CN108441665A - Multi-dimensional vibration assists the method for being synthetically prepared nanodispersed granular materials - Google Patents

Multi-dimensional vibration assists the method for being synthetically prepared nanodispersed granular materials Download PDF

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CN108441665A
CN108441665A CN201810169414.5A CN201810169414A CN108441665A CN 108441665 A CN108441665 A CN 108441665A CN 201810169414 A CN201810169414 A CN 201810169414A CN 108441665 A CN108441665 A CN 108441665A
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vibration
dimensional
granular materials
assists
electric machine
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CN108441665B (en
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王宏明
李桂荣
赵玉涛
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Jiangsu University
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Jiangsu University
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Priority to PCT/CN2018/093489 priority patent/WO2019165736A1/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/047Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • C22C1/1047Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • C22C1/1047Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
    • C22C1/1052Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites by mixing and casting metal matrix composites with reaction
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C32/00Non-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
    • C22C32/001Non-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
    • C22C32/0015Non-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
    • C22C32/0036Matrix based on Al, Mg, Be or alloys thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00Aspects linked to processes or compositions used in powder metallurgy

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  • Composite Materials (AREA)
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  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Treatment Of Steel In Its Molten State (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The present invention provides a kind of methods that multi-dimensional vibration assists being synthetically prepared nanodispersed granular materials, belong to technical field of material.The vibration of multidimensional frequency low-amplitude is applied to melt in the fusant reaction building-up process of particulate reinforced composite in situ, promotes the progress of fusant reaction synthesis, meanwhile, to promoting particle dispersion, overcoming cluster and promoting the separation of slag gold that there is obvious action effect.Other advantages using the present invention also reside in, and the present invention has the technology economy advantages such as simple, contactless, the at low cost, significant effect of method.

Description

Multi-dimensional vibration assists the method for being synthetically prepared nanodispersed granular materials
Technical field
The present invention relates to the preparing technical field of particles reiforced metal-base composition, it is related specifically to utilize multi-dimensional vibration The method for assisting being synthetically prepared nanodispersed granular materials.
Background technology
Particles reiforced metal-base composition is due to having both good mechanical property and reason with compound structure feature Change performance, there is wide application in fields such as advanced electrotechnical, electronic device, aerospace vehicle, machinery, bridge tunnel engineerings Foreground, it has also become one of the research hotspot of metal-base composites in recent years;It is particle reinforced aluminium-based compound with going deep into for research Material is increasingly becoming a kind of using more and more extensive new material;Currently, fusant reaction synthetic method is to prepare particle enhancing The important method of aluminum matrix composite, this method are by the way that reactant is added into melt, by between reactant and aluminum substrate In-situ chemical reaction forms enhancing particle phase;Since the reactant of addition is essentially all solid phase, thus reactant and melt it Between reaction belong to typical solid-liquid phase reaction, the forming core of the dispersion of solid-phase reactant, in-situ chemical reaction and in-situ particle is long Greatly, dispersion etc. all has a major impact In-situ reaction preparation process, and then influences materials microstructure and performance, and therefore, melt is anti- The process control that should be synthesized is always the key that melting-reaction method prepares particle enhanced aluminum-based composite material, is had attracted much attention.
Through retrieval, metal matrix composition home-position synthesizing under a kind of combined electric magnetic field of Chinese patent CN101391291A propositions Method, the magnetic field combined by rotating excitation field and travelling-magnetic-field applied to the in-situ reactive synthesis process of melt, which can be with Improve solid-phase reactant and generate the dispersibility of particle, so as to improve the dynamic conditions of reaction;It is proposed building-up process in situ The prior art for applying low frequency magnetic field stirring also has:Chinese patent CN 101199989C (denominations of invention:Alien frequencies composite electromagnetic field The method of lower continuous casting particulate reinforced metal matrix composite material) and Chinese patent CN 1667147C (denominations of invention:A kind of work Industry scale prepares the preparation method of endogenous granular reinforced aluminum base composite material) etc.;The above prior art synthesizes fusant reaction Whole process applies a form of low frequency magnetic field, and the particle of the melt and its formation that make in-situ reactive synthesis process generates orientation Movement has certain limitation in terms of the dynamics for overcoming particle clusters, improvement reaction.
The process that melt directly reaction is synthetically prepared in-situ particle enhancing composite material is typical solid-liquid phase reaction, in height Under temperature, reaction in-situ process, the forming core precipitation process of particle, the movement dispersion process of particle and the limit of slag gold separation process Speed link is all the dynamic conditions of reaction in-situ, therefore, further increases rate, the particle recovery rate of reaction in-situ, with And particle refinement dispersion is promoted to be detached with slag gold, need to develop a kind of abundant improvement in-situ reactive synthesis process kinetics condition Method.
Invention content
The purpose of the present invention is:Preparing in-situ particle according to melting-reaction method enhances the building-up process dynamics of composite material Needs, provide it is a kind of using multi-dimensional vibration assist be synthetically prepared nanodispersed granular materials method, solve melt it is anti- Fabricated in situ is answered to prepare problem caused by particulate reinforced composite process kinetics condition speed limit.
The purpose of the present invention is achieved through the following technical solutions:
In the preparation process that direct reaction method synthesis particle enhances composite material, i.e., adjusted after the refining of Metal Substrate melt Whole to arrive reacting initial temperature, the reaction medicinal powder for generating particle phase can be reacted with melt in situ by, which being added, carries out synthetic reaction, anti- It answers in building-up process and the vibration of multidimensional frequency low-amplitude is applied to melt, play and improve reaction rate and utilization rate, shorten generated time, And achievees the purpose that control particle size, pattern and be distributed in matrix.
Multi-dimensional vibration assists the method for being synthetically prepared nanodispersed granular materials, which is characterized in that it is main include with Lower step:
(1) the preheated drying of reacting salt, metal bath melting to synthesis temperature;
(2) reacting salt is added in metal bath and carries out in-situ reactive synthesis;
(3) vibration is opened, multi-dimensional vibration is applied to melt, in-situ reactive synthesis process is made to complete under vibration;
(4) reaction terminates, and stops vibration, starts to cast.
Further, in the step (3), the vibration dimension for applying multi-dimensional vibration to the melt during reaction in-situ is It is more than three-dimensional and three-dimensional.
Further, multi-dimensional vibration is multidimensional high-frequency vibration, vibration frequency of the multi-dimensional vibration on each dimension direction Rate is in 500-1000Hz ranges, and the vibration frequency on each dimension direction is identical.
Further, multi-dimensional vibration is multidimensional low amplitude vibration, vibration width of the multi-dimensional vibration on each dimension direction Value is in 2-20 micron ranges, and the vibration amplitude on each dimension direction is identical.
Further, the multi-dimensional vibration is provided by vibrating device, and the vibrating device includes being connected to reaction in-situ Each four elastic wires, fixing bracket, the first shock electric machine, the second shock electric machine of the upper and lower ends of synthesis crucible, it is described The other end of elastic wire is connect with fixed holder, and the first shock electric machine and the second shock electric machine are separately mounted to the bottom of crucible Portion, the first shock electric machine make the two-dimension vibration of crucible generation horizontal direction, the second shock electric machine that crucible be made to generate vertical direction Two-dimension vibration.
Further, the coefficient of elasticity of 8 elastic wires is identical.
Further, the coefficient of elasticity of 8 elastic wires is not exactly the same.
Further, the first shock electric machine is formed by two single vibration motor combinations, and two single vibration motors shake In same level, direction is mutually perpendicular in dynamic direction.
It is to realize by the following method to apply the vibration of multidimensional frequency low-amplitude during in-situ reactive synthesis of the present invention 's:The upper and lower ends of in-situ reactive synthesis crucible are respectively connect by four elastic wires with fixed holder, at the bottom of crucible Portion's installation makes the shock electric machine that crucible generates the shock electric machine of horizontal direction two-dimension vibration and crucible is made to generate vertical vibration;Separately Outside, shock electric machine can also be that two single vibration motor combinations form, and the direction of vibration of two single vibration motors is same On horizontal plane, direction is mutually perpendicular to;When 8 elastic wires of fixed crucible are identical, in-situ reactive synthesis crucible reality Show three-dimensional vibrating, the melt and reacting salt in crucible vibrate therewith, and in-situ synthesized reaction is made to be completed under three-dimensional vibrating;When 8 When the coefficient of elasticity of elastic wire is not exactly the same, due to resonant frequency difference, in-situ reactive synthesis generates three with crucible crucible Vibration more than dimension, melt and reacting salt in crucible vibrate therewith, make effect of vibration of the in-situ synthesized reaction more than three-dimensional Lower completion.
Multi-dimensional vibration of the present invention assists the method for being synthetically prepared nanodispersed granular materials, is shaken using multidimensional Moving the principle of control in-situ reactive synthesis process is:
In fusant reaction building-up process, the mixed process of reacting salt and melt, forming core, precipitation and the long serious offense of particle phase The dispersion of journey and particle phase and slag gold separation process these links are the speed limit links of entire building-up process, to reaction System applies the main function that multidimensional high-frequency vibration plays:(1) accelerate the dispersion and melting of the reacting salt in powder state, The mixed process speed of reacting salt and melt is set to significantly improve;(2) vibration makes particle phase forming core rate improve, and precipitation rate increases Add, solves the problems, such as particle phase forming core, speed limit is precipitated, meanwhile, multi-dimensional vibration has the function of keeping bulky grain shatter, it is suppressed that Particle is grown up, notable micronized particles;(3) multi-dimensional vibration is conducive to refinement and the dispersion movement of particle, and helps to realize slag Gold due to density differential from Sunk-fund effect;Therefore, it is expected to using multi-dimensional vibration control in-situ reactive synthesis process in the present invention The bottleneck problem that fusant reaction synthetic method prepares particulate reinforced composite is solved, realizes more having to in-situ reactive synthesis process Effect control, improves reaction rate and particle recovery rate, and reaches control particle size, pattern in turn and uniformly divide in matrix The purpose of cloth.
Compared with prior art present invention has the advantage that:
Particulate reinforced composite synthesizes under multi-dimensional vibration effect, and most significant advantage is as follows:
(1) it is effectively improved the dynamic conditions of building-up process, improves the rate of fusant reaction building-up process links, Effectively shorten generated time and improve reactant utilization rate and recovery rate, experiments have shown that:Reaction generated time compares the prior art Shorten 50% or so, and utilization rate, that is, recovery rate of reactant is improved to 90% or more, and 10~20% are improved than the prior art.
(2) vibration of multidimensional frequency low-amplitude can inhibit the clusters of reinforced phase and grow up, control large-size particle and formed, particle Size Control is in nanoscale, and the apparent rounding of particle, improves the bond strength of particle and matrix, and is conducive to particle point It dissipates, improves the comprehensive performance of composite material.
(3) slag gold separative efficiency after reaction in-situ improves, and can shorten the refining after reaction and time of repose to original Half is especially a cancellation oversize particle and large scale slag inclusion.
Description of the drawings
Fig. 1 is that multi-dimensional vibration of the present invention assists the method equipment for being synthetically prepared nanodispersed granular materials to show It is intended to.
Fig. 2 is the scanning electron microscope (SEM) photograph that the embodiment 1 prepares material.
Fig. 3 is the scanning electron microscope (SEM) photograph that the embodiment 2 prepares material.
In figure:
1- holders;2- elastic wires;3- crucibles;The first shock electric machines of 4-;The second shock electric machines of 5-.
Specific implementation mode
The invention will be further elaborated with reference to embodiments;Embodiment is merely to illustrate the present invention, rather than with Any mode limits the present invention.
The present invention is to enhance the preparation process of composite material in direct reaction method synthesis particle, i.e. Metal Substrate melt essence Reacting initial temperature is adjusted to after refining, the reaction medicinal powder for generating particle phase can be reacted with melt in situ by, which being added, synthesize instead It answers, the vibration of multidimensional frequency low-amplitude is applied to melt in reacting building-up process, plays and improves reaction rate and utilization rate, shortens and closes At the time, and achievees the purpose that control particle size, pattern and be distributed in matrix.
It is the vibration of multidimensional frequency low-amplitude to the vibration that the melt during reaction in-situ applies, vibration dimension is three-dimensional and three More than dimension, the vibration frequency on each dimension direction is in 500-1000Hz ranges, and the vibration frequency on each dimension direction Identical, the vibration amplitude on each dimension direction is in 2-20 micron ranges, and the vibration amplitude on each dimension direction is identical.
Apply the vibration of multidimensional frequency low-amplitude during the in-situ reactive synthesis to realize by the following method:It is in situ The upper and lower ends of reaction synthesis crucible 3 are respectively connect by four elastic wires 2 with fixed holder 1, are pacified in the bottom of crucible 3 Dress makes the second exciting that crucible generates the first shock electric machine 4 of horizontal direction two-dimension vibration and crucible is made to generate vertical direction vibration Motor 5;It is formed in addition, the first shock electric machine 4 can also be two single vibration motor combinations, two single vibration motors shake In same level, direction is mutually perpendicular in dynamic direction.When the coefficient of elasticity of 8 elastic wires of fixed crucible is identical When, in-situ reactive synthesis realizes three-dimensional vibrating with crucible 3, and the melt and reacting salt in crucible vibrate therewith, keep fabricated in situ anti- It should be completed under three-dimensional vibrating.It is in situ due to resonant frequency difference when the coefficient of elasticity of 8 elastic wires is not exactly the same The vibration that synthesis generates three-dimensional or more with 3 crucible of crucible is reacted, the melt and reacting salt in crucible vibrate therewith, make fabricated in situ It reacts and is completed under the effect of vibration more than three-dimensional.
Embodiment one:Prepare (Al3Zr(s)+Al2O3(s)) particle enhanced aluminum-based composite material
Raw material:Parent metal:Commercial-purity aluminium;Solid powder:Industrial carbonic acid zirconium (Zr (CO3)2) pulvis, purity is 99.20wt.% refines degasser and agent of skimming;
Reaction in-situ equation:13Al(l)+3Zr(CO3)2(s)=3Al3Zr(s)+2Al2O3(s)+6CO2
Particulates reinforcements:Al3Zr(s)And Al2O3(s)
Preparation process is as follows:
The first step:The preheated drying of reacting salt, metal bath melting to synthesis temperature;
Commercial-purity aluminium 1Kg melts in 20kW crucible type resistance furnaces is warming up to 850 DEG C, deaerates, skims;Agents useful for same exists It is fully dried at 250 DEG C, wherein Zr (CO3)2It is ground into fine powder sieving, granularity is less than 100 μm, for use after weighing, Zr (CO3)2Add The weight entered is the 8% of weight metal.
Second step:Reacting salt is added in metal bath and carries out in-situ reactive synthesis;
The crucible for filling metal bath is placed in vibratile crucible 3, by solid reactant Zr (CO3)2Powder is added to In melt, in-situ reactive synthesis is carried out.
Third walks:Vibration is opened, in-situ reactive synthesis process is made to complete under vibration;
After reacting salt is added, the first shock electric machine 4, the vibration of the second shock electric machine 5 are immediately turned on.
In the present embodiment, the coefficient of elasticity of 8 elastic wires of fixed crucible is identical, in-situ reactive synthesis crucible 3 vibration dimension is three-dimensional, and the vibration frequency on each dimension direction is in 800Hz, the vibration on each dimension direction Amplitude is all 10 microns.Melt and reacting salt in crucible vibrate therewith, and in-situ synthesized reaction is made to be completed under three-dimensional vibrating.
(4):4th step:Reaction terminates, and stops vibration, starts to cast.
After reaction, the first shock electric machine 4, the second shock electric machine 5 are closed, vibration is stopped, (Al is made in casting3Zr(s) +Al2O3(s)) particle enhanced aluminum-based composite material.
Sampling analysis, dense internal organization, without the solidified structures defect such as loose, shrinkage cavity, particle size<100nm belongs to nanometer The as-cast structure scanning electron microscope (SEM) photograph of particulate reinforced composite, material is as shown in Figure 2.
It is using the outstanding feature of the invention:Particle size obviously refine to nanoscale, and granule roundness improves, big ruler Very little particle disappears, and nano particle shortened to 10 minutes without Cluster Phenomenon, reaction time from 20~30 minutes, and the yield of reactant carries It is high by about 20%, illustrate that reaction rate and yield improve, after sample corrodes, without any slag inclusion in composite material.
Embodiment two:Prepare Al2O3(s)Particle enhanced aluminum-based composite material
Raw material:Parent metal:Commercial-purity aluminium;Solid powder:Industrial carbonic acid cerium (Ce2(CO3)3) pulvis, purity is 99.20wt.% refines degasser and agent of skimming.
Reaction in-situ equation:4Al+3CeO2→2Al2O3+3Ce
Particulates reinforcements:Al2O3(s)
Preparation process is as follows:
The first step:The preheated drying of reacting salt, metal bath melting to synthesis temperature;
Commercial-purity aluminium 1Kg melts in 20kW crucible type resistance furnaces is warming up to 850 DEG C, deaerates, skims;Agents useful for same exists It is fully dried at 250 DEG C, wherein industrial carbonic acid cerium (Ce2(CO3)3) pulvis be ground into fine powder sieving, granularity be less than 100 μm, weigh It is for use afterwards, Ce2(CO3)3The weight of addition is the 10% of weight metal.
Second step:Reacting salt is added in metal bath and carries out in-situ reactive synthesis;
The crucible for filling metal bath is placed in vibratile crucible 3, by solid reactant Ce2(CO3)3Powder is added Into melt, in-situ reactive synthesis is carried out.
Third walks:Vibration is opened, in-situ reactive synthesis process is made to complete under vibration;
After reacting salt is added, the first shock electric machine 4, the vibration of the second shock electric machine 5 are immediately turned on.
In the present embodiment, the coefficient of elasticity of 8 elastic wires of fixed crucible is not exactly the same, not due to resonant frequency Together, in-situ reactive synthesis crucible 3 generates the vibration of three-dimensional or more, and the vibration frequency on each dimension direction exists 1000Hz, the vibration amplitude on each dimension direction are 2 microns.Melt and reacting salt in crucible 3 vibrate therewith, make original Position synthetic reaction is completed under the effect of vibration more than three-dimensional.
4th step:Reaction terminates, and stops vibration, starts to cast.
After reaction, vibrating motor is closed, vibration is stopped, Al is made in casting2O3(s)Particle enhanced aluminum-based composite material.
Sampling analysis, dense internal organization, without the solidified structures defect such as loose, shrinkage cavity, particle size<100nm belongs to nanometer The as-cast structure scanning electron microscope (SEM) photograph of particulate reinforced composite, material is as shown in Figure 3.
It is using the outstanding feature of the invention:Particle size obviously refine to nanoscale, and granule roundness improves, big ruler Very little particle disappears, and nano particle shortened to 10 minutes without Cluster Phenomenon, reaction time from 20 minutes, and the rate of the receipts of reactant improves About 18%, illustrate that reaction rate and yield improve, after sample corrodes, without any slag inclusion in composite material.
Embodiment three:Prepare (Al3Zr(s)+Al2O3(s)) particle enhanced aluminum-based composite material
Raw material:Parent metal:Commercial-purity aluminium;Solid powder:Industrial carbonic acid zirconium (Zr (CO3)2) pulvis, purity is 99.20wt.% refines degasser and agent of skimming;
Reaction in-situ equation:13Al(l)+3Zr(CO3)2(s)=3Al3Zr(s)+2Al2O3(s)+6CO2
Particulates reinforcements:Al3Zr(s)And Al2O3(s)
Preparation process is as follows:
The first step:The preheated drying of reacting salt, metal bath melting to synthesis temperature;
Commercial-purity aluminium 1Kg melts in 20kW crucible type resistance furnaces is warming up to 850 DEG C, deaerates, skims;Agents useful for same exists It is fully dried at 250 DEG C, wherein Zr (CO3)2It is ground into fine powder sieving, granularity is less than 100 μm, for use after weighing, Zr (CO3)2Add The weight entered is the 8% of weight metal.
Second step:Reacting salt is added in metal bath and carries out in-situ reactive synthesis;
The crucible for filling metal bath is placed in vibratile crucible 3, by solid reactant Zr (CO3)2Powder is added to In melt, in-situ reactive synthesis is carried out.
Third walks:Vibration is opened, in-situ reactive synthesis process is made to complete under vibration;
After reacting salt is added, the first shock electric machine 4, the vibration of the second shock electric machine 5 are immediately turned on.
In the present embodiment, the coefficient of elasticity of 8 elastic wires of fixed crucible is identical, in-situ reactive synthesis crucible 3 vibration dimension is three-dimensional, and the vibration frequency on each dimension direction is in 500Hz, the vibration on each dimension direction Amplitude is all 20 microns.
4th step:Reaction terminates, and stops vibration, starts to cast.
After reaction, the first shock electric machine 4, the second shock electric machine 5 are closed, vibration is stopped, (Al is made in casting3Zr(s) +Al2O3(s)) particle enhanced aluminum-based composite material.
Sampling analysis, dense internal organization, without the solidified structures defect such as loose, shrinkage cavity, particle size<100nm belongs to nanometer Particulate reinforced composite is using the outstanding feature of the invention:Particle size obviously refine to nanoscale, granule roundness It improves, large-size particle disappears, and nano particle shortened to 10 minutes without Cluster Phenomenon, reaction time from 20~30 minutes, reacts The rate of the receipts of object improves about 20%, illustrates that reaction rate and yield improve, after sample corrodes, without any slag inclusion in composite material.
Example IV:Prepare Al2O3(s)Particle enhanced aluminum-based composite material
Raw material:Parent metal:Commercial-purity aluminium;Solid powder:Industrial carbonic acid cerium (Ce2(CO3)3) pulvis, purity is 99.20wt.% refines degasser and agent of skimming;
Reaction in-situ equation:4Al+3CeO2→2Al2O3+3Ce
Particulates reinforcements:Al2O3(s)
Preparation process is as follows:
The first step:The preheated drying of reacting salt, metal bath melting to synthesis temperature;
Commercial-purity aluminium 1Kg melts in 20kW crucible type resistance furnaces is warming up to 850 DEG C, deaerates, skims;Agents useful for same exists It is fully dried at 250 DEG C, wherein industrial carbonic acid cerium (Ce2(CO3)3) pulvis be ground into fine powder sieving, granularity be less than 100 μm, weigh It is for use afterwards, Ce2(CO3)3The weight of addition is the 10% of weight metal.
Second step:Reacting salt is added in metal bath and carries out in-situ reactive synthesis;
The crucible for filling metal bath is placed in vibratile crucible 3, by solid reactant Ce2(CO3)3Powder is added Into melt, in-situ reactive synthesis is carried out.
Third walks:Vibration is opened, in-situ reactive synthesis process is made to complete under vibration;
After reacting salt is added, the first shock electric machine 4, the vibration of the second shock electric machine 5 are immediately turned on.
The first shock electric machine 4 is that two single vibration motor combinations form in the present embodiment, two single vibration motors In same level, direction is mutually perpendicular to direction of vibration;The coefficient of elasticity of 8 elastic wires is not exactly the same, due to resonance Frequency is different, and in-situ reactive synthesis generates the vibration of three-dimensional or more with 3 crucible of crucible, and the melt and reacting salt in crucible shake therewith It is dynamic, make to complete under effect of vibration of the in-situ synthesized reaction more than three-dimensional.Vibration frequency on each dimension direction exists 700Hz, the vibration amplitude on each dimension direction are 10 microns.
4th step:Reaction terminates, and stops vibration, starts to cast.
After reaction, vibrating motor is closed, vibration is stopped, Al is made in casting2O3(s)Particle enhanced aluminum-based composite material.
Sampling analysis, dense internal organization, without the solidified structures defect such as loose, shrinkage cavity, particle size<100nm belongs to nanometer Particulate reinforced composite is using the outstanding feature of the invention:Particle size obviously refine to nanoscale, granule roundness It improves, large-size particle disappears, and nano particle shortened to 10 minutes without Cluster Phenomenon, reaction time from 20 minutes, reactant The rate of receipts improves about 18%, illustrates that reaction rate and yield improve, after sample corrodes, without any slag inclusion in composite material.
The embodiment is the preferred embodiments of the present invention, but present invention is not limited to the embodiments described above, not Away from the present invention substantive content in the case of, those skilled in the art can make it is any it is conspicuously improved, replace Or modification all belongs to the scope of protection of the present invention.

Claims (8)

1. multi-dimensional vibration assists the method for being synthetically prepared nanodispersed granular materials, which is characterized in that include mainly following Step:
(1) the preheated drying of reacting salt, metal bath melting to synthesis temperature;
(2) reacting salt is added in metal bath and carries out in-situ reactive synthesis;
(3) vibration is opened, multi-dimensional vibration is applied to melt, in-situ reactive synthesis process is made to be completed under multi-dimensional vibration;
(4) reaction terminates, and stops vibration, starts to cast.
2. multi-dimensional vibration according to claim 1 assists the method for being synthetically prepared nanodispersed granular materials, special Sign is, in the step (3), the vibration dimension for applying multi-dimensional vibration to the melt during reaction in-situ is three-dimensional and three-dimensional More than.
3. multi-dimensional vibration according to claim 1 assists the method for being synthetically prepared nanodispersed granular materials, special Sign is that multi-dimensional vibration is multidimensional high-frequency vibration, and vibration frequency of the multi-dimensional vibration on each dimension direction is in 500- 1000Hz ranges, and the vibration frequency on each dimension direction is identical.
4. multi-dimensional vibration according to claim 1 assists the method for being synthetically prepared nanodispersed granular materials, special Sign is that multi-dimensional vibration is multidimensional low amplitude vibration, and vibration amplitude of the multi-dimensional vibration on each dimension direction is micro- in 2-20 Rice range, and the vibration amplitude on each dimension direction is identical.
5. multi-dimensional vibration described in claim 1 assists the method for being synthetically prepared nanodispersed granular materials, feature to exist In the multi-dimensional vibration is provided by vibrating device, and the vibrating device includes being connected to in-situ reactive synthesis crucible (3) Each four elastic wires (2) of upper and lower ends, fixing bracket (1), the first shock electric machine (4), the second shock electric machine (5), it is described The other end of elastic wire (2) is connect with fixed holder (1), and the first shock electric machine (4) and the second shock electric machine (5) are pacified respectively Mounted in the bottom of crucible, the first shock electric machine (4) makes the two-dimension vibration of crucible generation horizontal direction, the second shock electric machine
(5) crucible is made to generate the two-dimension vibration of vertical direction.
6. the multi-dimensional vibration described in claim 5 assists the method for being synthetically prepared nanodispersed granular materials, feature to exist In the coefficient of elasticity of 8 elastic wires (2) is identical.
7. the multi-dimensional vibration described in claim 5 assists the method for being synthetically prepared nanodispersed granular materials, feature to exist In the coefficient of elasticity of 8 elastic wires (2) is not exactly the same.
8. the multi-dimensional vibration described in claim 5 assists the method for being synthetically prepared nanodispersed granular materials, feature to exist In the first shock electric machine (4) is formed by two single vibration motor combinations, and the direction of vibration of two single vibration motors is same On horizontal plane, direction is mutually perpendicular to.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112458331A (en) * 2020-10-28 2021-03-09 北京康普锡威科技有限公司 Equipment for dispersing nano particles in alloy and preparation method of high-strength alloy

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20010016925A (en) * 1999-08-05 2001-03-05 황해웅 Device and Method for producing metal matrix composite materials by using plasma source
CN101055221A (en) * 2007-05-25 2007-10-17 江苏大学 Parallel device multiple-dimensional vibration platform
CN102121075A (en) * 2011-02-15 2011-07-13 江苏大学 Method for synthesizing particle reinforced aluminum-based composite under high-intensity ultrasonic field and pulsed electric field
US20140219861A1 (en) * 2010-11-10 2014-08-07 Purdue Research Foundation Method of producing particulate-reinforced composites and composites produced thereby
CN105132733A (en) * 2015-09-29 2015-12-09 华中科技大学 Method for preparing nano particle reinforced aluminum matrix composites

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104532046B (en) * 2014-12-24 2017-01-18 南昌大学 Method for preparing nano-aluminum-nitride reinforced aluminum-based composite semi-solid slurry based on ultrasonic and mechanical vibration combination
WO2016146829A1 (en) * 2015-03-18 2016-09-22 Innomaq 21, Sociedad Limitada Method of manufacturing of a casted part or ingot of a metallic alloy attaining a minimal segregation in the casting process
CN108359829A (en) * 2018-02-28 2018-08-03 江苏大学 The method in magnetic field and the lower synthesis particle enhancing composite material of vibration synergistic effect

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20010016925A (en) * 1999-08-05 2001-03-05 황해웅 Device and Method for producing metal matrix composite materials by using plasma source
CN101055221A (en) * 2007-05-25 2007-10-17 江苏大学 Parallel device multiple-dimensional vibration platform
US20140219861A1 (en) * 2010-11-10 2014-08-07 Purdue Research Foundation Method of producing particulate-reinforced composites and composites produced thereby
CN102121075A (en) * 2011-02-15 2011-07-13 江苏大学 Method for synthesizing particle reinforced aluminum-based composite under high-intensity ultrasonic field and pulsed electric field
CN105132733A (en) * 2015-09-29 2015-12-09 华中科技大学 Method for preparing nano particle reinforced aluminum matrix composites

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112458331A (en) * 2020-10-28 2021-03-09 北京康普锡威科技有限公司 Equipment for dispersing nano particles in alloy and preparation method of high-strength alloy

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