CN101956120A - Method and device for preparing nanoparticle reinforced aluminum base composite material - Google Patents
Method and device for preparing nanoparticle reinforced aluminum base composite material Download PDFInfo
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- CN101956120A CN101956120A CN 201010505938 CN201010505938A CN101956120A CN 101956120 A CN101956120 A CN 101956120A CN 201010505938 CN201010505938 CN 201010505938 CN 201010505938 A CN201010505938 A CN 201010505938A CN 101956120 A CN101956120 A CN 101956120A
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Abstract
The invention provides a method and a device for preparing a nanoparticle reinforced aluminum base composite material, and relates to the technical field of particle reinforced aluminum base composite material preparation. The method and the device are characterized in that: a combination electromagnetic field is formed by a high frequency magnetic field and a low frequency magnetic field; and the combination electromagnetic field and an ultrasonic field are coupled and applied to a melt reaction synthetic process of an in-situ particle reinforced aluminum base composite material so as to synthesize the endogenous nanoparticle reinforced metal base composite material under the action of coupling the double-frequency combination electromagnetic field and the high-energy ultrasonic field. The method and the device overcome the defects that only the electromagnetic field or the ultrasonic field is applied, and the single electromagnetic field is coupled with the ultrasonic field; and under the action of coupling the combination electromagnetic field and the ultrasonic field, a reinforced phase is refined to nanoscale, the shape of the particles is rounded off, the bonding strength of the particles and a substrate is improved, particle dispersion is facilitated, and the comprehensive performance of the composite material is improved.
Description
Technical field
The present invention relates to the preparing technical field of particle enhanced aluminum-based composite material, specially refer to the novel method that a kind of coupling outfield that utilizes combined electric magnetic field and ultrasonic field to form is controlled the fusant reaction building-up process of aluminum matrix composite.
Background technology
Particles reiforced metal-base composition has both good mechanical performance and physicochemical property owing to having the compound constitutional features, have broad application prospects in fields such as advanced person's electrotechnical, electronic device, aerospacecraft, machinery, bridge tunnel engineerings, become one of research focus of metal-base composites in recent years.Along with going deep into of research, particle enhanced aluminum-based composite material becomes a kind of application type material more and more widely just gradually.At present, the fusant reaction synthesis method is the important method of preparation particle enhanced aluminum-based composite material, and this method is by adding reactant in melt, forms enhanced granule mutually by reactant with in-situ chemical reaction between aluminum substrate.Because the reactant that adds all is solid phase basically, so the reaction between reactant and the melt belongs 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 grown up, dispersion etc. all has material impact to the compound preparation process of original position, and then influence the tissue and the performance of material, therefore, the process control of fusant reaction synthetic is the key that melting-reaction method prepares particle enhanced aluminum-based composite material always, enjoys attention.
By retrieval, Chinese patent CN101391291A proposes the method for metal matrix composition home-position synthesizing under a kind of combined electric magnetic field, reaction in building-up process to melt applies the magnetic field of being made up by rotatingfield and travelling-magnetic-field, this invention can improve solid-phase reactant and generate the particulate dispersiveness, thereby improve the dynamic conditions of reaction, the combination field that this invention applied, all be low frequency magnetic field (＜100Hz) to realize function composite by electromagnetic stirring, because the energy of low frequency magnetic field is low and dispersion, a little less than the thermodynamic condition influence to chemical reaction.Proposing building-up process in position applies the prior art that low frequency magnetic field stirs and also has: Chinese patent CN 101199989 (denomination of invention: the alien frequencies composite electromagnetic is the method for continuous casting particulate reinforced metal matrix matrix material after the match) and Chinese patent CN 1667147C (denomination of invention: a kind of preparation method of endogenous particle reinforced aluminium-based composite material) etc.Above prior art applies a kind of low frequency magnetic field of form to the whole process of fusant reaction synthetic, a little less than the thermodynamics influence of this magnetic field to complex reaction.
(denomination of invention: a kind of magnetic field and ultrasonic field coupling prepare the method for metal-base composites down to Chinese patent CN 101391290A, the process that proposes reaction in position applies magnetic field and ultransonic coupled field, the magnetic field that this invention proposed is single strong pulsed magnetic field, HF oscillation magnetic field or low frequency alternating magnetic field, this single magnetic field has characteristic separately, strong pulsed magnetic field and HF oscillation magnetic field can cause the fluctuation of energy of melt inside, the effect of the thermodynamic condition of influence reaction is outstanding, but a little less than its stirring action, to melt and reacting salt mix and the dynamic conditions influence of reaction faint; And adopt low frequency magnetic field to have good stirring action, but low frequency magnetic field is very little to the influence of thermodynamics of reactions.Therefore, adopt the coupling of single magnetic field and ultrasonic field, do not give full play to the advantage of electromagnetic field, the purpose of fusant reaction building-up process is accurately controlled in the realization outfield.
The process of the synthetic preparation of melt direct reaction in-situ particle reinforced composite is typical solid-liquid phase reaction, its reaction process relates to the thermodynamics and kinetics of reaction, therefore, desire realizes effect and the control to the reaction building-up process, should change the thermodynamics and kinetics condition of in-situ synthesized reaction simultaneously, the coupling outfield of selecting combined electric magnetic field and ultrasonic field to form is that an ideal is selected.
Summary of the invention
The objective of the invention is: the needs that prepare the building-up process thermodynamics and kinetics of particulate reinforced composite according to melting-reaction method, provide the coupled field that adopts combined electric magnetic field and ultrasonic field to form melt direct reaction legal system to be equipped with the method and apparatus of the building-up process control of in-situ nano particle enhanced aluminum-based composite material, give full play to outfield control advantage, improve the thermodynamics and kinetics condition of original position building-up process.
The objective of the invention is to realize by following technical proposal:
Preparation process according to the synthetic particle enhanced aluminum-based composite material of melt direct reaction method, be to adjust to reacting initial temperature after the aluminium base melt refining, adding can obtain Composite Melt with aluminium base melt in situ reaction generation particle reactant pulvis mutually and carry out building-up reactions, in the reaction building-up process, apply combined electric magnetic field and high-energy ultrasonic field simultaneously, question response finishes, and pours into a mould after leaving standstill teeming temperature.
Adopt characteristic feature of the present invention to be: in the fusant reaction synthesis method prepares the reaction in building-up process of particle enhanced aluminum-based composite material, to apply combined electric magnetic field and ultrasonic field simultaneously, the coupled field that realization combined electric magnetic field and ultrasonic field form is controlled the reaction in process, and then reach and improve thermodynamics of reactions and kinetics, realize control particle size, pattern and the purpose that in matrix, distributes.Realize that concrete technical scheme of the present invention is as follows in conjunction with the schematic view illustrating of Fig. 1:
The reaction building-up process of Composite Melt is carried out in the container (or crucible) that the thermal insulation fire-resistant material is made, combination field is installed in the outside at container, this combination field is made of high frequency magnetic field and low frequency magnetic field, high frequency magnetic field is installed on the outer wall of container, low frequency magnetic field is installed in the outside of high frequency magnetic field, leave between high frequency magnetic field and the low frequency magnetic field coil and guarantee the insulating gap, be generally 2～4cm.Assign the horn of Vltrasonic device on the top of Composite Melt.
In the fusant reaction synthesis method prepares the reaction in building-up process of particle enhanced aluminum-based composite material, apply combined electric magnetic field and ultrasonic field simultaneously, realize that the combined electric magnetic field and the coupled field of ultrasonic field formation control the reaction in process.Combined electric magnetic field is by high frequency magnetic field and low frequency magnetic field combination, and wherein the electromagnetic parameter of high frequency magnetic field is: frequency 1kHz～20kHz, and electric current 10～500A presents significantly disturbance with melt and determines optimum frequency and current value; The electromagnetic parameter of low frequency magnetic field is: frequency is 1～20Hz, and outward current 100～1000A determines optimum frequency and current value by stirring intensity.The frequency 15kHz of ultrasonic field～25kHz, the intensity 6.1W/cm of ultrasonic field
2～60W/cm
2
Adopt the principle of combined electric magnetic field and ultrasonic field coupling to be among the present invention:
The combination of high frequency magnetic field and low frequency magnetic field can realize the complementation of action effect, and the stirring action of low frequency magnetic field is obvious, is aided with the effect of ultrasonic vibration and high frequency magnetic field electromagnetic distu, can obviously improve the dynamic conditions of in-situ synthesized reaction; The outstanding role of high frequency magnetic field is the electromagnetism thermal shock effect, can increase the fluctuation of energy of fusant reaction particle, is aided with the cavitation effect and the ultrasonic energy vibration effect of ultrasonic field, can obviously improve the thermodynamic condition of in-situ synthesized reaction.Therefore, the coupling outfield of adopting combined electric magnetic field of the present invention and ultrasonic field to form is controlled the in-situ synthesized reaction process, the kinetics and the thermodynamic condition of building-up process have effectively been improved, realization is to more effective control of reaction in building-up process, and then reaches control particle size, pattern and equally distributed purpose in matrix.
Compared with prior art the advantage that has of the present invention is:
Matrix material is synthetic under the coupled field effect of combined electric magnetic field and ultrasonic field formation, has overcome the deficiency that only applies electromagnetic field or ultrasonic field, has also overcome single electromagnetic field and ultrasonic field coupled deficiency, and its most significant advantage is as follows:
(1) the present invention improves the thermodynamic condition and the dynamic conditions of building-up process simultaneously, improved the speed of each link of fusant reaction building-up process, effectively shorten the utilization ratio and the recovery rate of generated time and raising reactant, experimental results show that: the reaction generated time shortens 30～50% than prior art, and the utilization ratio of reactant is recovery rate raising 10～20%.
(2) coupling of combined electric magnetic field and the ultrasonic field cluster that can suppress wild phase is assembled and to be grown up, particle size is controlled at nanoscale, and the obvious roundingization of particle, has improved particle and high base strength, and help particles dispersed, improve the over-all properties of matrix material.
Description of drawings
Fig. 1 synoptic diagram of the present invention
Caption: 1 Composite Melt; 2 containers; 3 high frequency magnetic fields; 4 low frequency magnetic fields; 5 horn.
The sem photograph of Fig. 2 embodiment 1 preparation material
The sem photograph of Fig. 3 embodiment 2 preparation materials
Embodiment
The invention will be further elaborated below in conjunction with embodiment.Embodiment only is used to illustrate the present invention, rather than limits the present invention by any way.
Embodiment one: preparation (Al
3Zr
(s)+ Al
2O
3 (s)) particle enhanced aluminum-based composite material
Starting material: matrix metal: commercial-purity aluminium; Pressed powder: industrial carbonic acid zirconium (Zr (CO
3)
2) pulvis (purity is 99.20%), the refining air release agent and the agent of skimming;
Reaction in equation: 13Al
(1)+ 3Zr (CO
3)
2 (s)=3Al
3Zr
(s)+ 2Al
2O
3 (s)+ 6CO
2↑
Particle wild phase: Al
3Zr
(s)And Al
2O
3 (s)
Preparation process is as follows:
(1) at first carry out Metal Melting and powder preparing:
Commercial-purity aluminium 10Kg melts in 25kW crucible type resistance furnace and is warmed up to 850 ℃, outgases, skims.Agents useful for same is all fully dried down at 250 ℃～300 ℃, wherein Zr (CO
3)
2Grind to form fine powder (granularity is less than 100 μ m), stand-by after the weighing, Zr (CO
3)
2The weight that adds is 10% of weight metal.
(2): the multielement magnetic field combination is the preparation Composite Melt down:
After melt temperature is qualified, carry out initial refining, good and meet in the container 2 of molten metal impouring band heat insulation function of temperature requirement (850 ℃) in refining, in melt, be pressed into solid reactant Zr (CO with bell jar
3)
2Powder.
Open high frequency magnetic field and low frequency magnetic field successively, the electromagnetic parameter of adjusting combination field is to stated limit, and wherein the electromagnetic parameter of high frequency magnetic field is: frequency 1kHz, electric current 500A; The electromagnetic parameter of low frequency magnetic field is: frequency is 2Hz, outward current 900A.Open Vltrasonic device then, adjustment ultrasonic field parameter is: the frequency 15kHz of ultrasonic field, the intensity 6.1W/cm of ultrasonic field
2, reaction is closed all outfields after finishing, and the molten bath is left standstill and is prepared casting after 3 minutes.
(3): metal pours in the metal pattern die, makes composite castings, sampling analysis, dense internal organization, solidified structure defectives such as nothing is loose, shrinkage cavity, particle size＜100nm, the metal nano-particle reinforced composite, the as-cast structure sem photograph of material as shown in Figure 2.
Adopt the outstanding feature of this invention to be: particle size obviously refine to nanoscale, the particle roundness improves, no cluster phenomenon, reaction times shortened to 10 minutes from 20～30 minutes, the rate of the receipts of reactant improves about 20%, illustrate that speed of reaction and productive rate improve, thereby the thermodynamics and kinetics condition that confirms the reaction building-up process is substantially improved.
Embodiment two: preparation Al
2O
3 (s)Particle enhanced aluminum-based composite material
Starting material: matrix metal: commercial-purity aluminium; Pressed powder: industrial carbonic acid cerium (Ce
2(CO
3)
3) pulvis (purity is 99.20%), the refining air release agent and the agent of skimming;
Reaction in equation: 4Al+3CeO
2→ 2Al
2O
3+ 3Ce
Particle wild phase: Al
2O
3 (s)
Preparation process is as follows:
(1) at first carry out Metal Melting and powder preparing:
Commercial-purity aluminium 10Kg melts in 25kW crucible type resistance furnace and is warmed up to 850 ℃, outgases, skims.All 250 ℃～300 ℃ fully oven dry down, wherein cerous carbonate grinds to form fine powder (granularity is less than 100 μ m) to agents useful for same, and is stand-by after the weighing, and the weight that cerous carbonate adds is 10% of weight metal.
(2): the multielement magnetic field combination is the preparation Composite Melt down:
After melt temperature is qualified, carry out initial refining, good and meet in the molten metal impouring band heat insulation function container 2 of temperature requirement (850 ℃) in refining, in melt, be pressed into the solid reactant cerium carbonate powder with bell jar.
Open high frequency magnetic field and low frequency magnetic field successively, the electromagnetic parameter of adjusting combination field is to stated limit, and wherein the electromagnetic parameter of high frequency magnetic field is: frequency 20kHz, electric current 30A; The electromagnetic parameter of low frequency magnetic field is: frequency is 20Hz, outward current 150A.Open Vltrasonic device then, adjustment ultrasonic field parameter is: the frequency 25kHz of ultrasonic field, the intensity 60W/cm of ultrasonic field
2, reaction is closed all outfields after finishing, and the molten bath is left standstill and is prepared casting after 3 minutes.
(3): metal pours in the metal pattern die, makes composite castings, sampling analysis, and particle size＜100nm, the metal nano-particle reinforced composite, the as-cast structure sem photograph of material is as shown in Figure 3.
Adopt the outstanding feature of this invention to be: particle size obviously refine to nanoscale, the particle roundness improves, no Cluster Phenomenon, reaction time shortened to 12 minutes from 20 minutes, the rate of the receipts of reactant improves about 18%, illustrate that reaction rate and productive rate improve, thereby the thermodynamics and kinetics condition that confirms the reaction building-up process is substantially improved.
Claims (5)
1. the preparation method of a nano particle reinforced aluminum matrix composites, it is characterized in that: the combined electric magnetic field and the ultrasonic field that in the fusant reaction synthesis method prepares the reaction in building-up process of particle enhanced aluminum-based composite material, apply high frequency magnetic field and low frequency magnetic field simultaneously, the coupled field that realization combined electric magnetic field and ultrasonic field form is controlled the reaction in process, and then the purpose that reaches control particle size, pattern and distribute in matrix.
2. the preparation method of a kind of nano particle reinforced aluminum matrix composites according to claim 1, it is characterized in that: the electromagnetic parameter scope of described high frequency magnetic field is frequency 1kHz～20kHz, electric current 10～500A presents tangible disturbance with melt and determines optimum frequency and current value.
3. the preparation method of a kind of nano particle reinforced aluminum matrix composites according to claim 1, it is characterized in that: the electromagnetic parameter of described low frequency magnetic field is: frequency is 1～20Hz, outward current 100～1000A determines optimum frequency and current value by the whole stirring intensity of melt.
4. the preparation method of a kind of nano particle reinforced aluminum matrix composites according to claim 1 is characterized in that: the frequency 15kHz of described ultrasonic field～25kHz, the intensity 6.1W/cm of ultrasonic field
2～60W/cm
2
5. the preparation facilities of a nano particle reinforced aluminum matrix composites, comprise the container (2) that the thermal insulation fire-resistant material is made, it is characterized in that: the high frequency magnetic field coil is installed on the outer wall of container (2), the low frequency magnetic field coil is installed in the outside of high frequency magnetic field coil, leave between high frequency magnetic field and the low frequency magnetic field coil and guarantee the insulating gap, be 2～4cm, the horn (5) of Vltrasonic device is assigned on the top of the Composite Melt (1) in container (2).
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| CN105983682A (en) * | 2015-02-04 | 2016-10-05 | 中国科学院金属研究所 | Method for preparing metal matrix composite under compounding effect of low-pressure pulsed magnet field and ultrasound |
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Application publication date: 20110126 Assignee: Asia-Pacific Light Alloy (Nantong) Technology Co., Ltd. Assignor: Jiangsu University Contract record no.: 2014320000175 Denomination of invention: Method and device for preparing nanoparticle reinforced aluminum base composite material Granted publication date: 20120620 License type: Exclusive License Record date: 20140306 |
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