C, deep cooling soaking time For 8-120h, the time of rising again is 20min-1200min.
CN201910609328.6A 2019-07-08 2019-07-08 A kind of cryogenic treating process of continuous filament reinforced metallic matrix composite Pending CN110184550A (en)

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