CN108220644A - A kind of Nano-meter SiO_22The preparation method of reinforced aluminum matrix composites - Google Patents

A kind of Nano-meter SiO_22The preparation method of reinforced aluminum matrix composites Download PDF

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CN108220644A
CN108220644A CN201711342990.7A CN201711342990A CN108220644A CN 108220644 A CN108220644 A CN 108220644A CN 201711342990 A CN201711342990 A CN 201711342990A CN 108220644 A CN108220644 A CN 108220644A
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powder
nano
meter sio
preparation
aluminum matrix
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颜巍巍
包崇玺
许凯
秦晓冬
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NBTM New Materials Group Co Ltd
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Priority to US16/161,557 priority patent/US20190185974A1/en
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0036—Matrix based on Al, Mg, Be or alloys thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/40—Intermetallics other than rare earth-Co or -Ni or -Fe intermetallic alloys
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2302/00—Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
    • B22F2302/25—Oxide
    • B22F2302/256—Silicium oxide (SiO2)
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2304/00—Physical aspects of the powder
    • B22F2304/05—Submicron size particles
    • B22F2304/054—Particle size between 1 and 100 nm
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2304/00—Physical aspects of the powder
    • B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/16—Both compacting and sintering in successive or repeated steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder

Abstract

A kind of Nano-meter SiO_22The preparation method of reinforced aluminum matrix composites, it is characterised in that include the following steps：(1) powder is mixed：By aluminum substrate powder and Nano-meter SiO_22Powder is mixed to get raw material powder, and the raw material powder is uniformly mixed using hand mix or mixing machine mixing, wherein, the average particle size of aluminium elemental powders or Al alloy powder is 30~100 μm, Nano-meter SiO_22The average particle size of powder be 5~145nm, Nano-meter SiO_22Mass percent in raw material powder is 0.01%~5%, and surplus is aluminum substrate powder, and the aluminum substrate powder is aluminium elemental powders or the forming of Al alloy powder or aluminum matrix composite powder (2):By powder pressing obtained by step (1), green body is obtained；(3) it is sintered:In N2Green body obtained by step (2) is sintered under atmosphere, sintering temperature is 550~660 DEG C, and soaking time is 5~60min, furnace cooling after heat preservation continues in N2Slow cooling under atmosphere protection, cooling time are 0.5~3h, obtain sintered part；(4) it is heat-treated.Preparation method Properties of Aluminum Matrix Composites simple for process, prepared is preferable.

Description

A kind of Nano-meter SiO_22The preparation method of reinforced aluminum matrix composites
Technical field
The present invention relates to aluminum matrix composite preparation field more particularly to a kind of Nano-meter SiO_2s2Reinforced aluminum matrix composites Preparation method.
Background technology
Aluminium alloy be a kind of low-density, high specific strength light material, aluminium alloy substitution iron-based is conducive to after copper-based element Mitigate dead weight, energy-saving and emission-reduction, aluminium alloy has obtained in fields such as aerospace, automobile, machine-building, ship, chemical industry It widely applies.For example, the blade of the crossbeam of aluminium pot can body, supersonic fighterplane, high-pressure cylinder, vehicle cantilever component, engine, Aluminium alloy is widely used in casing and cylinder sleeve etc..However, many do not require nothing more than lightweight, and require high wearability, low heat The coefficient of expansion, excellent mechanical behavior under high temperature working environment in, conventional aluminum alloy materials can not meet practical application need It asks.In order to solve this problem there is technical staff using ceramic phase come the performance of reinforced aluminum matrix composites, ceramic phase enhancing Aluminum matrix composite has both the advantage of aluminium alloy and ceramic enhancement phase, at a high speed, vibration, moist, unlubricated, few lubrication, requirement High-performance and high reliability can be kept under the harsh conditions such as lightweight, aggressive atmosphere, there is very extensive industrial prospect.Such as Notification number is the Chinese invention of CN1182063A《The preparation method of ceramic particle reinforced aluminium base composite material》Utilize ceramic particle With the compound performance for substantially increasing aluminum matrix composite of aluminium powder.
Ceramic phase and the manufacturing method of aluminium base bluk recombination have it is many such as diffusion bonds, method of impregnation, disperse mix, spray mist Change, In-situ reaction, powder metallurgic method etc..The composite material reinforced phase that wherein prepared by powder metallurgic method is evenly distributed, and performance is higher, And be a kind of environmentally friendly manufacturing technology of energy-saving material-saving, more it is suitble to commercial Application.Wherein powder metallurgic method when the ceramic phase that uses Powder can further preferred nanometer grade powder, nano material has the particular advantages such as skin effect, small-size effect, with routine The physics of material, chemical property difference are apparent；Using the good complex effect of nano particle and alloy matrix aluminum, base is given full play to The respective performance advantage of body and reinforced phase, the aluminum matrix composite of availability brilliance.It is CN104498752A to have notification number Chinese invention patent《A kind of preparation method of micro-nano particle reinforced》Disclose a kind of Al alloy powder with Reinforced phase powder high-energy ball milling mixes, then carries out the preparation method of activated sintering densification, but this method processing step is relative complex, into This is higher.In addition, there is the Chinese invention patent that notification number is CN105039793A《A kind of micro-nano granules enhance aluminum-base composite material The preparation method of material》Disclose using aluminium powder as matrix, using nano silicon carbide granulate as reinforced phase particle by mixing, ball milling with And hot pressed sintering step carrys out the preparation method of Matrix Composites Reinforced by Stirring.Although the preparation method step is simple, use Nano silicon carbide granulate is as ceramic phase, and the performance of prepared aluminum matrix composite also needs to further enhance.Using biography System powder metallurgical technique, by Nano-meter SiO_22Powder carrys out the preparation of reinforced aluminum matrix composites with alloy matrix aluminum powder direct combination Method, it is not yet reported.
Invention content
The technical problems to be solved by the invention be for the prior art present situation provide it is a kind of simple for process, prepared The preferable Nano-meter SiO_2 of Properties of Aluminum Matrix Composites2The preparation method of reinforced aluminum matrix composites.
Technical solution is used by the present invention solves above-mentioned technical problem：This kind of Nano-meter SiO_22Reinforced aluminum matrix composites Preparation method, it is characterised in that include the following steps：
(1) powder is mixed：By aluminum substrate powder and Nano-meter SiO_22Powder is mixed to get raw material powder, and the raw material powder uses hand Dynamic mixing or mixing machine mix to be uniformly mixed, wherein, the average particle size of aluminium elemental powders or Al alloy powder is 30~100 μ M, Nano-meter SiO_22The average particle size of powder be 5~145nm, Nano-meter SiO_22Mass percent in raw material powder for 0.01%~ 5%, surplus is aluminum substrate powder, and the aluminum substrate powder is aluminium elemental powders or Al alloy powder or aluminum matrix composite powder End；
(2) it shapes:By powder pressing obtained by step (1), green body is obtained；
(3) it is sintered:In N2Green body obtained by step (2) is sintered under atmosphere, sintering temperature is 550~660 DEG C, heat preservation Time is 5~60min, furnace cooling after heat preservation continues in N2Slow cooling under atmosphere protection, cooling time 0.5 ~3h；
(4) it is heat-treated：Sintered part obtained by step (3) is carried out to solid solution and artificial aging heat treatment, solid solubility temperature successively Be 450~580 DEG C, solution time is 0.5~6h, and artificial aging temperature is 100~200 DEG C, the artificial aging time for 3~for 24 hours.
Preferably, aluminum substrate powder mean particle sizes are 60~80 μm in step (1), Nano-meter SiO_22Powder mean particle sizes are 10 ~50nm, Nano-meter SiO_22Mass percent of the powder in composite powder is 0.1%~1.5%.
Preferably, the mixing machine in step (1) uses ball mill, and drum's speed of rotation is 180~230r/min, during ball milling Between be 4~8h.
Preferably, the drum's speed of rotation is 180~210r/min, and Ball-milling Time is 5~6h.
Preferably, it is characterised in that：
Nano-meter SiO_2 in step (1)2Powder is hydrophobic fumed silica, and major parameter see the table below：
For the ease of demoulding and shaping, during the mixed powder of step (1), lubricant is added into raw material powder, the profit The quality of lubrication prescription is the 0.5%~2% of raw material powder quality.Lubricant can select stearic acid lubricant or paraffin.
Preferably, the addition manner of lubricant is mixed for hand mix or mixing machine, wherein, ball milling is selected in mixing machine mixing Any one mixing machine in machine, V-type blender, cone blender, fat formula mixer, ribbon mixer is mixed.
Lubricant influences composite material in order to prevent, first carries out dewaxing treatment, dewaxing to green body before the sintering of step (3) Temperature is 350~450 DEG C, and the dewaxing time is 20~50min.
Preferably, in step (2) the compression moulding mode of raw material powder using die forming, forming pressure for 150~ 500MPa。
In addition, for sintered part be pure aluminum substrate or heat treatment can not strengthen alloy matrix aluminum without step (4)。
Compared with prior art, the advantage of the invention is that：The present invention directly adds nanometer reinforcing phase, work in aluminum substrate Skill is simple, and required is general power metallurgy equipment, simple for process, suitable for Nano-meter SiO_22The Multiple components aluminium base zero of enhancing The powder metallurgically manufacturing of part has universality, conducive to promoting and mass producing.
The second phase Nano-meter SiO_2 is added in aluminum substrate2Particle, due to Nano-meter SiO_22The different conditions that particle is combined with matrix, Cause distortion of lattice occurs at particle and basal body interface, form complicated strain regime, therefore matrix is played significant strong Change acts on.Meanwhile Nano-meter SiO_22The presence of particle hinders dislocation motion so that the driving force needed for the movement of aluminum substrate Dislocations It greatly increases, so as to improve intensity.In addition, Nano-meter SiO_22The coefficient of thermal expansion difference of particle and matrix is larger, in sintering and heat It is differently strained caused by temperature change in processing procedure, a large amount of dislocation is necessarily introduced, also matrix is made to obtain partial reinforment Effect.Nano-meter SiO_22Powder or flow velocity reinforcing agent can improve the mobility and fillibility of raw material powder, be conducive to improve forming The uniformity of density improves intensity.Therefore obtained Properties of Aluminum Matrix Composites is preferable.
Description of the drawings
Fig. 1 is Nano-meter SiO_2 in the embodiment of the present invention 22The microscopic appearance figure of particle；
Fig. 2 is the fracture apperance figure of sintered part in the embodiment of the present invention 2；
Fig. 3 is the microscopic appearance figure of mixed-powder in the embodiment of the present invention 7.
Specific embodiment
With reference to the accompanying drawings and examples, the specific embodiment of the present invention is described in further detail.
Embodiment 1：
The present embodiment is by taking pure aluminum substrate as an example, to Nano-meter SiO_22The preparation method of reinforced aluminum matrix composites illustrates, Specifically include following steps：
(1) powder is mixed：The Nano-meter SiO_2 for being 50nm with average grain diameter by the aluminium elemental powders that average grain diameter is 60 μm2Powder is used Mortar grinder is uniformly mixed, and obtains raw material powder, wherein Nano-meter SiO_22Mass fraction of the powder in raw material powder is 0.01%, Surplus is aluminium elemental powders.Nano-meter SiO_2 used in the step2Powder can be preferably hydrophobic fumed silica, main Parameter see the table below：
(2) it shapes：Powder obtained by step (1) is subjected to die forming, pressing pressure 150MPa, dwell time 15s.
(3) it is sintered：It is sintered using tube furnace, sintering protective atmosphere is high-purity N2, sintering temperature is 650 DEG C, sintered heat insulating Time is 60min, furnace cooling after heat preservation.The sintering environment of the step can be preferably oxygen content less than 10ppm, dew point Less than -40 DEG C.
By test, non-plus nano SiO2The flow velocity of the pure aluminium powder of powder is 110S/50g；Add in 0.01% Nano-meter SiO_22 After powder, flow velocity becomes 102S/50g.Non- plus nano SiO2Intensity is 68MPa after the fine aluminium powder sintering of powder；Pure aluminium powder adds in 0.01% Nano-meter SiO_22After powder, the intensity for the aluminum matrix composite being sintered is 76MPa.
Embodiment 2：
The present embodiment is by taking 2014 alloy matrix aluminums as an example, to Nano-meter SiO_22The preparation method of reinforced aluminum matrix composites carries out Illustrate, specifically include following steps：
(1) powder is mixed：The Nano-meter SiO_2 for being 16nm with average grain diameter by 2014 Al alloy powders that average grain diameter is 78 μm2Powder End is mixed to get raw material powder, and raw material powder ball milling 4h on the planetary ball mill that rotating speed is 180r/min is uniformly mixed, Middle Nano-meter SiO_22Mass fraction of the powder in raw material powder is 1%, and surplus is 2014 Al alloy powders.Nanometer used in the step SiO2Powder is preferably hydrophobic fumed silica, and major parameter see the table below：
(2) it shapes：Using V-type blender, it is the mass fraction that accounts for raw material powder will be mixed into powder obtained by step (1) Powder after mixing, is carried out die forming, pressing pressure 400MPa is protected by the zinc stearate of 0.5wt% as lubricant The pressure time is 20s；
(3) it is sintered：It is sintered using net belt type continuous oven, sintering protective atmosphere is high-purity N2, dewaxing temperature is 350 DEG C, is taken off The wax time is 30min；Sintering temperature is 560 DEG C, and the sintered heat insulating time is 40min, and furnace cooling after heat preservation controls cooling Speed makes to be down to room temperature in 2h, obtains sintered part.The sintering environment of step sintering can be preferably that oxygen content is less than 10ppm, dew point are less than -40 DEG C.As shown in Fig. 2, Nano-meter SiO_22Enhance the sintered part section dimple of 2014 Al alloy composites Significantly, show that sintered part realizes good metallurgical binding, there is higher mechanical performance.
(4) it is heat-treated：Above-mentioned sintered part is carried out to solid solution and artificial aging heat treatment successively, solid solubility temperature is 510 DEG C, Gu The molten time is 1h, and artificial aging temperature is 180 DEG C, and the artificial aging time is 15h.
And by test, non-plus nano SiO2The flow velocity of 2014 Al alloy powders of powder is 90S/50g；Add in 1% Nano-meter SiO_22After powder, flow velocity becomes 79S/50g.Non- plus nano SiO2Intensity is after the 2014 Al alloy powders sintering of powder 210MPa；2014 Al alloy powders add in 1% Nano-meter SiO_22After powder, the intensity for the aluminum matrix composite being sintered is 235MPa。
Embodiment 3：
The present embodiment is by taking 7039 alloy matrix aluminums as an example, to Nano-meter SiO_22The preparation method of reinforced aluminum matrix composites carries out Illustrate, specifically include following steps：
(1) powder is mixed：The Nano-meter SiO_2 for being 10nm with average grain diameter by 7039 Al alloy powders that average grain diameter is 45 μm2Powder End is mixed to get raw material powder, and raw material powder ball milling 4.5h on the planetary ball mill that rotating speed is 185r/min is uniformly mixed, Wherein Nano-meter SiO_22Mass fraction of the powder in raw material powder is 1.5%, and surplus is 7039 Al alloy powders.Used in the step Nano-meter SiO_22Powder is preferably hydrophobic fumed silica, and major parameter see the table below：
(2) it shapes：Using ribbon mixer, the mass fraction for accounting for raw material powder will be mixed into powder obtained by step (1) Powder after mixing, is carried out die forming, pressing pressure 180MPa is protected by the zinc stearate for 0.8% as lubricant The pressure time is 15s；
(3) it is sintered：It is sintered using net belt type continuous oven, sintering protective atmosphere is high-purity N2, dewaxing temperature is 350 DEG C, is taken off The wax time is 22min；Sintering temperature is 550 DEG C, and the sintered heat insulating time is 5min, and furnace cooling after heat preservation controls cooling Speed makes to be down to room temperature in 0.5h, obtains sintered part.The sintering environment of step sintering can be preferably that oxygen content is less than 10ppm, dew point are less than -40 DEG C.
(4) it is heat-treated：Above-mentioned sintered part is carried out to solid solution and artificial aging heat treatment successively, solid solubility temperature is 450 DEG C, Gu The molten time is 0.8h, and artificial aging temperature is 150 DEG C, and the artificial aging time is 3h.
By test, non-plus nano SiO2The flow velocity of 7039 Al alloy powders of powder is 92S/50g；Addition 1.5% is received Rice SiO2After powder, flow velocity becomes 86S/50g.Non- plus nano SiO2Intensity is 134MPa after the 7039 Al alloy powders sintering of powder； 7039 Al alloy powders add in 1.5% Nano-meter SiO_22After powder, the intensity for the aluminum matrix composite being sintered is 143MPa.
Embodiment 4：
The present embodiment is by taking 6061 alloy matrix aluminums as an example, to Nano-meter SiO_22The preparation method of reinforced aluminum matrix composites carries out Illustrate, specifically include following steps：
(1) powder is mixed：The Nano-meter SiO_2 for being 5nm with average grain diameter by 6061 Al alloy powders that average grain diameter is 80 μm2Powder It is mixed to get raw material powder, wherein Nano-meter SiO_22The mass fraction that powder accounts for raw material powder is 5%, and surplus is 6061 Al alloy powders End.Raw material powder ball milling 5h, 0.5h before ball milling terminates on the planetary ball mill that rotating speed is 180r/min, to raw material powder Middle add accounts for stearic acid that the mass fraction of raw material powder is 1.5% as lubricant, after ball milling, acquisition mixed-powder. Nano-meter SiO_2 used in the step2Powder can be preferably hydrophobic fumed silica, and major parameter see the table below：
(2) it shapes：Powder obtained by step (1) is subjected to die forming, pressing pressure 200MPa, dwell time 10s.
(3) it is sintered：It is sintered using push-down continuous oven, sintering protective atmosphere is high-purity N2, the oxygen content for being sintered environment is low In 10ppm, dew point is less than -40 DEG C, and dewaxing temperature is 450 DEG C, and the dewaxing time is 20min；Sintering temperature is 590 DEG C, and sintering is protected The warm time is 60min, and furnace cooling after heat preservation controls cooling velocity to make to be down to room temperature in 3h, obtains sintered part.The step Rapid sintering environment is preferably that oxygen content is less than 10ppm, and dew point is less than -40 DEG C.
(4) it is heat-treated：Above-mentioned sintered part is carried out to solid solution and artificial aging heat treatment successively, solid solubility temperature is 580 DEG C, Gu The molten time is 0.5h；Artificial aging temperature is 160 DEG C, and the artificial aging time is for 24 hours.
By test, non-plus nano SiO2The flow velocity of 6061 Al alloy powders of powder is 93S/50g；Add in 5% nanometer SiO2After powder, flow velocity becomes 84S/50g.Non- plus nano SiO2Intensity is 127MPa after the 6061 Al alloy powders sintering of powder； 6061 Al alloy powders add in 5% Nano-meter SiO_22After powder, the intensity for the aluminum matrix composite being sintered is 151MPa.
Embodiment 5：
The present embodiment is by taking 6061 alloy matrix aluminums as an example, to Nano-meter SiO_22The preparation method of reinforced aluminum matrix composites carries out Illustrate, specifically include following steps：
(1) powder is mixed：The Nano-meter SiO_2 for being 35nm with average grain diameter by 6061 Al alloy powders that average grain diameter is 75 μm2Powder End is mixed to get raw material powder, wherein Nano-meter SiO_22The mass fraction that powder accounts for raw material powder is 1.2%, and surplus is closed for 6061 aluminium Bronze end.Raw material powder ball milling 5.5h, 0.5h, Xiang Yuan before ball milling terminates on the planetary ball mill that rotating speed is 185r/min The stearic acid that the mass fraction that addition accounts for raw material powder in feed powder end is 1.8% after ball milling, is mixed as lubricant Powder.Nano-meter SiO_2 used in the step2Powder can be preferably hydrophobic fumed silica, and major parameter see the table below：
(2) it shapes：Powder obtained by step (1) is subjected to die forming, pressing pressure 350MPa, dwell time 25s.
(3) it is sintered：It is sintered using push-down continuous oven, sintering protective atmosphere is high-purity N2, the oxygen content for being sintered environment is low In 10ppm, dew point is less than -40 DEG C, and dewaxing temperature is 370 DEG C, and the dewaxing time is 45min；Sintering temperature is 660 DEG C, and sintering is protected The warm time is 55min, and furnace cooling after heat preservation controls cooling velocity to make to be down to room temperature in 2.5h, obtains sintered part.It should The sintering environment of step is preferably that oxygen content is less than 10ppm, and dew point is less than -40 DEG C.
(4) it is heat-treated：Above-mentioned sintered part is carried out to solid solution and artificial aging heat treatment successively, solid solubility temperature is 550 DEG C, Gu The molten time is 3.5h；Artificial aging temperature is 200 DEG C, and the artificial aging time is 15h.
By test, non-plus nano SiO2The flow velocity of 6061 Al alloy powders of powder is 95S/50g；Addition 1.2% is received Rice SiO2After powder, flow velocity becomes 82S/50g.Non- plus nano SiO2Intensity is 193MPa after the 6061 Al alloy powders sintering of powder； 6061 Al alloy powders add in 1.2% Nano-meter SiO_22After powder, the intensity for the aluminum matrix composite being sintered is 209MPa.
Embodiment 6：
The present embodiment is by taking 7075 alloy matrix aluminums as an example, to Nano-meter SiO_22The preparation method of reinforced aluminum matrix composites carries out Illustrate, specifically include following steps：
(1) powder is mixed：The Nano-meter SiO_2 for being 8nm with average grain diameter by 7075 Al alloy powders that average grain diameter is 100 μm2Powder End mixing obtains raw material powder, the wherein Nano-meter SiO_2 in raw material powder2The mass fraction of powder is 0.5%, and surplus is 7075 aluminium Alloy powder.Raw material powder ball milling 5h, 0.5h, Xiang Yuan before ball milling terminates on the planetary ball mill that rotating speed is 200r/min The paraffin that the mass fraction that addition accounts for raw material powder in feed powder end is 2% after ball milling, obtains mixed powder as lubricant End.Nano-meter SiO_2 used in the step2Powder can be preferably hydrophobic fumed silica, and major parameter see the table below：
(2) it shapes：Powder obtained by step (1) is subjected to die forming, pressing pressure 450MPa, dwell time 30s.
(3) it is sintered：It is sintered using push-down continuous oven, sintering protective atmosphere is high-purity N2, dewaxing temperature is 350 DEG C, is taken off The wax time is 50min；Sintering temperature is 620 DEG C, and the sintered heat insulating time is 30min, and furnace cooling after heat preservation controls cooling Speed makes to be down to room temperature in 3h, obtains sintered part.The sintering environment of step sintering can be preferably that oxygen content is less than 10ppm, dew point are less than -40 DEG C.
(4) it is heat-treated:Above-mentioned sintered part is carried out to solid solution and artificial aging heat treatment successively, solid solubility temperature is 460 DEG C, Gu The molten time is 6h, and artificial aging temperature is 100 DEG C, and the artificial aging time is 8h.
By test, non-plus nano SiO2The flow velocity of 7075 Al alloy powders of powder is 98S/50g；Addition 0.5% is received Rice SiO2After powder, flow velocity becomes 85S/50g.Non- plus nano SiO2Intensity is 241MPa after the 7075 Al alloy powders sintering of powder； 7075 Al alloy powders add in 0.5% Nano-meter SiO_22After powder, the intensity for the aluminum matrix composite being sintered is 282MPa.
Embodiment 7：
The present embodiment is by taking silumin 4A11 alloy matrix aluminums as an example, to Nano-meter SiO_22The system of reinforced aluminum matrix composites Preparation Method illustrates, and specifically includes following steps：
(1) powder is mixed：The Nano-meter SiO_2 for being 145nm with average grain diameter by the 4A11 Al alloy powders that average grain diameter is 30 μm2Powder End is mixed to get raw material powder, the wherein Nano-meter SiO_2 in raw material powder2The mass fraction of powder is 0.08%, surplus 4A11 Al alloy powder.Raw material powder ball milling 6h, 0.5h before ball milling terminates on the planetary ball mill that rotating speed is 200r/min, to The stearic acid that the mass fraction that addition accounts for raw material powder in raw material powder is 1.5%, after ball milling, obtains mixed-powder.It should Nano-meter SiO_2 used in step2Powder can be preferably hydrophobic fumed silica, and major parameter see the table below：
(2) it shapes：Powder obtained by step (1) is subjected to die forming, pressing pressure 250MPa, dwell time 10s.
(3) it is sintered：It is sintered using tube furnace, sintering protective atmosphere is high-purity N2, dewaxing temperature is 400 DEG C, dewaxing Time is 35min；Sintering temperature is 610 DEG C, and the sintered heat insulating time is 50min, and furnace cooling after heat preservation, control cools down fast Degree makes to be down to room temperature in 1h, obtains sintered part.The sintering environment of step sintering can be preferably that oxygen content is less than 10ppm, Dew point is less than -40 DEG C.
(4) it is heat-treated：Above-mentioned sintered part is carried out to solid solution and artificial aging heat treatment successively, solid solubility temperature is 525 DEG C, Gu The molten time is 1.5h, and artificial aging temperature is 175 DEG C, and the artificial aging time is 10h.
By test, non-plus nano SiO2The flow velocity of the 4A11 Al alloy powders of powder is 103S/50g；Add in 0.08% Nano-meter SiO_22After powder, flow velocity becomes 97S/50g.Non- plus nano SiO2Intensity is after the 4A11 Al alloy powders sintering of powder 186MPa；4A11 Al alloy powders add in 0.08% Nano-meter SiO_22After powder, the intensity for the aluminum matrix composite being sintered is 198MPa。
Embodiment 8：
The present embodiment is by taking silumin Al-10Si matrixes as an example, to Nano-meter SiO_22The preparation of reinforced aluminum matrix composites Method illustrates, and specifically includes following steps：
(1) powder is mixed：The nanometer for being 100nm with average grain diameter by the Al-10Si Al alloy powders that average grain diameter is 50 μm SiO2Powder is mixed to get raw material powder, the wherein Nano-meter SiO_2 in raw material powder2The mass fraction of powder is 0.05%, and surplus is Al-10Si Al alloy powders.Raw material powder ball milling 8h on the planetary ball mill that rotating speed is 230r/min, before ball milling terminates 0.5h, the paraffin that the mass fraction that addition accounts for raw material powder into raw material powder is 1.5% is as lubricant, after ball milling, Obtain mixed-powder.Nano-meter SiO_2 used in the step2Powder can be preferably hydrophobic fumed silica, major parameter It see the table below：
(2) it shapes：Powder obtained by step (1) is subjected to die forming, pressing pressure 250MPa, dwell time 10s.
(3) it is sintered：It is sintered using net belt type continuous oven, sintering protective atmosphere is high-purity N2, dewaxing temperature is 380 DEG C, is taken off The wax time is 40min；Sintering temperature is 595 DEG C, and the sintered heat insulating time is 45min, and furnace cooling after heat preservation controls cooling Speed makes to be down to room temperature in 3h, obtains sintered part.The sintering environment of step sintering can be preferably that oxygen content is less than 10ppm, dew point are less than -40 DEG C.
(4) it is heat-treated：Above-mentioned sintered part is carried out to solid solution and artificial aging heat treatment successively, solid solubility temperature is 520 DEG C, Gu The molten time is 2h, and artificial aging temperature is 170 DEG C, and the artificial aging time is 10h.
By test, non-plus nano SiO2The flow velocity of the Al-10Si Al alloy powders of powder is 107S/50g；Add in 0.05% Nano-meter SiO_22After powder, flow velocity becomes 95S/50g.Non- plus nano SiO2Intensity is after the Al-10Si Al alloy powders sintering of powder 130MPa；Al-10Si Al alloy powders add in 0.05% Nano-meter SiO_22After powder, the intensity for the aluminum matrix composite being sintered It is 145MPa.
Embodiment 9：
The Al that the present embodiment is enhanced with ceramic particle2O3For -2024 aluminum matrix composite matrixes, to Nano-meter SiO_22Enhancing The preparation method of aluminum matrix composite illustrates, and specifically includes following steps：
(1) powder is mixed：By the Al that average grain diameter is 85 μm2O3- 2024 aluminum matrix composite powder are 15nm's with average grain diameter Nano-meter SiO_22Powder mixing obtains raw material powder, the wherein Nano-meter SiO_2 in raw material powder2The mass fraction of powder is 0.1%, remaining It measures as Al2O3- 2024 aluminum matrix composite powder.Raw material powder ball milling 7h on the planetary ball mill that rotating speed is 210r/min, The 0.5h before ball milling terminates, the zinc stearate that the mass fraction that addition accounts for raw material powder into raw material powder is 1% is as lubrication Agent after ball milling, obtains mixed-powder.As shown in Figure 3, it is seen that Al2O3- 2024 based composites powder and Nano-meter SiO_22Powder End is uniformly mixed, Nano-meter SiO_22Particle can be well combined with matrix after sintering, significantly increase mechanical property.It is received used in the step Rice SiO2Powder can be preferably hydrophobic fumed silica, and major parameter see the table below：
(2) it shapes：Powder obtained by step (1) is subjected to die forming, pressing pressure 300MPa, dwell time 20s.
(3) it is sintered：It is sintered using net belt type continuous oven, sintering protective atmosphere is high-purity N2, dewaxing temperature is 440 DEG C, is taken off The wax time is 25min；Sintering temperature is 585 DEG C, and the sintered heat insulating time is 40min, and furnace cooling after heat preservation controls cooling Speed makes to be down to room temperature in 2h, obtains sintered part.The sintering environment of step sintering can be preferably that oxygen content is less than 10ppm, dew point are less than -40 DEG C.
(4) it is heat-treated：Above-mentioned sintered part is subjected to solid solution and artificial aging heat treatment, solid solubility temperature is 490 DEG C, during solid solution Between for 1h, artificial aging temperature is 190 DEG C, and the artificial aging time is 20h.
By test, non-plus nano SiO2The Al of powder2O3The flow velocity of -2024 powder is 94S/50g；Add in 0.1% nanometer SiO2After powder, flow velocity becomes 81S/50g.Non- plus nano SiO2The Al of powder2O3Intensity is 226MPa after -2024 powder sinterings； Al2O3- 2024 powder add in 0.1% Nano-meter SiO_22After powder, the intensity for the aluminum matrix composite being sintered is 257MPa.
Embodiment 10：
The present embodiment is for being heat-treated 3003 alloy matrix aluminums that can not strengthen, to Nano-meter SiO_22Enhance aluminum-base composite material The preparation method of material illustrates, and specifically includes following steps：
(1) powder is mixed：The Nano-meter SiO_2 for being 70nm with average grain diameter by 3003 Al alloy powders that average grain diameter is 70 μm2Powder End mixing obtains raw material powder, the wherein Nano-meter SiO_2 in raw material powder2The mass fraction of powder is 0.4%, and surplus is 3003 aluminium Alloy powder.Raw material powder ball milling 4h, 0.5h, Xiang Yuan before ball milling terminates on the planetary ball mill that rotating speed is 190r/min The paraffin that the mass fraction that addition accounts for raw material powder in feed powder end is 1.5% after ball milling, obtains mixed powder as lubricant End.Nano-meter SiO_2 used in the step2Powder can be preferably hydrophobic fumed silica, and major parameter see the table below：
(2) it shapes:Die forming, pressing pressure 500MPa, dwell time 10s will be carried out obtained by step (1).
(3) it is sintered：It is sintered using push-down continuous oven, sintering protective atmosphere is high-purity N2, dewaxing temperature is 400 DEG C, is taken off The wax time is 30min；Sintering temperature is 570 DEG C, and the sintered heat insulating time is 40min, and furnace cooling after heat preservation controls cooling Speed makes to be down to room temperature in 3h, obtains sintered part.The sintering environment of step sintering can be preferably that oxygen content is less than 10ppm, dew point are less than -40 DEG C.
By test, non-plus nano SiO2The flow velocity of 3003 Al alloy powders of powder is 91S/50g；Addition 0.4% is received Rice SiO2After powder, flow velocity becomes 78S/50g.Non- plus nano SiO2Intensity is 112MPa after the 3003 Al alloy powders sintering of powder； 3003 Al alloy powders add in 0.4% Nano-meter SiO_22After powder, the intensity for the aluminum matrix composite being sintered is 140MPa.

Claims (10)

1. a kind of Nano-meter SiO_22The preparation method of reinforced aluminum matrix composites, it is characterised in that include the following steps：
(1) powder is mixed：By aluminum substrate powder and Nano-meter SiO_22Powder is mixed to get raw material powder, and the raw material powder is using mixed manually It closes or mixing machine mixes to be uniformly mixed, wherein, the average particle size of aluminium elemental powders or Al alloy powder is 30~100 μm, is received Rice SiO2The average particle size of powder be 5~145nm, Nano-meter SiO_22Mass percent in raw material powder is 0.01%~5%, Surplus is aluminum substrate powder, and the aluminum substrate powder is aluminium elemental powders or Al alloy powder or aluminum matrix composite powder；
(2) it shapes:By powder pressing obtained by step (1), green body is obtained；
(3) it is sintered:Green body obtained by step (2) is sintered under protective atmosphere, sintering temperature is 550~660 DEG C, during heat preservation Between for 5~60min, furnace cooling after heat preservation continues the Slow cooling in the case where protective atmosphere is protected, cooling time 0.5 ~3h obtains sintered part；
(4) it is heat-treated：Sintered part obtained by step (3) is carried out to solid solution and artificial aging heat treatment, solid solubility temperature 450 successively ~580 DEG C, solution time is 0.5~6h, and artificial aging temperature is 100~200 DEG C, the artificial aging time for 3~for 24 hours.
2. Nano-meter SiO_2 according to claim 12The preparation method of reinforced aluminum matrix composites, it is characterised in that：Step (1) Middle aluminum substrate powder mean particle sizes are 60~80 μm, Nano-meter SiO_22Powder mean particle sizes be 10~50nm, Nano-meter SiO_22Powder is multiple It is 0.1%~1.5% to close the mass percent in powder.
3. the Nano-meter SiO_2 according to right wants 12The preparation method of reinforced aluminum matrix composites, it is characterised in that：In step (1) In mixing machine using ball mill, drum's speed of rotation is 180~230r/min, and Ball-milling Time is 4~8h.
4. Nano-meter SiO_2 according to claim 32The preparation method of reinforced aluminum matrix composites, it is characterised in that：The ball Mill speed is 180~210r/min, and Ball-milling Time is 5~6h.
5. the Nano-meter SiO_2 according to right wants 12The preparation method of reinforced aluminum matrix composites, it is characterised in that：
Nano-meter SiO_2 in step (1)2Powder is hydrophobic fumed silica, and major parameter see the table below：
6. Nano-meter SiO_2 according to claim 12The preparation method of reinforced aluminum matrix composites, it is characterised in that：In step (1) during mixed powder, lubricant is added into raw material powder, the quality of the lubricant for raw material powder quality 0.5%~ 2%.
7. Nano-meter SiO_2 according to claim 62The preparation method of reinforced aluminum matrix composites, it is characterised in that：Lubricant Addition manner mixed for hand mix or mixing machine, wherein, ball mill, V-type blender, taper mixing are selected in mixing machine mixing Any one mixing machine in device, fat formula mixer, ribbon mixer is mixed.
8. the Nano-meter SiO_2 described according to claim 6 or 72The preparation method of reinforced aluminum matrix composites, it is characterised in that：
Dewaxing treatment is first carried out to green body before the sintering of step (3), dewaxing temperature is 350~450 DEG C, the dewaxing time for 20~ 50min。
9. Nano-meter SiO_2 according to claim 12The preparation method of reinforced aluminum matrix composites, it is characterised in that：Step (2) The compression moulding mode of middle raw material powder uses die forming, and forming pressure is 150~500MPa.
10. Nano-meter SiO_2 according to claim 12The preparation method of reinforced aluminum matrix composites, it is characterised in that：For burning Knot part be pure aluminum substrate or be heat-treated can not strengthen alloy matrix aluminum without step (4).
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